Preparation of metal chalcogenides

Patent metadata

Field	Value
Publication number	US-2019039913-A1
Application number	US-201815998266-A
Country	US
Kind code	A1
Filing date	Jul 26, 2018
Priority date	Aug 1, 2017
Publication date	Feb 7, 2019
Grant date	—

Abstract

A method embodiment involves preparing single metal or mixed transition metal chalcogenide using exfoliation of two or more different bulk transition metal dichalcogenides in a manner to form an intermediate hetero-layered transition metal chalcogenide structure, which can be treated to provide a single-phase transition metal chalcogenide.

First claim

We claim:

1 . A method for preparing a transition metal chalcogenide, comprising the step of exfoliating two or more different starting transition metal chalcogenides separately or together to produce exfoliated products and combining the exfoliated products to form a transition metal chalcogenide structure having layers of different composition.

2 . The method of claim 1 wherein exfoliating is conducted by mechanical processing of the starting transition metal chalcogenides.

3 . The method of claim 2 wherein the exfoliating is conducted by dry mechanical processing of the two or more different transition metal chalcogenides together.

4 . The method of claim 2 wherein dry mechanical processing is carried out in an inert atmosphere or atmosphere that is non-reactive towards the two or transition metal chalcogenides and the produced transition metal chalcogenide structure.

5 . The method of claim 2 wherein the exfoliating is conducted by mechanical processing in a liquid medium.

6 . The method of claim 5 wherein the two or more different transition metal chalcogenides are exfoliated separately.

7 . The method of claim 5 wherein the two or more different transition metal chalcogenides are exfoliated together.

8 . The method of claim 1 wherein the exfoliated products self-combine to form a layered 3D heterostructure.

9 . The method of claim 1 wherein the exfoliated products are mixed to combine to form a layered 3D heterostructure.

10 . The method of claim 5 wherein the liquid medium comprises at least one of isopropanol, water, dimethylsulphoxide, N-vinyl-pyrrolidinone, N-methyl-pyrrolidinone, benzonitrile or any solvent that does not react with exfoliated materials under the processing conditions.

11 . The method of claim 2 wherein mechanical processing is carried out using pestle and mortar, shaker ball mills of any configuration, planetary ball mills of any configurations, any type of laboratory or industrial grinders, sonication, or other milling, or grinding equipment.

12 . The method of claim 1 wherein exfoliating is carried out by ultrasonic irradiation.

13 . The method of claim 1 including the further step of treating the transition metal chalcogenide structure to form a substantially single-phase structure.

14 . The method of claim 13 wherein the mixed transition metal chalcogenide is substantially devoid of separate phases of the two or more different transition metal chalcogenides.

15 . The method of claim 13 wherein a substantially homogenous solid solution of the two or more different transition metal chalcogenides is produced.

16 . The method of claim 13 wherein the transition metal chalcogenide structure is treated by heat treating at a temperature for a time to achieve a substantially single-phase structure.

17 . The method of claim 16 wherein heat treating is conducted at elevated temperatures between 100 and 1500 degrees C. in an inert or non-reactive gas atmosphere to produce a single-phase transition metal chalcogenide.

18 . The method of claim 16 wherein the heat treating time is between 1 minute to 72 hours or longer.

19 . The method of claim 16 wherein heat treating is conducted in an atmosphere comprising at least one of helium, argon, krypton, xenon, nitrogen, methane and any other gas, which shows no reactivity towards the transition metal chalcogenides or the produced mixed disordered layered transition metal chalcogenide.

20 . The method of claim 1 including the further step of exfoliating the transition metal chalcogenide structure.

21 . The method of claim 1 wherein that forms a three dimensional layered material or a two dimensional layer material.

22 . The method of claim 21 including heat treating the layered material to form a single phase.

23 . The method of claim 1 wherein the starting transition metal chalcogenides comprise transition metal dichalcogenides selected from the group consisting of the group 4 transition metal dichalcogenides (M=Ti, Zr, Hf), group 5 transition metal dichalcogenides (M=V, Nb, Ta) or group 6 transition metal dichalcogenides (M=Cr, Mo, W), group 7 transition metal dichalcogenides (M=Mn, Re), group 10 transition metal dichalcogenides (M=Pd, Pt)], group 11 transition metal dichalcogenides (Cu, Ag), group 12 transition metal dichalcogenides (Zn, Cd), group 13 transition metal dichalcogenides (e.g., M=In, Ga) as well as lanthanum group metals chalcogenides (Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu).

24 . The method of claim 1 that produces a hetero-layered transition metal chalcogenide having a chemical composition represented by (M a M 2 b M 3 c . . . n )(X d X 2 e X 3 f ), where the formula unit includes two or more different metals (M), and X, X 2 and X 3 represent S, Se, or Te, whereby the sum of a+b+c+ . . . n is between 1 and 3 and the sum of d+e+f is between 1 and 6.

25 . A transition metal chalcogenide having a structure having layers of different composition derived from different transition metal chalcogenides.

26 . The material of claim 25 that comprises a substantially homogenous solid solution of two or more different transition metal chalcogenides.

27 . A nanoplate obtained by the method of claim 1 .

28 . Composition of matter comprising a single layer or multi-layer mixed transition metal chalcogenide in the form 2D or 3D-nanoplates having a chemical composition represented by (M a M 2 b M 3 c . . . n )(X d X 2 e X 3 f ), where the formula unit includes three or more different metals (M), and X, X 2 and X 3 represent S, Se, or Te, whereby the sum of a+b+c+ . . . n is between 1 and 3 and the sum of d+e+f is between 1 and 6.

29 . A method for preparing a transition metal chalcogenide, comprising exfoliating in a liquid medium a transition metal chalcogenide material, exfoliating in the same or in a different liquid medium, a different transition metal chalcogenide material, and combining dispersions of the exfoliated products of the exfoliating in a manner to form a transition metal chalcogenide structure having layers of different composition.

30 . The method of claim 29 where the transition metal chalcogenide structure comprises a mixed metal dichalcogenide material and/or a mixed metal trichalcogenide material, a same metal dichalcogenide material, or a same metal trichalcogenide material.

31 . The method of claim 29 the metal is selected from the group consisting of Ti, Zr, Hf, Nb, Ta, Mo, W, Re, Pd, Pt, In, Ga and Sn.

32 . The method of claim 29 wherein the exfoliated materials include the presence of at least one of graphite, black phosphorus, and boron nitride.

33 . The method of claim 29 wherein the combining step is conducted by mixing the dispersions of the exfoliated products together or by additive assembly of the exfoliated products.

34 . The method of claim 29 wherein the combining step includes mixing liquid dispersions of the exfoliated products together in any proportion and removing the liquid medium.

35 . The method of claim 29 including the further step of treating the transition metal chalcogenide structure to form a substantially homogeneous solid solution.

36 . The method of claim 29 w

Assignees

• Univ Iowa State Res Found Inc

Inventors

• Balema Viktor
• Hlova Ihor
• Pecharsky Vitalij K

Classifications

• B02C19/06

  Jet mills · CPC title

• C01P2004/30

  extending in three dimensions · CPC title

• C01G39/06 Primary

  Sulfides · CPC title

• C01G41/00

  Compounds of tungsten · CPC title

• C01P2004/03

  obtained by SEM · CPC title