# US 2020/0399481 A1 · Pickering emulsions

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- Number: US 2020/0399481 A1
- Document ID: US20200399481A1
- Status: Published application
- Kind: A1
- Application number: 16/960,705
- Filed: 2019-01-07
- Published: 2020-12-24
- Earliest claimed: 2018-01-08
- Assignees: The University of Sussex
- Applicants: The University of Sussex
- Inventors: Matthew James LARGE; Alan Brian DALTON; Sean Paul OGILVIE
- Web page: https://patentgrep.com/patent/US20200399481A1

## CPC

- C09D 11/023: Emulsion inks
- A61K 8/06: Emulsions
- A61K 8/19: containing inorganic ingredients
- A61Q 19/00: Preparations for care of the skin
- C01B 19/007: {Tellurides or selenides of metals (C01B19/002 takes precedence)}
- C01B 21/0648: {After-treatment, e.g. grinding, purification (transformation of hexagonal into cubic or wurtzitic boron nitride C04B35/5831)}
- C01B 32/19: by exfoliation
- C01B 32/194: After-treatment
- C01G 39/06: Sulfides
- C01G 41/00: Compounds of tungsten
- C09D 11/033: characterised by the solvent
- C09D 11/037: characterised by the pigment
- C09D 11/101: Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
- C09D 11/322: Pigment inks
- C09D 11/36: based on non-aqueous solvents
- C09D 11/52: Electrically conductive inks
- G01B 7/18: {using change in resistance}
- G01B 13/24: for measuring the deformation in a solid
- G01L 1/20: by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids (of piezo-resistive materials G01L1/18); by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- A61K 2800/10: General cosmetic use
- C01B 2204/22: Electronic properties
- C01B 2204/28: Solid content in solvents
- C01P 2004/02: obtained by optical microscopy
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- A61Q: SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- G01B: MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01L: MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE (weighing G01G)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present invention relates to a method for making a Pickering emulsion, the method comprising: exfoliating a non-silicate layered 3D material in a solvent to produce particles of a non-silicate unfunctionalised 2D material; forming a dispersion of the particles of the 2D material in a first liquid phase; adding a second liquid phase; and homogenising the dispersion of the 2D material in the first liquid phase with the second liquid phase to form a Pickering emulsion comprising the first liquid phase, the second liquid phase, and the particles of the 2D material.

## Claims

### Claim 1

A method for making a Pickering emulsion, the method comprising:
(a) exfoliating a non-silicate layered 3D material in a solvent to produce particles of a non-silicate unfunctionalised 2D material;
(b) forming a dispersion of the particles of the 2D material in a first liquid phase;
(c) adding a second liquid phase and homogenising the dispersion of the 2D material in the first liquid phase with the second liquid phase to form a Pickering emulsion comprising the first liquid phase, the second liquid phase, and the particles of the 2D material.

### Claim 2 (depends on 1)

The method of claim 1, wherein the unfunctionalised 2D material is selected from graphene, borophene, germanene, silicene, stanene, phosphorene, bismuthene, hexagonal boron nitride, MXenes, 2D perovskites and transition metal dichalcogenides.

### Claim 3 (depends on 1, 2)

The method of claim 1 or 2, wherein the solvent used in step (a) is different to the first liquid phase, and wherein step (b) comprises:
(b) removing at least some of the solvent and then adding a first liquid phase to form a dispersion of the particles of the 2D material in the first liquid phase.

### Claim 4

The method of any preceding claim, wherein the solvent is selected from N-methyl-2-pyrrolidone, N-cyclohexyl-2-pyrrolidone, 1,3-dimethyl-2-imidazolidinone, N-ethyl-2-pyrrolidone, isopropanol, acetone, cyclopentanone and cyclohexanone, or a mixture of water and a surfactant.

### Claim 5

The method of any preceding claim, wherein the magnitude of the difference between the surface tension of the first liquid phase and the surface tension of the 2D material is within 30 mN/m of the magnitude of the difference between the surface tension of the second liquid phase and the surface tension of the 2D material.

### Claim 6

The method of any preceding claim, wherein one of the first and second liquid phases has a surface tension which is from about 5 to about 35 mN/m higher than the surface tension of the 2D material, whilst the other liquid phase has a surface tension which is from about 5 to about 35 mN/m lower than the surface tension of the 2D material.

### Claim 7

The method of any preceding claim, wherein the first liquid phase has a surface tension lower than that of the 2D material, and the second liquid phase has a surface tension higher than that of the 2D material.

### Claim 8

The method of any preceding claim, wherein the first liquid phase is selected from pentane, hexane, ethyl acetate, cyclohexane, chloroform, dichloromethane, methyl methacrylate, styrene, cyclopentanone, or combinations thereof.

### Claim 9

The method of any preceding claim, wherein the second liquid phase is selected from glycerol, water, formamide, diethylene glycol, ethylene glycol, propylene glycol or combinations thereof.

### Claim 10

The method of any preceding claim, wherein the particles of 2D material are from 1 to 5 nm thick, and have an average length of from about 50 nm to about 2000 nm.

### Claim 11

The method of any preceding claim, wherein the 2D material is graphene, hexagonal boron nitride, phosphorene or a transition metal dichalcogenide, preferably graphene.

### Claim 12

The method of any preceding claim, wherein the mixture is homogenized in step (c) by applying high shear forces, ultrasonic mixing, or by the use of a microfluidizer.

### Claim 13

The method of any preceding claim, wherein step (c) comprises:
(c) adding a second liquid phase and homogenising the dispersion of the 2D material in the first liquid phase with the second liquid phase with a microfluidizer to form a Pickering emulsion comprising the first liquid phase, the second liquid phase, and the 2D material, where the average diameter of droplets of the dispersed phase within the emulsion is about 10 μm or less.

### Claim 14

The method of any preceding claim, further comprising the step of forming a solid structure from the Pickering emulsion.

### Claim 15 (depends on 14)

The method of claim 14, wherein one or both of the liquid phases comprises monomers and a reaction initiator, and wherein the step of forming a solid structure from the Pickering emulsion comprises polymerising the monomers.

### Claim 16 (depends on 15)

The method of claim 15, wherein the monomers comprise styrene, methyl methacrylate, methacrylic acid, acrylic acid, butyl acrylate, a mixture of styrene and butadiene, or a mixture of acrylonitrile and butadiene.

### Claim 17 (depends on 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13)

A Pickering emulsion formed by the method of any of claims 1-13.

### Claim 18

A Pickering emulsion stabilised by a non-silicate unfunctionalised 2D material, wherein the 2D material is not graphene or boron nitride.

### Claim 19

A Pickering emulsion stabilised by a non-silicate unfunctionalised 2D material, wherein the emulsion comprises a continuous liquid phase and a dispersed liquid phase, wherein the dispersed liquid phase is in the form of droplets having an average diameter of about 50 μm or less.

### Claim 20

A Pickering emulsion stabilised by a non-silicate unfunctionalised 2D material, wherein the emulsion comprises a continuous liquid phase and a dispersed liquid phase, and wherein the amount of 2D material present in the emulsion is from about 0.0001 to about 1 vol. %, based on the volume of the dispersed phase.

### Claim 21

A liquid strain sensor comprising a Pickering emulsion stabilised by a non-silicate unfunctionalised 2D material, wherein the 2D material is electrically conductive.

### Claim 22

Use of a Pickering emulsion stabilised by a non-silicate unfunctionalised 2D material in a strain sensor, wherein the 2D material is electrically conductive.

### Claim 23

Use of a Pickering emulsion stabilised by a non-silicate unfunctionalised 2D material as an ink.

### Claim 24 (depends on 23)

A use according to claim 23, wherein the 2D material is electrically conductive or thermally conductive, or is a semiconductor.

### Claim 25

A method of printing, comprising applying an ink comprising a Pickering emulsion stabilised by a non-silicate unfunctionalised 2D material to a substrate, and drying the substrate.

### Claim 26 (depends on 19, 20, 21, 22, 23, 24, 25)

A Pickering emulsion according to claim 19 or 20, a liquid strain sensor according to claim 21, a use according to any of claims 22-24, or a method according to claim 25, wherein the 2D material is graphene.