Aqueous-based method of preparing metal chalcogenide nanomaterials

Patent metadata

Field	Value
Publication number	US-2018170754-A1
Application number	US-201515579141-A
Country	US
Kind code	A1
Filing date	Jun 1, 2015
Priority date	Jun 1, 2015
Publication date	Jun 21, 2018
Grant date	—

Abstract

Provided is a method for producing metal chalcogenide nanomaterials, comprising the steps of forming an aqueous solution of a chalcogen precursor, a reducing agent and a metal salt; mixing the aqueous solution for a duration of time at a reaction temperature of between about 10° C. to about 40° C., inclusively; and separating the produced metal chalcogenide nanomaterials from the aqueous solution. Also provided is a method of converting metal chalcogenide nanoparticles into metal chalcogenide nanotubes or nanosheets, comprising the steps of forming an aqueous mixture of a chalcogen precursor, a reducing agent and the metal chalcogenide nanoparticles in water; and forming the nanotubes or nanosheets by stirring or not stirring the aqueous mixture, respectively.

First claim

1 . A method for producing metal chalcogenide nanomaterials, comprising the steps of:
forming an aqueous solution of a chalcogen precursor, a reducing agent and a metal salt; mixing the aqueous solution for a duration of time at a reaction temperature of between about 10° C. to about 40° C., inclusively; and, separating a produced metal chalcogenide nanomaterial from the aqueous solution.

2 . The method of claim 1 , wherein the metal chalcogenide nanomaterial is produced without use of a surfactant.

3 . The method of claim 1 , wherein the reaction temperature is between about 10° C. to about 30° C., inclusively.

4 . The method of claim 1 , wherein the reaction temperature is between about 20° C. to about 30° C., inclusively.

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

6 . The method of claim 5 , wherein external heating is not used.

7 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial has a formula of M x E y , where:
M is Bi, Cu, Pb, Ag, In, Sn, or Sb; E is O, S, Se or Te when M is Cu, or E is S, Se or Te when M is Bi, Pb, Ag, In, Sn, or Sb; and 1≤x≤2 and 1≤y≤3.

8 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial has a formula of M x E y , where:
M is Bi, Cu or Pb; E is O, S, Se or Te when M is Cu, or E is S, Se or Te when M is Bi or Pb; and 1≤x≤2 and 1≤y≤3.

9 . The method of claim 1 , wherein the metal salt is water soluble.

10 . The method of claim 1 , wherein the metal salt is selected from the group of a bismuth salt, a copper salt, a lead salt, a silver salt, an indium salt, a tin salt and an antimony salt, and the produced metal chalcogenide nanomaterial is bismuth, copper, lead, silver, indium, tin and/or antimony chalcogenide nanoparticles.

11 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial is bismuth chalcogenide nanoparticles, and the metal salt is a water soluble bismuth salt.

12 . The method of claim 11 , wherein the bismuth salt is bismuth chloride and/or bismuth nitrate.

13 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial is copper chalcogenide nanoparticles, and the metal salt is a water soluble copper salt.

14 . The method of claim 13 , where the copper salt is copper chloride, copper nitrate and/or copper sulfate.

15 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial is lead chalcogenide nanoparticles, and the metal salt is a water soluble lead salt.

16 . The method of claim 15 , where the lead salt is lead nitrate.

17 . The method of claim 1 , wherein the chalcogen precursor is water soluble.

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

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

20 . The method of claim 1 , wherein the chalcogen precursor is selected from the group of sodium sulfide (Na 2 S.9H 2 O), ammonium sulfide [(NH 4 ) 2 S], sodium selenite (Na 2 SeO 3 ), sodium tellurite (Na 2 TeO 3 ), selenium oxide (SeO 2 ), and tellurium oxide (TeO 2 ).

21 . The method of claim 1 , wherein the reducing agent is sodium borohydride (NaBH 4 ), LiBH 4 , and/or KBH 4 .

22 . The method of claim 1 , wherein the ratio of the reducing agent to the chalcogen precursor is from between about 1:1 to about 100:1.

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

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

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

26 . The method of claim 1 , wherein the produced metal chalcogenide nanomaterial is separated by centrifugation.

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

28 . A method of converting metal chalcogenide nanoparticles into metal chalcogenide nanotubes or metal chalcogenide nanosheets, comprising the steps of:
forming an aqueous mixture of a chalcogen precursor, a reducing agent and the metal chalcogenide nanoparticles in water; and forming metal chalcogenide nanotubes by stirring the aqueous mixture; or, forming metal chalcogenide nanosheets by not stirring the aqueous mixture.

29 . The method of claim 28 , wherein the method is performed at a reaction temperature of between about 10° C. to about 40° C., inclusively, or between about 10° C. to about 30° C., inclusively, or between about 20° C. to about 30° C., inclusively.

30 . The method of claim 28 , wherein the method is performed at a reaction temperature that is about room temperature.

31 . The method of claim 30 , wherein external heating is not used.

32 . The method of claim 28 , wherein the metal chalcogenide nanotubes or nanosheets are separated by centrifugation.

33 . The method of claim 28 , wherein the nanoparticles are mostly formed into nanotubes or nanosheets within less than about 1 hour.

34 . The method of claim 28 , wherein the nanoparticles are mostly formed into nanotubes or nanosheets within less than about 30 min.

35 . The method of claim 28 , wherein the nanoparticles are mostly formed into nanotubes or nanosheets within less than about 20 min.

36 . The method of claim 28 , wherein the metal chalcogenide nanoparticles are produced according to claim 1 .

37 . The method of claim 28 , wherein a diameter of the formed nanotubes is tuned by selecting a size of the metal chalcogenide nanoparticles.

38 . The method of claim 28 , wherein a size of the formed nanosheets is tuned by selecting a reaction time without stirring.

39 . The method of claim 28 , wherein the stirring uses magnetic or mechanical stirring.

40 . The method of claim 28 , further including the metal chalcogenide nanomaterials being formed into a pellet.

Assignees

• Baoshan Iron & Steel

Inventors

• Li Zhen
• Han Chao
• Dou Shixue

Classifications

• C01G5/00

  Compounds of silver · CPC title

• C01P2006/32

  Thermal properties · CPC title

• C01G30/008

  Sulfides (C01G30/001 takes precedence) · CPC title

• H01L35/34

  Electricity · mapped topic

• C01B19/002

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