CN107845791A - A kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode - Google Patents
A kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode, belong to technical field of new energy material preparation.This method is used as carbon source using low softening point asphalt first, ball milling is carried out with ferric lithium phosphate precursor material, again carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing is obtained by low-temperature bake, again by itself and high softening point bitumen mixed at high speed, by low temperature softening and the step of high temperature cabonization two, Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode is finally given.The low softening point asphalt used in this method can effectively prevent growing up for LiFePO4 crystal grain, and tentatively realize carbon coating, again after mixing and sintering with high softening point bitumen, LiFePO4 surface potential energy distribution state can be optimized, improve the high-speed transfer of lithium ion in the material.Lithium iron phosphate positive material prepared by the present invention has the advantages that electronics and ionic conductivity are high, and specific capacity is high, and the positive electrode for being highly suitable as lithium-ion-power cell uses.
Description
Technical field
The present invention relates to technical field of lithium ion, more particularly to a kind of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive pole material
The preparation method of material.
Background technology
Lithium ion battery have the characteristics that higher ratio energy, longer service life cycle and receive much concern, extensively
It is general to be applied in the fields such as portable electric appts, computer.Lithium ion battery mainly by positive electrode, negative material, barrier film and
The most of composition of electrolyte four, wherein positive electrode is to govern one of battery performance and price most critical technology, therefore is aligned
The research of pole material turns into focus of concern, and it is mainly LiFePO4, cobalt acid lithium, mangaic acid to study more positive electrode
Lithium, lithium-rich manganese-based etc..Goodenough in 1997 proposes that LiFePO4 can be as the positive electrode of lithium ion battery, phosphorus first
Sour iron lithium anode material has abundant raw materials, cheap, pollution-free, security is good, charge and discharge platform is obvious, rate charge-discharge is special
The advantages that property and good cycling stability, it is especially suitable for the positive electrode of power-type lithium ion battery.The preparation of LiFePO 4 material
Method has high temperature solid-state method, carbothermic method, hydro-thermal method and coprecipitation etc..
However, the electronic conductivity and ionic conductivity of LiFePO4 are all relatively low, chemical property greatly affected
Play.Carbon coating is also referred to as carbon dope, is a kind of effective method for improving LiFePO4 electric conductivity, and currently used carbon matrix precursor has
Sucrose, glucose, polyvinyl alcohol, citric acid, polyacrylic acid, starch etc., generally it is mixed with LiFePO4 or its presoma,
Pyrolysis produces conductive carbon at a certain temperature, is coated on LiFePO4Particle surface forms LiFePO4/ C composite.This is a kind of
The method of in-stiu coating, carbon matrix precursor can not only play reduction in roasting process but also can prevent LiFePO4Particle
Grow up and reunite, performance all obtains a certain degree of raising, therefore receives much concern.But material electricity prepared by these presoma carbon
The improved degree of chemical property is all limited.The problem of selecting suitable carbon matrix precursor to be one in the urgent need to address.
In view of the present situation of prior art, the invention provides a kind of system of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode
Preparation Method, this method cost is relatively low, simple to operate, is well suited for mass producing.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive pole
The preparation method of material, growing up for LiFePO4 crystal grain is effectively prevented using low softening point asphalt, tentatively realize carbon coating, then with
After high softening point bitumen mixing, sintering, optimization LiFePO4 surface potential energy distribution state, the high speed of lithium ion in the material is improved
Transmission, gained lithium iron phosphate positive material have the advantages that electronics and ionic conductivity are high, and specific capacity is high, are highly suitable as lithium
The positive electrode of ion battery uses.
A kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode proposed by the present invention, including following step
Suddenly：
S1, after mixing low softening point asphalt and mixed solvent, lithium source, source of iron and phosphorus source are sequentially added, then ball milling,
Drying, sintering obtains carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing under inert gas shielding；
S2, carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening point bitumen mixed, heat up, be incubated, then rise under inert atmosphere
Temperature, insulation carbonization, cooling obtain Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode.
Preferably, in S1, the softening point of low softening point asphalt is 60~120 DEG C.
Preferably, in S1, mixed solvent is 1 by volume by water and alcohol compound：1 is mixed to get.
Preferably, alcohol compound is methanol, ethanol, ethylene glycol, normal propyl alcohol, propane diols, glycerine, n-butanol, new penta
At least one of alcohol.
Preferably, in S1, lithium source is at least one in lithium carbonate, lithia, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate
Kind.
Preferably, in S1, source of iron be ferric oxalate, ferric phosphate, ferrous phosphate, ferrous ammonium phosphate, in di-iron trioxide extremely
Few one kind.
Preferably, in S1, phosphorus source be ammonium dihydrogen phosphate, ammonium hydrogen phosphate, lithium dihydrogen phosphate, ferric phosphate, in phosphoric acid at least
It is a kind of.
Preferably, in S1, the mol ratio of elemental lithium, ferro element and P elements is 1：1：1.
Preferably, in S1, the theoretical synthetic quantity of LiFePO4 and the mass ratio of low softening point asphalt are 1：0.002~0.1.
Preferably, in S1, Ball-milling Time is 8~36h.
Preferably, in S1, drying temperature is 95~105 DEG C, preferably 100 DEG C.
Preferably, in S1, sintering temperature is 300~400 DEG C, and sintering time is 4~10h.
Preferably, in S2, the mass ratio of carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening point bitumen is 1：0.05~0.2.
Preferably, in S2, the softening point of high softening point bitumen is 270~350 DEG C.
Preferably, in S2, carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening point bitumen is mixed into 5~25min, are placed in rotation
In formula rotary furnace, rotary rotary furnace rotating speed is 1~15 turn/min, is warming up to 250~350 DEG C under inert atmosphere, insulation 1~
3h, then 600~800 DEG C are warming up to, insulation 4~12h of carbonization, naturally cool to room temperature and obtain Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries
Positive electrode.
Preferably, in S2, heating rate is 5~15 DEG C/min.
Preferably, above-mentioned inert atmosphere is at least one of nitrogen, helium, neon, argon gas, xenon.
A kind of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode that the present invention also proposes, using above-mentioned Double-layer asphalt carbon bag
The preparation method for covering lithium iron phosphate positive material is made.
Because low softening point asphalt carries out ball milling low softening point asphalt relatively easily, in S1 of the present invention can be used as carbon
Source, it is dispersed in mechanical milling process to be advantageous to pitch, while during follow-up low-temperature sintering, can fully infiltrate
Grain is internally formed conductive network, prevents growing up for LiFePO4 crystal grain, while preliminarily form certain thickness on the surface of particle
Carbon-coating；For S1 using water and the mixed solution of alcohol, its reclaimed water can be with dissolving phosphoric acid ferrimanganic lithium presoma (i.e. lithium source, source of iron, phosphorus
Source), and alcohol can dissolve pitch, while be advantageous to follow-up drying；S2 using high softening point bitumen as carbon source, on the one hand by
In easy heat production is blended at a high speed, high softening point bitumen is non-fusible, still can keep graininess, and it is equal to be advantageous to material mixing
Even, the carbonation rate of another aspect high softening point bitumen is higher, is advantageous to the formation of carbon-coating；S2 is made high soft using rotary rotary furnace
When change point pitch softens near softening point, fully infiltration is on LiFePO4 pre-burning thing surface, then can uniformly be coated after heating up
On the surface of LiFePO4.
The method that the present invention is successively coated using low softening point asphalt and high softening point bitumen, can be than in general carbon source more
Fill uniformly with, be dispersed between lithium iron phosphate positive material particle, form conductive network structure, control LiFePO4 crystal grain
Growth, while the double-deck carbon coating formed is fairly evenly coated on the surface of lithium iron phosphate positive material, optimizes LiFePO4
Surface potential energy distribution state, improve the high-speed transfer of lithium ion in the material.
Gained lithium iron phosphate positive material of the invention has the advantages that electronics and ionic conductivity are high, and specific capacity is high, very
The positive electrode for being suitable as lithium-ion-power cell uses.
Brief description of the drawings
Fig. 1 is the SEM pictures of the gained Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode of the embodiment of the present invention 3.
Fig. 2 is that a kind of preparation method flow of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode proposed by the present invention is illustrated
Figure.
Fig. 3 is Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode putting under 0.1C multiplying powers described in the embodiment of the present invention 3
Electric curve synoptic diagram.
Embodiment
As shown in Figure 1, 2, 3, Fig. 1 is the gained Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode of the embodiment of the present invention 3
SEM pictures, Fig. 2 are that a kind of preparation method flow of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode proposed by the present invention is illustrated
Figure.Fig. 3 is electric discharge of the gained of the embodiment of the present invention 3 Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode under 0.1C multiplying powers
Curve synoptic diagram.
Embodiment 1
A kind of reference picture 2, preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode, comprises the following steps：
S1, low softening point asphalt and mixed solvent mixed, solvent is 1 by volume by water and ethanol：1 is mixed to get；
Lithium acetate, ferric phosphate and lithium dihydrogen phosphate are sequentially added, the wherein mol ratio of elemental lithium, ferro element and P elements is 1：1：1,
The theoretical synthetic quantity of LiFePO4 and the mass ratio of low softening point asphalt are 1：0.002, then ball milling 36h, 95 DEG C of drying, xenon
The lower 400 DEG C of sintering 4h of gas shield, obtains carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing；
S2, by carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening point bitumen it is 1 in mass ratio：0.2 mixing 5min, is placed in rotation
In rotatable rotary furnace, rotary rotary furnace rotating speed is 15 turns/min, and 250 DEG C are warming up under helium atmosphere, is incubated 3h, then be warming up to
600 DEG C, insulation carbonization 12h, heating rate is 5 DEG C/min, naturally cools to room temperature and obtains Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries
Positive electrode.It is that negative pole is assembled into after button cell under 0.1C multiplying powers specific discharge capacity as 161.5mAh/g using metal lithium sheet.
Embodiment 2
A kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode, comprises the following steps：
S1, low softening point asphalt and mixed solvent mixed, solvent is 1 by volume by water and glycerine：1 mixes
Arrive；Lithia, di-iron trioxide and phosphoric acid are sequentially added, the wherein mol ratio of elemental lithium, ferro element and P elements is 1：1：
1, the theoretical synthetic quantity of LiFePO4 and the mass ratio of low softening point asphalt are 1：0.1, then ball milling 8h, 105 DEG C of drying, xenon
The lower 300 DEG C of sintering 10h of gas shield, obtains carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing；
S2, by carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening point bitumen it is 1 in mass ratio：0.05 mixing 25min, is placed in
In rotary rotary furnace, rotary rotary furnace rotating speed is 1 turn/min, and 350 DEG C are warming up under neon atmosphere, is incubated 1h, then heat up
To 800 DEG C, insulation carbonization 4h, heating rate is 15 DEG C/min, naturally cools to room temperature and obtains Double-layer asphalt carbon coating ferric phosphate
Lithium anode material.It is that negative pole is assembled into after button cell under 0.1C multiplying powers specific discharge capacity as 158.8mAh/g using metal lithium sheet.
Embodiment 3
A kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode, comprises the following steps：
S1,4g low softening points (70~85 DEG C) pitch is added in ceramic ball grinder, using water/methanol, (volume ratio is 1：
1) it is solvent, sequentially adds 9.37g lithium carbonates, 45.6g ferrous oxalates and 29.2g ammonium dihydrogen phosphates, the theory of LiFePO4
The mass ratio of synthetic quantity and low softening point asphalt is 1：0.1；Ball grinder is put into progress ball milling 24h in planetary ball mill, taken
Go out to be put into and dried in 100 DEG C of drying boxes；It is then placed in the tube furnace of nitrogen protection and sinters 4h in 400 DEG C, obtains carbon coating phosphorus
Sour iron lithium pre-burning thing；
S2, by above-mentioned carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening-point (270~290 DEG C) pitch it is 1 in mass ratio：
0.2 mixing, 15min being mixed in high mixer high speed, is then placed in rotary rotary furnace, stove rotating speed is 15 turns/min, in
Under argon gas atmosphere, heating rate is 5 DEG C/min, is first warming up to 290 DEG C, constant temperature 3h, then is warming up to 800 DEG C, constant temperature carbonization 4h, from
Room temperature discharging is so cooled to, obtains Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode.
Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode obtained by the present embodiment is subjected to electron-microscope scanning, as shown in Figure 1.Such as
Shown in Fig. 3, show for discharge curve of the Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode under 0.1C multiplying powers described in the present embodiment
It is intended to.It is that negative pole is assembled into after button cell under 0.1C multiplying powers specific discharge capacity as 164.8mAh/g using metal lithium sheet.
Embodiment 4
A kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode, comprises the following steps：
S1,10g low softening points (80~100 DEG C) pitch is added in ceramic ball grinder, with water/propane diols (volume ratio
For 1：1) it is solvent, sequentially adds 30.3g lithium hydroxides, 228.0g ferrous oxalates and 124.2g phosphoric acid, the reason of LiFePO4
It is 1 by the mass ratio of synthetic quantity and low softening point asphalt：0.05；Ball grinder is put into progress ball milling 8h in planetary ball mill,
Taking-up is put into 100 DEG C of drying boxes and dried；It is then placed in the tube furnace of helium protection and sinters 8h in 300 DEG C, obtains carbon coating
LiFePO4 pre-burning thing；
S2, by above-mentioned carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening-point (290~300 DEG C) pitch it is 1 in mass ratio：
0.1 mixing, 25min is mixed in high mixer high speed, is then placed in rotary rotary furnace, stove rotating speed is 5 turns/min, in nitrogen
Under gas atmosphere, heating rate is 8 DEG C/min, is first warming up to 300 DEG C, constant temperature 2h, then is warming up to 750 DEG C, constant temperature carbonization 12h, from
Room temperature discharging is so cooled to, obtains Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode.Button is assembled into by negative pole of metal lithium sheet
Specific discharge capacity is 162.5mAh/g under 0.1C multiplying powers after formula battery.
Embodiment 5
A kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode, comprises the following steps：
S1,4g low softening points (95~110 DEG C) pitch is added in ceramic ball grinder, using water/n-butanol (volume ratio as
1：1) it is solvent, sequentially adds 9.37g lithium carbonates, 45.6g ferrous oxalates and 29.2g ammonium dihydrogen phosphates, the reason of LiFePO4
It is 1 by the mass ratio of synthetic quantity and low softening point asphalt：0.1；Ball grinder is put into progress ball milling 12h in planetary ball mill,
Taking-up is put into 100 DEG C of drying boxes and dried；It is then placed in the tube furnace of inert gas shielding and sinters 8h in 400 DEG C, obtains carbon
Coated LiFePO 4 for lithium ion batteries pre-burning thing；
S2, by above-mentioned carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening-point (330~350 DEG C) pitch it is 1 in mass ratio：
0.2 mixing, 15min being mixed in high mixer high speed, is then placed in rotary rotary furnace, stove rotating speed is 15 turns/min, in
Under inert atmosphere, heating rate is 5 DEG C/min, is first warming up to 340 DEG C, constant temperature 3h, then is warming up to 700 DEG C, constant temperature carbonization 8h, from
Room temperature discharging is so cooled to, obtains Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode.Button is assembled into by negative pole of metal lithium sheet
Specific discharge capacity is 165.0mAh/g under 0.1C multiplying powers after formula battery.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that comprise the following steps：
S1, after low softening point asphalt and mixed solvent are mixed, lithium source, source of iron and phosphorus source are sequentially added, then ball milling, dried
Dry, sintering obtains carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing under inert gas shielding；
S2, carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening point bitumen mixed, heat up, be incubated under inert atmosphere, then heated up, protected
Temperature carbonization, cooling obtain Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode.
2. the preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode according to claim 1, it is characterised in that S1
In, the softening point of low softening point asphalt is 60~120 DEG C.
3. the preparation method of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode according to claim 1 or claim 2, its feature exist
In in S1, mixed solvent is 1 by volume by water and alcohol compound：1 is mixed to get；Preferably, alcohol compound is first
At least one of alcohol, ethanol, ethylene glycol, normal propyl alcohol, propane diols, glycerine, n-butanol, neopentyl alcohol.
4. according to the preparation method of any one of the claim 1-3 Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrodes, it is special
Sign is, in S1, lithium source is at least one of lithium carbonate, lithia, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate；It is preferred that
Ground, in S1, source of iron is at least one of ferric oxalate, ferric phosphate, ferrous phosphate, ferrous ammonium phosphate, di-iron trioxide；It is preferred that
Ground, in S1, phosphorus source is at least one of ammonium dihydrogen phosphate, ammonium hydrogen phosphate, lithium dihydrogen phosphate, ferric phosphate, phosphoric acid；Preferably,
In S1, the mol ratio of elemental lithium, ferro element and P elements is 1：1：1.
5. according to the preparation method of any one of the claim 1-4 Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrodes, it is special
Sign is, in S1, the theoretical synthetic quantity of LiFePO4 and the mass ratio of low softening point asphalt are 1：0.002~0.1.
6. according to the preparation method of any one of the claim 1-5 Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrodes, it is special
Sign is, in S1, Ball-milling Time is 8~36h；Preferably, in S1, sintering temperature be 300~400 DEG C, sintering time be 4~
10h。
7. according to the preparation method of any one of the claim 1-5 Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrodes, it is special
Sign is, in S2, the mass ratio of carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening point bitumen is 1：0.05~0.2；Preferably, S2
In, the softening point of high softening point bitumen is 270~350 DEG C.
8. according to the preparation method of any one of the claim 1-5 Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrodes, it is special
Sign is, in S2, carbon-coated LiFePO 4 for lithium ion batteries pre-burning thing and high softening point bitumen are mixed, 250~350 are warming up under inert atmosphere
DEG C, 1~3h is incubated, then 600~800 DEG C are warming up to, insulation 4~12h of carbonization, naturally cool to room temperature and obtain Double-layer asphalt carbon bag
Cover lithium iron phosphate positive material.
9. according to the preparation method of any one of the claim 1-5 Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrodes, it is special
Sign is, in S2, heating rate is 5~15 DEG C/min.
10. a kind of Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that using any one of claim 1-9 institutes
The preparation method for stating Double-layer asphalt carbon-coated LiFePO 4 for lithium ion batteries positive electrode is made.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110931756A (en) * | 2019-12-13 | 2020-03-27 | 成都爱敏特新能源技术有限公司 | High-performance silicon-carbon composite negative electrode material with adjustable particle size and preparation method thereof |
| CN111170294A (en) * | 2020-01-19 | 2020-05-19 | 江苏乐能电池股份有限公司 | Preparation method of low-cost lithium iron phosphate composite material |
| CN113054195A (en) * | 2021-03-16 | 2021-06-29 | 河北九丛科技有限公司 | Post-treatment method of phosphate anode material |
| CN113054173A (en) * | 2021-03-12 | 2021-06-29 | 合肥国轩高科动力能源有限公司 | Low-temperature lithium iron phosphate and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746741A (en) * | 2008-12-11 | 2010-06-23 | 中国电子科技集团公司第十八研究所 | Precursor used for coating iron phosphate lithium |
| CN105591100A (en) * | 2014-10-27 | 2016-05-18 | 深圳市比克电池有限公司 | Method of preparing lithium iron phosphate cathode material through hydrothermal method, and the cathode material |
| CN106848222A (en) * | 2017-01-18 | 2017-06-13 | 深圳市沃特玛电池有限公司 | A kind of preparation method of LiFePO4/bis- carbon-coating clad composite material |
| CN107240696A (en) * | 2017-07-12 | 2017-10-10 | 北方奥钛纳米技术有限公司 | The preparation method and carbon-coated LiFePO 4 for lithium ion batteries and lithium ion battery of carbon-coated LiFePO 4 for lithium ion batteries |
-
2017
- 2017-10-17 CN CN201710962747.9A patent/CN107845791B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746741A (en) * | 2008-12-11 | 2010-06-23 | 中国电子科技集团公司第十八研究所 | Precursor used for coating iron phosphate lithium |
| CN105591100A (en) * | 2014-10-27 | 2016-05-18 | 深圳市比克电池有限公司 | Method of preparing lithium iron phosphate cathode material through hydrothermal method, and the cathode material |
| CN106848222A (en) * | 2017-01-18 | 2017-06-13 | 深圳市沃特玛电池有限公司 | A kind of preparation method of LiFePO4/bis- carbon-coating clad composite material |
| CN107240696A (en) * | 2017-07-12 | 2017-10-10 | 北方奥钛纳米技术有限公司 | The preparation method and carbon-coated LiFePO 4 for lithium ion batteries and lithium ion battery of carbon-coated LiFePO 4 for lithium ion batteries |
Non-Patent Citations (1)
| Title |
|---|
| 曹杰 等: ""双层碳包覆Li4Ti5O12的合成和电化学性能研究"", 《上海电力学院学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110931756A (en) * | 2019-12-13 | 2020-03-27 | 成都爱敏特新能源技术有限公司 | High-performance silicon-carbon composite negative electrode material with adjustable particle size and preparation method thereof |
| CN111170294A (en) * | 2020-01-19 | 2020-05-19 | 江苏乐能电池股份有限公司 | Preparation method of low-cost lithium iron phosphate composite material |
| CN113054173A (en) * | 2021-03-12 | 2021-06-29 | 合肥国轩高科动力能源有限公司 | Low-temperature lithium iron phosphate and preparation method and application thereof |
| CN113054195A (en) * | 2021-03-16 | 2021-06-29 | 河北九丛科技有限公司 | Post-treatment method of phosphate anode material |
| CN113054195B (en) * | 2021-03-16 | 2022-05-03 | 河北九丛科技有限公司 | Post-treatment method of phosphate anode material |
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