CN109037658A - A kind of lithium iron phosphate positive material preparation method of polymer overmold - Google Patents

A kind of lithium iron phosphate positive material preparation method of polymer overmold Download PDF

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CN109037658A
CN109037658A CN201811015199.XA CN201811015199A CN109037658A CN 109037658 A CN109037658 A CN 109037658A CN 201811015199 A CN201811015199 A CN 201811015199A CN 109037658 A CN109037658 A CN 109037658A
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iron phosphate
lithium
polymer overmold
positive material
obtains
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高媛
熊昆
朱冰峰
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Chongqing Technology and Business University
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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
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/624—Electric conductive 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/028—Positive 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

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Abstract

The present patent application belongs to electrode material preparation technical field, specifically disclose a kind of lithium iron phosphate positive material preparation method of polymer overmold, the following steps are included: (1) is according to lithium: iron: phosphorus molar ratio is that 3~5:1:1 weighs inorganic salt raw material, and lithium source and phosphorus source are dissolved in ethylene glycol solvent, it is reacted at a certain temperature；(2) source of iron and surfactant are added in the mixture that step (1) obtains, stirs evenly；(3) mixed solution that step (2) obtains is transferred in reaction kettle, reaction obtains iron phosphate powder；(4) oxidant is added in the iron phosphate powder that step (3) obtains and water is stirred mixing, add pyrroles；Obtained suspension is stirred and is polymerize, polymer is handled to obtain polymer overmold lithium iron phosphate positive material.Present invention is mainly used for lithium iron phosphate positive material is prepared, solve the problems, such as that the low specific capacity of lithium iron phosphate positive material, low power are forthright.

Description

A kind of lithium iron phosphate positive material preparation method of polymer overmold
Technical field
The invention belongs to electrode material preparation technical fields, specifically disclose a kind of iron phosphate lithium positive pole of polymer overmold Material preparation method.
Background technique
Rechargeable secondary battery of the lithium ion battery as a new generation, has that energy density is big, has a safety feature, recycles The many merits such as the service life is long, self discharge is low, at " National Program for Medium-to Long-term Scientific and Technological Development (2006-2020) " In be listed in the new high-tech industry that primary study project and China's energy field emphasis are supported.Positive electrode is in lithium ion Play highly important role in secondary cell, performance (specific capacity, cyclic reversibility, high power be forthright, safety and at This) restrict lithium ion secondary battery practicability and development.
Olivine-type LiFePO4 (LiFePO4), it can be in~3.5V (vs.Li/Li+) reversibly deintercalate lithium ions, charge and discharge Level platform is very steady, materials theory specific capacity height (170mAh.g-1), volume energy density is larger, has a safety feature, can be in height It is used under warm environment, raw material are nontoxic, pollution-free, and from a wealth of sources (Fe rich content in the earth's crust, abundance are four), cheap The advantages that, it is the lithium-ion-power cell positive electrode of most future.LiFePO4 large-scale application is also by some at present The restriction of Pinch technology, LiFePO4The poor electric conductivity of material itself and lower lithium ion diffusion coefficient, make its again it is forthright compared with Difference, charging and discharging capacity decaying is severe especially under high current density.Lithium-ion-power cell will be realized within 10 years futures Commercialization and popularization and application, must just solve LiFePO first4The two are prominent for positive electrode high current fast charging and discharging and cost It goes wrong.Therefore design, preparation have height ratio capacity, and high power is forthright, stability, cheap power type LiFePO4Anode Material is of great significance.
The modification of LiFePO4 is concentrated mainly at present bulk phase-doped, surface cladding and control pattern, partial size are to mentioning The electronic conductivity and lithium ion of high material are in the diffusivity in body phase in terms of these.All using carbon coating and ion doping The charge-discharge performance that can be obviously improved under lithium iron phosphate high multiplying, but what cannot be ignored be these is all to sacrifice LiFePO4 Volume energy density is the means of cost.Therefore, the requirement with power battery to high-energy density, high power density, for The performances such as electric conductivity, circulation volume holding, high rate charge-discharge performance, the quick charge of LiFePO4 need further to mention It is high.
Summary of the invention
The purpose of the present invention is to provide a kind of lithium iron phosphate positive material preparation methods of polymer overmold, to solve phosphorus The forthright problem of the low specific capacity of sour iron lithium anode material, low power.
In order to achieve the above object, a kind of base case of the invention are as follows: lithium iron phosphate positive material of polymer overmold Preparation method, comprising the following steps:
(1) according to lithium source: source of iron: the mole ratio of phosphorus source is that 3~5:1:1 weighs inorganic salt raw material, and by lithium source and phosphorus Source is dissolved in solvent and being reacted；
(2) source of iron and surfactant are added in the mixture that step (1) obtains, stirs evenly；
(3) mixed solution that step (2) obtains is transferred in reaction kettle, 5~20h is reacted at 80~300 DEG C and is obtained Iron phosphate powder；Iron phosphate powder is cooling, separation, washing, and be dried in vacuo；
(4) oxidant is added in the iron phosphate powder that step (3) obtains and water is stirred mixing, add pyrrole It coughs up, the molar ratio of pyrroles and oxidant is 3~5:1, and the mass ratio of pyrroles and iron phosphate powder is 2~20:100；By gained The suspension stirring 16~20h of polymerization arrived, cleans polymer, is centrifugated, vacuum drying obtains polymer overmold phosphorus Sour iron lithium anode material.
The principle and beneficial effect of this base case are:
1, pass through control reaction temperature and reaction time, the nanometer LiFePO of one-step synthesis high-crystallinity4Dusty material, nothing Subsequent high temperature sintering and inert gas shielding are needed, keeps synthesis technology more simple, reduces cost.
2, the polypyrrole using in-situ oxidizing-polymerizing method in LiFePO4 coated with uniform with high conductivity carries out Coating modification significantly improves the high rate charge-discharge ability of LiFePO4, reduces LiFePO4 and follow under high current density The decaying of ring capacity improves its high-multiplying power discharge specific capacity；Meanwhile the internal resistance of cell is effectively reduced, it is dynamic to improve LiFePO4 The specific power of power battery adapts to power battery deep-cycle demand.
3, compared with common carbon coating technological means, using the LiFePO4 after polypyrrole cladding in technical solution of the present invention Be obviously improved high rate charge-discharge ability, cell testing results: current density 1C, 5C, 10C capacity may be up to respectively 145mAh/g, 126mAh/g, 118mAh/g, 10C recycle 20 weeks capacity retention ratios 98% or more.
Compared with prior art, this method preparation process is easy, easy to operate, is suitble to industrialization large-scale production.
Further, the range of reaction temperature in the step (1) is 20~60 DEG C.In 20~60 DEG C of reactions convenient for control temperature Degree, while reducing security risk and energy consumption.
Further, the surfactant of the step (2) is lauric acid, dodecyl sodium sulfate or dodecyl benzene sulfonic acid One of sodium.It is found by Experimental comparison, after surfactant, surfactant is cooperateed in initial reaction stage with ethylene glycol Effect, can promote the preferential forming core of LiFePO4, be conducive to generate LiFePO in the reaction in this way4, thus in lower temperature The LiFePO4 of high-crystallinity is formed under degree.
Further, the dosage of surfactant of the step (2) is 0.5~5gL-1.By in above-mentioned concentration range Regulate and control surfactant, keeps the supermolecular module concentration generated in reaction system different, to change the life of crystal in solution Long mode can also adjust the micromorphology of nano-grade lithium iron phosphate, by controlling the type and dosage of surfactant, obtain To the LiFePO4 particle of special appearance, is conducive to lithium ion and is moved in [0 1 0] crystal face along one-dimensional square, to reach raising The purpose of material ions conductivity.
Further, the reaction temperature in the step (3) is 180 DEG C, reaction time 12h.It is chemical at higher temperature The activity of reaction is higher.
Further, the oxidant in the step (4) is one in ammonium persulfate, ferric trichloride or p-methyl benzenesulfonic acid iron Kind.Oxidant can induce pyrrole monomer in-situ oxidizing-polymerizing during coating modification, obtain the clad of high conductivity.
Further, the solvent in step (1) is one of ethyl alcohol, ethylene glycol or water.
Detailed description of the invention
Fig. 1 is a kind of electron-microscope scanning of the lithium iron phosphate positive material preparation method embodiment one of polymer overmold of the present invention Figure；
Fig. 2 is the specific discharge capacity figure under 1C multiplying power of the embodiment of the present invention 1；
Fig. 3 is the specific discharge capacity figure that the embodiment of the present invention 1 recycles 20 times in different multiplying.
Specific embodiment
It is further described below by specific embodiment:
A kind of lithium iron phosphate positive material preparation method of polymer overmold is described in detail by taking embodiment one as an example below, makes Raw material is lithium acetate, frerrous chloride, phosphoric acid and pyrrole monomer, and other embodiment and comparative examples embody in table 1, The part that his embodiment and comparative example does not embody in table 1 is same as Example 1.
Embodiment one
A kind of lithium iron phosphate positive material preparation method of polymer overmold, comprising the following steps:
(1) according to lithium: iron: phosphorus molar ratio is that 3:1:1 weighs inorganic salt raw material, and it is molten that lithium source and phosphorus source be dissolved in ethylene glycol In agent, reacted at a temperature of 20 DEG C；
(2) source of iron and surfactant are added in the mixture that step (1) obtains, stirs evenly；
(3) mixed solution that step (2) obtains is transferred in reaction kettle, 18h is reacted at 180 DEG C and obtains LiFePO4 Powder；Iron phosphate powder is cooling, centrifuge separation, washing, are dried in vacuo 2h at 120 DEG C；
(4) oxidant is added in the iron phosphate powder that step (3) obtains and water is stirred mixing, add pyrrole It coughs up, the molar ratio of pyrroles and oxidant is 3:1, and the mass ratio of pyrroles and iron phosphate powder is 2:100；By obtained suspension Liquid stirs polymerization reaction 18h, alternately cleans 3-5 times, centrifuge separation to polymer acetone and water, 100 DEG C of vacuum drying 2h are obtained To polymer overmold lithium iron phosphate positive material.
Embodiment 1-5 is as shown in table 1.
Table 1
A kind of test of the lithium iron phosphate positive material of polymer overmold prepared by embodiment 1.
Positive electrode obtained and acetylene black, Kynoar bonding agent are mixed in the ratio of 80:12:8, with N- methyl Pyrrolidones (NMP) is solvent, stirs into homogeneous paste, and paste is coated on aluminium foil, is dried in vacuo 12 hours, tabletting, Positive plate is obtained, positive plate diameter is 10mm.Using lithium metal as cathode and to electrode, the LiPF containing 1mol/L is used6, carbonic acid second Alkene rouge (EC) and dimethyl carbonate (DMC) (volume ratio 1:1) organic mixed electrolytic solution, diaphragm are microporous polypropylene membrane produced in USA (Celgard2300), it is assembled into CR2032 button cell.Button cell is assembled in the glove box full of argon gas.Charge and discharge The BTS-5V 5mA tester that test is produced using new Weir Electronics Co., Ltd. of Shenzhen.Charging/discharging voltage range: 2.5- 4.2V.Specific discharge capacity under different current densities after each embodiment progress charge-discharge test is as shown in table 2.
Table 2
Embodiment 1 2 3 4 5
1C specific discharge capacity (mAh/g) 120 140 135 138 145
5C specific discharge capacity (mAh/g) 108 118 110 111 126
10C specific discharge capacity (mAh/g) 85 110 102 105 118
The test result of embodiment 1 is as shown in Figures 2 and 3.
From Fig. 1 it is observed that passing through the type and dosage of control surfactant, the high-crystallinity of special appearance is obtained Lithium iron phosphate nano stick, this is conducive to shorten the distance that lithium ion is moved in [0 1 0] crystal face along one-dimensional square, mention to reach The purpose of high material ions conductivity.Later by being coated in LiFePO4 particle surface upper one layer uniform high after in-situ polymerization Electric polypyrrole layer.The conducting polymer clad of suitable thickness can improve the high rate charge-discharge ability of LiFePO4, drop Low LiFePO4 under high current density the decaying of circulation volume, improve its high-multiplying power discharge specific capacity.
From Fig. 2 it can be observed that each embodiment carries out the specific discharge capacity after charge-discharge test, each reality under 1C multiplying power It applies example and shows excellent chemical property under 1C multiplying power, specific discharge capacity has reached 145mAh/g.
From Fig. 3 it is observed that having 118mAh/g electric discharge specific volume under the lithium iron phosphate positive material 10C of polymer overmold It measures, after charge and discharge cycles 20 times, capacity retention ratio is still higher than 98%.LiFePO4 can be improved in conductive polymer polypyrrole cladding The surface electronic conductivity of particle, the charge-discharge performance of compound and cycle performance have obtained obviously mentioning under higher current density It is high.
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented Effect and patent practicability.

Claims (7)

1. a kind of lithium iron phosphate positive material preparation method of polymer overmold, which comprises the following steps:
(1) according to lithium source: source of iron: the mole ratio of phosphorus source is 3~5:1:1 weighing inorganic salt raw material, and lithium source and phosphorus source is molten It is reacted in solvent；
(2) source of iron and surfactant are added in the mixture that step (1) obtains, stirs evenly；
(3) mixed solution that step (2) obtains is transferred in reaction kettle, 5~20h is reacted at 80~300 DEG C and obtains phosphoric acid Iron lithium powder；Iron phosphate powder is cooling, separation, washing, and be dried in vacuo；
(4) oxidant is added in the iron phosphate powder that step (3) obtains and water is stirred mixing, add pyrroles, pyrrole Coughing up with the molar ratio of oxidant is 3~5:1, and the mass ratio of pyrroles and iron phosphate powder is 2~20:100；It will be obtained outstanding Supernatant liquid stirring polymerization 16-20h, cleans polymer, is centrifugated, vacuum drying is obtaining polymer overmold LiFePO4 just Pole material.
2. a kind of lithium iron phosphate positive material preparation method of polymer overmold according to claim 1, which is characterized in that Range of reaction temperature in the step (1) is 20~60 DEG C.
3. a kind of lithium iron phosphate positive material preparation method of polymer overmold according to claim 1, which is characterized in that The surfactant of the step (2) is one of lauric acid, dodecyl sodium sulfate or neopelex.
4. a kind of lithium iron phosphate positive material preparation method of polymer overmold according to claim 1, which is characterized in that The dosage of surfactant of the step (2) is 0.5~5gL-1。
5. a kind of lithium iron phosphate positive material preparation method of polymer overmold according to claim 1, which is characterized in that Reaction temperature in the step (3) is 180 DEG C, reaction time 12h.
6. a kind of preparation method of the LiFePO4 of polymer overmold according to claim 1, which is characterized in that the step Suddenly the oxidant in (4) is one of ammonium persulfate, ferric trichloride or p-methyl benzenesulfonic acid iron.
7. a kind of preparation method of the LiFePO4 of polymer overmold according to claim 1, which is characterized in that step (1) solvent in is one of ethyl alcohol, ethylene glycol or water.
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CN112271293A (en) * 2020-08-14 2021-01-26 安徽德亚电池有限公司 Preparation method of high-conductivity lithium iron phosphate cathode material
CN114784249A (en) * 2022-04-29 2022-07-22 楚能新能源股份有限公司 Lithium iron phosphate composite positive electrode material and preparation method thereof
CN115714199A (en) * 2022-11-17 2023-02-24 楚能新能源股份有限公司 Lithium iron phosphate cathode material and preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112271293A (en) * 2020-08-14 2021-01-26 安徽德亚电池有限公司 Preparation method of high-conductivity lithium iron phosphate cathode material
CN114784249A (en) * 2022-04-29 2022-07-22 楚能新能源股份有限公司 Lithium iron phosphate composite positive electrode material and preparation method thereof
CN115714199A (en) * 2022-11-17 2023-02-24 楚能新能源股份有限公司 Lithium iron phosphate cathode material and preparation method and application thereof
CN115714199B (en) * 2022-11-17 2023-10-31 楚能新能源股份有限公司 Lithium iron phosphate positive electrode material, and preparation method and application thereof

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Application publication date: 20181218