CN107154489A - A kind of preparation method of LiFePO4/graphene composite material - Google Patents

A kind of preparation method of LiFePO4/graphene composite material Download PDF

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Publication number
CN107154489A
CN107154489A CN201710376462.7A CN201710376462A CN107154489A CN 107154489 A CN107154489 A CN 107154489A CN 201710376462 A CN201710376462 A CN 201710376462A CN 107154489 A CN107154489 A CN 107154489A
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graphene
lifepo4
composite material
preparation
lithium
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CN201710376462.7A
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陈召勇
张曾
罗丁
段军飞
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CHANGSHA LUOSI TECHNOLOGY Co Ltd
Changsha University of Science and Technology
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CHANGSHA LUOSI TECHNOLOGY Co Ltd
Changsha University of Science and Technology
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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
    • 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
    • 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
    • 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)
  • Composite Materials (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 preparation method of LiFePO4/graphene composite material.Graphene and Riboflavine sodium phosphate are added in solvent, make its dispersed using ultrasound and stirring, complexing agent, Li source compound, molysite compound are dissolved in solution respectively, are then added sequentially in graphene dispersing solution, LiFePO4/graphene composite material is obtained after reaction；Obtained LiFePO4/graphene is well mixed in the way of ball milling with carbon source, after drying under inert gas shielding, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 600~850 DEG C of 3~24h of calcining at constant temperature.Riboflavine sodium phosphate in the present invention makees surfactant in the scattered of graphene, can also be used as phosphorus source in the generating process of LiFePO4.The lithium iron phosphate/carbon composite material that graphene prepared by the present invention is modified may be used as the positive electrode of lithium ion battery, and the cyclical stability that can be allowed under battery performance particularly high magnification is significantly improved.

Description

A kind of preparation method of LiFePO4/graphene composite material
Technical field
The invention belongs to technical field of lithium ion battery positive pole material preparation, and in particular to a kind of LiFePO4/graphite The preparation method of alkene composite.
Background technology
The anode material for lithium-ion batteries being currently known has cobalt acid lithium (LiCoO2), LiFePO4 (LiFePO4), LiMn2O4 (LiMn2O4), lithium nickel cobalt dioxide (LiNixCo1-xO2), nickle cobalt lithium manganate (LiNi1/3Co1/3Mn1/3O2) etc. material.Compared to others Positive electrode LiFePO4There is higher specific discharge capacity（3.47V）, more stable discharge platform, good cyclical stability, heat Stability and it is cheap the advantages of.But LiFePO4Electronic conductivity is low, bulk density is small and ion diffuser efficiency Low defect makes LiFePO4High rate performance it is poor, this significantly limit LiFePO4Practical application.
In the LiFePO being currently known4Method of modifying in, carbon coating is a kind of effective modified LiFePO4Method, can be with Increase substantially LiFePO4High rate charge-discharge performance, obtain higher specific discharge capacity.But carbon coating can reduce material Energy density and tap density, and graphene due to good conductivity, quality is small, specific surface area is big the advantages of be expected to change well It is apt to disadvantages mentioned above and obtains the structurally consummate and high positive electrode of energy density.But up to the present can not be by graphene The method effectively mixed with LiFePO4.
The content of the invention
In order to make up the deficiencies in the prior art part, the present invention provides a kind of system of LiFePO4/graphene composite material Preparation Method.The composite material preparation process is simple and advantage of lower cost, and electricity can be realized by being applied in lithium ion battery Cyclical stability under pond chemical property particularly high magnification is obviously improved.
In order to realize the purpose of the present invention, the present invention is implemented by following scheme：
（1）Graphene and surfactant Riboflavine sodium phosphate are added in solvent, then stirred using bath ultrasound and machinery Mix device to disperse graphene mixed liquor, graphene dispersing solution is obtained after 3~20 h jitter time；
（2）Complexing agent, Li source compound, molysite compound are dissolved in solution respectively, described Li source compound, molysite chemical combination Thing, the inventory of Riboflavine sodium phosphate need to ensure Li: Fe: P=2 ~ 4: 1: 1, then sequentially add at room temperature Into graphene dispersing solution, pH=6~10 are adjusted at 40~60 DEG C, height is moved into after then heating to 80~90 DEG C of 1~5h of stirring Press in reactor, LiFePO4/graphene composite material is filtrated to get after 2~30h of reaction at a temperature of 100~200 DEG C；
（3）By obtained LiFePO4/graphene and carbon source and ball-milling medium proportionally put into ball milling 2 in ball mill~ 10h, ratio of grinding media to material is 1:3~1:8, regulation ball milling speed is 100 ~ 500 rpm, is dried at 30~50 DEG C after ball milling, puts into high temperature furnace Under the inert gas shielding such as nitrogen or argon gas, in obtained after 500~850 DEG C of 3~24h of calcining at constant temperature graphene modification Lithium iron phosphate/carbon composite material.
Step of the present invention（1）Described solvent be 1-Methyl-2-Pyrrolidone, DMF, isopropanol, 1, The mixed solvent of one or more of compositions in 4- butanediols, deionized water.
Step（2）Described complexing agent is one or several kinds of mixtures in ammonium citrate, citric acid, ascorbic acid； Described Li source compound is one or several kinds of mixtures in lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate；Described Molysite compound is ferrous oxalate, ferrous acetate, ferrous sulfate, ferrous nitrate and ferric phosphate one or several kinds of mixing therein Thing.
Step of the present invention（3）Described carbon source is the mixture of one or both of glucose, sucrose, starch；It is described Ball-milling medium be water, ethanol, methanol, acetone in one or several kinds of mixtures.
The microstructure for the lithium iron phosphate/carbon composite material that graphene of the present invention is modified is covered in phosphoric acid for carbon-coating Iron lithium nano grain surface, and graphene film is wrapped in the nano particle insertion graphite of lithium iron phosphate nano particle or LiFePO4 Between alkene.The invention has the advantages that：
（1）Micro carbon coating is carried out on LiFePO4 surface, lithium iron phosphate particles surface is formed conductive network, while increase again The specific surface area of big material, improves the electric conductivity between lithium iron phosphate particles；
（2）Graphene is the minimum material of world resistivity, with LiFePO4Compound can greatly reduce LiFePO4Resistance, So as to improve LiFePO4High rate performance；
（3）Electrical conductivity is high in the lithium iron phosphate/carbon material that graphene is modified, and can improve its big multiplying power discharging capacity.
Embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
Weigh 40mg graphenes and 23.915g Riboflavine sodium phosphates are added in 40ml deionized waters, then utilize bath ultrasound Graphene mixed liquor is disperseed with mechanical stirring device, graphene dispersing solution is obtained after 5h jitter time；Will 9.7287g ammonium citrates, 5.2554g lithium acetates, 20.5255g ferric nitrates are dissolved in 30ml deionized waters respectively, then in room temperature Under by being added sequentially in graphene dispersing solution, adjust behind pH=6 and moved into autoclave at 50 DEG C, in 180 DEG C of temperature LiFePO4/graphene composite material is filtrated to get after lower reaction 2h；By obtained LiFePO4/graphene and 0.9465g Portugals Ball milling 6h in grape sugar and ethanol input ball mill, ratio of grinding media to material is 1:6, regulation ball milling speed is 35 DEG C of bakings after 200rpm, ball milling It is dry, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 750 DEG C of calcining at constant temperature 12h under nitrogen atmosphere protection.
Embodiment 2
Weigh 40mg graphenes and 23.915g Riboflavine sodium phosphates are added in 40ml deionized waters, then utilize bath ultrasound Graphene mixed liquor is disperseed with mechanical stirring device, graphene dispersing solution is obtained after 7.5 h jitter time；Will 9.7287g ammonium citrates, 5.2554g lithium acetates, 20.5255g ferric nitrates are dissolved in 30ml deionized waters respectively, then in room temperature Under by being added sequentially in graphene dispersing solution, adjust behind pH=7 and moved into autoclave at 50 DEG C, in 180 DEG C of temperature LiFePO4/graphene composite material is filtrated to get after lower reaction 3h；By obtained LiFePO4/graphene and 0.9465g Portugals Ball milling 6h in grape sugar and ethanol input ball mill, ratio of grinding media to material is 1:6, regulation ball milling speed is 35 DEG C of bakings after 200rpm, ball milling It is dry, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 750 DEG C of calcining at constant temperature 12h under nitrogen atmosphere protection.
Embodiment 3
Weigh 80mg graphenes and 23.915g Riboflavine sodium phosphates are added in 40ml deionized waters, then utilize bath ultrasound Graphene mixed liquor is disperseed with mechanical stirring device, graphene dispersing solution is obtained after 10 h jitter time；Will 9.7287g ammonium citrates, 5.2554g lithium acetates, 20.5255g ferric nitrates are dissolved in 30ml deionized waters respectively, then in room temperature Under by being added sequentially in graphene dispersing solution, adjust behind pH=8 and moved into autoclave at 50 DEG C, in 180 DEG C of temperature LiFePO4/graphene composite material is filtrated to get after lower reaction 4h；By obtained LiFePO4/graphene and 0.9465g Portugals Ball milling 6h in grape sugar and ethanol input ball mill, ratio of grinding media to material is 1:6, regulation ball milling speed is 35 DEG C of bakings after 200rpm, ball milling It is dry, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 750 DEG C of calcining at constant temperature 12h under nitrogen atmosphere protection.
Embodiment 4
Weigh 40mg graphenes and 23.915g Riboflavine sodium phosphates are added in 40ml deionized waters, then utilize bath ultrasound Graphene mixed liquor is disperseed with mechanical stirring device, graphene dispersing solution is obtained after 10 h jitter time；Will 9.7287g ammonium citrates, 5.2554g lithium acetates, 20.5255g ferric nitrates are dissolved in 30ml deionized waters respectively, then in room temperature Under by being added sequentially in graphene dispersing solution, adjust behind pH=6 and moved into autoclave at 50 DEG C, in 150 DEG C of temperature LiFePO4/graphene composite material is filtrated to get after lower reaction 2h；By obtained LiFePO4/graphene and 0.9465g Portugals Ball milling 6h in grape sugar and ethanol input ball mill, ratio of grinding media to material is 1:6, regulation ball milling speed is 35 DEG C of bakings after 400rpm, ball milling It is dry, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 750 DEG C of calcining at constant temperature 12h under nitrogen atmosphere protection.
Embodiment 5
Weigh 40mg graphenes and 23.915g Riboflavine sodium phosphates are added in 40ml deionized waters, then utilize bath ultrasound Graphene mixed liquor is disperseed with mechanical stirring device, graphene dispersing solution is obtained after 10 h jitter time；Will 9.7287g ammonium citrates, 5.2554g lithium acetates, 20.5255g ferric nitrates are dissolved in 30ml deionized waters respectively, then in room temperature Under by being added sequentially in graphene dispersing solution, adjust behind pH=6 and moved into autoclave at 50 DEG C, in 200 DEG C of temperature LiFePO4/graphene composite material is filtrated to get after lower reaction 2h；By obtained LiFePO4/graphene and 0.9465g Portugals Ball milling 3h in grape sugar and ethanol input ball mill, ratio of grinding media to material is 1:6, regulation ball milling speed is 35 DEG C of bakings after 400rpm, ball milling It is dry, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 750 DEG C of calcining at constant temperature 12h under nitrogen atmosphere protection.
Embodiment 6
Weigh 40mg graphenes and 23.915g Riboflavine sodium phosphates are added in 40ml deionized waters, then utilize bath ultrasound Graphene mixed liquor is disperseed with mechanical stirring device, graphene dispersing solution is obtained after 10 h jitter time；Will 9.7287g ammonium citrates, 5.2554g lithium acetates, 20.5255g ferric nitrates are dissolved in 30ml deionized waters respectively, then in room temperature Under by being added sequentially in graphene dispersing solution, adjust behind pH=6 and moved into autoclave at 50 DEG C, in 180 DEG C of temperature LiFePO4/graphene composite material is filtrated to get after lower reaction 2h；By obtained LiFePO4/graphene and 0.9465g Portugals Ball milling 6h in grape sugar and ethanol input ball mill, ratio of grinding media to material is 1:6, regulation ball milling speed is 45 DEG C of bakings after 300rpm, ball milling It is dry, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 650 DEG C of calcining at constant temperature 12h under nitrogen atmosphere protection.
Embodiment 7
Weigh 40mg graphenes and 23.915g Riboflavine sodium phosphates are added in 40ml deionized waters, then utilize bath ultrasound Graphene mixed liquor is disperseed with mechanical stirring device, graphene dispersing solution is obtained after 10 h jitter time；Will 9.7287g ammonium citrates, 5.2554g lithium acetates, 20.5255g ferric nitrates are dissolved in 30ml deionized waters respectively, then in room temperature Under by being added sequentially in graphene dispersing solution, adjust behind pH=6 and moved into autoclave at 50 DEG C, in 180 DEG C of temperature LiFePO4/graphene composite material is filtrated to get after lower reaction 2h；By obtained LiFePO4/graphene and 0.9465g Portugals Ball milling 4h in grape sugar and ethanol input ball mill, ratio of grinding media to material is 1:6, regulation ball milling speed is 35 DEG C of bakings after 400rpm, ball milling It is dry, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 750 DEG C of calcining at constant temperature 15h under nitrogen atmosphere protection.
Embodiment 8
Weigh 80mg graphenes and 23.915g Riboflavine sodium phosphates are added in 40ml deionized waters, then utilize bath ultrasound Graphene mixed liquor is disperseed with mechanical stirring device, graphene dispersing solution is obtained after 10 h jitter time；Will 9.7287g ammonium citrates, 5.2554g lithium acetates, 20.5255g ferric nitrates are dissolved in 30ml deionized waters respectively, then in room temperature Under by being added sequentially in graphene dispersing solution, adjust behind pH=6 and moved into autoclave at 50 DEG C, in 180 DEG C of temperature LiFePO4/graphene composite material is filtrated to get after lower reaction 2h；By obtained LiFePO4/graphene and 0.9465g Portugals Ball milling 4h in grape sugar and ethanol input ball mill, ratio of grinding media to material is 1:6, regulation ball milling speed is 35 DEG C of bakings after 400rpm, ball milling It is dry, in the lithium iron phosphate/carbon composite material that graphene modification is obtained after 700 DEG C of calcining at constant temperature 12h under nitrogen atmosphere protection.

Claims (8)

1. a kind of preparation method of LiFePO4/graphene composite material, it is characterised in that comprise the following steps：
Graphene and surfactant Riboflavine sodium phosphate are added in solvent, bath ultrasound and mechanical agitation dress is then utilized Put and graphene mixed liquor is disperseed, graphene dispersing solution is obtained after 3~20 h jitter time；
Complexing agent, Li source compound, molysite compound are dissolved in solution respectively, described Li source compound, molysite compound, The inventory of Riboflavine sodium phosphate need to ensure Li: Fe: P=2 ~ 4: 1: 1, and stone is then added sequentially at room temperature In black alkene dispersion liquid, pH=6~10 are adjusted at 40~60 DEG C, immigration high pressure after 80~90 DEG C of 1~5h of stirring are then heated to anti- Answer in kettle, LiFePO4/graphene composite material is filtrated to get after 2~30h of reaction at a temperature of 100~200 DEG C；
Obtained LiFePO4/graphene and carbon source and ball-milling medium are proportionally put into 2~10h of ball milling in ball mill, Ratio of grinding media to material is 1:3~1:8, regulation ball milling speed is 100 ~ 500 rpm, is dried at 30~50 DEG C after ball milling, and input high temperature furnace is in nitrogen Under the inert gas shielding such as gas or argon gas, in the phosphoric acid that graphene modification is obtained after 500~850 DEG C of 3~24h of calcining at constant temperature Iron lithium/carbon composite material.
2. a kind of preparation method of LiFePO4/graphene composite material according to claim 1, it is characterised in that：Step Suddenly（1）Described solvent be 1-Methyl-2-Pyrrolidone class, DMF, isopropanol, BDO, go from The mixed solvent of one or more of compositions in sub- water.
3. a kind of preparation method of LiFePO4/graphene composite material according to claim 1, it is characterised in that：Step Suddenly（1）Described graphene includes single-layer graphene, multi-layer graphene and graphene nanometer sheet.
4. a kind of preparation method of LiFePO4/graphene composite material according to claim 1, it is characterised in that：Step Suddenly（2）Described complexing agent is one or several kinds of mixtures in ammonium citrate, citric acid, ascorbic acid.
5. a kind of preparation method of LiFePO4/graphene composite material according to claim 1, it is characterised in that：Step Suddenly（2）Described Li source compound is one or several kinds of mixtures in lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate.
6. a kind of preparation method of LiFePO4/graphene composite material according to claim 1, it is characterised in that：Step Suddenly（2）Described molysite compound is ferrous oxalate, ferrous acetate, ferrous sulfate, ferrous nitrate and ferric phosphate one kind therein Or several mixtures.
7. a kind of preparation method of LiFePO4/graphene composite material according to claim 1, it is characterised in that：Step Suddenly（3）Described carbon source is the mixture of one or both of glucose, sucrose, starch.
8. a kind of preparation method of LiFePO4/graphene composite material according to claim 1, it is characterised in that：Step Suddenly（3）Described ball-milling medium is one or several kinds of mixtures in water, ethanol, methanol, acetone.
CN201710376462.7A 2017-05-25 2017-05-25 A kind of preparation method of LiFePO4/graphene composite material Pending CN107154489A (en)

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CN111640951A (en) * 2020-05-25 2020-09-08 湖南西瑞尔新材料科技有限公司 Preparation method and application of air electrode catalyst layer

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