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The Chemical Activators of Cathodoluminescence in Jadeite

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The Chemical Activators of Cathodoluminescence in Jadeite The Chemical Activators of Cathodoluminescence in Jadeite Erin C. Dopfel A thesis presented to the faculty of Mount Holyoke College in partial fulfillment of the requirements for the degree of Bachelor of Arts with Honor Department of Earth and Environment Mount Holyoke College South Hadley, Massachusetts May 2006 Thesis Advisor: Dr. M. Darby Dyar Department Chair: Dr. Mark McMenamin ACKNOWLEDGMENTS I would like to thank my advisor, Darby Dyar, for her patience and guidance, and all the support she has shown toward this project over the past year. I am also grateful to Dean Connie Allen and Mark McMenamin, members of my thesis committee, for reading this document and providing me with extraordinarily helpful suggestions. And to the faculty of Mount Holyoke’s Department of Earth and Environment, especially Michelle Markley, Al Werner, and Steve Dunn, who have acted not only as mentors, but as true friends. Endless thanks to the donors of the Mount Holyoke Summer Research Fellowship, the Martha Godchaux Field Scholarship, and the Department of Earth and Environment funds, as well as Darby Dyar and the Sorena Sorensen, for supporting my travels and research expenses. Thanks to Mike Jercinovic at the University of Massachusetts – Amherst Microprobe Lab, who somehow managed to run all of my EPMA analyses on the shortest-notice-known-to-man. I am especially grateful to William F. McDonough and Richard Ash at the University of Maryland’s Isotope Geochemistry Lab, for allowing me to utilize their facilities to collect my LA ICP-MS data. Also, thanks to Gerard Marchand, Yarrow Rothstein, and Eli Sklute of Mount Holyoke College for helping to prepare and change ii samples, and fit messy Mössbauer curves. And for all their reference assistance and statistical know-how, I must thank Mount Holyoke’s library staff, especially Sarah Oelker, Mary Glackin, and Jim Burke. Special thanks must be given to Dr. Sorena S. Sorensen, of the National Museum of Natural History, for sharing with me her lab, samples, guidance, and friendship. And lastly, thank you to my friends and family, for their endless encouragement, patience, and love. iii ABSTRACT Jadeite, nominally NaAlSi2O6, has long been observed to emit green, blue, or red luminescence. The chemical origin of these phenomena is currently unclear. The goal of this study is to determine the chemical activators of cathodoluminescence (CL) in Na-rich pyroxene using chemical characterization by four analytical techniques. Seventeen samples of jadeite from Guatemala, Burma, California, Russia, and Japan were selected from the collections of the Smithsonian National Museum of Natural History (NMNH). These samples were analyzed using the electron microprobe for major elements, Mössbauer spectroscopy for Fe3+/Fe2+, ICP-MS for trace and minor elements, and CL for emission energies. The complete chemical data acquired from these techniques are used to examine the variations in jadeite chemistry as a function of paragenesis, and to link the chemistry of these minerals with their luminescent behavior. Samples were qualitatively assigned to either dull green CL, bright green CL, blue CL or red CL. Prominent peaks were identified at 442 nm, 561-579 nm, and 682 nm. The source of jadeite’s “blue band” at 442 nm has previously been hypothesized to be due to the presence of one or more unknown defect centers (Ponahlo, 1999). However, the CL analyses of tectosilicates have concluded that peaks in the 400 nm-range are correlated with the abundance of Al3+ or Eu2+. Results of this study show that the 3+ influence of Al on the intensity of this peak is especially significant. The iv “green peaks” observed between 561 – 579 nm have been assigned by previous studies of feldspars and pyroxenes to represent contributions from Mn2+ ions. This Mn2+ peak is also observed in pyroxenes and many other silicate minerals, including feldspars. Despite a general consensus that Mn2+ is the primary activator in green luminescence, this study suggests that this wide peak is, in fact, a series of smaller peaks stacked side-to-side. Results from ICP-MS analyses show that a handful of REE’s, including Dy and Tm, are also correlated with the intensities in the energy range of 570-590 nm. The intensity of the red peak at 682 nm is well-correlated with the presence of Al3+, Ti2+, Ca2+, and Eu3+, as suggested by previous work. Mössbauer data acquired as part of this study allow us to constrain separately the influence of Fe2+ and Fe3+ on both the intensities of luminescence and the activation of red emission energies. While this research brings light to the possible luminescence activators in jadeite, it is evident that the uncertainties in these studies require further research in order to bring more quantitative insights to the origin of such luminescence phenomena. v TABLE OF CONTENTS ACKNOWLEDGMENTS ................................................................................ ii ABSTRACT..................................................................................................... iv TABLE OF CONTENTS................................................................................. vi LIST OF FIGURES ........................................................................................ vii LIST OF TABLES.........................................................................................viii INTRODUCTION ............................................................................................ 1 BACKGROUND .............................................................................................. 3 GEOLOGY OF JADEITE .............................................................................. 18 MINERALOGY OF JADEITE....................................................................... 20 METHODS ..................................................................................................... 22 RESULTS ....................................................................................................... 29 Cathodoluminescence Petrography ............................................................. 29 Peak Identification: Summer 2005........................................................... 29 SEM CL – Summer 2005......................................................................... 32 Grain Mount CL: Spring 2006 ................................................................. 34 Electron Microprobe Analysis..................................................................... 36 LA ICP-MS Analysis................................................................................... 40 Mössbauer Spectroscopy ............................................................................. 42 DISCUSSION................................................................................................. 44 Intensity Discrepancies................................................................................ 44 Contributions to Activation and Quenching of Jadeite CL ......................... 46 Blue Peak.................................................................................................. 49 Green Peak ............................................................................................... 50 Red Peak................................................................................................... 53 Future Work................................................................................................. 56 CONCLUSION............................................................................................... 57 REFERENCES ............................................................................................... 58 vi LIST OF FIGURES Figure 1 Qualitative picture of the interaction of an electron beam with a solid.. .................... 5 Figure 2 Cross-section of luminoscope. (From Herzog et al. [1970])........................................6 Figure 3 The basic process of luminescence...............................................................................7 Figure 4 The relationship between color of emitted light (a) and the wavelength.....................8 Figure 5 Quantum model of a sodium atom.............................................................................. 9 Figure 6 Energy diagram for free molecule made up of two atoms of the same species..........11 Figure 7 Crystal structure of jadeite........................................................................................ 21 Figure 8 Calculation of relative peak intensities..................................................................... 26 Figure 9 Example of oscillatory zoning in Guatemalan jadeitite sample 108369................... 29 Figure 10 Multiple crystallization sequences illuminated by CL............................................ 30 Figure 11 Examples of different luminescence in jadeite (green CL)..................................... 31 Figure 11 (cont.) Examples of different luminescence in jadeite (red and blue CL) .............. 31 Figure 12 SEM CL and macroscopic CL, with corresponding and spectra. ........................... 33 Figure 13 SEM CL spectrum vs. CL spectrum along same scale.............................................34 Figure 14 Example of laser ablation damage on grain mount..................................................35 Figure 15 Average MnO weight % by CL type. ..................................................................... 39 Figure 16 Average Cr2O3 weight % by CL type.................................................................... 39 Figure 17 Average
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