Preparation method for ultrathin SB2S3 nanosheet as anode material for Li/Na ion battery applications

Patent metadata

Field	Value
Publication number	US-11302909-B2
Application number	US-201916522898-A
Country	US
Kind code	B2
Filing date	Jul 26, 2019
Priority date	Jul 27, 2018
Publication date	Apr 12, 2022
Grant date	Apr 12, 2022

Abstract

Methods of synthesizing few-layer two-dimensional (2D) Sb2S3 nanosheets using scalable chemical exfoliation are provided. The 2D Sb2S3 nanosheets can be developed as bi-functional anode materials in both lithium ion batteries and sodium ion batteries. The unique structural and functional features brought by 2D Sb2S3 nanosheets can offer short electron/ion diffusion paths and abundant active sites for surface redox reactions.

First claim

What is claimed is:

1. A method for synthesizing two-dimensional (2D) nanosheets, the method comprising:
providing a bulk precursor;
performing solvothermal intercalation of lithium (Li) atoms into van der Waals bonded interlayers of particles of the bulk precursor in the presence of a solvent to form Li-intercalated bulk compounds;
performing a sonication process on the Li-intercalated bulk compounds to exfoliate the Li-intercalated bulk compounds into 2D nanosheets;
performing a centrifugation process to separate the exfoliated 2D nanosheets and then washing the exfoliated 2D nanosheets;
freeze drying the separated and washed 2D nanosheets; and
collecting the 2D nanosheets after freeze drying,
wherein: a) the bulk precursor is a Sb 2 S 3 bulk precursor and the collected 2D nanosheets are Sb 2 S 3 2D nanosheets; b) the bulk precursor is a Sb 2 Se 3 bulk precursor and the collected 2D nanosheets are Sb 2 Se 3 2D nanosheets; c) the bulk precursor is a Bi 2 S 3 bulk precursor and the collected 2D nanosheets are Bi 2 S 3 2D nanosheets; or d) the bulk precursor is a Sb 2 Te 3 bulk precursor and the collected 2D nanosheets are Sb 2 Te 3 2D nanosheets.

2. The method according to claim 1 , wherein the bulk precursor is a Sb 2 S 3 bulk precursor and the collected 2D nanosheets are Sb 2 S 3 2D nanosheets.

3. The method according to claim 2 , wherein freeze drying the separated and washed 2D nanosheets comprises freeze drying the separated and washed 2D nanosheets into a 2D nanosheet powder comprising the 2D nanosheets, and
wherein collecting the 2D nanosheets after freeze drying comprises collecting the 2D nanosheet powder after freeze drying.

4. The method according to claim 2 , wherein the solvent is benzyl alcohol.

5. The method according to claim 2 , wherein the sonication process is a mild bath sonication process comprising sonicating in a mixture of deionized water and N-methyl-2-pyrrolidone (DI water/NMP).

6. The method according to claim 2 , wherein washing the exfoliated 2D nanosheets comprises washing the exfoliated 2D nanosheets a plurality of times with diluted HCl and DI water.

7. The method according to claim 2 , wherein the collected 2D nanosheets have a thickness of less than 5 nm each.

8. The method according to claim 2 , wherein freeze drying the separated and washed 2D nanosheets comprises freeze drying the separated and washed 2D nanosheets into a 2D nanosheet powder comprising the 2D nanosheets,
wherein collecting the 2D nanosheets after freeze drying comprises collecting the 2D nanosheet powder after freeze drying,
wherein the solvent is benzyl alcohol,
wherein the sonication process is a mild bath sonication process comprising sonicating in a mixture of DI water/NMP,
wherein washing the exfoliated 2D nanosheets comprises washing the exfoliated 2D nanosheets a plurality of times with diluted HCl and DI water, and
wherein the collected 2D nanosheets have a thickness of less than 5 nm each.

9. The method according to claim 1 , wherein freeze drying the separated and washed 2D nanosheets comprises freeze drying the separated and washed 2D nanosheets into a 2D nanosheet powder comprising the 2D nanosheets, and
wherein collecting the 2D nanosheets after freeze drying comprises collecting the 2D nanosheet powder after freeze drying.

10. The method according to claim 1 , wherein the solvent is benzyl alcohol.

11. The method according to claim 1 , wherein the sonication process is a mild bath sonication process comprising sonicating in a mixture of DI water/NMP.

12. The method according to claim 1 , wherein washing the exfoliated 2D nanosheets comprises washing the exfoliated 2D nanosheets a plurality of times with diluted HCl and DI water.

13. The method according to claim 1 , wherein the collected 2D nanosheets have a thickness of less than 5 nm each.

14. The method according to claim 1 , wherein freeze drying the separated and washed 2D nanosheets comprises freeze drying the separated and washed 2D nanosheets into a 2D nanosheet powder comprising the 2D nanosheets,
wherein collecting the 2D nanosheets after freeze drying comprises collecting the 2D nanosheet powder after freeze drying,
wherein the solvent is benzyl alcohol,
wherein the sonication process is a mild bath sonication process comprising sonicating in a mixture of DI water/NMP,
wherein washing the exfoliated 2D nanosheets comprises washing the exfoliated 2D nanosheets a plurality of times with diluted HCl and DI water, and
wherein the collected 2D nanosheets have a thickness of less than 5 nm each.

15. A method for synthesizing an anode comprising two-dimensional (2D) nanosheets, the method comprising:
providing a bulk precursor;
performing solvothermal intercalation of lithium (Li) atoms into van der Waals bonded interlayers of particles of the bulk precursor in the presence of a solvent to form Li-intercalated bulk compounds;
performing a sonication process on the Li-intercalated bulk compounds to exfoliate the Li-intercalated bulk compounds into 2D nanosheets;
performing a centrifugation process to separate the exfoliated 2D nanosheets and then washing the exfoliated 2D nanosheets;
freeze drying the separated and washed 2D nanosheets;
collecting the 2D nanosheets after freeze drying; and
depositing the collected 2D nanosheets on a conductive substrate and heating to form the anode,
wherein: a) the bulk precursor is a Sb 2 S 3 bulk precursor and the collected 2D nanosheets are Sb 2 S 3 2D nanosheets; b) the bulk precursor is a Sb 2 Se 3 bulk precursor and the collected 2D nanosheets are Sb 2 Se 3 2D nanosheets; c) the bulk precursor is a Bi 2 S 3 bulk precursor and the collected 2D nanosheets are Bi 2 S 3 2D nanosheets; or d) the bulk precursor is a Sb 2 Te 3 bulk precursor and the collected 2D nanosheets are Sb 2 Te 3 2D nanosheets.

16. The method according to claim 15 , wherein freeze drying the separated and washed 2D nanosheets comprises freeze drying the separated and washed 2D nanosheets into a 2D nanosheet powder comprising the 2D nanosheets,
wherein collecting the 2D nanosheets after freeze drying comprises collecting the 2D nanosheet powder after freeze drying,
wherein the solvent is benzyl alcohol,
wherein the sonication process is a mild bath sonication process comprising sonicating in a mixture of DI water/NMP,
wherein washing the exfoliated 2D nanosheets comprises washing the exfoliated 2D nanosheets a plurality of times with diluted HCl and DI water, and
wherein the collected 2D nanosheets have a thickness of less than 5 nm each.

17. The method according to claim 15 , wherein the bulk precursor is a Sb 2 S 3 bulk precursor and the collected 2D nanosheets are Sb 2 S 3 2D nanosheets,
wherein freeze drying the separated and washed 2D nanosheets comprises freeze drying the separated and washed 2D nanosheets into a 2D nanosheet powder comprising the 2D nanosheets,
wherein collecting the 2D nanosheets after freeze drying comprises collecting the 2D nanosheet powder after freeze drying,
wherein the solvent is benzyl alcohol,
wherein the sonication process is a mild bath sonication process comprising sonicating in a mixture of DI water/NMP,
wherein washing the exfoliated 2D nanosheets comprises washing the exfoliated 2D nanosheets a plurality of times with diluted HCl and DI water, and
wherein the collected 2D nanosheets have a thickness of less than 5 nm each.

18. The method according to claim 15 , further comprising:
mixing the collected 2D nanosheets with a conductive agent and a binder in a solvent to

Assignees

• Univ Hong Kong Science & Tech

Inventors

• Kim Jang Kyo
• Yao Shanshan
• Cui Jiang

Classifications

• C01P2004/02

  obtained by optical microscopy · CPC title

• H01M10/054

  Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium · CPC title

• H01M4/581

  Chalcogenides or intercalation compounds thereof · CPC title

• H01M4/0471

  involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title