Method for purifying a thallium compound using a carbon powder

Patent metadata

Field	Value
Publication number	US-11725303-B2
Application number	US-202117341899-A
Country	US
Kind code	B2
Filing date	Jun 8, 2021
Priority date	Aug 26, 2016
Publication date	Aug 15, 2023
Grant date	Aug 15, 2023

Abstract

Methods for purifying reaction precursors used in the synthesis of inorganic compounds and methods for synthesizing inorganic compounds from the purified precursors are provided. Also provided are methods for purifying the inorganic compounds and methods for crystallizing the inorganic compounds from a melt. γ and X-ray detectors incorporating the crystals of the inorganic compounds are also provided.

First claim

What is claimed is:

1. A method for forming a purified thallium compound, the method comprising:
combining: at least one starting oxidized thallium compound or at least two solid starting inorganic precursor materials, wherein the at least two starting inorganic precursors are elemental transition metals, elemental semi-metals, halides, metal halides, metal chalcogenides, or a combination thereof and at least one of said at least two solid starting inorganic precursor materials comprises oxidized thallium; and a carbon powder in a reaction vessel;
sealing the reaction vessel under vacuum;
melting the at least one oxidized thallium compound or the at least two solid starting inorganic precursor materials to form a melt, wherein the carbon from the carbon powder reduces the thallium oxide to form a reduced, thallium compound or a reduced, thallium-containing inorganic precursor material; and
solidifying the melt.

2. The method of claim 1 , wherein the at least one starting oxidized thallium compound is combined with the carbon powder and solidifying the melt provides a solid purified thallium compound having a lower oxygen concentration than the starting oxidized thallium compound.

3. The method of claim 1 , wherein the purified thallium compound is Tl 6 SI 4 , Tl 6 SBr 4 , Tl 6 SeI 4 , Tl 4 HgI 6 , TlGaSe 2 , TlBr, Tl 4 AsSe, Tl 3 AsSe 3 , TlInSe 2 , TlSn 2 I 5 , or TlPbI 3 .

4. The method of claim 1 , wherein the at least two starting inorganic precursor materials are combined with the carbon powder, the at least two starting inorganic precursor materials react to form the thallium compound in the melt, and solidifying the melt provides a solid purified thallium compound.

5. The method of claim 4 , wherein the at least two starting inorganic precursor materials are selected from elemental thallium, elemental sulfur, elemental tin, binary thallium halide compounds, binary thallium sulfide compounds, and binary thallium tin compounds, and further wherein the purified thallium compound is a thallium-containing chalcogenide compound, a thallium-containing halide compound, or both.

6. The method of claim 4 , wherein the at least two starting inorganic precursors comprise Tl 2 S, Tl 2 Se, or TlX, where X is a halide element or a combination of halide elements, Tl, S, Se, I 2 , or a combination of two or more thereof.

7. The method of claim 4 , wherein the purified thallium compound is Tl 6 SI 4 , Tl 6 SBr 4 , Tl 6 SeI 4 , Tl 4 HgI 6 , TlGaSe 2 , TlBr, Tl 4 AsSe, Tl 3 AsSe 3 , TlInSe 2 , TlSn 2 I 5 , or TlPbI 3 .

8. The method of claim 4 , further comprising melting the purified thallium compound and growing a crystal of the purified thallium compound from the melt via Bridgman growth.

9. The method of claim 4 , wherein at least one of the starting inorganic precursor materials further comprises one or more impurity elements, the method further comprising pre-purifying the at least one starting inorganic precursor material comprising one or more impurity elements by combining the at least one starting inorganic precursor material comprising one or more impurity elements with a carbon powder in a reaction vessel; sealing the reaction vessel under vacuum; and melting the at least one starting inorganic precursor material comprising one or more impurity elements to form a melt, wherein the carbon from the carbon powder reacts with the one or more impurity elements to form a purified inorganic precursor material; and further wherein the step of combining at least two starting inorganic precursor materials and a carbon powder comprises combining the purified inorganic precursor material with the rest of the two or more starting inorganic precursor materials and a carbon powder.

10. The method of claim 9 , wherein the one or more impurity elements include Al, Bi, Pb, or Si.

11. The method of claim 9 , further comprising melting the purified thallium compound and growing a crystal of the purified thallium compound from the melt via Bridgman growth.

12. The method of claim 1 , wherein the purified thallium compound is Tl 4 HgI 6 and the at least two starting inorganic precursor materials are selected from Tl, Hg, I 2 , HgI, Tl, and HgI 2 .

13. The method of claim 1 , wherein the purified thallium compound is TlGaSe 2 and the at least two starting inorganic precursor materials are selected from Tl, Ga, Se, Tl 2 Se, and Ga 2 Se 3 .

14. The method of claim 1 , wherein the purified thallium compound is Tl 3 AsSe 3 and the at least two starting inorganic precursor materials are selected from Tl, As, Se, Tl 2 Se, and As 2 Se 3 .

15. The method of claim 1 , wherein the purified thallium compound is TlInSe 2 and the at least two starting inorganic precursor materials are selected from Tl, In, Se, Tl 2 Se, and In 2 Se 3 .

16. The method of claim 1 , wherein the purified thallium compound is TlSn 2 I 5 and the at least two starting inorganic precursor materials are selected from Tl, Sn, I 2 , TlI, and SnI 2 .

17. The method of claim 1 , wherein the purified thallium compound is TlPbI 3 and the at least two starting inorganic precursor materials are selected from Tl, Pb, I 2 , PbI 2 , and TlI.

Assignees

• Univ Northwestern

Inventors

• Kanatzidis Mercouri G
• Lin Wenwen

Classifications

• C30B35/007 Primary

  Apparatus for preparing, pre-treating the source material to be used for crystal growth · CPC title

• C01B19/007 Primary

  Tellurides or selenides of metals (C01B19/002 takes precedence) · CPC title

• C01G15/00

  Compounds of gallium, indium or thallium · CPC title

• C30B9/04

  by cooling of the solution · CPC title

• C30B13/06

  the molten zone not extending over the whole cross-section · CPC title