Crystal Growth and Defects
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Sapphire: Properties, Growth, and Applications
Sapphire: Properties, Growth, and 1904), which is sometimes called the flame fusion method. In this technique, alumina powder to be Applications crystallized is fused in a hydrogen–oxygen flame and falls on the molten upper surface of an oriented seed Sapphire has a high refractive index and a broad crystal placed in a furnace (Fig. 1(a)). transmission band spanning the UV, visible, and IR Since this is not a refined process, the material can bands. Sapphire also has a high hardness and melting contain voids and powder inclusions and is likely to be point, and very good thermal conductivity, tensile strained. However, crystals of up to 60mm in diameter strength, and thermal shock resistance (Table 1). The can be grown by this method. Figure 2 shows typical favorable combination of excellent optical and mech- sapphire boules grown by the Verneuil technique. anical properties of sapphire, together with high chemical durability, makes it an attractive structural material for high-technology applications. Sapphire crystals are used in medicine and blood chemistry as 1.2 Czochralski Growth they are resistant to human blood and body fluids, and are totally impervious to moisture and chemically This technique originates from pioneering work by inert. Frequently it is the combination of two, or more, Czochralski (1917). Crystals grow from the meniscus of its properties that make sapphire the only material formed on a free surface of the melt onto the seed available to solve complex engineering design crystal of the required crystallographic orientation. problems. The pull rod is lifted and rotated, and crystallization However, sapphire is difficult to shape owing to its onto the end of the seed occurs (Fig. -
Development Team
Material science Paper No. : Crystallography & crystal growth Module : Growth from melt II Development Team Prof. Vinay Gupta, Department of Physics and Astrophysics, Principal Investigator University of Delhi, Delhi Prof. P. N. Kotru ,Department of Physics, University of Jammu, Paper Coordinator Jammu-180006 Content Writer Prof. P. N. Kotru ,Department of Physics, University of Jammu, Jammu-180006 Prof Mahavir Singh Department of Physics, Himachal Pradesh Content Reviewer University, Shimla 1 Crystallography & crystal growth Material science Growth from melt II Description of Module Subject Name Physics Paper Name Crystallography & crystal growth Module Name/Title Growth from melt II Module Id 31 2 Crystallography & crystal growth Material science Growth from melt II 31 Bridgman-Stockbarger Growth Technique. 31.1 Introduction The techniques were originated by Bridgman (1925) and Stockbarger (1938) and so are named after them. In these techniques a crucible containing the material to be grown is lowered through a furnace in such a way that the lowest point in the crucible and the solidification surface rises slowly up the crucible. It means that the melt contained in the crucible is progressively frozen to yield a single crystal. The rate of lowering the crucible may range from about 0.1 to 200 mmh─1 but in most of the cases it may range somewhere in between 1-30 mmh─1. There are situations where the movement of the crucible is reversed. In other words, the crucible is raised up through the furnace and so is advantageously applicable for materials which are volatile; the interface with the vapour being the coolest part of the charge. -
Ga2o3 and Its Vertical Structure Leds
micromachines Review Epitaxy of III-Nitrides on β-Ga2O3 and Its Vertical Structure LEDs Weijiang Li 1,2,3, Xiang Zhang 1,2,3, Ruilin Meng 1,2,3, Jianchang Yan 1,2,3, Junxi Wang 1,2,3, Jinmin Li 1,2,3 and Tongbo Wei 1,2,3,* 1 State Key Laboratory of Solid-State Lighting, Institute of Semiconductors, University of Chinese Academy of Sciences, Beijing 100083, China; [email protected] (W.L.); [email protected] (X.Z.); [email protected] (R.M.); [email protected] (J.Y.); [email protected] (J.W.); [email protected] (J.L.) 2 Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China 3 Beijing Engineering Research Center for the 3rd Generation Semiconductor Materials and Application, Beijing 100083, China * Correspondence: [email protected]; Tel.: +86-010-8230-5430 Received: 7 April 2019; Accepted: 8 May 2019; Published: 13 May 2019 Abstract: β-Ga2O3, characterized with high n-type conductivity, little lattice mismatch with III-Nitrides, high transparency (>80%) in blue, and UVA (400–320 nm) as well as UVB (320–280 nm) regions, has great potential as the substrate for vertical structure blue and especially ultra violet LEDs (light emitting diodes). Large efforts have been made to improve the quality of III-Nitrides epilayers on β-Ga2O3. Furthermore, the fabrication of vertical blue LEDs has been preliminarily realized with the best result that output power reaches to 4.82 W (under a current of 10 A) and internal quantum efficiency (IQE) exceeds 78% by different groups, respectively, while there is nearly no demonstration of UV-LEDs on β-Ga2O3. -
INTERNSHIP REPORT Single Crystal Growth of Constantan by Vertical
INTERNSHIP REPORT Single Crystal Growth of Constantan by Vertical Bridgman Method Supervisor: Prof. Henrik Rønnow Laboratory for Quantum Magnetism (LQM) Rahil H. Bharani 08D11004 Third year Undergraduate Metallurgical Engineering and Materials Science IIT Bombay May – July 2011 ACKNOWLEDGEMENT I thank École Polytechnique Fédérale de Lausanne (EPFL) and Prof. Henrik Rønnow, my guide, for having me as an intern here. I have always been guided with every bit of help that I could possibly require. I express my gratitude to Prof. Daniele Mari, Iva Tkalec and Ann-Kathrin Maier for helping me out with my experimental runs and providing valuable insights on several aspects of crystal growth related to the project. I thank Julian Piatek for his help in clearing any doubts that I have had regarding quantum magnetism pertaining to understanding and testing the sample. I am indebted to Neda Nikseresht and Saba Zabihzadeh for teaching me to use the SQUID magnetometer, to Nikolay Tsyrulin for the Laue Camera and Shuang Wang at PSI for the XRF in helping me analyse my samples. I thank Prof. Enrico Giannini at the University of Geneva for helping me with further trials that were conducted there. Most importantly, I thank Caroline Pletscher for helping me with every little thing that I needed and Caroline Cherpillod, Ursina Roder and Prof Pramod Rastogi for co-ordinating the entire internship program. CONTENTS INTRODUCTION REQUIREMENTS OF THE SAMPLE SOME METHODS TO GROW SINGLE CRYSTALS • CZOCHRALSKI • BRIDGMAN • FLOATING ZONE TESTING THE SAMPLES • POLISH AND ETCH • X-RAY DIFFRACTION • LAUE METHOD • SQUID • X-RAY FLUORESCENCE THE SETUP TRIAL 1 TRIAL 2 TRIAL 3 TRIAL 4 Setup, observations, results and conclusions. -
Growth from Melt by Micro-Pulling Down (Μ-PD) and Czochralski (Cz)
Growth from melt by micro-pulling down (µ-PD) and Czochralski (Cz) techniques and characterization of LGSO and garnet scintillator crystals Valerii Kononets To cite this version: Valerii Kononets. Growth from melt by micro-pulling down (µ-PD) and Czochralski (Cz) techniques and characterization of LGSO and garnet scintillator crystals. Theoretical and/or physical chemistry. Université Claude Bernard - Lyon I, 2014. English. NNT : 2014LYO10350. tel-01166045 HAL Id: tel-01166045 https://tel.archives-ouvertes.fr/tel-01166045 Submitted on 22 Jun 2015 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. N° d’ordre Année 2014 THESE DE L‘UNIVERSITE DE LYON Délivrée par L’UNIVERSITE CLAUDE BERNARD LYON 1 ECOLE DOCTORALE Chimie DIPLOME DE DOCTORAT (Arrêté du 7 août 2006) Soutenue publiquement le 15 décembre 2014 par VALERII KONONETS Titre Croissance cristalline de cristaux scintillateurs de LGSO et de grenats à partir de l’état liquide par les techniques Czochralski (Cz) et micro-pulling down (μ-PD) et leurs caractérisations Directeur de thèse : M. Kheirreddine Lebbou Co-directeur de thèse : M. Oleg Sidletskiy JURY Mme Etiennette Auffray Hillemans Rapporteur M. Alain Braud Rapporteur M. Alexander Gektin Examinateur M. -
Study of Growth Parameters for Refractory Carbide Single Crystals
Final Report I March 7, 1964 to June 30, 1967 STUDY OF GROWTH PARAMETERS FOR REFRACTORY CARBIDE SINGLE CRYSTALS Prepared for: OFFICE OF RESEARCH GRANTS AND CONTRACTS CODE SC NATIONAL AERONAUTICS AND SPACE ADMINISTRATION WASHINGTON, D.C. 20546 CONTRACT NASr-49(19) 69: R. W. BARTLETT AE 4D F. A. HALDEN SRI Proie ct FMU-48 92 N I CT June 30, 7967 Final Report March 7, 7964 to June 30, 7967 "g_".,I ?)STUDY OF GROWTH PARAMETERS FOR REFRACTORY CARBIDE SINGLE CRYSTALS Prepared for: OFFICE OF RESEARCH GRANTS AND CONTRACTS CODE SC NA TI ONAL A ERONAUTI CS AND SP AC E ADMl N IST RAT I ON WASHINGTON, D.C. 20546 CONTRACT NASr-49(19) "I * i>L ! . W. BARTLETT AND F. A. HALDEN S R I Project FMU-4892 Approved: A. E. GORUM, ASSOCIATE EXECUTIVE DIRECTOR MA TERl AL SCIENCES LABOR ATORl ES FOREWORD The research described in this report was performed at Stanford Research Institute under Contract NASr-49(19) with the Office of Research Grants and Contracts, National Aeronautics and Space Admin- istration. Dr. H. B. Probst was the Project Monitor. The assistance of Mr. James J. Gangler is gratefully acknowledged. This report covers work conducted between 1 March 1964 and 30 June 1967. The principal investigators were F. A. Halden and R. W. Bartlett. The authors wish to acknowledge the assistance of J. W. Fowler, melt growth; W. E. Nelson, solution growth; J. B. Saunders, X-ray diffraction; H. J. Eding, vaporization and stoichi- ometry calculations; and C. W. Smith, sound velocity measurements. iii ABSTRACT The feasibility of growing single crystals of the most refractory metal carbides from their melts and from liquid metal solutions was investigated. -
Fundamental Methods of Single-Crystal Growth
Fundamental methods of single‐crystal growth RNDr. Otto Jarolímek, CSc. Single‐crystal and its growth • Single‐crystal – regular arrangement of basic building blocks (atoms, ions, molecules) is preserved on the macroscopic scale → structure anisotropy is mirrored in the physical property anisotropy • Single‐crystal growth – solid phase must be created under the physical conditions close to the thermodynamic equilibrium (stacking „atom‐by‐atom“ on the seed crystal surface) Methods of single‐crystal growth Classification by Wilke: 1) From the dispersion phase (solutions, gases,…) 2) From the own melt 3) From the solid phase Single‐crystal growth from the dispersion phase • From the gas phase – sublimation – chemical reaction (e.g. “hot wire” method) • From the (low temperature) solutions – evaporation (isothermal) – cooling (speed growth) – gradient method – chemical reaction • Hydrothermal • From the melt solutions (flux) Single‐crystal growth from the own melt • Crucible methods – stationary crucible methods – Czochralski method – Bridgman‐Stockbarger method – Stěpanov method (EFG) – zonal melting • Methods without crucible – Verneuil method – „cool crucible“ method Single‐crystal growth from the solid phase • Recrystallization – mechanical – by annealing Low temperature solutions • materials solvable at room temperature in suitable solvent (water, ethanol, aceton, …), e.g. TGS ((NH2CH2ClOH)3 ∙ H2SO4), KDP (KH2PO4), ADP (NH4H2PO4), … C Solubility curve Curve of mass crystallization Boundary of unstable range c E oversaturation 100[%] B A c dc C D solubility ratio dT T for the most materials 0 T ϵ (15°C – 60°C) Low temperature solutions Principles of methods: – AE –evaporation – AB – cooling – ABCD –gradient method C E B A C D T Evaporation • Advantages – simple isothermal method – independent from α • Drawback – difficult control of evaporaon speed → growth fluctuaon → defects and parasitic crystal occur Suitable method for the easy tentative laboratory single‐crystal growth (e.g. -
The Separation of Natural from Synthetic Colorless Sapphire
THE SEPARATION OF NATURAL FROM SYNTHETIC COLORLESS SAPPHIRE By Shane Elen and Emmanuel Fritsch Greater amounts of colorless sapphire—promot- undreds of millions of carats of colorless syn- ed primarily as diamond substitutes, but also as thetic sapphire are manufactured annually (all natural gemstones—have been seen in the gem growth techniques combined), according to B. market during the past decade. In the absence of MudryH of Djevahirdjian in Monthey, Switzerland, a leading inclusions or readily identifiable growth struc- producer of Verneuil synthetics (pers. comm., 1997). He esti- tures, natural colorless sapphires can be separat- mates that about 5%–10% of this production (50–100 mil- ed from their synthetic counterparts by their lion carats) is used by the jewelry industry. Distinguishing trace-element composition and short-wave ultraviolet (SWUV) transparency. Energy-disper- natural from synthetic colorless sapphire can often, but not sive X-ray fluorescence (EDXRF) analysis shows always, be accomplished by standard gemological testing higher concentrations of trace elements (i.e., Fe, (see below). However, this distinction is time consuming for Ti, Ca, and Ga) in natural sapphires. These large parcels, and it is difficult to impossible for melee-size impurities cause a reduction in SWUV trans- stones. parency that can be detected by UV-visible spec- As first described more than 50 years ago (Wild and trophotometry (i.e., a total absorption in the UV Biegel, 1947), natural colorless corundum can be separated region below 280–300 nm, which is not seen in from flame-fusion synthetic colorless corundum (only their synthetic counterparts). This article Verneuil material was being produced at that time) by a dif- describes a SWUV transparency tester that can ference in transparency to short-wave ultraviolet (SWUV) rapidly identify parcels of colorless sapphires. -
Temperature Gradient: a Simple Method for Single Crystal Growth
VNU Journal of Science: Mathematics – Physics, Vol. 35, No. 1 (2019) 41-46 Original Article Temperature Gradient: A Simple Method for Single Crystal Growth Duong Anh Tuan1,2,*, Nguyen Thi Thanh Huong3, Nguyen Thi Minh Hai3, Pham Anh Tuan3, Dinh Thi My Hao4, Sunglae Cho3 1Phenikaa Institute for Advanced Study, Phenikaa University, Yen Nghia, Ha Dong, Hanoi, Vietnam 2Phenikaa Research and Technology Institute, A&A Green Phoenix Group, 167 Hoang Ngan, Hanoi, Vietnam 3Department of Physics and Energy Harvest-Storage Research Center, University of Ulsan, Ulsan 680-749, Republic of Korea 4Department of Physics, Quy Nhon University, 170 An Duong Vuong, Quy Nhon, Vietnam Received 22 December 2018 Revised 21 January 2019; Accepted 25 January 2019 Abstract: In this article, we provide a simple method for the growth of bulk single crystalline. By the control temperature along a vertical furnace, we can easily fabricate bulk single crystals. This technique is called the temperature gradient method. To create a temperature gradient along the body of the furnace, the density of resistance wire which is coiled along the body of furnace is different. The density increases from the bottom to the top of the furnace. So that, at any time of the growing process, the temperature at the bottom of furnace is the smallest. During could down process, single crystal in the ampoule has been grown up from a seed at the bottom. Using this method, we successfully grew layer structure single crystals such as SnSe, SnSe2, SnS, GaTe, InSe2, GaSe. X-ray diffraction and FE-SEM measurements indicated the high quality of single crystals. -
Growth and Characterization of Titanium Doped Spinel Crystals V.T
Vol. 133 (2018) ACTA PHYSICA POLONICA A No. 4 Proceedings of the International Conference on Oxide Materials for Electronic Engineering, May 29–June 2, 2017, Lviv Growth and Characterization of Titanium Doped Spinel Crystals V.T. Gritsynaa;∗, Yu.G. Kazarinova;b, V.A. Kobyakova and L.A. Lytvynovc aV.N. Karazin Kharkiv National University, 4, Svoboda Sq., Kharkiv, 61022, Ukraine bNSC Kharkov Institute of Physics and Technology, 1, Akademicheskaya Str., Kharkiv, 61108, Ukraine cInstitute for Single Crystals of NAS of Ukraine, 60 Nauky Ave., Kharkiv, 61001, Ukraine MgAl2O4 (magnesium aluminates spinel, MAS) single crystals doped with titanium ions obtained by the Verneuil method were non-uniformly colored along of the growth crystallographic direction. The crystals were characterized measuring lattice parameter, optical absorption spectra and relative concentration of impurity atoms (Ti, Mn, Cr, and Fe) in different spots of grown Ti:MAS boule. There was observed the correlation of the intensity of absorption band at 800 nm to the relative concentration of iron supporting the identification of this band with charge transfer transition in complexes Ti4++Fe2+ ! Ti3++Fe3+. The new resonant structure at the wavelength of 470 nm was found and tentatively identified with the Fano resonance in the complexes formed by lattice defects and impurity ions. DOI: 10.12693/APhysPolA.133.774 PACS/topics: 81.10.Fq, 61.10.Nz, 42.70.Hj 1. Introduction eral peaks when was excited by 260 nm wavelength [8]. It was shown that both absorption and emission bands Magnesium aluminates spinel (MAS) MgAl2O4 pos- in blue range of wavelength are highly overlapped [9]. -
Dual-Color Double Stars in Ruby, Sapphire, and Quartz
FEATURE ARTICLES DUAL -C OLOR DOUBLE STARS IN RUBY , SAPPHIRE , AND QUARTZ : CAUSE AND HISTORICAL ACCOUNT Karl Schmetzer, Martin P. Steinbach, H. Albert Gilg, and Andrea R. Blake A largely overlooked form of asterism consisting of dual-color double stars is found in natural sapphire, in diffusion-treated and non-diffusion-treated synthetic rubies and sapphires, and in natural quartz. To characterize and explain this phenomenon, examples of these materials were examined. In transparent or translucent samples, an optical pattern of a white six-rayed star and a bodycolored (e.g., red, orange, yellow, green, blue) six-rayed star was frequently observed. Grinding and repolishing experiments showed that the asterism of part of the synthetic samples was produced or enhanced by diffusion treat - ment. The mechanism responsible for the formation of the dual-color double stars is discussed. To pro - duce the pattern, acicular inclusions must either be present in relatively thin layers confined to the dome and the base of diffusion-treated ruby or sapphire cabochons, or be distributed throughout the complete corundum (natural or synthetic) or quartz samples. The white star is caused by interaction of light with the upper layer of the cabochon’s dome. The bodycolored star, in contrast, is generated by light that enters the cabochon, is reflected and scattered at the base layer of the cabochon, and then travels a sec - ond time back through the body of the sample. As further prerequisites for observation of the phenom - enon, the gemstones must be transparent or translucent, with polished base and dome. A historical summary of the manufacture and improvement of synthetic asteriated corundum by dif - fusion treatment offers additional insight into dual-color double-star stones. -
Verneuil's Rubies Auguste Verneuil
Verneuil’s Rubies Auguste Verneuil (1856 – 1913) Where should we go for a field trip? When a colleague suggested the Minerals Gallery at the Natural History Museum it seemed a no-brainer; the range of materials and crystals would suffice to inspire the most jaded of scientists. And as we wandered through the gallery, stories billowed about chemistry and how we’ve learned about our world. With one group of students I paused by a case of synthetic crystals marvelling at a rod, opaque at one end, before narrowing down to a narrow neck and then swelling to a stunning deep red ball of ruby. “Grown by the Verneuil process”, read the label. I told my students I had no idea, and promised that I would find out. Attempts to make gems disappear into the mists of time, but only became serious in 19th century as chemical analysis gradually revealed the peculiarities of different gemstones. While diamond was shown by Smithson Tennant to be composed of pure carbon, others found that rubies and sapphires were made mostly of alumina with small amounts of metals; there also seemed to be silicon but in small, variable quantities. It was not until the 1830 that Heinrich Rose, the German codifier of qualitative inorganic analysis and reigning master analyst, proved that the silicon was a contaminant introduced when the stones were ground in an agate mortar. Thus the problem of making gems was reduced (to misrepresent the challenge) to find a way to melt and crystallise highly pure alumina. This material was available thanks to the work of Gay-Lussac who had shown that thermal decomposition of ammonium alum gave exceptionally pure aluminium oxide.