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“Internal Characteristics, Chemical Compounds and Spectroscopy of Sapphire As Single Crystals”

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“Internal Characteristics, Chemical Compounds and Spectroscopy of Sapphire As Single Crystals” “Internal characteristics, chemical compounds and spectroscopy of sapphire as single crystals” Dissertation zur Erlangung des Grades „Doktor der Naturwissenschaften“ im Promotionsfach Mineralogie am Fachbereich Chemie, Pharmazie und Geowissenschaften der Johannes Gutenberg-Universität Mainz Phan Thi Minh Diep geb. in Dongnai, Vietnam Mainz 2015 Dekan: Univ.-Prof. Dr. Dirk Schneider 1. Berichterstatter: Prof. Dr. rer. nat. habil. Wolfgang Hofmeister 2. Berichterstatter: Dr. Häger Tobias Tag der mündlichen Prüfung: 17.07.2015 ERKLÄRUNG Hiermit bestätige ich, dass ich diese Arbeit selbständig verfasst und keine anderen als die angegebenen Quellen und Hilfsmittel verwendet habe. Mainz, May 2015 Phan Thi Minh Diep For my Family and my Love Table of contents Abstract ......................................................................................................................................1 Zusammenfassung......................................................................................................................4 Figures and Tables .....................................................................................................................7 Chapter 1: Introduction ...........................................................................................................14 1.1. Objective of the thesis ........................................................................................14 1.2. Corundum in general ..........................................................................................14 1.2.1. The corundum structure .........................................................................14 1.2.2. Properties of corundum ..........................................................................17 Chapter 2: Research Materials and Methods ...........................................................................20 2.1. Research materials ..............................................................................................20 2.1.1. Sapphire from Vietnam ..........................................................................20 2.1.2. Sapphire from Ban Huay Sai in Bokeo, Laos ........................................24 2.1.3. Sapphire from Khao Ploi Waen in Chanthaburi and Bo Ploi in Kanchanaburi, Thailand ..........................................................................25 2.1.4. Sapphire from Australia .........................................................................25 2.1.5. Sapphire from Changle in Shandong, China ..........................................26 2.1.6. Sapphire from Andapa, Antsirabe and Nosibe, Madagascar .................27 2.1.7. Sapphire from Ballapana, Sri Lanka ......................................................27 2.1.8. Sapphire from Brazil ..............................................................................28 2.1.9. Sapphire from Russia .............................................................................28 2.1.10. Sapphire from Colombia ......................................................................29 2.1.11. Sapphire from Tansania .......................................................................30 2.1.12. Sapphire from Malawi ..........................................................................30 2.2. Experimental methods ........................................................................................31 2.2.1. Gemological microscope ........................................................................31 2.2.2. Confocal micro Raman and luminescence spectroscopy .......................31 2.2.3. FTIR absorption spectroscopy ...............................................................32 i 2.2.4. UV-Vis-NIR absorption spectroscopy ...................................................32 2.2.5. Electron Probe Micro-Analysis (EPMA) ...............................................33 2.2.6. Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA- ICP-MS) ..................................................................................................34 Chapter 3: Internal Characteristics of Sapphire .......................................................................35 3.1. Trapiche patterns ................................................................................................35 3.2. Color zoning .......................................................................................................37 3.3. Twinning .............................................................................................................38 3.4. Healed fissures ....................................................................................................39 3.5. Fluid inclusions ...................................................................................................40 3.6. Iron oxide inclusions ...........................................................................................43 3.7. Needle or whitish tubes ......................................................................................47 3.8. Boehmite, diaspore, kaolinite and OH-groups ...................................................48 3.9. Spinel inclusion ..................................................................................................50 3.10. Feldspar inclusions ...........................................................................................51 3.11. Zircon inclusions ..............................................................................................53 3.12. Mica inclusions .................................................................................................57 3.13. Cordierite inclusion ..........................................................................................57 3.14. Tantalite inclusions ...........................................................................................58 Chapter 4: Chemical Compounds of Sapphire.........................................................................64 4.1. Chemistry of sapphire by EPMA ........................................................................64 4.2. The ratio of Cr2O3/Ga2O3 and Fe2O3 ..................................................................71 4.3. Chemical analyses by LA-ICP-MS ....................................................................73 Chapter 5: Raman Spectroscopy of Sapphire and the Influence of the Fe2O3 Content on the Spectra......................................................................................................................................79 5.1. Overview on Raman spectroscopy of corundum ................................................79 5.2. Relationship between Raman spectra and the Fe2O3 content of sapphire ..........84 Chapter 6: Luminescence Spectroscopy of Sapphire and the Influence of Fe2O3 Content .....92 6.1. Luminescence spectroscopy of corundum in general .........................................92 6.2. Effect of Fe2O3 content on the R-line position of sapphires ...............................94 ii Chapter 7: FTIR Spectroscopy of Sapphire and the Influence of Fe2O3 Content on the Spectra....................................................................................................................................100 7.1. FTIR spectroscopy of sapphire .........................................................................100 7.2. OH bond angles in sapphire ..............................................................................107 -1 7.3. The correlation of 3310 cm peak and the Fe2O3 contents of sapphires ..........109 Chapter 8: UV-Vis-NIR Spectroscopy of Sapphire ...............................................................112 8.1. Group 1: The blue, green or bluish green sapphire ..........................................113 8.2. Group 2: The light pink sapphire ......................................................................115 8.3. Group 3: The brown to grey, or nearly colorless sapphire ...............................116 Chapter 9: Conclusions ..........................................................................................................118 Bibliography ..........................................................................................................................120 Programs ................................................................................................................................132 Acknowledgements ................................................................................................................133 List of publication ..................................................................................................................135 Curriculum Vitae ...................................................................................................................135 iii Internal features, chemical compounds and spectroscopy of sapphire as single crystal Abstract In this study more than 450 natural sapphire samples (most of basaltic type) collected from 19 different areas were examined. They are from Dak Nong, Dak Lak, Quy Chau, two unknown sources from the north (Vietnam); Bo Ploi, Khao Ploi Waen (Thailand); Ban Huay Sai (Laos); Australia; Shandong (China); Andapa, Antsirabe, Nosibe (Madagascar); Ballapana (Sri Lanka); Brazil; Russia; Colombia; Tansania and Malawi. The samples were studied on internal characteristics, chemical compositions, Raman-, luminescence-, Fourier transform infrared (FTIR)-, and ultraviolet-visible-near infrared (UV- Vis-NIR)- spectroscopy. The internal features of these sapphire samples were observed and identified
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