CN106876700B - Two steps are co-precipitated the method for preparing micro--nano porous structure ferric phosphate presoma and lithium iron phosphate positive material - Google Patents
Two steps are co-precipitated the method for preparing micro--nano porous structure ferric phosphate presoma and lithium iron phosphate positive material Download PDFInfo
- Publication number
- CN106876700B CN106876700B CN201610943742.7A CN201610943742A CN106876700B CN 106876700 B CN106876700 B CN 106876700B CN 201610943742 A CN201610943742 A CN 201610943742A CN 106876700 B CN106876700 B CN 106876700B
- Authority
- CN
- China
- Prior art keywords
- phosphate
- ferric
- reactor
- micro
- porous structure
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A kind of method that two steps coprecipitation prepares micro--nano porous structure ferric phosphate precursor and lithium iron phosphate positive material, it is characterised in that: step includes: continuous quickly preparation nanoscale iron phosphate primary particle presoma in first reactor；Nanoscale iron phosphate primary particle presoma aggregation group dress in second reactor generates the micron order ferric phosphate second particle of micro--nano porous structure；Micron order ferric phosphate second particle with micro-nano structure mixes lithium and calcining prepares lithium iron phosphate positive material.Advantage conductive and forthright good again, that voidage is high, particle diameter distribution is uniform, tap density is high, easy to process.
Description
Technical field
The present invention relates to technical field of material, and in particular to is co-precipitated using two steps of two kinds of different structure reactors
The method for preparing micro--nano porous structure ferric phosphate presoma and lithium iron phosphate positive material.
Background technique
1992, lithium ion battery was introduced market for the first time by Sony.Nowadays, lithium ion battery is used extensively
In field of portable devices such as mobile phone, computers, electric car field and other energy storage device fields.In numerous lithium-ion electrics
In the positive electrode of pond, the lithium iron phosphate positive material with olivine structural, because iron resource is abundant, nontoxic, inexpensive, Yi Jiyou
The advantages that good chemical property and good cycle performance, occupy in the development of lithium ion battery more and more importantly
Position.But the theoretical discharge capacity of lithium iron phosphate positive material is 170mAh g-1, and actual discharge capacity generally only has
110mAh g-1, this is because lower electronic conductivity (10-10~10-9S/cm), lithium ion diffusion coefficient (1.8 × 10- 14cm2/ S) the disadvantages of it is caused, these disadvantages also seriously restrict always lithium iron phosphate positive material in actual life and life
Application in production.
Summary of the invention
The present invention is directed to the above-mentioned deficiency of the prior art, provides a kind of electric conductivity and forthright good again, voidage height, partial size point
The two step coprecipitations that cloth is uniform, tap density is high, easy to process prepare micro--nano porous structure ferric phosphate precursor and ferric phosphate
The method of lithium anode material.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows: a kind of two step coprecipitations prepare it is micro--receive
The method of porous structure ferric phosphate precursor and lithium iron phosphate positive material, step include: continuous quickly system in first reactor
Standby nanoscale iron phosphate primary particle presoma；Nanoscale iron phosphate primary particle presoma aggregation group in second reactor fills
Generate the micron order ferric phosphate second particle of micro--nano porous structure；Micron order ferric phosphate second particle with micro-nano structure is mixed
Lithium and calcining prepare lithium iron phosphate positive material.
Continuous quickly preparation nanoscale iron phosphate primary particle presoma, specific steps in the above-mentioned first reactor of the present invention
Include:
(1.1) it weighs phosphate and trivalent iron salt is dissolved in deionized water, be each configured to the phosphorus of 0.1mol/L~3mol/L
The ferric salt solution of acid salt solution and 0.1mol/L~3mol/L；By the dense ammonia of 25-28% (mass percentage concentration of ammonia NH3)
Water dilutes the weak aqua ammonia for being configured to 0.1mol/L~3mol/L；
(1.2) phosphate-containing solution and ferric salt solution are injected by first reactor using peristaltic pump or metering pump
In, it is ensured that the molar ratio of phosphate radical and iron ion is 0.98~1.02:1；
(1.3) phosphate anion is quickly mixed and is reacted in first reactor with ferric ion, and breaks out nucleation, raw
At nano-scale lithium iron phosphate primary particle.
Molysite described in step (1.1) of the present invention is trivalent iron salt, such as ferric nitrate, iron chloride etc..
Phosphate described in step (1.1) of the present invention can be diammonium hydrogen phosphate, ammonium dihydrogen phosphate or phosphoric acid.
First reactor described in step (1.2) of the present invention is with high-intensitive microcosmic mixed, realizes explosion type
The characteristic of nucleation is mixed such as intensified by ultrasonic wave impact flow reactor, using ultrasonic wave with percussion flow reinforcing reactant.
The preparation of the micron order ferric phosphate second particle of the above-mentioned micro--nano porous structure of the present invention, specific preparation step include:
(2.1) mother liquor containing step (1.3) made nano-scale lithium iron phosphate primary particle is placed in second reactor,
The reaction was continued 1~60 hour under conditions of low whipping speed is 200-1500rpm；
(2.2) in the process, peristaltic pump is passed through phosphate solution into reaction kettle with certain flow rate and trivalent iron salt is molten
Liquid, and be slowly added to weak aqua ammonia and pH value is regulated and controled in 1.5~2.2 ranges；Temperature in second reactor is controlled at 50-70 DEG C；
With the progress of reaction, there are a large amount of pale yellow precipitates to generate in reaction solution.
The certain flow rate of above-mentioned steps (2.2) of the present invention is that 20-100rpm is equal to 4.34-21.7ml/min.
The features such as second reactor in step (2.1) of the present invention has reactor residence time long, is uniformly mixed, can
To be stirred tank reactor or Taylor's reactor.
The micron order ferric phosphate second particle of the above-mentioned micro-nano structure of the present invention mixes lithium method, and specific steps include:
(3.1) pale yellow precipitate obtained by abovementioned steps (2.2) is spent into ion-cleaning for several times, is placed in 80-120 DEG C
Drying box in dry, it is ground crush obtain have micro--nano porous structure ferric phosphate presoma powder；
(3.2) ferric phosphate presoma powder is mixed with Li source compound with the molar ratio of 1:0.98-1.08, and in ball
With the revolving speed ball milling of 200-800rpm 0.5-8 hours in grinding machine, uniformly mixed ferric phosphate and Li source compound mixture is obtained.
Li source compound can be lithium hydroxide or lithium carbonate in step (3.2) of the present invention.
The method that the above-mentioned calcining of the present invention prepares lithium iron phosphate positive material, specifically includes:
(4.1) by the ferric phosphate of abovementioned steps (3.2) preparation and Li source compound mixture and carbon original compound with phosphoric acid
Iron: carbon-source cpd=1:0.1-0.2 molar ratio uniformly mixes；Under nitrogen or other inert atmospheres, in 650-750 DEG C
It is calcined 3-20 hours under hot conditions, the lithium iron phosphate positive material of micro--nano porous structure is made.
Carbon-source cpd in step (4.1) of the present invention can be starch, sucrose or carbon dust etc..
The advantages of the present invention:
1. the present invention uses specific processing step: (1) in the first reactor with quick microcosmic mixed, such as
Intensified by ultrasonic wave impact flow reactor, quick mixed reactant are reacted, are precipitated, and generate even-grained nanoscale phosphorus
Sour iron primary particle；(2) in second reactor, such as stirred reactor or Taylor's reactor, reactant and aforementioned system is added
Standby nanoscale iron phosphate primary particle, reacts, precipitates, and aggregation group fills nanoscale iron phosphate primary particle, and generation has
The ferric phosphate second particle of micro--nano porous structure.And the preparation step of corresponding lithium iron phosphate positive material includes: (3) carbon packet
Cover the ferric phosphate precursor of micro-/nano porous structure；(4) ferric phosphate precursor is mixed with lithium source, and sintering is preparing LiFePO4 just
Pole material.The technique ensure that preparing for quick, the accurate effect of the intermediate products of each step, improve production efficiency.
2. high-tap density prepared by the present invention it is micro--receive the spherical ferrous phosphate and its positive electrode of package assembly,
I.e. with the satisfactory electrical conductivity of nano-scale lithium iron phosphate and forthright again, and solves low scarce of nano-scale lithium iron phosphate tap density
Point.Compared to ferrous phosphate obtained by traditional co-precipitation method and its positive electrode particle, micron order positive electrode tool prepared by the present invention
Have that porosity is high, particle diameter distribution is uniform, tap density is high, easy to process.Also, preparation method simple process of the invention, at
The advantages that this is low, product morphology controllable.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of the ferric phosphate presoma of preparation
Fig. 2 is scanning electron microscope (SEM) figure of the ferric phosphate presoma individual particle of preparation
The BET specific surface area and lacunarity analysis instrument figure of Fig. 3 ferric phosphate presoma
Fig. 4 is X-ray diffraction (XRD) figure of the ferric lithium phosphate precursor of preparation
Fig. 5 is scanning electron microscope (SEM) figure of the carbon-coated LiFePO 4 for lithium ion batteries of preparation
Fig. 6 is X-ray diffraction (XRD) figure of the LiFePO4 of preparation
Fig. 7 is the corresponding button cell charge and discharge electrograph of the carbon-coated LiFePO 4 for lithium ion batteries of preparation
Specific embodiment
The present invention is described in further detail below by embodiment, but the present invention is not limited solely to following embodiment.
Embodiment
1. accurately weighed using assay balance nine water ferric nitrates (410.14g, 98.5%) and diammonium hydrogen phosphate (133.39g,
99%) it, is dissolved in deionized water respectively, stirring and dissolving is simultaneously filtered to remove insoluble matter impurity, and the ferric nitrate for being prepared into 1mol/L is molten
Liquid and 1mol/L ammonium dibasic phosphate solution；
2. by prepared nine water iron nitrate solution and ammonium dibasic phosphate solution respectively through being located at intensified by ultrasonic wave percussion flow
The throat-fed of reactor two sides, wriggling revolution speed are uniformly that 57.6rpm (12.5ml/min) starts to surpass in the process
Sound pattern carries out continuous ultrasound to the solution for entering impact flow reactor with 20kHz frequency；
3. the reaction mother liquor of the primary particle containing nanoscale iron phosphate leave enter after impact flow reactor stirred autoclave after
Continuous reaction 24 hours；In the process, controlling reaction temperature in reaction kettle is 50-70 DEG C；Controlling rotating speed of agitator is
1500rpm；PH 1.90-2.00 is controlled by the addition of 3mol/L ammonium hydroxide；Ammonium dibasic phosphate solution and nine water iron nitrate solutions are logical
The feed pipe crossed inside stirred autoclave is persistently fed, and control feed rate is 0.5-2rpm.With the progress of reaction, instead
Answering in liquid has a large amount of pale yellow precipitates to generate.
4. reaction solution is filtered, and be washed with deionized for several times, obtained after drying it is micro--receive multistage porous structure ferric phosphate
Presoma (as illustrated in fig. 1 and 2).It is measured through particle size analyzer Bettersizer 2000, the ferric phosphate forerunner synthesized using the method
Body second particle average grain diameter is 5.878um.It is measured through BET, the ferric phosphate presoma primary particle synthesized using the method is flat
Equal partial size is 44.60nm, specific surface area 134.54m2 g-1.As shown in Figure 3, micro--to receive multistage porous structure ferric phosphate presoma
Hole be concentrated mainly on 2-50nm.This hole helps to improve the contact area of lithium iron phosphate positive material and electrolyte, from
Hold the conductivity for improving LiFePO4.
5. micro--multistage porous structure ferric phosphate precursor powder of receiving is put into groom's furnace, calcines 8 hours, obtain at 750 DEG C
Have crystalline texture it is micro-/receive multistage porous structure ferric phosphate presoma, and X-ray diffraction (XRD) measurement (such as Fig. 3 is carried out to it
It is shown).It is surely closed through calcined ferric phosphate XRD diagram and hexagonal crystal system ferric phosphate standard card PDF#29-0715, it was demonstrated that after calcining
Sample be pure phase six side's ferric phosphates
6. it is micro--receive Li source compound and carbon-source cpd be added in multistage porous structure ferric phosphate precursor powder, make
Lithium, iron and carbon molar ratio are 1.05:1:0.1, and obtained mixture carries out ball milling, drum's speed of rotation 400rpm.Ball milling
After 6h, mixture be placed in nitrogen atmosphere in 650-750 DEG C high-temperature calcination 6-8 hours, obtain it is micro--receive multilevel structure LiFePO4
Positive electrode, tap density 1.53g/cm-3It is measured scanning electron microscope (SEM, Fig. 5) and X-ray diffraction (XRD,
Fig. 6) measure.As shown in fig. 6, the LiFePO4 standard card PDF#97- of the diffraction maximum of sample and peak and olivine-type structure
015-4117 is consistent, that is, the sample synthesized is the LiFePO4 for the orthorhombic system olivine structural that space group is Pnmb.
The resulting carbon-coated LiFePO 4 for lithium ion batteries positive electrode of 0.8g is weighed, 0.15g acetylene black is added as conductive agent and 0.05g
PVDF (polyvinyladine floride) makees adhesive, uniformly mixes and is coated on aluminium foil in solvent NMP (N-Methyl pyrrolidone) and is made
Make anode.After CR2032 button cell is made in anode with carbon-coated LiFePO 4 for lithium ion batteries, 0.1C first discharge specific capacity is
130.47mAhg-1, 0.2C first discharge specific capacity is 128.88mAhg-1, 0.5C first discharge specific capacity is 116.39mAhg-1,
1C first discharge specific capacity is 96.70mAhg-1(as shown in Figure 6).
Above-described embodiment prove high-tap density prepared by the present invention it is micro--receive package assembly spherical ferrous phosphate and
Its positive electrode, the i.e. satisfactory electrical conductivity with nano-scale lithium iron phosphate with it is forthright again, and solve nano-scale lithium iron phosphate vibration
The low disadvantage of real density.Compared to ferrous phosphate obtained by traditional co-precipitation method and its positive electrode particle, micron prepared by the present invention
Grade positive electrode is high with porosity, particle diameter distribution is uniform, tap density is high, easy to process.Also, preparation method of the invention
The advantages that simple process, at low cost, product morphology controllable.
Claims (5)
1. a kind of two steps are co-precipitated the method for preparing micro--nano porous structure ferric phosphate presoma and lithium iron phosphate positive material,
Be characterized in that: step includes: continuous quickly preparation nanoscale iron phosphate primary particle presoma in first reactor；Nanoscale phosphorus
Sour iron primary particle presoma aggregation group dress in second reactor generates micron order ferric phosphate secondary of micro--nano porous structure
Grain；Micron order ferric phosphate second particle with micro-nano structure mixes lithium and calcining prepares lithium iron phosphate positive material；
Continuous quickly preparation nanoscale iron phosphate primary particle presoma, specific steps include: in the first reactor
(1.1) it weighs phosphate and trivalent iron salt is dissolved in deionized water, be each configured to the phosphate of the mol/L of 0.1 mol/L ~ 3
The ferric salt solution of solution and the mol/L of 0.1 mol/L ~ 3；The concentrated ammonia liquor that the mass percentage concentration of ammonia is 25-28% is diluted
It is configured to the weak aqua ammonia of the mol/L of 0.1 mol/L ~ 3；
(1.2) phosphate-containing solution and ferric salt solution are injected into first reactor using peristaltic pump or metering pump, really
The molar ratio for protecting phosphate radical and iron ion is 0.98 ~ 1.02:1；
(1.3) phosphate anion is quickly mixed and is reacted in first reactor with ferric ion, and breaks out nucleation, and generation is received
Meter level LiFePO4 primary particle；
The micron order ferric phosphate second particle of the micro--nano porous structure of generation, specific preparation step include:
(2.1) mother liquor containing step (1.3) made nano-scale lithium iron phosphate primary particle is placed in second reactor, stirred
Speed is mixed as the reaction was continued 1 ~ 60 hour under conditions of 200-1500 rpm；
(2.2) in the process, peristaltic pump is passed through phosphate solution and ferric salt solution into reaction kettle with certain flow rate, and
Weak aqua ammonia is slowly added to regulate and control in 1.5 ~ 2.2 ranges pH value；Temperature in second reactor is controlled at 50-70 DEG C；With anti-
The progress answered has in reaction solution a large amount of pale yellow precipitates to generate；
The micron order ferric phosphate second particle of the micro-nano structure mixes lithium and calcining prepares lithium iron phosphate positive material, specifically
Step includes:
(3.1) pale yellow precipitate obtained by abovementioned steps (2.2) is spent into ion-cleaning for several times, is placed in 80-120 DEG C
It is dried in drying box, it is ground to crush the ferric phosphate presoma powder for obtaining and there is micro--nano porous structure；
(3.2) ferric phosphate presoma powder is mixed with Li source compound with the molar ratio of 1:0.98-1.08, and in ball milling
With the revolving speed ball milling of 200-800rpm 0.5-8 hours in machine, uniformly mixed ferric phosphate and Li source compound mixture is obtained；
(4.1) by the ferric phosphate of abovementioned steps (3.2) preparation and Li source compound mixture and carbon original compound with ferric phosphate: carbon
Source compound=1:0.1-0.2 molar ratio uniformly mixes；Under nitrogen or other inert atmospheres, in 650-750 DEG C of high temperature item
It is calcined 3-20 hours under part, the lithium iron phosphate positive material of micro--nano porous structure is made；
First reactor described in step (1.2) is intensified by ultrasonic wave impact flow reactor；The second reaction in step (2.1)
Device is stirred tank reactor or Taylor's reactor.
2. two steps co-precipitation according to claim 1 is preparing micro--nano porous structure ferric phosphate presoma and LiFePO4 just
The method of pole material, it is characterised in that: trivalent iron salt described in step (1.1) is ferric nitrate or iron chloride；Step (1.1)
Described in phosphate be diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
3. two steps co-precipitation according to claim 1 is preparing micro--nano porous structure ferric phosphate presoma and LiFePO4 just
The method of pole material, it is characterised in that: the certain flow rate of step (2.2) is 4.34-21.7 ml/min.
4. two steps co-precipitation according to claim 1 is preparing micro--nano porous structure ferric phosphate presoma and LiFePO4 just
The method of pole material, it is characterised in that: lithium source chemical combination is lithium hydroxide or lithium carbonate in step (3.2).
5. two steps co-precipitation according to claim 1 is preparing micro--nano porous structure ferric phosphate presoma and LiFePO4 just
The method of pole material, it is characterised in that: the carbon-source cpd in step (4.1) is starch, sucrose or carbon dust.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610943742.7A CN106876700B (en) | 2016-11-02 | 2016-11-02 | Two steps are co-precipitated the method for preparing micro--nano porous structure ferric phosphate presoma and lithium iron phosphate positive material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610943742.7A CN106876700B (en) | 2016-11-02 | 2016-11-02 | Two steps are co-precipitated the method for preparing micro--nano porous structure ferric phosphate presoma and lithium iron phosphate positive material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106876700A CN106876700A (en) | 2017-06-20 |
| CN106876700B true CN106876700B (en) | 2019-10-01 |
Family
ID=59239468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610943742.7A Active CN106876700B (en) | 2016-11-02 | 2016-11-02 | Two steps are co-precipitated the method for preparing micro--nano porous structure ferric phosphate presoma and lithium iron phosphate positive material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106876700B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109835879B (en) * | 2017-11-24 | 2020-07-07 | 成都开飞高能化学工业有限公司 | Preparation method of submicron lithium iron phosphate cathode material |
| CN108557794A (en) * | 2018-04-28 | 2018-09-21 | 贵州贵航新能源科技有限公司 | A kind of preparation method of porous calcium phosphate iron nano powder |
| CN110021752B (en) * | 2019-01-24 | 2022-10-25 | 湖北锂诺新能源科技有限公司 | Lithium, aluminum and fluorine co-doped lithium iron phosphate cathode material and preparation method thereof |
| CN110835122A (en) * | 2019-12-16 | 2020-02-25 | 杨杭福 | Method for preparing perovskite magnetic refrigeration material by using Lobed type Taylor reactor |
| CN111762767B (en) * | 2020-07-29 | 2022-11-18 | 中国药科大学 | Method for simultaneously preparing iron phosphate with micro-nano porous structure and 5-hydroxymethylfurfural, material obtained by method and application of material |
| CN113603071B (en) * | 2021-07-23 | 2023-11-03 | 广东邦普循环科技有限公司 | Nanometer flaky ferric phosphate and preparation method and application thereof |
| CN114014290B (en) * | 2021-11-30 | 2022-11-29 | 中钢天源股份有限公司 | Method and equipment for preparing stable iron phosphate at low cost |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102556994A (en) * | 2011-12-02 | 2012-07-11 | 江西赣锋锂业股份有限公司 | Preparation method of nanoscale iron phosphate |
| CN102583292A (en) * | 2011-01-11 | 2012-07-18 | 中国科学院宁波材料技术与工程研究所 | Ferric phosphate having micro-nano structure and preparation method thereof as well as lithium iron phosphate material |
| CN102695760A (en) * | 2009-09-18 | 2012-09-26 | A123***公司 | Ferric phosphate and methods of preparation thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101253319B1 (en) * | 2010-09-10 | 2013-04-10 | 국립대학법인 울산과학기술대학교 산학협력단 | Positive active material for rechargeable lithium battery, method of preparing the same, and rechargeable lithium battery including the same |
-
2016
- 2016-11-02 CN CN201610943742.7A patent/CN106876700B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102695760A (en) * | 2009-09-18 | 2012-09-26 | A123***公司 | Ferric phosphate and methods of preparation thereof |
| CN102583292A (en) * | 2011-01-11 | 2012-07-18 | 中国科学院宁波材料技术与工程研究所 | Ferric phosphate having micro-nano structure and preparation method thereof as well as lithium iron phosphate material |
| CN102556994A (en) * | 2011-12-02 | 2012-07-11 | 江西赣锋锂业股份有限公司 | Preparation method of nanoscale iron phosphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106876700A (en) | 2017-06-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106876700B (en) | Two steps are co-precipitated the method for preparing micro--nano porous structure ferric phosphate presoma and lithium iron phosphate positive material | |
| CN108878818B (en) | Core-shell structure nickel-cobalt-manganternary ternary anode material presoma and preparation method thereof | |
| CN101443273B (en) | Preparation method of lithium-metal composite oxides | |
| CN101145611B (en) | Lithium ion cell anode material lithium vanadium phosphate preparation method | |
| CN102348634B (en) | Method for producing iron lithium phosphate | |
| CN101106194B (en) | Cathode material Li3V2(PO4)3 of lithium ion battery and its making method | |
| CN101789507B (en) | Electrode active material for anion-deficient lithium transition metal phosphate compound, method of preparing same, and electrochemical device using same | |
| CN102173403B (en) | Preparation method of micro-nano lithium ferric phosphate (LiFePO4) positive electrode material of lithium-ion battery | |
| CN101693532B (en) | Method for preparing lithium ferrous phosphate | |
| CN101478045B (en) | Preparation for high vibration high density lithium iron phosphate | |
| CN107359318A (en) | The method for synthesizing spherical loose structure ferric phosphate presoma and lithium iron phosphate positive material | |
| CN100503453C (en) | Preparation method of nickel magnesium cobalt hydroxide | |
| CN103825024B (en) | A kind of battery-grade iron phosphate and preparation method thereof | |
| CN102110814B (en) | Preparation method of lithium iron phosphate and battery anode | |
| CN110085858A (en) | A kind of nickelic tertiary cathode material of niobium-phosphor codoping and its preparation method and application | |
| CN105036103A (en) | Preparation method of cuboid lithium battery anode lithium ferric manganese phosphate material | |
| CN105118983A (en) | Method for preparing lithium nickel manganese oxide anode material | |
| CN101891180A (en) | Method for preparing sub-micrometer lithium iron phosphate (LiFePO4) | |
| CN103427081A (en) | Simple preparation method for FePO4 | |
| Dai et al. | Influence of anion species on the morphology of solvothermal synthesized LiMn0. 9Fe0. 1PO4 | |
| CN100483809C (en) | Method for producing ultra-fine LiFePO4/C of lithium ion battery anode material | |
| CN104485441B (en) | A kind of quaternary metal phosphate anode material for lithium-ion batteries and preparation method thereof | |
| CN103346315B (en) | A kind of take mesoporous carbon CMK-3 as the preparation method of the carbon-coated LiFePO 4 for lithium ion batteries material of carbon source | |
| CN101673821A (en) | Method for preparing manganese phosphate lithium/carbon composite material by using manganese hydrogen phosphate | |
| CN107275593B (en) | Method for preparing elliptical micro/nano porous structure substance and lithium iron phosphate positive electrode material by two-step hydrothermal method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |