CN103855391A - Fluorine lithium iron phosphate/graphene composite and preparation method and application thereof - Google Patents

Fluorine lithium iron phosphate/graphene composite and preparation method and application thereof Download PDF

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Publication number
CN103855391A
CN103855391A CN201210504953.2A CN201210504953A CN103855391A CN 103855391 A CN103855391 A CN 103855391A CN 201210504953 A CN201210504953 A CN 201210504953A CN 103855391 A CN103855391 A CN 103855391A
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graphene composite
lithium
composite material
fluorophosphoric acid
acid iron
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周明杰
钟玲珑
王要兵
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering 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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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

Abstract

The invention belongs to the field of electrochemical materials, and discloses a fluorine lithium iron phosphate / graphene composite and a preparation method and application thereof; the composite consists of 50-95wt% of fluorine lithium iron phosphate and 5-50wt% of graphene. The fluorine lithium iron phosphate / graphene composite is good in safety, and more stable in circulation, the composite can maintain good cycle stability under 60 DEG C, the discharge capacity attenuates from 144mAh / g to 13 1mAh / g, the capacity retention rate is about 91%, and compared with common transition metal oxide positive pole materials, the fluorine lithium iron phosphate / graphene composite has unique advantages in price, safety performance and electrochemical performance and the like, and can be used as a power type lithium ion battery positive pole.

Description

Fluorophosphoric acid iron lithium/graphene composite material and its preparation method and application
Technical field
The present invention relates to electrochemical material field, relate in particular to a kind of fluorophosphoric acid iron lithium/graphene composite material and its preparation method and application.
Background technology
Along with the development of various new forms of energy, the miniaturization development of portable electric appts and the widespread demand of electric automobile to large-capacity high-power chemical power source.Current commercial lithium ion battery adopts inorganic positive pole/graphite system mostly, and wherein these positive electrodes are mainly LiFePO4s, LiMn2O4, cobalt acid lithium, the system of lithium nickelate and mixing.Although the chemical property excellence of this class system, due to itself capacity lower (as the theoretical 170mAh/g of LiFePO4), complicated process of preparation, the shortcoming that high in cost of production is many.So the positive electrode of other kind of development of new has been subject to people's attention widely.
The key that lithium ion battery success maximizes is a bit that can the fail safe of lithium ion battery fundamentally be improved, the chemical reaction mechanism occurring from safety problem, selecting electrochemistry and heat-staple lithium ion battery electrode material is that to cause the most basic of safety problem be also most important means to prevention battery core abuse.Generally speaking, the electrode material particularly thermal stability of positive electrode is the key factor of security of lithium-ion-power cell, thereby the high positive electrode of searching security performance has very important significance with the exploitation of lithium ion battery to electrical source of power.
Summary of the invention
Problem to be solved by this invention is to provide fluorophosphoric acid iron lithium/graphene composite material that a kind of fail safe is good, circulation is more stable, and this composite material can be used as power type and bury the positive pole of ion battery.
Technical scheme of the present invention is as follows:
A kind of fluorophosphoric acid iron lithium/graphene composite material, according to mass percent, comprises 50 ~ 95% fluorophosphoric acid iron lithium and 5 ~ 50% Graphene.
The preparation method of above-mentioned fluorophosphoric acid iron lithium/graphene composite material, comprises the steps:
According to the molar ratio of ferro element and P elements 1:1, the source compound of iron and phosphate are ground, obtain precursor powder;
Described precursor powder is calcined 6 ~ 24 hours at 700 ~ 1000 ℃, obtained ferric phosphate;
Ferric phosphate, graphite oxide and lithium fluoride are ground, obtain mixed powder; Wherein, the mol ratio of ferric phosphate and lithium fluoride is 1:1, and the addition of graphite oxide is ferric phosphate and lithium fluoride gross mass 0.088 ~ 1.66 times;
Under inert gas shielding, at 500 ~ 1000 ℃, to mixed powder calcining 60 ~ 180 minutes, obtain described fluorophosphoric acid iron lithium/graphene composite material.
The preparation method of described fluorophosphoric acid iron lithium/graphene composite material, wherein, the source compound of described iron is one or more in iron oxide, ferrous oxide and tri-iron tetroxide.
The preparation method of described fluorophosphoric acid iron lithium/graphene composite material, wherein, one or more in described phosphate phosphoric acid ammonium, ammonium hydrogen phosphate and ammonium dihydrogen phosphate.
The preparation method of described fluorophosphoric acid iron lithium/graphene composite material, wherein, grinding is to carry out in ball mill, and milling time is 1 ~ 10 hour.
The preparation method of described fluorophosphoric acid iron lithium/graphene composite material, wherein, described inert gas is one or more in nitrogen, argon gas, helium and neon.
The invention still further relates to a kind of anode, comprise aluminium foil, and be coated in the positive electrode on aluminium foil, this positive electrode comprises that mass ratio is fluorophosphoric acid iron lithium/graphene composite material, Kynoar and the acetylene black of 85:5:10; According to mass percent, described fluorophosphoric acid iron lithium/graphene composite material comprises 50 ~ 95% fluorophosphoric acid iron lithium and 5 ~ 50% Graphene.
Above-mentioned anode can be applied to lithium ion cell positive field.
Fluorophosphoric acid iron lithium/graphene composite material of the present invention, fail safe is good, circulation is more stable, this material all can keep good cyclical stability at 60 ℃, discharge capacity decays to 131mAh/g from 144mAh/g, capability retention is about 91%, compared with common transition metal oxide positive electrode, there is unique advantage at aspects such as price, security performance and chemical properties, can become power type and bury ion battery positive pole.
Accompanying drawing explanation
Fig. 1 is preparation technology's flow chart of fluorophosphoric acid iron lithium/graphene composite material of the present invention.
Embodiment
This kind of active material that can be used for lithium ion cell positive providing, i.e. fluorophosphoric acid iron lithium/graphene composite material, wherein, calculates according to mass percent, and composite material comprises 50 ~ 95% fluorophosphoric acid iron lithium (LiFePO 4f) and 5 ~ 50% Graphene.
The preparation method of above-mentioned fluorophosphoric acid iron lithium/graphene composite material, as shown in Figure 1, comprises the steps:
S1, according to ferro element and the P elements molar ratio of 1: 1, will the source compound of iron and phosphate put into ball mill after mixing, ball milling 1 ~ 10h, obtains precursor powder;
S2, precursor powder is put into Muffle furnace, at 700 ~ 1000 ℃, calcine 6～24h, obtain ferric phosphate (FePO 4);
S3, the FePO that graphite oxide, step S2 are obtained 4put into ball mill with lithium fluoride (LiF), ball milling 1 ~ 10h, obtains mixed powder; Wherein, the mol ratio of ferric phosphate and lithium fluoride is 1:1, and the addition of graphite oxide is ferric phosphate and lithium fluoride gross mass 0.088 ~ 1.66 times;
S4, mixed powder is put into the Muffle furnace of inert gas shielding, 500 ~ 1000 ℃ of calcinings 60 ~ 180 minutes, obtain fluorophosphoric acid iron lithium/graphene composite material.
Above-mentioned preparation method, in step S1, the source compound of iron can be one or more in iron oxide, ferrous oxide and tri-iron tetroxide; Phosphate can be one or more in ammonium hydrogen phosphate, ammonium dihydrogen phosphate and ammonium phosphate;
Above-mentioned preparation method, in step S4, the inert gas of employing can nitrogen, the one or any multiple mixing wherein such as argon gas, helium and neon.
The application of fluorophosphoric acid iron lithium/graphene composite material: be generally used for the positive electrode of lithium ion battery, as:
A kind of anode, comprises aluminium foil, and is coated in the positive electrode on aluminium foil, this positive electrode comprises that mass ratio is fluorophosphoric acid iron lithium/graphene composite material, Kynoar and the acetylene black of 85:5:10; Calculate according to mass percent, described fluorophosphoric acid iron lithium/graphene composite material comprises 50 ~ 95% fluorophosphoric acid iron lithium and 5 ~ 50% Graphene.
Above-mentioned anode can be applied to lithium ion cell positive field, below introduces the method that uses this material to be made into lithium ion battery.
1, prepare anode
First, select fluorophosphoric acid iron lithium/graphene composite material prepared by above method as positive electrode;
Secondly, the ratio that is 85:5:10 according to mass ratio, fluorophosphoric acid iron lithium/graphene composite material, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make based lithium-ion battery positive plate.
2, preparation battery cathode
First, the ratio that is 85:5:10 according to mass ratio, graphite, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry;
Secondly, slurry is coated on Copper Foil paper tinsel, drying, roll film, trimming processing, make anode plate for lithium ionic cell.
3, the assembling of lithium ion battery
By positive plate, barrier film, negative plate in order stack of laminations dress up battery core, then use battery housing seal battery core, in battery container, inject electrolyte by the liquid injection port being arranged on battery container subsequently, sealing liquid injection port, obtains lithium ion battery.
In electrolyte, solute adopts LiPF 6, LiBF 4, LiTFSI (LiN (SO 2cF 3) 2), LiFSI (LiN (SO 2f) 2) etc., solvent adopts one or more mixing in dimethyl carbonate, diethyl carbonate, propene carbonate, ethylene carbonate, acetonitrile.
The concentration of electrolyte is generally 1mol/L.
Fluorophosphoric acid iron lithium/graphene composite material of the present invention, fail safe is good, circulation is more stable, this material all can keep good cyclical stability at 60 ℃, discharge capacity decays to 131mAh/g from 144mAh/g, capability retention is about 91%, compared with common transition metal oxide positive electrode, there is unique advantage at aspects such as price, security performance and chemical properties, can become power type and bury ion battery positive pole.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1 ~ 4th, the preparation method of fluorophosphoric acid iron lithium/graphene composite material, embodiment 5 ~ 8th, the material of embodiment 1 ~ 4 preparation is as the application of lithium ion cell positive.
Embodiment 1
(1) by 80g Fe 2o 3and 132g(NH 4) 2hPO 4for putting into ball mill, ball milling 1h, obtains precursor powder;
(2) precursor powder (1) being obtained is put into Muffle furnace, at 700 ℃, calcines 24h, obtains FePO 4;
(3) by 15.66g graphite oxide, the 152g FePO that obtains 4put into ball mill with 26g LiF, ball milling 1h,
(4) the 500 ℃ of calcining 180min of Muffle furnace that again ball milling mixture put into nitrogen gas protection prepare the fluorophosphoric acid iron lithium/graphene composite material of fluorine-containing LiFePO4 95%.
Embodiment 2
(1) by 72g ferrous oxide and 115g ammonium dihydrogen phosphate for putting into ball mill, ball milling 10h, obtains precursor powder;
(2) precursor powder (1) being obtained is put into Muffle furnace, at 1000 ℃, calcines 6h, obtains FePO 4;
(3) 152g FePO 295.5g graphite oxide, step (2) being obtained 4put into ball mill with 26g LiF, ball milling 10h,
(4) the 1000 ℃ of calcining 60min of Muffle furnace that again ball milling mixture put into nitrogen gas protection prepare the fluorophosphoric acid iron lithium/graphene composite material of fluorine-containing LiFePO4 50%.
Embodiment 3
(1) by 77.2g tri-iron tetroxide and 203g ammonium phosphate for putting into ball mill, ball milling 3h, obtains precursor powder;
(2) precursor powder (1) being obtained is put into Muffle furnace, at 800 ℃, calcines 15h, obtains FePO 4;
(3) 152g FePO 178g graphite oxide, step (2) being obtained 4put into ball mill with 26g LiF, ball milling 3h,
(4) the 700 ℃ of calcining 150min of Muffle furnace that again ball milling mixture put into nitrogen gas protection prepare the fluorophosphoric acid iron lithium/graphene composite material of fluorine-containing LiFePO4 62.5%.
Embodiment 4
(1) by 80g Fe 2o 3for putting into ball mill, ball milling 6h, obtains precursor powder with 115g ammonium dihydrogen phosphate;
(2) precursor powder (1) being obtained is put into Muffle furnace, at 900 ℃, calcines 10h, obtains FePO 4;
(3) 152g FePO 100g graphite oxide, step (2) being obtained 4put into ball mill with 26g LiF, ball milling 6h,
(4) the 900 ℃ of calcining 80min of Muffle furnace that again ball milling mixture put into nitrogen gas protection prepare the fluorophosphoric acid iron lithium/graphene composite material of fluorine-containing LiFePO4 74.8%.
Embodiment 5
1, prepare anode
First, select fluorophosphoric acid iron lithium/graphene composite material prepared by embodiment 1 as positive electrode;
Secondly, the ratio that is 85:5:10 according to mass ratio, fluorophosphoric acid iron lithium/graphene composite material, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make based lithium-ion battery positive plate.
2, preparation battery cathode
First, the ratio that is 85:5:10 according to mass ratio, graphite, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry;
Secondly, slurry is coated on Copper Foil, drying, roll film, trimming processing, make anode plate for lithium ionic cell.
3, the assembling of lithium ion battery
By positive plate, barrier film, negative plate in order stack of laminations dress up battery core, then use battery housing seal battery core, subsequently by being arranged on liquid injection port on battery container toward the LiPF that injects 1mol/L in battery container 6/ dimethyl carbonate electrolyte, sealing liquid injection port, obtains lithium ion battery.
Solute electrolyte in electrolyte adopts the conventional electrolyte LiPF of lithium ion battery 6, LiBF 4, LiTFSI (LiN (SO 2cF 3) 2), LiFSI (LiN (SO 2f) 2) etc.
The concentration of electrolyte is generally 1mol/L
Solvent adopts one or more mixing in dimethyl carbonate, diethyl carbonate, propene carbonate, ethylene carbonate, acetonitrile.
Embodiment 6 ~ 8 difference from Example 5 are:
Cell positive material adopts respectively the prepared fluorophosphoric acid iron lithium/graphene composite material out of embodiment 2 ~ 4; And electrolyte is respectively the LiBF of 1mol/L 4the LiTFSI/ propene carbonate electrolyte of/diethyl carbonate electrolyte, 1mol/L, LiFSI/ ethylene carbonate+acetonitrile electrolyte of 1mol/L.
Table 1 is that embodiment 5 ~ 8 carries out the result after charge-discharge test result and 100 circulations at 60 ℃ of temperature.
? Specific capacity (60 ℃) mAh/g Capacity retention % after 100 circulations
Embodiment 5 144 91%
Embodiment 6 70 98%
Embodiment 7 90 97%
Embodiment 8 107 95%
The fluorophosphoric acid iron lithium/graphene composite material that adopts the present invention to prepare can reach the capacity level of commercial li-ion positive electrode, at 60 ℃, carry out capacity and also can reach 144mAh/ simultaneously, after crossing 100 circulations, capacity can also keep more than 90%, and this material can prove that it has good high-temperature electrochemical properties by the high power capacity conservation rate at 60 ℃ of temperature.
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.

Claims (8)

1. fluorophosphoric acid iron lithium/graphene composite material, is characterized in that, according to mass percent, comprises 50 ~ 95% fluorophosphoric acid iron lithium and 5 ~ 50% Graphene.
2. a preparation method for fluorophosphoric acid iron lithium/graphene composite material, is characterized in that, comprises the steps:
According to ferro element and the P elements molar ratio of 1: 1, the source compound of iron and phosphate are ground, obtain precursor powder;
Described precursor powder is calcined 6 ~ 24 hours at 700 ~ 1000 ℃, obtained ferric phosphate;
Ferric phosphate, graphite oxide and lithium fluoride are ground, obtain mixed powder; Wherein, the mol ratio of ferric phosphate and lithium fluoride is 1:1, and the addition of graphite oxide is ferric phosphate and lithium fluoride gross mass 0.088 ~ 1.66 times;
Under inert gas shielding, at 500 ~ 1000 ℃, to mixed powder calcining 60 ~ 180 minutes, obtain described fluorophosphoric acid iron lithium/graphene composite material.
3. the preparation method of fluorophosphoric acid iron lithium/graphene composite material according to claim 2, is characterized in that, the source compound of described iron is one or more in iron oxide, ferrous oxide and tri-iron tetroxide.
4. the preparation method of fluorophosphoric acid iron lithium/graphene composite material according to claim 2, is characterized in that, described phosphate is one or more in ammonium phosphate, ammonium hydrogen phosphate and ammonium dihydrogen phosphate.
5. the preparation method of fluorophosphoric acid iron lithium/graphene composite material according to claim 2, is characterized in that, grinding is to carry out in ball mill, and milling time is 1 ~ 10 hour.
6. the preparation method of fluorophosphoric acid iron lithium/graphene composite material according to claim 2, is characterized in that, described inert gas is one or more in nitrogen, argon gas, helium and neon.
7. an anode, comprise aluminium foil, and be coated in the positive electrode on aluminium foil, this positive electrode comprises that mass ratio is fluorophosphoric acid iron lithium/graphene composite material, Kynoar and the acetylene black of 85:5:10, it is characterized in that, according to mass percent, described fluorophosphoric acid iron lithium/graphene composite material comprises 50 ~ 95% fluorophosphoric acid iron lithium and 5 ~ 50% Graphene.
8. a lithium ion battery, is characterized in that, the positive pole of this lithium ion battery adopts anode claimed in claim 7.
CN201210504953.2A 2012-11-30 2012-11-30 Fluorine lithium iron phosphate/graphene composite and preparation method and application thereof Pending CN103855391A (en)

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CN107946584A (en) * 2017-12-21 2018-04-20 洛阳名力科技开发有限公司 A kind of preparation method for the iron phosphate lithium positive pole composite material that carbon coating Fluorin doped is modified
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CN106410119A (en) * 2015-07-31 2017-02-15 罗伯特·博世有限公司 Method for producing an electrode of a lithium-ion battery
CN107946584A (en) * 2017-12-21 2018-04-20 洛阳名力科技开发有限公司 A kind of preparation method for the iron phosphate lithium positive pole composite material that carbon coating Fluorin doped is modified
CN109980221A (en) * 2017-12-27 2019-07-05 中国科学院上海硅酸盐研究所 A kind of anode material for high-voltage lithium ion and its preparation method and application
CN109980221B (en) * 2017-12-27 2021-04-16 中国科学院上海硅酸盐研究所 High-voltage lithium ion battery positive electrode material and preparation method and application thereof

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Application publication date: 20140611