CN101699639A - Method for preparing carbon-coated nano-grade lithium iron phosphate composite anode material - Google Patents
Method for preparing carbon-coated nano-grade lithium iron phosphate composite anode material Download PDFInfo
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- CN101699639A CN101699639A CN200910088078A CN200910088078A CN101699639A CN 101699639 A CN101699639 A CN 101699639A CN 200910088078 A CN200910088078 A CN 200910088078A CN 200910088078 A CN200910088078 A CN 200910088078A CN 101699639 A CN101699639 A CN 101699639A
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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
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- 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 discloses a method for preparing a carbon-coated nano-grade lithium iron phosphate composite anode material. The method comprises the following steps: dissolving a lithium source compound, a phosphor source compound, a ferrous source compound and a carbon source in de-ionized water in a mole ratio of Li to P to Fe to C of 2.5-3.2:1:0.98-1:0-0.5, uniformly mixing the materials in a reactor under the protection of an inert atmosphere, and sealing the reactor after stirring the materials for 1 to 5 hours; heating the mixture by microwave until the temperature reaches 120 to 300 DEG C, keeping the temperature for 5 to 20 minutes, and filtering the mixture after the mixture is cooled to be at a room temperature; and vacuum drying the filtrate at the temperature of below 100 DEG C after the filtrate is washed by the de-ionized water and absolute ethanol, and keeping the temperature of between 400 and 700 DEG C for 1 hour under the inert atmosphere to obtain the uniformly dispersed carbon-coated nano-grade lithium iron phosphate composite anode material with a grain diameter between 40 and 500 nm. The method is characterized by short reaction time, less process flow, low power consumption and no pollution. The anode material is characterized by uniform granularity, good dispersity, little aggregation, integral crystalline grains, good crystallinity and good electrical property.
Description
Technical field
The present invention relates to a kind of secondary lithium battery technology, relate in particular to a kind of preparation method of carbon-coated nano-grade lithium iron phosphate composite anode material.
Background technology
The anode material for lithium-ion batteries of broad research concentrates on the transition metal oxide of lithium such as the LiMO of layer structure at present
2(M=Co, Ni, Mn) and the LiMn of spinel structure
2O
4They differ from one another as positive electrode, LiCoO
2The cost height, natural resources shortage, toxicity is big; Lithium nickelate (LiNiO
2) the preparation difficulty, poor heat stability; LiMn
2O
4Capacity is lower, and cyclical stability is relatively poor.
In order to solve the defective of above material, battery circle has been done big quantity research, above positive electrode is being carried out various modifications with when improving its performance, and the exploitation of novel anode material also is the emphasis of paying close attention to always.Therefore, seek the ideal electrode active material of lithium ion battery from resource, environmental protection and security performance aspect, be still the research focus of quite a while World chemical power supply circle from now on and develop the key of pure electric vehicle.Consider from resource and environmental, be accompanied by the appearance of lithium ion battery, iron system is anodal just to be that people expect to substitute LiCoO always
2Alternative materials.LiFeO to stratiform
2Many deep researchs are arranged, but because Fe
4+/ Fe
+ 3Fermi energy level and Li that electricity is right
+Being separated by of/Li is too far away, and Fe
3+/ Fe
2+The electricity to again with Li
+Being separated by of/Li is too near, simultaneously, and Fe
3+Ionic radius and Li
+The ratio of radius does not meet structural requirement, so, the LiFeO that has significant practical applications
2Research never has big progress.
In the prior art, adopt LiFePO
4Positive electrode as lithium ion battery; LiFePO
4Real density (3.64g/cm
3) other iron phosphate is much bigger relatively; Calculate LiFePO during charging according to lattice constant
4Change FePO into
4Volume reduces 6.81%, can compensate the expansion of C anode in this process thereby can utilize the volume efficiency of practical lithium-ion better; Since the olivine structural quite stable, LiFePO
4Charge and discharge cycles behavior excellence, capacity attenuation is very little; LiFePO under low current density
4In Li almost can 100% embed and take off embedding, the quantity of and reversible embedding/take off embedding Li can increase along with the rising of working temperature, under high temperature (80 ℃) condition, LiFePO
4The utilance of theoretical capacity is near 100%.LiFePO
4There is not moisture absorption to handle easily; LiFePO
4Even if since in the structure inertia not as safe as a house under higher temperature with electrolyte solution reaction yet.From price and security consideration, LiFePO
4Be suitable as very much the positive electrode of large scale lithium ion battery.
Prepare LiFePO at present
4Method, mainly comprise solid-phase synthesis, co-precipitation synthetic method, collosol and gel synthetic method, hydrothermal synthesis method etc.
There is following shortcoming at least in above-mentioned prior art:
Complex process, high, the gained LiFePO of power consumption
4Positive electrode second-rate.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of carbon-coated nano-grade lithium iron phosphate composite anode material, this method have the reaction time short, technological process is few, less energy consumption, pollution-free; Gained positive electrode epigranular, good dispersion, reunion less, the advantage of the complete good crystallinity of crystal grain, good electrical property.
The objective of the invention is to be achieved through the following technical solutions:
The preparation method of carbon-coated nano-grade lithium iron phosphate composite anode material of the present invention comprises step:
At first, Li source compound, P source compound, ferrous iron source compound, carbon source are pressed the mol ratio Li of following element: P: Fe: C=2.5-3.2: 1: 0.98-1: 0-0.5, use deionized water dissolving respectively, under inert atmosphere protection, in reactor, mix, stir sealing after 1-5 hour;
Then, add microwave and be warmed up to 120-300 ℃, be incubated 5-20 minute, filter behind the cool to room temperature;
Afterwards, after cleaning with deionized water and absolute ethyl alcohol, in vacuumize below 100 ℃, 400-700 ℃ of insulation 1 hour under inert atmosphere at last, obtaining particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate composite anode material of 40-500nm.
As seen from the above technical solution provided by the invention, the preparation method of carbon-coated nano-grade lithium iron phosphate composite anode material of the present invention, owing at first Li source compound, P source compound, ferrous iron source compound, carbon source are pressed the mol ratio Li of following element: P: Fe: C=2.5-3.2: 1: 0.98-1: 0-0.5, use deionized water dissolving respectively, under inert atmosphere protection, in reactor, mix, stir sealing after 1-5 hour; Add microwave then and be warmed up to 120-300 ℃, be incubated 5-20 minute, filter behind the cool to room temperature; After cleaning with deionized water and absolute ethyl alcohol afterwards, in vacuumize below 100 ℃, 400-700 ℃ of insulation 1 hour under inert atmosphere at last, obtaining particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate composite anode material of 40-500nm.Reaction time is short, technological process is few, less energy consumption, pollution-free; Gained positive electrode epigranular, good dispersion, reunion less, the complete good crystallinity of crystal grain, good electrical property.
Embodiment
The preparation method of carbon-coated nano-grade lithium iron phosphate composite anode material of the present invention, its preferable embodiment is to comprise step:
At first, Li source compound, P source compound, ferrous iron source compound, carbon source are pressed the mol ratio Li of following element: P: Fe: C=2.5-3.2: 1: 0.98-1: 0-0.5, use deionized water dissolving respectively, under inert atmosphere protection, in reactor, mix, stir sealing after 1-5 hour;
Then, add microwave and be warmed up to 120-300 ℃, be incubated 5-20 minute, filter behind the cool to room temperature;
Afterwards, after cleaning with deionized water and absolute ethyl alcohol, in vacuumize below 100 ℃, 400-700 ℃ of insulation 1 hour under inert atmosphere at last, obtaining particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate composite anode material of 40-500nm.
Specifically:
With Li source compound (LiOHH
2O, LiAc, Li
2CO
3, LiCl, LiNO
3, Li
2SO
4Wait one or more), P source compound (H
3PO
4, NH
4H
2PO
4, (NH
4)
2HPO
4, LiH
2PO
4Wait one or more), ferrous iron source compound (FeSO
47H
2O, (NH
4)
2Fe (SO
4) 6H
2O, FeC
2O
42H
2O, FeAc
2Wait one or more) and carbon source (glucose; sucrose; citric acid; ascorbic acid; carbon black etc. one or more) by following element mol ratio Li: P: Fe: C (in the carbon source phosphorus content)=2.5-3.2: 1: 0.98-1: 0-0.5; use deionized water dissolving respectively; under inert atmosphere protection, in reactor, mix in certain sequence; stir sealing after 1-5 hour; add microwave and be warmed up to 120-300 ℃ of insulation 5-20 minute; filter behind the cool to room temperature; after deionized water and absolute ethyl alcohol cleaning; vacuumize below 100 ℃; at last under inert atmosphere 400-700 ℃ the insulation 1 hour, can obtain particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate composite anode material powder of 40-500nm.Gained positive electrode specific capacity can reach 166mAh/g, and near theoretical value (170mAh/g), 100 circulations are undamped.
The present invention adopts microwave-hydrothermal method to prepare carbon-coated nano-grade lithium iron phosphate composite anode material fast, and material is synthetic to coat once-combined moulding with carbon, has reduced technological process, reaction time weak point, less energy consumption, pollution-free; The gained material has fabulous electrical property, is desirable novel secondary lithium battery positive electrode, has a extensive future.
Further the present invention is described in detail with instantiation below:
Example 1:
With LiOHH
2O, H
3PO
4, FeSO
47H
2O and glucose were in Li: P: Fe: C (with the carbon source phosphorus content)=3: 1: 1: 0.25; use deionized water dissolving respectively; under the Ar gas shiled, in reactor, mix in certain sequence; stir sealing after 4 hours; add microwave and be warmed up to 250 ℃ of insulations 10 minutes; filter behind the cool to room temperature; after deionized water and absolute ethyl alcohol cleaning; 80 ℃ of following vacuumizes; at last under 2%H2/98%Ar atmosphere 600 ℃ the insulation 1 hour, can obtain particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate powder of 100nm.Gained positive electrode specific capacity can reach 152mAh/g (theoretical value 170mAh/g), and 100 circulations are undamped.
Example 2:
With LiOHH
2O, H
3PO
4, (NH4)
2Fe (SO
4) 6H
2O and sucrose were in Li: P: Fe: C (with the carbon source phosphorus content)=3: 1: 1: 0.3, use deionized water dissolving respectively, at N
2Mix in reactor in certain sequence under the gas shiled, stir sealing after 5 hours, add microwave and be warmed up to 200 ℃ of insulations 20 minutes, filter behind the cool to room temperature, after cleaning with deionized water and absolute ethyl alcohol, 60 ℃ of following vacuumizes are at last at 2%H
2The following 700 ℃ of insulations of/98%Ar atmosphere 1 hour, can obtain particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate powder of 120nm.Gained positive electrode specific capacity can reach 147mAh/g (theoretical value 170mAh/g), and 100 circulations are undamped.
Example 3
With LiOHH
2O, NH
4H
2PO
4, FeC
2O
42H
2O and citric acid were in Li: P: Fe: C (with the carbon source phosphorus content)=3: 1: 1: 0.5; use deionized water dissolving respectively; under the Ar gas shiled, in reactor, mix in certain sequence; stir sealing after 3 hours; add microwave and be warmed up to 235 ℃ of insulations 15 minutes, filter behind the cool to room temperature, after cleaning with deionized water and absolute ethyl alcohol; 80 ℃ of following vacuumizes are at last at 2%H
2The following 650 ℃ of insulations of/98%Ar atmosphere 1 hour, can obtain particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate powder of 80nm.Gained positive electrode specific capacity can reach 159mAh/g (theoretical value 170mAh/g), and 100 circulations are undamped.
Example 4
With LiAc, LiH
2PO
4, FeAc
2With ascorbic acid in Li: P: Fe: C (with the carbon source phosphorus content)=3.15: 1: 0.98: 0.1; use deionized water dissolving respectively; under the Ar gas shiled, in reactor, mix in certain sequence; stir sealing after 2 hours; add microwave and be warmed up to 280 ℃ of insulations 5 minutes, filter behind the cool to room temperature, after cleaning with deionized water and absolute ethyl alcohol; 80 ℃ of following vacuumizes are at last at 2%H
2The following 500 ℃ of insulations of/98%Ar atmosphere 1 hour, can obtain particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate powder of 40nm.Gained positive electrode specific capacity can reach 166mAh/g, and near theoretical value (170mAh/g), 100 circulations are undamped.
Method of the present invention has overcome the deficiency among the present LiFePO 4 powder preparation technology, have the reaction time short, technological process is few, less energy consumption, pollution-free; Gained nanometer product epigranular, good dispersion, reunion less, the advantage of the complete good crystallinity of crystal grain, good electrical property.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (6)
1. the preparation method of a carbon-coated nano-grade lithium iron phosphate composite anode material is characterized in that, comprises step:
At first, Li source compound, P source compound, ferrous iron source compound, carbon source are pressed the mol ratio Li of following element: P: Fe: C=2.5-3.2: 1: 0.98-1: 0-0.5, use deionized water dissolving respectively, under inert atmosphere protection, in reactor, mix, stir sealing after 1-5 hour;
Then, add microwave and be warmed up to 120-300 ℃, be incubated 5-20 minute, filter behind the cool to room temperature;
Afterwards, after cleaning with deionized water and absolute ethyl alcohol, in vacuumize below 100 ℃, 400-700 ℃ of insulation 1 hour under inert atmosphere at last, obtaining particle diameter is all dispersions carbon-coated nano-grade lithium iron phosphate composite anode material of 40-500nm.
2. the preparation method of carbon-coated nano-grade lithium iron phosphate composite anode material according to claim 1 is characterized in that, described Li source compound comprises following one or more materials:
LiOH·H
2O、LiAc、Li
2CO
3、LiCl、LiNO
3、Li
2SO
4。
3. the preparation method of carbon-coated nano-grade lithium iron phosphate composite anode material according to claim 1 is characterized in that, described P source compound comprises following one or more materials:
H
3PO
4、NH
4H
2PO
4、(NH
4)
2HPO
4、LiH
2PO
4。
4. the preparation method of carbon-coated nano-grade lithium iron phosphate composite anode material according to claim 1 is characterized in that, described ferrous iron source compound comprises following one or more materials:
FeSO
4·7H
2O、(NH4)
2Fe(SO
4)·6H
2O、FeC
2O
4·2H
2O、FeAc
2。
5. the preparation method of carbon-coated nano-grade lithium iron phosphate composite anode material according to claim 1 is characterized in that, described carbon source comprises following one or more materials:
Glucose, sucrose, citric acid, ascorbic acid, carbon black.
6. according to the preparation method of each described carbon-coated nano-grade lithium iron phosphate composite anode material of claim 1 to 5, it is characterized in that the specific capacity of described positive electrode is more than or equal to 166mAh/g, the circulation above 100 times is undamped.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102104144A (en) * | 2010-12-30 | 2011-06-22 | 常州华科新能源科技有限公司 | Method for preparing lithium iron phosphate compound anode material |
| CN102185138A (en) * | 2011-01-28 | 2011-09-14 | 厦门钨业股份有限公司 | Preparation method of composite lithium iron phosphate material |
| CN102347477A (en) * | 2010-08-02 | 2012-02-08 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-performance lithium iron phosphate / carbon anode material by microwave method |
| CN102530906A (en) * | 2010-12-16 | 2012-07-04 | 中国科学院福建物质结构研究所 | Microwave-hydrothermal method for preparing cathode materials of nano lithium iron phosphate batteries |
| CN102569792A (en) * | 2011-11-07 | 2012-07-11 | 四川大学 | Preparation method for one-step synthesis of high-rate-performance carbon-coated lithium iron phosphate cathode material by in-situ hydrothermal carbonization |
| CN102593457A (en) * | 2012-02-22 | 2012-07-18 | 中国石油大学(北京) | Preparation method of lithium iron phosphate-carbon material composite |
| CN102842716A (en) * | 2012-08-03 | 2012-12-26 | 江苏力天新能源科技有限公司 | Preparation method for nano-scale lithium iron phosphate |
| CN103030128A (en) * | 2011-09-29 | 2013-04-10 | 北京当升材料科技股份有限公司 | Industrial production method for preparing nanometer lithium iron phosphate by adopting solvent thermal method |
| CN103380529A (en) * | 2010-10-20 | 2013-10-30 | 科学与工业研究会 | Cathode material and lithium ion battery therefrom |
| CN103531813A (en) * | 2013-10-23 | 2014-01-22 | 山东大学 | Preparation method of high-capacity nano-level lithium iron phosphate/carbon composite positive material |
| CN103708434A (en) * | 2012-10-09 | 2014-04-09 | 上海交通大学 | Lithium iron phosphate material and preparation method thereof |
| CN103904325A (en) * | 2014-03-21 | 2014-07-02 | 天津大学 | High-multiplying-power type lithium iron phosphate/carbon composite material and preparation method thereof |
| CN104167542A (en) * | 2014-08-06 | 2014-11-26 | 西南民族大学 | Nickel-cobalt-lithium manganate powder of lithium battery positive electrode material and preparation method of nickel-cobalt-lithium manganate powder |
| CN105452158A (en) * | 2013-08-09 | 2016-03-30 | 巴斯夫欧洲公司 | Process for the preparation of an electrode material and its use in lithium-ion batteries |
| CN105958058A (en) * | 2016-06-14 | 2016-09-21 | 陕西科技大学 | Method for preparing self-assembled carbon-coated nickel oxide hollow microspheres |
| CN111348637A (en) * | 2020-03-24 | 2020-06-30 | 广东邦普循环科技有限公司 | Nano lithium iron phosphate and preparation method thereof |
| CN112125292A (en) * | 2020-08-14 | 2020-12-25 | 中国科学院金属研究所 | Hydrothermal synthesis method of lithium manganese iron phosphate |
| CN112331846A (en) * | 2019-08-27 | 2021-02-05 | 万向一二三股份公司 | Preparation method of high-rate positive electrode material lithium iron phosphate |
| CN115986065A (en) * | 2022-12-29 | 2023-04-18 | 贵州胜泽威化工有限公司 | Method for preparing lithium iron phosphate cathode material by microwave-assisted hydrothermal method |
-
2009
- 2009-07-01 CN CN200910088078A patent/CN101699639A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102347477A (en) * | 2010-08-02 | 2012-02-08 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-performance lithium iron phosphate / carbon anode material by microwave method |
| CN103380529A (en) * | 2010-10-20 | 2013-10-30 | 科学与工业研究会 | Cathode material and lithium ion battery therefrom |
| CN102530906A (en) * | 2010-12-16 | 2012-07-04 | 中国科学院福建物质结构研究所 | Microwave-hydrothermal method for preparing cathode materials of nano lithium iron phosphate batteries |
| CN102104144B (en) * | 2010-12-30 | 2013-08-28 | 常州华科新能源科技有限公司 | Method for preparing lithium iron phosphate compound anode material |
| CN102104144A (en) * | 2010-12-30 | 2011-06-22 | 常州华科新能源科技有限公司 | Method for preparing lithium iron phosphate compound anode material |
| CN102185138A (en) * | 2011-01-28 | 2011-09-14 | 厦门钨业股份有限公司 | Preparation method of composite lithium iron phosphate material |
| CN103030128A (en) * | 2011-09-29 | 2013-04-10 | 北京当升材料科技股份有限公司 | Industrial production method for preparing nanometer lithium iron phosphate by adopting solvent thermal method |
| CN102569792A (en) * | 2011-11-07 | 2012-07-11 | 四川大学 | Preparation method for one-step synthesis of high-rate-performance carbon-coated lithium iron phosphate cathode material by in-situ hydrothermal carbonization |
| CN102593457A (en) * | 2012-02-22 | 2012-07-18 | 中国石油大学(北京) | Preparation method of lithium iron phosphate-carbon material composite |
| CN102842716A (en) * | 2012-08-03 | 2012-12-26 | 江苏力天新能源科技有限公司 | Preparation method for nano-scale lithium iron phosphate |
| CN103708434A (en) * | 2012-10-09 | 2014-04-09 | 上海交通大学 | Lithium iron phosphate material and preparation method thereof |
| CN105452158A (en) * | 2013-08-09 | 2016-03-30 | 巴斯夫欧洲公司 | Process for the preparation of an electrode material and its use in lithium-ion batteries |
| CN103531813A (en) * | 2013-10-23 | 2014-01-22 | 山东大学 | Preparation method of high-capacity nano-level lithium iron phosphate/carbon composite positive material |
| CN103904325A (en) * | 2014-03-21 | 2014-07-02 | 天津大学 | High-multiplying-power type lithium iron phosphate/carbon composite material and preparation method thereof |
| CN104167542A (en) * | 2014-08-06 | 2014-11-26 | 西南民族大学 | Nickel-cobalt-lithium manganate powder of lithium battery positive electrode material and preparation method of nickel-cobalt-lithium manganate powder |
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| CN112331846A (en) * | 2019-08-27 | 2021-02-05 | 万向一二三股份公司 | Preparation method of high-rate positive electrode material lithium iron phosphate |
| CN111348637A (en) * | 2020-03-24 | 2020-06-30 | 广东邦普循环科技有限公司 | Nano lithium iron phosphate and preparation method thereof |
| CN111348637B (en) * | 2020-03-24 | 2022-01-07 | 广东邦普循环科技有限公司 | Nano lithium iron phosphate and preparation method thereof |
| CN112125292A (en) * | 2020-08-14 | 2020-12-25 | 中国科学院金属研究所 | Hydrothermal synthesis method of lithium manganese iron phosphate |
| CN115986065A (en) * | 2022-12-29 | 2023-04-18 | 贵州胜泽威化工有限公司 | Method for preparing lithium iron phosphate cathode material by microwave-assisted hydrothermal method |
| CN115986065B (en) * | 2022-12-29 | 2023-09-29 | 贵州胜泽威化工有限公司 | Method for preparing lithium iron phosphate anode material by microwave-assisted hydrothermal method |
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Application publication date: 20100428 |