CN102856553A - Preparation method of hydrothermal synthesis carbon coated lithium iron phosphate - Google Patents
Preparation method of hydrothermal synthesis carbon coated lithium iron phosphate Download PDFInfo
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- CN102856553A CN102856553A CN2012103839279A CN201210383927A CN102856553A CN 102856553 A CN102856553 A CN 102856553A CN 2012103839279 A CN2012103839279 A CN 2012103839279A CN 201210383927 A CN201210383927 A CN 201210383927A CN 102856553 A CN102856553 A CN 102856553A
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method of preparing lithium ion battery anode material, namely, carbon coated lithium iron phosphate by utilizing ascorbic acid as reducing agent and carbon source, and the method comprises: adding ascorbic acid in a reaction solution to prevent Fe2<+> from being oxidized to Fe3<+>, and hydrothermal synthesizing LiFePO4; adding the ascorbic acid in the LiFePO4 to serve as reducing agent and carbon source to prepare a LiFePO4/C precursor; and roasting the LiFePO4/C precursor at a high temperature under the shield of argon atmosphere to obtain lithium iron phosphate uniformly coated by carbon. The method disclosed by the invention wraps the carbon to control the morphology of the crystalline grain and improve the lithium-ion diffusion coefficient of lithium iron phosphate so as to obtain a lithium iron phosphate material with uniform dimension and excellent electrochemical performance. The preparation method disclosed by the invention is simple and economic and is suitable for industrial mass production.
Description
Technical field
The invention belongs to the new energy materials technical field, relate to a kind of preparation method of LiFePO4, be specifically related to a kind of method for preparing carbon-coated lithium iron phosphate composite with hydrothermal synthesis method.
Background technology
The large electric current Study on Li-ion batteries using of high power capacity is not only extremely important to the development in electric automobile field, and also significant to effective storage, the utilization of the clean energy resourcies such as wind, electricity, solar energy.Yet the development of lithium ion battery is limited by the raising of electrode material performance to a large extent, so the research of high-performance positive electrode is the effective way that solves the lithium ion battery applications bottleneck.
The positive electrode that proposes the earliest is the LiCoO with layer structure
2Material, through for a long time development, the existing positive electrode of lithium ion battery mainly is represented as the LiCoO of layer structure at present
2, LiNiO
2, LiMnO
2And their solid solution, the LiMn of spinel structure
2O
4, and have olivine structural LiFePO
4At present, LiFePO
4It is anode material for lithium-ion batteries of new generation of greatest concern on the market.The reported first such as goodenough in 1997 have a LiFePO of olivine structural
4Embedding that can be reversible and deviating from after the Li, this material receives great concern.LiFePO
4Theoretical capacity be 170 mAh/g, be 3.4V with respect to the stable discharging platform of lithium an-ode, with traditional lithium ion anode material LiMn
2O
4And LiCoO
2Compare LiFePO
4Raw material sources are more extensive, have extended cycle life, Heat stability is good, price is cheaper and environmental friendliness, pollution-free, is one of the strongest competitor of anode material for lithium-ion batteries of future generation.
Because LiFePO
4Special structure causes Li
+So the passage that only has one dimension to transmit is Li
+Diffusion rate at material internal is lower.Researcher overcomes this shortcoming by method of modifying such as doping, coatings.
(the Chung S Y such as Chiang, Bloking J T, Chiang Y M. Electronically conductive phospho-olivines as lithium storage electrocles[J], Nature Materials, 2002,1 (2): the 123-128) LiFePO of employing synthesizing cationic defective
4, and carry out therein high-valency metal (Nb
5+, Mg
2+, Al
3+, Ti
4+, W
6+Deng) the solid solution doping, thereby LiFePO
4Conductivity improved 8 orders of magnitude, surpassed traditional LiCoO
2, LiMn
2O
4Conductivity.The people such as Croce (Croce F, Epifanio A D, Hassoun J, et al. A novel concept for the synthesis of an improved LiFePO
4Lithium battery cathode [J]. Elecrochem Solid-State Lett, 2002,5 (3): 47-50) Cu and the Ag of doping 1% in LiFePO4, the specific capacity of material has improved 25mAh/g.Reason is to be dispersed in LiFePO
4In metallic to LiFePO
4The effect of conducting bridge is provided, has strengthened the conductive capability between the particle, reduced the impedance between the particle, metal Cu and mixing also of Ag can be reduced LiFePO simultaneously
4The size of particle, thereby the reversible specific capacity of raising material.Because at LiFePO
4In, Li
+Be the one dimension diffusion, therefore, effectively control LiFePO
4Particle size be to improve LiFePO
4The key of the diffusivity of middle lithium ion.The people such as Huang (Huang H, Yings C, Nazra L F. Approachong theoretical capacity of LiFePO
4At room temperature at high rates [J]. Electrochemical and solid-State Letters, 2001,4 (10): 170-172) be used in the mixed solution of reactant and add by HNO
3/ H
2SO
4The carbon black of processing because the carbon black of partial oxidation contains carboxyl, serves as into nuclear particle, has obtained the LiFePO of particle diameter less than 200nm
4Discharge can obtain the specific capacity more than the 150mAh/g under the 0.1C electric current, and the performance under the large electric current is the very excellent specific capacity that can obtain about 130mAh/g also.At LiFePO
4Middle dispersion or coated with conductive carbon can strengthen the electron conduction between particle and the particle on the one hand, reduce the polarization of battery; Also can be LiFePO on the other hand
4Provide electron tunnel, with compensation Li
+Take off the charge balance in the embedding process.
Summary of the invention
The object of the invention is to overcome lithium ion battery anode material lithium iron phosphate conductivity and the low problem of lithium ion diffusion coefficient, a kind of Hydrothermal Synthesis carbon-coated LiFePO 4 for lithium ion batteries (LiFePO is provided
4/ C composite material) preparation method.
The present invention adopts following technical scheme:
A kind of preparation method of Hydrothermal Synthesis carbon-coated LiFePO 4 for lithium ion batteries may further comprise the steps:
(1) LiFePO
4Synthesizing of precursor: at FeSO
4, H
3PO
4In the mixed solution of an amount of ascorbic acid, add LiOH solution, wherein FeSO
4, H
3PO
4With the mol ratio of LiOH be 1:1:3, hydro-thermal reaction is also carried out in heating under stirring condition; After the product cooling, centrifugal, cleaning and dry obtains LiFePO
4The precursor powder;
(2) LiFePO
4/ C precursor synthetic: the LiFePO that step (1) is obtained
4After precursor powder and ascorbic acid disperseed with alcohol, ball milling mixed, and 100 ℃ of vacuumizes are to obtaining black powder;
(3) LiFePO
4/ C composite material synthetic: under inert atmosphere protection, the LiFePO that step (2) is obtained
4The roasting of/C precursor obtains the LiFePO4 that carbon coats.
In the step (1), described hydrothermal temperature is 100～140 ℃, and the reaction time is 1～4h.
In the step (2), described LiFePO
4The mass ratio of precursor powder and ascorbic acid is LiFePO
4: ascorbic acid=1:0.005～0.10, preferred 1:0.03～0. 07.
In the step (3), described sintering temperature is 600～800 ℃, and roasting time is 6～15h.
More specifically and optimally, described method may further comprise the steps:
(1) LiFePO
4Synthesizing of precursor: take by weighing FeSO take mol ratio as 1:1:3
4.7H
2O, H
3PO
4And LiOH.H
2O is first with FeSO
4.7H
2O, H
3PO
4Be dissolved in the 50 ml water, then add the ascorbic acid of 0.2 g to prevent Fe
2+Be oxidized to Fe
3+, add at last the LiOH.H that has been dissolved in the water
2O transfers to solution rapidly in the 500 ml stainless steel cauldrons, places it in the heat collecting type magnetic force heating stirrer, and set temperature is 120 ℃ and stirring reaction 2h; After reactor is cooled to room temperature, product is centrifugal, after water cleaning and alcohol disperse, place the dry 2h of vacuum drying chamber to obtain jade-green powder.
(2) LiFePO
4/ C precursor synthetic: the LiFePO that step (1) is obtained
4Precursor powder and ascorbic acid be LiFePO in mass ratio
4: ascorbic acid=1:0.03～0.07 usefulness alcohol behind ball milling 4h on the ball mill, is placed in the vacuum drying chamber after disperseing, and 100 ℃ of dry 2h obtain black powder.
(3) LiFePO
4Synthesizing of/C composite material: under the argon gas atmosphere protection, with above-mentioned LiFePO
4/ C precursor is transferred in the tube furnace, at 700 ℃ of lower 10h that process, obtains the LiFePO4 that carbon evenly coats.
Carbon-coated LiFePO 4 for lithium ion batteries (the LiFePO that the present invention is made
4/ C) material structure characterizes and performance evaluation, and evaluation method is as follows:
Analyze phase structure, the crystal parameters of crystal grain by wide-angle X ray diffractor (XRD), such as microstructure characteristics such as lattice constant, unit cell volume, crystallite dimensions.The instrument model is A Rigaku D/Max-3C, and condition is: Cu target K alpha ray, pipe is pressed 50kV, tube current 200mA.As shown in Figure 1, the difference of carbon content does not cause the variation of phase in the sample.Do not have spuious peak in the sample and occur, all demonstrate the single-phase structure, little to the LiFePO4 Effects on Microstructure.
The internal structure of pattern, particle diameter and crystalline particle by ESEM (SEM) and transmission Electronic Speculum (TEM) analysing particulates, and particle surface carbon coating situation etc., the instrument model is: JSM-5610LV JEOL(SEM), JEM-2100F(TEM), accelerating voltage is 200kv.As shown in Figure 2, it is 200-300nm that LiFePO4 does not have the particle size of carbon coated, and the particle size after the carbon coated is about 100-150nm.
Come the charge-discharge performance (comprising charge/discharge capacity, cycle life, voltage platform) of research material and the electrochemical kinetics performance of positive electrode etc. by charge-discharge test and electrochemical impedance spectroscopy (EIS).The instrument model is: electrochemical workstation (Arbin) and CHI660D.Take open circuit voltage as benchmark, applying amplitude is 5mV, 10
5Scan in the frequency range of ~ 0.01H.
The preparation method of Hydrothermal Synthesis carbon-coated LiFePO 4 for lithium ion batteries of the present invention is by the synthetic LiFePO of low-temperature hydrothermal
4As reducing agent and carbon source, prepare carbon-coated LiFePO 4 for lithium ion batteries by argon gas atmosphere protection heating carbon coated with ascorbic acid, obtain the nanosphere of size uniform, pattern homogeneous; control the pattern of crystal grain and the lithium ion diffusion coefficient of raising LiFePO4 by carbon coated, its chemical property is good.The present invention adopts cheap FeSO
4Be source of iron, prepare the good LiFePO4 of chemical property by hydrothermal synthesis method, the preparation method is simple, synthesis path is more single, cost is low, non-environmental-pollution, is suitable for large-scale industrial production.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not limited with embodiment, but is limited by claim.
Description of drawings
Fig. 1 is the LiFePO of different carbon contents prepared according to the methods of the invention
4The XRD collection of illustrative plates of/C composite material.
Fig. 2 is the LiFePO of different carbon contents prepared according to the methods of the invention
4The SEM of/C composite material and TEM collection of illustrative plates.Wherein A1, A2 are LiFePO
4The SEM of-0%C and TEM collection of illustrative plates, B1, B2 are LiFePO
4The SEM of-5%C and TEM collection of illustrative plates.
Fig. 3 is the LiFePO of different carbon contents prepared according to the methods of the invention
4Charging/discharging voltage-the Capacity Plan of/C composite material.Wherein (a) is LiFePO
4-0%C; (b) be LiFePO
4-3%C, (c) LiFePO
4-5%C is that (d) is LiFePO
4-7%C.
Fig. 4 is the LiFePO of different carbon contents prepared according to the methods of the invention
4The electrochemical impedance collection of illustrative plates of/C composite material.
Embodiment
A kind of Hydrothermal Synthesis carbon-coated LiFePO 4 for lithium ion batteries (LiFePO
4/ C composite material) synthetic method may further comprise the steps:
(1) LiFePO
4Synthesizing of precursor: take by weighing FeSO take mol ratio as 1:1:3
4.7H
2O, H
3PO
4And LiOH.H
2O is first with FeSO
4.7H
2O, H
3PO
4Be dissolved in the distilled water of 50 ml, then add the ascorbic acid of 0.2 g to prevent Fe
2+Be oxidized to Fe
3+, add at last the LiOH.H that has dissolved
2O transfers to solution rapidly in the 500 ml stainless steel cauldrons, places it in the heat collecting type magnetic force heating stirrer, and set temperature is 120 ℃ and stirring reaction 2h.After reactor is cooled to room temperature, product is centrifugal, after distilled water cleaning and alcohol dispersion, place the dry 2h of vacuum drying chamber to obtain jade-green powder.
(2) LiFePO
4/ C precursor synthetic: the precursor powder that step (1) is obtained and ascorbic acid are by certain mass ratio (LiFePO
4: ascorbic acid=1:0.03, w/w) place the agate tank to disperse with alcohol after, behind ball milling 4h (450r) on the planetary ball mill, be placed in the vacuum drying chamber, 100 ℃ of dry 2h obtain black powder.
(3) LiFePO
4Synthesizing of/C composite material: under the argon gas atmosphere protection, with above-mentioned LiFePO
4/ C precursor is transferred in the tube furnace, obtains the LiFePO4 that carbon evenly coats at 700 ℃ of lower 10h of processing.
Embodiment 2
A kind of Hydrothermal Synthesis carbon-coated LiFePO 4 for lithium ion batteries (LiFePO
4/ C composite material) synthetic method may further comprise the steps:
(1) LiFePO
4Synthesizing of precursor: take by weighing FeSO take mol ratio as 1:1:3
4.7H
2O, H
3PO
4And LiOH.H
2O is first with FeSO
4.7H
2O, H
3PO
4Be dissolved in the distilled water of 50 ml, then add the ascorbic acid of 0.2 g to prevent Fe
2+Be oxidized to Fe
3+, add at last the LiOH.H that has dissolved
2O transfers to solution rapidly in the 500 ml stainless steel cauldrons, places it in the heat collecting type magnetic force heating stirrer, and set temperature is 120 ℃ and stirring reaction 2h.After reactor is cooled to room temperature, product is centrifugal, after distilled water cleaning and alcohol dispersion, place the dry 2h of vacuum drying chamber to obtain jade-green powder.
(2) LiFePO
4/ C precursor synthetic: the precursor powder that step (1) is obtained and ascorbic acid are by certain mass ratio (LiFePO
4: ascorbic acid=1:0.05 w/w) place the agate tank to disperse with alcohol after, behind ball milling 4h (450r) on the planetary ball mill, be placed in the vacuum drying chamber, 100 ℃ of dry 2h obtain black powder.
(3) LiFePO
4Synthesizing of/C composite material: under the argon gas atmosphere protection, with above-mentioned LiFePO
4/ C precursor is transferred in the tube furnace, obtains the LiFePO4 that carbon evenly coats at 700 ℃ of lower 10h of processing.
A kind of Hydrothermal Synthesis carbon-coated LiFePO 4 for lithium ion batteries (LiFePO
4/ C composite material) synthetic method may further comprise the steps:
(1) LiFePO
4Synthesizing of precursor: take by weighing FeSO take mol ratio as 1:1:3
4.7H
2O, H
3PO
4And LiOH.H
2O is first with FeSO
4.7H
2O, H
3PO
4Be dissolved in the distilled water of 50 ml, then add the ascorbic acid of 0.2 g to prevent Fe
2+Be oxidized to Fe
3+, add at last the LiOH.H that has dissolved
2O transfers to solution rapidly in the 500 ml stainless steel cauldrons, places it in the heat collecting type magnetic force heating stirrer, and set temperature is 120 ℃ and stirring reaction 2h.After reactor is cooled to room temperature, product is centrifugal, after distilled water cleaning and alcohol dispersion, place the dry 2h of vacuum drying chamber to obtain jade-green powder.
(2) LiFePO
4/ C precursor synthetic: the precursor powder that step (1) is obtained and ascorbic acid are by certain mass ratio (LiFePO
4: ascorbic acid=1:0.07 w/w) place the agate tank to disperse with alcohol after, behind ball milling 4h (450r) on the planetary ball mill, be placed in the vacuum drying chamber, 100 ℃ of dry 2h obtain black powder.
(3) LiFePO
4Synthesizing of/C composite material: under the argon gas atmosphere protection, with above-mentioned LiFePO
4/ C precursor is transferred in the tube furnace, obtains the LiFePO4 that carbon evenly coats at 700 ℃ of lower 10h of processing.
Comparative Examples 1
A kind of synthetic method of Hydrothermal Synthesis LiFePO4 may further comprise the steps:
(1) LiFePO
4Synthesizing of precursor: take by weighing FeSO take mol ratio as 1:1:3
4.7H
2O, H
3PO
4And LiOH.H
2O is first with FeSO
4.7H
2O, H
3PO
4Be dissolved in the distilled water of 50 ml, then add the ascorbic acid of 0.2 g to prevent Fe
2+Be oxidized to Fe
3+, add at last the LiOH.H that has dissolved
2O transfers to solution rapidly in the 500 ml stainless steel cauldrons, places it in the heat collecting type magnetic force heating stirrer, and set temperature is 120 ℃ and stirring reaction 2h.After reactor is cooled to room temperature, product is centrifugal, after distilled water cleaning and alcohol dispersion, place the dry 2h of vacuum drying chamber to obtain jade-green powder.
(2) the precursor powder that step (1) is obtained behind ball milling 4h (450r) on the planetary ball mill, is placed in the vacuum drying chamber 100 ℃ of dry 2h after placing the agate tank to disperse with alcohol.
(3) LiFePO
4Synthetic: under the argon gas atmosphere protection, above-mentioned precursor is transferred in the tube furnace, is obtained LiFePO4 at 700 ℃ of lower 10h that process.
Claims (6)
1. the preparation method of a Hydrothermal Synthesis carbon-coated LiFePO 4 for lithium ion batteries is characterized in that, described method may further comprise the steps:
(1) LiFePO
4Synthesizing of precursor: at FeSO
4, H
3PO
4In the mixed solution of an amount of ascorbic acid, add LiOH solution, wherein FeSO
4, H
3PO
4With the mol ratio of LiOH be 1:1:3, hydro-thermal reaction is also carried out in heating under stirring condition; After the product cooling, centrifugal, cleaning and dry obtains LiFePO
4The precursor powder;
(2) LiFePO
4/ C precursor synthetic: the LiFePO that step (1) is obtained
4After precursor powder and ascorbic acid disperseed with alcohol, ball milling mixed, and 100 ℃ of vacuumizes are to obtaining black powder;
(3) LiFePO
4/ C composite material synthetic: under inert atmosphere protection, the LiFePO that step (2) is obtained
4The roasting of/C precursor obtains the LiFePO4 that carbon coats.
2. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries according to claim 1 is characterized in that, in the step (1), described hydrothermal temperature is 100～140 ℃, and the reaction time is 1～4h.
3. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries according to claim 1 is characterized in that, in the step (2), and described LiFePO
4The mass ratio of precursor powder and ascorbic acid is LiFePO
4: ascorbic acid=1:0.005～0.10.
4. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries according to claim 3 is characterized in that, in the step (2), and described LiFePO
4The mass ratio of precursor powder and ascorbic acid is LiFePO
4: ascorbic acid=1:0.03～0. 07.
5. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries according to claim 1 is characterized in that, in the step (3), described sintering temperature is 600～800 ℃, and roasting time is 6～15h.
6. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries according to claim 1 is characterized in that, described method may further comprise the steps:
(1) LiFePO
4Synthesizing of precursor: take by weighing FeSO take mol ratio as 1:1:3
4.7H
2O, H
3PO
4And LiOH.H
2O is first with FeSO
4.7H
2O, H
3PO
4Be dissolved in the water of 50 ml, then add the ascorbic acid of 0.2g to prevent Fe
2+Be oxidized to Fe
3+, add at last the LiOH.H that has been dissolved in the water
2O transfers to solution rapidly in the 500 ml stainless steel cauldrons, places it in the heat collecting type magnetic force heating stirrer, and set temperature is 120 ℃ and stirring reaction 2h; After reactor is cooled to room temperature, product is centrifugal, after water cleaning and alcohol disperse, place the dry 2h of vacuum drying chamber to obtain jade-green powder;
(2) LiFePO
4/ C precursor synthetic: the LiFePO that step (1) is obtained
4Precursor powder and ascorbic acid be LiFePO in mass ratio
4: ascorbic acid=1:0.03～0.07 usefulness alcohol behind ball milling 4h on the ball mill, is placed in the vacuum drying chamber after disperseing, and 100 ℃ of dry 2h obtain black powder;
(3) LiFePO
4Synthesizing of/C composite material: under the argon gas atmosphere protection, with above-mentioned LiFePO
4/ C precursor is transferred in the tube furnace, at 700 ℃ of lower 10h that process, obtains the LiFePO4 that carbon evenly coats.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104091950A (en) * | 2014-07-21 | 2014-10-08 | 中国科学院青海盐湖研究所 | Method for preparing lithium iron phosphate material with hydrothermal process |
| CN104617296A (en) * | 2015-01-23 | 2015-05-13 | 上海大学 | Method for preparing mesoporous carbon coated LiFePO4 electrode material |
| CN105336926A (en) * | 2015-09-27 | 2016-02-17 | 常州市奥普泰科光电有限公司 | Preparation method of copper-silver doped lithium iron phosphate positive electrode material |
| CN105789605A (en) * | 2014-12-22 | 2016-07-20 | 深圳市比克电池有限公司 | Carbon coated LiFePO4, preparing method of the carbon coated LiFePO4 and power lithium ion cell |
| CN107507975A (en) * | 2017-08-24 | 2017-12-22 | 扬州大学 | A kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nano-hollow ball |
| US20180198130A1 (en) * | 2014-10-24 | 2018-07-12 | Semiconductor Energy Laboratory Co., Ltd. | Storage battery electrode, manufacturing method thereof, storage battery, and electronic device |
| CN112928268A (en) * | 2021-04-01 | 2021-06-08 | 神华准能资源综合开发有限公司 | Preparation method of carbon-coated lithium iron phosphate composite material and carbon-coated lithium iron phosphate composite material |
| CN114039045A (en) * | 2021-11-01 | 2022-02-11 | 天能帅福得能源股份有限公司 | Preparation method of in-situ carbon-coated modified lithium iron phosphate lithium ion battery |
| CN114715871A (en) * | 2022-04-26 | 2022-07-08 | 张粒新 | Modified lithium iron phosphate cathode material for lithium battery and preparation method |
| CN115084529A (en) * | 2022-08-16 | 2022-09-20 | 四川富临新能源科技有限公司 | Surface modification method of lithium iron phosphate positive electrode material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102315450A (en) * | 2011-08-31 | 2012-01-11 | 合肥国轩高科动力能源有限公司 | Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate |
| 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 |
-
2012
- 2012-10-11 CN CN2012103839279A patent/CN102856553A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102315450A (en) * | 2011-08-31 | 2012-01-11 | 合肥国轩高科动力能源有限公司 | Hydrothermal synthesis preparation method of ion doping high-performance lithium iron phosphate |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| DENG HONG-GUI,ET AL.: "LiFePO4/C Nanocomposites Synthesized from Fe2O3 by a Hydrothermal Reaction-calcination Process and Their Electrochemical Performance", 《无机材料学报》 * |
| HONGFA XIANG,ET AL.: "Hydrothermal synthesis of ultra-thin LiFePO4 platelets for Li-ion batteries", 《J MATER SCI》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104091950A (en) * | 2014-07-21 | 2014-10-08 | 中国科学院青海盐湖研究所 | Method for preparing lithium iron phosphate material with hydrothermal process |
| US20180198130A1 (en) * | 2014-10-24 | 2018-07-12 | Semiconductor Energy Laboratory Co., Ltd. | Storage battery electrode, manufacturing method thereof, storage battery, and electronic device |
| CN105789605A (en) * | 2014-12-22 | 2016-07-20 | 深圳市比克电池有限公司 | Carbon coated LiFePO4, preparing method of the carbon coated LiFePO4 and power lithium ion cell |
| CN104617296A (en) * | 2015-01-23 | 2015-05-13 | 上海大学 | Method for preparing mesoporous carbon coated LiFePO4 electrode material |
| CN105336926B (en) * | 2015-09-27 | 2017-12-29 | 金久科技有限公司 | A kind of preparation method of copper doped, silver-colored lithium iron phosphate positive material |
| CN105336926A (en) * | 2015-09-27 | 2016-02-17 | 常州市奥普泰科光电有限公司 | Preparation method of copper-silver doped lithium iron phosphate positive electrode material |
| CN107507975A (en) * | 2017-08-24 | 2017-12-22 | 扬州大学 | A kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nano-hollow ball |
| CN112928268A (en) * | 2021-04-01 | 2021-06-08 | 神华准能资源综合开发有限公司 | Preparation method of carbon-coated lithium iron phosphate composite material and carbon-coated lithium iron phosphate composite material |
| CN114039045A (en) * | 2021-11-01 | 2022-02-11 | 天能帅福得能源股份有限公司 | Preparation method of in-situ carbon-coated modified lithium iron phosphate lithium ion battery |
| CN114715871A (en) * | 2022-04-26 | 2022-07-08 | 张粒新 | Modified lithium iron phosphate cathode material for lithium battery and preparation method |
| CN114715871B (en) * | 2022-04-26 | 2023-09-12 | 四川朗晟新材料科技有限公司 | Modified lithium iron phosphate positive electrode material for lithium battery and preparation method |
| CN115084529A (en) * | 2022-08-16 | 2022-09-20 | 四川富临新能源科技有限公司 | Surface modification method of lithium iron phosphate positive electrode material |
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