Single crystal of nitride containing metal element of group...

Single-crystal – oriented-crystal – and epitaxy growth processes; – Processes of growth from liquid or supercritical state – Havin growth from molten state

Reexamination Certificate

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C117S075000, C117S071000, C117S079000, C117S952000, C117S940000

Reexamination Certificate

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07115165

ABSTRACT:
β-ZrNCl polycrystalline powder prepared by chemical transport method and NH4Cl are mixed in a molar ratio of 1:2. The mixture is encapsulated in a Au capsule (6 mm in inner diameter and 6 mm in depth) of a reaction vessel2, which is then enclosed in a highly heat-conductivitive sodium chloride block as an electrically insulating pressure medium6. The mixture held in the sodium chloride block is placed in a carbon tube8for serving as a heater. In a cubic-pressing apparatus using a pyrophyllite12as a pressure-transmitting medium, the mixture is heated at 900° C. for 2 hours under an applied pressure of 3 GPa. After the mixture is allowed to stand until it is cooled down to room temperature, the Au capsule is taken out and light green β-ZrNCl single crystals are obtained. A large single crystal among them had a hexagonal plate-like habit and is transparent with dimensions about 2 mm in diameter, and 0.3 mm in thickness.

REFERENCES:
patent: 2001-72499 (2001-03-01), None
Vlassov et al., “Chemical Transport Synthesis, Electrochemical Behavior and Electroic Structure of Superconducting Zirconium and Hafnium Nitride Halides”, Inorganic Chemistry, 1999, vol. 38 pp. 4530-4538.
Fogg et al., “Crystal Structure of MNX ( M=Zr, Hf; X=Cl, Br)” Chemical Communications 1998 pp. 2269-2270.
Shoji Yamanaka et al.; Inorganic Chemistry, vol. 39, No. 4, pp. 806-809. Feb. 21, 2000. Cited in the int'l. search report.
T. Ishii et al.; Journal of Crystal Growth, vol. 61, No. 3, pp. 689-690, Apr./May 1983. Cited in the int'l. search report.
Mr. Ohashi et al., Journal of Solid State Chemistry 77, 342-347 (1988), “Chemical Vapor Transport of Layer Structured Crystal β-ZrNCI”.
Mr. Ohashi et al., Journal of Solid State Chemistry 75, 99-104 (1988), “Novel Synthesis of the Layer Structured β-ZrNCI by the Direct Reactions of Zirconium Metal or Zirconium Hydride with Ammonium Chloride.”

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