Method of preparing metal chalcogenide nanomaterials

Patent metadata

Field	Value
Publication number	US-2018162732-A1
Application number	US-201515579138-A
Country	US
Kind code	A1
Filing date	Jun 1, 2015
Priority date	Jun 1, 2015
Publication date	Jun 14, 2018
Grant date	—

Abstract

Disclosed are chalcogenide nanomaterials, preferably metal chalcogenide nanomaterials, for example, copper, lead and/or silver chalcogenide nanomaterials. Also provided is a method or process of synthesizing or preparing a chalcogenide nanomaterial, preferably a metal chalcogenide nanomaterial. In an example, a wet-chemical method is used to prepare metal chalcogenide nanomaterials, preferably in a solvent and in the presence of one or more organic ligands. Another example method involves producing metal chalcogenide nanomaterial and includes the steps of forming a mixture of a metal precursor, a chalcogen-based ligand, a solvent and a chalcogen precursor, heating the mixture at a reaction temperature for a duration of reaction time, and separating a produced metal chalcogenide nanomaterial.

First claim

1 . A method for producing metal chalcogenide nanomaterial, comprising the steps of:
forming a mixture of a metal precursor, where the metal precursor is a pure metal or a metal oxide, a chalcogen-based ligand, a solvent, and a chalcogen precursor; heating the mixture at a reaction temperature between about 0° C. to about 200° C., inclusively, for a duration of reaction time; and, separating a produced metal chalcogenide nanomaterial, wherein, the produced metal chalcogenide nanomaterial is a copper, lead or silver chalcogenide nanomaterial.

2 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial has a formula of M 2-x E, where:
M is Cu, Pb or Ag; E is S, Se or Te; and 0≤x≤1.

3 . The method of claim 1 , wherein the reaction temperature is between about 10° C. to about 80° C., inclusively.

4 . The method of claim 1 , wherein the reaction temperature is between about 20° C. to about 60° C., inclusively.

5 . The method of claim 1 , wherein the reaction temperature is about room temperature.

6 . The method of claim 1 , wherein the duration of reaction time is from about 1 minute to about 72 hours, inclusively.

7 . The method of claim 1 , wherein the duration of reaction time is from about 1 minute to about 24 hours, inclusively.

8 . The method of claim 1 , wherein the duration of reaction time is from about 1 minute to about 12 hours, inclusively.

9 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial is formed as nanoparticles, nanowires, nanotubes and/or nanosheets.

10 . The method of claim 1 , wherein the mixture is a liquid mixture.

11 . The method of claim 1 , wherein the metal precursor is a copper, lead or silver precursor.

12 . The method of claim 1 , wherein the metal precursor is a powder.

13 . The method of claim 1 , wherein the metal precursor is formed of pure metal or metal oxide nanoparticles, nanowires or nanosheets.

14 . The method of claim 1 , wherein the chalcogen-based ligand is a chalcogen-based organic ligand.

15 . The method of claim 1 , wherein the chalcogen-based ligand is a sulfur-based ligand.

16 . The method of claim 1 , wherein the chalcogen-based ligand is a thiol or mercapto-substituted organic compound.

17 . The method of claim 1 , wherein the chalcogen-based ligand is a monothiol [CH 3 (CH 2 ) n —CH 2 SH, n=0-16], dithiol [HSCH 2 (CH 2 ) n —CH 2 SH, n=0-6] or multithiol [HSCH 2 (CH 2 ) n1 (CHSH) n2 —CH 2 SH, n 1 =0-6; n 2 =0-4], where a —SH position is variable.

18 . The method of claim 1 , wherein the chalcogen-based ligand is a mono-mercapto-substituted primary, secondary or tertiary monohydric alcohol.

19 . The method of claim 1 , wherein the chalcogen-based ligand is a mono-mercapto-substituted polyhydric alcohol.

20 . The method of claim 1 , wherein the chalcogen-based ligand is a dimercapto-substituted monohydric or polyhydric alcohol.

21 . The method of claim 1 , wherein the chalcogen-based ligand is a mercapto-substituted primary, secondary and tertiary amine or imide.

22 . The method of claim 1 , wherein the chalcogen-based ligand is a mercapto-substituted acid [HS(CH 2 ) n COOH, n=0-10], where a SH position is variable.

23 . The method of claim 1 , wherein the chalcogen-based ligand is a thioacetic acid (CH 3 COSH), thiourea (H 2 NCSNH 2 ), or thioamide (R 1 CSNR 2 R 3 , R 1 =methyl, ethyl, propyl, R 23 =hydrogen, methyl, ethyl, propyl).

24 . The method of claim 1 , wherein the chalcogen-based ligand is a multi-mercapto-substituted primary, secondary or tertiary alcohol, amine, acid or imide.

25 . The method of claim 1 , wherein the solvent is an organic solvent.

26 . The method of claim 1 , wherein the solvent is one or more alcohols.

27 . The method of claim 1 , wherein the solvent is ethanol, methanol or acetone.

28 . The method of claim 1 , wherein the solvent is a monohydric alcohol or primary alcohol [CH 3 (CH 2 ) n —OH, n=0-10; CH 3 O—(CH 2 CH 2 O) n —H, n=1-20], a secondary alcohol [CH 3 (CHOH)(CH 2 ) n —CH 3 , n=0-10,] and/or a tertiary alcohol [(CH 3 ) 2 (COH)(CH 2 ) n CH 3 , n=0-10].

29 . The method of claim 1 , wherein the solvent is a polyhydric alcohol [HOCH 2 (CHOH) n CH 2 OH, n=0-4; HO—(CH 2 CH 2 O) n —H, n=1-20].

30 . The method of claim 1 , wherein the solvent is a symmetric or an asymmetric ketone [R 1 COR 2 , R 1,2 =methyl, ethyl and propyl].

31 . The method of claim 1 , wherein the chalcogen precursor is a chalcogen, a chalcogen powder, a chalcogen solution, a chalcogen-based powder or a chalcogen-based solution.

32 . The method of claim 1 , wherein the chalcogen precursor is sulfur, selenium or tellurium.

33 . The method of claim 1 , wherein the chalcogen precursor is a chalcogen solution having chalcogen powder dissolved in an alkyl phosphine [(R) 3 P, R=butyl, octyl] or a liquid alkylamine.

34 . The method of claim 1 , wherein additional reactive groups of —SH, —OH, —NH 2 and/or —COOH are added to the mixture.

35 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial is separated by centrifugation or solvent precipitation.

36 . The method of claim 1 , wherein the steps are performed in order of:
mixing the metal precursor and the chalcogen-based ligand; adding the solvent; adding the chalcogen precursor; mixing and heating the mixture at the reaction temperature for the duration of reaction time.

37 . A metal chalcogenide nanomaterial, produced according to the method of claim 1 .

Assignees

• Baoshan Iron & Steel

Inventors

• Li Zhen
• Chen Xinqi
• Dou Shixue

Classifications

• H01G9/2022

  characterized by he counter electrode · CPC title

• C01P2004/16

  Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer · CPC title

• C01B19/007 Primary

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

• H01L35/34

  Electricity · mapped topic

• H01L35/26

  Electricity · mapped topic