CN108963223A - A kind of graphene power battery material and preparation method thereof - Google Patents

A kind of graphene power battery material and preparation method thereof Download PDF

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Publication number
CN108963223A
CN108963223A CN201810776993.XA CN201810776993A CN108963223A CN 108963223 A CN108963223 A CN 108963223A CN 201810776993 A CN201810776993 A CN 201810776993A CN 108963223 A CN108963223 A CN 108963223A
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power battery
graphene
battery material
hours
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孙艺宾
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Hefei Ai Feixin Materials Co Ltd
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Hefei Ai Feixin Materials Co Ltd
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    • 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
    • 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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of graphene power battery materials and preparation method thereof, and the battery material is made of the raw material of following weight parts: lithium hydroxide 100-110, ferrous ammonium phosphate 400-500, graphene oxide 30-34, aluminium isopropoxide 10-15, Dodecydimethylammonium bronides 0.6-1, glycidyl methacrylate 2-3, methyl methacrylate 20-30, ammonium persulfate 0.3-0.5.The present invention has good adhesive property in the alumina sol that high-temperature burning process obtains, and can effectively improve the mechanical stability of finished-product material；Material of the invention has good electric conductivity as power battery, and cyclical stability is high, and comprehensive performance is superior.

Description

A kind of graphene power battery material and preparation method thereof
Technical field
The invention belongs to field of new materials, and in particular to a kind of graphene power battery material and preparation method thereof.
Background technique
Lithium-ion-power cell is generally acknowledged most potential on-vehicle battery both at home and abroad at present, mainly by positive electrode, negative The part such as pole material, diaphragm, electrolyte forms；Wherein, positive electrode is the important component of lithium ion battery, and is determined The key factor of performance of lithium ion battery；Therefore, from the aspect of resource, environmental protection and security performance, lithium ion battery is found Ideal electrode active material is still international energy material worker primary problem to be solved；
Current commercialized anode material for lithium-ion batteries mainly has cobalt acid lithium, LiMn2O4 and LiFePO4；Cobalt acid Lithium is the positive electrode for being now widely used for small-scale lithium ion cell, but since cobalt is toxic, resource reserve is limited expensive, And the battery security that assembles as positive electrode of cobalt acid lithium material and thermal stability are bad, can generate oxygen at high temperature, it is full The foot not technical requirements of power battery；LiMn2O4 is although cheap, environmentally friendly, safety, high rate performance and has a safety feature, but It is that its theoretical capacity is not high, recycling performance, thermal stability and high-temperature behavior are poor, and greatest problem in the application is circulation Performance is bad, especially under high temperature, bivalent manganese that when Manganic ion and big multiplying power discharging in material is formed in particle surface Ion finally destroys the structure of LiMn2O4 so that the dissolution of material in the electrolytic solution is obvious, also reduces the cyclicity of material Energy；Therefore, find that a kind of conductive stability is good, development of the superior lithium-ion-power cell material of comprehensive performance for modernization It is particularly significant.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of graphene power battery material and Preparation method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of graphene power battery material, it is composed of the following raw materials by weight: lithium hydroxide 100-110, Ferrous ammonium phosphate 400-500, graphene oxide 30-34, aluminium isopropoxide 10-15, Dodecydimethylammonium bronides 0.6-1, first Base glycidyl acrylate 2-3, methyl methacrylate 20-30, ammonium persulfate 0.3-0.5.
The preparation method of the graphene power battery material, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 30-40 times of its weight, stirs evenly；
(2) take ferrous ammonium phosphate, glycidyl methacrylate mixing, be added to 2-3 times of mixture weight go from It in sub- water, stirs evenly, methyl methacrylate is added, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 50-70 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, discharging cooling obtained epoxy polyester lotion；
(3) take aluminium isopropoxide, Dodecydimethylammonium bronides mixing, be added to 20-30 times of mixture weight go from It in sub- water, stirs evenly, graphene oxide is added, is stirred to react 4-6 hours, above-mentioned epoxy polyester lotion is added, increase temperature It is 160-180 DEG C, lithium hydroxide is added, insulated and stirred 3-5 hours, filters, filter cake is washed, be sent into sintering furnace, be passed through argon Gas is calcined 10-20 hours, and discharging is cooling to get the graphene power battery material.
A kind of preparation method of graphene power battery material, calcining described in step (3), temperature are 800-950℃。
Advantages of the present invention:
The present invention handles methyl methacrylate using glycidyl methacrylate, then gathers under initiator effect It closes, obtains epoxy polyester lotion；Then using aluminium isopropoxide as presoma, using Dodecydimethylammonium bronides as dispersing agent processing Obtained graphene Aluminum sol and China's reference polyester blend are promoted the hydroxyl of epoxy group and surface of graphene oxide by graphene Reaction, to promote the dispersion compatibility between each raw material, during the reaction by lithium hydroxide, ferrous ammonium phosphate it is anti- It answering, obtains the major ingredient ingredient of battery, the present invention has good adhesive property in the alumina sol that high-temperature burning process obtains, The mechanical stability of finished-product material can effectively be improved；Material of the invention has good electric conductivity as power battery Can, and cyclical stability is high, comprehensive performance is superior；Power battery material of the invention is relative to directly by graphene, ferric phosphate The composite material that lithium is blended has better mechanics, conductive endless stability.
Specific embodiment
Embodiment 1
A kind of graphene power battery material, it is composed of the following raw materials by weight: lithium hydroxide 110, phosphoric acid Ferrous ammonium 500, graphene oxide 34, aluminium isopropoxide 15, Dodecydimethylammonium bronides 1, glycidyl methacrylate 3, methyl methacrylate 30, ammonium persulfate 0.5.
The preparation method of the graphene power battery material, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 40 times of its weight, stirs evenly；
(2) ferrous ammonium phosphate, glycidyl methacrylate mixing are taken, 3 times of mixture weight of deionization is added to It in water, stirs evenly, methyl methacrylate is added, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 70 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 5 hours, discharging cooling obtained epoxy polyester lotion；
(3) aluminium isopropoxide, Dodecydimethylammonium bronides mixing are taken, 30 times of mixture weight of deionized water is added to In, it stirs evenly, graphene oxide is added, is stirred to react 6 hours, above-mentioned epoxy polyester lotion is added, increasing temperature is 180 DEG C, lithium hydroxide is added, insulated and stirred 5 hours, filters, filter cake is washed, be sent into sintering furnace, is passed through argon gas, calcining 20 is small When, discharging is cooling to get the graphene power battery material.
A kind of preparation method of graphene power battery material, calcining described in step (3), temperature are 950℃。
Embodiment 2
A kind of graphene power battery material, it is composed of the following raw materials by weight: lithium hydroxide 100, phosphoric acid Ferrous ammonium 400, graphene oxide 30, aluminium isopropoxide 10, Dodecydimethylammonium bronides 0.6, methyl propenoic acid glycidyl Ester 2, methyl methacrylate 20, ammonium persulfate 0.3.
The preparation method of the graphene power battery material, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly；
(2) ferrous ammonium phosphate, glycidyl methacrylate mixing are taken, 2 times of mixture weight of deionization is added to It in water, stirs evenly, methyl methacrylate is added, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 50 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3 hours, discharging cooling obtained epoxy polyester lotion；
(3) aluminium isopropoxide, Dodecydimethylammonium bronides mixing are taken, 20 times of mixture weight of deionized water is added to In, it stirs evenly, graphene oxide is added, is stirred to react 4 hours, above-mentioned epoxy polyester lotion is added, increasing temperature is 160 DEG C, lithium hydroxide is added, insulated and stirred 3 hours, filters, filter cake is washed, be sent into sintering furnace, is passed through argon gas, calcining 10 is small When, discharging is cooling to get the graphene power battery material.
A kind of preparation method of graphene power battery material, calcining described in step (3), temperature are 800℃。
Performance test:
The graphene power battery material of embodiment 1；
Apparent density: 1.29g/cm3；
Tap density: 2.30g/cm3；
Specific capacity (25 DEG C, 1C, vs li, mAh/g) 133.3；
After circulation 10 times, specific capacity 124.5mAh/g；
The graphene power battery material of embodiment 2；
Apparent density: 1.31g/cm3；
Tap density: 2.32g/cm3；
Specific capacity (25 DEG C, 1C, vs li, mAh/g) 134.0；
After circulation 10 times, specific capacity 124.8mAh/g.

Claims (3)

1. a kind of graphene power battery material, which is characterized in that it is composed of the following raw materials by weight:
Lithium hydroxide 100-110, ferrous ammonium phosphate 400-500, graphene oxide 30-34, aluminium isopropoxide 10-15, dodecyl Ditallowdimethyl ammonium bromide 0.6-1, glycidyl methacrylate 2-3, methyl methacrylate 20-30, ammonium persulfate 0.3- 0.5。
2. a kind of preparation method of graphene power battery material as described in claim 1, which is characterized in that including following step It is rapid:
(1) ammonium persulfate is taken, is added in the deionized water of 30-40 times of its weight, stirs evenly；
(2) ferrous ammonium phosphate, glycidyl methacrylate mixing are taken, the deionized water of 2-3 times of mixture weight is added to In, it stirs evenly, methyl methacrylate is added, is sent in reaction kettle, be passed through nitrogen, adjusting temperature of reaction kettle is 50-70 DEG C, above-mentioned ammonium persulfate aqueous solution is added, insulated and stirred 3-5 hours, discharging cooling obtained epoxy polyester lotion；
(3) aluminium isopropoxide, Dodecydimethylammonium bronides mixing are taken, the deionized water of 20-30 times of mixture weight is added to In, it stirs evenly, graphene oxide is added, is stirred to react 4-6 hours, above-mentioned epoxy polyester lotion is added, increasing temperature is 160-180 DEG C, lithium hydroxide is added, insulated and stirred 3-5 hours, filters, filter cake is washed, be sent into sintering furnace, be passed through argon gas, Calcining 10-20 hours, discharging are cooling to get the graphene power battery material.
3. a kind of preparation method of graphene power battery material according to claim 2, which is characterized in that step (3) Described in calcining, temperature be 800-950 DEG C.
CN201810776993.XA 2018-07-14 2018-07-14 A kind of graphene power battery material and preparation method thereof Withdrawn CN108963223A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110676445A (en) * 2019-09-19 2020-01-10 安徽清泉新能源科技集团有限责任公司 Sol-coated lithium battery material and preparation method thereof

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CN102040714A (en) * 2010-11-02 2011-05-04 浙江大学 Preparation method of polymer-grafted graphene
CN102044666A (en) * 2010-11-19 2011-05-04 杭州电子科技大学 Method for preparing lithium iron phosphate composite material for lithium cells
CN102315423A (en) * 2010-07-08 2012-01-11 中国科学院宁波材料技术与工程研究所 Graphene/lithium iron phosphate compound anode material, preparation method thereof and lithium ion secondary battery
CN102504145A (en) * 2011-11-15 2012-06-20 苏州大学 Preparation method for polymer grafted graphene oxide
CN106410151A (en) * 2016-10-28 2017-02-15 合肥国轩高科动力能源有限公司 Preparation method of graphene/aluminum oxide co-coated lithium ion battery positive electrode material
CN106632878A (en) * 2016-12-15 2017-05-10 陕西科技大学 Oxidized graphene/waterborne polyurethane acrylate composite emulsion and preparation method and application thereof
CN107068967A (en) * 2011-12-16 2017-08-18 株式会社半导体能源研究所 The manufacture method of lithium ion secondary battery anode
CN107652817A (en) * 2017-10-24 2018-02-02 广东工业大学 A kind of modified graphene oxide/polyacrylate nano-composite coating and preparation method thereof

Patent Citations (8)

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Publication number Priority date Publication date Assignee Title
CN102315423A (en) * 2010-07-08 2012-01-11 中国科学院宁波材料技术与工程研究所 Graphene/lithium iron phosphate compound anode material, preparation method thereof and lithium ion secondary battery
CN102040714A (en) * 2010-11-02 2011-05-04 浙江大学 Preparation method of polymer-grafted graphene
CN102044666A (en) * 2010-11-19 2011-05-04 杭州电子科技大学 Method for preparing lithium iron phosphate composite material for lithium cells
CN102504145A (en) * 2011-11-15 2012-06-20 苏州大学 Preparation method for polymer grafted graphene oxide
CN107068967A (en) * 2011-12-16 2017-08-18 株式会社半导体能源研究所 The manufacture method of lithium ion secondary battery anode
CN106410151A (en) * 2016-10-28 2017-02-15 合肥国轩高科动力能源有限公司 Preparation method of graphene/aluminum oxide co-coated lithium ion battery positive electrode material
CN106632878A (en) * 2016-12-15 2017-05-10 陕西科技大学 Oxidized graphene/waterborne polyurethane acrylate composite emulsion and preparation method and application thereof
CN107652817A (en) * 2017-10-24 2018-02-02 广东工业大学 A kind of modified graphene oxide/polyacrylate nano-composite coating and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110676445A (en) * 2019-09-19 2020-01-10 安徽清泉新能源科技集团有限责任公司 Sol-coated lithium battery material and preparation method thereof
CN110676445B (en) * 2019-09-19 2022-11-08 安徽清泉新能源科技集团有限责任公司 Lithium battery material and preparation method thereof

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