CN104051731B - A kind of method that LiFePO4 is prepared in pollution-free zero-emission - Google Patents
A kind of method that LiFePO4 is prepared in pollution-free zero-emission Download PDFInfo
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- CN104051731B CN104051731B CN201410141204.7A CN201410141204A CN104051731B CN 104051731 B CN104051731 B CN 104051731B CN 201410141204 A CN201410141204 A CN 201410141204A CN 104051731 B CN104051731 B CN 104051731B
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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
- H01M4/58—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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- 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
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- 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 present invention relates to a kind of method that LiFePO4 is prepared in pollution-free zero-emission.The present invention has fully demonstrated environmental friendliness, sustainable development, free of contamination Green Chemistry, fine chemistry industry theory.Lithium source, source of iron, phosphorus source are dissolved, are mixed by the present invention under appropriate circumstances.By the control to synthesis conditioned response process, the LiFePO4 crystal of synthesis of high purity, and control the easily separated process of product different component, extract LiFePO4 crystal presoma and carry out inclusion, then carbonization annealing heat treatment；Remaining liquid and side-product carry out the green Posterior circle that processes and recycle, the energy recovery recycling of temperature-fall period.LiFePO 4 material chemical property prepared by this technique is good, and purity is high, good processability.Constituent content is reasonable, and batch is stable, it is most important that pollution-free zero-emission, it is simple to large-scale production.
Description
Technical field
The invention belongs to chemical industry synthetic material field, specifically the present invention relates to a kind of pollution-free zero-emission and prepare phosphoric acid
The green chemistry process method of ferrum lithium.
Background technology
AyMPO is disclosed first from the NTT of Japan in 19964(A is alkali metal, and M is the combination of both CoFe: LiFeCOPO4)
Olivine structural anode material of lithium battery after, within 1997, Texas, USA founds university John. B.
Goodenough etc. study group, it has been reported that LiFe PO4Olivine structural (LiM PO4), European have also discovered natural Fructus Canarii albi
The LiFePO of stone structure4。LiFePO4Also commercialization secondary battery material such as cobalt acid lithium, lithium nickelate, ternary it is found to have
Deng the superior function that material is incomparable.This material possesses that raw material sources is extensive, cheap, memory-less effect, circulates the longevity
Life is long, and security performance is good, and high-temperature behavior is good, without series of advantages such as heavy metal, non-environmental-pollutions.
Although LiFePO4There is plurality of advantages, be also considered as the most promising lithium ion secondary battery anode material, draw
Playing various countries' research and development manufacture energetically to this material, consequent patent and paper are the most too numerous to enumerate, and great majority research and development manufacture all
Only lay particular emphasis in the pursuit of material self performance and value, and have ignored one will as the whole world a new generation energy carrier materials
The produced pollution in production process.
But we but think the birth of a kind of new green energy resource, it should be from the aborning of it be all green
Rather than in order to obtain a kind of new green energy resource, before obtaining, just have resulted in serious environmental pollution, so may
Can be to lose more than gain.The LiFePO that traditional solid phase method and liquid phase method or microwave synthesize4, not only the time is long, and energy consumption is big, grain
Degree skewness, performance is undesirable, discharges substantial amounts of waste gas, the pollutant such as waste water, dust simultaneously, causes serious environment dirty
Dye.Traditional high temperature solid-state method uses Li2CO3+2FeC2O4+2NH4H2PO4= 2LiFePO4 +2NH3↑+5CO2↑+3H2O, often
Produce 1 ton of LiFePO4 It is necessary to produce about 350m3 CO2 Gas, the most also to produce about 153 m3 NH3Gas, these gas
Body all has the biggest pollution to air, and is difficult to recovery, the most a large amount of moisture discharge.These problems are entered by just
Row considers analysis, and planning of science activities devises a kind of pollution-free zero-emission and prepares the green chemistry process of high-quality LiFePO4
Method.
Summary of the invention
It is an object of the invention to provide a kind of method that LiFePO4 is prepared in pollution-free zero-emission, fully demonstrate environment friend
Good, sustainable development, free of contamination Green Chemistry, fine chemistry industry theory, by the control to synthesis conditioned response process, synthesis
Highly purified LiFePO4 crystal, carries out the green Posterior circle that processes and recycles remaining liquid and side-product.
The lithium iron phosphate preparation method of a kind of pollution-free zero-emission that the present invention provides, is characterized in that comprising the following steps:
First by H3 PO4、FeCl2And LiOH, weigh at 1: 1: 3 in molar ratio；The most respectively by load weighted H3 PO4、
FeCl2Dissolve in deionized water with LiOH supersaturation, form the H of molecular level3 PO4Precursor solution, FeCl2Precursor solution
With LiOH precursor solution, then by described H3 PO4Precursor solution adds in autoclave, and makes high pressure temperature in the kettle rise to
50-110 DEG C, then it is slowly added to FeCl2Precursor solution, makes H3 PO4Precursor solution and FeCl2Precursor solution mixing is all
After even, in described autoclave, it is passed through noble gas, in described autoclave, then adds LiOH precursor solution, then high pressure
Reaction i.e. FeCl is started to warm up in still2 + H3 PO4 + 3LiOH→2LiCl+ LiFePO4 ↓+ 3H2O, during temperature reaction
Making high pressure temperature in the kettle rise to 120-260 DEG C with 1-10 DEG C/min speed, in described autoclave, Stress control is at 0.2-4.7MPa,
Whole temperature reaction process continues 4-15 hour, material in autoclave does not stop during whole temperature reaction stirring, heats up
After completion of the reaction, carry out cold oil circulation by the heat-conducting oil furnace supporting with autoclave to make to lower the temperature speed with 1-20 DEG C/min in autoclave
Rate cooling down is to room temperature, and heat-conducting oil furnace carries out cold oil and follows the thermal energy storage of rear cold oil recovery and be cycled to used at follow-up concentration
Reason, then the material in autoclave by baiting valve and drainage pump introduce solid-liquid separating equipment isolate LiFePO4 crystal with
LiCl solution, fully washs LiFePO4 crystal water, then makees after the water deionization process of washing LiFePO4 crystal
Deionized water for cycling and reutilization uses, by LiCl solution by cell reaction i.e. 2H2O + 2Cl- = Cl2↑+ H2↑+
2OH-And 2H2O + 2LiCl = Cl2 ↑ + H2↑+2LiOH, the concentrated process of LiOH solution that will generate in cell reaction
Posterior circle is used for preparing LiFePO4 crystal, the chlorine generated is passed through in water generation hydrochloric acid, adds in hydrochloric acid in cell reaction
Enter iron powder and generate again FeCl2Solution, this FeCl2Solution concentration Posterior circle is used for preparing LiFePO4 crystal, by cell reaction
The hydrogen of middle generation provides heat energy as fuel gas buring for concentration and heating autoclave after collecting, and concentration produces
Water recycles as deionized water after deionization processes.
Further, after temperature reaction, material in autoclave carrying out solid-liquid separation, gained solid is LiFePO4
Crystal, washs isolated LiFePO4 crystal, keeps the percentage by weight of water in the LiFePO4 crystal after washing
30 80%, form LiFePO4 crystal suspension after washing, in LiFePO4 crystal suspension, then add clathrate,
The clathrate added is 1-2.5: 1 with the mol ratio of LiFePO4 crystal, and clathrate supersaturation is dissolved in LiFePO4 crystal and hangs
In turbid liquid, then pass through physical and chemical effect and make inclusion process complete under the mechanism that saturated solution and ultrasonic disperse interact, shape
Becoming LiFePO4 clathrate crystal presoma, clathrate process completes final vacuum or cold drying LiFePO4 clathrate crystal forerunner
Body, then LiFePO4 clathrate crystal presoma is added in inert atmosphere protection or vacuum drying oven, carry out high temperature cabonization annealing, carbon
Annealing temperature controls at 600 800 DEG C, and constant temperature time controls between 46 hours, uses air-cooled heat reclaim unit to make
Vacuum drying oven is down to room temperature the heat energy reclaiming in temperature-fall period, and the heat circulation of recovery is used for described concentration, finally obtains
The LiFePO4 crystal being coated with.
Further, described clathrate is hydroquinone or beta cyclodextrin.
The present invention by research that synthesis technique is become more meticulous, the scientific design to synthetic route, reasonable to side-product
Processing cycle utilizes.Electrochemical performances of lithium iron phosphate prepared by this technique is good, batch stable and consistent, good processability, energy
Enough be competent at the electrokinetic cell high requirement to positive electrode, and whole production process meet fine chemistry industry, green chemical concept without
Pollute.Method used in the present invention is pollution-free, does not produce three industrial wastes after recovery, and the product reclaimed all becomes former material
Material, directly utilizes, for reproduction next time, by making this manufacture of materials cost decline 1/3 after the recovery of this process cycles, and not
Produce and pollute.
Accompanying drawing explanation
Fig. 1 is the technological process rough schematic of the present invention；
Fig. 2 is the gram volume test figure of the LiFePO 4 material prepared by the present invention；
Fig. 3 is the multiplying power test figure of the LiFePO 4 material prepared by the present invention；
Fig. 4 is the cycle performance test figure of the LiFePO 4 material prepared by the present invention；
Fig. 5 is the particle size distribution figure of the LiFePO 4 material prepared by the present invention；
Fig. 6 is the XRD figure of the LiFePO 4 material prepared by the present invention.
Detailed description of the invention
Embodiment one
Referring to Fig. 1, the lithium iron phosphate preparation method of a kind of pollution-free zero-emission, it is characterized in that comprising the following steps:
First by H3 PO4、FeCl2And LiOH, weigh at 1: 1: 3 in molar ratio；The most respectively by load weighted H3 PO4、
FeCl2Dissolve in deionized water with LiOH supersaturation, form the H of molecular level3 PO4Precursor solution, FeCl2Precursor solution
With LiOH precursor solution, then by described H3 PO4Precursor solution adds in autoclave, and makes high pressure temperature in the kettle rise to
50 110 DEG C, then it is slowly added to FeCl2Precursor solution, makes H3 PO4Precursor solution and FeCl2Precursor solution mixing is all
After even, in described autoclave, it is passed through noble gas, in described autoclave, then adds LiOH precursor solution, then high pressure
Reaction i.e. FeCl is started to warm up in still2 + H3 PO4 + 3LiOH→2LiCl+ LiFePO4 ↓+ 3H2O, during temperature reaction
Making high pressure temperature in the kettle rise to 120-260 DEG C with 1-10 DEG C/min speed, in described autoclave, Stress control is at 0.2-4.7MPa,
Whole temperature reaction process continues 4-15 hour, material in autoclave does not stop during whole temperature reaction stirring, heats up
After completion of the reaction, carry out cold oil circulation by the heat-conducting oil furnace supporting with autoclave to make to lower the temperature speed with 1-20 DEG C/min in autoclave
Rate cooling down is to room temperature, and heat-conducting oil furnace carries out cold oil and follows the thermal energy storage of rear cold oil recovery and be cycled to used at follow-up concentration
Reason, then the material in autoclave by baiting valve and drainage pump introduce solid-liquid separating equipment isolate LiFePO4 crystal with
LiCl solution, fully washs LiFePO4 crystal water, then makees after the water deionization process of washing LiFePO4 crystal
Deionized water for cycling and reutilization uses, by LiCl solution by cell reaction i.e. 2H2O + 2Cl- = Cl2↑+ H2↑+
2OH-And 2H2O + 2LiCl = Cl2 ↑ + H2↑+2LiOH, the concentrated process of LiOH solution that will generate in cell reaction
Posterior circle is used for preparing LiFePO4 crystal, the chlorine generated is passed through in water generation hydrochloric acid, adds in hydrochloric acid in cell reaction
Enter iron powder and generate again FeCl2Solution, this FeCl2Solution concentration Posterior circle is used for preparing LiFePO4 crystal, by cell reaction
The hydrogen of middle generation provides heat energy as fuel gas buring for concentration and heating autoclave after collecting, and concentration produces
Water recycles as deionized water after deionization processes.
The detailed process of described cell reaction is as follows:
The device that described cell reaction uses is ion-exchange membrane electrolyzer, the cathode chamber of ion-exchange membrane electrolyzer and anode chamber's sun
Ion exchange membrane separates；Described LiCl solution enters anode chamber, H during energising20 electrolysis generates hydrogen, Li at cathode surface+From
Son passes through ionic membrane by anode chamber and OH-In conjunction with LiOH；LiOH is the raw material preparing LiFePO4；Cl-Ion is then at anode table
Face generates chlorine, by Cl2Being passed through in water generation chlorine water, chlorine water ultimately becomes hydrochloric acid after treatment, and hydrochloric acid and iron powder react generation
Ferrous chloride, ferrous chloride is also the raw material preparing LiFePO4.
The detailed equation of described cell reaction is as follows:
Anode: 2Cl- -2e-→Cl2 ↑, the Cl that anode pool produces2.By Cl2Being passed through in water generation chlorine water, chlorine water is treated
After ultimately become hydrochloric acid Fe+2HCl=FeCl2 + H2↑
Negative electrode: 2H++2e-→H2 ↑, the OH that cathode pool produces-Select through the Li come with cationic membrane+In conjunction with generating
LiOH.Such as OH-+ Li+ → LiOH
Overall reaction: 2H2O+2Cl-=Cl2 ↑+H2 ↑+2OH-and 2H2O+2LiCl=Cl2 ↑+H2
↑ + 2LiOH。
Steam produced by described concentration passes through condensing tower recycling.
Embodiment two
In the method step described by embodiment one, further, after temperature reaction, material in autoclave is entered
Row solid-liquid separation, gained solid is LiFePO4 crystal, is washed by isolated LiFePO4 crystal, after keeping washing
In LiFePO4 crystal, the percentage by weight of water is 30 80%, forms LiFePO4 crystal suspension, then to phosphoric acid after washing
Adding clathrate in ferrum crystalline lithium suspension, the clathrate of addition is 1-2.5: 1 with the mol ratio of LiFePO4 crystal, clathrate
Supersaturation is dissolved in LiFePO4 crystal suspension, then passes through physical and chemical effect and makes inclusion process saturated solution and ultrasonic point
Completing under the mechanism of dephasing interaction, form LiFePO4 clathrate crystal presoma, clathrate process completes final vacuum or low temperature
It is dried LiFePO4 clathrate crystal presoma, then LiFePO4 clathrate crystal presoma is added inert atmosphere protection or true
In empty stove, carrying out high temperature cabonization annealing, carbonization annealing temperature controls at 600 800 DEG C, constant temperature time control 46 hours it
Between, use air-cooled heat reclaim unit to make vacuum drying oven be down to room temperature the heat energy reclaiming in temperature-fall period, the heat circulation of recovery
For described concentration, finally obtain the LiFePO4 crystal being coated with.
Embodiment three
In the method step described by embodiment two, further, described clathrate is hydroquinone or β ring paste
Essence.
Detection is analyzed:
Entrust the detection that the global group in Xinxiang does, by the LiFePO 4 material of a kind of carbo-nitriding provided by the present invention
The preparation-obtained LiFePO 4 material of preparation method, after testing, the theoretical gram volume of LiFePO4 is 170mAH/g, this method
The LiFePO 4 material of preparation can stably accomplish 163mAH/g, tests figure accompanying drawing 2 referring specifically to gram volume；Phosphorus prepared by this method
The high rate performance of acid ferrum lithium material, the standard of European Union is that 1C charge and discharge is not less than 130mAH/g, domestic relatively do at present good
Can reach 1C charge and discharge 135mAH/g, and LiFePO 4 material prepared by this method, data are 1C charge and discharge 154mAH/g after testing
Left and right, tests figure accompanying drawing 3 referring specifically to multiplying power；It addition, the lattice stability of LiFePO 4 material prepared by this method is to pass through
Cycle performance embodies, the figure provided at present be 50 times undamped, referring specifically to Fig. 4；Further, this LiFePO 4 material material
The physical property of material, can directly be detected, including granularity, can be detected by laser fineness gage, and I divides with granularity
Butut i.e. Fig. 5；It is the purity of target product LiFePO4 and this product as this powder body material synthesized, Ke Yitong
Crossing XRD figure spectrum and carry out check analysis, I am also with XRD figure i.e. Fig. 6；Finally, the lot stability of this LiFePO 4 material, by pressing
According to the method that this technique is same, same condition, be repeated 10 times test, detection gram volume all between 158-163 mAH/g, ripple
Move about 3%, it is believed that lot stability concordance is controlled.
Claims (3)
1. a lithium iron phosphate preparation method for pollution-free zero-emission, is characterized in that comprising the following steps: first by H3 PO4、
FeCl2And LiOH, weigh at 1: 1: 3 in molar ratio；The most respectively by load weighted H3 PO4、FeCl2It is dissolved in LiOH supersaturation
In deionized water, form the H of molecular level3 PO4Precursor solution, FeCl2Precursor solution and LiOH precursor solution, then will
Described H3 PO4Precursor solution adds in autoclave, and makes high pressure temperature in the kettle rise to 50-110 DEG C, is then slowly added to
FeCl2Precursor solution, makes H3 PO4Precursor solution and FeCl2After precursor solution mix homogeneously, logical in described autoclave
Enter noble gas, in described autoclave, then add LiOH precursor solution, then start to warm up reaction in autoclave i.e.
FeCl2 + H3 PO4 + 3LiOH→2LiCl + LiFePO4 ↓+ 3H2O, makes high pressure temperature in the kettle with 1-during temperature reaction
10 DEG C/min speed rises to 120-260 DEG C, and in described autoclave, Stress control is at 0.2-4.7MPa, and whole temperature reaction process is held
Continuous 4-15 hour, during whole temperature reaction, material in autoclave is not stopped stirring, after temperature reaction, by with height
The pressure supporting heat-conducting oil furnace of still carries out cold oil circulation to be made in autoclave with 1-20 DEG C/min rate of temperature fall cooling down to room temperature, leads
Hot oil furnace carries out cold oil and follows the thermal energy storage of rear cold oil recovery and be cycled to used in follow-up concentration, then the thing in autoclave
Expect that introducing solid-liquid separating equipment by baiting valve and drainage pump isolates LiFePO4 crystal and LiCl solution, LiFePO4 is brilliant
Body water fully washs, then as the deionized water of cycling and reutilization after the water deionization process that LiFePO4 crystal will be washed
Use, by LiCl solution by cell reaction i.e. 2H2O + 2Cl- = Cl2↑+ H2↑+ 2OH-And 2H2O + 2LiCl = Cl2
↑ + H2↑+2LiOH, is used for preparing LiFePO4 brilliant by the LiOH solution concentrated process Posterior circle generated in cell reaction
Body, is passed through in water generation hydrochloric acid by the chlorine generated in cell reaction, adds iron powder and generate again FeCl in hydrochloric acid2Solution, should
FeCl2Solution concentration Posterior circle is used for preparing LiFePO4 crystal, the hydrogen generated is made after collecting in cell reaction
Being that concentration provides heat energy with heating autoclave for fuel gas buring, the water that concentration produces conduct after deionization processes is gone
Ionized water recycles.
The lithium iron phosphate preparation method of pollution-free zero-emission the most as claimed in claim 1, is characterized in that: will divide through described solid-liquid
Fully wash from equipment isolated LiFePO4 crystal water, keep the weight percent of water in the LiFePO4 crystal after washing
Ratio, 30 80%, forms LiFePO4 crystal suspension, then adds inclusion in LiFePO4 crystal suspension after washing
Thing, the clathrate of addition is 1-2.5: 1 with the mol ratio of LiFePO4 crystal, and clathrate supersaturation is dissolved in LiFePO4 crystal
In suspension, then pass through physical and chemical effect and make inclusion process complete under the mechanism that saturated solution and ultrasonic disperse interact,
Form LiFePO4 clathrate crystal presoma, before clathrate process completes final vacuum or cold drying LiFePO4 clathrate crystal
Drive body, then LiFePO4 clathrate crystal presoma added in inert atmosphere protection or vacuum drying oven, carry out high temperature cabonization annealing,
Carbonization annealing temperature controls at 600 800 DEG C, and constant temperature time controls, between 46 hours, to use air-cooled heat reclaim unit
Making vacuum drying oven be down to room temperature the heat energy reclaiming in temperature-fall period, the heat circulation of recovery is used for described concentration, finally obtains
The LiFePO4 crystal that must be coated with.
The lithium iron phosphate preparation method of pollution-free zero-emission the most as claimed in claim 2, is characterized in that: described clathrate is right
Benzodiazepines or beta cyclodextrin.
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| CN104600302A (en) * | 2015-01-27 | 2015-05-06 | 江苏华东锂电技术研究院有限公司 | Hot preparation technology of lithium iron phosphate solvent |
| CN104577122B (en) * | 2015-01-27 | 2017-02-22 | 江苏华东锂电技术研究院有限公司 | Lithium iron phosphate solvothermal preparation device |
| CN108609594B (en) * | 2018-03-29 | 2021-08-17 | 宁夏滨河新材料科技有限公司 | Method for treating and recycling wastewater in iron phosphate production |
| CN110615419A (en) * | 2019-07-01 | 2019-12-27 | 湖北虹润高科新材料有限公司 | Iron phosphate production facility |
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| CN101999187A (en) * | 2008-04-25 | 2011-03-30 | 住友大阪水泥股份有限公司 | Method for production of cathode active material for lithium ion battery, cathode active material for lithium ion battery produced by the method, electrode for lithium ion battery, and lithium ion battery |
| CN102356488A (en) * | 2009-03-27 | 2012-02-15 | 住友大阪水泥股份有限公司 | Method for producing positive electrode active material for lithium ion battery, positive electrode active material for lithium ion battery, electrode for lithium ion battery, and lithium ion battery |
| CN103080000A (en) * | 2010-09-03 | 2013-05-01 | 昭和电工株式会社 | Method for producing lithium metal phosphate |
| CN103258993A (en) * | 2013-04-24 | 2013-08-21 | 北京化工大学 | Preparation method of lithium iron phosphate powder for anode material of lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101999187A (en) * | 2008-04-25 | 2011-03-30 | 住友大阪水泥股份有限公司 | Method for production of cathode active material for lithium ion battery, cathode active material for lithium ion battery produced by the method, electrode for lithium ion battery, and lithium ion battery |
| CN102356488A (en) * | 2009-03-27 | 2012-02-15 | 住友大阪水泥股份有限公司 | Method for producing positive electrode active material for lithium ion battery, positive electrode active material for lithium ion battery, electrode for lithium ion battery, and lithium ion battery |
| CN103080000A (en) * | 2010-09-03 | 2013-05-01 | 昭和电工株式会社 | Method for producing lithium metal phosphate |
| CN103258993A (en) * | 2013-04-24 | 2013-08-21 | 北京化工大学 | Preparation method of lithium iron phosphate powder for anode material of lithium ion battery |
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