CN101826616A - Method for preparing lithium iron phosphate cathode material - Google Patents

Method for preparing lithium iron phosphate cathode material Download PDF

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Publication number
CN101826616A
CN101826616A CN201010161398A CN201010161398A CN101826616A CN 101826616 A CN101826616 A CN 101826616A CN 201010161398 A CN201010161398 A CN 201010161398A CN 201010161398 A CN201010161398 A CN 201010161398A CN 101826616 A CN101826616 A CN 101826616A
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iron
source
lithium
iron phosphate
described step
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唐昌平
郑金龙
关勇辉
蔡静
胡大伟
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ZHEJIANG RICHPOWER TECHNOLOGY Co Ltd
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ZHEJIANG RICHPOWER TECHNOLOGY Co Ltd
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    • 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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to a method for preparing lithium iron phosphate cathode material, which comprises the following steps that: 1) iron sources, lithium dihydrogen phosphate and carbon sources are weighed according certain proportions, wherein molar ratio of Fe to P in the iron sources and the lithium dihydrogen phosphate is 1:1 and the mass proportion of the carbon sources and the iron sources is 5-10 percent; 2) the iron sources, the lithium dihydrogen phosphate and the carbon sources are added in deionized water and are put into an agitator ball mill for grinding after being mixed to obtain precursor pulp with solid content of 20-40 percent; 3) the precursor pulp is delivered to a spray dryer through a metering pump for spray drying and granulation to obtain spherical precursor powder; and 4) the precursor powder is contained in a crucible and is put in a microwave oven for sintering under the protection of inert gas, and the sintered product is naturally cooled to room temperature to obtain. The invention has the advantages that the process is simple, the cost is low, the environment is protected, the method is suitable for producing stable-quality high-performance lithium iron phosphate material, the product prepared through the method has good electrochemical properties, the physical properties of the product are excellent, the powder particles are spherical, the fluidity is good, the specific area is small, the tap density is high and the workability is good.

Description

A kind of method for preparing lithium iron phosphate positive material
Technical field
The present invention relates to a kind of energy and material preparing technical field, especially a kind of method for preparing lithium iron phosphate positive material.
Background technology
The energy, information, material are called three of human modern civilization side by side and indicate greatly.Enter 21st century, the battery conduct the most mobile energy will be penetrated into social every nook and cranny, and always usefulness is omnipresent.On the one hand, as the energy of mobile electronic terminal equipment such as mobile phone, notebook computer, video camera, low-power battery has had significant progress.After particularly on behalf of the lithium ion battery of contemporary chemical power source state-of-the-art technology, nineteen ninety come out, because advantages such as it has the voltage height, volume is little, energy density is big, good cycle, self discharge are little, memory-less effect, occupy " 3C " market (Computer, Communication, Consumer) rapidly, be the gesture of standing like the legs of a tripod with Ni-MH battery, nickel-cadmium cell.Perfect day by day along with performance, lithium ion battery occupies a clear edge, can capture " 4C " market (Cordless Tools) very soon, and this initiates strong the impact to all small-sized secondary batteries markets.On the other hand, in the vehicle technology that forms coordinating resource, environmental protection and economic development, be the key that can the decision electric motor car industrialization as the secondary cell of its driving power.Lithium-ion-power cell with superior function is hopeful to satisfy the requirement of electric motor cars such as electric bicycle, battery-operated motor cycle and electric automobile most.
At present, lithium ion battery negative material and electrolyte system aspect obtain bigger progress, and the development of positive electrode relatively lags behind, and this has had a strong impact on the motorization process of lithium ion battery.It mainly shows as: the one, and safety problem, unique business-like positive electrode LiCoO 2Stable inadequately, can decompose when overheated overcharging, may cause battery explosion, this shows particularly outstanding on electrokinetic cell; The 2nd, the cost problem, the reserves of global cobalt are limited, because price is very high, limited LiCoO 2Application in electrokinetic cell; The 3rd, environmental problem, cobalt can cause certain infringement to environment and human body.Therefore, seek safety and stability more, raw material sources are more extensive and cheap, and more the positive electrode of environmental protection is pressing for of development lithium-ion-power cell.LiNiO 2Structure and LiCoO 2Similar, it has the advantage on price and the reserves, but has synthetic difficulty, structure easily undergoes phase transition and shortcoming such as poor stability.Even through doping vario-property, its actual possibility of its application is also little.Spinel-type LiMn 2O 4Having good, the easy advantage such as synthetic of fail safe, is one of more anode material for lithium-ion batteries of research at present.But LiMn 2O 4Theoretical capacity is lower, and has the John-Teller effect in the lattice, and easily recurring structure distortion causes capacity to decay rapidly in charge and discharge process, and particularly under the service condition of higher temperature, capacity attenuation is more outstanding.
Reported first such as Goodenough in 1997 have the LiFePO4 (LiFePO of olivine-type structure 4) can reversibly embed and the removal lithium embedded ion, have nontoxic, environmentally friendly, abundant, the advantages such as specific capacity is high, Heat stability is good, cycle performance excellence in raw material source, be considered to the most promising positive electrode.But there is following significant disadvantages in LiFePO4: Fe in (1) building-up process 2+Be oxidized to Fe easily 3+, be difficult to obtain the LiFePO4 of pure phase; (2) Li +Diffusion rate in LiFePO4 is low, causes the utilance of active material low; (3) permittivity of LiFePO4 itself is low, causes its high-rate charge-discharge capability poor.These shortcomings have seriously hindered the practical application of LiFePO 4 material.In recent years, along with to the going deep into of the various method researchs that improve its conductivity, the conductivity of such material has reached the invention level and has been subjected to people to be paid close attention to greatly.Improve one's methods and mainly contain: (1) adopts the inert gas shielding sintering, prevents Fe 2+Oxidation; (2) reduce the size of LiFePO4 crystal grain, shorten Li +Diffusion length, improve the ionic conductivity of material; (3) surperficial coated with conductive material or bulk phase-doped high volence metal ion, the electron conduction of raising material.
The main method of synthesizing iron lithium phosphate is a high temperature solid-state method at present.Be characterized in using ferrous oxalate (source of iron), ammonium dihydrogen phosphate (phosphorus source) and three kinds of raw materials of lithium carbonate (lithium source) through mixing and ball milling, sintering forms under inert atmosphere protection.This method mainly contains three significant disadvantages:
(1) the source of iron ferrous oxalate (FeC of Cai Yonging 2O 42H 2O) unstable in air, ferrous iron is oxidized to ferric iron easily.In addition, it contains the crystallization water, is difficult for accurately metering.The instability of raw material can be brought to product quality and seriously influence.Because the restriction of technology and equipment is difficult to three kinds of raw materials are mixed by stoichiometric proportion, thereby influence batch stability of product.
(2) owing to produce a large amount of gases in the production process, solid burns the mistake rate greater than 50%, and product structure is fluffy, and tap density is extremely low (has only 0.5g/cm 3).Improved high temperature solid-state method adopts sintering twice, all needs inert gas shielding.Be low temperature (about 350 ℃) sintering for the first time, remove gas a large amount of in the raw material reaction thing, form the fluffy intermediate of structure.After intermediate was handled through pulverizing, compound stalk forming etc., high temperature (about 700 ℃) double sintering 10～20h under inert gas shielding generated LiFePO4 again.
(3) for improving material activity, adopt wet ball grinding usually.Make solvent with inflammable organic substances such as absolute ethyl alcohol or acetone, the organic solvent volatilization can produce strong smell in the dry run, and causes disaster hidden-trouble easily; Except producing water and carbon dioxide, the ammonium dihydrogen phosphate decomposition can generate the ammonia that has the intense stimulus smell in a large number, and atmosphere is polluted in the sintering process.
Summary of the invention
The present invention will solve the shortcoming of above-mentioned prior art, and the method for preparing lithium iron phosphate positive material of a kind of simple controllable, energy-conserving and environment-protective, constant product quality is provided.
The present invention solves the technical scheme that its technical problem adopts: this method for preparing lithium iron phosphate positive material, carry out according to the following steps:
1) take by weighing source of iron, lithium dihydrogen phosphate and carbon source by a certain percentage, wherein Fe in source of iron and the lithium dihydrogen phosphate: the P mol ratio is 1: 1, and carbon source and source of iron mass ratio are 5～10%;
2) source of iron, lithium dihydrogen phosphate and carbon source are added deionized water, mix to be placed in the agitating ball mill and grinds, obtain solid content and be 20～40% precursor pulp;
3) precursor pulp is transported to spray dryer by measuring pump and carries out spray drying granulation, obtain spherical precursor powder grain;
4) precursor powder is packed into place microwave oven to carry out sintering in the crucible, naturally cool to room temperature and obtain product with inert gas shielding.
As preferably, source of iron is iron oxide red (Fe in the described step 1) 2O 3), iron oxide black (Fe 3O 4) or iron oxide yellow (Fe 2O 3H 2O), carbon source is acetylene black or superconduction carbon black.The effect of carbon source has three: one is the strong absorption microwave, and presoma is heated up rapidly; One is to serve as reducing agent, at high temperature ferric iron is reduced into ferrous iron; The 3rd, be coated on the conductivity that particle surface improves material.
As preferably, described step 2) grinding revolution in is 100～400 commentaries on classics/min, and milling time is 2～6h.
As preferably, spray inlet temperature is 240～350 ℃ in the described step 3), and outlet temperature is 100～150 ℃, and charging rate is 0.2～1L/min.Can wait and control the precursor powder granular size by adjustment grinding condition, slurry solid content, inlet temperature.
As preferably, the material of crucible is a graphite in the described step 4).Graphite energy strong absorption microwave can heat the presoma powder, and the graphite composition is a simple substance carbon simultaneously, can at high temperature can combine and provide reducing atmosphere with oxygen.
As preferably, the inert gas in the described step 4) is a high pure nitrogen, and ventilation flow rate is 1～5L/min, and sintering temperature is 600～800 degrees centigrade, and the constant temperature sintering time is 10～20min.Inert gas and prevent Fe 2+Oxidized.
Inventing useful effect is: one, because the employing deionized water is a solvent, DIC so have only water and amounts of carbon dioxide gas to produce in the whole process of production, belongs to the production technology of environmental protection as reducing agent; Two, simple, with low cost, the suitable stable high-performance iron phosphate lithium material of the quality of production of technology, the product of preparing with this method is except having better electrochemical performance, its every physical property is also preferable, powder granule is spherical in shape, good fluidity, specific surface is little, and the tap density height has better machining property.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 gained lithium iron phosphate positive material;
Fig. 2 is the SEM image of embodiment 1 gained lithium iron phosphate positive material;
Fig. 3 is the charging and discharging curve of embodiment 1 gained lithium iron phosphate positive material;
Embodiment
The invention will be further described below in conjunction with accompanying drawing:
Embodiment 1: take by weighing 3000g Fe 2O 3, 3905g LiH 2PO 4, 240g acetylene black, 13269g deionized water places agitating ball mill to grind 3h with 300 commentaries on classics/min, obtains solid content and be 35% brownish red suspension-turbid liquid, i.e. precursor pulp.With precursor pulp under continuous condition of stirring by measuring pump with the flow volume delivery of 0.5L/min atomizing disk to spray dryer, inlet temperature is set at 300 ℃, outlet temperature is set at 130 ℃, can obtain henna precursor powder from the powder gatherer.With the precursor powder graphite crucible of packing into, place to have the high pure nitrogen protection, gas flow is in the microwave oven of 2L/min, 700 ℃ of sintering 12min of constant temperature naturally cool to room temperature, can obtain the spherical LiFePO 4 powder material of black.The average grain diameter of powder granule is 7～10 μ m, and tap density is 1.2～1.3g/cm 3, specific area is 11～12m 2/ g.
Take by weighing 0.4g embodiment 1 gained LiFePO 4 powder, adding 0.05g acetylene black conductive agent and 0.05g are dissolved in polyvinylidene fluoride (PVDF) binding agent of N-methyl pyrrolidone (NMP), being mixed into slurry evenly is coated on Φ 15 aluminium foils and makes positive plate, with the metal lithium sheet is negative pole, polypropylene film (celgard2400) is a barrier film, the LiPF of 1mol/L 6EC+DEC (1: 1) solution be electrolyte, in being full of the glove box of argon gas, be assembled into button cell.Under the room temperature, the 0.1C constant current charge is to 4.2V, and constant voltage is to 0.02C, and the 0.1C constant-current discharge is to 2.5V again, and the specific capacity that records LiFePO4 is 146mAh/g.
Embodiment 2: take by weighing 2500g Fe 3O 4, 3367g LiH 2PO 4, 175g acetylene black, 14097g deionized water places agitating ball mill to grind 4h with 200 commentaries on classics/min, obtains solid content and be 30% black suspension, i.e. precursor pulp.With precursor pulp under continuous condition of stirring by measuring pump with the flow volume delivery of 0.4L/min atomizing disk to spray dryer, inlet temperature is set at 350 ℃, outlet temperature is set at 150 ℃, can obtain the precursor powder of black from the powder gatherer.With the precursor powder graphite crucible of packing into, place to have the high pure nitrogen protection, gas flow is in the microwave oven of 1L/min, 650 ℃ of sintering 15min of constant temperature naturally cool to room temperature, can obtain the spherical LiFePO 4 powder material of black.The average grain diameter of powder granule is 5～7 μ m, and tap density is 1.1～1.2g/cm 3, specific area is 13～14m 2/ g.The specific capacity that records LiFePO4 with the method for embodiment 1 is 149mAh/g.
Embodiment 3: take by weighing 3500g Fe 2O 3H 2O, 4094g LiH 2PO 4, 228g superconduction carbon black, 11732g deionized water place agitating ball mill to grind 6h with 400 commentaries on classics/min, obtains solid content and be 40% yellow suspension-turbid liquid, i.e. precursor pulp.With precursor pulp under continuous condition of stirring by measuring pump with the flow volume delivery of 0.6L/min atomizing disk to spray dryer, inlet temperature is set at 280 ℃, outlet temperature is set at 120 ℃, can obtain yellow precursor powder from the powder gatherer.With the precursor powder graphite crucible of packing into, place to have the high pure nitrogen protection, gas flow is in the microwave oven of 2L/min, 720 ℃ of sintering 10min of constant temperature naturally cool to room temperature, can obtain the spherical LiFePO 4 powder material of black.The average grain diameter of powder granule is 2～4 μ m, and tap density is 1.0～1.1g/cm 3, specific area is 16～17m 2/ g.The specific capacity that records LiFePO4 with the method for embodiment 1 is 152mAh/g.
In addition to the implementation, the present invention can also have other execution modes.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection range of requirement of the present invention.

Claims (7)

1. method for preparing lithium iron phosphate positive material is characterized in that carrying out according to the following steps:
1) takes by weighing source of iron, lithium dihydrogen phosphate LiH in proportion 2PO 4And carbon source, the wherein Fe in source of iron and the lithium dihydrogen phosphate: the P mol ratio is 1: 1, and carbon source and source of iron mass ratio are 5～10%;
2) source of iron, lithium dihydrogen phosphate and carbon source are added deionized water, mix to be placed in the agitating ball mill and grinds, obtain solid content and be 20～40% precursor pulp;
3) precursor pulp is transported to spray dryer by measuring pump and carries out spray drying granulation, obtain the spherical precursor powder grain;
4) the precursor powder is packed into place microwave oven to carry out sintering in the crucible, naturally cool to room temperature and obtain product with inert gas shielding.
2. the method for preparing lithium iron phosphate positive material according to claim 1 is characterized in that: source of iron is iron oxide red Fe in the described step 1) 2O 3, iron oxide black Fe 3O 4Or iron oxide yellow Fe 2O 3H 2O.
3. the method for preparing lithium iron phosphate positive material according to claim 1 is characterized in that: carbon source is acetylene black or superconduction carbon black in the described step 1).
4. the method for preparing lithium iron phosphate positive material according to claim 1 is characterized in that: grinding revolution described step 2) is 100～400 commentaries on classics/min, and milling time is 2～6h.
5. the method for preparing lithium iron phosphate positive material according to claim 1 is characterized in that: spray inlet temperature is 240～350 ℃ in the described step 3), and outlet temperature is 100～150 ℃, and charging rate is 0.2～1L/min.
6. the method for preparing lithium iron phosphate positive material according to claim 1 is characterized in that: the material of crucible is a graphite in the described step 4).
7. according to claim 1 or the 6 described methods that prepare lithium iron phosphate positive material, it is characterized in that: the inert gas in the described step 4) is a high pure nitrogen, ventilation flow rate is 1～5L/min, and sintering temperature is 600～800 degrees centigrade, and the constant temperature sintering time is 10～20min.
CN201010161398A 2010-04-28 2010-04-28 Method for preparing lithium iron phosphate cathode material Pending CN101826616A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101973539A (en) * 2010-10-28 2011-02-16 浙江瑞邦科技有限公司 Method for synthesizing lithium iron phosphate anode material at low cost
CN102107862A (en) * 2011-01-20 2011-06-29 铜陵金泰电池材料有限公司 Method for preparing lithium iron phosphate by using wood fibers as carbon source
CN102569737A (en) * 2010-12-30 2012-07-11 中国电子科技集团公司第十八研究所 Preparation method of lithium ion battery Li3V2(PO4)3/C composite cathode material
CN103050693A (en) * 2012-12-24 2013-04-17 彩虹集团公司 Preparation method for spherical LiMnPO4 anode material
CN103043639A (en) * 2012-12-24 2013-04-17 彩虹集团公司 Preparation method of spherical lithium iron phosphate anode materials
CN111217347A (en) * 2018-11-23 2020-06-02 深圳市贝特瑞纳米科技有限公司 High-compaction lithium iron phosphate material and preparation method thereof
CN115417394A (en) * 2022-09-20 2022-12-02 广西自贸区量孚新能源科技有限公司 Lithium iron phosphate material and preparation process and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101420034A (en) * 2008-06-02 2009-04-29 李庆余 Carbon coated granularity controllable spherical lithium ferric phosphate composite positive pole material and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101420034A (en) * 2008-06-02 2009-04-29 李庆余 Carbon coated granularity controllable spherical lithium ferric phosphate composite positive pole material and preparation method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101973539A (en) * 2010-10-28 2011-02-16 浙江瑞邦科技有限公司 Method for synthesizing lithium iron phosphate anode material at low cost
CN101973539B (en) * 2010-10-28 2012-01-25 浙江瑞邦科技有限公司 Method for synthesizing lithium iron phosphate anode material at low cost
CN102569737A (en) * 2010-12-30 2012-07-11 中国电子科技集团公司第十八研究所 Preparation method of lithium ion battery Li3V2(PO4)3/C composite cathode material
CN102107862A (en) * 2011-01-20 2011-06-29 铜陵金泰电池材料有限公司 Method for preparing lithium iron phosphate by using wood fibers as carbon source
CN103050693A (en) * 2012-12-24 2013-04-17 彩虹集团公司 Preparation method for spherical LiMnPO4 anode material
CN103043639A (en) * 2012-12-24 2013-04-17 彩虹集团公司 Preparation method of spherical lithium iron phosphate anode materials
CN111217347A (en) * 2018-11-23 2020-06-02 深圳市贝特瑞纳米科技有限公司 High-compaction lithium iron phosphate material and preparation method thereof
CN115417394A (en) * 2022-09-20 2022-12-02 广西自贸区量孚新能源科技有限公司 Lithium iron phosphate material and preparation process and application thereof
CN115417394B (en) * 2022-09-20 2023-12-12 上海量孚新能源科技有限公司 Lithium iron phosphate material and preparation process and application thereof

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Application publication date: 20100908