Conservation and Restoration programme, Masters, Photograph Specialisation
Electrotyping Daguerreotypes: Reconstruction of an Early Reproduction Technique
Student: Magdalena Pilko Student number: 10666664 Supervisor: Clara von Waldthausen, UvA Amsterdam External advisors: Martin Jürgens, Rijksmuseum Amsterdam Dr. Bill Wei, Dutch Cultural Heritage Agency Date: July 2017
Electrotyping Daguerreotypes: Reconstruction of an Early Reproduction Technique
Acknowledgements I am very grateful to Martin Jürgens, photograph conservator, Rijksmuseum Amsterdam, who kindly introduced me to his working methods and most generously provided me with unpublished information and other valuable resources at all times. My course coordinator, Clara von Waldthausen, UvA, I thank for her kind support in many ways, in particular for making materials available as well as for critical reflection and encouragement. I am very grateful to Dr. Bill Wei, RCE, who kindly advised me throughout the process of writing and to Dr. René Peschar, UvA, for his kind contribution of chemical expertise.
Furthermore, I would like to thank all UvA R&C Master / PI students of the metal department, who generously shared their workspace and tools, particularly Michaela Groeneveld and Marianne Nuij for their continued practical assistance. I thank Tonny Beentjes, coordinator of the metal department, UvA, who provided me with his personal rectifier and shared his practical knowledge in electrotyping. Thanks are also due to Tamar Davidowitz, metal conservator, UvA/Rijksmuseum Amsterdam, for her practical introduction into electrotyping.
I thank Nicholas Burnett, conservator, for his warm reception in Cambridge, not only providing me with a bicycle to commute to and from his laboratory but all of his facilities and by contributing data. I am grateful to Dr. Iris Buisman, University of Cambridge, and Dr. Ineke Joosten, RCE, for their patience in the search for image particles with SEM and to Bas van Velzen, coordinator of paper conservation, UvA, for assisting with the use of the Hirox microscope.
Thanks are also due to Anton Orlov, daguerreotypist, San Diego, USA, whom I experienced as a neighbour communicating to me on the making of his daguerreotypes in the most open and comprehensive manner, to Johan de Zoete, graphic craftsman, who provided me with literature and kindly offered further assistance in electrotyping, to Dr. Han Neevel, RCE, for his assistance with the interpretation of XRF and EDS results, to Marinus Ortelee, daguerreotypist, for offering the possibility to make daguerreotypes as well as to Rosina Herrera Garrido, Rijksmuseum Amsterdam, Prof. Dr. Marc Koper, professor for surface chemistry, Leiden University, Ellen van Bork, Rijksmuseum Amsterdam/UvA and Sanne Berbers, UvA, for their interest in my work. My fellow students, in particular, Kayleigh van der Gulik, I thank for sharing experiences.
Last but not least, Im profoundly grateful to my family, Michael, Celia and Leonard who enabled me to do this work.
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Abstract (English) Electrotyping Daguerreotypes: Reconstruction of an Early Reproduction Technique, a thesis by Magdalena Pilko in the context of the conservation and restoration master programme with a specialization in photography at the University of Amsterdam, 2017.
In the 19th century the electrotype process was used to reproduce daguerreotypes as copper plate facsimiles. The characteristics of this technique can be studied best by examining the copper copy plate together with its master daguerreotype, but only a very small number of these plate pairs are known today. A reconstruction of the process was therefore attempted to understand whether the results from visual and analytical analysis of historical electrotyped daguerreotypes can be considered as typical characteristics of the process. For this reconstruction, Lerebours instructions from 1843 on electrotyping daguerreotypes, supplemented with information by other authors, were followed as precisely as possible. In addition to a literature study of historical and modern technical sources, three historical objects and reconstructions were photographically documented and examined visually in ambient and ultraviolet (UV) fluorescence light, with X-ray Fluorescence Spectroscopy (XRF) and in the Scanning Electron Microscope with Energy Dispersive Spectroscopy (SEM-EDS). Working parameters for electrotyping daguerreotypes could be specified with a current density of approximately 3.46 A/dm2 for approximately 8 hours resulting in an approximately 0.4 mm thick electrodeposit. These parameters were applied to two contemporary and two 19th century daguerreotypes. The initial results with visual examination and instrumental analysis with XRF and SEM-EDS indicates that during the separation of the plates, the top silver-gold layer including the image particles of the daguerreotype transferred from the daguerreotype to the electrotype. From this we may conclude that it is likely that some kind of surface treatment of the daguerreotype took place prior to electrotyping; however, this aspect is not described in the historical instructions considered in this study. This author went beyond Lerebours instructions by applying a beeswax separation layer on one historical and two contemporary daguerreotypes prior to electrotyping them. This layer produced electrotypes that resemble the original historical objects by visual examination and by SEM microscopy. Although further research on the reconstruction is required, the results of this study as well as the modern daguerreotype electrotypes that were produced can be used to aid in the identification of yet unidentified daguerreotype electrotypes and in the study of their mechanisms of aging.
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Abstract (Dutch) Deze scriptie Electrotyping Daguerreotypes: Reconstruction of an Early Reproduction Technique is geschreven door Magdalena Pilko in het kader van de Masteropleiding in Conservering en Restauratie van Cultureel Erfgoed, specialisatie fotorestauratie, aan de Universiteit van Amsterdam, 2017.
In de 19e eeuw werden door galvanotechniek reproducties van daguerreotypieën op koperplaten gemaakt. Deze techniek, toegepast op daguerreotypieën, kan het beste bestudeerd worden aan de hand van een koperplaat kopie met zijn master daguerreotypie, maar er zijn maar weinig dergelijke sets van platen bekend. Daarom is er geprobeerd om dit procedé te reconstrueren, om zodoende te begrijpen of kenmerken van geanalyseerde historische galvano-daguerreotypieën met dit procedé geproduceerd zijn. De instructies van Lerebours over galvanoplastische reproducties van daguerreotypieën uit 1843 is aangevuld met informatie door andere auteurs en dat procedé is zo nauwkeurig mogelijk gereconstrueerd. Naast het bestuderen van historische en technische literatuur zijn drie historische objecten en resultaten van de reconstructies fotografisch gedocumenteerd en visueel onderzocht in zichtbaar licht en met ultraviolet (UV) fluorescentie, met X-ray Fluorescentie Spectroscopie (XRF) en met Scanning Electron Microscopie met Energy Dispersive Spectroscopy (SEM-EDS). Werkparameters voor galvano-daguerreotypieën konden worden bepaald. Een stroomdichtheid van ongeveer 3,46 A/dm2 gedurende ongeveer acht uur, resultereerde in een ongeveer 0,4 mm dikke elektrodepositie. Deze parameters werden toegepast op twee hedendaagse en twee historische daguerreotypieën. Resultaten daarvan zijn niet vergelijkbaar met de onderzochte historische galvano- daguerreotypieën. Visueel onderzoek en analyse met XRF en SEM-EDS geven aan dat tijdens de scheiding van de platen de bovenste zilver-goud laag inclusief beelddeeltjes van het daguerreotype overgebracht wordt op de galvano-daguerreotypie. Hieruit kunnen wij concluderen dat het waarschijnlijk is dat er een soort behandeling van de daguerreotypie voorafgaand aan het galvaniseren plaatsvond, die niet in de gebruikte historische instructies is beschreven. De auteur heeft Lerebours instructies uitgebreid en een scheidingslaag in de vorm van een bijenwaslaag op een historische en twee hedendaagse daguerreotypieën aangebracht, voorafgaand aan het galvaniseren. Dit heeft het mogelijk gemaakt galvano-daguerreotypieën te maken die volgens visueel en SEM-EDS onderzoek op de onderzochte historische objecten lijken. Hoewel verder reconstructieonderzoek nodig is, kan het resulterende onderzoek evenals de gereconstrueerde galvano- daguerreotypieën gebruikt worden bij de veilige identificatie van nog niet geïdentificeerde galvano- daguerreotypieën en bij de studie naar hun veroudering.
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Table of contents
1. Introduction to the research project ...... 7 1.1. Introduction ...... 7 1.2. Research objectives ...... 8 1.3. Methodology ...... 8
2. Literature review ...... 10 2.1. Terminology...... 10 2.2. The daguerreotype...... 10 2.3. Introduction to electrochemical terms ...... 11 2.4. Historical context of daguerreotype electrotypes ...... 12 2.5. Current scientific knowledge on the electrotype process as applied to daguerreotypes...... 13 2.6. Instructions on electrotyping daguerreotypes in 19th century sources ...... 15 2.6.1. Choice of historical process description ...... 15 2.6.2. Lerebours' process description supplemented by other sources as implemented in initial testing and the reconstruction ...... 17
3. Experimental Procedure...... 23 3.1. Initial testing and reconstructions...... 23 3.1.1. Setup of the electrolytic cell ...... 23 3.1.2. Initial tests with silver coupons...... 24 3.1.3. Reconstruction tests with daguerreotypes ...... 25 3.2. Examination methods ...... 27 3.2.1. Visual examination...... 27 3.2.2. UV Fluorescence examination ...... 28 3.2.3. XRF examination ...... 28 3.2.4. SEM-EDS examination...... 28
4. Results ...... 30 4.1. Results of the examination of the SM-1927-1680 1 & 2 plates and the NB plate...... 30 4.1.1. Results of the visual examination of the SM-1927-1680 1 & 2 plates ...... 30 4.1.2. Results of the UV fluorescence examination of SM-1927-1680 1 & 2...... 34 4.1.3. Results of the XRF examination of SM-1927-1680 1 & 2...... 34 4.1.4. Results of the SEM-EDS examination of SM-1927-1680 1 & 2 ...... 35 4.1.5. Results of visual examination of the NB plate ...... 36 4.1.6. Results of XRF examination of the NB plate...... 37 4.1.7. Results of SEM-EDS examination of the NB plate ...... 38 4.2. Results of initial tests with silver coupons...... 38 4.2.1. Appropriate consistency of the electrodeposit ...... 39 4.2.2. Thickness and rate of electrodeposition...... 39 4.2.3. Separating the electrotype and the silver coupon...... 40 4.3. Results of the examination of the reconstructions...... 40 4.3.1. Results of the visual examination of the reconstructions ...... 40 4.3.2. Results of UV fluorescence examination of the AO plates ...... 45 4.3.3. Results of XRF of the AO-4-1, AO-4-2, AO-4-2 electrotype plates ...... 45 4.3.4. Results of SEM-EDS examination of the AO-1 and AO-2 plates ...... 45
5. Discussion...... 49 5.1. Discussion of main results ...... 49
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5.2. The identification of daguerreotype electrotypes...... 51
6. Conclusion ...... 55
7. References...... 56
List of figures and tables ...... 60
Appendices...... 62 Appendix I Terminology...... 62 Appendix II References in literature to makers of daguerreotype electrotypes ...... 63 Appendix III Overview of potential daguerreotype electrotypes in collections ...... 64 Appendix IV Historical instructions on electrotyping daguerreotypes...... 65 Appendix V Materials and Suppliers...... 66 Appendix VI Documentation of specimens before and after electrotyping...... 68 VI.1. Anton Orlov daguerreotypes (AO) ...... 68 VI.2. AO-1 plate ...... 69 VI.3. AO-2 plate ...... 70 VI.4. AO-3 plate ...... 71 VI.5. AO-4 plate ...... 72 VI.6. UvA study collection plate (UvA) ...... 73 VI.7. Daniel Blau plate (DB) ...... 74 VI.8. Marinus Ortelee daguerreotype (MO) ...... 76 Appendix VII XRF examination...... 77 VII.1. SM-1927-1680 1 & 2 and NB plate ...... 77 VII.2. NB plate ...... 79 VII.3. AO-4 plates ...... 80 Appendix VIII SEM-EDS examination ...... 82 VIII.1. SM-1927-1680 1 & 2 ...... 82 VIII.2. NB plate ...... 87 VIII.3. AO-1 plates...... 89 VIII.4. AO-2 plates...... 95
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1. Introduction to the research project
1.1. Introduction
The daguerreotype process, publicly announced in 1839, was the first commercially successful photographic process. A daguerreotype has an extremely high image resolution due to image-forming silver-amalgam particles of submicron size on top of a silver-plated copper plate without the presence of a binder. Daguerreotypes were often gold-toned, which improved their optical qualities and their physical resistance.1 The daguerreotype was very successful, but its major disadvantages were that the photographic image was mirrored and difficult to reproduce. Several attempts were therefore made early on to find a method for reproducing daguerreotypes.2 One method that proved successful was the electrotype process. Electrotyping, or electroforming, is the reproduction of a metal artefact by means of the electrodeposition of metal ions upon its conductive surface, resulting in a physical copy that is subsequently separated from the original artefact.3 In the 19th century, this process was widely applied to fabricate copper reproductions of various kinds of industrial articles and art objects such as sculptures or medals.4 An electrotype taken from a daguerreotype depicts a mirrored image on a copper plate. Figure 1 depicts a schematic diagram of the composite structure of a daguerreotype and its electrotype reproduction.
Figure 1. Schematic cross- section of a daguerreotype and its electrotype.5 Illustration: M. Pilko.
Although the reproductions of daguerreotypes obtained by electrotyping were praised for their fine results in 19th century sources such as in a treatise by the Austrian physician and photographer Anton Martin, at present only 13 copper plates have been identified as probable electrotypes in different collections worldwide (see Appendix III Overview of potential daguerreotype electrotypes in collections).6 Little has been published on the process and its characteristics, and it is therefore possible that unidentified daguerreotype electrotypes exist in collections. To gain a better understanding of the technology and materials of the electrotype process as applied to daguerreotypes, the photograph conservator of the Rijksmuseum Amsterdam, The Netherlands, Martin Jürgens, in partnership with others, has been researching this process. The process
1 Gold-toning daguerreotypes is known also as gilding, a process of rapid hardening of the image particles in which mercury is replaced by gold. Barger 1991: 159. 2 Find several examples of processes for the reproduction and transfer of daguerreotypes in Eder: 1927: 35. 3 Larsen 1984: 17 and ASTM B832-93 (2013) 2013: 1. 4 See for example Meissner, Doktor and Mach on electrotypes from sculptures (2000) and Wharton on electrotypes from medals (1984). 5 As model for daguerreotype served a transmission electron microscopy (TEM) cross-section image. Marquis et al. 2015: 441. 6 Martin 1856: 110.
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is best understood when comparing an electrotype with its matching daguerreotype. However, of the known plates existing, only four are stored together with their matching daguerreotypes. To date, Jürgens has analysed two daguerreotype electrotypes and their matching daguerreotypes, and one presumed daguerreotype electrotype without a matching daguerreotype. However, the analysis of but two pairs of plates (daguerreotype and electrotype) and one single electrotype plate is statistically insufficient to confirm that these objects are indeed daguerreotype electrotypes. In addition, it is unclear whether the results of the analysis performed so far constitute typical characteristics of daguerreotype electrotypes or if they are unique to the examined plates. One way of achieving a better understanding of the process is to reconstruct the process following historical recipes. This was the main focus of this thesis.
1.2. Research objectives
The main objective was the reconstruction of the electrotype process as applied to daguerreotypes based on historical instructions. Further questions concerned the translation of historical instructions and materials to materials available today, and also the practical parameters for the reconstruction, such as the appropriate consistency of the electrodeposit. The information gained from making reconstructions should: contribute to the identification of electrotype plates in collections, enhance knowledge on the material-technological aspects of the process, help establish preservation measures for the plates, as far as possible.
The results of this research can eventually lead to the development of a protocol for the identification of electrotypes made from daguerreotypes. However, due to time constraints, the development of such a protocol is beyond the scope of this research.
1.3. Methodology
In order to establish a basis for the reconstruction experiments, a detailed literature study of historical, technical and art historical sources was conducted first (Chapter 2). Nine historical process descriptions from between 1841 and 1860 were found. Of these, the instructions written by Noël M. P. Lerebours in 1843 were chosen as the main source to use for reconstructing daguerreotype electrotypes. Relevant details in other sources that complemented Lerebours instructions were added to the reconstruction description as deemed necessary. Modern literature from contemporary practitioners of electrotypy was used to gain a contemporary understanding of the electrochemical principles and translate information from historical sources to materials available today. An unpublished report by Martin Jürgens (2015) on the detailed examination of a daguerreotype and its matching electrotype (DM-69896 1 & 2) owned by the Deutsches Museum in Munich, Germany, aided particularly in the understanding of process-inherent features of these objects.7 The structure Jürgens used in his report served as an example in the examination of historical plates during this research.
7 Jürgens 2015.
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Three historical plates were examined to obtain a first-hand reference for the comparison of visual features and the results of measurements and analysis (4.1): a daguerreotype (SM-1927-1680 1) and its matching electrotype (SM-1927-1680 2) from the London Science Museum and a single electrotype plate in the private reference collection of Nicholas Burnett, Museum Conservation Services Ltd., (NB plate) were examined together with Martin Jürgens and Nicholas Burnett in Cambridge, UK. The examination of these objects took place in situ within two days. During this relatively short time frame and due to the fact that some analytical instruments were not available, not all analysis could be performed that had been performed by Jürgens on the DM-69898 plates. The observed features of the daguerreotype and the copper plates that are probably a result of the electrotype process are described, and results from the reconstruction are compared to these. Next, experiments were performed to reconstruct the electrotype process following Lerebours instructions. Initial testing was carried out on small silver coupons that simulated the silver surface of a daguerreotypes bare plate. The parameters that proved to be successful were then used to make electrotypes from modern and historical daguerreotypes. Modern daguerreotypes were produced specifically for the reconstruction and historical daguerreotypes were taken from the University of Amsterdam (UvA) and Rijksmuseum Amsterdam study collections. The results of the reconstruction and the historical objects were photographically documented and examined visually in ambient light at various angles of incidence and in ultraviolet (UV) fluorescence, as well as with optical stereomicroscopy and digital microscopy. This visual examination had the goal of determining process-specific features of daguerreotype electrotypes. X-ray Fluorescence Spectroscopy (XRF) analysis was conducted in order to detect the elemental composition of the materials involved. The implications of the process of separating the two plates for the microstructure of the plates surfaces were of particular interest for their characterization. For this reason, the reconstructions and the historical objects were also examined in a Scanning Electron Microscope with Energy Dispersive Spectroscopy (SEM-EDS). In general, the integrity of the plates was preserved by using only non-invasive examination techniques.
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2. Literature review
2.1. Terminology
The terminology for the process discussed in this thesis varies in historical sources and in different languages (see Appendix I). The terms galvanoplasty, electroforming and electrotyping are the most common terms used in historical and contemporary literature. These terms are used in a general sense and not exclusively with regard to daguerreotypes. The chemist William Draper introduced the term tithonotype in 1843 when discussing reproduction methods for daguerreotypes. However, this term is also applied to other reproduction processes.9 In at least one source, the apparatus itself is referred to as an electrotype.10 As the term electrotype is most common in both historical sources as well as in contemporary conservation literature, it is this term that will be used in this thesis to describe the object made by means of electrotypy.11 To refer specifically to the electrotype from a daguerreotype the term daguerreotype electrotype will be used. The action of copying daguerreotypes by electrotypy will be referred to as electrotyping and the process will be referred to as the electrotype process.
2.2. The daguerreotype
In short, making a gold-toned daguerreotype entails the polishing of a silver-plated copper plate until the surface is highly reflective, much like that of a mirror. Polishing is usually performed in the direction opposite to the way the image is viewed, for example, a daguerreotype in portrait format is polished horizontally.12 The silver surface is made light-sensitive by exposure to the halogen vapours iodine and/or bromine. After exposure to light from a lens in a camera, the image is developed by fuming the plate with mercury vapours. This results in the creation of image-forming particles on the plates surface, which consist of silver-mercury amalgam.13 Residual, unexposed silver salts are then removed by fixing the plate in a solution of sodium thiosulfate. From 1840 on, this is followed by gold-toning using a gold chloride solution.14 Recently, Marquis et al. and Vicenzi, Landin and Herzing found gold-toned daguerreotypes to have a continuous layer of silver and gold covering the silver surface and the silver-mercury particles. This layer was found to anchor the particles to the substrate by fully encapsulating them instead of only coating them on the outside.15 The daguerreotype thus holds a negative image with a particulate structure. This structure is only perceived as an image as a result of the difference between diffuse reflection of light at the relatively rough surface of the image particles and direct reflection at the smooth polished silver surface. The daguerreotype image appears positive when the silver surface reflects dark contrasting with the
9 Draper introduced the term tithonotype in 1843. Firstly, he refers to copies of daguerreotypes using isinglass, and at a later point he also mentions copper tithonotypes. Draper 1843 (May): 366; 1843 (September): 175. 10 Lerebours 1843 (September): 117. 11 McLeod 2010, Scott 2013. 12 Graphics atlas. 2017 Image Permanence Institute. 26 February 2017.
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whitish-reflecting image particles, and negative when the silver surface reflects light. In the latter case, the image particles block the reflected light and form dark silhouettes.
2.3. Introduction to electrochemical terms
In the following section, a brief outline of the electrochemical principles of the process is provided for better understanding and clarification of some general terms that are used throughout the thesis. Electrotyping or electroforming is commonly considered to be a form of electroplating.16 The main difference between the processes is the following: whereas the adhesion of the deposited coating to the substrate is desirable in electroplating, in electrotyping the substrate is treated to specifically prevent adhesion. However, the electrochemical principles for both processes are basically the same. Figure 2 shows a schematic diagram of the electrotype process.
Figure 2. Schematic electrolytic cell. Illustration: M. Pilko.
An electrolytic cell is supplied with an external potential source, which can be a battery or a rectifier. A direct current of electrons passes through a solution of metal ions known as the electrolyte. In the particular case of electrotyping daguerreotypes, the electrolyte is an acidic copper (II) sulfate solution consisting of copper (II) sulfate dissolved in water and sulfuric acid. This solution contains positively charged copper (II) ions (cations), negatively charged sulfate ions (anions) and hydronium cations. The electric current is connected to the electrolyte by means of electrodes. The negatively charged electrode (cathode), in this case the daguerreotype, attracts the copper cations and provides them with electrons. As a result, the copper cations are reduced to metallic copper, and electrodeposition takes place on the surface of the daguerreotype. The reduction reaction applicable to this process is the following:
Cu2+ + 2e- Cu (s)
The hydronium cations are also attracted to the daguerreotype, but, according to the Electromotive Force Series, the reduction potential of the hydronium ion is lower than that of the copper (II) cation.17 This means that the copper (II) is more reactive and that copper will precipitate on the plate first. The
16 Lowenheim 1978: 115. 17 A list of the Standard Electromotive Force Potentials is given for example in Jones 1996: 44.
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hydronium only gets reduced if the potential is high enough and if the ratio of hydronium electrons to copper cations is higher.18 This is usually not the case for electroplating when conventional settings are used.19 The oxidation reaction takes place at the positive electrode, or anode, which in the case of the daguerreotype electrotype is a plate of copper. The anode closes the electric circuit by removing electrons from the copper. As a result, the copper plate is gradually corroded while continuously supplying the electrolyte with copper cations in order to maintain a sufficient amount of copper cations in the bath. The oxidation reaction applicable to this process is the following:
Cu (s) Cu2+ + 2e-
Under acidic conditions the sulfate anion can be reduced to sulfurous acid (and water) but this reduction potential is lower than that of the reduction of the copper (II) cation to copper. Moreover, the sulfate anions will migrate towards the positively charged anodic surface of the copper plate, and will not be oxidized unless the supplied direct current is very large.20 For a more in depth understanding of the transport of metal ions through the electrolyte and their adsorption and precipitation at the cathodic surface, see for example Nasser Kanani.21
Current density When a direct current passes through the cathode and enters the electrolyte, copper will precipitate on the cathode, but the deposit can be of differing quality, ranging from crystalline and non-coherent, dark brown, and brittle, to high quality copper that is coherent, rose-coloured, and flexible. In modern electroplating, the correct electric intensity is calculated in advance. The key parameter is not the total current, but the current density.22 This is the current flowing to a unit area of an electrode surface, in Ampere per square decimetre (A/dm2).23 The current density needs to be applied within certain limits to ensure a high-quality deposit. For electrotyping with an acid copper sulfate electrolyte, Larsen advises a cathode current density between 0.5-1.5 A/dm2.24 For electrotyping with the same electrolyte, ASTM B832-93 allows a greater margin of 1-10 A/dm2.25
2.4. Historical context of daguerreotype electrotypes
Electrotyping dates back to observations made by several individuals of the 19th century. Among these was the Prussian scientist Moritz Hermann von Jacobi, who was the first to understand its practical possibilities in 1838.26 It remains unclear who the first person was to electrotype a daguerreotype and when precisely this took place, and it is possible that several individuals experimented with the process independently. In 1843, the optician and daguerreotypist of the observatory in Paris, Noël M.
18 Larsen 1984: 18. 19 Larsen 1984: 35. 20 Larsen 1984: 22. 21 Kanani 2004: 141ff. 22 Larsen 1984: 24. 23 ASM International Handbook Committee 1998: 4. 24 Larsen 1984: 50. 25 ASTM B832 -93 (2013) 2013: 6. 26 Heinrich, 1938: 566.
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P. Lerebours, refers to his collaborator, the physician Hippolyte Louis Fizeau, as being the first.27 The German photographer and scientist, Hermann Krone, who gives a full description of the process in his treatise Die für alle Zeit von praktischem Wert bleibenden photographischen Urmethoden (1907) also points to Fizeau as the inventor in 1841.28 The proceedings of the French Academy of Sciences indeed report the presentation of daguerreotype electrotypes made by Fizeau on 24 May 1841.29 A different source from 1848 reclaims the invention for the Parisian optician and daguerreotypist Charles Chevalier.30 In his Encyclopedia of printing, photographic and photomechanical processes (1990), Luis Nadeau refers to the tithonotype as a process for obtaining metallic copies of daguerreotypes by electrotypy discovered by J. W. Draper, of New York. Nadeau does not indicate a specific date.31 Accounts by for example Chevalier or Lerebours give an understanding of the daguerreotype electrotype the plate itself as a separate entity, the final result of the process. However, the source for electrotyping daguerreotypes could also originate in the context of printing. Daguerreotype electrotypes are an offspring from earliest photo history when photography was still rivalling with the graphic arts, which had much experience in producing fine images that could easily be printed and spread to a larger audience.32 An account from as early as 1840 mentions electrotyping daguerreotypes in one line with electrotyping engraving plates.33 It appears possible that Fizeau at least initially also intended to use the daguerreotype electrotype as a printing plate. This is supported by a short reference to Fizeau in the extensive works of the Austrian photo-chemist Josef Maria Eder.34 In 1841, Fizeau, together with his former teacher Alfred Donné, actually developed a method to pull intaglio prints from etched daguerreotypes. His method also partly entailed the use of electroplating.35 However, Eder also states that Fizeau had poor results with printing from daguerreotype electrotypes. Hippolyte Fizeau, Alphonse Poitevin and Walter Woodbury were pioneering experimental photographers to whom some of the known existing daguerreotype electrotypes are currently attributed. References to at least 13 other makers of daguerreotype electrotypes were found in several sources, indicating that the process was possibly more widely used than previously thought (Appendix II References in literature to makers of daguerreotype electrotypes). It is not known when the practice of this technique came to an end, but it can be assumed that this coincided with the decline of the daguerreotype process around 1860, at the latest.36
2.5. Current scientific knowledge on the electrotype process as applied to daguerreotypes
To the knowledge of this author, there are no modern publications on electrotyping daguerreotypes, and a reconstruction of the process following historical recipes has not been attempted to date. As can be seen from the lack of contemporary publications, these objects have not attracted much attention in cultural institutions. Reference to daguerreotype electrotypes in contemporary sources
27 Lerebours 1843 (September): 117. 28 Krone, 1985: 35. 29 Académie des Sciences 1841: 957. 30 Pelouze 1848: 713. 31 Nadeau 1990: 450. 32 More information on printing attempts from daguerreotypes is given in: Bonetti 2014: 30- 43. 33 Watt Watt 1840: 344. 34 Eder 1905: 73. 35 Font-Réaulx 2008: 19, Krone 1985: 40. 36 Barger, 1991: 2.
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were found in French Daguerreotypes by Janet Buerger (1989). Buerger was curator of photography at the George Eastman House at the time of publishing the book. She writes a short note on Fizeaus duplication methods for daguerreotypes and gives an illustration of a daguerreotype and its photogalvanic copy (see Appendix III, No. 4).37 Susan Barger, who conducted extensive research on daguerreotypes at the Materials Research Laboratory of the Pennsylvania State University, mentions Drapers tithonotype shortly with reference to Drapers original text Note on the Tithonotype from 1843, which is one of the recipes considered in this thesis.38 In his book on German daguerreotypes, the German conservator Jochen Voigt briefly mentions a daguerreotype electrotype from the Grassi collection in Leipzig, of which he includes two images.39 The plate in the Grassi collection is listed along with three other assumed daguerreotype electrotypes on Daguerreobase, an online daguerreotype database managed by the conservation department of The Netherlands Museum of Photography in Rotterdam.40 In their article Electrotypes in Science and Art, David Scott, a professor in the UCLA conservation program, and Donna Stevens, a senior metals conservator at the Victoria & Albert Museum name Levi Hill as a maker of daguerreotype electrotypes.41 However, Hills process description is an exact transcript of Lerebours text from 1843.42 Upon review, historical sources on electrotyping daguerreotypes appear more numerous than they substantially are and, as in the example of Hill, simply appear to be republished by other authors. In their publication, Scott and Stevens take a close look at the microstructure of electrotype replicas such as vases, which prove to be very different from actual worked and annealed copper artefacts. Even though this kind of research might be considered helpful in the identification of electrotypes in general, the applied method is destructive, so other kinds of analysis such as SEM-EDS appear more suitable for research on daguerreotype electrotypes. The most substantial research on daguerreotype electrotypes is documented in the unpublished report by Martin Jürgens (see chapter 1.3.) on the DM 69896 plates. It includes results of photo documentation and examination using a 3D digital microscope (Hirox), XRF, SEM-EDS, Infrared Fourier Transform Spectroscopy (FTIR) and UV fluorescence. The documentation of the edges of the DM-69896 electrotype was particularly useful for the reconstruction performed in this thesis. The copper edges differ from those of the other examined plates in that they display typical matte, bumpy, nodular growth structures (Figure 3).43 Particularly informative was also Jürgens observation of wax traces along the edges on the recto of the daguerreotype (Figure 4). The presence of wax on the recto could potentially have been relevant in the making of the electrotype.
37 Buerger 1989: 86. 38 Barger 1991: 43. 39 Voigt 2004: 42. 40 Daguerreobase. 6 March 2017.
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Figure 3. DM-69896 electrotype verso, Figure 4. DM-69896 daguerreotype, recto, wax along right edge raking light. (raking light photomicrograph), scale bar is 800 µm. Photo: M. Jürgens. Photo: M. Jürgens.
Jürgens research with SEM-EDS indicated that approximately half of all image particles were transferred from the daguerreotype to the electrotype, leaving craters on the surface of the daguerreotype. It is initially surprising that, despite retaining a surface damaged from electrotyping, the daguerreotype still displays a fine and contrasty image. Jürgens remarked that diffuse reflection of light at the craters must be enough to make the image very visible.44 This implies that a protruding image particle, a crater or even a pit on the electrotype is apparently able to scatter incident light in a similar way, as illustrated in Figure 5.
Figure 5. Schematic reflection of light at the daguerreotype and electrotype surface. Incident light is specularly reflected at the smooth daguerreotype and electrotype surface. Disruptions of the smooth surface by particles, craters or pits result in diffuse reflection. Illustration: M. Pilko.
2.6. Instructions on electrotyping daguerreotypes in 19th century sources
2.6.1. Choice of historical process description
We have no information on the production of the historical daguerreotype electrotypes found in collections today. Therefore, the practical instructions on electrotyping daguerreotypes found in
44 Source: e-mail communication with Martin Jürgens, 28.07.2017.
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treatises from nine authors, dating from the daguerrean era, were very helpful.45 The treatises vary in length from half a page to full eight pages (see Appendix IV Historical instructions on electrotyping daguerreotypes). The different instructions also vary in setup and degree of detail but they basically provide similar recipes and tend to be repetitive to a large extent. This coincides with the fact that the underlying chemical principles are essentially the same (see 2.3. Introduction to electrochemical terms). It is difficult to assess to which extent an author actually worked with the process himself or rather just copied other accounts. For example, the metallurgist Alfred Smee states that he has not practiced the process himself, but that he is instead reporting an account of Dr. Symon and Mr. Horn.46 In his treatise, Humphrey Davy quotes a description of the process by daguerreotypist John Fitzgibbon. A written record on electrotyping daguerreotypes actually written by one of the persons to whom historical objects are currently attributed could not be found. The authors appear to have at least partly copied texts from one another. For example, Lerebours compares the appropriate thickness of the electrotype plate to that of a stout card, and the exact same comparison is made by von Pauly.47 Given these circumstances, this author considered the information in the earliest sources to be the most original account on making daguerreotype electrotypes. In addition, this author focused on authors who actually practiced the process themselves. For instance, Chevalier declares that he practiced the process himself, and he gives the first account of electrotyping daguerreotypes as early as 1841. However, the reconstruction of his setup (Figure 6) confronted this author with practical constraints: the daguerreotype to be reproduced is integrated in a battery circuit that requires the use of mercury. As mercury is extremely poisonous, this author decided to use another historical description as starting point.
Figure 6. Illustration of Chevaliers assumed setup for electrotyping daguerreotypes. Chevalier used a device made by Tito Puliti from Florence, which essentially consisted of two vessels, the inner being porous and containing a copper sulfate solution and a cathode, and the outer containing diluted sulfuric acid and an anode (Chevalier 1840: 61). This device appears similar to a horizontal version of a single-cell apparatus as described, for example, in historic manuals by the electrical engineer Walker Charles and the metallurgist Alfred Smee (Smee 1843: 59, Walker 1848: 34). Illustration: M. Pilko.
The second earliest account is from a rivalling optician, Lerebours, who, in his manual Traité de photographie derniers perfectionnements apportés au daguerréotype from 1843, includes a chapter on copying daguerreotypes by the electrotype process. As the original French manual was translated into English in the same year, Lerebours instructions may have reached many readers. Lerebours describes a setup with an external power supply, for which a battery was used (called a Bunsen element).48 This
45Authors considered were: Charles Louis Chevalier (1841), Noël M. P. Lerebours (1843), Theodor von Pauly (1843), John William Draper (1843), George Shaw (1844), L. E. Uhlenhut (1849), Alfred Smee (1841/1852), Samuel Humphrey (1858 and James Napier (1860). After completion of the reconstruction work a tenth source by A. Lipowitz (1845) was found, which for reasons of time could not be considered any further. 46 Smee 1841: 134-135; Smee 1852: 328. 47 Lerebours 1843: 118; von Pauly 1843: 83. 48 Lerebours 1843: 117. 50 Smee 1851: 99, 107.
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setup can be reconstructed to a large extent and can be imagined to work similarly to the illustration in Figure 2, chapter 2.3. Due to the fact that they both appear relatively original, influential and feasible to follow, Lerebours instructions were chosen as the main source for the reconstruction part of this study. However, no clear evidence could be found as to whether Lerebours actually practiced the process himself.
2.6.2. Lerebours' process description supplemented by other sources as implemented in initial testing and the reconstruction
Lerebours setup consists of an external battery and a glass basin with a saturated solution of copper sulfate (see for the original instructions Appendix IV, No. 3 and No. 4). The solution is considered to be sufficiently saturated when copper sulfate crystals cease to dissolve after shaking the solution. According to Lerebours, the following basic steps were performed:
1. The copper plate (positive electrode) is connected to the negative pole of the battery (which is carbon). The gold-toned daguerreotype is connected via a wire, attached at one corner, to the positive pole of the battery (which is zinc). 2. The verso and edges of the daguerreotype are coated with melted beeswax or beeswax in turpentine (2:1) in order to avoid unnecessary deposit of copper. The wax layer requires a certain thickness that is not sufficiently defined by Lerebours. The spot at which the wire is attached to the daguerreotype is kept free of wax in order to allow current to flow. 3. The copper plate is immersed first in the glass basin holding the copper sulfate solution. 4. The daguerreotype is then immersed in the bath. Copper will immediately start to deposit on the daguerreotype and the copper plate will dissolve. During the process, the daguerreotype should be removed only for a short time, if at all, as oxidation may occur and interrupt the process. 5. When the deposit is sufficiently thick (as thick as a stout card), the daguerreotype with copper deposition is removed from the bath and rinsed in water. It is then dried with blotters or sawdust. Droplets are not allowed to remain as these could penetrate between the plates and stain them. Drying may be sped up by wetting the surface with spirits of wine to retain the pearly colour of the copper. 6. The plate of copper deposition is pried off the daguerreotype. If necessary, the daguerreotype is cut down by 2 mm at all edges in order to be able to separate the new copper sheet from it. 7. Touching the electrotype is to be avoided, and since copper will oxidize, the electrotype should immediately be sealed in a frame.
Lerebours instructions were partly not clear to this author or lacked information necessary to reconstruct the process. In the following, Lerebours instructions were therefore supplemented with information from other historical and modern sources as well as translated to modern materials where this was regarded necessary:
Setup of the electrolytic cell Lerebours does not specify the position of the electrodes, but the metallurgist Alfred Smee suggests both horizontal and vertical setups for the general purpose of electrotyping that could both be
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appropriate for daguerreotypes (Figure 7, Figure 8).50 According to Smee, the vertical setup is more suitable for slow plating and for small plates.51 The vertical setup was used in the reconstruction experiments as it also allowed for a simple fixture for the electrodes.
Figure 7 (left). Vertical setup for electrotyping, with a battery to the right side.52
Figure 8 (right). Horizontal setup for electrotyping, with a battery to the right side.53
Connecting the electrodes Lerebours description on connecting the electrodes with the battery is contradictory to the contemporary understanding of a functioning electrolytic cell. Even though Lerebours' descriptions are in accordance with historical accounts by Smee and Shaw, modern terminology is different.54 As explained in Section 2.3, in an electrolytic cell the copper plate is termed the positive electrode (anode) and connected to the plus pole of the battery whereas the daguerreotype is the negative electrode (cathode) and connected to the minus pole of the battery.55
Mixing the copper sulfate solution In contemporary electrotyping, sulfuric acid is generally added to the copper sulfate solution to improve the quality of the copper deposit. For this reason, it was used in all the reconstructions even though Lerebours does not mention it. This was justified by another source from 1840, which has detailed instructions on the preparation of the electrolyte, which also mention the addition of sulfuric acid.56 Anton Martin also describes the use of sulfuric acid for electrotyping and attributes to it an increased flexibility of the copper deposit.57 For the preparation of the saturated solution, the ratio of sulfuric acid, copper sulfate and water was used as described in Larsen.58 Other additions to the electrolyte, which are common in contemporary electrotyping and which are also described by Larsen, were disregarded, as no reference to their use could be found in 19th century literature. Future research might study the impact of different electrolytic mixtures on making daguerreotype electrotypes.
51 Smee 1851: 294-295. 52 Smee 1851: 99. 53 Smee 1851: 107. 54 Smee 1851: 98, Shaw 1844: 175. 55 Larsen 1984: 42. 56 Allgemeinfaßliche Beschreibung des Verfahrens zur Herstellung galvanischer Kupferstiche 1840: 5-9. 57 Martin 1856: 186, 188. 58 Larsen 1984: 50.
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The anodic copper plate Krone states that a cleaned copper plate having at least the size of the daguerreotype should be used as an anode and that this plate will be consumed during the electrotyping process.59 From this it was concluded that any oxidation products present on the copper plate would need to be removed first and that the copper plate might need to be replaced regularly.
Fixture of electrodes Various methods to fix the battery wire to the electrodes in order to suspend them in the electrolytic bath are known, and each method would probably have a different physical impact on the daguerreotype. Lerebours mentions binding screws with which the battery wire is attached to the daguerreotype.60 Historical binding screws were not available and the historical battery wire probably also looked different. Paper clips were chosen instead of the binding screws to allow the current to flow.
Coating of the daguerreotype According to Lerebours, the daguerreotype is partially coated with wax to prevent electrodeposition where it is unwanted. Pure, hot wax is difficult to apply in a controlled way, due to its rapid cooling after which it becomes thick and difficult to spread. Even though diluting the wax with white spirits facilitates its application, a relatively thick wax layer requires a long time to harden due to the long evaporation time of the solvent. The use of Paraloid B72 in a solvent instead of wax allowed for a more controlled application of the protective coating with a much shorter drying time.
Distance between electrodes The distance between the cathode and the anode is not specified by Lerebours. However, the metallurgist Moritz von Jacobi indicates that the electrodes should not be placed closer than 1½ inches to 2 inches.61 Another metallurgist, Partridge, states that the moulds should be separated from the anodes by a distance of about two inches; but if it is found that the deposit is very dark in colour or granulated in texture, this distance may be increased, thereby increasing the resistance of the solution, which is equivalent in its effect to cutting down the current strength.62 This indicates that there is a certain margin of error for the right distance. In the reconstruction of the process, a distance was therefore chosen that fitted the dimensions of the available basin and the required plating intensity.
Current intensity A single bunsen battery, which Lerebours recommends, generates a potential between 1.86 V to 1.96 V.63 For this study, a low power rectifier was chosen, since it can simulate the characteristics of a Bunsen cell, the reconstruction of which would have been beyond the scope of this research. Von Pauly judges the strength of the electric current by the amount of hydrogen bubbles. If the electric current is too strong, hydrogen bubbles will rapidly form at the daguerreotype, and the deposited
59 Krone and Schmidt 1907: 35. 60 Lerebours 1843: 119, Chevalier mentions soldering as an alternative. Chevalier 1841: 62. 61 Jacobi 1840: 43. 62 Partridge 1908: 102. 63 Sivasankar 2008: 129.
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copper will be spongy and weak.64 Smee writes that the metals are invariably thrown down as a black powder, when the current of electricity is so strong in relation to the strength of the solution, that hydrogen is violently evolved from the negative plate of the decomposition cell.65 Humphrey explicitly warns of a too strong electric current.66
Duration of electrotyping Different sources indicate greatly varying durations for electrotyping daguerreotypes, ranging between 3 to 20 hours. Lerebours states that a single Bunsen battery reproduces a 16 x 22 cm plate within just a few hours. According to von Pauly, Gaudin also succeeded in reproducing daguerreotypes within only 3 hours.67 Draper, on the other hand, indicates that the complete process takes 12-20 hours.68 Von Pauly suggests starting with a cold bath and warming up the solution to 30-40°C once the daguerreotype has received an initial coating of copper, which accelerates plating speed.69 This accelerated plating would then still take 8-12 hours.70 From these diverse specifications it was concluded that, firstly, there is some flexibility in the duration of the process that will result in different thicknesses of the electrotype, and secondly, that the precise duration appears to be dependent on whether the plating speed was accelerated at a certain point or not. For the reconstruction the plating speed was held steady throughout the whole process as this provided the most helpful insight into the characteristics of the copper growth. The duration of electrotyping was evaluted according to the desired thickness of the electrodeposit. Lerebours specification of a stout card was determined to be approximately 0.4 mm.71
Method of separation The historical literature contains several methods of separating the electrotype from the daguerreotype. In regards to Lerebours' recommendations on cutting the edges of the plate, Krone remarks that if the daguerreotype is to be electrotyped more than once, then cutting the edges is to be avoided in order to prevent it from getting smaller each time. Chevalier describes filing off the copper rims that form along the edges and then a knife blade is carefully inserted between the two metallic plates and towards the corners, gently raising and lowering it, to push the plates apart.72 During the initial electrotyping tests, Lerebours instructions were followed, however the edges of the plates were not trimmed in the actual reconstructions. Trimming the edges would have further reduced the size of the already small plates.
Number of copies According to von Pauly and Napier, several daguerreotype electrotypes can be made from a single daguerreotype.73 Fitzgibbon specifies that he made 12 copies from one daguerreotype.74 Draper
64 von Pauly 1843: 84. 65 Smee 1841: 66. 66 Humphrey 1858: 168. 67 Von Pauly 1843: 84. 68 Draper 1843: 175. 69 von Pauly 1843: 82. 70 Humphrey 1858: 168. 71 Lerebours 1843: 118. 72 Chevalier 1841: 64. 73 von Pauly 1843: 84; Napier 1860: 66.
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remarks that more than one copy can be obtained by electrotyping the electrotype.75 This indicates that if the reconstruction is correctly performed, it should be possible to make more than one reproduction. For this reason, making a second reproduction was attempted in the reconstruction.
Considerations in the making of daguerreotypes used for electrotyping A crucial part in the reconstruction concerned the daguerreotype itself. For technical and ethical reasons, the use of historical daguerreotypes was initially not intended in this research. Firstly, the number of historical daguerreotypes is limited. Conservators regard each daguerreotype as unique cultural heritage that should be preserved. Secondly, historical daguerreotypes have aged naturally for over 170 years, their conservation history is not well documented, and the aging of daguerreotypes is not yet fully understood. For this reason, historical daguerreotypes are not representative of the daguerreotypes that were electrotyped at the period of production in the 19th century. Therefore, it was initially decided to use modern daguerreotypes, made according to Daguerres original process, and prepared specifically for this reconstruction experiment. A study indicates that modern daguerreotypes can serve as a good representation for historic plates even though, as with any obsolete photographic process, practice and materials may have undergone change.76 Furthermore, modern daguerreotypes have the advantage that the parameters of their making and their subsequent history is known. However, during this research, the reconstruction plates produced unexpected results, and it was deemed necessary to use historical daguerreotypes as control for a number of aspects of the reconstruction. The contemporary daguerreotypist Anton Orlov was commissioned by this author to make five daguerreotypes (designated AO plates). Given the time of the year during which this research was carried out, it would have been difficult to make daguerreotypes in Europe, as UV and sun light are weak in winter and daguerreotype plates are most sensitive to UV light and the blue region of the spectrum.77 However, Orlov had appropriate climate conditions in San Diego, USA, were he lives. A small plate size (a ninth plate, 72 x 54 mm), similar to the size of the DM-69896 plates, was chosen.78 A large contrast range, sharpness and recognizability were criteria in the selection of the image, all of which are sufficiently present in the view to a backyard as seen from Orlovs studio window. Historical instructions specifically for the production of daguerreotypes to be electrotyped are provided by Samuel Humphrey, and Orlov followed these as closely as possible. Important points were that more iodine and less accelerators were used and the development using mercury lasted ideally relatively long, between 6 to 8 minutes.79 Accelerators are additional halogen vapours, in particular bromine, which are used in increasing the light sensitivity of the silver plate.80 Gold-toning was to be performed slowly, and at low heat, in order to achieve a uniform result. For the reconstructions, it was also important that after gold-toning, the daguerreotype be kept for a day or two, so it may become enfilmed with air.81 This recommendation suggests that corrosion products
74 Humphrey 1858: 169. 75 Draper 1843 (September): 176. 76 Ravines, Chan, Nowell, McElroy 2013: 158. 77 Barger 1991: 30. 78 Plate sizes of daguerreotypes are traditionally specified in proportion to a 1/1 or whole plate, which is 216 x 162 mm (8 x 6 pied). Accordingly, a ninth plate is 72 x 54 mm. Eder 1927: 12. 79 Humphrey 1858: 169. 80 Barger 1991: 45. 81 Draper 1843 (September): 175.
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may benefit the electrotype process. A statement by Smee actually indicates that a film of oxide at other times a thin film of sulphuret will prevent adhesion between the metals.82
82 Smee 1851: 110, see also: Shaw 1844: 94-95.
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3. Experimental Procedure
3.1. Initial testing and reconstructions
This section describes initial testing and the attempted reconstructions. The main goal in the available time was to put the process in practice, so the many variables described in the sections above could be tested only to a minor extent. The setup of the electrolytic cell and the mixing of the electrolyte used for the tests is described first, followed by details of initial testing and producing the reconstructions.
3.1.1. Setup of the electrolytic cell
Figure 9. Setup of the electrolytic cell for the reconstructions. Figure 10. DB Letters are defined in the text below. Photo: M. Pilko. daguerreotype suspended in the electrolytic bath. Photo: M. Pilko.
The experimental setup is shown in Figure 9. The setup consisted of a glass basin (A), 18 x 18 x 13 cm (H x W x D) in which the specimen to be electrotyped (B) was suspended vertically. A Weir 460 rectifier with a DC of 0-60V and a maximum of 3A was used (C). The glass basin was filled with an acidic copper (II) sulfate solution. Two copper wires (diameter = 1 mm) were placed over the shorter sides of the glass basin at a distance of approximately 8 cm (D). A copper plate (anode) (E) cut to a size of 50 x 65 x 0.5 mm with a drilled hole at each corner of one of the long sides was used as anode.83 The copper plate was replaced with each test and rubbed with steel wool prior to its use in order to remove copper oxidation. It was then suspended in the electrolytic bath held by wires hooked into the drilled holes. The rectifier was switched on and amperage and potential were adjusted to the desired values. Next, a specimen (cathode) (B) was suspended on the other wire facing the copper
83 During initial testing, the relatively large size of the anode did not visibly influence the result. However, it is generally advised to have both the anode and the cathode at approximately the same size, which was considered for the actual reconstruction.
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plate. Initially, specimens were suspended in the electrolytic bath by wires hooked into previously drilled holes, later they were fixed with metallic paper clamps (Figure 10). With few exceptions, both electrodes were partially immersed so that the wires would not touch the electrolyte. This made it possible to retain an unprocessed area as a control, and it also made it unnecessary to isolate the copper wires. A cable with battery clamps (F) connected the cathode to the minus pole (G) of the rectifier (black input). A second cable connected the anode to the plus pole (H) of the rectifier (red input). A sheet of polyester (I) on top of the basin weighed down with cardboard was used to prevent evaporation of the electrolyte.
Mixing the electrolyte The acidic copper electrolyte consisted of 300 g copper (II) sulfate in 1500 ml demineralised water and 75 g sulfuric acid (95%, D = 1.84 g/cm3). The copper (II) sulfate was added to boiling water, resulting in a chemical reaction that causes the solution to briefly foam up. A beaker considerably larger than the required size was therefore used in order to prevent spillage. After the solution cooled down, 75 g sulfuric acid was added while stirring. The electrolyte was used at room temperature (20°C). Measuring the electrolyte with pH strips (pH 0-14 universal indicator by MColorpHast) yielded an indicative value of 1 pH. The saturation of the solution was maintained by regularly adding copper sulfate until the crystals ceased to dissolve.
3.1.2. Initial tests with silver coupons
Initial testing with silver coupons had the goal of determining working parameters for: (I) the appropriate consistency of the copper deposit by testing different current densities; (II) the duration of electrotyping needed to obtain a deposit with an approximate thickness of 0.4 mm; and (III) the feasibility of separating the electrodeposit from the coupon. (I) Current densities were tested in a range from 25 to 2.5 A/dm2. (II) The thickness of the electrodeposit and the time taken to obtain it was mainly visually assessed, but it could be mathematically calculated as well. (III) Rims of copper that formed around the edges of the coupon were cut off.
Description of the cathodes used in initial testing The coupons used were obtained from a 925 sterling, polished silver plate, cut into 20 x 20 x 0.5 mm or 10 x 10 x 0.5 mm (H x W x D) squares. A 2 mm hole was drilled through the coupon at the top centre. The coupons were subsequently polished with three different grades of sanding paper (500, 1,200, 1,600 grits) to remove deep scratches. A mirror like, high polish finish was provided with a polishing machine using the polishing paste Rouge de Paris. The polishing paste was cleaned off with white spirit and the coupons were degreased with analytical grade ethanol. A 40% solution of Paraloid B72 in analytical grade acetone was applied on the verso and the edges to prevent copper deposition. The specimens were left to rest for several days to let oxidation occur as indicated in historical instructions.
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3.1.3. Reconstruction tests with daguerreotypes
Successfully established parameters from initial testing were then applied to daguerreotypes with the objective of obtaining one or more electrotypes that would show a reversed image of the daguerreotype, with a positive image in reflected dark and a negative image in reflected light.
Description of the cathodes used in the reconstruction tests The main test specimens were four gold-toned daguerreotypes made by the contemporary daguerreotypist Anton Orlov (AO-1 to AO-4 plates). The plate dimensions varied slightly at approximately 60 x 48 x 0.5 mm (H x W x D). Orlov used daguerreotype substrates made by the traditional roll clad process.84 The plates were polished with a Makita electric random sander, using red rouge and lamp black as a polishing compound. The plates were sensitized consecutively with iodine for 30-40 seconds, bromine for 8-12 seconds, and finally iodine again for 8 seconds. Light exposure was between 25-30 seconds in a camera fitted with a Schneider Super Angulon 65 mm lens. Processing was performed with mercury fumes at 65°C for 5 minutes, and the plate was fixed in a 2- 3% w/v sodium thiosulfate pentahydrate solution in tap water. Gold-toning the developed and fixed image was performed by holding the plate on a layer of aluminium foil over a butane torch. The gold- toning solution consisted of a 0.2% w/v solution of gold chloride in distilled water mixed with a solution of 1 % w/v sodium thiosulfate in distilled water. The pH of the solution was buffered by a 2% solution of sodium metaborate: 1 drop per 2 ml of gilding solution.85 See Appendix VI.1. Anton Orlov daguerreotypes (AO) for details on each plate.
Other test specimens used as control group included two historical and one modern daguerreotype: A 19th century daguerreotype from the UvA study collection, in the following named UvA plate. A 19th century daguerreotype donated to the Rijksmuseum Amsterdam by Daniel Blau, in the following DB plate. The DB plate exhibits scratches overall and appears to have been previously cleaned. A contemporary daguerreotype by a different maker, Marinus Ortelee, in the following the MO plate. In contrast to the AO plates, the MO plate has an electroplated substrate. The MO daguerreotype is also only partially gold-toned. It rested for over one year during which the surface likely oxidized to a great extent.
To expand testing possibilities, several plates were cut into pieces using a jewellers saw with saw blades Nr 2/0. All daguerreotypes were coated on the verso and the edges with a 40% solution of Paraloid B72 in acetone (Figure 11) to prevent copper deposition. In some cases this coating was also applied along the edges on the recto to prevent copper deposition from forming around the edges. After removal from the electrolytic bath, a knife blade was inserted between the metal layers and the electrodeposit was then pried off by hand.
84 The earliest substrate used for daguerreotypes are roll-clad plates, made by hammering or rolling a thin silver plate on a thicker copper plate. Since the mid-1840s electroplated copper plates became more common. Krone and Schmidt 1907: 10. 85 The addition of sodium metaborate is not known in Daguerres original process, but Orlov commonly uses it for gold-toning. Da Silva et al. (2010: 656) also mentions it in the making of modern daguerreotypes for research purposes.
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Figure 11. Coating the edges of the AO-2 daguerreotype with Paraloid B-72 in acetone. Photo: M. Pilko.
Reconstruction tests were carried out either (I) in accordance with Lerebours' instructions as supplemented by other sources, (II) included the application of a coating not mentioned by Lerebours, or (III) attempted to achieve a second reproduction from one daguerreotype. An overview on all tests is given Table 1 and in Appendix VI Documentation of specimens before and after electrotyping.
(I) The following daguerreotypes were electrotyped according to Lerebours instructions as supplemented by other sources and as specified above (2.6.2 and 3.1.1). AO-3 and AO-4 daguerreotypes. Following the first results, further current densities were tested to see if this parameter influenced the separation of the electrodeposit from the daguerreotype. The goal was an electrodeposit with individual nodular formations in an otherwise fine-grained copper surface on the verso, comparable to the verso of the DM-69896 electrotype and SM-1927-1680 electrotype (see Figure 3, Figure 25). DB and MO daguerreotype. The historical DB plate and the contemporary MO plate were electrotyped to understand whether consistent results could be achieved with very different daguerreotypes. Electrotyping the partly toned MO plate offered additional insight into the effect of gold-toning on the process.
(II) Following the results from (I), an additional step was introduced to the process, which is not listed in any of the historical instructions: a thin coating was applied to the recto of the daguerreotype prior to electrotyping. The aim was to add a separation layer at which the copper deposit would easily separate, thereby preventing damage to the surface of the daguerreotype. Other parameters remained unchanged. The use of a coating was tested on the following daguerreotypes: AO-2 daguerreotype. The daguerreotype was coated by swiping over the recto with a piece of deerskin that had previously been dipped into beeswax dissolved in white spirit (2:1). Excess wax was then rubbed off. UvA daguerreotype. The same wax solution was applied in one single swipe, but excess wax was not removed in an attempt to prevent physical damage to the daguerreotype surface. For the purpose of comparison, the daguerreotype was divided into different sections: the upper area of the plate was not electrotyped, the lower left half was coated with beeswax, and the lower right half was left uncoated.
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AO-1 daguerreotype. The same wax solution was applied to the surface.. A thinner and more uniform coating was attempted by heating the daguerreotype with a Bunsen burner during the treatment in order to keep the wax fluid. For the purpose of comparison, a strip near the right edge was left uncoated, and the far right edge was not electrotyped. DB (right half). A coating of boiled linseed oil was applied to the surface of the plate in place of beeswax.
(III) The making of multiple electrotypes from a single daguerreotype is described in the historical literature, so this was also attempted in the reconstruction. The procedure as described for AO-1 was applied to the previously electrotyped AO-2 daguerreotype to produce a second electrotype.
I. In accordance with II. Use of an additional coating III. Making a second electrotype Lerebours instructions as on the recto of the daguerreotype of the same daguerreotype supplemented by other sources (not mentioned by Lerebours)
Contemporary AO-3 Contemporary AO-2 Contemporary AO-3 daguerreotype: daguerreotype: daguerreotype: heated daguerreotype different current densities wax coating on the recto wax coating
Contemporary AO-4 Contemporary AO-1 daguerreotype: daguerreotype: different current densities heated daguerreotype partial wax coating on the recto left half: thin wax coating right edge: uncoated far right edge: untreated control
Contemporary MO daguerreotype 19th century UvA daguerreotype: (lower half) wax coating on the recto top: untreated control lower left half: wax coating lower right half: no coating
19th century DB daguerreotype 19th century DB daguerreotype (left half) (right half) - boiled linseed oil coating on the recto Table 1. Overview of the reconstruction tests carried out on different daguerreotypes.
3.2. Examination methods
3.2.1. Visual examination
Visual examination was performed on the SM-1927-1680 plate, the NB plate and all reconstructions with and without magnification. An optical stereo microscope (Nikon binocular microscope SMZ-10 with a Nikon 20x/13 eyepiece and Euromex fibre optic lights) and a digital microscope (Hirox KH
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7700 with a MX(G)-2016Z lens) was used for examining the reconstructions.86 A Nikon D750 with a 60 mm lens, a Canon EOS 5D Mark III with a 100 mm lens, a Nikon D3s with a 50 mm lens and a colour target (AIC PhD Target 2011 or X-Rite colorchecker) were used for photographic documentation. Photographs of the SM-1927-1680 plate and NB plate with UV radiation and optical stereomicroscopy were taken in situ.87
3.2.2. UV Fluorescence examination
UV fluorescence examination was conducted in a darkened room. The SM-1927-1680 plates were examined with a handheld UV lamp under UV-A (365 nm) and a UV LED torch under UV-A (385 nm).88 The AO-1, AO-2, AO-3, AO-4 plates were examined with a handheld UV lamp under UV-A (365 nm) and UV-C (254 nm) using a NU-4 KL UV light (Benda, 220 V, 2x4 W, 0.18 A).
3.2.3. XRF examination
XRF spectroscopy was conducted on the SM-1927-1680 1 & 2 and the NB plate by Nicholas Burnett in Duxford with a XRF spectrometer (Bruker Tracer LER538) using a rhodium tube, operated at 45 kV and 30 µA, with an average measurement time of 70.43 seconds. The recto and verso of SM-1927- 1680 1 & 2 were each only analysed once due to time constraints. The measurements were conducted in the centre of the recto and verso of both plates. The instrument had no integrated camera to facilitate orientation, nor did the setup allow precise positioning. Nicholas Burnett, who provided this author with the data, measured the recto of the NB plate on a different occasion. XRF spectroscopy was performed by Martin Jürgens on the AO-4 daguerreotype (fragments AO- 4-1, not electrotyped, control area, and AO-4-2, electrotyped area). as well as on the AO-4-2 electrotype (Figure 46). The recto of each object was analysed in a highlight, midtone and shadow region. Measuring the verso was regarded as irrelevant in this context. Analysis was conducted with a XRF spectrometer (Bruker Artax) at the Rijksmuseum/RCE Amsterdam using a molybdenum tube, and a XFlash 3001 SSD detector, operated at 50 kV and 400 µA, with a live time of 122 seconds. Atmospheric argon was eliminated by a helium flush between the spectrometer and the object, as some argon peaks overlap silver peaks. Dr. Han Neevel, scientist of the Cultural Heritage Agency of the Netherlands assisted in the interpretation of the results. Other reconstructions were not examined with XRF spectroscopy due to time constraints.
3.2.4. SEM-EDS examination
SEM-EDS analysis of the SM-1927-1680 1 & 2 plates and the NB plate was performed at the Department of Earth Sciences, Cambridge University, by Dr. Iris Buisman using the FEI Quanta 650 instrument, operated at an accelerating voltage of 15 kV, high vacuum, with spot 4 and a working
86 The exact type of optical stereomicroscope used for the examination of the historical objects could not be established. 87 Photomicrographs were taken using a mobile phone due to the fact that the microscope did not allow the attachment of a camera. 88 The exact type of instrument could not be established.
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distance of 14.6-14.8 mm for images and 13 mm for EDS analysis. The EDS detectors were XFlash 6130 (Bruker) and Esprit software was used to process the data.
Analysis of the AO-1 and AO-2 plates was performed at the RCE in Amsterdam by Dr. Ineke Joosten using a FEI NovaNanoSem 450 device, operated at an accelerating voltage of 15 kV, high vacuum, with spot 3 and a working distance of 5.3-7.4 mm for images. EDS analysis employed a Thermo Scientific Silicon Drift Detector (SDD) with NSS software. The analysed samples were chosen for to their high image quality. SEM analysis of all samples was carried out in situ as these were small enough to fit into the instruments chambers.
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4. Results
4.1. Results of the examination of the SM-1927-1680 1 & 2 plates and the NB plate
The SM-1927-1680 1 & 2 plates and the NB plate are enclosed in typical housings made for daguerreotypes at the time. The SM-1927-1680 plates were housed in a European type passepartout frame and the NB plate in a British wooden and leather case. The maker, date and origin of the plates are unknown.89 According to an inscription on the passepartout, the NB plate could not have been made before 22 November 1843. In the following, features of these objects that are possibly related to or are a result of the electrotype process are described.
4.1.1. Results of the visual examination of the SM-1927-1680 1 & 2 plates
Visual features related to both SM-1927-1680 plates The daguerreotype depicts a portrait of a man in three-quarter view and the copper-coloured electrotype shows the identical image laterally reversed (Figure 12 to Figure 15). The image appears as a positive in reflecting dark and as negative in reflecting light on both plates. However, the documentation picture of the SM-1927-1680 daguerreotype shows a positive image also in reflecting light for some unknown reason (Figure 14). Using Adobe Photoshop software, the images perfectly match when mirroring one and superimposing it onto the other. This also includes fine, parallel horizontal lines, which can be seen with the naked eye on both plates. Horizontal lines on daguerreotypes in portrait format are common and may be associated with marks from polishing.90 Polishing marks on the electrotype were determined to be exact copies of the corresponding marks on the daguerreotype.
Figure 12 (left). SM-1927-1680 daguerreotype, recto, reflecting dark. 77 x 68 x ca. 0.39 mm (H x W x D). Photo: M. Pilko.
Figure 13 (right). SM-1927-1680 electrotype, recto, reflecting dark. 77 x 68 x ca. 0.25 mm (H x W x D)91. Photo: M. Pilko.
89 The SM-1927-1680 plates are a loan from Kings College to the London Science Museum and were previously in the King George III collection. The NB plate was purchased at an auction in Paris. Source: personal communication with Nicholas Burnett, Cambridge, 13 April 2017. 90 Graphics Atlas. 26. February 2017.
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Figure 14 (left). SM-1927-1680 daguerreotype, recto, reflecting light. Photo: M. Pilko.
Figure 15 (right). SM-1927-1680 electrotype, recto, reflecting light. Photo: M. Pilko.
Figure 16 (left). SM-1927-1680 daguerreotype, verso, raking light. The dark mark was possibly caused during gold-toning, by the use of a circular stand. Photo: M. Pilko.
Figure 17 (right). SM-1927-1680 electrotype verso, raking light. Photo: M. Pilko.
There are several indications that the plates were cut down at the edges prior to their separation: The plates are identical in size and just a few millimetres smaller than a standard sixth plate, which would be 81 x 72 mm.92 The edges of both plates are irregular and the serrated marks along the edges can be associated with the cutting marks left by scissors (Figure 25). While the edges of the daguerreotype are slightly bowed upwards, the matching edges of the electrotype are instead bowed downwards (Figure 16, Figure 17, Figure 18, Figure 19). The upper left edge of the daguerreotype is irregularly shaped and it seems likely that the scissors were twisted around at this point resulting in a deformation of the metal. This area corresponds to the upper right edge on the electrotype, where the plate is bent. This bent edge must be the actual end of the electrotype since there are nodular copper growth formations (Figure 20).
92 Plate sizes of daguerreotypes are traditionally specified in proportion to a 1/1 or whole plate, which is 216 mm x 162 mm (8 x 6 pied). Accordingly, a sixth plate is 81 x 72 mm. Eder 1927: 12.
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Figure 18. SM-1927-1680 daguerreotype, recto, top Figure 19. SM-1927-1680 electrotype, recto, top left right corner. corner. Raking light photomicrograph, scale bar is 1 mm. Raking light photomicrograph, scale bar is 1 mm. Photo: M. Jürgens. Photo: M. Jürgens.
Figure 20. SM-1927-1680 electrotype, verso, upper left edge (90° CCW93). Scale bar is 1 mm. Image stitching from 10 raking light photomicrographs. Photo: M. Jürgens.
Part of an unidentified hallmark is present at the upper left corner on the recto of the SM-1927- 1680 daguerreotype (Figure 21). This hallmark was found reproduced at the electrotypes upper right corner on the recto (Figure 22). Due to the thinness of the electrotype plate, the hallmark is also visible on the verso, which demonstrates how the copper deposition precisely followed the daguerreotypes topography during electrotyping.
Figure 21. SM-1927-1680 daguerreotype with a Figure 22. SM-1927-1680 electrotype with a partial hallmark, recto, upper left corner. reproduced partial hallmark, recto, upper right corner. Raking light photomicrograph, scale bar is 1 mm. Raking light photomicrograph, scale bar is 1 mm. Photo: M. Jürgens. Photo: M. Jürgens.
93 CCW = Counterclockwise.
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Feature specifically related to the SM-1927-1680 daguerreotype Local nodular copper growth surrounded by a whitish substance, which is similar to wax, was observed on the verso (Figure 23).
Figure 23. SM-1927-1680 daguerreotype, verso. Copper growths with white substance, possibly wax, and green-bluish accretions. Raking light photomicrograph, scale bar is 1 mm. Photo: M. Jürgens.
Features specifically related to the SM-1927-1680 electrotype The copper coloured electrotype is very thin, light and undulated overall (Figure 24). The verso is slightly rough, the result of a fine-grained copper deposit with individual, globular copper growth (Figure 17, Figure 25). Copper nodules were also visible at a spot at the lower left edge as seen on the verso (Figure 26). A circular greenish spot, possibly copper corrosion, is present on the recto in the lower right quadrant (Figure 27).
Figure 24. SM-1927-1680 electrotype, side view, verso Figure 25. SM-1927-1680 electrotype, verso, facing up. serrated marks from scissors. Approximately 40% of the verso is covered with dark Fine-grained copper deposit with an individual greenish accretions, which are possibly adhesive circular copper growth. Raking light residues associated with mounting. The differential photomicrograph, scale bar is 1 mm. Photo: M. gloss seen in the photo is due to these accretions. Jürgens. Photo: M. Pilko.
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Figure 26. SM-1927-1680 electrotype, verso. Figure 27. SM-1927-1680 electrotype, recto, Spot with typical copper growth formations at the probable copper corrosion spot, lower right lower left edge (90° CCW). quadrant. Raking light photomicrograph, scale bar is 1 mm. Raking light photomicrograph, scale bar is 1 mm. Photo: M. Jürgens. Photo: M. Jürgens.
4.1.2. Results of the UV fluorescence examination of SM-1927-1680 1 & 2
Examination with an UV lamp with a wavelength of 365 nm (UV-A) showed no fluorescence. A UV LED torch emitting 385 nm (UV-A) showed yellowish fluorescence on the recto of both plates as shown in Figure 28 and Figure 29.
Figure 28 (left). SM-1927-1680 daguerreotype, recto.
Figure 29 (right). SM-1927-1680 electrotype, recto. UV fluorescence induced on both plates by 385 nm irradiation (UV- A). Photo: M. Pilko.
4.1.3. Results of the XRF examination of SM-1927-1680 1 & 2
As anticipated, the major peaks in the XRF spectrum of the SM-1927-1680 daguerreotype are copper, silver, mercury and gold, which are characteristic elements of a mercury-developed and gold-toned daguerreotype. Results for the SM-1927-1680 electrotype show pure copper on both verso and recto. However, a more differentiated measurement of the elemental composition of the electrotype was achieved by SEM-EDS analysis (see 4.1.4). XRF spectra are supplemented in Appendix VII.1. SM- 1927-1680 1 & 2.
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4.1.4. Results of the SEM-EDS examination of SM-1927-1680 1 & 2
The midtone area of the SM-1927-1680 daguerreotype exhibits a surface with horizontal, fine, parallel lines and many particles, from small to large, with round and polygonal shapes, resting on top of the surface. According to EDS analysis, the particles consist of either silver and mercury or silver and gold. On the surface of the plate, mainly silver and gold were detected as well as mercury, albeit with a smaller peak. The major EDS results are listed in Table 2, and the spectra are given in Appendix VIII.1. SM-1927-1680 1 & 2. At a magnification of 1,000x and above it becomes apparent that the SM-1927-1680 electrotype is an exact reproduction of the SM-1927-1680 daguerreotype down to its smallest image particles and finest lines (Figure 30, Figure 31).
Figure 30. SM-1927-1680 daguerreotype. Figure 31. SM-1927-1680 electrotype, SE image, 15kV, 14.8 mm WD, spot 4, corresponding area to Figure 30. 3µs, high vacuum, 5,000x, scale bar is Particles, pits, craters and lines match 20µm. perfectly. SE image horizontally flipped and rotated 105.3° CCW, 15kV, 14.7 mm WD, spot 4, 3µs, high vacuum, 5,000x, scale bar is 20µm.
The SM-1927-1680 electrotype exhibits cavities in the copper surface that Jürgens called pits.94 These pits are probably negative moulds, formed by copper deposition around the image particles of the daguerreotype.. The pits on the electrotype range from small to large, and they have various polygonal shapes (triangular, tetragonal, hexagonal). The smallest pits appear roundish, which may just be due to a combination of their small size and the lack of higher resolution at this magnification. Although SEM does not allow for accurate spatial interpretation, the fine, parallel lines on the electrotype appear to be protruding and the pits appear to be quite shallow. The electrotype also has particles that range in both size and shape. EDS analysis of specific particles on the electrotype showed an elemental composition of copper and silver. At the corresponding spots on the daguerreotype, the surface is marked by rectangular and irregular ruptures, which Jürgens named
94 Jürgens 2015: 13.
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craters.95 Image particles that were pulled off from the daguerreotype during the separation of the plates must have left a crater in the daguerreotype surface. The electrotype has fewer transferred image particles than it does pits, with an approximate ratio of 1:23.96 An individual crater on the SM-1927-1680 daguerreotype and a corresponding particle on the SM- 1927-1680 electrotype were examined at approximately 50,000x (Figure 32, Figure 33). The part of the particle that is visible to us has the form of a cauliflower and is probably the bottom surface of the material that was pried off the daguerreotype surface.
Figure 32. SM-1927-1680 daguerreotype, crater Figure 33. SM-1927-1680 electrotype, particle matching the particle in Figure 33. matching crater in Figure 32. SE image, 15kV, 14.8 mm WD, spot 4, 3µs, high SE image, 15kV, 14.7 mm WD, spot 4, 3µs, high vacuum, 50,762x, scale bar is 2µm. vacuum, 47,568x, scale bar is 2µm.
Element Cu Ag Hg Au Spot SM-1927-1680 daguerreotype Plate surface X X X Particle 1 X X Particle 3 X X Crater X X X SM-1927-1680 electrotype Plate surface X Particle 1 X Particle 2 X X Pit X Table 2. Major EDS peaks for the SM-1927-1680 plates. X indicates the presence of the respective element. Spectra are given in Appendix VIII.1. SM-1927-1680 1 & 2.
4.1.5. Results of visual examination of the NB plate
The image of this copper-coloured electrotype, a post mortem painting portraying Florimond de Coster, appears positive in reflecting dark and negative in reflecting light (Figure 34, Figure 35). It shows some disruptions of the image along the edges. The plate size (73 x 94 mm (H x W)) deviates
95 Jürgens 2015: 13. 96 The area seen in Figure 31 results in approximately 328 pits and 14 transferred image particles.
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considerably from a standard plate size of which the closest would be a quarter plate at 81 x 108 mm (H x W). The edges are straight and partly porous, and the corners are clipped, which indicates that the plate was trimmed. The electrotype is approximately 0.43 mm thick, very lightweight and has a slight convex bow. Fine, parallel, vertical lines are visible overall; these may be polishing marks reproduced from the original daguerreotype. Several green accretions are present in the lower left quadrant, and dark discolouration is present at the corners and along the edges; this linear discolouration corresponds with the window of the paper mat behind which this electrotype is framed. Future research could investigate whether this discolouration can be associated with copper corrosion. Characteristic for the plate is the rough, grainy copper deposit on the verso (Figure 36), which stands in contrast with the highly smooth recto. When examining the verso with an optical stereomicroscope, the rough deposit appears to rest on a more compact base (Figure 37).
Figure 34. NB electrotype, recto, reflecting dark. Figure 35. NB electrotype, recto, reflecting light. 73 x 94 x 0.43 mm (H x W x D). Photo: M. Pilko. Photo: M. Pilko.
Figure 36. NB electrotype, verso in raking light. Figure 37. NB electrotype, verso, raking light Photo: M. Pilko. photomicrograph. Photo: M. Jürgens.
4.1.6. Results of XRF examination of the NB plate
XRF analysis showed the recto to be pure copper, but SEM-EDS analysis resulted in more detailed data (see 4.1.7). The XRF spectrum of the NB plate is given in the Appendix VIII.2. NB plate.
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4.1.7. Results of SEM-EDS examination of the NB plate
At a magnification of 1,000x, the surface of the NB electrotype, in a shadow area, is quite smooth and shows fine, vertical, parallel lines. These lines appear to be protruding, although SEM does not allow for accurate spatial interpretation. In the shadow area there are many small (and some large), round and polygonal cavities (pits). In contrast, a highlight area exihibits relatively long pits, which give the surface a porous appearance. Shadow and highlight areas are shown in Figure 38 and Figure 39.
Figure 38. NB electrotype, shadow area. Figure 39. NB electrotype, highlight area. SE image, 20 kV, 41.4 µm, 15 mm WD, spot 4, 3µs, SE image, 20 kV, 41.4 µm, 15 mm WD, spot 4, 3µs, high vacuum, 10,000x, scale bar is 10µm. high vacuum, 20,000x, scale bar is 10µm.
Individual particles of various sizes with roundish edges were also observed on the surface. Specific particles that were measured with EDS show an elemental composition of copper, silver and gold, while the plate and the inside of an individual pit were pure copper (see Table 3 and spectra in Appendix VIII.2 NB plate). Compared to the SM electrotype, there are many more pits than particles on the NB electrotype.
Element Cu Ag Hg Au Spot NB electrotype Plate surface X Particle 1 X X X Pit X Table 3. Major EDS peaks for the NB daguerreotype electrotype. X indicates presence of the respective element. Spectra are reproduced in Appendix VIII.2. NB plate.
4.2. Results of initial tests with silver coupons
Initial tests demonstrated that silver coupons were suitable for testing the appropriate electrochemical conditions for electrotyping, which were subsequently applied to daguerreotypes. First tests with an excessive current resulted in a spongy electrodeposit, but subsequent tests resulted in the production of actual copper electrotypes that precisely copied the surfaces of the silver coupons.
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4.2.1. Appropriate consistency of the electrodeposit
The consistency of the electrodeposit is dependent on the applied current density (for an explanation of this parameter, see 2.3, Current density). Initial electroplating with a current density of 25 A/dm2 resulted in a non-coherent, dark copper deposit, which only adhered to the silver coupon poorly (Figure 40). The evolution of hydrogen, as described by von Pauly, was indeed observed at the daguerreotype plate (see 2.6.2, Current intensity). The use of a less powerful rectifier allowed for the operation at a more finely tunable current, for example 0.09 A and 0.5 V, values that more closely resemble the possibilities of Lerebours battery. Electroplating with a current density of 2.5 A/dm2 resulted in a compact copper electrodeposit with a
pearly rose colour, as described by Lerebours and shown in Figure 41.
Figure 40. Silver coupon with Figure 41. Silver coupon with dark, non-coherent copper bright, compact copper deposit. deposit Obtained from 0.8 mol dm-3 -3 -3 Obtained from 0.8 mol dm CuSO4 in 0.5 mol dm H2SO4. -3 2 CuSO4 in 0.5 mol dm H2SO4. Current density: 2.5 A/dm ; Current density: 25 A/dm2; duration of deposition: 2 hours. duration of deposition: 5 min. Dimensions 21 x 21 x 0,6 mm Dimensions 12 x 12 x 1,5 mm (H x W x D). Photo: M. Pilko. (H x W x D). Photo: M. Pilko.
4.2.2. Thickness and rate of electrodeposition
With the initial results as a starting point, it was estimated that an approximately 0.4 mm thick copper deposit would require around 8 hours of treatment, given a continuous current density of 3.46A/dm2. This duration is similar to that found in historical sources. The required time to gain a 0.4 mm deposit thickness is calculated as following97:
had 0,04 × 28.92 × 8,93 t = s = 4 = 31398,86sec = 8,72hours = 8h,43min ZI 3,29 ×10 ×1 h = thickness of electrodeposit (in cm) a = surface area (in cm2) d = density of copper (in g/cm3)
97 Paunovic 2010: 13-17.
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Z = electrochemical equivalent (g) I = Intensity (s)
4.2.3. Separating the electrotype and the silver coupon
The electrodeposit of an appropriate consistency was separated mechanically from the silver coupon following the method described by Lerebours: after trimming the rims of copper that had formed around the edges of the coupon, the electrodeposit was released automatically (Figure 42, Figure 43). In contrast, a very coarse copper deposit did not allow separation at the interface of the coupon and the copper electrotype (Figure 44). It became apparent that a thinner electrodeposit released easier from the substrate. However, a thinner electrodeposit was generally also easier undulated by mechanical impact such as from trimming.
Figure 42. Silver coupon with Figure 43. Silver coupon (left) Figure 44. Copper deposit partly copper deposit. from Figure 42 with trimmed separated from silver coupon. edges and after separation of the Obtained from a 0.8 mol dm-3 Obtained from a 0.8 mol dm-3 -3 copper deposit. -3 CuSO4 and 0.5 mol dm H2SO4. CuSO4 in 0.5 mol dm H2SO4. Current density: 2.5 A/dm2, Electrotyped coupon (right). Note Current density: 12 A/dm2 (first 30 exposure time: 32 hours.. the highly reflective copper- min), then 5 A/dm2, exposure time: Dimensions: 22 x 22 x 1 mm (H x coloured surface of the 22 hours. Dimensions: 20 x 20 x 1,1 W x D). Photo: M. Pilko. electrotype, on which the mm (H x W x D). Photo: M. Pilko. scratches perfectly match those of
the silver coupon. Dimensions: 10 x 10 x 0,5 mm (H x W x D). Photo: M. Pilko.
4.3. Results of the examination of the reconstructions
4.3.1. Results of the visual examination of the reconstructions
I. Electrotyping according to Lerebours instructions supplemented by other sources The separation of the electrodeposit from the daguerreotypes resulted in image loss on the daguerreotype in all cases. On the recto, the daguerreotypes exhibit a dull, white haze and a faint, often streaky image. The recto of the obtained electrotypes exhibit a reflective surface
with a low contrast, positive image that has a silver-yellowish hue (Figure 45, Figure 46).
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Figure 45. AO-4-2 Figure 46. AO-4-2 Daguerreotype, recto, after separation, in Daguerreotype with copper normal illumination (left). deposit prior to separation, AO-4-2 electrotype, recto (right). Photo: M. Pilko. recto in raking light. Obtained from a 0.8 mol dm-3 -3 CuSO4 in 0.5 mol dm H2SO4. Current density: 3.42 A/dm2; exposure time: 8 hours. Dimensions: 30 x 24 x 0.5 (H x W x D in mm). Photo: M. Pilko.
Different current densities tested on the AO-3 and AO-4 plates resulted in the same matte, low contrast image as seen above (Appendix VI.4. AO-3 plate, and VI.5. AO-4 plate). The gold-toned area of the modern MO plate was also electrotyped in the same fashion. However, the untoned areas at the edges of the MO daguerreotype electrotyped quite differently. Here, the MO daguerreotype and the MO electrotype both exhibit a highly reflective surface with a very faint image. While the daguerreotype is silver, the electrotype has a copper colour here (Figure 47).
Figure 47. Daguerreotype fragment MO-3, recto, after separation (left) and MO-3 electrotype (right) in normal illumination. Obtained from a 0.8 -3 -3 mol dm CuSO4 in 0.5 mol dm H2SO4. Current density: 3.6 A/dm2, exposure time: 9 hours. Dimensions (each plate): 41 x 57 x 0,5 (H x W x D in mm). Photo: M. Pilko.
Some variation was seen in the electrotyped right half of the 19th century DB plate: while a dull, white haze prevails on the daguerreotype, some areas do partly show the image on a silver background. The corresponding areas on the electrotype exhibit a copper-coloured image that appears positive in reflected dark and negative in reflected light (Appendix VI.7. Daniel Blau plate (DB)).
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II. Implications of an additional coating on the recto of the daguerreotype not mentioned by Lerebours The reconstruction tests showed that a thick isolation layer of Paraloid B-72 or wax reduced the conductivity of the specimen, thereby preventing electrodeposition; this phenomenon had been described by Lerebours. Interestingly, however, a thin isolation layer with Paraloid B-72 or beeswax did actually permit electrodeposition, and the deposit did not adhere well to the substrate. This promised to be a mechanism that could result in better electrotypes, so the following tests were designed that added a thin surface layer to the daguerreotype before electrotyping commenced. Beeswax dissolved in white spirits was applied to the recto of the AO-1 daguerreotype, where it quickly hardened as the solvent evaporated. Excess wax was then rubbed off, which caused surface scratching and resulted in the partial removal of the daguerreotype image. The electrotype pulled from this daguerreotype has a relatively high reproduction quality. The resulting image is positive in reflected dark and negative in reflected light. Even after electrotyping, the daguerreotype image still exhibits good contrast (Figure 48 and Figure 49). Streaks caused during the application of the wax are visible on both plates. Traces of residual wax are present on the electrotype, however more research is necessary to establish the extent to which the coating actually transfers from the daguerreotype to the electrotype.
Figure 48. AO-1 daguerreotype, recto, after separation (left), with AO-1-1 electrotype, recto (right), normal illumination, reflecting dark. The daguerreotype was coated prior to electrotyping. Electrotype obtained from a 0.8 mol dm-3 -3 CuSO4 in 0.5 mol dm H2SO4. Current density: 3.46 A/dm2; exposure time: 8.5 hours. Dimensions daguerreotype: 60 x 48 x 0.5 mm (H x W x D in mm). Photo: M. Pilko.
Figure 49. AO-1 daguerreotype, recto, after separation (left), with AO-1 electrotype, recto (right), reflecting light. The daguerreotype was coated prior to electrotyping. Electrotype obtained from a 0.8 mol dm-3 -3 CuSO4 in 0.5 mol dm H2SO4. Current density: 3.46 A/dm2; exposure time: 8.5 hours. Dimensions daguerreotype: 60 x 48 x 0.5 mm (H x W x D in mm). Photo: M. Pilko.
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Figure 50. AO-1 daguerreotype, verso, after separation (left), with AO-1 electrotype, verso (right), normal illumination. Dimensions daguerreotype: 60 x 48 x 0,5 mm (H x W x D in mm). The daguerreotype was coated prior to electrotyping. Electrotype obtained from a 0.8 mol dm-3 -3 CuSO4 in 0.5 mol dm H2SO4. Current density: 3.46 A/dm2; exposure time: 8.5 hours. Photo: M. Pilko.
Figure 51. AO-1 electrotype, verso top left corner with individual copper nodules on a fine grained copper substrate. Raking light digital photomicrograph, 40x, scale bar is 2000 µm. Photo: Bas van Velzen. Electrotype obtained from a 0.8 mol -3 -3 dm CuSO4 in 0.5 mol dm H2SO4. Current density: 3.46 A/dm2; exposure time: 8.5 hours.
The optimal current density for a compact electrodeposit was ultimately determined to be approximately 3.46 A/dm2. The verso and the edges of the AO-1 daguerreotype exhibit partly nodular copper growth (Figure 50, Figure 51), which is comparable to the verso of the historical DM-69896 electrotype (Figure 3) and the SM-1927-1680 electrotype (Figure 51). The AO-1 electrotype locally adhered strongly along the edges to the AO-1 daguerreotype and was therefore torn off at the upper left and lower right edges during separation of the two plates. Droplets of the electrolyte that were accidentally present during the separation caused the formation of spots on the AO-1 electrotype. A small area at the lower right edge of the AO-1 daguerreotype shows a dull, white haze. At the corresponding area, the electrotype is silver-coloured, which resembles the plates that had been electrotyped without a coating. The results of electrotyping the historical UvA plate were very similar to that of the AO-1 plate; this observation emphasizes the importance of a coating on the recto of the daguerreotype prior to electrotyping (Figure 25).
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Figure 52. UvA daguerreotype after separation (left) with electrotype (right), normal illumination, reflecting dark. The left half of the daguerreotype surface was coated prior to electrotyping. The upper 1.5 cm of the daguerreotype was not electrotyped. Electrotype obtained from a 0.8 mol dm-3 -3 CuSO4 in 0.5 mol dm H2SO4. Current density: 3.46 A/dm2, exposure time: 8.5 hours. Dimensions of the daguerreotype: 60 x 48 x 0.5 mm (H x W x D in mm). Photo: M. Pilko.
The AO-2 daguerreotype was given a particularly thin wax coating prior to electrotyping. The resulting electrotype has a coppery colour and displays a positive image in reflected dark and a negative image in reflected light. The image of the AO-2 electrotype has less contrast than that of the AO-1 electrotype, with the exception of a small area at the border area between the coated and the uncoated areas. Here, the image has the highest brilliance and contrast; This area was examined with SEM-EDS (see 4.3.4). As anticipated, the uncoated strip near the left edge of the AO-2 daguerreotype and the corresponding area on the electrotype exhibit the same characteristics described previously for the other uncoated plates (Figure 53).
Figure 53. AO-2 daguerreotype after separation (left) with electrotype (right), normal illumination, reflecting dark. The centre and right of the daguerreotype surface was coated with beeswax prior electrotyping. The left edge was not electrotyped, and the far left 1 cm edge strip was not coated as a control. Electrotype -3 obtained from a 0.8 mol dm CuSO4 -3 in 0.5 mol dm H2SO4. Current density: 3.46 A/dm2; exposure time: 8.5 hours. Dimensions daguerreotype 60 x 48 x 0,5 mm (H x W x D in mm). Photo: M. Pilko.
Tests with a coating of linseed oil on the left half of the DB daguerreotype resulted in a poor reproduction quality: whitish haze on the daguerreotype, and an only partly visible image. The resulting DB electrotype partly exhibits a silvery image and partly a copper-coloured image (Appendix VI.7. Daniel Blau plate (DB)).
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III. Production of a second daguerreotype electrotype from the same daguerreotype A second electrotype could be obtained from the AO-1 daguerreotype. It has a high reproduction quality and exhibits a positive image in reflected dark and a negative image in reflected light (Figure 54).
Figure 54. AO-1-I electrotype (left) and AO-1-II electrotype (right) in normal illumination, reflecting dark.
Electrotypes obtained from a 0.8 mol -3 -3 dm CuSO4 in 0.5 mol dm H2SO4. Current density: 3.46 A/dm2; exposure time: 8 hours. Photo: M. Pilko.
4.3.2. Results of UV fluorescence examination of the AO plates
No fluorescence was observed on the AO-1, AO-2, AO-3 and AO-4 plates when irradiated with UV-A (365 nm) and UV-C (254 nm). Other plates were not examined due to time constraints.
4.3.3. Results of XRF of the AO-4-1, AO-4-2, AO-4-2 electrotype plates
XRF measurements on the unprocessed AO-4-1 daguerreotype (control) show the elements gold, silver and mercury, which is consistent with the fact that these are mercury-developed, gold-toned daguerreotypes (see Section 3.1.3 Description of the cathodes used in the reconstruction tests). Highlight, midtone and shadow areas showed peaks for gold, with the highlight exhibiting a slightly higher gold peak. By contrast, the measured areas of the electrotyped areas of the daguerreotype lacked gold and mercury or have only a very small amount of it. As anticipated, the AO-4-2 electrotype consists of copper, but silver was also detected, as well as precisely those elements that the daguerreotype lacked: gold and mercury. The spectra are given in Appendix VII.3. AO-4 plates.
4.3.4. Results of SEM-EDS examination of the AO-1 and AO-2 plates
Examination with SEM-EDS revealed that the AO-1 daguerreotype surface exhibits very small holes and a darkish pattern in the shadow area, and many particles, from small to large, with round and polygonal shapes in the highlight area. A small number of fine, straight lines are randomly distributed across the surface. The AO-1 daguerreotype shows also an individual crater and, though unexpected, the AO-1 electrotype exhibits pits at the corresponding spot (Figure 55, Figure 56). Electrotyping a pit
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on the daguerreotype would be expected to result in a protrusion on the electrotype, and it is therefore surprising that the AO-1 electrotype has a pit in the corresponding area. The AO-1 electrotype displays a relatively smooth surface in the shadow area and many irregularly shaped pits in the highlight area, which match indeed particles on the AO-1 daguerreotype.
Figure 55. AO-1 daguerreotype with image particles Figure 56. AO-1 electrotype with pits. and craters. Corresponding area of Figure 55. SE image Corresponding area of Figure 56. BSE image, 15 kV, horizontally flipped and rotated 168° CCW, 15 kV, 5.5 5.6 mm WD, spot 3, 254 µm, 60 Pa, 500x, scale bar is mm WD, spot 3, 254 µm, 60 Pa, 350x, scale bar is 50µm. 50µm.
Only few particles were found on the AO-1 electrotype, and the ones that were analysed are composed of copper, silver and either gold or mercury (Table 4). On the AO-1 electrotype fewer particles were observed than pits. A small number of fine, straight lines are randomly distributed across the surface. While the reconstructed AO-1 electrotype does have pits and transferred particles, the definition of the pits is rather poor when compared to the clearly defined particle shapes on the daguerreotype (Figure 57, Figure 58).
Figure 57. AO-1 daguerreotype. Figure 58. AO-1 electrotype. Few large and many smaller image forming particles Many pits. Highlight area, SE image, 15 kV, 5.5 mm and craters. Highlight area, BSE image, 15 kV, WD, spot 3, 50.8 µm HFW, 60 Pa, 2,500x, scale bar is 5.6 mm WD, spot 3, 63.5 µm HFW, 60 Pa, 2,000x, 10 µm. scale bar is 10 µm.
A different result was seen with the AO-2 electrotype at an area with a presumably thinner wax
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coating. While the AO-2 daguerreotype has a surface comparable to the AO-1 daguerreotype, the AO- 2 electrotype displays clearly defined pits. Comparing the AO-2 daguerreotype with the AO-2 electrotype shows that the shape of the pits on the AO-2 electrotype correspond precisely to the shape of image particles on the AO-2 daguerreotype (Figure 59, Figure 60, Figure 61). Figure 60 also shows an individual particle (Particle B) on the AO-2 electrotype with an elemental composition of mercury, silver and copper, as determined by EDS analysis. At this magnification of 1,000x, the corresponding spot on the AO-2 daguerreotype does not show any disturbance at the spot where the particle was pulled off the surface. Higher magnification images were not taken due to time constraints.
Figure 59. AO-2 daguerreotype, image Figure 60. AO-2 electrotype. Area particles in a midtone area. corresponding with Figure 59. SE image, 15 kV, 7.4 mm Many pits and an individual particle are WD, spot 3, 127 µm HFW, 7.87e-5 Pa, visible, midtone area, BSE image, 1,000x, scale bar is 20 µm. horizontally flipped and rotated for 171° CCW, 15 kV, 7.3 mm WD, spot 3, 127 µm HFW, 7.87e-5 Pa, 1,000x, scale bar is 20 µm.
Figure 61. AO-2 electrotype. White arrow points to the area examined with SEM-EDS.
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Finally, the AO-2 daguerreotype also exhibits local ruptures in the surface in uncoated areas. EDS analysis indicated a pure silver substrate within the disrupted area. At corresponding areas of the AO-2 electrotype fragments of a layer consisting of silver and gold was observed resting on top of the copper substrate. This layer includes particles composed of copper, silver and mercury. Besides copper this is a composition comparable to image particles on the daguerreotype (Figure 62, Figure 63).
Figure 62. AO-2 daguerreotype with rupture in the Figure 63. AO-2 electrotype. surface. Midtone area, BSE, 15 kV, 7 mm WD, spot 3, 63.5 µm Midtone area, SE image, 15 kV, 7.4 mm WD, spot 3, HFW, 9.64e-4 Pa, 2,000x, scale bar is 10 µm. 50.8 µm HFW, 8.61e-4 Pa, 2,500x, scale bar is 10 µm.
Element Cu Ag Hg Au O Fe C Spot AO-1 daguerreotype Plate surface X X X X Particle X X X X Hole X X X X AO-1 electrotype Plate surface X X X Large particle X X X X X Small particle X X X X X Pit X X X AO-2 daguerreotype Plate surface X X X Particle (large) X X X Hole X X X Rupture X AO-2 electrotype Plate surface X X Particle X X X X Layer on top X X X X Particle in top layer X X X Table 4. Major EDS peaks for the AO-1 & AO-2 plates. X indicates presence of the respective element. Spectra are reproduced in Appendix VIII.1. SM-1927-1680 1 & 2.
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5. Discussion
5.1. Discussion of main results
The reconstruction following Lerebours instructions supplemented by other sources was partially successful. While it was possible to create a coherent, solid copper electrotype plate, the image reproduction initially failed. All three examined historical daguerreotype electrotypes characteristically exhibit a copper coloured image, as a positive in reflecting dark and as a negative in reflecting light. However, by strictly following Lerebours' instructions, these image characteristics could not be reproduced. Results from XRF (3.2.3) and SEM-EDS analysis (4.3.2) support the theory that the uppermost layer, including the image-forming particles, of the daguerreotype was stripped off and transferred to the electrotype. The dull, white haze exhibited by the daguerreotypes after electrotyping them is therefore an indication of a stripped silver-gold layer including the loss of image particles. The faint image on the corresponding electrotypes is considered to be formed by transferred image-forming particles from the daguerreotype, seen from the bottom. Conversely, the faint image left behind on the daguerreotype is probably a result of a disrupted surface, which scatters light to a greater or lesser degree depending on the amount and location of the pried off image particles. The ambiguous results of the electrotyping of the DB daguerreotype can be attributed to fact that the plate had previously been cleaned and that some substance left on the surface may have influenced the results. Electrotyping the only partially gold-toned MO daguerreotype (4.3.1, Figure 47) indicated that the gold-toning of the daguerreotype forms a continuous layer including image particles which, during the separation of the plates, is stripped off the surface. Several researchers also support the concept of a continuous gold layer on a daguerreotype.100 It was initially hypothesized that current density would be a key parameter for the successful production of a daguerreotype image on the electrotype. The surface structure of the verso of historical daguerreotype electrotypes provides an insight into the current density used to obtain them. Whereas the SM-1927-1680 and DM-69896 electrotypes have a fine-grained verso, the NB electrotype exhibits a very rough electrodeposit, indicating the use of a much higher current density. In the reconstruction, a very coarse copper deposit did not allow separation at the interlayer of specimen and electrotype (Figure 44). From this it may be concluded that while the coarse deposit as seen on the verso of the NB electrotype was suitable enough to build up the thickness of the plate, the initial deposition rate must have been lower in order to achieve a fine copper deposit, which would in turn allow for a successful separation from the daguerreotype. The practice of accelerating the plating speed at a later stage of electrotyping is also described in the historical literature (2.6.2 Current intensity) and supports this hypothesis. Testing with different current densities ultimately strongly indicated that the appropriate current density is primarily crucial for obtaining a coherent copper deposit. However, the quality of the image reproduction was not further positively influenced (Appendix VI.4. AO-3 plate and VI.5. AO-4 plate). Since the close following of the historical recipes did not result in the successful reproduction of daguerreotype image by the electrotype process, the question was raised as to whether the instructions are indeed complete. All of the results from tests with contemporary and historical daguerreotypes
100 E.g. Da Silva et al. 2010: 661, Wiegand et al. 2013: 168, Marquis et al: 2015: 444.
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suggest that an additional treatment of the daguerreotype prior to electrotyping, such as the application of an intermediate separation layer, is required. The specifications of the production of the daguerreotypes as well as the presence or absence of a corrosion layer did not seem to influence the image reproduction process very much. On the contrary, daguerreotypes that were coated on the recto with beeswax prior to electrotyping resulted in electrotypes that very closely resembled historical daguerreotype electrotypes. The presence of a surface coating appeared plausible, since the surface of a gold-toned daguerreotype showed a certain resistance against mechanical manipulation. The use of beeswax was also common in historical electrotyping. When electrotyping copper coins, Napier actually recommends the application of beeswax in turpentine, wiped off with a silk cloth, to prevent adhesion of the electrodeposit to a coin.101 Lerebours' instructions also mention beeswax, except that here the purpose is to isolate the edges and verso of the daguerreotype from copper deposit with a thick wax layer. The historical DM-69896 daguerreotype does indeed have traces of wax along the edges on the recto, and both the DM-69896 daguerreotype and SM-1927-1680 daguerreotype have wax on the verso to prevent the entire plate to be covered by copper deposit during electrotyping. However, no data is available as to whether some kind of coating is also present on the actual image area on the recto of the historical plates. The application of wax on the daguerreotype prior to electrotyping also allowed the production of a second electrotype from the same plate. Making several reproductions from the same daguerreotype was also described in historical sources (2.6.2. Number of copies). In fact, two copper plates with the same photographic image, thought to be daguerreotype electrotypes, are held in the collection of the Bibliotheque nationale de France in Paris (see Appendix II). On the other hand, the wax coating in the reconstructions clearly improved the precision of the reproduction in most cases. Its impact was seen with the naked eye and studied by SEM (4.3.4). A wax coating with the appropriate thickness could only be partially achieved once on the AO-2 daguerreotype. While the larger part of the AO-2 plate exhibits a low contrast image, a small area between the thoroughly coated and uncoated control area shows the image with good contrast to the naked eye (Figure 61). Examination with SEM-EDS (Figure 59, Figure 60) shows indeed a microstructure at that small area which is comparable to the three examined historical daguerreotype electrotypes. Time constraints did not allow to test whether this result is reproducible. However, the difficulties in finding the appropriate amount of wax speak against the use of a wax coating, and it is possible that other substances may have been used as separation layer. Krone, for example, describes Fizeaus heliographic etching process as follows: Fizeau applied a thin layer of linseed oil on a daguerreotype and rubbed it off, similar to how a copperplate engraver applies varnish.102 Although this is a different context, it illustrates that Fizeau was familiar with applying a substance onto the surface of a daguerreotype prior to electroplating it with a very thin layer of copper. Initial reconstruction tests with a linseed oil film on the daguerreotype did not have a convincing result
101 Have the fore part or face well cleaned, and the surface moistened with sweet oil, by a camels hair pencil, and then cleaned off by a silk cloth, till the surface appears dry [ ]. Take a gill of rectified spirits of turpentine, and add to it about the size of an ordinary pea of bees wax. When this is dissolved, wet over the surface of the mould with it, and then allow it to dry. But when fine line engravings are to be coated, the little wax dissolved in the turpentine may be objectionable; so also black lead, for both have a tendency to fill up the fine lines. In this case, let the wash with turpentine be wiped off by a silk handkerchief, instead of drying it. Napier 1860: 50. 102 Krone and Schmidt 1907: 40.
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(Appendix VI.7. Daniel Blau plate (DB)). However, according to Krone, linseed oil needs to dry for several days, and it is possible that the drying time in the reconstruction test was too short. The UV-fluorescence on the DM-69896 and SM-1927-1680 electrotypes (no data is available on the NB plate) could potentially be an indication for a coating.103 In a study by de la Rie, it was found that linseed oil films show fluorescence after degradation begins.104 Given the traces of residual wax that were present on the reconstructed daguerreotype electrotypes it even appears possible that the beeswax will develop fluorescence after some time. Further research could be conducted to understand in how far fluorescence might be related to the electrotype process. Further examination of historical plates could also help in this respect. Until now, FTIR analysis was conducted only on the verso and the edges of the DM-69896 plates, but examining an daguerreotype electrotype and/or its daguerreotype on the recto could potentially give more information on the possible presence of a yet unknown substance that could have facilitated the separation of the plates. A historical source from 1845, which was only found in the final phase of writing this thesis, mentions a pre-treatment of the daguerreotype with diluted ammonia in water prior to electrotyping.105 Contemporary technical sources on electroforming state that most metallic masters require an additional chemical treatment such as with sodium dichromate or sodium sulfide to form a parting film.106 Another modern source mentions egg albumen.107 Due to time constraints, none of these alternatives could be considered in the present study, and further research would therefore be beneficial.
5.2. The identification of daguerreotype electrotypes
Initially, the establishment of identification characteristics had not been a goal of this thesis. However, as several features of the historical daguerreotype electrotypes proved reproducible in the reconstruction, they may be considered characteristic of the process. Features that were seen on historical and reconstructed electrotypes are listed in Table 5 in the order of their usefulness for identification, and some of these are discussed in more detail in the following.
103 UV fluorescence was observed overall on the recto of the historical DM-69896 plates under an irradiation of 254 nm (UV-C). Jürgens 2015: 10, 11. 104De la Rie 1982: 68. 105 Lippowitz 1845: 29. 106 ASTM B832 -93 (2013) 2013: 3, 4. 107 Finishing.com. 3.5.2017.
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Object DM-69896 SM-1927-1680 NB Re-
electrotype electrotype electrotype construction Feature Visual examination Copper colour X X X X Positive image in reflected dark and X X X X negative image in reflected light Highly reflective surface X X X X Fine grained copper deposit with X X X individual copper nodules on the verso Rough copper deposit on the verso X X Thin plate (ca. 0.4 mm) X X X X Bumpy edges with nodular copper X X growth structure Straight edges with no copper formation: X X X trimmed Undulated overall X X X Flat plate X Corner is bent X X X Small crack in surface: marks from X X separation with sharp tool Image partially disrupted X X X X SEM Pits (small to large, polygonal and round X X X X shapes, also longish, appear shallow) Particles X X X X Fine, parallel lines: polishing marks X X X 108
EDS Particles: Ag, Au, Hg X X X X Substrate: Cu X X X X
Table 5. Features of historical daguerreotype electrotypes that could be reproduced by the reconstruction tests. X indicates the presence of the respective feature.
108 The absence of polishing marks on the examined reconstruction AO daguerreotypes is attributed to the fact that a polishing machine was used. Polishing marks are expected when hand-polished daguerreotypes are electrotyped.
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Visual examination Daguerreotype electrotypes are primarily characterized by their copper-coloured, highly reflective surface on the recto, showing the image as a positive in reflected dark and as a negative in reflected light. The verso exhibits a fine to rough-grained copper deposit, and individual nodular copper growth structures are typical for fine-grained deposits. These nodules can be recognized with a minimum magnification of 30x. From the reconstruction tests it was learned that the edges of a daguerreotype electrotype provide some insight into how the plates were separated. Whereas the SM-1927-1680 and NB electrotypes have relatively straight edges, the DM-69896 electrotype shows nodular copper formations, and wax residues were observed along the edges of the recto of the DM-69896 daguerreotype. In the reconstruction tests, it was possible to obtain edges with nodular copper formations comparable to the DM-69896 electrotype (Figure 46) by applying a narrow strip of isolation layer (Paraloid B-72) along the daguerreotype edges on the recto. Nodular surface protrusions and cauliflower-like shapes as seen on the DM-69896 electrotype and the reconstructions are typical for a copper electrodeposit.109 According to Lowenheim, the growth of nodules due to uneven deposition can be observed on so- called growth sites, which attract more current than their surroundings and therefore grow faster.110 Since the electromagnetic field is concentrated along the edges, copper nodules tend to build up there.111 Hence, nodular copper formations at the edges of a daguerreotype electrotype indicate that it was not trimmed, while daguerreotype electrotypes with straight edges were trimmed.
Examination with SEM-EDS SEM-EDS is particularly helpful for the identification of daguerreotype electrotypes. Characteristic for all of the daguerreotype electrotypes examined with SEM-EDS in this study are pits in the surface. Corresponding areas were located on all of the historical and reconstructed electrotypes, where the pits on the electrotypes exactly match image particles at the corresponding areas of the daguerreotypes. Whereas the pits on the DM-69896, the SM-1927-1680 and the reconstructed AO-2 electrotypes have clearly defined polygonal or round shapes in the midtone areas, pits in a highlight area of the NB electrotype are longish, and the surface appears porous. A possible explanation for these shapes is that the cavities merged into one another when forming around closely situated image-forming particles on the daguerreotype. On all of the examined daguerreotype electrotypes, SEM also revealed the presence of characteristic particles with a similar elemental composition as that of a daguerreotypes image particles. This strongly suggests that image particles were transferred from the daguerreotype to the electrotype, which, in logical consequence, are resting there bottom-side up. Finding a crater on the daguerreotype and an image particle at the exact corresponding area on the electrotype further proves this theory. While these matching crater-particle pairs were found on the DM-69896 and the SM- 1927-1680 plates, it was not possible to find them on the reconstruction plates. Although an individual crater was found on the AO-1 daguerreotype, the AO-1 electrotype showed no transferred particle at the corresponding spot, but instead a pit. In another examination, a transferred image particle was located on the AO-2 electrotype, but no crater was observed at the corresponding area of the AO-2
109 Popov 2002: 57. 110 Lowenheim 1978: 129. 111 Larsen 1984: 31.
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daguerreotype. It is possible, however, that some form of disruption of the AO-2 daguerreotype surface resembling a crater might become visible at a yet higher magnification. This could not be further investigated as the SEM session was interrupted due to time constraints. Image particles of the AO-1 daguerreotype were analysed with EDS (4.3.4), which showed them to be composed of silver and mercury, whereas the substrate is composed of silver and gold. Gold would also be expected to be present in the image particle, but a likely reason why gold does not appear in the spectrum of the image particles is that the X-ray lines of mercury and gold are so close in energy that a standard EDS system based on detection by a SDD cannot resolve them sufficiently, and the gold peak merged with that of mercury.112 In fact, gold and mercury were indicated in all EDS- measurements individually, possibly obscuring the presence of the other. The amount of image particles transferred from the daguerreotype to the electrotype varies considerably. While approximately half of all image particles were transferred from the DM-69896 daguerreotype to the DM-69896 electrotype, the SM-1927-1680 electrotype and NB electrotype exhibit only few, and the reconstructions even fewer. An explanation for the small number of transferred image particles on the AO-1 electrotype could be that the relatively thick wax layer on the daguerreotype protected the majority of image particles from being pulled off during the separation of the plates. With the use of SEM, Jürgens identified parallel lines on the DM-69896 daguerreotype as polishing marks; these were found reproduced on the DM-69896 electrotype.113 The same type of lines were observed on the SM-1927-1680 daguerreotype and the NB electrotype. The contemporary AO-1 and AO-2 plates did not show such a regular line pattern. A reason for this could be a different method of polishing: the AO daguerreotypes were not polished by hand, but instead with an electric random sander. The lines that are visible on the AO-1 electrotype in particular may be attributed to the reproduction of streaks from the application of wax to the daguerreotype surface.
Examination with XRF spectroscopy Daguerreotype electrotypes show a characteristic XRF spectrum that is a result of transferred particles. While pure copper was detected on both the verso and the recto of the DM-69896 electrotype in shadow areas, minute amounts of silver, gold and mercury were found on the recto in a highlight area. This result is attributed to the fact that more particles are present in highlight areas of daguerreotypes, and it is here where the most particles must have transferred to the electrotype. In contrast, XRF spectroscopy of the SM-1927-1680 and NB electrotype at unspecified areas indicates only pure copper on both sides. Only the use of EDS indicated the presence of particles with a silver, gold and mercury composition (4.1.3, 4.1.4, 4.1.6, 4.1.7.). The reason for this discrepancy may be due to the fact that measurements of the SM-1927-1680 and NB electrotypes were probably only made in shadow areas. Another explanation could be that the XRF spectroscopy instrument was not sensitive enough to detect such a small number of transferred particles on the SM-1927-1680 and NB electrotypes.
112 Da Silva et al. 2010: 655. 113 Jürgens: 2015: 15.
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6. Conclusion
The goal of this study was to reconstruct the electrotype process as applied to daguerreotypes following historical sources. The study demonstrates that historical instructions on electrotyping daguerreotypes by Lerebours as supplemented by other sources do not result in daguerreotype electrotypes that are comparable to the three examined historical daguerreotype electrotypes. The working parameters for electrotyping daguerreotypes could be specified as a current density of approximately 3.46 A/dm2 for approximately 8 hours resulting in an approximately 0.4 mm thick electrodeposit. However, the image of the daguerreotype could initially not be reproduced on the electrotype, since the gold layer of the daguerreotype including the image particles was transferred to the electrotype when the two plates were separated. While the examined historical daguerreotype electrotypes appear negative in reflected light and positive in reflected dark on a copper-coloured ground, this was not the case for the reproductions. Only by applying a separation layer of beeswax prior to electrotyping, as deduced from literature, produced daguerreotype electrotypes that closely resemble the historical objects. These reconstructions also reproduced a surface topography characteristic to that observed on historical daguerreotype electrotypes by SEM-EDS. Further research is required to determine the reproducibility of the process, and, in particular, to find the optimal separation layer. Ultimately, several features as observed on historical daguerreotype electrotypes were reproduced in the reconstruction and may be considered characteristic to the process.
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7. References
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Barger, Susan, William White. The Daguerreotype. Nineteenth Century Technology and Modern Science. Baltimore: The Johns Hopkins University Press, 1991.
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Buerger, Janet. French Daguerreotypes. Japan: University of Chicago Press, 1989.
Chevalier, Charles. Nouvelles instructions sur lusage du daguerréotype. Description dun nouveau photographe, et dun appareil très simple destine à la reproduction des épreuves au moyen de la galvanoplastie. Paris: Édouard Proux et C., 1841.
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Da Silva, Eric, Mike Robinson, Christopher Evans, Ana Pejovi-Mili, Darrick V. Heyd. Monitoring the Photographic Process, Degradation and Restoration of 21st century Daguerreotypes by wavelength-dispersie X-ray fluorescence spectrometry. Journal of Analytical Atomic Spectrometry 25 (2010): 654-651.
De la Rie, René. Fluorescence of Paint and Varnish Layers (Part II). Studies in Conservation. 27.2 (1982): 65-69.
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Draper, William. Note on the Tithonotype. The London, Edinburgh, and Dublin Philosophical Magazine and Journal of Science 23 (September 1843): 175-176.
Eder, Josef. Geschichte der Photographie. Halle a. S.: Wilhelm Knapp, 1905.
Eder, Josef. Die Daguerreotypie und die Anfänge der Negativphotographie auf Papier und Glas (Talbotypie and Niepcotypie). Halle a. S.: Wilhelm Knapp, 1927.
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Font-Réaulx, Dominique de. The daguerreotype. Milan: Continents Editions, 2008.
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Hill, Levi. A Treatise on Daguerreotype; the Whole Art made Easy, and all the Recent Improvements Revealed. Lexington: New York, 1850.
Humphrey, Samuel. American Handbook of the Daguerreotype: Giving the Most Approved and Convenient Methods for Preparing the Chemicals, and the Combinations used in the Art. Containing the Daguerreotype, Electrotype, and Various other Processes Employed in Taking Heliographic Impressions. New York: S. D. Humphrey, 1858.
Jacobi, Moritz. Die Galvanoplastik, oder das Verfahren cohärentes Kupfer in Platten oder sonst gegebenen Formen, unmittelbar aus Kupferauflösungen auf galvanischem Wege zu produciren. St. Petersburg: Eggers et Co.,1840.
Jones, Denny. Principles and Prevention of Corrosion. USA: Prentice Hall, 1996.
Jürgens, Martin. Report on the Examination and Analysis of a Daguerreotype and its Copper Copy Plate. Unpublished, Rijksmuseum Amsterdam: 2015.
Kanani, Nasser. Electroplating. Basic Principles, Processes and Practice. Oxford: Elsevier Advanced Technology, 2004.
Krone, Hermann, Irene Schmidt. Die für alle Zeit von praktischem Wert bleibenden photographischen Urmethoden: aus eigener Praxis in alter Zeit mit allen Rezepten mitgeteilt. Fotokinoverlag: Leipzig, 1985. Reprint of edition: Dresden, 1907.
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Lequeux, James. Hippolyte Fizeau. Physicien de la lumière. Les Ulis: Sciences, 2014.
Lerebours, Noël. Traité de photographie derniers perfectionnements apportés au daguerréotype. Paris: Béthune et Plon, June 1843.
Lerebours, Noël. A treatise on photography, containing the latest discoveries and improvements appertaining to the daguerreotype. London: Longman, Brown, Green and Longmans, September 1843.
Lipowitz, A. Die Daguerreotypie oder: praktische Anleitung Lichtbilder sicher und schnell darzustellen und durch galvanoplastisches Verfahren Abdrücke von ihnen zu machen. 1845.
Lowenheim, Frederick. Electroplating. New York: McGraw Hill Book Company, 1978.
Martin, Anton. Repertorium der Galvanoplastik und Galvanostegie oder der Metallreduction auf nassem Wege in dicken und dünnen Schichten, mit besonderer Berücksichtigung der Galvanographie, Glyphography, Chemitypie und der speciellen Anwenung auf das Vergolden, Versilbern, Verbleien, Verzinken u. u. Wien: Karl Gerolds Sohn, 1856.
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Marquis, Emmanuelle, et al. Exposing the sub-surface of historical daguerreotypes and the effects of sulfur-induced corrosion. Corrosion Science 94 (2015): 438-444.
McLeod, Bet, Marian Campbell, Odile Nouvel. A Christofle Electrotype of the Medieval Maître Alpais Ciborium. Susan La Niece, Stefan Röhrs, Bet McLeod (eds.) The Heritage of Maître Alpais. London: British Museum, 2010.
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Nadeau, Luis. Encyclopaedia of Printing, Photographic and Photomechanical Processes. A Comprehensive Reference to Reproduction Technologies containing invaluable information on over 1500 processes. New Brunswick: Atelier, 1990.
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Spencer, Thomas. For the Multiplication of Works of Art in Metal, by Voltaic Electricity. Glasgow: Richard Griffin and Company, 1840.
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Voigt, Jochen, Christoph Kaufmann, Eberhard Patzig, Roland Schwarz, Frank Weiss. Der gefrorene Augenblick. Daguerreotypie in Sachsen 1939-1860. Chemnitz: Edition Mobilis, 2004. von Pauly, Theodor. Gegenwärtiger Standpunkt der Daguerreotypie in Frankreich oder Gründliche Anweisung in dem zehnten Theile einer Secunde Personen und belebte Landschaften abzubilden. Mit besonderer Berücksichtigung der Chemie, so wie mit Angabe eines Verfahrens die Versuche zu colorieren, in Kupfer abzubilden und galvanisch zu vergolden. Nebst einer Beschreibung des Herschelschen Chrysotyps. Arnoldische Buchhandlung: Dresden und Leipzig, 1843.
Walker, Charles. Electrotype Manipulation. Part I. Being the Theory, and Plain Instructions in the Art of Working in Metals, by Precipitating Them from Their Solutions, Through the Agency of Galvanic or Voltaic Electricity. London: George Knight and Sons, 1848.
Ward, John. Encyclopedia of Nineteenth-Century Photography. John Hannavy (ed). New York: Routledge, 2008.
Watt, Charles, John Watt (eds). The Chemist; or, Reporter of Chemical Discoveries and Improvements,and Protector of the Rights of the Chemist and Chemical Manufacturer. London: Stewart and Murray, Old Bailey: 1840.
Wharton, Glenn. Technical Examination of Renaissance Medals the Use of Laue Back Reflection X- Ray Diffraction to Identify Electroformed Reproductions. Journal of the American Institute for Conservation 23.2 (1984): 88-100.
Wiegandt, Ralph, Nicholas Bigelow, Brian McIntyre. A Summary of the National Science Foundation (SCIART) Supported Research of the Daguerreotype: George Eastman House International Museum of Photography and Film, and the University of Rochester. Topics in Photographic Preservation 15 (2013). 160-175.
Wilson, Edward. Wilsons Cyclopaedic Photography. A Complete Hand-Book of the Terms, Processes, Formulae and Appliances Available in Photography, Arranged in Cyclopaedic Form for Ready Reference. New York: Edward L. Wilson, 1894.
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List of figures and tables
Figure 1. Schematic cross-section of a daguerreotype and its electrotype...... 7 Figure 2. Schematic electrolytic cell...... 11 Figure 3. DM-69896 electrotype verso, raking light...... 15 Figure 4. DM-69896 daguerreotype, recto, wax along right edge (raking light photomicrograph)...... 15 Figure 5. Schematic reflection of light at the daguerreotype and electrotype surface...... 15 Figure 6. Illustration of Chevaliers assumed setup for electrotyping daguerreotypes...... 16 Figure 7 (left). Vertical setup for electrotyping, with a battery to the right side...... 18 Figure 8 (right). Horizontal setup for electrotyping, with a battery to the right side...... 18 Figure 9. Setup of the electrolytic cell for the reconstructions...... 23 Figure 10. DB daguerreotype suspended in the electrolytic bath...... 23 Figure 11. Coating the edges of the AO-2 daguerreotype with Paraloid B-72 in acetone. Photo: M. Pilko...... 26 Figure 12 (left). SM-1927-1680 daguerreotype, recto, reflecting dark...... 30 Figure 13 (right). SM-1927-1680 electrotype, recto, reflecting dark...... 30 Figure 14 (left). SM-1927-1680 daguerreotype, recto, reflecting light...... 31 Figure 15 (right). SM-1927-1680 electrotype, recto, reflecting light...... 31 Figure 16 (left). SM-1927-1680 daguerreotype, verso, raking light...... 31 Figure 17 (right). SM-1927-1680 electrotype verso, raking light...... 31 Figure 18. SM-1927-1680 daguerreotype, recto, top right corner...... 32 Figure 19. SM-1927-1680 electrotype, recto, top left corner...... 32 Figure 20. SM-1927-1680 electrotype, verso, upper left edge (90° CCW)...... 32 Figure 21. SM-1927-1680 daguerreotype with a partial hallmark, recto, upper left corner...... 32 Figure 22. SM-1927-1680 electrotype with a reproduced partial hallmark, recto, upper right corner...... 32 Figure 23. SM-1927-1680 daguerreotype, verso...... 33 Figure 24. SM-1927-1680 electrotype, side view, verso facing up...... 33 Figure 25. SM-1927-1680 electrotype, verso, serrated marks from scissors...... 33 Figure 26. SM-1927-1680 electrotype, verso...... 34 Figure 27. SM-1927-1680 electrotype, recto, probable copper corrosion spot, lower right quadrant...... 34 Figure 28 (left). SM-1927-1680 daguerreotype, recto...... 34 Figure 29 (right). SM-1927-1680 electrotype, recto...... 34 Figure 30. SM-1927-1680 daguerreotype...... 35 Figure 31. SM-1927-1680 electrotype, corresponding area to Figure 30...... 35 Figure 32. SM-1927-1680 daguerreotype, crater matching the particle in Figure 33...... 36 Figure 33. SM-1927-1680 electrotype, particle matching crater in Figure 32...... 36 Figure 34. NB electrotype, recto, reflecting dark...... 37 Figure 35. NB electrotype, recto, reflecting light...... 37 Figure 36. NB electrotype, verso in raking light...... 37 Figure 37. NB electrotype, verso, raking light photomicrograph...... 37 Figure 38. NB electrotype, shadow area...... 38 Figure 39. NB electrotype, highlight area...... 38 Figure 40. Silver coupon with dark, non-coherent copper deposit ...... 39 Figure 41. Silver coupon with bright, compact copper deposit...... 39 Figure 42. Silver coupon with copper deposit...... 40 Figure 43. Silver coupon (left) from Figure 42 with trimmed edges and after separation of the copper deposit. 40 Figure 44. Copper deposit partly separated from silver coupon...... 40 Figure 45. AO-4-2 Daguerreotype with copper deposit prior to separation, recto in raking light...... 41 Figure 46. AO-4-2 Daguerreotype, recto, after separation, in normal illumination (left)...... 41 Figure 47. Daguerreotype fragment MO-3, recto, after separation (left) and MO-3 electrotype (right) in normal -3 -3 2 illumination. Obtained from a 0.8 mol dm CuSO4 in 0.5 mol dm H2SO4. Current density: 3.6 A/dm , exposure time: 9 hours. Dimensions (each plate): 41 x 57 x 0,5 (H x W x D in mm). Photo: M. Pilko...... 41 Figure 48. AO-1 daguerreotype, recto, after separation (left), with AO-1-1 electrotype, recto (right), normal illumination, reflecting dark...... 42 Figure 49. AO-1 daguerreotype, recto, after separation (left), with AO-1 electrotype, recto (right), reflecting light...... 42 Figure 50. AO-1 daguerreotype, verso, after separation (left), with AO-1 electrotype, verso (right), normal illumination. Dimensions daguerreotype: 60 x 48 x 0,5 mm (H x W x D in mm)...... 43 Figure 51. AO-1 electrotype, verso top left corner with individual copper nodules on a fine grained copper substrate...... 43
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Figure 52. UvA daguerreotype after separation (left) with electrotype (right), normal illumination, reflecting dark...... 44 Figure 53. AO-2 daguerreotype after separation (left) with electrotype (right), normal illumination, reflecting dark...... 44 Figure 54. AO-1-I electrotype (left) and AO-1-II electrotype (right) in normal illumination, reflecting dark...... 45 Figure 55. AO-1 daguerreotype with image particles and craters...... 46 Figure 56. AO-1 electrotype with pits...... 46 Figure 57. AO-1 daguerreotype...... 46 Figure 58. AO-1 electrotype...... 46 Figure 59. AO-2 daguerreotype, image particles in a midtone area...... 47 Figure 60. AO-2 electrotype. Area corresponding with Figure 59...... 47 Figure 61. AO-2 electrotype...... 47 Figure 62. AO-2 daguerreotype with rupture in the surface...... 48 Figure 63. AO-2 electrotype...... 48 Figure 64. AO-1 daguerreotype, reflecting dark, before electrotyping...... 69 Figure 65. AO-1 daguerreotype after electrotyping (left) with AO-1 electrotype (right), reflecting dark...... 69 Figure 66. AO-2 daguerreotype, reflecting dark, before electrotyping...... 70 Figure 67. AO-2 daguerreotype after electrotyping (left) with AO-2 electrotype (right), reflecting dark...... 70 Figure 68. AO-3 daguerreotype , reflecting dark, before electrotyping...... 71 Figure 69. Left: fragments of the AO-3 daguerreotype (AO-3-1 to AO-3-4) after electrotyping...... 71 Figure 70. AO-4 daguerreotype, reflecting dark, before electrotyping...... 72 Figure 71. Left: AO-4 daguerreotype: control (AO-4-1) and fragments after electrotyping (AO-4-2 to AO-4-4).72 Figure 72. UvA daguerreotype, reflecting dark, before electrotyping...... 73 Figure 73. Left: UvA daguerreotype after electrotyping...... 73 Figure 74. DB daguerreotype, reflecting dark, before electrotyping...... 74 Figure 75. Left: left half of DB daguerreotype (fragments DB-1-1 to DB-1-4) after electrotyping...... 74 Figure 76. Left: right half of DB daguerreotype (DB-2) after electrotyping...... 74 Figure 77. MO daguerreotype, reflecting dark, before electrotyping...... 76 Figure 78. MO daguerreotype cut into fragments (MO-1, MO-2, MO-3), after electrotyping, with MO electrotypes (MO-1, MO-3), reflecting dark...... 76 Figure 79. Set up of XRF analysis for the SM-1927-1680 plates...... 77 Figure 80. Set up of SEM-EDS analysis for the SM-1927-1680 plates...... 82 Figure 81. SM-1927-1680 daguerreotype, SEM BSE image, magnified 14,452x...... 83 Figure 82. SM-1927-1680 electrotype, SEM BSE image, magnified 12,152x...... 85 Figure 83. NB electrotype, SEM BSE image, magnified 10,000x...... 87 Figure 84. AO-2 electrotype mounted to the stage of the SEM-EDS instrument with copper tape...... 89 Figure 85. AO-1 daguerreotype, SEM BSE image, magnified 16299...... 90 Figure 87. AO-1 electrotype, SEM BSE image, magnified 5705...... 92 Figure 87. AO-1 electrotype, SEM BSE image, magnified 8150...... 93 Figure 88. AO-1 electrotype, SEM BSE image, magnified 8150...... 94 Figure 89. AO-2 daguerreotype, SEM BSE image, magnified 13039...... 95 Figure 90. AO-2 daguerreotype, SEM BSE image, magnified 4075...... 97 Figure 91. AO-2 electrotype, SEM BSE image, magnified 8150...... 98 Figure 92. AO-2 electrotype, SEM BSE image, magnified 13039...... 99 Figure 93. AO-2 electrotype, SEM BSE image, magnified 3260...... 100
Table 1. Overview of the reconstruction tests carried out on different daguerreotypes...... 27 Table 2. Major EDS peaks for the SM-1927-1680 plates...... 36 Table 3. Major EDS peaks for the NB daguerreotype electrotype. X indicates presence of the respective element. Spectra are reproduced in Appendix VIII.2. NB plate...... 38 Table 5. Major EDS peaks for the AO-1 & AO-2 plates...... 48 Table 6. Features of historical daguerreotype electrotypes that could be reproduced by the reconstruction tests. X indicates the presence of the respective feature...... 52 Table 6. Information on the making of the modern AO-daguerreotypes...... 68 Table 7. Testing of a coating on the AO-1 daguerreotype...... 69 Table 8. Testing on the AO-2 daguerreotype of a coating thinner than that of the AO-1 daguerreotype...... 70 Table 9. Testing the effect of different current densities for electrotyping daguerreotypes...... 71 Table 10. Testing the effect of different current densities and beeswax coating (fragment AO-4-3) on a daguerreotype to be electrotyped...... 72 Table 11. Testing the effect of a beeswax coating on a 19th century daguerreotype to be electrotyped...... 73 Table 12. Testing the effect of different coatings on a 19th century daguerreotype to be electrotyped...... 75 Table 13. Testing the effect of gold-toning for a daguerreotype to be electrotyped...... 76
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Appendices
Appendix I Terminology
Terms used specifically in the context of Author / Source electrotyping daguerreotypes Epreuves électrotypiques Chevalier 1841: 60. Electrotype Smee: 1841: 134. Electrotype process Smee 1852: 328. Electrotype copy Shaw 1844: 173. Counter-proof Lerebours 1843 (September): 119. Contre-épreuve Lerebours 1843 (June): 127. Tithonotype Draper 1843: 175. Electrotype copy Humphrey 1858: 167. Galvanic daguerreotypes Wilson 1894: 168. Galvanoplastische Reproduktion Krone 1985 (1907): 35. Photogalvanic copy Buerger 1989: 86. Tithonotype, Tithnotype, Tithonotypie Nadeau 1990: 450. Galvano Voigt 2004: 42.
BnF 2017: 17 April 2017. Galvanoplastie
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Appendix II References in literature to makers of daguerreotype electrotypes
Date Name Place Reference 1840 Mr. F. W. Enzmann Dresden Voigt 2004: 43. Hippolyte Fizeau Paris Lerebours September 1843: 117. 1840 Saxton, Joseph Philadelphia Gillespie 2016: 145. 1841 Charles Louis Chevalier Paris Chevalier 1841: 60 1841 Dr. Symon Dover Smee 1841: 134. 1842 F. Strehlke ? Strehlke 1843: 146 1843 Gaudin, Marc-Antoine ? von Pauly 1843, 84. 1843 Mr Endicott New York Draper 1843: 176. 1851 Griffiths & Le Beau 15 Coborn Road, Mile End, Royal Commission 1851: 441. London 1858 Fitzgibbon, John H. ? Humphrey 1858: 169. 1856 Captain Pöschel Dresden Martin 1856: 110. 1852 Mr. Horn Newgate street Smee 1852: 328. ? Henry Collen England Ward 2008: 312. 1860 Dr Thomas Paterson Glasgow Napier 1860: 67. 1860 Mr Bawtree London Napier 1860: 67.
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Appendix III Overview of potential daguerreotype electrotypes in collections
Dimensions Inventory Photographer Object Description Collection H x W x L in Number mm Daguerreotype Deutsches Not given & Portrait of man 71 x 53 x ca. 0.5 DM 69896 Museum Electrotype
Daguerreotype Science SM 1927- Not given & Portrait of man Museum 54 x 39 x ca. 0.39 1680 [?] Electrotype London Musée d'art Daguerreotype Vue de Poitevin, moderne et MAMCS & Conflans-sur- 105 x 140 Alphonse contemporain 77.992.8.1 Electrotype Anille Strasbourg Fizeau, Daguerreotype Young man GEH Hippolyte; George Eastman & seated with cigar 101 x 76 1969.0265.020 Foucault, House Electrotype in mouth 0 Léon
Fizeau, Dôme des J. Paul Getty GET Electrotype 176 x 112 Hippolyte Invalides, Paris Museum 84.XT.265.5
Countryside view with Fizeau, J. Paul Getty GET Electrotype chateau or 92 x 154 Hippolyte Museum 84.XT.1052 palace at crest of hill
Fizeau, Entrée du port Unknown Electrotype Not given Not given Hippolyte du Havre (Auctioned)
Woodbury, National Media NMM 1888- Walter Electrotype Portrait of man Museum 52 x 39 163 Bentley Bradford
Street scene with Unknown Not given Electrotype Not given Not given tree (Auctioned)
Repro of a painting of a Nicholas post mortem Burnett Not given Electrotype 66 x 86 x ca. 0.43 Not given portrait of Reference Florimond de Collection Coster GRASSI Detail of Museum für GRA Not given Electrotype 64 x 53 architecture Angewandte B.2002.78 Kunst Leipzig First of two Bibliotheque Not given corresponding Male nude nationale de 105 x 80 BN 69033069 electrotypes France
Second of two Bibliotheque Not given corresponding Male nude nationale de 105 x 80 BN 6903307 electrotypes France
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Appendix IV Historical instructions on electrotyping daguerreotypes See additional Appendix IV
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Appendix V Materials and Suppliers
Materials Suppliers Van der Linde Beeswax, bleached, in beads Rozengracht 36-38 NL-1016 NT Amsterdam
Copper plates, 0.5 mm thick Inventory UvA, metal department
Copper wire, diameter 1 mm Inventory UvA, metal department
Snap-off knife (Stanley) Inventory UvA, photography department
Filter paper, circles, diameter 185 mm Personal loan from M. Jürgens
Glass basin Inventory UvA, metal department
Glass beakers (Fisher Brand) Inventory UvA, metal department
Gloves, nitrile (Kimtech Science Brand) Inventory UvA, photography department
Jigsaw with metal saw blades No. 2/0 (Gazelle) Inventory UvA, metal department
Van der Linde Paper clips, iron, silver, 2.5 cm (Sumind) Rozengracht 36-38 NL- 1016 NT Amsterdam Linseed oil varnish (Kremer Pigmente) Inventory UvA, wood and furniture department
Paraloid B-72 Inventory UvA, photo department
Pipette, plastic Inventory UvA, photo department
PH strips, pH 0 - 14 universal indicator Inventory UvA, metal department (MColorpHast)
Polyester film (Melinex) Inventory UvA, photo department
Rouge de Paris (DiaLux) Inventory UvA, metal department
Bijou modern, Postbus 99, Sterling silver plate 925, 0.5 mm NL- 2665 ZH Bleiswijk, personal loan from M. Jürgens
Steel wool Inventory UvA, metal department
Tyvek tape (Lineco) Inventory UvA, photography department
Wooden cocktail sticks Inventory UvA, photography department
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Chemicals Supplier
Acetone, > 99.0 %, CAS: 67-64-1 (Acros Organics) Inventory UvA, photo department
Copper (II) sulfate pentahydrate, ACS, 98.0-102.0%, Thermo Fisher (Kandel) GmbH Postfach, 110765 Crystalline, CAS: 7758-99-8 (Alfa Aesar) GE-76057, Karlsruhe
Ethanol, 99.8%, CAS: 64-17-5 (Acros Organics) Inventory UvA, photo department
Sulfuric acid, CAS: 7664-93-9 (Acros Organics) Inventory UvA, metal department
White Spirits, for laboratory use, CAS: 8052-41-3 Inventory UvA, photo department (Chem-Lab)
Equipment Supplier
Bunsen burner Personal loan from M. Jürgens
Cables with battery clamps Inventory UvA, metal department
Hot plate, Inventory UvA, photo department (IKA, RCT basic) Rectifier 1: Inventory UvA, metal department EA-PS 3016-10, with DC 0-16V, max. 10A Rectifier 2: Personal loan from T. Beentjes Weir 460, with a DC of 0-60V, max. 3A
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Appendix VI Documentation of specimens before and after electrotyping
VI.1. Anton Orlov daguerreotypes (AO)
Photographer: Anton Orlov Size: ca. 60.25 x 48 x 0.5 mm (H x W x D) Place of making: San Diego Date of making: 4 February 2017 Lens: Schneider Super Angulon 65 mm (older 5.6 version) Daguerreotype plate: traditional roll clad plate (Sheffield plate) purchased from Mike Robinson, Century Darkroom, Canada. Collection: Magdalena Pilko study collection
Plate No. AO-1 AO-2 AO-3 AO-4 Treatment 40 sec: 35 sec: 35 sec: 35 sec: Sensitizing/ deep gold, deep gold, deep gold, gold, Iodine hints of pink pink edges hints of pink hints of pink Sensitizing/ 10 sec.: 12 sec.: 10 sec.: 8 sec.: Bromine deep rose, centre light rose medium rose light rose Sensitizing/ 8 sec 8 sec 8 sec 8 sec Iodine Mercury 5 min at 65°C 5 min at 65°C 5 min at 65°C 5 min at 65°C Development
Gilding 1 -2 min 1 -2 min 1 -2 min 1 -2 min
Exposure time 30 sec 25 sec 25 sec 25 sec
Aperture 8 8 8 8
4-02-2017, 4-02-2017, 4-02-2017, 4-02-2017, Date / Time 1 pm, 1: 24 pm, 1:50, 2:06 pm, full sun full sun full sun full sun Table 6. Information on the making of the modern AO-daguerreotypes.
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VI.2. AO-1 plate
Figure 64. AO-1 daguerreotype, Figure 65. AO-1 daguerreotype after electrotyping (left) with AO-1 reflecting dark, before electrotype (right), reflecting dark. electrotyping.
Treatment Current Specimen Result daguerreotype density Daguerreotype: positive image in Coating of Paraloid B72 reflected light, negative image in on the verso and along reflected dark. Yellowish image the edges 2 hue, wipe marks, copper residues AO-1 Application of a 3.46 A/dm along the edges beeswax coatingon the Electrotype: copper colour, recto of the positive image in reflected dark, daguerreotype negative image in reflected light Table 7. Testing of a coating on the AO-1 daguerreotype.
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VI.3. AO-2 plate
Figure 66. AO-2 daguerreotype, Figure 67. AO-2 daguerreotype after electrotyping (left) with AO-2 reflecting dark, before electrotype (right), reflecting dark. electrotyping.
Treatment Current Specimen Result daguerreotype density Daguerreotype: positive image in reflected light, negative image in Coating of Paraloid B72 on reflected dark. Yellowish image hue, the verso and along the wipe marks, copper residues along edges the edges Main image area: Electrotype: Main image area: Application of a beeswax copper colour, positive image in AO-2 3.46 A/dm2 coating on the recto of the reflected dark, negative image in heated daguerreotype reflected light. Slight silver- Left edge: no coating yellowish cast, less contrast than Far left edge: not AO-1 electrotyped Right edge: silver-yellowish cast with faint positive image. Table 8. Testing on the AO-2 daguerreotype of a coating thinner than that of the AO-1 daguerreotype.
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VI.4. AO-3 plate
Figure 68. AO-3 daguerreotype , Figure 69. Left: fragments of the AO-3 daguerreotype (AO-3-1 to AO-3- reflecting dark, before 4) after electrotyping. electrotyping. Right: AO-3 electrotypes (AO-3-1, AO-3-3 and AO-3-4), reflecting dark.
Treatment Current Specimen Result daguerreotype density Daguerreotype: matte, white haze 2 AO-3-1 1.39 A/dm Electrotype: silver-yellowish cast with faint positive image 2 AO-3-2 0.96 A/dm Not separated Coating of Paraloid B72 Daguerreotype: matte, white haze on the verso and along 2 AO-3-3 the edges. 0.8 A/dm Electrotype: silver-yellowish cast with faint positive image Daguerreotype: matte, white haze 2 AO-3-4 3.42 A/dm Electrotype: silver-yellowish cast with faint positive image Table 9. Testing the effect of different current densities for electrotyping daguerreotypes.
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VI.5. AO-4 plate
Figure 70. AO-4 daguerreotype, Figure 71. Left: AO-4 daguerreotype: control (AO-4-1) and fragments reflecting dark, before after electrotyping (AO-4-2 to AO-4-4). electrotyping. Right: E-AO-4 electrotypes (AO-4-2 to E-AO-4-4), reflecting dark.
Treatment Current Specimen Result daguerreotype density AO-4-1 No treatment (control) Daguerreotype: matte, white haze Coating of Paraloid B72 AO-4-2 on the verso and along 3.42 A/dm2 Electrotype: silver - yellowish cast the edges with faint positive image
Coating of Paraloid B72 on verso and along the Daguerreotype: positive image in edges reflected light, negative image in Beeswax in turpentine 2 reflected dark AO-4-3 3.42 A/dm on recto, applied and Electrotype: copper colour, wiped off with deerskin positive image in reflected light, Application directly negative image in reflected dark before electrotyping Coating of Paraloid B72 Daguerreotype: matte, white haze 2 AO-4-4 on the verso and along 5.06 A/dm Electrotype: silveryellowish cast the edges with faint positive image Table 10. Testing the effect of different current densities and beeswax coating (fragment AO-4-3) on a daguerreotype to be electrotyped.
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VI.6. UvA study collection plate (UvA)
Photographer: unknown Date: approx. 1840-1860 Dimensions: 62 x 50 x 0.5 (H x W x D, in mm) Collection: UvA study collection
Figure 72. UvA daguerreotype, reflecting Figure 73. Left: UvA daguerreotype after electrotyping. dark, before electrotyping. Right: UvA electrotype. Both reflecting dark.
Treatment Current Specimen Result daguerreotype density - Daguerreotype: Left half: positive image in reflected dark and negative Coating of Paraloid B72 image in reflected light. on the verso and along 2 Right half: white haze with faint UvA 3.57 A/dm the edges image Left half of the recto is Electrotype: coated with beeswax in Left half: silvery cast turpentine Right half: positive image in reflected dark and negative image in reflected light Table 11. Testing the effect of a beeswax coating on a 19th century daguerreotype to be electrotyped.
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VI.7. Daniel Blau plate (DB)
Photographer: unknown Date: 1840-1860 Dimensions: 82 x 57 x 0.5 (H x W x D, in mm) Collection: Rijksmuseum Amsterdam study collection
Figure 74. DB Figure 75. Left: left half of DB Figure 76. Left: right half of DB daguerreotype, reflecting daguerreotype (fragments DB-1-1 to daguerreotype (DB-2) after dark, before electrotyping. DB-1-4) after electrotyping. electrotyping. Right: corresponding electrotypes Right: corresponding electrotype (fragments DB-1-1, DB-1-3 and DB-1- (DB-2). 4).
Treatment Current Specimen Result daguerreotype density Coating of Paraloid B72 on verso and along the edges 2 Daguerreotype: white haze DB-1-1 3.57 A/dm Coating of linseed oil Electrotype: copper colour with (Kremer) on recto, silvery cast application directly before electrotyping DB-1-2 No treatment.
(control) Coating of Paraloid B72 on verso and along the Daguerreotype: fine wax streaks edges and droplets on surface, which Coating of beeswax in could be wiped off DB-1-3 turpentine on recto, 3.57 A/dm2 Electrotype: copper colour with applied on heated faint image and streaks. The daguerreotype and copper shows local droplet wiped off with deerskin. formations Application directly before electrotyping
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Coating of Paraloid B72 on verso and along the Daguerreotype: tiny oil droplets, edges which could be wiped off Coating of linseed oil 2 Electrotype: copper colour with 3.57 A/dm DB-1-4 (Kremer) on recto, silvery cast (thin oil layer, right
applied and wiped off edge and centre) and cast of with deerskin circular oil droplets (thick oil Application directly layer, left edge) before electrotyping Daguerreotype: white haze in large areas. Image partially visible as positive in reflected dark and as Coating of Paraloid B72 2 DB-2 3.57 A/dm negative in reflected light on the verso and along Electrotype: silvery cast in large the edges areas. Image partially visible as positive in reflected dark and as negative in reflected light Table 12. Testing the effect of different coatings on a 19th century daguerreotype to be electrotyped.
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VI.8. Marinus Ortelee daguerreotype (MO)
Photographer: Marinus Ortelee Date of making: 2016 Dimensions: 82 x 57 x 0.5 (H x W x D, in mm) Collection: Rijksmuseum Amsterdam study collection
Figure 77. MO daguerreotype, reflecting Figure 78. MO daguerreotype cut into fragments (MO-1, MO- dark, before electrotyping. Brownish area 2, MO-3), after electrotyping, with MO electrotypes (MO-1, (centre) of this daguerreotype was gold- MO-3), reflecting dark. toned.
Treatment Current Specimen Result daguerreotype density No clear interpretation. Coating of Paraloid B72 Electrodeposition took place on on the verso and along both sides of the daguerreotype due the edges MO-1 to a lacking coating with Paraloid (upper left) Application of a coating 3.6 A/dm2 B72. The electrotyped verso was (beeswax diluted in folded backwards at the left edge white spirits 1:25) on and the three other edges were cut the recto of the off daguerreotype MO-2 (upper right, No treatment. control) Daguerreotype: matte, white haze at the centre, reflective silver along the edges Coating of Paraloid B72 MO-3 on the verso and along 3.6 A/dm2 Electrotype: Gold-toned area: (lower half) the edges. silver-yellowish cast with faint positive image Not gold-toned area: copper colour with faint, positive image Table 13. Testing the effect of gold-toning for a daguerreotype to be electrotyped.
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Appendix VII XRF examination
VII.1. SM-1927-1680 1 & 2 and NB plate
Conducted by Nicholas Burnett Instrument specifications: Tracer LER538 by Broker, light Element detector, (Silicon Drift) calibrated for RoHS elements and standard metal alloys Place: Museum Conservation Services Ltd, Duxford Conditions: operated at 45.00 kV and 30.00 µA, time of measurement 70.34 seconds, Date: 12-04-2017
Figure 79. Set up of XRF analysis for the SM-1927- 1680 plates.
1. Tracer XRF Spectrum of SM-1927-1680 daguerreotype, recto:
x 1E3 Pulses 150
100
Au Hg Hg Ag Cu Au Ag Cu Au Ag
50
0 0 500 1000 1500 2000
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2. Tracer XRF Spectrum of SM-1927-1680 daguerreotype, verso:
3. Tracer XRF Spectrum of SM-1927-1680 electrotype, recto:
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4. Tracer XRF Spectrum of SM-1927-1680 electrotype, verso:
VII.2. NB plate
1. Tracer XRF Spectrum of NB-electrotype, recto:
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VII.3. AO-4 plates
Conducted by Martin Jürgens Instrument specifications: Artax by Bruker Place: RCE/Rijksmuseum Amsterdam Conditions: molybdenum tube, operated at 50 kV and 400 µA, time of measurement 122 seconds for each measurement, helium atmosphere (see further specifications on the conditions at the end of this appendix). Date: 10-5-2017
1. Artax XRF Spectrum of AO-4-1 daguerreotype (unprocessed area):
red = highlight green = shadow
2. Artax XRF Spectrum of AO-4-2 daguerreotype (after electrotyping):
red = highlight green = shadow
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3. Artax XRF Spectrum of AO-4-2 electrotype:
red = highlight green = shadow
Exemplary parameters of AO-4-2 electrotype (The energy, dead time, and axes parameters for the other measurements vary slightly):
Channel count: 4096 Energy absolute: -1-1964 keV Energy linear: 0.0124444 keV/ch FWHM Mn-K: 144.01 eV Fano factor: 0.11
Excitation Anode: Mo Filter: No filter Energy: 48.8 keV Optic: Lens 0.060 Atmosphere: Helium
Measurement Real time: 122s Live time: 120s Dead time: 1.9% Pulse density: 9448 cps
X-ray Generator Voltage: 50 kV Current: 400 µA
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VIII.1. SM-1927-1680 1 & 2
Conducted by Dr. Iris Buisman Instrument specifications: FEI instrument, model: Quanta 650F. Place: Earth Sciences Department, University of Cambridge. Conditions: Uncoated sample, final aperture of 50 um, 15 kV, high vacuum. Date: 13-04-2017
Figure 80. Set up of SEM-EDS analysis for the SM-1927-1680 plates.
Electrotyping Daguerreotypes: Reconstruction of an Early Reproduction Technique
Figure 81. SM-1927-1680 daguerreotype, SEM BSE image, magnified 14,452x. SEM-EDS measurements at 7 points, of which only 4 are given here.
1. EDS Spectrum of SM-1927-1680 daguerreotype, surface 1:
2. EDS Spectrum of SM-1927-1680 daguerreotype, crater (point crator(sic), meaning crater):
3. EDS Spectrum of SM-1927-1680 daguerreotype, particle 1:
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4. EDS Spectrum of SM-1927-1680 daguerreotype, particle 3:
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Figure 82. SM-1927-1680 electrotype, SEM BSE image, magnified 12,152x. SEM-EDS measurements at 7 points, of which only 4 are given.
1. EDS Spectrum of SM-1927-1680 electrotype, surface 1:
2. EDS Spectrum of SM-1927-1680 electrotype, particle 1:
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3. EDS Spectrum of SM-1927-1680 electrotype, particle 2:
4. EDS Spectrum of SM-1927-1680 electrotype, pit:
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VIII.2. NB plate
Figure 83. NB electrotype, SEM BSE image, magnified 10,000x. SEM-EDS measurements at 4 points, of which only 3 are shown.
1. EDS Spectrum of NB electrotype, surface:
2. EDS Spectrum of NB electrotype, spec 1:
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3. EDS Spectrum of NB electrotype, pit:
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VIII.3. AO-1 plates
Conducted by Dr. Ineke Joosten Instrument specifications: NovaNano SEM45, FEI, EDX: SDD from Thermo Scientific with NSS software Owner/Place: RCE Amsterdam Conditions: Uncoated sample, 15 kV, high vacuum. Date: 16-05-2017
Figure 84. AO-2 electrotype mounted to the stage of the SEM-EDS instrument with copper tape.
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Figure 85. AO-1 daguerreotype, SEM BSE image, magnified 16299. SEM-EDS measurements at 7 points, of which only 3 are shown.
1. EDS Spectrum of the AO-1 daguerreotype, large image particle (point 1):
2. EDS Spectrum of the AO-1 daguerreotype, hole (point 2):
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3. EDS Spectrum of the AO-1 daguerreotype, surface (point 3):
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Figure 86. AO-1 electrotype, SEM BSE image, magnified 5705. SEM-EDS measurements at 7 points, of which only 2 are shown.
1. EDS Spectrum of the AO-1 electrotype, surface (point 1):
2. EDS Spectrum of the AO-1 electrotype, pit (point 4):
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Figure 87. AO-1 electrotype, SEM BSE image, magnified 8150. SEM-EDS measurement at 1 point.
1. EDS Spectrum of the AO-1 electrotype, large particle (point 1):
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Figure 88. AO-1 electrotype, SEM BSE image, magnified 8150. SEM-EDS measurement at 1 point.
1. EDS Spectrum of the AO-1 electrotype, small particle (point 1):
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VIII.4. AO-2 plates
Conducted by Dr. Ineke Joosten Instrument specifications: NovaNano SEM45, FEI, EDX: SDD from Thermo Scientific with NSS software Owner/Place: RCE Amsterdam Conditions: Uncoated sample, 15 kV, high vacuum. Date: 9/06/20017
Figure 89. AO-2 daguerreotype, SEM BSE image, magnified 13039.
SEM-EDS measurements at 3 points.
1. EDS Spectrum of the AO-2 daguerreotype, particle (point 1):
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2. EDS Spectrum of the AO-2 daguerreotype, surface (point 2):
3. EDS Spectrum of the AO-2 daguerreotype, hole (point 3):
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Figure 90. AO-2 daguerreotype, SEM BSE image, magnified 4075. SEM-EDS measurements at 3 points, of which only 2 are shown.
1. EDS Spectrum of the AO-2 daguerreotype, rupture (point 1):
2. EDS Spectrum of the AO-2 daguerreotype, surface without rupture (point 2):
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Figure 91. AO-2 electrotype, SEM BSE image, magnified 8150. SEM-EDS measurements at 3 points, of which only 1 is shown.
1. EDS Spectrum of the AO-2 electrotype, layer on top of copper substrate (point 1):
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Figure 92. AO-2 electrotype, SEM BSE image, magnified 13039. SEM-EDS measurement at 1 point.
1. EDS Spectrum of the AO-2 electrotype, particle (point 1):
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Figure 93. AO-2 electrotype, SEM BSE image, magnified 3260. SEM-EDS measurements at 4 points, of which only 2 are shown.
1. EDS Spectrum of the AO-2 electrotype, particle in layer on top of copper substrate (point 1):
2. EDS Spectrum of the AO-2 electrotype, surface (point 4):
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