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Study on Microbubble of Cellulose Acetate

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Study on Microbubble of Cellulose Acetate Jia et al. Herit Sci (2020) 8:29 https://doi.org/10.1186/s40494-020-00374-3 RESEARCH ARTICLE Open Access Study on microbubble of cellulose acetate microflm of the Republic of China (AD 1912– 1949) collected in the Second Historical Archives of China Zhihui Jia*, Yuhu Li*, Yunpeng Qi, Yajun Zhou, Daodao Hu, Xiaolian Chao, Huiping Xing and Jing Li Abstract The white spots known as microbubbles that are formed in cellulose acetate flm, signifcantly afects the texture of the image. However, the formation of microbubbles and their corresponding microstructure are poorly understood. In this paper, cellulose acetate microflm from the Republic of China (AD 1912–1949) collected in the Second Histori- cal Archives of China was chosen as a prototype to investigate the causes of microbubble disease for the frst time. A comparative study was conducted between the flm samples with and without microbubbles. Herein, the microstruc- tural analyses including optical and SEM microscopy were conducted. The crystals in the microbubbles proved to be triphenyl phosphate as identifed by NMR spectroscopy and SEM–EDX. Comparative properties of the flm substrate with and without microbubbles were measured by TG, XRD and FT-IR spectroscopy. The results show that formation of microbubbles was generally accompanied with the vinegar syndrome and was produced between the protective and emulsion layers with the diferent types of shapes along the closed structure (the diameter of ~ 0.1–2 mm). The formed microbubble was flled with plasticizer. Based on the above-mentioned results, the possible formation process of microbubble was proposed in the present study. The results can provide support for the cause of microbubbles and basis for the conservation of photographic flms. Keywords: Microstructural analysis, Cellulose acetate, Photographic flm, Microbubble Introduction as mildew, vinegar syndrome etc. which result from the Photographic flms, the most important carriers of artis- materials properties and preservation environment [3– tic information and archives, record some key historical 7]. White spotted disease is a special disease produced events (e.g. economic, cultural, and lifestyle). Tey mainly in the cellulose acetate flm, often called “microbubble” include cellulose nitrates, cellulose acetates and polyester disease, signifcantly afects the texture of image and the [1]. Cellulose acetate ester materials have been widely safety of flm (Fig. 1). used in various felds all over the world for their ease of Te deterioration processes efect on the stability of access and safety for about 100 years. In particular, it was cellulose ester plastics has attracted signifcant atten- used as a substrate for photographic flm instead of the tion [8–11]. In general, the remarkable character of cel- highly fammable cellulose nitrate [2]. However, cellu- lulose acetate degradation is deacetylation, which is lose acetate flm can be afected by many diseases such mainly expressed by the increase of acidity [12, 13]. Te stability of the substrate will be greatly reduced with *Correspondence: [email protected]; [email protected] the increasing concentration of acetic acid [14–16]. Engineering Research Center of Historical Cultural Heritage Conservation, In addition, the loss of plasticizer leads to a decrease Ministry of Education, School of Materials Science and Engineering, Shaanxi Normal University, Xi’an, Shaanxi 710119, China of mechanical strength of materials and deformation © The Author(s) 2020. This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http://creat​iveco​ mmons​.org/licen​ses/by/4.0/. The Creative Commons Public Domain Dedication waiver (http://creat​iveco​mmons​.org/publi​cdoma​in/ zero/1.0/) applies to the data made available in this article, unless otherwise stated in a credit line to the data. Jia et al. Herit Sci (2020) 8:29 Page 2 of 10 Fig. 1 Cellulose acetate microflm of the 1946s collected in the Second Historical Archives of China: a The sample with microbubbles disease; b The sample without microbubbles disease during the degradation process, which results in embrit- structure and composition were identifed by NMR spec- tlement [17–19]. In terms of repair and protection, the troscopy and SEM–EDX. Comparative properties of the flm foundation of America has invested a lot of fnan- flm substrate with and without microbubbles have been cial resources in supporting flm protection projects and tested by TG, XRD and FT-IR spectroscopy. developing flm protection guidelines, which provide the most basic theoretical knowledge of flm protection [20, Materials and methods 21]. In contrast to the above-mentioned methods, digital Sample description restoration technology is a safe and reliable restoration Cellulose acetate microflms of the Republic of China method, which can obviously improve the quality of flm (1946s) collected in the Second Historical Archives of images [22–24]. Our group has been engaged in the pro- China were selected in this study. Tese microflms tection research of cellulose acetate flm for many years, belong to cellulose acetate positive flm and record some and some important achievements have been made in important China’s diplomacy events during the repub- terms of scratches, mildew and comprehensive treatment lic of China. Tey are very valuable cultural relics. Some of vinegar syndrome [25–28]. All the above milestone regions of the microflms produced white spots (micro- investigations provide fundamental insights and lay solid bubbles) disease and its distribution was uncertain. Te foundations for the prevention and control of flm dis- disease was found throughout the flm (Fig. 1a), while the ease. Among these diseases, microbubbles are a special other parts were not found to have such disease (Fig. 1b). disease, produced in cellulose acetate flm, signifcantly In the present study, two rolls of microflms with and afecting the texture of the image. However, to the best without microbubbles were investigated. Te sample of our knowledge, there are no previous studies about with image information was selected when non-destruc- the cause of flm microbubble disease. Furthermore, the tive testing was used (e.g. optical microscopy), whereas repair method is limited to date. Terefore, in order to the sample without image information was selected at the better preserve the flm and to eliminate the negative edge of microflms when the damaged testing was used impact of microbubbles, a sound understanding of the (e.g. scanning electron microscope (SEM)). cause of microbubble formation is indispensable. Te purpose of this study is to explore the causes of Methods microbubble disease and provide a scientifc basis for bet- Microscopic analysis ter preservation of cellulose acetate flm. Samples of cel- Te shape of the microbubbles was observed using lulose acetate microflm from the Republic of China (AD transmitted light under an optical microscope (XWY-VI 1912–1949) collected in the Second Historical Archives Fiber analyzer). Te flm was placed in the microscope of China, including flm with and without microbub- with the image layer facing up. Te SEM images were bles disease, were selected to study the causes of micro- obtained from the image layer: Two pieces of flm with 2 bubble disease for the frst time. Te microstructural and without microbubbles (~ 5 × 5 mm ) which con- analyses were conducted on cellulose acetate microflm tain no image information were chosen at the edge of samples by optical microscopy and SEM. Te crystals in flm and placed on a double sided sticky tape on alu- the microbubbles were extracted and purifed, and their minum SEM specimen holders. Several coupons were Jia et al. Herit Sci (2020) 8:29 Page 3 of 10 examined using a Hitachi SU3500 SEM. Analyses were Characterization of substrate microstructure performed at low vacuum (1–150 Pa), with an acceler- To investigate the substrate microstructures, the image ating voltage of 5 kV. Magnifcation was 40 × . Cellu- layer of the microflm samples was removed to obtain the losic acetate microflms with and without microbubbles substrate materials which were tested as follows: were soaked in distilled water for 10 min, placed in the freeze-dryer for 24 h for routine freeze-drying, the mor- (a) TG: Q600 thermal gravimetric analyzer (TG) was phology of microflm image layer was observed by SEM. used to analyze the thermal stability of the sheet For the cellulosic acetate microflms with microbubbles, substrate material with and without microbubble it was cut in the middle microbubble using a scalpel. disease. Samples of initial weight was 3 mg, nitro- SEM images and elemental maps were generated with gen fow was 10 ml/min, the heating rate was 10 °C/ a HITACHI SU3500 SEM coupled with an AMETEK min, temperature range was 40–600 °C. EDAX Octane Elite EDX System. Magnifcation was (b) XRD: Te samples were two small pieces of sub- 2 150 × . strate materials (about 5 × 5 mm ). Rigaku D/max- iii powder X-ray difractometer (XRD) was used to Hydrophilic test test the crystalline structure of substrate with and without microbubble disease. Test condition: Cu (a) Contact angle: Te contact angle of the microflm target Kα line was radiation source, lambda = 1.5418 samples was measured by hanging drop method Å, voltage was 40 kV, current was 30 mA, scanning with video optical contact angle tester (Dataphys- speed was 8°/min, scanning range was 10°–40°.
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