Melt stabilization and vapor-phase synthesis of cesium germanium halides

Patent metadata

Field	Value
Publication number	US-8945418-B2
Application number	US-201213675890-A
Country	US
Kind code	B2
Filing date	Nov 13, 2012
Priority date	Nov 16, 2011
Publication date	Feb 3, 2015
Grant date	Feb 3, 2015

Abstract

The method described herein allows for melt stabilization and vapor-phase synthesis of a cesium germanium halide utilizing germanium dihalides formed in situ. This disclosure allows for the melting of cesium germanium halides without decomposition, which allows for growing crystals of these materials from the melt. This disclosure allows for a direct synthesis of these materials without the use of water or the introduction of other possible contaminants.

First claim

What we claim is:

1. A method of vapor-phase synthesis of a cesium germanium halide, comprising:
utilizing germanium dihalides as cover gases;
reacting Ge(0) with GeX 4 vapor and producing germanium dihalide vapor in situ; and
reacting the germanium dihalide vapor with CsX; and
producing CsGeX 3 .

2. The method of vapor-phase synthesis of a cesium germanium halide of claim 1 wherein the reaction is not exposed to water.

3. The method of vapor-phase synthesis of a cesium germanium halide of claim 2 further including:
decomposing CsGeX 3 to reactants including CsX from decomposition;
reacting the CsX from decomposition with GeX 2 vapor formed in situ; and
forming CsGeX 3 in situ.

4. A method of vapor-phase synthesis of a cesium germanium halide comprising:
loading a charge of CGC into a first tube;
loading a charge of Ge(0) into a second tube;
loading the first tube and the second tube into a vessel;
capping the vessel with a plug and thereby sealing;
fitting a transfer tube into the plug;
placing the vessel with the first tube and the second tube into a furnace;
evacuating and removing the room air and any water;
injecting GeCl 4 into the vessel;
boiling the GeCl 4 ;
filling the vessel to its vapor pressure;
increasing the temperature of the furnace to about 360 degrees C.;
melting the CGC;
reacting the GeCl 4 with the Ge(0) and generating GeCl 2 gas; and
reacting the GeCl 2 gas with CsX and producing CsGeX 3 .

5. The method of vapor-phase synthesis of a cesium germanium halide of claim 4
wherein the charge of CGC is about 10 g; and
wherein the charge of Ge(0) is about 1 g.

6. The method of vapor-phase synthesis of a cesium germanium halide of claim 5 wherein the GeCl 4 is about 5 g.

7. The method of vapor-phase synthesis of a cesium germanium halide of claim 6 wherein the GeCl 4 vapor pressure is about 200 torr at 293K.

8. A method of vapor-phase synthesis of a cesium germanium halide comprising:
loading a charge of CsCl beads into a first tube with an opening;
placing a third tube near the opening for collecting the product;
loading a charge of Ge(0) into a second tube;
loading the first tube and the second tube into a vessel;
capping the vessel with a plug and thereby sealing;
placing the vessel with the first tube and the second tube into a furnace;
evacuating and removing the room air and any water;
injecting GeCl 4 into the vessel;
boiling the GeCl 4 ;
filling the vessel to its vapor pressure;
increasing the temperature of the furnace to about 360 degrees C.;
reacting the GeCl 4 with the Ge(0) and generating GeCl 2 gas;
reacting the GeCl 2 gas with CsCl beads; and
producing CsGeX 3 .

9. The method of vapor-phase synthesis of a cesium germanium halide of claim 8 wherein the cesium chloride beads have a particle size of about −30 mesh.

10. The method of vapor-phase synthesis of a cesium germanium halide of claim 9 wherein the charge of Ge(0) is about 1 g;
wherein the GeCl 4 is about 5 g; and
wherein the GeCl 4 vapor pressure is about 200 torr at 293K.

11. The method of vapor-phase synthesis of a cesium germanium halide of claim 9 wherein the reaction is not exposed to water.

12. A cesium germanium halide that is formed in situ by vapor-phase synthesis and is composed of 85% CGC and 15% CsCl.

13. The cesium germanium halide of claim 12 that is formed in situ by vapor-phase synthesis and wherein the cesium germanium halide does not contain water or other contaminants.

Assignees

• Condon Nicholas J
• Bowman Steven R
• O'Connor Shawn P
• Us Navy

Inventors

• Condon Nicholas J
• Bowman Steven R
• O'Connor Shawn P

Classifications

• C09K11/665 Primary

  with alkali or alkaline earth metals · CPC title

• C01G17/00

  Compounds of germanium · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2002/82

  by IR- or Raman-data · CPC title

• C30B11/02

  without using solvents (C30B11/06 takes precedence) · CPC title