IP Library Granted Patent US 10,050,189
Granted Patent B2
US 10,050,189 · App. 15/335,736 · Granted Aug 14, 2018

Method of synthesizing bismuth-antimony seleno-telluride nanocrystals

Inventors: Rutvik J. Mehta (Colonie, NY); Douglas Y. Desario (Albany, NY); Alexander O'Toole (Troy, NY)
Assignee: ThermoAura Inc.
H01L35/26C01B19/007H01L35/16H01L35/18H01L35/34C01P2006/32C01P2006/40
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Quick Facts
Patent No.
US 10,050,189
App. No.
15/335,736
Granted
Aug 14, 2018
Kind
B2
Abstract

A first aspect of the disclosure provides for method of synthesizing bismuth-antimony seleno-telluride thermoelectric nanocrystals. The method may comprise: synthesizing an oxidative chalcogen precursor, the synthesizing including: dissolving a metal in acidic deionized water by reacting the metal with a caustic solution in the deionized water to synthesize a first solution, and adjusting at least one of: pH level or a pE level of the first solution; exposing the oxidative chalcogen precursor to a pnictogen precursor to create nanoseeds; and subjecting the nanoseeds to a microwave thereby synthesizing the bismuth-antimony seleno-telluride thermoelectric nanocrystals.

Claims (38)

1. A method of synthesizing thermoelectric nanocrystals, the method comprising:

synthesizing an oxidative chalcogen precursor, the synthesizing including:

dissolving a chalcogen in acidified deionized water by reacting the chalcogen with a caustic solution in the acidified deionized water to synthesize a first solution, and

adjusting at least one of: a pH level or a pE level of the first solution;

exposing the oxidative chalcogen precursor to a pnictogen precursor to create nanoseeds; and

subjecting the nanoseeds to a microwave thereby synthesizing the thermoelectric nanocrystals.

2. The method of claim 1 , wherein the chalcogen includes at least one of: tellurium, selenium, a tellurium oxide, a selenium oxide, tellurous acid, telluric acid, sodium tellurate, selenous acid, or selenic acid.

3. The method of claim 1 , wherein the caustic solution includes hydrogen peroxide.

4. The method of claim 1 , wherein the adjusting the pH level and the pE level of the first solution includes reacting the first solution with at least one of: sodium hydroxide, potassium hydroxide, a pyridine, an amine, or ammonium hydroxide.

5. The method of claim 1 , wherein the pnictogen precursor includes at least one of: bismuth or antimony.

6. The method of claim 1 , wherein the subjecting the nanoseeds to the microwave includes subjecting the nanoseeds to a microwave energy dose of approximately equal to or greater than 2.5 kilojoules per gram (KJ/g).

7. The method of claim 1 , further comprising separating the thermoelectric nanocrystals via at least one of: filtration or centrifugation.

8. The method of claim 1 , wherein the adjusting the pH level of the first solution includes adjusting the pH level to approximately 4.5 to approximately 6.5.

9. The method of claim 1 , wherein the adjusting the pE level of the first solution includes adjusting the pE level to approximately 10 millivolts (mV) to approximately 35 mV.

10. The method of claim 1 ,

wherein the adjusting the pE level of the first solution includes dissolving a reducing agent by adjusting the pH level to greater than 11 using at least one of: sodium hydroxide, potassium hydroxide, a pyridine, an amine, or ammonium hydroxide; and

wherein the reducing agent includes at least one of: sodium hydride, lithium hydride, aluminum hydride, sodium borohydride, potassium borohydride, lithium borohydride or aluminum borohydride.

11. The method of claim 1 , wherein the thermoelectric nanocrystals have a particle size of approximately 5 nanometers (nm) to approximately 100 nm.

12. The method of claim 1 , wherein the dissolving the chalcogen in acidified deionized water by reacting the chalcogen with the caustic solution in the acidified deionized water to synthesize the first solution includes providing 20% excess of the caustic solution relative to the first solution.

13. The method of claim 1 , wherein the thermoelectric nanocrystals include Sb 2-x Bi x Se 3-y Te y , wherein 0≤x≤2 and 0≤y≤3.

14. The method of claim 1 , wherein the thermoelectric nanocrystals are doped with sodium up to 1 atomic percent.

15. A method of synthesizing thermoelectric nanocrystals, the method comprising:

synthesizing an oxidative chalcogen precursor, the synthesizing including:

dissolving a chalcogen in acidified deionized water by reacting the chalcogen with hydrogen peroxide in the acidified deionized water to synthesize a first solution, the chalcogen including at least one of: tellurium, selenium a tellurium oxide, a selenium oxide, tellurous acid, telluric acid, sodium tellurate, selenous acid, or selenic acid; and

adjusting at least one of: a pH level or a pE level of the first solution;

exposing the oxidative chalcogen precursor to a pnictogen precursor to create nanoseeds; and

subjecting the nanoseeds to a microwave thereby synthesizing the thermoelectric nanocrystals.

16. The method of claim 15 , wherein the adjusting the pH level and the pE level of the first solution includes reacting the first solution with at least one of: sodium hydroxide, potassium hydroxide, a pyridine, an amine, or ammonium hydroxide.

17. The method of claim 15 , wherein the pnictogen precursor includes at least one of: bismuth or antimony.

18. The method of claim 15 , wherein the subjecting the nanoseeds to the microwave includes subjecting the nanoseeds to a microwave energy dose of approximately equal to or greater than 2.5 kilojoules per gram (KJ/g).

19. The method of claim 15 , further comprising separating the thermoelectric nanocrystals via at least one of: filtration or centrifugation.

20. The method of claim 15 , wherein the adjusting the pH level of the first solution includes adjusting the pH level to approximately 4.5 to approximately 6.5.

21. The method of claim 15 , wherein the adjusting the pE level of the first solution includes adjusting the pE level to approximately 10 millivolts (mV) to approximately 35 mV.

22. The method of claim 15 ,

wherein the adjusting the pE level of the first solution includes dissolving a reducing agent by adjusting the pH level to greater than 11 using at least one of: sodium hydroxide, potassium hydroxide, a pyridine, an amine, or ammonium hydroxide; and

wherein the reducing agent includes at least one of: sodium hydride, lithium hydride, aluminum hydride, sodium borohydride, potassium borohydride, lithium borohydride or aluminum borohydride.

23. The method of claim 15 , wherein the thermoelectric nanocrystals include Sb 2-x Bi x Se 3-y Te y , wherein 0≤x≤2 and 0≤y≤3.

24. The method of claim 15 , wherein the thermoelectric nanocrystals are doped with sodium up to 1 atomic percent.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 27, 2016
From: MEHTA, RUTVIK J; DESARIO, DOUGLAS Y; O'TOOLE, ALEXANDER
To: THERMOAURA INC.
Reel/Frame 040150/0646 →
Continuity (3)
Continuation PCTUS2016057886 · Oct 20, 2016
Provisional Application 62253897 · Nov 11, 2015
Related Publication 20170133569A1 · May 11, 2017
Cited By (1)
US 12,698,442