Exfoliation

Patent metadata

Field	Value
Publication number	US-10421875-B2
Application number	US-201515114571-A
Country	US
Kind code	B2
Filing date	Jan 30, 2015
Priority date	Jan 31, 2014
Publication date	Sep 24, 2019
Grant date	Sep 24, 2019

Abstract

This invention relates to a method for exfoliating inorganic layered compounds to form two-dimensional (2D) inorganic compounds. The exfoliation is carried out in aqueous media in the present of polycyclic aromatic compounds. The invention also relates to aqueous suspensions of two-dimensional compounds which arise from the exfoliation method. The invention further relates to methods of forming thin films of two-dimensional compounds from suspensions and to devices comprising thin films of two-dimensional (2D) inorganic compounds.

First claim

The invention claimed is:

1. A method of producing an aqueous suspension of particles of a two-dimensional inorganic compound, the method comprising:
a) providing multilayered particles of the inorganic compound in an aqueous medium which comprises at least one polycyclic aromatic compound, or a salt thereof; wherein the polycyclic aromatic compound is present in the aqueous medium in an amount from 1 ×10 −4 mol/L to 200 ×10 −4 mol/L, wherein the or each polycyclic aromatic compound independently has a ring system which comprises from 2 to 10 fused benzene rings, the ring system being substituted with from 1 to 4 independently selected hydrophilic groups, each hydrophilic group consisting of less than 20 atoms;
b) subjecting the multilayered particles of the inorganic compound in the aqueous medium to energy to obtain a suspension;
c) when the suspension obtained in step b) also comprises multilayered particles of the inorganic compound, the method further comprises the step of reducing the amount of multilayered particles of the inorganic compound in the suspension to obtain an aqueous suspension comprising particles of the two-dimensional inorganic compound and the at least one polycyclic aromatic compound.

2. A method of claim 1 , wherein the ring system of the polycyclic aromatic compound contains 3 to 6 fused benzene rings and at least one ring contains two atoms in common with each of two or more other rings.

3. A method of claim 1 , wherein the independently selected hydrophilic groups of the polycyclic aromatic compound may consist of less than 6 atoms independently selected from S, O, P, H, C, N, B and I.

4. A method of claim 1 , wherein at least one hydrophilic group is a sulfonic acid or a base addition salt of a sulfonic acid.

5. A method of claim 1 , wherein the polycyclic aromatic compound is selected from:

6. A method of claim 1 , wherein the polycyclic aromatic compound is present in the aqueous medium in an amount from 1 ×10 −4 mol/L to 66 ×10 −4 mol/L.

7. A method of claim 1 , wherein the aqueous medium comprises an alcohol and wherein the alcohol may form from 10 to 30% by volume of the aqueous media.

8. A method of claim 1 , wherein the aqueous medium is deuterated water.

9. A method of claim 1 , wherein the aqueous medium has a pH in the range from 1 to 7.

10. A method of claim 1 , wherein greater than 75% by weight of the particles of the two dimensional inorganic compound have a diameter between 50 and 750 nm.

11. A method of claim 1 , wherein the inorganic compound is h-BN.

12. A method of claim 11 , wherein greater than 75% by weight of the two dimensional inorganic compound has a thickness of from 1 to 3 molecular layers.

13. A method of claim 1 , wherein the inorganic compound is a transition metal dichalcogenide.

14. A method of claim 13 , wherein greater than 75% by weight of the two dimensional inorganic compound has a thickness of from 4 to 6 molecular layers.

15. A method of claim 1 , wherein the energy is sonic energy.

16. A suspension of particles of a two-dimensional inorganic compound in an aqueous medium comprising at least one polycyclic aromatic compound; wherein the or each polycyclic aromatic compound independently has a ring system which comprises from 2 to 6 fused benzene rings, the ring system being substituted with from 1 to 4 hydrophilic groups each independently consisting of less than 20 atoms.

17. A suspension of claim 16 , wherein the suspension has been made by a method comprising:
a) providing multilayered particles of the inorganic compound in an aqueous medium which comprises at least one polycyclic aromatic compound, or a salt thereof; wherein the polycyclic aromatic compound is present in the aqueous medium in an amount from 1 ×10 −4 mol/L to 200 ×10 ×4 mol/L, wherein the or each polycyclic aromatic compound independently has a ring system which comprises from 2 to 10 fused benzene rings, the ring system being substituted with from 1 to 4 independently selected hydrophilic groups, each hydrophilic group consisting of less than 20 atoms;
b) subjecting the multilayered particles of the inorganic compound in the aqueous medium to energy to obtain a suspension;
c) when the suspension obtained in step b) also comprises multilayered particles of the inorganic compound, the method further comprises the step of reducing the amount of multilayered particles of the inorganic compound in the suspension to obtain an aqueous suspension comprising particles of the two-dimensional inorganic compound and the at least one polycyclic aromatic compound.

18. An electronic device, the device comprising at least one thin film layer which comprises a plurality of particles of a two-dimensional inorganic compound, wherein the or each thin film contains at least one polycyclic aromatic compound; wherein the or each polycyclic aromatic compound independently has a ring system which comprises from 2 to 6 fused benzene rings, the ring system being substituted with from 1 to 4 hydrophilic groups each independently consisting of less than 20 atoms.

19. A method of forming a thin film comprising a plurality of particles of a two-dimensional inorganic compound, the method comprising
a) obtaining an aqueous suspension of particles of a two-dimensional inorganic compound using the method of claim 1 ; and
b) depositing the suspension of particles of the two-dimensional inorganic compound in an aqueous medium onto a substrate to form the thin film comprising a plurality of particles of the two-dimensional inorganic compound.

Assignees

• Univ Manchester

Inventors

• Casiraghi Cinzia
• Yang Huafeng

Classifications

• C01P2004/24

  Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer · CPC title

• C01P2004/04

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

• C01P2002/82

  by IR- or Raman-data · CPC title

• C01G41/00

  Compounds of tungsten · CPC title

• C01G39/06

  Sulfides · CPC title