CN108987709A - A kind of graphene-based negative electrode material of lithium battery and preparation method thereof - Google Patents
A kind of graphene-based negative electrode material of lithium battery and preparation method thereof Download PDFInfo
- Publication number
- CN108987709A CN108987709A CN201810795328.5A CN201810795328A CN108987709A CN 108987709 A CN108987709 A CN 108987709A CN 201810795328 A CN201810795328 A CN 201810795328A CN 108987709 A CN108987709 A CN 108987709A
- Authority
- CN
- China
- Prior art keywords
- parts
- negative electrode
- graphene
- electrode material
- lithium battery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses graphene-based negative electrode material of a kind of lithium battery and preparation method thereof, the graphene-based negative electrode material of lithium battery therein includes the raw material of following parts by weight: 22-26 parts of coal tar pitch, 28-32 parts of asphalt, 25-29 parts of coal tar, 21-25 parts of Heavy aromatic hydrocarbon, 18-22 parts of mink cell focus, 3-7 parts of aluminium isopropoxide, 1-5 parts of oxalic acid aluminium, 4-8 parts of ferrous oxalate, 2-6 parts of cyclopentadienyl group dicarbapentaborane iron, 1-5 parts of nickel sulfamic acid, 2-6 parts of citric acid three-iron, 21-25 parts of graphene oxide.The present invention has rational design, and the preparation process of negative electrode material is simple, it is easy to accomplish scale, industrialization production; graphite oxide alkenyl negative electrode material capacitance obtained is high; power generation performance is excellent, improves the comprehensive performance of negative electrode material, the electrode material suitable for various batteries.
Description
Technical field
The present invention relates to li-ion electrode materials preparation technical field more particularly to a kind of graphene-based cathode materials of lithium battery
Material and preparation method thereof.
Background technique
One of key technology of lithium ion battery is the selection and research of negative electrode material, and the quality of negative electrode material
Directly affect the chemical property of battery.Currently, carbon material has become commercialized lithium ion battery negative material.Wherein, day
Right graphite has many advantages, such as height ratio capacity, low price, but in the presence of irreversible capacity is larger, cycle performance is poor, unsuitable for the first time
The defects of high rate charge-discharge；The structural stability of artificial graphite is high, and embedding lithium function admirable has extended cycle life, pole piece processability
Can be good, obtain extensive affirmative and use in the industry.Graphene is a kind of new material of individual layer laminated structure being made of carbon atom.
It is a kind of flat film that hexangle type is formed in honeycomb lattice with sp2 hybridized orbit by carbon atom, only one carbon atom thickness
Two-dimensional material.Graphene oxide thin slice is product of the powdered graphite after chemical oxidation and removing, and graphene oxide is single
Atomic layer, some tens of pm can be expanded on lateral dimension at any time.
Through retrieving, application No. is 201710879991.9 patent document, to disclose a kind of graphene-based lithium ion battery negative
Pole material and preparation method thereof, the negative electrode material are combined by foam copper, graphene and Co-Cu-Zn-ZIF, the foam
Copper is braced frame, and in the braced frame, the Co-Cu-Zn-ZIF is modified in graphene table the graphene modified
Face and exposed foam copper surface.Preparation method is as follows: 1) pretreatment of foam copper；2) preparation of Co-Zn-ZIF；3)
The preparation of Co-Cu-Zn-ZIF；4) preparation of Co-Cu-Zn-ZIF/RGO/ foam carbon/carbon-copper composite material；5) calcination processing.The preparation
The theoretical capacity of cell negative electrode material made from method is big, and has hollow nanostructures, and lithium ion battery can be effectively relieved
Volumetric expansion in charge and discharge process and the distance for shortening lithium ion diffusion can be directly used as adhesive-free and conductive agent
Electrode simplifies technology for preparing electrode, and the lithium ion battery reversible specific capacity being prepared by it is high, high rate performance is excellent, follows
Ring has good stability, and coulombic efficiency still can keep nearly 100% after multiple cycle charge-discharge.
But the preparation method of existing lithium cell cathode material is mostly more complicated, is not suitable for the scale with negative electrode material
Metaplasia produces, therefore we have proposed graphene-based negative electrode materials of a kind of lithium battery and preparation method thereof for solving the above problems.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of graphene-based negative electrode material of lithium battery and its
Preparation method.
The graphene-based negative electrode material of a kind of lithium battery proposed by the present invention, the raw material including following parts by weight: coal tar pitch 22-
26 parts, 28-32 parts of asphalt, 25-29 parts of coal tar, 21-25 parts of Heavy aromatic hydrocarbon, 18-22 parts of mink cell focus, aluminium isopropoxide 3-
7 parts, 1-5 parts of oxalic acid aluminium, 4-8 parts of ferrous oxalate, 2-6 parts of cyclopentadienyl group dicarbapentaborane iron, 1-5 parts of nickel sulfamic acid, lemon
Sour three-iron 2-6 parts, 21-25 parts of graphene oxide.
Preferably, the raw material including following parts by weight: 23-25 parts of coal tar pitch, 29-31 parts of asphalt, coal tar 26-28
Part, 22-24 parts of Heavy aromatic hydrocarbon, 19-21 parts of mink cell focus, 4-6 parts of aluminium isopropoxide, 2-4 parts of oxalic acid aluminium, 5-7 parts of ferrous oxalate,
3-5 parts of cyclopentadienyl group dicarbapentaborane iron, 2-4 parts of nickel sulfamic acid, 3-5 parts of citric acid three-iron, 22-24 parts of graphene oxide.
Preferably, the raw material including following parts by weight: 24 parts of coal tar pitch, 30 parts of asphalt, 27 parts of coal tar, heavy virtue
23 parts of fragrant hydrocarbon, 20 parts of mink cell focus, 5 parts of aluminium isopropoxide, 5 parts of oxalic acid aluminium, 6 parts of ferrous oxalate, cyclopentadienyl group dicarbapentaborane iron 4
Part, 3 parts of nickel sulfamic acid, 4 parts of citric acid three-iron, 23 parts of graphene oxide.
The invention also provides a kind of preparation methods of the graphene-based negative electrode material of lithium battery, comprising the following steps:
S1: material prepares: raw material, catalyst and graphene oxide are successively weighed by weight, it is spare；
S2: raw material mixing: raw material described in S1, catalyst and graphene oxide are launched to carrying out in reaction vessel and to anti-
It answers and solvent is added in solution, obtain solidliquid mixture；
S3: stirring: carrying out ultrasonic agitation mixing to solidliquid mixture described in S2, and mixing material is made；
S4: it increases temperature: the reaction temperature of mixing material described in S3 being increased to 380 DEG C -500 DEG C, in 10-100Mpa item
Constant temperature keeps 2h-15h to carry out thermal polycondensation reaction under part, and reaction mixing mother liquor is made；
S5: it prepares mesophasespherule: washing oil is added into the mother liquor of reaction mixing described in S4, and successively it is stirred
It mixes, wash, be centrifugated, mesophasespherule is made；
S6: charing: heating treatment is carried out to mesophasespherule described in S5, and constant temperature keeps 2h-12h, and interphase is made
Carbon microspheres；
S7: separation: the dispensing of mesocarbon microspheres described in S6 is subjected to dipping doping treatment into maceration extract, and to successively right
It is centrifuged, washs, and wet feed is made；
S8: low-temperature sintering: wet feed described in S7 is subjected to low-temperature sintering, and constant temperature keeps 2h-24h, and graphene oxide is made
Base negative electrode material.
Preferably, in the S1, when weighing to raw material and catalyst, choose an electronic balance, by raw material and
Catalyst is placed on electronic balance and is weighed.
Preferably, in the S2, solvent is deionized water or ethyl alcohol.
Preferably, in the S4, when improving the reaction temperature of mixing material, the heating rate of mixing material is 1 DEG C/
min-10℃/min。
Preferably, in the S5, when being washed to reaction mixing mother liquor, wash time 2h-6h.
Preferably, in the S6, when heating up to mesophasespherule, temperature is increased to 500 DEG C -1100 DEG C.
Preferably, in the S8, when carrying out low-temperature sintering to wet feed, sintering temperature is 100 DEG C -300 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
Selected from coal tar pitch and petroleum asphalt, coal tar and Heavy aromatic hydrocarbon in the preparation process of the graphene-based negative electrode material of the lithium battery
Raw material is prepared for negative electrode material, wherein mink cell focus, aluminium isopropoxide, oxalic acid aluminium, ferrous oxalate, cyclopentadienyl group dicarbapentaborane
Iron, nickel sulfamic acid, citric acid three-iron are catalyst；
By the way that raw material in high temperature (380 DEG C -500 DEG C), high pressure (10-100Mpa), and is carried out pyrocondensation under the effect of the catalyst
Poly- reaction, can be made the reaction mixing mother liquor containing mesophasespherule, be washed in washing oil by that will react mixing mother liquor
And after separating treatment, mesocarbon microspheres can be made, after carrying out dipping doping and low-temperature sintering to mesocarbon microspheres
Graphene-based negative electrode material can be made；
Charge-discharge performance, capacitance can be improved using the graphene oxide with porous structure, can also be the transmission of ion
More diffusion admittances are provided, graphite oxide alkenyl negative electrode material can be used as lithium ion battery, sodium-ion battery and super electricity
The electrode material of container etc.；
The present invention has rational design, and the preparation process of negative electrode material is simple, it is easy to accomplish scale, industrialization production, oxygen obtained
Fossil mertenyl negative electrode material capacitance is high, and power generation performance is excellent, improves the comprehensive performance of negative electrode material, is suitable for various electricity
The electrode material in pond.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment one
A kind of graphene-based negative electrode material of lithium battery, the raw material including following parts by weight: coal tar pitch 22 are proposed in the present embodiment
Part, 28 parts of asphalt, 25 parts of coal tar, 21 parts of Heavy aromatic hydrocarbon, 18 parts of mink cell focus, 3 parts of aluminium isopropoxide, 1 part of oxalic acid aluminium,
4 parts of ferrous oxalate, 2 parts of cyclopentadienyl group dicarbapentaborane iron, 1 part of nickel sulfamic acid, 2 parts of citric acid three-iron, 21 parts of graphene oxide.
The present embodiment also proposed a kind of preparation method of graphene-based negative electrode material of lithium battery, comprising the following steps:
S1: material prepares: raw material, catalyst and graphene oxide are successively weighed by weight, it is spare；
S2: raw material mixing: raw material described in S1, catalyst and graphene oxide are launched to carrying out in reaction vessel and to anti-
It answers and solvent is added in solution, obtain solidliquid mixture；
S3: stirring: carrying out ultrasonic agitation mixing to solidliquid mixture described in S2, and mixing material is made；
S4: it increases temperature: the reaction temperature of mixing material described in S3 being increased to 380 DEG C -500 DEG C, in 10-100Mpa item
Constant temperature keeps 2h-15h to carry out thermal polycondensation reaction under part, and reaction mixing mother liquor is made；
S5: it prepares mesophasespherule: washing oil is added into the mother liquor of reaction mixing described in S4, and successively it is stirred
It mixes, wash, be centrifugated, mesophasespherule is made；
S6: charing: heating treatment is carried out to mesophasespherule described in S5, and constant temperature keeps 2h-12h, and interphase is made
Carbon microspheres；
S7: separation: the dispensing of mesocarbon microspheres described in S6 is subjected to dipping doping treatment into maceration extract, and to successively right
It is centrifuged, washs, and wet feed is made；
S8: low-temperature sintering: wet feed described in S7 is subjected to low-temperature sintering, and constant temperature keeps 2h-24h, and graphene oxide is made
Base negative electrode material.
In the present embodiment, in S1, when weighing to raw material and catalyst, choose an electronic balance, by raw material and
Catalyst is placed on electronic balance and is weighed, and in S2, solvent is deionized water or ethyl alcohol, in S4, is improving mixing material
Reaction temperature when, the heating rate of mixing material is 1 DEG C/min-10 DEG C/min, in S5, is washed to reaction mixing mother liquor
When washing, in wash time 2h-6h, S6, when heating up to mesophasespherule, temperature is increased to 500 DEG C -1100 DEG C,
In S8, when carrying out low-temperature sintering to wet feed, sintering temperature is 100 DEG C -300 DEG C.
Embodiment two
A kind of graphene-based negative electrode material of lithium battery, the raw material including following parts by weight: coal tar pitch 23 are proposed in the present embodiment
Part, 29 parts of asphalt, 26 parts of coal tar, 22 parts of Heavy aromatic hydrocarbon, 19 parts of mink cell focus, 4 parts of aluminium isopropoxide, 2 parts of oxalic acid aluminium,
5 parts of ferrous oxalate, 3 parts of cyclopentadienyl group dicarbapentaborane iron, 2 parts of nickel sulfamic acid, 3 parts of citric acid three-iron, graphene oxide 22.
The present embodiment also proposed a kind of preparation method of graphene-based negative electrode material of lithium battery, comprising the following steps:
S1: material prepares: raw material, catalyst and graphene oxide are successively weighed by weight, it is spare；
S2: raw material mixing: raw material described in S1, catalyst and graphene oxide are launched to carrying out in reaction vessel and to anti-
It answers and solvent is added in solution, obtain solidliquid mixture；
S3: stirring: carrying out ultrasonic agitation mixing to solidliquid mixture described in S2, and mixing material is made；
S4: it increases temperature: the reaction temperature of mixing material described in S3 being increased to 380 DEG C -500 DEG C, in 10-100Mpa item
Constant temperature keeps 2h-15h to carry out thermal polycondensation reaction under part, and reaction mixing mother liquor is made；
S5: it prepares mesophasespherule: washing oil is added into the mother liquor of reaction mixing described in S4, and successively it is stirred
It mixes, wash, be centrifugated, mesophasespherule is made；
S6: charing: heating treatment is carried out to mesophasespherule described in S5, and constant temperature keeps 2h-12h, and interphase is made
Carbon microspheres；
S7: separation: the dispensing of mesocarbon microspheres described in S6 is subjected to dipping doping treatment into maceration extract, and to successively right
It is centrifuged, washs, and wet feed is made；
S8: low-temperature sintering: wet feed described in S7 is subjected to low-temperature sintering, and constant temperature keeps 2h-24h, and graphene oxide is made
Base negative electrode material.
In the present embodiment, in S1, when weighing to raw material and catalyst, choose an electronic balance, by raw material and
Catalyst is placed on electronic balance and is weighed, and in S2, solvent is deionized water or ethyl alcohol, in S4, is improving mixing material
Reaction temperature when, the heating rate of mixing material is 1 DEG C/min-10 DEG C/min, in S5, is washed to reaction mixing mother liquor
When washing, in wash time 2h-6h, S6, when heating up to mesophasespherule, temperature is increased to 500 DEG C -1100 DEG C,
In S8, when carrying out low-temperature sintering to wet feed, sintering temperature is 100 DEG C -300 DEG C.
Embodiment three
A kind of graphene-based negative electrode material of lithium battery, the raw material including following parts by weight: coal tar pitch 24 are proposed in the present embodiment
Part, 30 parts of asphalt, 27 parts of coal tar, 23 parts of Heavy aromatic hydrocarbon, 20 parts of mink cell focus, 5 parts of aluminium isopropoxide, 5 parts of oxalic acid aluminium,
6 parts of ferrous oxalate, 4 parts of cyclopentadienyl group dicarbapentaborane iron, 3 parts of nickel sulfamic acid, 4 parts of citric acid three-iron, 23 parts of graphene oxide.
The present embodiment also proposed a kind of preparation method of graphene-based negative electrode material of lithium battery, comprising the following steps:
S1: material prepares: raw material, catalyst and graphene oxide are successively weighed by weight, it is spare；
S2: raw material mixing: raw material described in S1, catalyst and graphene oxide are launched to carrying out in reaction vessel and to anti-
It answers and solvent is added in solution, obtain solidliquid mixture；
S3: stirring: carrying out ultrasonic agitation mixing to solidliquid mixture described in S2, and mixing material is made；
S4: it increases temperature: the reaction temperature of mixing material described in S3 being increased to 380 DEG C -500 DEG C, in 10-100Mpa item
Constant temperature keeps 2h-15h to carry out thermal polycondensation reaction under part, and reaction mixing mother liquor is made；
S5: it prepares mesophasespherule: washing oil is added into the mother liquor of reaction mixing described in S4, and successively it is stirred
It mixes, wash, be centrifugated, mesophasespherule is made；
S6: charing: heating treatment is carried out to mesophasespherule described in S5, and constant temperature keeps 2h-12h, and interphase is made
Carbon microspheres；
S7: separation: the dispensing of mesocarbon microspheres described in S6 is subjected to dipping doping treatment into maceration extract, and to successively right
It is centrifuged, washs, and wet feed is made；
S8: low-temperature sintering: wet feed described in S7 is subjected to low-temperature sintering, and constant temperature keeps 2h-24h, and graphene oxide is made
Base negative electrode material.
In the present embodiment, in S1, when weighing to raw material and catalyst, choose an electronic balance, by raw material and
Catalyst is placed on electronic balance and is weighed, and in S2, solvent is deionized water or ethyl alcohol, in S4, is improving mixing material
Reaction temperature when, the heating rate of mixing material is 1 DEG C/min-10 DEG C/min, in S5, is washed to reaction mixing mother liquor
When washing, in wash time 2h-6h, S6, when heating up to mesophasespherule, temperature is increased to 500 DEG C -1100 DEG C,
In S8, when carrying out low-temperature sintering to wet feed, sintering temperature is 100 DEG C -300 DEG C.
Example IV
A kind of graphene-based negative electrode material of lithium battery, the raw material including following parts by weight: coal tar pitch 25 are proposed in the present embodiment
Part, 31 parts of asphalt, 28 parts of coal tar, 24 parts of Heavy aromatic hydrocarbon, 21 parts of mink cell focus, 6 parts of aluminium isopropoxide, 6 parts of oxalic acid aluminium,
7 parts of ferrous oxalate, 5 parts of cyclopentadienyl group dicarbapentaborane iron, 4 parts of nickel sulfamic acid, 5 parts of citric acid three-iron, 24 parts of graphene oxide.
The present embodiment also proposed a kind of preparation method of graphene-based negative electrode material of lithium battery, comprising the following steps:
S1: material prepares: raw material, catalyst and graphene oxide are successively weighed by weight, it is spare；
S2: raw material mixing: raw material described in S1, catalyst and graphene oxide are launched to carrying out in reaction vessel and to anti-
It answers and solvent is added in solution, obtain solidliquid mixture；
S3: stirring: carrying out ultrasonic agitation mixing to solidliquid mixture described in S2, and mixing material is made；
S4: it increases temperature: the reaction temperature of mixing material described in S3 being increased to 380 DEG C -500 DEG C, in 10-100Mpa item
Constant temperature keeps 2h-15h to carry out thermal polycondensation reaction under part, and reaction mixing mother liquor is made；
S5: it prepares mesophasespherule: washing oil is added into the mother liquor of reaction mixing described in S4, and successively it is stirred
It mixes, wash, be centrifugated, mesophasespherule is made；
S6: charing: heating treatment is carried out to mesophasespherule described in S5, and constant temperature keeps 2h-12h, and interphase is made
Carbon microspheres；
S7: separation: the dispensing of mesocarbon microspheres described in S6 is subjected to dipping doping treatment into maceration extract, and to successively right
It is centrifuged, washs, and wet feed is made；
S8: low-temperature sintering: wet feed described in S7 is subjected to low-temperature sintering, and constant temperature keeps 2h-24h, and graphene oxide is made
Base negative electrode material.
In the present embodiment, in S1, when weighing to raw material and catalyst, choose an electronic balance, by raw material and
Catalyst is placed on electronic balance and is weighed, and in S2, solvent is deionized water or ethyl alcohol, in S4, is improving mixing material
Reaction temperature when, the heating rate of mixing material is 1 DEG C/min-10 DEG C/min, in S5, is washed to reaction mixing mother liquor
When washing, in wash time 2h-6h, S6, when heating up to mesophasespherule, temperature is increased to 500 DEG C -1100 DEG C,
In S8, when carrying out low-temperature sintering to wet feed, sintering temperature is 100 DEG C -300 DEG C.
Embodiment five
A kind of graphene-based negative electrode material of lithium battery, the raw material including following parts by weight: coal tar pitch 26 are proposed in the present embodiment
Part, 32 parts of asphalt, 29 parts of coal tar, 25 parts of Heavy aromatic hydrocarbon, 22 parts of mink cell focus, 7 parts of aluminium isopropoxide, 5 parts of oxalic acid aluminium,
8 parts of ferrous oxalate, 6 parts of cyclopentadienyl group dicarbapentaborane iron, 5 parts of nickel sulfamic acid, 6 parts of citric acid three-iron, 25 parts of graphene oxide.
The present embodiment also proposed a kind of preparation method of graphene-based negative electrode material of lithium battery, comprising the following steps:
S1: material prepares: raw material, catalyst and graphene oxide are successively weighed by weight, it is spare；
S2: raw material mixing: raw material described in S1, catalyst and graphene oxide are launched to carrying out in reaction vessel and to anti-
It answers and solvent is added in solution, obtain solidliquid mixture；
S3: stirring: carrying out ultrasonic agitation mixing to solidliquid mixture described in S2, and mixing material is made；
S4: it increases temperature: the reaction temperature of mixing material described in S3 being increased to 380 DEG C -500 DEG C, in 10-100Mpa item
Constant temperature keeps 2h-15h to carry out thermal polycondensation reaction under part, and reaction mixing mother liquor is made；
S5: it prepares mesophasespherule: washing oil is added into the mother liquor of reaction mixing described in S4, and successively it is stirred
It mixes, wash, be centrifugated, mesophasespherule is made；
S6: charing: heating treatment is carried out to mesophasespherule described in S5, and constant temperature keeps 2h-12h, and interphase is made
Carbon microspheres；
S7: separation: the dispensing of mesocarbon microspheres described in S6 is subjected to dipping doping treatment into maceration extract, and to successively right
It is centrifuged, washs, and wet feed is made；
S8: low-temperature sintering: wet feed described in S7 is subjected to low-temperature sintering, and constant temperature keeps 2h-24h, and graphene oxide is made
Base negative electrode material.
In the present embodiment, in S1, when weighing to raw material and catalyst, choose an electronic balance, by raw material and
Catalyst is placed on electronic balance and is weighed, and in S2, solvent is deionized water or ethyl alcohol, in S4, is improving mixing material
Reaction temperature when, the heating rate of mixing material is 1 DEG C/min-10 DEG C/min, in S5, is washed to reaction mixing mother liquor
When washing, in wash time 2h-6h, S6, when heating up to mesophasespherule, temperature is increased to 500 DEG C -1100 DEG C,
In S8, when carrying out low-temperature sintering to wet feed, sintering temperature is 100 DEG C -300 DEG C.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of graphene-based negative electrode material of lithium battery, which is characterized in that the raw material including following parts by weight: coal tar pitch 22-26
Part, 28-32 parts of asphalt, 25-29 parts of coal tar, 21-25 parts of Heavy aromatic hydrocarbon, 18-22 parts of mink cell focus, aluminium isopropoxide 3-7
Part, 1-5 parts of oxalic acid aluminium, 4-8 parts of ferrous oxalate, 2-6 parts of cyclopentadienyl group dicarbapentaborane iron, 1-5 parts of nickel sulfamic acid, citric acid
2-6 parts of three-iron, 21-25 parts of graphene oxide.
2. the graphene-based negative electrode material of a kind of lithium battery according to claim 1, which is characterized in that including following parts by weight
Raw material: 23-25 parts of coal tar pitch, 29-31 parts of asphalt, 26-28 parts of coal tar, 22-24 parts of Heavy aromatic hydrocarbon, mink cell focus
19-21 parts, 4-6 parts of aluminium isopropoxide, 2-4 parts of oxalic acid aluminium, 5-7 parts of ferrous oxalate, 3-5 parts of cyclopentadienyl group dicarbapentaborane iron, ammonia
2-4 parts of base nickel sulphonic acid, 3-5 parts of citric acid three-iron, 22-24 parts of graphene oxide.
3. the graphene-based negative electrode material of a kind of lithium battery according to claim 1, which is characterized in that including following parts by weight
Raw material: 24 parts of coal tar pitch, 30 parts of asphalt, 27 parts of coal tar, 23 parts of Heavy aromatic hydrocarbon, 20 parts of mink cell focus, aluminium isopropoxide 5
Part, 5 parts of oxalic acid aluminium, 6 parts of ferrous oxalate, 4 parts of cyclopentadienyl group dicarbapentaborane iron, 3 parts of nickel sulfamic acid, 4 parts of citric acid three-iron,
23 parts of graphene oxide.
4. a kind of preparation method of the graphene-based negative electrode material of lithium battery, which comprises the following steps:
S1: material prepares: raw material, catalyst and graphene oxide are successively weighed by weight, it is spare；
S2: raw material mixing: raw material described in S1, catalyst and graphene oxide are launched to carrying out in reaction vessel and to anti-
It answers and solvent is added in solution, obtain solidliquid mixture；
S3: stirring: carrying out ultrasonic agitation mixing to solidliquid mixture described in S2, and mixing material is made；
S4: it increases temperature: the reaction temperature of mixing material described in S3 being increased to 380 DEG C -500 DEG C, in 10-100Mpa item
Constant temperature keeps 2h-15h to carry out thermal polycondensation reaction under part, and reaction mixing mother liquor is made；
S5: it prepares mesophasespherule: washing oil is added into the mother liquor of reaction mixing described in S4, and successively it is stirred
It mixes, wash, be centrifugated, mesophasespherule is made；
S6: charing: heating treatment is carried out to mesophasespherule described in S5, and constant temperature keeps 2h-12h, and interphase is made
Carbon microspheres；
S7: separation: the dispensing of mesocarbon microspheres described in S6 is subjected to dipping doping treatment into maceration extract, and to successively right
It is centrifuged, washs, and wet feed is made；
S8: low-temperature sintering: wet feed described in S7 is subjected to low-temperature sintering, and constant temperature keeps 2h-24h, and graphene oxide is made
Base negative electrode material.
5. a kind of preparation method of the graphene-based negative electrode material of lithium battery according to claim 4, which is characterized in that described
In S1, when being weighed to raw material and catalyst, an electronic balance is chosen, raw material and catalyst are placed into electronic balance
On weighed.
6. a kind of preparation method of the graphene-based negative electrode material of lithium battery according to claim 4, which is characterized in that described
In S2, solvent is deionized water or ethyl alcohol.
7. a kind of preparation method of the graphene-based negative electrode material of lithium battery according to claim 4, which is characterized in that described
In S4, when improving the reaction temperature of mixing material, the heating rate of mixing material is 1 DEG C/min-10 DEG C/min.
8. a kind of preparation method of the graphene-based negative electrode material of lithium battery according to claim 4, which is characterized in that described
In S5, when being washed to reaction mixing mother liquor, wash time 2h-6h.
9. a kind of preparation method of the graphene-based negative electrode material of lithium battery according to claim 4, which is characterized in that described
In S6, when heating up to mesophasespherule, temperature is increased to 500 DEG C -1100 DEG C.
10. a kind of preparation method of the graphene-based negative electrode material of lithium battery according to claim 4, which is characterized in that institute
It states in S8, when carrying out low-temperature sintering to wet feed, sintering temperature is 100 DEG C -300 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810795328.5A CN108987709A (en) | 2018-07-19 | 2018-07-19 | A kind of graphene-based negative electrode material of lithium battery and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810795328.5A CN108987709A (en) | 2018-07-19 | 2018-07-19 | A kind of graphene-based negative electrode material of lithium battery and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108987709A true CN108987709A (en) | 2018-12-11 |
Family
ID=64550340
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810795328.5A Pending CN108987709A (en) | 2018-07-19 | 2018-07-19 | A kind of graphene-based negative electrode material of lithium battery and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108987709A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112670452A (en) * | 2020-12-10 | 2021-04-16 | 中国科学院深圳先进技术研究院 | Preparation method of negative electrode of sodium ion secondary battery and sodium ion secondary battery |
| CN114314555A (en) * | 2021-11-30 | 2022-04-12 | 上海巴库斯超导新材料有限公司 | Negative electrode material prepared by coke without graphitization |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103050663A (en) * | 2012-11-05 | 2013-04-17 | 天津市贝特瑞新能源科技有限公司 | Lithium ion battery cathode material as well as preparation method and applications thereof |
| CN107221662A (en) * | 2017-06-21 | 2017-09-29 | 合肥嘉仕诚能源科技有限公司 | A kind of preparation method of lithium ion battery negative material |
-
2018
- 2018-07-19 CN CN201810795328.5A patent/CN108987709A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103050663A (en) * | 2012-11-05 | 2013-04-17 | 天津市贝特瑞新能源科技有限公司 | Lithium ion battery cathode material as well as preparation method and applications thereof |
| CN107221662A (en) * | 2017-06-21 | 2017-09-29 | 合肥嘉仕诚能源科技有限公司 | A kind of preparation method of lithium ion battery negative material |
Non-Patent Citations (2)
| Title |
|---|
| 孙帅: "石墨烯缺陷的特点与应用研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
| 杨铁军: "《产业专利分析报告 第44册》", 30 June 2016, 知识产权出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112670452A (en) * | 2020-12-10 | 2021-04-16 | 中国科学院深圳先进技术研究院 | Preparation method of negative electrode of sodium ion secondary battery and sodium ion secondary battery |
| CN114314555A (en) * | 2021-11-30 | 2022-04-12 | 上海巴库斯超导新材料有限公司 | Negative electrode material prepared by coke without graphitization |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105914374B (en) | Composite material of nitrogen-doped carbon cladding selenizing molybdenum/graphene nucleocapsid array interlayer structure and its preparation method and application | |
| CN108796551B (en) | Sea urchin-shaped cobalt sulfide catalyst loaded on foamed nickel, preparation method thereof and application of catalyst as electrolyzed water oxygen evolution catalyst | |
| CN105789592B (en) | Surface is loaded with three-dimensional grapheme combination electrode of the flower-shaped nickel of curing three and its preparation method and application | |
| CN109698326B (en) | Organic tin phosphide/graphite oxide composite material for negative electrode of sodium-ion battery | |
| CN109326460A (en) | A kind of preparation method of di-iron trioxide/carbon cloth composite and flexible electrode | |
| CN103553149A (en) | Method for preparing cobaltosic oxide of nanometer level lamellar structure | |
| CN107068993B (en) | A kind of compound Co of three-dimensional3O4The preparation method of-Si-C negative electrode material | |
| CN105810920A (en) | Preparation method of negative electrode material of organic system sodium-ion battery | |
| CN113948681B (en) | Biomass-based hard carbon compound composite material and preparation method and application thereof | |
| CN110828785A (en) | Preparation method of sodium ion battery cathode material of zinc-cobalt bimetallic sulfide | |
| CN112010291B (en) | Preparation method and application of nickel-doped molybdenum disulfide/graphene three-dimensional composite material | |
| CN107731568A (en) | A kind of preparation method of flexible metal hydroxide electrode material for super capacitor | |
| CN111312999A (en) | Preparation method of graphene-coated nickel-iron bimetallic sulfide sodium-ion battery negative electrode material | |
| CN108987709A (en) | A kind of graphene-based negative electrode material of lithium battery and preparation method thereof | |
| CN111921529A (en) | Preparation method and application of nickel-cobalt metal organic framework/nickel-cobalt metal hydroxide heterogeneous material | |
| CN105084425B (en) | A kind of preparation method and application with undefined structure cobalt disulfide micron ball | |
| CN114284480A (en) | Nitrogen doped carbon/MoSe2/NiO/graphene flexible composite material, and preparation method and application thereof | |
| CN110444407A (en) | A kind of preparation method and applications based on the porous vulcanization nickel electrode material of metal organic frame nucleocapsid | |
| CN106981650A (en) | A kind of preparation method of nanoscale bismuth with elementary | |
| CN109686576A (en) | A kind of lithium-ion capacitor negative electrode material three-dimensional MoS2The preparation method of the compound porous fiber of@C | |
| CN106356203B (en) | A kind of cobalt acid nickel nano film/graphite felt composite material and its preparation and application | |
| CN110492099B (en) | Layered polyanion positive electrode material, preparation method, potassium ion battery positive electrode, potassium ion battery and application | |
| CN111039332A (en) | Preparation method and application of multifunctional double-layer nanowire layered composite material | |
| CN106129349A (en) | A kind of anode material for lithium-ion batteries ammonium vanadate/Graphene and preparation method thereof | |
| CN110571060A (en) | preparation method of vanadium dioxide/foamed nickel integrated electrode |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181211 |
|
| RJ01 | Rejection of invention patent application after publication |