CN108682854A - Carbon coating LiFe1-xCoxPO4Anode material for lithium-ion batteries and preparation method - Google Patents
Carbon coating LiFe1-xCoxPO4Anode material for lithium-ion batteries and preparation method Download PDFInfo
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- CN108682854A CN108682854A CN201810494304.6A CN201810494304A CN108682854A CN 108682854 A CN108682854 A CN 108682854A CN 201810494304 A CN201810494304 A CN 201810494304A CN 108682854 A CN108682854 A CN 108682854A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of carbon coating LiFe1‑xCoxPO4Anode material for lithium-ion batteries and preparation method utilize soluble trivalent iron salt, acetylene black, soluble ammonium salt, according to molar concentration rate meter, soluble trivalent iron salt：Acetylene black：Soluble ammonium salt is 0.9:0.21:0.7‑1：1：1, by obtaining FePO after coprecipitation reaction4·2H2O C presomas, pass through FePO4·2H2O C presomas and lithium salts, cobalt salt and sucrose pyroreaction, obtain carbon coating LiFe1‑xCoxPO4Composite material, by means of the above-mentioned technical proposal of the present invention, the carbon coating LiFe of preparation1‑xCoxPO4Positive electrode and pure phase LiFePO4It compares, there is more excellent chemical property；The method of the present invention preparation process is simple simultaneously, and easy to operate, cost of material is low, it is easy to accomplish scale industrial production.
Description
Technical field
The present invention relates to lithium ion battery electrode material preparing technical fields, it particularly relates to a kind of solid by high temperature
Phase method prepares carbon coating LiFe1-xCoxPO4The method of positive electrode,.
Background technology
Lithium ion battery LiFePO4With LiCoO2、LiNiO2、LiMn2O4Equal positive electrodes are compared, high with discharge capacity,
The advantages that platform stable, safety be good, of low cost, service life is long and non-environmental-pollution, is a kind of very potential
Positive electrode.But due to body phase LiFePO4The conductive capability of material is poor, and charge/discharge capacity needs to be further increased.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Invention content
The purpose of the present invention is to provide a kind of carbon coating LiFe1-xCoxPO4The preparation method of positive electrode, is easy to scale
Metaplasia is produced.
To realize the above-mentioned technical purpose, the technical proposal of the invention is realized in this way：
A kind of carbon coating LiFe1-xCoxPO4The preparation method of anode material for lithium-ion batteries, includes the following steps：
S1. presoma is prepared：Weigh following raw material：Soluble trivalent iron salt, acetylene black, soluble ammonium salt, wherein according to rubbing
That concentration ratio meter, soluble trivalent iron salt：Acetylene black：Soluble ammonium salt is 0.9:0.21:0.7-1：1：1, it is anti-by being co-precipitated
Should after obtain solid product, solid product is then washed with deionized, until filtrate pH value be 7~8, by being dried to obtain
FePO4·2H2O-C presomas；
S2. following material is weighed：FePO prepared by step S14·2H2O-C presomas, lithium salts, cobalt salt, sucrose, wherein according to
Molar concentration rate meter, FePO4·2H2O-C presomas：Lithium salts：Cobalt salt is 19:26.1:25-1:1:1, according to mass percent meter,
It weighs sucrose and accounts for FePO4·2H2The 7-10% of O-C presomas, lithium salts and cobalt salt gross mass；
S3. by all raw material ground and mixeds in step S2；
S4. the raw material after step S3 ground and mixeds is calcined under an inert atmosphere, calcination temperature is 500~800oC, when heat preservation
Between be 1~20h；
S5. it cools to room temperature with the furnace, obtains carbon coating LiFe1-xCoxPO4Composite material, wherein, 0<x<1.
Further, coprecipitation reaction described in step S1 the specific steps are：By soluble trivalent iron salt and oxidation acetylene
It is added in deionized water, is sufficiently stirred to obtain solution A；Soluble ammonium salt is dissolved in deionized water, is sufficiently stirred and dissolves to obtain solution
B, acquired solution B is added dropwise into solution A, is continued to stir after completion of dropwise addition, is obtained solid product.
Further, solution B rate of addition is often to drip for 2-5 seconds.
Further, drying condition described in step S1 is：Drying temperature 100~200oC, 6~12 hours drying times.
Further, it is 1-10 that heating rate is calcined described in step S4oC/ minutes.
Further, soluble trivalent iron salt described in the step S1 selects Fe (NO3)3Or FePO4, described in step S1
Soluble ammonium salt selects (NH4)2HPO4Or (NH4)3PO4。
Further, cobalt salt described in step S2 selects CoC4H6O4Or CoC2O4, the selection of lithium salts described in step S2
LiH2PO4Or LiOH.
Further, inert atmosphere described in step S4 is N2Or Ar.
A kind of carbon coating LiFe1-xCoxPO4Anode material for lithium-ion batteries comprising carbon coating LiFe1-xCoxPO4It is compound
Material, the carbon coating LiFe1-xCoxPO4Composite material is by with FePO4·2H2O-C is presoma, with lithium salts, cobalt salt and
The synthesis of sucrose pyroreaction is made.
Further, the FePO4·2H2O-C presomas are by soluble trivalent iron salt, acetylene black, soluble ammonium salt system
At, wherein according to molar concentration rate meter, soluble trivalent iron salt：Acetylene black：Soluble ammonium salt is 0.9:0.21:0.7-1：1：
1。
Beneficial effects of the present invention：By means of the above-mentioned technical proposal of the present invention, the carbon coating LiFe of preparation1-xCoxPO4Just
Pole material and pure phase LiFePO4It compares, there is more excellent chemical property；The method of the present invention preparation process is simple simultaneously,
Easy to operate, cost of material is low, it is easy to accomplish scale industrial production.
Description of the drawings
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the present invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is 1 gained LiFe of embodiment1-xCoxPO4The SEM electron microscopes of sample；
Fig. 2 is 2 gained LiFe of embodiment1-xCoxPO4Sample XRD spectra；
Fig. 3 is 3 gained LiFe of embodiment1-xCoxPO4Voltage-capacity curve under sample 2.5-4.5V potential ranges；
Fig. 4 is 4 gained LiFe of embodiment1-xCoxPO4Electrochemistry cycle performance curve under sample 0.3C.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained belong to what the present invention protected
Range.
Embodiment 1：
1）According to molar concentration rate Fe (NO3)3：(NH4)2HPO4It is 0.5, (NH4)2HPO4：Acetylene black weighs Fe (NO for 0.73)3、
(NH4)2HPO4, acetylene black, by Fe (NO3)3It is added in deionized water with oxidation acetylene, is sufficiently stirred to obtain solution A；By (NH4)2HPO4It is dissolved in deionized water, stirring and dissolving obtains solution B, and acquired solution B is added dropwise into solution A, and solution B rate of addition is 2 seconds
It often drips, continues to stir after completion of dropwise addition, reaction product is then washed with deionized, until filtrate pH value is 7, then 100oUnder C
It is 12 hours dry, obtain FePO4·2H2O-C presomas.
2）According to molar concentration rate FePO4·2H2O-C presomas：LiOH is 0.9, FePO4·2H2O-C presomas：
CoC4H6O4It is 20, weighs presoma, LiOH, CoC4H6O4, according to mass percent meter, weigh sucrose and account for FePO4·2H2Before O-C
Drive body, LiOH and CoC4H6O4The above raw material are fully ground mixing, are transferred in quartz boat, are placed in tubular type by the 7% of gross mass
In heating furnace, under nitrogen atmosphere cycle, 5oC/ minutes rates are warming up to 800oC keeps the temperature 15h, after reaction, with stove
It is cooled to room temperature and both obtains carbon coating LiFe0.65Co0.35PO4Composite material.
As shown in Figure 1, SEM observes LiFe1-xCoxPO4Surface is coated with carbon-coating, and uniform point of product grain size
It dissipates.
Embodiment 2：
1）According to molar concentration rate FePO4：(NH4)3PO4It is 0.6, (NH4)3PO4：Acetylene black weighs FePO for 0.74、(NH4)3PO4, acetylene black, by FePO4It is added in deionized water with oxidation acetylene, is sufficiently stirred to obtain solution A；By (NH4)3PO4Be dissolved in from
In sub- water, stirring and dissolving obtains solution B, and acquired solution B is added dropwise into solution A, and solution B rate of addition is often to drip for 5 seconds, completion of dropwise addition
After continue to stir, reaction product is then washed with deionized, until filtrate pH value is 8, then 130oIt is 8 hours dry under C, it obtains
To FePO4·2H2O-C presomas.
2）According to molar concentration rate FePO4·2H2O-C presomas：LiH2PO4It is 0.8, FePO4·2H2O-C presomas：
CoC2O4It is 19, weighs presoma, LiH2PO4、CoC2O4, according to mass percent meter, weigh sucrose and account for FePO4·2H2Before O-C
Drive body, LiH2PO4And CoC2O4The above raw material are fully ground mixing, are transferred in quartz boat, are placed in pipe by the 10% of gross mass
In formula heating furnace, under argon gas atmosphere cycle, 1oC/ minutes rates are warming up to 650oC keeps the temperature 10h, after reaction, with
Stove, which is cooled to room temperature, both obtains carbon coating LiFe0.95Co0.05PO4Composite material.
As shown in Fig. 2, obtaining XRD diagram by x-ray diffraction experiment, analysis obtains, carbon coating LiFe0.95Co0.05PO4It is multiple
Condensation material and LiFePO4It compares, carbon coating LiFe0.95Co0.05PO4Metallic element Co is adulterated in composite material.
Embodiment 3：
1）According to molar concentration rate FePO4：(NH4)3PO4It is 0.5, (NH4)3PO4：Acetylene black weighs FePO for 0.554、(NH4)3PO4, acetylene black, by FePO4It is added in deionized water with oxidation acetylene, is sufficiently stirred to obtain solution A；By (NH4)3PO4Be dissolved in from
In sub- water, stirring and dissolving obtains solution B, and acquired solution B is added dropwise into solution A, and solution B rate of addition is often to drip for 3 seconds, completion of dropwise addition
After continue to stir, reaction product is then washed with deionized, until filtrate pH value is 8, then 150oIt is 6 hours dry under C, it obtains
To FePO4·2H2O-C presomas.
2）According to molar concentration rate FePO4·2H2O-C presomas：LiH2PO4It is 0.9, FePO4·2H2O-C presomas：
CoC2O4It is 19, weighs presoma, LiH2PO4、CoC2O4, according to mass percent meter, weigh sucrose and account for FePO4·2H2Before O-C
Drive body, LiH2PO4And CoC2O4The above raw material are fully ground mixing, are transferred in quartz boat, are placed in pipe by the 8% of gross mass
In formula heating furnace, under argon gas atmosphere cycle, 3oC/ minutes rates are warming up to 750oC keeps the temperature 15h, after reaction, with
Stove, which is cooled to room temperature, both obtains carbon coating LiFe0.90Co0.10PO4Composite material.
As shown in figure 3, for the voltage-capacity measurement result curve under 2.5-4.5V potential ranges, voltage-capacity measures knot
Fruit curve shows the charge-discharge performance, it can be achieved that high power capacity.
Embodiment 4：
1）According to molar concentration rate FePO4：(NH4)3PO4It is 0.4, (NH4)3PO4：Acetylene black weighs FePO for 0.64、(NH4)3PO4, acetylene black, by FePO4It is added in deionized water with oxidation acetylene, is sufficiently stirred to obtain solution A；By (NH4)3PO4Be dissolved in from
In sub- water, stirring and dissolving obtains solution B, and acquired solution B is added dropwise into solution A, and solution B rate of addition is often to drip for 4 seconds, completion of dropwise addition
After continue to stir, reaction product is then washed with deionized, until filtrate pH value is 8, then 200oIt is 7 hours dry under C, it obtains
To FePO4·2H2O-C presomas.
2）According to molar concentration rate FePO4·2H2O-C presomas：LiH2PO4It is 0.95, FePO4·2H2O-C presomas：
CoC2O4It is 23, weighs presoma, LiH2PO4、CoC2O4, according to mass percent meter, weigh sucrose and account for FePO4·2H2Before O-C
Drive body, LiH2PO4And CoC2O4The above raw material are fully ground mixing, are transferred in quartz boat, are placed in pipe by the 7% of gross mass
In formula heating furnace, under argon gas atmosphere cycle, 10oC/ minutes rates are warming up to 700oC keeps the temperature 15h, after reaction, with
Stove, which is cooled to room temperature, both obtains carbon coating LiFe0.5Co0.5PO4Composite material.
Fig. 4 is the electrochemistry cycle performance carried out as a result, result shows that cycle performance is good.
Experiment is measured by SEM electron microscopes, XRD diagram, electrochemistry the cycle performance experiment of embodiment 1-4 and voltage-capacity
The result shows that LiFe1-xCoxPO4Surface coated with conductive carbonizable substance reduces intergranular contact resistance or conduction resistance, improves electricity
Conductance, LiFe1-xCoxPO4Metallic element Co is adulterated in lattice, makes occur free electron or hole in lattice, to improve
The carrier quantity and rate travel of material internal, and then improve the intrinsic conductivity of material, the Co ionic compartmentation iron of doping
Either the chemical property of material is improved in lithium position by improving conductivity or lithium ionic mobility for position.
In conclusion by means of the above-mentioned technical proposal of the present invention, the carbon coating LiFe1-xCoxPO of preparation4Positive electrode
With pure phase LiFePO4It compares, there is more excellent chemical property；The method of the present invention preparation process is simple simultaneously, operation side
Just, cost of material is low, it is easy to accomplish scale industrial production.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of carbon coating LiFe1-xCoxPO4The preparation method of anode material for lithium-ion batteries, which is characterized in that including following step
Suddenly：
S1. presoma is prepared：Weigh following raw material：Soluble trivalent iron salt, acetylene black, soluble ammonium salt, wherein according to rubbing
That concentration ratio meter, soluble trivalent iron salt：Acetylene black：Soluble ammonium salt is 0.9:0.21:0.7-1：1：1, it is anti-by being co-precipitated
Should after obtain solid product, solid product is then washed with deionized, until filtrate pH value be 7~8, by being dried to obtain
FePO4·2H2O-C presomas；
S2. following material is weighed：FePO prepared by step S14·2H2O-C presomas, lithium salts, cobalt salt, sucrose, wherein according to
Molar concentration rate meter, FePO4·2H2O-C presomas：Lithium salts：Cobalt salt is 19:26.1:25-1:1:1, according to mass percent meter,
It weighs sucrose and accounts for FePO4·2H2The 7-10% of O-C presomas, lithium salts and cobalt salt gross mass；
S3. by all raw material ground and mixeds in step S2；
S4. the raw material after step S3 ground and mixeds is calcined under an inert atmosphere, calcination temperature is 500~800oC, soaking time
For 1~20h；
S5. it cools to room temperature with the furnace, obtains carbon coating LiFe1-xCoxPO4Composite material, wherein 0<x<1.
2. carbon coating LiFe according to claim 11-xCoxPO4The preparation method of anode material for lithium-ion batteries, feature
Be, coprecipitation reaction described in step S1 the specific steps are：Deionized water is added in soluble trivalent iron salt and oxidation acetylene
In, it is sufficiently stirred to obtain solution A；Soluble ammonium salt is dissolved in deionized water, is sufficiently stirred and dissolves to obtain solution B, by acquired solution B
It is added dropwise into solution A, continues to stir after completion of dropwise addition, obtain solid product.
3. carbon coating LiFe according to claim 21-xCoxPO4The preparation method of anode material for lithium-ion batteries, feature
It is, solution B rate of addition is often to drip for 2-5 seconds.
4. carbon coating LiFe according to claim 11-xCoxPO4The preparation method of anode material for lithium-ion batteries, feature
It is, drying condition is described in step S1：Drying temperature 100~200oC, 6~12 hours drying times.
5. carbon coating LiFe according to claim 11-xCoxPO4The preparation method of anode material for lithium-ion batteries, feature
It is, it is 1-10 that heating rate is calcined described in step S4oC/ minutes.
6. carbon coating LiFe according to claim 11-xCoxPO4The preparation method of anode material for lithium-ion batteries, feature
It is, soluble trivalent iron salt described in the step S1 selects Fe (NO3)3Or FePO4, soluble ammonium salt choosing described in step S1
With (NH4)2HPO4Or (NH4)3PO4。
7. carbon coating LiFe according to claim 11-xCoxPO4The preparation method of anode material for lithium-ion batteries, feature
It is, cobalt salt described in step S2 selects CoC4H6O4Or CoC2O4, the selection of lithium salts described in step S2 LiH2PO4Or LiOH.
8. carbon coating LiFe according to claim 11-xCoxPO4The preparation method of anode material for lithium-ion batteries, feature
It is, inert atmosphere described in step S4 is N2Or Ar.
9. a kind of carbon coating LiFe1-xCoxPO4Anode material for lithium-ion batteries, which is characterized in that it includes carbon coating LiFe1- xCoxPO4Composite material, the carbon coating LiFe1-xCoxPO4Composite material is by with FePO4·2H2O-C is presoma, with
Lithium salts, cobalt salt and the synthesis of sucrose pyroreaction are made.
10. carbon coating LiFe according to claim 91-xCoxPO4Anode material for lithium-ion batteries, which is characterized in that described
FePO4·2H2O-C presomas are made of soluble trivalent iron salt, acetylene black, soluble ammonium salt, wherein according to molar concentration rate
Meter, soluble trivalent iron salt：Acetylene black：Soluble ammonium salt is 0.9:0.21:0.7-1：1：1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109638282A (en) * | 2018-12-19 | 2019-04-16 | 中科廊坊过程工程研究院 | A kind of cladded type lithium iron phosphate positive material and its preparation method and application |
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| CN102422467A (en) * | 2009-05-04 | 2012-04-18 | 觅科科技公司 | Electrode active composite materials and methods of making thereof |
| CN103247804A (en) * | 2013-04-27 | 2013-08-14 | 湖南大学 | Preparation method of nanocarbon coated lithium iron phosphate |
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2018
- 2018-05-22 CN CN201810494304.6A patent/CN108682854A/en active Pending
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| CN101519199A (en) * | 2009-03-19 | 2009-09-02 | 金川集团有限公司 | Method for preparing high-density spherical lithium iron phosphate for lithium ion power battery |
| CN102422467A (en) * | 2009-05-04 | 2012-04-18 | 觅科科技公司 | Electrode active composite materials and methods of making thereof |
| CN103247804A (en) * | 2013-04-27 | 2013-08-14 | 湖南大学 | Preparation method of nanocarbon coated lithium iron phosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109638282A (en) * | 2018-12-19 | 2019-04-16 | 中科廊坊过程工程研究院 | A kind of cladded type lithium iron phosphate positive material and its preparation method and application |
| CN109638282B (en) * | 2018-12-19 | 2021-08-06 | 中科廊坊过程工程研究院 | Coated lithium iron phosphate cathode material and preparation method and application thereof |
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Application publication date: 20181019 |