Method for preparing phase-separated lead telluride-lead sulfide nanopowder using solution synthesis and phase-separated lead telluride-lead sulfide nanopowder prepared thereby

Patent metadata

Field	Value
Publication number	US-10399148-B2
Application number	US-201615739536-A
Country	US
Kind code	B2
Filing date	Jun 24, 2016
Priority date	Jun 26, 2015
Publication date	Sep 3, 2019
Grant date	Sep 3, 2019

Abstract

The present invention relates to a method for preparing a phase-separated lead telluride-lead sulfide nanopowder using solution synthesis and a phase-separated lead telluride-lead sulfide nanopowder prepared by the method. The method includes: (a) mixing tellurium and a first solvent, followed by ultrasonic irradiation to prepare a tellurium precursor solution; (b) mixing an organosulfur compound and a second solvent, followed by ultrasonic irradiation to prepare a sulfur precursor solution; (c) mixing lead oxide, a third solvent, and a fourth solvent and heating the mixture to prepare a lead precursor solution; (d) adding the tellurium precursor solution to the lead precursor solution and allowing the mixture to react; (e) adding the sulfur precursor solution to the reaction mixture of step (d) and allowing the resulting mixture to react; and (f) cooling the reaction mixture of step (e) to room temperature to prepare a phase-separated lead telluride-lead sulfide nanopowder.

First claim

The invention claimed is:

1. A method for preparing a phase-separated lead telluride-lead sulfide nanopowder using solution synthesis, comprising:
(a) mixing tellurium (Te) and a first solvent, and exposing the mixture of the tellurium (Te) and the first solvent to ultrasonic irradiation to prepare a tellurium precursor solution;
(b) mixing an organosulfur (S) compound and a second solvent, and exposing the mixture of the organosulfur (S) compound and the second solvent to ultrasonic irradiation to prepare a sulfur precursor solution;
(c) mixing lead oxide (PbO), a third solvent, and a fourth solvent and heating the mixture of the lead oxide (PbO), the third solvent, and the fourth solvent to prepare a lead precursor solution;
(d) adding the tellurium precursor solution prepared in step (a) to the lead precursor solution prepared in step (c) to form a first reaction mixture and allowing the first reaction mixture to react;
(e) adding the sulfur precursor solution prepared in step (b) to the first reaction mixture of step (d) to form a second reaction mixture and allowing the second reaction mixture to react; and
(f) cooling the second reaction mixture of step (e) to room temperature to provide a phase-separated lead telluride-lead sulfide nanopowder.

2. The method according to claim 1 , wherein the first solvent used in step (a) is selected from the group consisting of trioctylphosphine (TOP), tridiethylaminophosphine (TDP), tributylphophine (TBP), and mixtures thereof.

3. The method according to claim 1 , wherein the organosulfur compound used in step (b) is selected from the group consisting of bis(trimethylsilyl)sulfide, dimethyl sulfide, and a mixture thereof.

4. The method according to claim 1 , wherein the second solvent used in step (b) is selected from the group consisting of 1-octadecene, trioctylphosphine (TOP), oleylamine, and mixtures thereof.

5. The method according to claim 1 , wherein the third solvent used in step (c) is selected from the group consisting of 1-octadecene, trioctylphosphine (TOP), oleylamine, and mixtures thereof.

6. The method according to claim 1 , wherein the fourth solvent is selected from the group consisting of oleic acid, octanoic acid, stearic acid, and mixtures thereof.

7. The method according to claim 1 , wherein, in step (c), the mixture is heated to 120 to 180° C.

8. The method according to claim 1 , wherein the reaction time in step (d) is from 3 to 7 minute.

9. The method according to claim 1 , wherein the reaction time in step (e) is from 1 to 5 minutes.

Assignees

• Univ Korea Res & Bus Found

Inventors

• Sung Yun-Mo
• Cho Ki-Hyun

Classifications

• C04B2235/5454

  nanometer sized, i.e. below 100 nm · CPC title

• C04B2235/3296

  Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate · CPC title

• C04B35/62828

  Non-oxide ceramics · CPC title

• C04B35/6264

  Mixing media, e.g. organic solvents · CPC title

• C01B19/002

  Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions · CPC title