# US 9,752,035 B2 · Composite lubricating material, engine oil, grease, and lubricant, and method of producing a composite lubricating material

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- Number: US 9,752,035 B2
- Document ID: US9752035B2
- Status: Granted
- Kind: B2
- Application number: 14/764,929
- Filed: 2015-03-23
- Published: 2017-06-22
- Granted: 2017-09-05
- Earliest claimed: 2014-09-09
- Assignees: Graphene Platform Corporation
- Applicants: Graphene Platform Corporation
- Inventors: Shoji Hasegawa; Nagisa Kamiya
- Web page: https://patentgrep.com/patent/US9752035B2

## CPC

- C01B 32/19: by exfoliation
- C01B 32/194: After-treatment
- C01B 32/20: Graphite
- C01B 32/205: Preparation
- C01B 32/21: After-treatment
- C01B 32/225: Expansion; Exfoliation
- C04B 14/024: {Graphite}
- C04B 28/14: containing calcium sulfate cements {(gypsum-paper plates E04C)}
- C04B 35/5611: {based on titanium carbides}
- C04B 35/6303: {Inorganic additives}
- C04B 35/83: Carbon fibres in a carbon matrix
- C08J 5/042: {with carbon fibres}
- C08K 3/04: Carbon
- C08K 7/00: Use of ingredients characterised by shape
- C08K 7/14: Glass
- C08L 23/10: Homopolymers or copolymers of propene
- C08L 31/04: Homopolymers or copolymers of vinyl acetate
- C08L 51/06: grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
- C08L 77/06: Polyamides derived from polyamines and polycarboxylic acids (C08L77/10 takes precedence)
- C08L 101/00: Compositions of unspecified macromolecular compounds
- C09C 1/46: Graphite {(C09C1/0015 takes precedence)}
- C09C 3/04: Physical treatment, e.g. grinding or treatment with ultrasonic vibrations {(C09C3/006 takes precedence)}
- C09D 5/24: Electrically-conducting paints {(conductive materials H01B1/00)}
- C09D 7/61: inorganic
- C09D 11/03: characterised by features other than the chemical nature of the binder
- C09D 11/037: characterised by the pigment
- C09D 11/52: Electrically conductive inks
- C10M 125/02: Carbon; Graphite
- C10M 169/04: Mixtures of base-materials and additives
- H01G 11/32: Carbon-based
- H01G 11/36: Nanostructures, e.g. nanofibres, nanotubes or fullerenes
- H01G 11/38: Carbon pastes or blends; Binders or additives therein
- H01G 11/86: specially adapted for electrodes (carbonisation or activation of carbon for the manufacture of electrodes H01G11/34)
- H01M 4/02: Electrodes composed of, or comprising, active material
- H01M 4/366: {as layered products}
- H01M 4/583: Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M 4/587: for inserting or intercalating light metals
- H01M 4/625: {Carbon or graphite}
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/74: by peak-intensities or a ratio thereof only
- C01P 2002/77: by unit-cell parameters, atom positions or structure diagrams
- C01P 2004/54: Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C04B 2235/425: Graphite
- C08K 2201/001: Conductive additives
- C08K 2201/005: Additives being defined by their particle size in general
- C10M 2201/041: Carbon; Graphite; Carbon black
- C10M 2203/003: used as base material
- C10M 2203/022: saturated
- C10M 2207/401: used as base material
- C10N 2030/10: Inhibition of oxidation, e.g. anti-oxidants
- C10N 2040/25: Internal-combustion engines
- C10N 2050/10: semi-solid; greasy
- H01M 4/133: Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M 4/1393: of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M 4/362: {Composites}
- H01M 10/052: Li-accumulators
- H01M 2004/021: {Physical characteristics, e.g. porosity, surface area}
- Y02E 60/10: Energy storage using batteries
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS}
- 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)
- C10M: LUBRICATING COMPOSITIONS (well drilling compositions C09K8/02); USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION (mould release, i.e. separating, agents for metals B22C3/00, for plastics or substances in a plastic state, in general B29C33/56, for glass C03B40/02; textile lubricating compositions D06M11/00, D06M13/00, D06M15/00; immersion oils for microscopy G02B21/33)
- H01G: CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE (selection of specified materials as dielectric H01B3/00; capacitors having potential barriers H10D1/62, H10K10/10)
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C10N: INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A composite lubricating material include at least a graphite-based carbon material and/or graphene-like graphite exfoliated from the graphite-based carbon material dispersed in a base material. The graphite-based carbon material is characterized by having a rhombohedral graphite layer (3R) and a hexagonal graphite layer (2H), wherein a Rate (3R) of the rhombohedral graphite layer (3R) and the hexagonal graphite layer (2H), based on an X-ray diffraction method, which is defined by following Equation 1 is 31% or more: Rate (3R)=P3/(P3+P4)×100 . . . Equation 1, wherein, P3 is a peak intensity of a (101) plane of the rhombohedral graphite layer (3R) based on the X-ray diffraction method, and P4 is a peak intensity of a (101) plane of the hexagonal graphite layer (2H) based on the X-ray diffraction method.

## Claims

### Claim 1

A composite lubricating material comprising at least a graphene exfoliated from a graphite-based carbon material dispersed in a base oil,
the graphite-based carbon material having a rhombohedral graphite layer (3R) and a hexagonal graphite layer (2H), wherein a Rate (3R) of the rhombohedral graphite layer (3R) and the hexagonal graphite layer (2H), based on an X-ray diffraction method, which is defined by following Equation 1 is 31% or more:
Rate(3R)=P3/(P3+P4)×100 Equation 1
wherein
P3 is a peak intensity of a (101) plane of the rhombohedral graphite layer (3R) based on the X-ray diffraction method, and
P4 is a peak intensity of a (101) plane of the hexagonal graphite layer (2H) based on the X-ray diffraction method,
the graphene being a crystal of a mean size of 100 nm or more and formed in a flake-like or sheet-like shape having 10 layers or less.

### Claim 2 (depends on 1)

The composite lubricating material according to claim 1, wherein a weight ratio of the graphite-based carbon material to the base material is 1/10,000 or more to less than 1.

### Claim 3 (depends on 1)

The composite lubricating material according to claim 1, wherein the base oil is derived from mineral, synthetic chemicals, plants or animals.

### Claim 4 (depends on 1)

The composite lubricating material according to claim 1, comprising one or more kinds of additives for a purpose of preventing oxidative deterioration.

### Claim 5 (depends on 4)

The composite lubricating material according to claim 4, wherein the additive is a radioactive substance.

### Claim 6 (depends on 1)

Engine oil comprising the composite lubricating material according to claim 1.

### Claim 7 (depends on 1)

Grease comprising the composite lubricating material according to claim 1.
