CN102315450A - Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate - Google Patents
Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate Download PDFInfo
- Publication number
- CN102315450A CN102315450A CN201110253634A CN201110253634A CN102315450A CN 102315450 A CN102315450 A CN 102315450A CN 201110253634 A CN201110253634 A CN 201110253634A CN 201110253634 A CN201110253634 A CN 201110253634A CN 102315450 A CN102315450 A CN 102315450A
- Authority
- CN
- China
- Prior art keywords
- source
- iron phosphate
- lithium
- mixed solution
- deionized water
- 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.)
- Pending
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate. Iron source, nickel source, organic acid and phosphorus source are dissolved in deionized water according to a certain proportion, added with a dispersing agent, and mixed to obtain a mixed solution; lithium source which is uniformly dissolved in deionized water is dropwise and slowly added into the mixed solution; a pH is adjusted to 7.5-8.2 after dropping; the obtained alkalescent mixed solution is transferred to an autoclave; the autoclave is enclosed and insulated at 80-220 DEG C for 1 h-3 h; after cooling the autoclave is opened, and products are taken out, filtered with deionized water for several times and washed; an obtained filter cake is dried; then the obtained nickelic lithium iron phosphate powder and carbon contained organic compound in a mass ratio of 10:1-4 are treated with ball-milling for 1-3 h in alcohol, dried and sintered for 1-4 h at 600-800 DEG C under protection of nitrogen to obtain the product.
Description
Technical field
The present invention relates to the preparation of anode material for lithium-ion batteries, the hydro-thermal of definite a kind of ion doping high-performance iron phosphate lithium of saying so is synthesized preparation method.
Background technology
In early 1990s, after lithium rechargeable battery is succeeded in developing by Japanese SONY company, just become the focus of whole world research.Compare with lead acid accumulator, nickel-cadmium cell and nickel-hydrogen cell, lithium rechargeable battery has that operating voltage height, specific energy are high, volume is little, memory-less effect and advantage such as have extended cycle life.At present, lithium rechargeable battery is widely used in the portable electric appts such as mobile phone, notebook computer and video camera; Simultaneously suitable application prospect is also arranged in fields such as electric automobile, Aeronautics and Astronautics and space technologies.The maximum anode material for lithium-ion batteries that uses at present is the transition metal oxide LiCoO of stratiform
2Material.In addition the positive electrode that is used for lithium ion battery also has LiNiO
2, spinel-type compound L iMn
2O
4Deng material.From the charging/discharging voltage of material, discharge and recharge the performance of aspects such as invertibity, efficiency for charge-discharge, discharge capacity, LiCoO
2Material is to be suitable as very much anode material for lithium-ion batteries, and its unique deficiency is that cost is too high, LiNiO
2Material has and LiCoO
2The structure that material is identical, stratiform LiNiO
2Material is very difficult to synthesize; LiMn
2O
4The theoretical capacity that is exactly it is less, and cycle performance is bad.
LiFePO
4Theoretical capacity be 170mAh/g, discharge platform 3.4V and since lithium deviate from telescopiny in do not have change in volume, discharge and recharge under the high temperature and do not disengage active oxygen, have good cyclicity and fail safe, these advantages promote LiFePO
4The development of positive electrode.But the electronic conductivity of LiFePO4 is extremely low, is merely 10-7～10-9S/cm under the room temperature, belongs to a kind of semi-conducting material; Moreover the lithium ion diffusion rate of this material also not as people's will, makes its capacity when high current charge-discharge descend rapidly, and high rate capability is poor, and LiFePO
4The preparation process in have complex process, shortcoming such as power consumption is big, cost is high, consistency of performance difference and distribution of particles are inhomogeneous, thereby restricted LiFePO
4Practical application
Solve LiFePO
4Low and the slow problem of ions diffusion of conductivity, the approach of research approval at present mainly contains two:
1, coats synthetic LiFePO through ion doping and carbon
4/ C composite material or strengthen its conductivity through other approach;
2, prepare the LiFePO that particle diameter is little and be evenly distributed
4Particle is to reduce the evolving path of lithium ion.Develop that a kind of technology is simple, the synthesis technique of even particle distribution, function admirable, solve LiFePO
4One of difficult problem that the development of positive electrode is met.
Summary of the invention
The object of the present invention is to provide that a kind of technology is simple, the synthetic preparation method of hydro-thermal of the ion doping high-performance iron phosphate lithium that is easy to control.
The present invention adopts following technical scheme:
The invention is characterized in that it may further comprise the steps:
A, source of iron, nickel source, organic acid and phosphorus source are dissolved in the deionized water according to a certain percentage, are incorporated as 1%～10% dispersant of ion doping high-performance iron phosphate lithium product theoretical yield, constantly stir; Get mixed solution; The lithium source that will evenly be dissolved in deionized water more slowly is added drop-wise in the mixed solution, Li:Fe:Ni:P=3～3.5:1-x:x:1～1.2 wherein, x=0.01～0.06; Drip and finish adjusting PH to 7.5～8.2, back, get the alkalescent mixed solution;
B, A step gained alkalescent mixed solution is transferred in the autoclave, the capping still is at 80 ℃～220 ℃ insulation 1h～3h down; After the cooling, take out reaction product, with the product filtration washing; Again that the gained filter cake is dry under 50 ℃～100 ℃, obtain nickeliferous iron phosphate powder;
C, with the nickeliferous iron phosphate powder of step B gained and carbon containing organic compound according to mass ratio 10:1～4 ball milling 1～3h in alcohol, 50 ℃～100 ℃ dry down, under nitrogen protection,, promptly get product again in 600 ℃～800 ℃ sintering 1～4h.
Described nickel source is nickel acetate or nickel chloride; Described source of iron is ferrous sulfate or frerrous chloride, and described organic acid is a kind of in maleic acid, citric acid and the ascorbic acid, and described dispersant is a polyvinyl alcohol; In the polyacrylamide one or both; Described phosphorus source is phosphoric acid or ammonium dihydrogen phosphate, and described lithium source is lithium hydroxide or lithium acetate, and described carbon containing organic compound is a kind of in maleic acid, sucrose and the starch.
The hydro-thermal of described a kind of ion doping high-performance iron phosphate lithium is synthesized preparation method, it is characterized in that: use 40 ℃～50 ℃ deionized water in the filter operation described in the step B, the drying among step B and the step C is all carried out in a vacuum.
Beneficial effect of the present invention is:
The present invention directly reacts under the environment of hydro-thermal through reaction raw materials and makes, and in reaction, adds metal ion, adds the dispersion of dispersant in mixed solution, and whole process control is simple, circulation timei is short and energy consumption is little.Resulting nickel ion doped iron phosphate lithium even particle distribution, chemical property is superior.This method synthesis technique of the present invention is simple, and energy consumption is low, and efficient is high; The even particle distribution of prepared nickel ion doped iron phosphate lithium material, good crystallinity, discharge platform is more smooth; Multiplying power and cycle performance are high, and the 0.2C discharge capacity is 158.9mAh/g, can be used for anode material of lithium battery.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 product;
Fig. 2 is the charge and discharge curve of the 0.2C multiplying power of embodiment 1 product;
Fig. 3 is the cycle performance of embodiment 1 product different multiplying.
Embodiment
In conjunction with following specific embodiment, the present invention is explained further details.
Embodiment 1
A): referring to Fig. 1-Fig. 3, with the FeSO of 1021.65g
47H
2O, 9.73gNiCl
2, 100g ascorbic acid and 432.5g content is 85% H
3PO
4Mix, add the polyvinyl alcohol of 5.925g, add the 2.5L deionized water again, the stirring that does not stop then,
Simultaneously with 472gLiOHH
2O (analyzing pure) is dissolved in the deionized water of 2.5L, stir lithia solution, prize lithium hydroxide solution in back slowly drips in mixed solution, regulates pH value to 8.Mixed solution is transferred in the agitated reactor of 10L again, suitably added deionized water, sealing is at 180 ℃ of insulation 2h.
B): after above-mentioned reaction is accomplished, cool to room temperature, with the product filtration washing, filter cake is dried 12h in 80 ℃ vacuum, obtains nickeliferous iron phosphate powder.
C): is that 4:1 carries out ball milling 2h with nickeliferous iron phosphate powder and maleic acid in alcoholic solution by mass ratio, and oven dry is carried out sintering 2h at 650 ℃ then, promptly obtains carbon and coats uniform high-performance LiFe
1-XNi xPO
4Powder-product, the 0.2C specific discharge capacity reaches 158.9mAh/g.
A): with the FeCl of 457.2g
2, 19.46gNiCl
2, 98.8g maleic acid and 432.5g content is 85% H
3PO
4Mix, add the polyacrylamide of 8.89g, add the 2.5L deionized water again, the stirring that does not stop then.Simultaneously 742.5g lithium acetate (analyzing pure) is dissolved in the deionized water of 2.5L, stirs and obtain pure clear solution.Lithium acetate solution slowly drips in mixed solution then, regulates pH value to alkalescent.Mixed solution is transferred in the agitated reactor of 10L again, suitably added deionized water, sealing is at 190 ℃ of insulation 2h.
B): after above-mentioned reaction is accomplished, cool to room temperature, with the product filtration washing, filter cake is dried 12h in 90 ℃ vacuum, obtains nickeliferous iron phosphate powder.
C): is that 10:3 carries out ball milling 2h with nickeliferous iron phosphate powder and citric acid in alcoholic solution by mass ratio, and oven dry is carried out sintering 1.5h at 650 ℃ then, promptly obtains carbon and coats uniform high-performance LiFe
1-XNi xPO
4Powder-product, the 0.2C specific discharge capacity reaches 157mAh/g.
Embodiment 3
A): with the NH of the ferric acetate of 409.93g, 8.84g nickel acetate, 100g ascorbic acid and 431.25
4H
2PO
4Mix, add the mixture of 11.85 polyvinyl alcohol and polyacrylamide, add the 2.5L deionized water again, the stirring that does not stop then.Simultaneously with 472gLiOHH
2O (analyzing pure) is dissolved in the deionized water of 2.5L, stirs and obtains pure clear solution, slowly drips then in mixed solution, regulates pH value to alkalescent.Mixed solution is transferred in the agitated reactor of 10L again, suitably added deionized water, sealing is at 200 ℃ of insulation 1.5h.
B): after above-mentioned reaction is accomplished, cool to room temperature, with the product filtration washing, filter cake is dried 12h in 95 ℃ vacuum, obtains nickeliferous iron phosphate powder.
C): is that 5:1 carries out ball milling 2h with nickeliferous iron phosphate powder and citric acid in alcoholic solution by mass ratio, and oven dry is carried out sintering 1h at 700 ℃ then, promptly obtains carbon and coats uniform high-performance LiFe
1-XNi xPO
4Powder-product, the 0.2C specific discharge capacity reaches 158.2mAh/g.
Claims (3)
1. the hydro-thermal of an ion doping high-performance iron phosphate lithium is synthesized preparation method, it is characterized in that it may further comprise the steps:
A, source of iron, nickel source, organic acid and phosphorus source are dissolved in the deionized water according to a certain percentage, are incorporated as 1%～10% dispersant of ion doping high-performance iron phosphate lithium product theoretical yield, constantly stir; Get mixed solution; The lithium source that will evenly be dissolved in deionized water more slowly is added drop-wise in the mixed solution, Li:Fe:Ni:P=3～3.5:1-x:x:1～1.2 wherein, x=0.01～0.06; Drip and finish adjusting PH to 7.5～8.2, back, get the alkalescent mixed solution;
B, A step gained alkalescent mixed solution is transferred in the autoclave, the capping still is at 80 ℃～220 ℃ insulation 1h～3h down; After the cooling, take out reaction product, with the product filtration washing; Again that the gained filter cake is dry under 50 ℃～100 ℃, obtain nickeliferous iron phosphate powder;
C, with the nickeliferous iron phosphate powder of step B gained and carbon containing organic compound according to mass ratio 10:1～4 ball milling 1～3h in alcohol, 50 ℃～100 ℃ dry down, under nitrogen protection,, promptly get product again in 600 ℃～800 ℃ sintering 1～4h.
2. according to the synthetic preparation method of the hydro-thermal of a kind of ion doping high-performance iron phosphate lithium described in the claim 1; It is characterized in that: described nickel source is nickel acetate or nickel chloride; Described source of iron is ferrous sulfate or frerrous chloride, and described organic acid is a kind of in maleic acid, citric acid and the ascorbic acid, and described dispersant is a polyvinyl alcohol; In the polyacrylamide one or both; Described phosphorus source is phosphoric acid or ammonium dihydrogen phosphate, and described lithium source is lithium hydroxide or lithium acetate, and described carbon containing organic compound is a kind of in maleic acid, sucrose and the starch.
3. according to the synthetic preparation method of the hydro-thermal of a kind of ion doping high-performance iron phosphate lithium described in claim 1 or 2; It is characterized in that: use 40 ℃～50 ℃ deionized water in the filter operation described in the step B, the drying among step B and the step C is all carried out in a vacuum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110253634A CN102315450A (en) | 2011-08-31 | 2011-08-31 | Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110253634A CN102315450A (en) | 2011-08-31 | 2011-08-31 | Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102315450A true CN102315450A (en) | 2012-01-11 |
Family
ID=45428387
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110253634A Pending CN102315450A (en) | 2011-08-31 | 2011-08-31 | Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102315450A (en) |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120237426A1 (en) * | 2011-03-18 | 2012-09-20 | Semiconductor Energy Laboratory Co., Ltd. | Method for manufacturing lithium-containing composite oxide |
| CN102856553A (en) * | 2012-10-11 | 2013-01-02 | 南京师范大学 | Preparation method of hydrothermal synthesis carbon coated lithium iron phosphate |
| CN102916183A (en) * | 2012-10-16 | 2013-02-06 | 上海锦众信息科技有限公司 | Preparation method of lithium iron phosphate composite material of lithium ion battery |
| CN103123968A (en) * | 2013-01-29 | 2013-05-29 | 中国科学院过程工程研究所 | High-performance lithium iron phosphate cathode material and preparation method of lithium iron phosphate cathode material |
| CN103151526A (en) * | 2013-04-08 | 2013-06-12 | 严百坤 | Preparation method of carbon-coated cerium-modified lithium iron phosphate composite anode material |
| CN104347873A (en) * | 2014-07-24 | 2015-02-11 | 机械科学研究总院先进制造技术研究中心 | Preparation method of sphere-like lithium ion battery positive pole material lithium iron phosphate (LiFePO4) |
| CN104659361A (en) * | 2013-11-25 | 2015-05-27 | 深圳市金和能电池科技有限公司 | LiFePO4 positive active material and preparation method thereof |
| US9059478B2 (en) | 2011-03-25 | 2015-06-16 | Semiconductor Energy Laboratory Co., Ltd. | Lithium-ion secondary battery with graphene and composite oxide layered electrode |
| CN104766956A (en) * | 2015-05-06 | 2015-07-08 | 田东 | Preparation method for nickel-coated lithium iron phosphate positive pole material |
| US9118077B2 (en) | 2011-08-31 | 2015-08-25 | Semiconductor Energy Laboratory Co., Ltd. | Manufacturing method of composite oxide and manufacturing method of power storage device |
| CN104953118A (en) * | 2015-05-21 | 2015-09-30 | 青海时代新能源科技有限公司 | Positive electrode material of lithium ion battery and preparation method thereof |
| US9249524B2 (en) | 2011-08-31 | 2016-02-02 | Semiconductor Energy Laboratory Co., Ltd. | Manufacturing method of composite oxide and manufacturing method of power storage device |
| CN107452949A (en) * | 2017-08-06 | 2017-12-08 | 长沙小新新能源科技有限公司 | A kind of LiFe1‑XNiXPO4The preparation method of/C Anode of lithium cell materials |
| CN107644993A (en) * | 2016-07-21 | 2018-01-30 | 深圳格林德能源有限公司 | A kind of phosphoric acid ferronickel lithium anode material and its synthetic method |
| CN108091867A (en) * | 2017-12-24 | 2018-05-29 | 扬州工业职业技术学院 | Application of the alcohol ether glucoside as carbon source presoma and its in anode material of lithium battery is prepared |
| CN108390061A (en) * | 2016-03-18 | 2018-08-10 | 王海峰 | A kind of LiFePO4 hydrothermal preparing process |
| CN109585791A (en) * | 2017-09-28 | 2019-04-05 | 江苏津谊新能源科技有限公司 | A kind of novel phosphoric acid iron lithium ion battery |
| CN109755487A (en) * | 2017-11-07 | 2019-05-14 | 中国石油化工股份有限公司 | The nickle cobalt lithium manganate and preparation method thereof of the LiFePO4 cladding of metallic element doping |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040151649A1 (en) * | 2001-04-10 | 2004-08-05 | Hemmer Reinhard P. | Binary, ternary and quaternary lithium phosphates, method for the production thereof and use of the same |
| CN101209821A (en) * | 2006-12-31 | 2008-07-02 | 比亚迪股份有限公司 | Preparation method for lithium ion secondary battery positive pole active substance lithium iron phosphate |
| US20090155689A1 (en) * | 2007-12-14 | 2009-06-18 | Karim Zaghib | Lithium iron phosphate cathode materials with enhanced energy density and power performance |
| CN101714627A (en) * | 2008-10-08 | 2010-05-26 | 中国科学院金属研究所 | Carbon nanotube/lithium iron phosphate composite positive electrode material and in situ preparation method thereof |
| CN101777648A (en) * | 2010-01-26 | 2010-07-14 | 中国科学院宁波材料技术与工程研究所 | Preparation method of monodisperse lithium iron phosphate nanometer material and lithium-ion secondary battery |
| CN101783405A (en) * | 2010-02-08 | 2010-07-21 | 江苏巨洋电池新材料有限公司 | Preparation method of nano flaky lithium iron phosphate material |
| CN102142544A (en) * | 2011-01-05 | 2011-08-03 | 河南捷和新能源材料有限公司 | Preparation method of carbon-doped lithium iron phosphate anode material |
-
2011
- 2011-08-31 CN CN201110253634A patent/CN102315450A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040151649A1 (en) * | 2001-04-10 | 2004-08-05 | Hemmer Reinhard P. | Binary, ternary and quaternary lithium phosphates, method for the production thereof and use of the same |
| CN101209821A (en) * | 2006-12-31 | 2008-07-02 | 比亚迪股份有限公司 | Preparation method for lithium ion secondary battery positive pole active substance lithium iron phosphate |
| US20090155689A1 (en) * | 2007-12-14 | 2009-06-18 | Karim Zaghib | Lithium iron phosphate cathode materials with enhanced energy density and power performance |
| CN101714627A (en) * | 2008-10-08 | 2010-05-26 | 中国科学院金属研究所 | Carbon nanotube/lithium iron phosphate composite positive electrode material and in situ preparation method thereof |
| CN101777648A (en) * | 2010-01-26 | 2010-07-14 | 中国科学院宁波材料技术与工程研究所 | Preparation method of monodisperse lithium iron phosphate nanometer material and lithium-ion secondary battery |
| CN101783405A (en) * | 2010-02-08 | 2010-07-21 | 江苏巨洋电池新材料有限公司 | Preparation method of nano flaky lithium iron phosphate material |
| CN102142544A (en) * | 2011-01-05 | 2011-08-03 | 河南捷和新能源材料有限公司 | Preparation method of carbon-doped lithium iron phosphate anode material |
Cited By (29)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8945498B2 (en) * | 2011-03-18 | 2015-02-03 | Semiconductor Energy Laboratory Co., Ltd. | Method for manufacturing lithium-containing composite oxide |
| US20120237426A1 (en) * | 2011-03-18 | 2012-09-20 | Semiconductor Energy Laboratory Co., Ltd. | Method for manufacturing lithium-containing composite oxide |
| US9627686B2 (en) | 2011-03-18 | 2017-04-18 | Semiconductor Energy Laboratory Co., Ltd. | Method for manufacturing lithium-containing composite oxide |
| US10205160B2 (en) | 2011-03-25 | 2019-02-12 | Semiconductor Energy Laboratory Co., Ltd. | Graphene composite oxide layered electrode for lithium-ion secondary batteries |
| US9059478B2 (en) | 2011-03-25 | 2015-06-16 | Semiconductor Energy Laboratory Co., Ltd. | Lithium-ion secondary battery with graphene and composite oxide layered electrode |
| US11101460B2 (en) | 2011-03-25 | 2021-08-24 | Semiconductor Energy Laboratory Co., Ltd. | Method of manufacturing electrode comprising graphene layer on current collector |
| US11799084B2 (en) | 2011-08-31 | 2023-10-24 | Semiconductor Energy Laboratory Co., Ltd. | Method for making LiFePO4 by hydrothermal method |
| US9249524B2 (en) | 2011-08-31 | 2016-02-02 | Semiconductor Energy Laboratory Co., Ltd. | Manufacturing method of composite oxide and manufacturing method of power storage device |
| US10270097B2 (en) | 2011-08-31 | 2019-04-23 | Semiconductor Energy Laboratory Co., Ltd. | Manufacturing method of composite oxide and manufacturing method of power storage device |
| US11283075B2 (en) | 2011-08-31 | 2022-03-22 | Semiconductor Energy Laboratory Co., Ltd. | Manufacturing method of composite oxide and manufacturing method of power storage device |
| US9118077B2 (en) | 2011-08-31 | 2015-08-25 | Semiconductor Energy Laboratory Co., Ltd. | Manufacturing method of composite oxide and manufacturing method of power storage device |
| CN102856553A (en) * | 2012-10-11 | 2013-01-02 | 南京师范大学 | Preparation method of hydrothermal synthesis carbon coated lithium iron phosphate |
| CN102916183A (en) * | 2012-10-16 | 2013-02-06 | 上海锦众信息科技有限公司 | Preparation method of lithium iron phosphate composite material of lithium ion battery |
| CN103123968B (en) * | 2013-01-29 | 2015-08-19 | 中国科学院过程工程研究所 | A kind of high-performance lithium iron phosphate cathode material and preparation method thereof |
| CN103123968A (en) * | 2013-01-29 | 2013-05-29 | 中国科学院过程工程研究所 | High-performance lithium iron phosphate cathode material and preparation method of lithium iron phosphate cathode material |
| CN103151526A (en) * | 2013-04-08 | 2013-06-12 | 严百坤 | Preparation method of carbon-coated cerium-modified lithium iron phosphate composite anode material |
| CN104659361A (en) * | 2013-11-25 | 2015-05-27 | 深圳市金和能电池科技有限公司 | LiFePO4 positive active material and preparation method thereof |
| CN104347873B (en) * | 2014-07-24 | 2017-05-10 | 机械科学研究总院先进制造技术研究中心 | Preparation method of sphere-like lithium ion battery positive pole material lithium iron phosphate (LiFePO4) |
| CN104347873A (en) * | 2014-07-24 | 2015-02-11 | 机械科学研究总院先进制造技术研究中心 | Preparation method of sphere-like lithium ion battery positive pole material lithium iron phosphate (LiFePO4) |
| CN104766956A (en) * | 2015-05-06 | 2015-07-08 | 田东 | Preparation method for nickel-coated lithium iron phosphate positive pole material |
| CN104953118B (en) * | 2015-05-21 | 2017-08-08 | 青海时代新能源科技有限公司 | Anode material for lithium-ion batteries and preparation method thereof |
| CN104953118A (en) * | 2015-05-21 | 2015-09-30 | 青海时代新能源科技有限公司 | Positive electrode material of lithium ion battery and preparation method thereof |
| CN108390061A (en) * | 2016-03-18 | 2018-08-10 | 王海峰 | A kind of LiFePO4 hydrothermal preparing process |
| CN107644993A (en) * | 2016-07-21 | 2018-01-30 | 深圳格林德能源有限公司 | A kind of phosphoric acid ferronickel lithium anode material and its synthetic method |
| CN107452949A (en) * | 2017-08-06 | 2017-12-08 | 长沙小新新能源科技有限公司 | A kind of LiFe1‑XNiXPO4The preparation method of/C Anode of lithium cell materials |
| CN109585791A (en) * | 2017-09-28 | 2019-04-05 | 江苏津谊新能源科技有限公司 | A kind of novel phosphoric acid iron lithium ion battery |
| CN109755487A (en) * | 2017-11-07 | 2019-05-14 | 中国石油化工股份有限公司 | The nickle cobalt lithium manganate and preparation method thereof of the LiFePO4 cladding of metallic element doping |
| CN108091867A (en) * | 2017-12-24 | 2018-05-29 | 扬州工业职业技术学院 | Application of the alcohol ether glucoside as carbon source presoma and its in anode material of lithium battery is prepared |
| CN108091867B (en) * | 2017-12-24 | 2020-06-26 | 扬州工业职业技术学院 | Alcohol ether glycoside as carbon source precursor and application thereof in preparation of lithium battery anode material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102315450A (en) | Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate | |
| CN101315981B (en) | Lithium iron phosphate anode material for lithium ion battery and modification method | |
| CN100448772C (en) | High density ultrafine composite ferric lithium phosphate anode material and preparation method | |
| CN101630739B (en) | Preparation method of modified doping lithium ferric phosphate | |
| CN101420034A (en) | Carbon coated granularity controllable spherical lithium ferric phosphate composite positive pole material and preparation method thereof | |
| CN101752562B (en) | Compound doped modified lithium ion battery anode material and preparation method thereof | |
| CN100491239C (en) | Preparation method of lithium ion battery positive pole material lithium iron phosphate and its product | |
| CN108039463A (en) | A kind of solid state battery of the preparation and application of solid electrolyte/electrode composite material material | |
| CN101339992B (en) | Preparation of lithium ionic cell positive electrode material vanadium lithium silicate | |
| CN110931781A (en) | Preparation method and application of biomass carbon/sodium iron fluorophosphate composite material | |
| CN105355908A (en) | Composite negative electrode material for lithium ion battery, preparing method thereof, negative electrode using material and lithium ion battery | |
| CN102427134A (en) | Mixed conductor composite material LiFePO4-MXy and preparation method thereof | |
| CN101651205A (en) | Method for preparing lithium vanadium phosphate as lithium ion battery anode material | |
| CN103956485A (en) | Lithium iron phosphate electrode material having three-dimensional hierarchical structure, and preparation method thereof | |
| CN102856553A (en) | Preparation method of hydrothermal synthesis carbon coated lithium iron phosphate | |
| CN102097616A (en) | Preparation method of high-energy and high-power density nano-scale lithium iron phosphate powder | |
| CN107204426A (en) | A kind of cobalt nickel oxide manganses lithium/titanate composite anode material for lithium of zirconium doping vario-property | |
| CN101070149B (en) | Lithium iron carbonate material prepared by vacuum carbon reduction and method | |
| CN101279725A (en) | Microwave fast solid phase sintering method for cathode material lithium iron phosphate of lithium ionic cell | |
| CN102832381A (en) | Preparation method of high-voltage cathode material Lil+xMn3/2-yNil/2-zMy+zO4 of lithium ion battery with long service life | |
| CN103078098A (en) | Preparation method of lithium-rich layered manganese-cobalt oxide composite positive electrode material | |
| CN102903918A (en) | Preparation method for manganese phosphate lithium nanosheet | |
| CN100483809C (en) | Method for producing ultra-fine LiFePO4/C of lithium ion battery anode material | |
| CN102683698B (en) | Preparation method of conductive modified lithium iron phosphate | |
| CN102040211B (en) | Method for synthesizing lithium ion battery cathode material LiFePO4 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 230000 Yaohai Industrial Park, Anhui, Hefei No. D weft Road, No. 7 Applicant after: Hefei Guoxuan High-Tech Power Energy Co., Ltd. Address before: 230000 Yaohai Industrial Park, Anhui, Hefei No. D weft Road, No. 7 Applicant before: Hefei Guoxuan High-Tech Power Energy Co., Ltd. |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: HEFEI GUOXUAN HIGH-TECH POWER ENERGY CO., LTD. TO: HEFEI GUOXUAN HIGH-TECH POWER ENERGY CO., LTD. |
|
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120111 |