growth of large single crystals by floating zone technique · branches of research as they present...

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Abstract Growth of Large Single Crystals by Floating Zone Technique Charis Cochran 1,3 , Jennifer Neu 2,3 , Kaya Wei 3 , Theo Siegrist 2,3 1 Trevecca Nazarene University, 2 Florida State University, 3 National High Magnetic Field Laboratory I would like to give a special thanks to the MagLab REU program for allowing me to participate in this research and to Dr. Theo Siegrist and Jennifer Neu for the guidance throughout the summer. This REU was funded by the National Science Foundation under grant DMR 1644779. This work was performed at the MagLab which is funded by the National Science Foundation under DMR-1644779. JN and TS acknowledge funding under NSF DMR 1606952. Chromium 3+ Titanium 4+ and Iron 3+ Chromium 3+ and Nickel 2+ Introduction Acknowledgement Floating Zone Synthesis Results Data and Analysis Conclusions and Future Work References Iron 3+ Color Chance Sapphire: Al 2 O 3 Ho 2 Ti 2 O 7 SrCu 2 (BO 3 ) 2 Single Crystal Diffraction Pattern of Orange Sapphire Ho 2 Ti 2 O 7 Powder Diffraction Pattern SrCu 2 (BO 3 ) 2 Powder Diffraction Pattern Al 2 O 3 Ho 2 Ti 2 O 7 SrCu 2 (BO 3 ) 2 Single crystal Sapphire, a form of Alumina (!-Al 2 O 3 ), Ho 2 Ti 2 O 7 , and SrCu 2 (BO 3 ) 2 , were grown using the Optical Floating Zone Technique in the Image Furnace. Two polycrystalline rods of each of these materials were used as preforms for the Image Furnace growths. The grown Sapphire crystals had very large single crystalline, optically active sections, and the grown Ho 2 Ti 2 O 7 crystal was almost entirely single crystalline. Structure and properties Applications Materials in which the physical geometry inhibits simultaneous satisfaction of local competing spin interactions are said to be frustrated. This inability to satisfy these interactions leads to degenerate ground states in the crystal system since multiple configurations can have the same energy. These materials have been of significant interest in recent years for their unique physical properties. Ho 2 Ti 2 O 7 is a frustrated system that crystalizes in the space group Fd3m, and SrCu 2 (BO 3 ) 2 is a frustrated system that crystalizes in the space group D4h. Sapphire is a hexagonal crystal system and crystalizes in the space group R3c. Sapphires are of interest to many branches of research as they present a unique combination of optical and electrical properties and applications. Most of these applications require large, high quality single crystal sapphire. Though commonly recognized as the blue gemstone, sapphire can take many colors. Transition metal dopants in the pure Aluminum Oxide crystal replace some of the aluminum, producing localized d-electrons. These localized electrons in their ground state can be excited by white light which causes the sapphire to appear a different color. Sapphire possesses unique optical properties and is a good lasing medium. It is also highly insulating, and is a good dielectric and substrate material. Sapphire is among the hardest crystals with a Mohs scale hardness of 9 just below diamond at 10. Ho 2 Ti 2 O 7 and SrCu 2 (BO 3 ) 2 are of significant interest in research due to their unique properties for different applications. The single crystals grown here are for use as substrates for thin film growth and research. Baroudi, Kristen. Princeton University, ProQuest Dissertations Publishing, 2015. 3712079. Xu, Hong, et al. “Growth and Characterization of Fe:Ti:Al2O3 Single Crystal by Floating Zone Method.” Journal of Crystal Growth, vol. 372, 2013, pp. 82–86., doi: 10.1016/j.jcrysgro.2013.02.024. Kageyama, H, et al. “Crystal Growth of the Two-Dimensional Spin Gap System SrCu2(BO3)2.” Journal of Crystal Growth, vol. 206, no. 1-2, 1999, pp. 65–67., doi: 10.1016/s0022-0248(99)00313-9. Victor G. Thomas, et al. “TAIRUS HYDROTHERMAL SYNTHETIC SAPPHIRES DOPED WITH NICKEL AND CHROMIUM”. Gem and Gemology. 1997. Print. The Image Furnace is a system of elliptical mirrors and energized filaments (High Wattage Lamps). The mirrors focus the energy into what is called the hot zone. Below the hot zone a polycrystalline rod (sometimes with a seed crystal in a desired orientation or a flux to help growth) is attached to the seed rod. A polycrystalline rod is attached to the top feed rod with a wire that has a high melting point. As the two rods come into the hot zone the ends of the rods melt and are then brought together so that they are connected by a molten zone. The rods are then pulled down through the hot zone, propagating the molten area through the feed rod. As each section of the rod moves out of the hot zone it recrystallizes into a single crystal. . Intensity Spectra of Rightmost Line of Single Crystal Pattern Single Crystal Ho 2 Ti 2 O 7 Oriented with Crystallographic Direction [111] to be Up Large optically active single crystalline sections of Sapphire were obtained using the floating zone technique. A large single crystalline sample of Ho 2 Ti 2 O 7 suitable for use as a substrate for thin film growth was grown and oriented to a specific crystallographic direction desired for the growth. Future research will include work with the SrCu 2 (BO 3 ) 2 growth as the preparation and floating zone melt of this material is highly unstable and makes single crystal growth difficult. We will also expand the research to include further systems such as MgAl 2 O 4 spinel, and Tb 2 Ti 2 O 7 . O Al Ho Ti O Sr Cu B O

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Page 1: Growth of Large Single Crystals by Floating Zone Technique · branches of research as they present a unique combination of optical and electrical properties and applications. Most

Abstract

Growth of Large Single Crystals by Floating Zone Technique Charis Cochran1,3, Jennifer Neu2,3, Kaya Wei3, Theo Siegrist2,3 1Trevecca Nazarene University, 2Florida State University, 3National High Magnetic Field Laboratory

I would like to give a special thanks to the MagLab REU program for allowing me to participate in this research and to Dr. Theo Siegrist and Jennifer Neu for the guidance throughout the summer. This REU was funded by the National Science Foundation under grant DMR 1644779. This work was performed at the MagLab which is funded by the National Science Foundation under DMR-1644779. JN and TS acknowledge funding under NSF DMR 1606952.

Chromium 3+ Titanium 4+ and Iron 3+

Chromium 3+ and Nickel 2+

Introduction

Floating Zone Synthesis

Acknowledgement

Floating Zone Synthesis

Results

Data and Analysis

Conclusions and Future Work

References Iron 3+

Color Chance

Sapphire: Al2O3

Ho2Ti2O7

SrCu2(BO3)2

Single Crystal Diffraction Pattern of Orange Sapphire

Ho2Ti2O7 Powder Diffraction Pattern

SrCu2(BO3)2 Powder Diffraction Pattern

Al2O3

Ho2Ti2O7

SrCu2(BO3)2

Single crystal Sapphire, a form of Alumina (!-Al2O3), Ho2Ti2O7, and SrCu2(BO3)2, were grown using the Optical Floating Zone Technique in the Image Furnace. Two polycrystalline rods of each of these materials were used as preforms for the Image Furnace growths. The grown Sapphire crystals had very large single crystalline, optically active sections, and the grown Ho2Ti2O7 crystal was almost entirely single crystalline.

Structure and properties

Applications

Materials in which the physical geometry inhibits simultaneous satisfaction of local competing spin interactions are said to be frustrated. This inability to satisfy these interactions leads to degenerate ground states in the crystal system since multiple configurations can have the same energy. These materials have been of significant interest in recent years for their unique physical properties. Ho2Ti2O7 is a frustrated system that crystalizes in the space group Fd3m, and SrCu2(BO3)2 is a frustrated system that crystalizes in the space group D4h. Sapphire is a hexagonal crystal system and crystalizes in the space group R3c. Sapphires are of interest to many branches of research as they present a unique combination of optical and electrical properties and applications. Most of these applications require large, high quality single crystal sapphire. Though commonly recognized as the blue gemstone, sapphire can take many colors. Transition metal dopants in the pure Aluminum Oxide crystal replace some of the aluminum, producing localized d-electrons. These localized electrons in their ground state can be excited by white light which causes the sapphire to appear a different color.

Sapphire possesses unique optical properties and is a good lasing medium. It is also highly insulating, and is a good dielectric and substrate material. Sapphire is among the hardest crystals with a Mohs scale hardness of 9 just below diamond at 10. Ho2Ti2O7 and SrCu2(BO3)2 are of significant interest in research due to their unique properties for different applications. The single crystals grown here are for use as substrates for thin film growth and research.

Baroudi, Kristen. Princeton University, ProQuest Dissertations Publishing, 2015. 3712079. Xu, Hong, et al. “Growth and Characterization of Fe:Ti:Al2O3 Single Crystal by Floating Zone Method.” Journal of Crystal Growth, vol. 372, 2013, pp. 82–86., doi:10.1016/j.jcrysgro.2013.02.024. Kageyama, H, et al. “Crystal Growth of the Two-Dimensional Spin Gap System SrCu2(BO3)2.” Journal of Crystal Growth, vol. 206, no. 1-2, 1999, pp. 65–67., doi:10.1016/s0022-0248(99)00313-9. Victor G. Thomas, et al. “TAIRUS HYDROTHERMAL SYNTHETIC SAPPHIRES DOPED WITH NICKEL AND CHROMIUM”. Gem and Gemology. 1997. Print.

The Image Furnace is a system of elliptical mirrors and energized filaments (High Wattage Lamps). The mirrors focus the energy into what is called the hot zone. Below the hot zone a polycrystalline rod (sometimes with a seed crystal in a desired orientation or a flux to help growth) is attached to the seed rod. A polycrystalline rod is attached to the top feed rod with a wire that has a high melting point. As the two rods come into the hot zone the ends of the rods melt and are then brought together so that they are connected by a molten zone. The rods are then pulled down through the hot zone, propagating the molten area through the feed rod. As each section of the rod moves out of the hot zone it recrystallizes into a single crystal. .

Intensity Spectra of Rightmost Line of Single Crystal Pattern

Single Crystal Ho2Ti2O7 Oriented with Crystallographic Direction

[111] to be Up

Large optically active single crystalline sections of Sapphire were obtained using the floating zone technique. A large single crystalline sample of Ho2Ti2O7 suitable for use as a substrate for thin film growth was grown and oriented to a specific crystallographic direction desired for the growth. Future research will include work with the SrCu2(BO3)2 growth as the preparation and floating zone melt of this material is highly unstable and makes single crystal growth difficult. We will also expand the research to include further systems such as MgAl2O4 spinel, and Tb2Ti2O7 .

Growth of Large Single Crystals by Floating Zone Technique

O

Al

Ho

Ti

O

Sr

Cu

B

O