Method for solid state crystal growth
Abstract
A novel method for high quality crystal growth of intermetallic clathrates is presented. The synthesis of high quality pure phase crystals has been complicated by the simultaneous formation of both clathrate type-I and clathrate type-II structures. It was found that selective, phase pure, single-crystal growth of type-I and type-II clathrates can be achieved by maintaining sufficient partial pressure of a chemical constituent during slow, controlled deprivation of the chemical constituent from the primary reactant. The chemical constituent is slowly removed from the primary reactant by the reaction of the chemical constituent vapor with a secondary reactant, spatially separated from the primary reactant, in a closed volume under uniaxial pressure and heat to form the single phase pure crystals.
- Inventors:
- Issue Date:
- Research Org.:
- DOESC (USDOE Office of Science (SC) (United States))
- Sponsoring Org.:
- USDOE
- OSTI Identifier:
- 1083808
- Patent Number(s):
- 8414858
- Application Number:
- 12/859,534
- Assignee:
- University of South Florida (Tampa, FL)
- Patent Classifications (CPCs):
-
C - CHEMISTRY C01 - INORGANIC CHEMISTRY C01B - NON-METALLIC ELEMENTS
C - CHEMISTRY C01 - INORGANIC CHEMISTRY C01P - INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- DOE Contract Number:
- FG02-04ER46145
- Resource Type:
- Patent
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE
Citation Formats
Nolas, George S., and Beekman, Matthew K. Method for solid state crystal growth. United States: N. p., 2013.
Web.
Nolas, George S., & Beekman, Matthew K. Method for solid state crystal growth. United States.
Nolas, George S., and Beekman, Matthew K. Tue .
"Method for solid state crystal growth". United States. https://www.osti.gov/servlets/purl/1083808.
@article{osti_1083808,
title = {Method for solid state crystal growth},
author = {Nolas, George S. and Beekman, Matthew K.},
abstractNote = {A novel method for high quality crystal growth of intermetallic clathrates is presented. The synthesis of high quality pure phase crystals has been complicated by the simultaneous formation of both clathrate type-I and clathrate type-II structures. It was found that selective, phase pure, single-crystal growth of type-I and type-II clathrates can be achieved by maintaining sufficient partial pressure of a chemical constituent during slow, controlled deprivation of the chemical constituent from the primary reactant. The chemical constituent is slowly removed from the primary reactant by the reaction of the chemical constituent vapor with a secondary reactant, spatially separated from the primary reactant, in a closed volume under uniaxial pressure and heat to form the single phase pure crystals.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Tue Apr 09 00:00:00 EDT 2013},
month = {Tue Apr 09 00:00:00 EDT 2013}
}
Works referenced in this record:
Sur une nouvelle famille de clathrates minéraux isotypes des hydrates de gaz et de liquides. Interprétation des résultats obtenus
journal, December 1970
- Cros, Christian; Pouchard, Michel; Hagenmuller, Paul
- Journal of Solid State Chemistry, Vol. 2, Issue 4
Intrinsic Electrical and Thermal Properties from Single Crystals of
journal, January 2010
- Beekman, M.; Schnelle, W.; Borrmann, H.
- Physical Review Letters, Vol. 104, Issue 1
High-pressure properties of group IV clathrates
journal, September 2005
- San-Miguel, Alfonso; Toulemonde, Pierre
- High Pressure Research, Vol. 25, Issue 3
Superconductivity in the Silicon Clathrate Compound (Na,Ba) S
journal, February 1995
- Kawaji, Hitoshi; Horie, Hiro-omi; Yamanaka, Shoji
- Physical Review Letters, Vol. 74, Issue 8
Direct Experimental Evidence for Atomic Tunneling of Europium in Crystalline
journal, July 2006
- Hermann, Raphaël P.; Keppens, Veerle; Bonville, Pierre
- Physical Review Letters, Vol. 97, Issue 1
A guest-free germanium clathrate
journal, September 2006
- Guloy, Arnold M.; Ramlau, Reiner; Tang, Zhongjia
- Nature, Vol. 443, Issue 7109
Clathrate compounds and manufacturing method thereof
patent, October 2002
- Eguchi, Haruki; Suzuki, Akihiko; Takahashi, Satoshi
- US Patent Document 6,461,581
Semiconducting Ge clathrates: Promising candidates for thermoelectric applications
journal, July 1998
- Nolas, G. S.; Cohn, J. L.; Slack, G. A.
- Applied Physics Letters, Vol. 73, Issue 2
A 4 Ge 9 (A = K, Rb) as Precursors for Hg-Substituted Clathrate-I Synthesis: Crystal Structure of A 8 Hg 3 Ge 43
journal, October 2008
- Kaltzoglou, Andreas; Ponou, Siméon; Fässler, Thomas F.
- European Journal of Inorganic Chemistry, Vol. 2008, Issue 29
Structural Principles and Amorphouslike Thermal Conductivity of Na-Doped Si Clathrates
journal, July 2000
- Tse, J. S.; Uehara, K.; Rousseau, R.
- Physical Review Letters, Vol. 85, Issue 1
Structural characterisations of the NaxSi136 and Na8Si46 silicon clathrates using the Rietveld method
journal, January 1998
- Reny, Edouard; Gravereau, Pierre; Cros, Christian
- Journal of Materials Chemistry, Vol. 8, Issue 12
Na–Si binary phase diagram and solution growth of silicon crystals
journal, July 2009
- Morito, H.; Yamada, T.; Ikeda, T.
- Journal of Alloys and Compounds, Vol. 480, Issue 2
Double-Helical Silicon Microtubes
journal, April 2010
- Morito, Haruhiko; Yamane, Hisanori
- Angewandte Chemie International Edition, Vol. 49, Issue 21
Synthesis and X-Ray Characterization of Silicon Clathrates
journal, July 1999
- Ramachandran, Ganesh K.; Dong, Jianjun; Diefenbacher, Jason
- Journal of Solid State Chemistry, Vol. 145, Issue 2
Inorganic clathrate-II materials of group 14: synthetic routes and physical properties
journal, January 2008
- Beekman, M.; Nolas, G. S.
- J. Mater. Chem., Vol. 18, Issue 8
Clathrate compounds and method of manufacturing
patent, May 2009
- Nolas, George S.; Witanachchi, Sarath; Mukherjee, Pritish
- US Patent Document 7,534,414
Hydrogen Encapsulation in a Silicon Clathrate Type I Structure: Na 5.5 (H 2 ) 2.15 Si 46 : Synthesis and Characterization
journal, November 2007
- Neiner, Doinita; Okamoto, Norihiko L.; Condron, Cathie L.
- Journal of the American Chemical Society, Vol. 129, Issue 45
Clathrate Structure of Silicon Na8Si46 and NaxSi136 (x < 11)
journal, December 1965
- Kasper, J. S.; Hagenmuller, P.; Pouchard, M.
- Science, Vol. 150, Issue 3704
Structure and Thermoelectric Characterization of Ba 8 Al 14 Si 31
journal, November 2006
- Condron, Cathie L.; Martin, J.; Nolas, G. S.
- Inorganic Chemistry, Vol. 45, Issue 23
Avoided crossing of rattler modes in thermoelectric materials
journal, August 2008
- Christensen, Mogens; Abrahamsen, Asger B.; Christensen, Niels B.
- Nature Materials, Vol. 7, Issue 10
Peierls or Jahn-Teller effect in endohedrally doped silicon clathrates: An EXAFS study
journal, June 2000
- Brunet, F.; Mélinon, P.; San Miguel, A.
- Physical Review B, Vol. 61, Issue 24
Clathrate compounds, manufacture thereof, and thermoelectric materials, thermoelectric modules, semiconductor materials and hard materials based thereon
patent, September 2004
- Eguchi, Haruki; Suzuki, Akihiko; Takahashi, Satoshi
- US Patent Document 6,797,199
Thermoelectric materials fabricated from clathrate compounds and other materials which form an inclusion complex and method for optimizing selected thermoelectric properties
patent, February 2001
- Nolas, George S.; Slack, Glen A.
- US Patent Document 6,188,011
On the Design of High-Efficiency Thermoelectric Clathrates through a Systematic Cross-Substitution of Framework Elements
journal, March 2010
- Shi, Xun; Yang, Jiong; Bai, Shengqiang
- Advanced Functional Materials, Vol. 20, Issue 5
Oxidation of M 4 Si 4 (M = Na, K) to Clathrates by HCl or H 2 O
journal, May 2007
- Böhme, Bodo; Guloy, Arnold; Tang, Zhongjia
- Journal of the American Chemical Society, Vol. 129, Issue 17
Interplay between thermoelectric and structural properties of type-I clathrate single crystals
journal, April 2010
- Tanaka, T.; Onimaru, T.; Suekuni, K.
- Physical Review B, Vol. 81, Issue 16
Preparation and Crystal Growth of Na 24 Si 136
journal, July 2009
- Beekman, Matt; Baitinger, Michael; Borrmann, Horst
- Journal of the American Chemical Society, Vol. 131, Issue 28
Cs8− x Si 46 : A Type-I Clathrate with Expanded Silicon Framework
journal, June 2009
- Wosylus, Aron; Veremchuk, Igor; Schnelle, Walter
- Chemistry - A European Journal, Vol. 15, Issue 24
Structural, magnetic, thermal, and transport properties of single crystals
journal, June 2001
- Sales, B. C.; Chakoumakos, B. C.; Jin, R.
- Physical Review B, Vol. 63, Issue 24
Controlled thermal decomposition of NaSi to derive silicon clathrate compounds
journal, January 2009
- Horie, Hiro-omi; Kikudome, Takashi; Teramura, Kyosuke
- Journal of Solid State Chemistry, Vol. 182, Issue 1
Clathrate structure for electronic and electro-optic applications
patent, August 2000
- Grigorian, Leonid; Eklund, Peter C.; Fang, Shaoli
- US Patent Document 6,103,403
Glasslike Heat Conduction in High-Mobility Crystalline Semiconductors
journal, January 1999
- Cohn, J. L.; Nolas, G. S.; Fessatidis, V.
- Physical Review Letters, Vol. 82, Issue 4
