CN101714634A - Method for preparing carbon-coated LiFePO4 by microwaves and carbon-coated LiFePO4 material - Google Patents
Method for preparing carbon-coated LiFePO4 by microwaves and carbon-coated LiFePO4 material Download PDFInfo
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Abstract
The invention provides a method for preparing carbon-coated LiFePO4 by microwaves, which comprises the following steps: respectively obtaining a lithium source compound, a ferrous iron source compound and a phosphorous source compound in a stoichiometric ratio of the LiFePO4 required to be prepared, and adding a microwave absorber, an organic carbon source and a liquid dispersant; performing ball milling on the obtained raw material and drying treatment; putting the dried product in a microwave heating reaction cavity, and introducing protective gas into the reaction cavity; and heating to the temperature of between 550 and 850DEG C with the microwaves, introducing carbon source gas, and performing pyrolysis on the carbon source gas at the temperature of between 550 and 850DEG C to prepare the carbon-coated LiFePO4. The invention also provides a carbon-coated LiFePO4 material prepared by the method. The preparation method adopts microwave heating, and the carbon source gas is subjected to pyrolysis, so that the carbon species are deposited on the surface of the LiFePO4 to obtain the complete, uniform and firm carbon-coated LiFePO4; and simultaneously, by the preparation method, the machining property and the electrochemical performance of the LiFePO4 material can be obviously improved.
Description
Technical field
The present invention relates to the preparation method of material with carbon element, relate in particular to a kind of LiFePO 4 by microwaves preparation method of carbon coating and the LiFePO 4 material that carbon coats.
Background technology
At present, along with industrialized process is accelerated and economic growth at full speed, energy problem has become one of human problem demanding prompt solution.Since half a century, the scientific research institution in the whole world starts to develop on the one hand such as new forms of energy such as water energy, solar energy, wind energy and nuclear energy; More and more pay attention to the efficient storage and the utilization of energy on the other hand.Existing storage mainly contains four kinds of lead-acid battery, ickel-cadmium cell (Cd/Ni), metal-hydrogen nickel battery (MH/Ni) and lithium ion batteries etc. with secondary cell.Wherein, lithium ion battery has voltage height, specific energy height, discharges and recharges safely and fast, self-discharge rate is low, recycle the life-span long, environmental pollution is little and advantage such as memory-less effect.
Lithium ion battery mainly comprises positive pole, electrolyte and three parts of negative pole.The electrode material of lithium ion battery is most important for chemical property that improves battery and aspect such as reduce cost.Because negative material uses the graphite material of modification more, has higher specific capacity.Thereby the research of current lithium ion battery electrode material mainly concentrates in the exploitation of excellent positive electrode.
LiFePO
4Start from the pioneering research of Padhi in 1997 as the research of positive electrode.With respect to current other positive electrode (cobalt acid lithium, lithium nickelate, LiMn2O4), LiFePO
4Have height safely, recycle life-span height, specific capacity height, overcharging resisting and anti-exoergic power height, high temperature capacity height, environmental protection and the distinguishing feature such as cheap crossed.Therefore, LiFePO
4It is a kind of more potential anode material for lithium-ion batteries.
The microwave preparation of LiFePO4 mainly is divided into solid phase method and liquid phase method.Traditional solid phase method manufacturing cycle is long and power consumption is high, the difficult LiFePO 4 powder of even structure and stable performance of preparing.And microwave technology utilization rate of electrical height especially can be finished the preparation of material in tens of even a few minutes, makes cost reduce greatly.
Since the restriction of self structure, LiFePO
4Exist conductivity low by (10
-9～10
-10S/cm) problem, and this is very important for the electrode charge and discharge process that is subjected to conductivity control, thus greatly limited LiFePO
4Application as anode material for lithium-ion batteries.The approach that addresses this problem at present mainly is by the outer mutually mode of mixing in (carbon or metal) and the body that coats of body.Wherein, coat complete, even, firm carbon coating layer at the LiFePO4 particle surface and not only can improve the tap density and the specific energy of material to a certain extent, and can significantly improve the chemical property of material.
At present, microwave method prepares lithium iron phosphate positive material, and the technology that adopts raw material mixing, drying, compressing tablet, activated carbon (or graphite) to cover the compressing tablet indirect mostly prepares lithium iron phosphate positive material.There is following deficiency in the bag carbon mode that these class methods adopt: the one, and conductive black only can form the bridging effect between the LiFePO4 particle, the 2nd, organic carbon source in the coating process because self decomposition can produce bubble, this all can influence the carbon cladding uniformity, is difficult to form complete conductive network.In addition, microwave absorption such as active carbon is because the poorly conductive of self also can bring pollution to lithium iron phosphate positive material.
Summary of the invention
In view of this, be necessary to provide the microwave preparation of a kind of carbon clad structure LiFePO4 that evenly firm carbon coats.
And, the LiFePO 4 material that the evenly firm carbon of a kind of carbon clad structure that is made by said method coats.
The microwave preparation of the LiFePO4 that a kind of carbon coats may further comprise the steps:
The stoichiometric proportion of Zhi Bei LiFePO4 is obtained Li source compound, ferrous iron source compound and P source compound respectively as required, and adds microwave absorption, organic carbon source and liquid dispersant;
The raw material that ball milling is obtained, and carry out dried;
Dried product is placed the microwave heating reaction chamber, in reaction chamber, feed protective gas;
To 550-850 ℃, feed carbon-source gas by microwave heating, pyrolysis carbon-source gas under 550-850 ℃ of temperature makes the LiFePO4 that carbon coats.
And the LiFePO 4 material that a kind of carbon coats comprises the LiFePO4 that carbon that the microwave preparation of the LiFePO4 that coats according to above-mentioned carbon makes coats.
In technique scheme, the microwave preparation of the LiFePO4 that described carbon coats adopts the method for microwave heating, simultaneously with the carbon-source gas vapour-phase pyrolysis, makes carbon species be deposited on the LiFePO4 surface.Coating mode by microwave heating technique and multiple carbon synergy (organic large source and carbon-source gas vapour-phase pyrolysis), complete, the even and firm LiFePO 4 material of carbon clad structure that obtains, this preparation method can significantly improve the machining property and the chemical property of LiFePO 4 material.
Description of drawings
Fig. 1 is the microwave preparation schematic flow sheet of the LiFePO4 that coats of the carbon of the embodiment of the invention.
Fig. 2 is the internal structure schematic diagram in the microwave reaction chamber of being adopted in the method among Fig. 1.
Fig. 3 is the XRD figure spectrum of the sample A of the embodiment of the invention 1 preparation.
Fig. 4 is transmission electron microscope (TEM) figure of the sample A of the embodiment of the invention 1 preparation.
Fig. 5 is the charging and discharging curve figure of the sample A of the embodiment of the invention 1 preparation.
Fig. 6 is the charging and discharging curve figure of the sample B of the embodiment of the invention 2 preparations.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with drawings and Examples.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
See also Fig. 1, the microwave preparation flow process of the LiFePO4 that the carbon of the demonstration embodiment of the invention coats may further comprise the steps:
S01: the stoichiometric proportion of Zhi Bei LiFePO4 is obtained Li source compound, ferrous iron source compound and P source compound respectively as required, and adds microwave absorption, organic carbon source and liquid dispersant;
S02: the raw material that ball milling is obtained, and carry out dried;
S03: dried product is placed the microwave heating reaction chamber, in reaction chamber, feed protective gas;
S04: to 550-850 ℃, feed carbon-source gas by microwave heating, pyrolysis carbon-source gas under 550-850 ℃ of temperature makes the LiFePO4 that carbon coats.
In step S01, Li source compound can be the inorganic matter that lithium carbonate, lithium hydroxide etc. contain lithium, perhaps chooses the organic substance that lithium oxalate and lithium lactate etc. contain lithium; Divalence source of iron (Fe (II)) compound can select ferrous oxalate, ferrous acetate or ferrous lactate etc. to contain ferrous organic salt; P source compound can be selected phosphorus-containing compounds such as ammonium dihydrogen phosphate and ammonium hydrogen phosphate; Organic carbon source can be chosen solid organic matters such as sucrose, glucose, powder-beta-dextrin, lactose or resin; Microwave absorption can be the material with carbon element of conductive and heat-conductive, for example selects the acetylene black of conductive and heat-conductive for use; Liquid dispersant can be chosen ethanol or acetone, utilizes liquid dispersant can guarantee the abundant mixing of powder in mechanical milling process, and significantly improves grinding efficiency.The selection that is appreciated that above compound is not limited to this as just for example.
Because the LiFePO4 chemical formula of final preparation is LiFePO
4So the ratio of Li, Fe, P was 1: 1: 1 left and right sides scope in Li source compound, ferrous iron source compound and the P source compound.In the present embodiment, three's ratio is as follows: Li: Fe (II): P=(0.95～1.20): 1: 1.
In addition, the addition of microwave absorption can be the 5-30% of the LiFePO4 weight that coats of the carbon that generates.The 5-30% of the LiFePO4 weight that the addition of organic carbon source can coat for the carbon that generates.
In step S02, will carry out ball milling according to the various raw materials that aforementioned proportion is chosen, for example adopt agate ball and dispersant high speed ball milling together, carry out dried again after ball milling is good.Wherein drying is to carry out under vacuum, and baking temperature is preferably 60-120 ℃, and drying time, for example, can be 2-24 hour drying time, but be not limited thereto so that the good powder acquisition intensive drying of ball milling is as the criterion.
In step S03, treat the good powder intensive drying of ball milling after, dried product is placed the microwave heating reaction chamber, and in reaction chamber, feeds protective gas.When feeding protective gas, open vacuum pump earlier, reaction chamber is vacuumized earlier, in reaction chamber, feed protective gas then, for example can be inflated to an atmospheric pressure.Protective gas can be nitrogen or inert gases such as helium, argon.
See also Fig. 2, show the employed microwave heating reaction chamber 10 of preparation method of present embodiment.Inhale ripple carrier 16 by outside to inside being provided with ripple insulation material 12, microwave absorbing auxiliary heating body 14 and porous in this microwave heating reaction chamber 10.Wherein, each composition material of reaction chamber 10 is as follows, and for example, saturating ripple insulation material 12 can be an aluminosilicate fiber cotton, and microwave absorbing auxiliary heating body 14 can be the active carbon calandria, and it can be porous graphite that porous is inhaled ripple carrier 16.Wherein, this microwave heating reaction chamber 10 is a tubular housing, for example adopts a quartz ampoule.Saturating ripple insulation material 12 and microwave absorbing auxiliary heating body 14 can be the drums with the coaxial setting of tubular housing, the chamber wall setting that saturating ripple insulation material 12 is pasting reaction chamber 10, and microwave absorbing auxiliary heating body 14 is pasting the inwall setting of saturating ripple insulation material 12.Microwave absorbing auxiliary heating body 14 forms a reaction compartment 18, and reaction compartment 18 has both ends open.Porous is inhaled ripple carrier 16 and is divided into the setting of two places, lays respectively at the both ends open place at reaction compartment 18.19 of the well also dried powders of ball milling are carried on porous and inhale on the ripple carrier 16.
See also Fig. 1 and 2, in step S04, make the temperature of reaction chamber 10 be increased to 550-850 ℃ by microwave, be incubated then, under this temperature, feed carbon-source gas, pyrolysis carbon-source gas under 550-850 ℃ of temperature makes the LiFePO4 that carbon coats.Particularly, be warming up to 550-850 ℃ by selected microwave input power control earlier, the insulation reaction time is 3～20min.Regulating pyrolysis carbon source gas flow and the stable flow that feeds carbon-source gas simultaneously, can be the bottom feeding by reaction chamber 10, then, the carbon-source gas pyrolysis, carbon laydown forms the LiFePO4 that carbon coats at the LiFePO4 particle surface that forms.After reaction finishes, stop the microwave input, and close the pyrolysis carbon-source gas.After waiting to naturally cool to room temperature, promptly get the LiFePO 4 material that carbon containing coats.
As from the foregoing, the LiFePO 4 material that coats of the carbon that makes by said method comprises that LiFePO4 particle and gas phase pyrolytic deposition are between the LiFePO4 particle and the carbon coating layer of coated LiFePO 4 for lithium ion batteries particle surface.By the mode of this microwave action in conjunction with vapour-phase pyrolysis carbon, this carbon coating layer is thin and evenly cover the LiFePO4 particle surface securely, and carbon coating layer also forms complete conductive network simultaneously.The lithium iron phosphate preparation method that the carbon of present embodiment coats is different from the bag carbon mode of existing carbon black that adopts and organic carbon source fully, can significantly improve the chemical property of LiFePO4 as anode material for lithium-ion batteries etc.In addition, the gas-phase product that reaction generates can also be in time taken away in the introducing of hydrocarbon gas, and this is very favourable for the synthetic dynamic process of LiFePO4.The advantage that also has of the embodiment of the invention is, the microwave absorption of conductive and heat-conductive is introduced directly into initial batch mixing process.This not only can guarantee the being heated evenly property of powder in the microwave building-up process, avoid existing compressing tablet that adopts usually and shattering process once more, and when being made into positive electrode, can effectively improve the conductivity of lithium iron phosphate positive material, eliminate the pollution that microwave absorptions such as adopting activated carbon brings to positive electrode, and can save the existing required step that in follow-up positive plate preparation process, still need add conductive carbon black, rational and effective has been simplified operation.
And, the synergistic coating mode of microwave heating technique that the embodiment of the invention relates to and multiple carbon (comprising organic carbon source and vapour-phase pyrolysis), can be in the short period (as 3-20min), finish the preparation of high performance carbon coated LiFePO 4 for lithium ion batteries positive electrode under the condition cheaply, and significantly improve its machining (mainly referring to tap density) and chemical property.
Below be the microwave preparation exemplifying embodiment of the LiFePO4 that coats of above-mentioned carbon, with the concrete operations technology that describes this method in detail and condition etc.
The preparation method of present embodiment 1 comprises following concrete steps:
(1) according to Li: Fe (II): P=0.95: 1: 1 mol ratio takes by weighing lithium hydroxide, ferrous oxalate and ammonium hydrogen phosphate respectively, microwave absorption 5wt% (calculating), the sucrose 25wt% (calculating) and the acetone that add conductive and heat-conductive by generating LiFePO4 by generating LiFePO4
(2) with agate ball high speed ball milling 10 hours, during ball milling, the mass ratio of each material was: raw material: dispersant: ball=1: 3: 6 forms powder;
(3) under 60 ℃, vacuum drying step (1) mill powder well placed microwave heating reaction chamber 10 after 24 hours;
(4) microwave heating reaction chamber 10 is vacuumized after, feed nitrogen to one atmospheric pressure;
(5) open microwave power 500W and be warming up to 550 ℃;
(6) regulating pyrolysis carbon source gas flow is 30sccm, insulation 20min;
Close gas when (7) stopping the microwave input, naturally cool to room temperature subsequently, promptly get the LiFePO4 that carbon coats.
To be designated as A by the identified as samples that above-mentioned steps makes.As shown in Figure 3, be the XRD figure spectrum of sample A, by this collection of illustrative plates as can be known, the powder of preparation is the high olivine-type LiFePO4 phase of degree of crystallinity.Fig. 4 is the transmission electron microscope photo of sample A, has shown that carbon coats intact LiFePO4 microscopic appearance.Recording product cut size is 1-5 μ m, and tap density is 2.1g/cm
3The LiFePO 4 material that the carbon that so obtains is coated is made into positive electrode, with the lithium sheet is negative pole, the LiFePO4 that test carbon coats is at the charge status of 0.1C multiplying power circulation 5 times, obtain charging and discharging curve as shown in Figure 5, as seen from the figure, at 25 ℃, under the 0.1C multiplying power for the third time discharge capacity be 143mAh/g.
Embodiment 2
The preparation method of present embodiment 2 comprises following concrete steps:
(1) according to Li: Fe (II): P=1.10: 1: 1 mol ratio takes by weighing lithium carbonate, ferric acetate and ammonium dihydrogen phosphate respectively, adds microwave absorption 15wt% (calculating by generating LiFePO4), powder-beta-dextrin 15wt% (calculating by generating LiFePO4) and the ethanol of conductive and heat-conductive;
(2) with agate ball high speed ball milling 6 hours, during ball milling, the mass ratio of each material was: raw material: dispersant: ball=1: 3: 5 forms powder;
(3) under 80 ℃, the powder that vacuumize (1) step is ground placed the microwave heating reaction chamber after 12 hours;
(4) vacuumize after, feed argon gas to an atmospheric pressure;
(5) open microwave power 1500W and be warming up to 700 ℃;
(6) regulating pyrolysis carbon source gas flow is 250sccm, insulation 12min;
Close gas when (7) stopping the microwave input, naturally cool to room temperature subsequently, promptly get the LiFePO4 that carbon coats.
To be designated as B by the identified as samples that above-mentioned steps makes.Similar with embodiment 1,, the analysis showed that the powder of preparation is that carbon coats LiFePO 4 material intact and that degree of crystallinity is high by XRD and TEM and discharge and recharge detection.Recording product cut size is 2-7 μ m, and tap density is 1.9g/cm
3The LiFePO 4 material that the carbon that so obtains is coated is made into positive electrode, with the lithium sheet is negative pole, the LiFePO4 that test carbon coats is at the charge status of 0.1C multiplying power circulation 5 times, obtain charging and discharging curve as shown in Figure 6, as seen from the figure, at 25 ℃, under the 0.1C multiplying power for the third time discharge capacity be 162mAh/g.
The preparation method of present embodiment 3 comprises following concrete steps:
(1) according to Li: Fe (II): P=1.20: 1: 1 mol ratio takes by weighing lithium oxalate, ferrous lactate and ammonium dihydrogen phosphate respectively, adds microwave absorption 25wt% (calculating by generating LiFePO4), glucose 5wt% (calculating by generating LiFePO4) and the ethanol of conductive and heat-conductive;
(2) with agate ball high speed ball milling 2 hours (raw material: dispersant: ball=1: 3: 4, mass ratio);
(3) under 120 ℃, the powder that vacuumize (1) step is ground placed the microwave heating reaction chamber after 2 hours;
(4) vacuumize after, feed nitrogen to one atmospheric pressure;
(5) open microwave power 2500W and be warming up to 850 ℃;
(6) regulating pyrolysis carbon source gas flow is 500sccm, insulation 6min;
Close gas when (7) stopping the microwave input, naturally cool to room temperature subsequently, promptly get carbon-coated LiFePO 4 for lithium ion batteries.
To be carried out XRD and TEM equally and be discharged and recharged detection by what above-mentioned steps made, the analysis showed that, the powder of preparation is that carbon coats LiFePO 4 material intact and that degree of crystallinity is high.Recording product cut size is 3-8 μ m, and tap density is 1.8g/cm
3With the lithium sheet is negative pole, and the LiFePO4 that test carbon coats is at the charge status of 0.1C multiplying power circulation 5 times, and the result shows, at 25 ℃, under the 0.1C multiplying power for the third time discharge capacity be 155mAh/g.
In each embodiment described above, the microwave preparation of the LiFePO4 that carbon coats adopts the method for microwave heating, simultaneously with the carbon-source gas vapour-phase pyrolysis, makes carbon species be deposited on the LiFePO4 surface.Coating mode by microwave heating technique and multiple carbon synergy (organic large source and carbon-source gas vapour-phase pyrolysis), obtain complete, the even and firm LiFePO 4 material of carbon clad structure, this preparation method can significantly improve the machining property and the chemical property of LiFePO 4 material.
The above only is preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of being done within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the microwave preparation of the LiFePO4 that coats of a carbon may further comprise the steps:
The stoichiometric proportion of Zhi Bei LiFePO4 is obtained Li source compound, ferrous iron source compound and P source compound respectively as required, and adds microwave absorption, organic carbon source and liquid dispersant;
The raw material that ball milling is obtained, and carry out dried;
Dried product is placed the microwave heating reaction chamber, in reaction chamber, feed protective gas;
To 550-850 ℃, feed carbon-source gas by microwave heating, pyrolysis carbon-source gas under 550-850 ℃ of temperature makes the LiFePO4 that carbon coats.
2. the microwave preparation of the LiFePO4 that carbon as claimed in claim 1 coats, it is characterized in that, described Li source compound is lithium carbonate, lithium hydroxide, lithium oxalate or lithium lactate, described ferrous iron source compound is ferrous oxalate, ferrous acetate or ferrous lactate, and described P source compound is ammonium dihydrogen phosphate or ammonium hydrogen phosphate; Organic carbon source is sucrose, glucose, powder-beta-dextrin, lactose or resin, and described liquid dispersant is ethanol or acetone.
3. the microwave preparation of the LiFePO4 that carbon as claimed in claim 1 coats is characterized in that described microwave absorption is the microwave absorption of conductive and heat-conductive.
4. the microwave preparation of the LiFePO4 that carbon as claimed in claim 1 coats is characterized in that described baking temperature is 60-120 ℃, and be 2-24 hour drying time.
5. the microwave preparation of the LiFePO4 that carbon as claimed in claim 1 coats is characterized in that described pyrolysis carbon-source gas is wave absorbtion or the low hydrocarbon gas of pyrolysis temperature.
6. the microwave preparation of the LiFePO4 that carbon as claimed in claim 1 coats is characterized in that, after feeding carbon-source gas, the pyrolysis carbon-source gas is 3-20 minute under 550-850 ℃ of temperature.
7. the microwave preparation of the LiFePO4 that carbon as claimed in claim 1 coats is characterized in that, the addition of described microwave absorption is the 5-30% of the LiFePO4 weight of the carbon coating of generation.
8. the microwave preparation of the LiFePO4 that carbon as claimed in claim 1 coats is characterized in that, the addition of described organic carbon source is the 5-30% of the LiFePO4 weight of the carbon coating of generation.
9. the microwave preparation of the LiFePO4 that carbon as claimed in claim 1 coats is characterized in that described Li source compound, ferrous iron source compound and P source compound are according to Li: Fe
2+: P=(0.95～1.20): 1: 1 mol ratio takes by weighing respectively.
10. the LiFePO 4 material that coats of a carbon is characterized in that, comprises the LiFePO4 that carbon that the microwave preparation of the LiFePO4 that coats according to each described carbon of claim 1 to 9 makes coats.
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Cited By (8)
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| CN102130328A (en) * | 2011-01-27 | 2011-07-20 | 东莞市迈科科技有限公司 | Preparation method of vanadium lithium phosphate/carbon superfine powder positive pole material |
| CN102674273A (en) * | 2012-03-23 | 2012-09-19 | 湖南阳东微波科技有限公司 | Device for continuously producing lithium iron phosphate by microwave heating method |
| CN103594711A (en) * | 2012-08-15 | 2014-02-19 | 深圳市天骄科技开发有限公司 | Preparation method of lithium iron phosphate material by low-thermal solid-phase microwave method |
| CN104681784A (en) * | 2015-02-10 | 2015-06-03 | 华中科技大学 | Lithium vanadate anode material, anode, battery and anode material preparation method |
| CN105722791A (en) * | 2013-11-15 | 2016-06-29 | 住友金属矿山株式会社 | Method for producing surface-treated oxide particles, and oxide particles produced by said production method |
| CN106340648A (en) * | 2016-10-19 | 2017-01-18 | 江苏海四达电源股份有限公司 | LiFePO4/C cathode material and preparation method thereof |
| CN106558699A (en) * | 2015-09-30 | 2017-04-05 | 住友大阪水泥股份有限公司 | Electrode for lithium ion secondary battery material, its manufacture method, electrode for lithium ion secondary battery and lithium rechargeable battery |
| CN111081997A (en) * | 2019-11-25 | 2020-04-28 | 德阳威旭锂电科技有限责任公司 | Preparation method of composite carbon source coated nano phosphoric acid lithium ion positive electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102130328A (en) * | 2011-01-27 | 2011-07-20 | 东莞市迈科科技有限公司 | Preparation method of vanadium lithium phosphate/carbon superfine powder positive pole material |
| CN102674273A (en) * | 2012-03-23 | 2012-09-19 | 湖南阳东微波科技有限公司 | Device for continuously producing lithium iron phosphate by microwave heating method |
| CN103594711A (en) * | 2012-08-15 | 2014-02-19 | 深圳市天骄科技开发有限公司 | Preparation method of lithium iron phosphate material by low-thermal solid-phase microwave method |
| CN105722791A (en) * | 2013-11-15 | 2016-06-29 | 住友金属矿山株式会社 | Method for producing surface-treated oxide particles, and oxide particles produced by said production method |
| CN105722791B (en) * | 2013-11-15 | 2018-01-26 | 住友金属矿山株式会社 | The manufacture method of surface treated oxide particle and the oxide particle obtained by this method |
| CN104681784A (en) * | 2015-02-10 | 2015-06-03 | 华中科技大学 | Lithium vanadate anode material, anode, battery and anode material preparation method |
| CN106558699A (en) * | 2015-09-30 | 2017-04-05 | 住友大阪水泥股份有限公司 | Electrode for lithium ion secondary battery material, its manufacture method, electrode for lithium ion secondary battery and lithium rechargeable battery |
| CN106558699B (en) * | 2015-09-30 | 2021-07-20 | 住友大阪水泥股份有限公司 | Electrode material for lithium ion secondary battery, method for producing same, electrode for lithium ion secondary battery, and lithium ion secondary battery |
| CN106340648A (en) * | 2016-10-19 | 2017-01-18 | 江苏海四达电源股份有限公司 | LiFePO4/C cathode material and preparation method thereof |
| CN111081997A (en) * | 2019-11-25 | 2020-04-28 | 德阳威旭锂电科技有限责任公司 | Preparation method of composite carbon source coated nano phosphoric acid lithium ion positive electrode material |
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Application publication date: 20100526 |