IP Library Granted Patent US 10,422,051
Granted Patent B2
US 10,422,051 · App. 15/677,706 · Granted Sep 24, 2019

Article comprising a semiconducting material

Inventors: Jeffrey Whalen (Tallahassee, FL); Theo Siegrist (Tallahassee, FL)
Assignee: The Florida State University Research Foundation, Inc.
C30B29/46C30B9/10C30B9/12C30B29/22H01B1/08H01B1/10
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Quick Facts
Patent No.
US 10,422,051
App. No.
15/677,706
Granted
Sep 24, 2019
Kind
B2
Abstract

Single crystals of the new semiconducting oxychalcogenide phase were synthesized using a novel crystal growth method. The crystals had low defects and homogeneous composition as characterized by single crystal X-ray diffraction and scanning electron microscopy, respectively. Heat capacity and resistivity measurements were in agreement with the calculated band structure calculations indicating semiconductivity, with a band gap of about 3 eV.

Claims (37)

1. A method for forming an oxychalcogenide composition, comprising:

providing a mixture having a molar ratio of about 20 R:1 RO:1 X, where R is an alkaline earth metal cation, X is an elemental chalcogen, and O is oxygen;

heating the mixture until the mixture melts;

fluxing the melted mixture at least at the melting point for about 10 hours;

allowing the mixture to cool; and

removing one or more oxychalcogenide crystals from the mixture, where the one or more oxychalcogenide crystals, comprise:

a tetragonal crystal of repeating units of RX′ and RO;

wherein R is an alkaline earth metal cation, X′ is an anionic chalcogen, and O is oxygen;

wherein the alkaline earth metal cation of RO is integrated into a crystalline structure with the unit of RX′; and

wherein the R:X′ molar ratio is about 2:1.

2. The method of claim 1 , wherein the mixture is heated to about 1,000° C.

3. The method of claim 1 , wherein the mixture is cooled to about 820° C. over a period of time ranging from about 24 hours to about 150 hours.

4. The method of claim 1 , wherein the oxychalcogenide composition is Ba 2 TeO.

5. The method of claim 1 , wherein the elemental chalcogen comprises tellurium.

6. The method of claim 1 , further comprising adding a doping agent other than the elemental chalcogen to the mixture such that a doping anion is substituted for a portion of the anionic chalcogen of the one or more oxychalcogenide crystals.

7. The method of claim 6 , wherein the doping agent comprises a pnictogen.

8. The method of claim 7 , wherein the pnictogen comprises bismuth.

9. A method for forming an oxychalcogenide composition, comprising:

providing a mixture having a molar ratio of about 20 R:1 RO:1 X, where R is an alkaline earth metal cation, X is an elemental chalcogen, and O is oxygen;

placing the mixture in a crucible;

sealing the crucible;

heating the mixture until the mixture melts;

fluxing the melted mixture at least at the melting point for about 10 hours;

allowing the mixture to cool; and

removing one or more oxychalcogenide crystals from the mixture, where the one or more oxychalcogenide crystals, comprise:

a tetragonal crystal of repeating units of RX′ and RO;

wherein R is an alkaline earth metal cation, X′ is an anionic chalcogen, and O is oxygen;

wherein the alkaline earth metal cation of RO is integrated into a crystalline structure with the unit of RX′; and

wherein the R:X′ molar ratio is about 2:1.

10. The method of claim 9 , wherein the step of heating the mixture until the mixture melts is performed to a temperature of 1000° C.

11. The method of claim 9 , wherein the step of allowing the mixture to cool is performed at a rate of 1.2 degrees per hour to 7.4 degrees per hour.

12. The method of claim 9 , wherein the step of placing the mixture into the crucible is performed in an inert atmosphere.

13. The method of claim 12 , wherein the inert atmosphere is a single inert gas or a mixture of inert gases.

14. The method of claim 13 , wherein the single inert gas is argon.

15. The method of claim 12 , wherein the step of placing the mixture into the crucible is performed at an elevated pressure.

16. The method of claim 9 , further comprising doping the mixture, wherein the doping of the mixture comprises:

adding a pnictogen to the mixture such that the pnictogen is present in the one or more oxychalcogenide crystals at an amount up to about 20 atomic percent of the anionic chalcogen.

Assignments (2)
CONFIRMATORY LICENSE Recorded Mar 9, 2020
From: FLORIDA STATE UNIVERSITY
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 052123/0409 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 16, 2017
From: WHALEN, JEFFREY; SIEGRIST, THEO
To: THE FLORIDA STATE UNIVERSITY RESEARCH FOUNDATION, INC.
Reel/Frame 043309/0670 →
Continuity (4)
Division 14674567 · Mar 31, 2015
Continuation PCTUS2013067045 · Oct 28, 2013
Provisional Application 61718945 · Oct 26, 2012
Related Publication 20180023213A1 · Jan 25, 2018