CN106450298A - Preparation method of lithium iron phosphate-lithium vanadium phosphate flaky composite cathode material - Google Patents
Preparation method of lithium iron phosphate-lithium vanadium phosphate flaky composite cathode material Download PDFInfo
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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
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- 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
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Abstract
The invention discloses a preparation method of a lithium iron phosphate-lithium vanadium phosphate flaky composite cathode material. The preparation method comprises the following steps that 1, a vanadium source, an iron source, a phosphorus source, a lithium source and an organic carbon source are dissolved into deionized water according to the molar ratio 2:1:4:4:(3-5) of vanadium atoms to iron atoms to phosphorus atoms to lithium atoms to carbon atoms, a surfactant is added, the pH value is regulated, and stirring is conducted; 2, the mixture is transferred into a high-pressure reaction kettle, protective gas is introduced, reacting is conducted for 10 h to 30 h at the speed of 200 rpm to 1,200 rpm at the temperature of 200 DEG C to 300 DEG C, and after washing, filtering and drying are conducted, grinding is conducted; 3, roasting is conducted in a non-oxidative atmosphere at the temperature of 600 DEG C to 800 DEG C, and then the material is obtained. The lithium iron phosphate-lithium vanadium phosphate flaky composite cathode material synthesized through the method has the excellent electronic conductivity and ionic conductivity and is excellent in electrochemical performance, good and stable in product homogeneity and low in cost.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery anode material lithium iron phosphate-phosphoric acid vanadium lithium and in particular to
A kind of preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium.
Background technology
The electric conductivity of LiFePO4 is very poor, and in heavy-current discharge, capacity attenuation is fast, and cryogenic property and high rate performance are poor；Phosphorus
In sour its crystal structure of vanadium lithium, metal ion relatively far apart, reduces the mobility of electronics in material, leads to the electronics of material to be led
Electric rate is relatively low, carries out that charge and discharge effect is undesirable under high current, and two kinds of traditional phosphate-based positive electrodes are combined together
Prepare, put using the high ion conductivity of phosphoric acid vanadium lithium, high theoretical specific capacity, high discharge voltage plateau, good low temperature
The advantages such as electrical property LiFePO4 sill is modified, and are a kind of effective methods.
But, the high rate charge-discharge performance how improving composite further is so as to fully meet electrokinetic cell
Use requirement, is current problem demanding prompt solution.
Content of the invention
The technical problem to be solved is to overcome prior art not enough, provide a kind of lamellar composite positive pole
The preparation method of LiFePO4-phosphoric acid vanadium lithium, the lamellar composite positive pole LiFePO4 obtained by the method-phosphoric acid vanadium lithium electricity
Preferably, big multiplying power discharging property is excellent for chemical property.
The technical solution adopted for the present invention to solve the technical problems is：Lamellar composite positive pole LiFePO4-phosphoric acid
The preparation method of vanadium lithium, comprises the following steps：
（1）By vanadium source, source of iron, phosphorus source, lithium source, organic carbon source, rub by vanadium atom, iron atom, phosphorus atoms, lithium atom, carbon atom
That ratio is 2:1:4:4:3～5（Preferably 3.5～4.5）Ratio be dissolved in deionized water, then by theoretical gained LiFePO4-phosphorus
1～5% addition surfactant of sour vanadium lithium quality, controls vanadium ion concentration in solution to be 0.05～0.1mol/L（Preferably 0.06
～0.09mol/L）, adjusting pH value with ammonia is 2～8（Preferably 5～7）, stirring（Preferably 5～20h, more preferably 10～12h）, obtain
To transparent and homogeneous solution；
（2）By step（1）The transparent and homogeneous solution of gained is transferred in autoclave, is passed through protective gas, with 200～
1200rpm（Preferably 800～1000rpm）Speed, 200～300 DEG C（Preferably 240～260 DEG C）Temperature, react 10～30h
（Preferably 15～25h）, scrubbed, filter, be dried, grind, obtain LiFePO4-phosphoric acid vanadium lithium composite material precursor powder；
（3）By step（2）The precursor powder of gained, in 600～800 DEG C under non-oxidizing atmosphere（Preferably 700～780 DEG C）
Roasting 10～20h（Preferably 15～18h）, obtain LiFePO4-phosphoric acid vanadium lithium composite positive pole.
Further, step（1）In, described vanadium source is vanadic anhydride, sodium vanadate, ammonium metavanadate, Vanadium sesquioxide, vanadium
One or more of sour ammonium, vanadic acid sodium, vanadyl oxalate.
Further, step（1）In, described source of iron is ferroso-ferric oxide, iron sesquioxide, ferrous chloride, ferric nitrate, oxalic acid
One or more of ferrous iron, Ferrous ammonium sulfate.
Further, step（1）In, phosphorus source is monoammonium phosphate, ammonium dihydrogen phosphate, ammonium phosphate, lithium phosphate, di(2-ethylhexyl)phosphate
One or more of hydrogen lithium, tertiary sodium phosphate, triethyl phosphate, tributyl phosphate, phosphate ester.
Further, step（1）In, described lithium source be lithium oxalate, lithium dihydrogen phosphate, Lithium hydrate, lithium acetate, lithium carbonate,
One or more of lithium phosphate, lithium chloride, lithium nitrate.
Further, step（1）In, described organic carbon source is sucrose, shitosan, lactic acid, glucose, malic acid, acetic acid, phenol
One or more of urea formaldehyde, acrylic resin, epoxy resin, oxalic acid, citric acid.
Further, step（1）In, described surfactant be dioctyl sodium sulfosuccinate, sodium lauryl sulphate, ten
One or more of six alkyl trimethyl ammonium bromides, octyl phenyl polyvinylether, Macrogol 4000, sorbester p17.
Further, step（2）In, described protective atmosphere is one or more of argon, nitrogen, helium.
Further, step（3）In, described non-oxidizing atmosphere is argon, nitrogen, hydrogen, carbon dioxide, in carbon monoxide
One or more.
The present invention utilizes hydro-thermal method synthesizing iron lithium phosphate-phosphoric acid vanadium lithium presoma, then recycles solid-phase sintering to material
Carry out material with carbon-coated surface, ultimately form the LiFePO4-phosphoric acid vanadium lithium composite positive pole with stereochemical structure.The product being obtained
Product have laminated structure, have well-bedded gap between piece and piece, and this is conducive to the infiltration of electrolyte, and lithium ion
Diffusion transport；Flaky material surface also covers one layer of carbon net, becomes to have the structure of stereo structure with regard to framework between this print and piece,
This is conducive to the transmission of electronics between material.This structure is conducive to improving the electron conduction of composite positive pole and ion is led
Electrically.
The lamellar ion composite positive pole LiFePO4-phosphoric acid vanadium lithium of present invention synthesis has excellent electron conduction
And ionic conductivity, high rate performance is greatly improved.
Brief description
Fig. 1 is the SEM figure of the product obtained by embodiment 1；
Fig. 2 is the XRD spectrum of the product obtained by embodiment 1；
First charge-discharge curve chart under the conditions of Fig. 3 0.1C, 1C, 10C of product obtained by embodiment 1.
Specific embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1
Weigh ammonium metavanadate 9.36g respectively（0.08mol）, iron sesquioxide 3.19g（0.02mol）, ammonium dihydrogen phosphate 18.40g
（0.16mol）, lithium carbonate 5.91g（0.08mol）, oxalic acid 7.20g（0.08mol）, former by vanadium atom, iron atom, phosphorus atoms, lithium
Son, carbon atom mol ratio are 2:1:4:4:4 are dissolved in 1L ionized water, then by theoretical gained LiFePO4-phosphoric acid vanadium lithium quality
3% addition surfactant cetyl trimethylammonium bromide 0.678g, control solution in vanadium ion concentration be 0.08mol/L,
Adjusting pH value with ammonia is 6, uses magnetic stirrer 11h, obtains transparent and homogeneous solution；By obtained transparent and homogeneous solution
Be transferred in autoclave, be passed through argon, with the speed of 900rpm, 250 DEG C of temperature, react 20h, scrubbed, filter, dry
After dry, grind, obtain LiFePO4-phosphoric acid vanadium lithium composite material precursor powder；By the precursor powder of gained, non-oxide
In 750 DEG C of roasting 16h under property atmosphere, obtain LiFePO4-phosphoric acid vanadium lithium composite positive pole.
Understand as shown in Figure 1, LiFePO4-phosphoric acid vanadium lithium composite positive pole is lamellar.Understand as shown in Figure 2, phosphoric acid
Ferrum lithium-phosphoric acid vanadium lithium composite positive pole is complete crystalline structure.
The assembling of battery：Weigh the LiFePO4-phosphoric acid vanadium lithium of 0.4g gained, add 0.05g acetylene black make conductive agent and
0.05g NMP（N-Methyl pyrrolidone）Make binding agent, be coated in after mix homogeneously on aluminium foil and make positive plate, in vacuum glove box
In with metal lithium sheet as negative pole, with Celgard 2300 as barrier film, 1mol/L LiPF6/EC∶DMC（Volume ratio 1: 1）For electrolysis
Liquid, can be assembled into the button cell of CR2025, and 0.1C first discharge specific capacity is 148.9mAh/g, and 1C first discharge specific capacity is
141.6mAh/g, 10C first discharge specific capacity is 125.8mAh/g.
Embodiment 2
Take vanadic anhydride 5.46g（0.03mol）, Ferrox. 4.32g（0.03mol）, lithium dihydrogen phosphate 12.47g
（0.12mol）, citric acid 3.36g（0.01075mol）, by vanadium atom, iron atom, phosphorus atoms, lithium atom, carbon atom mol ratio
For 2:1:4:4:3.5 are dissolved in 1L ionized water, then live by 1% addition surface of theoretical gained LiFePO4-phosphoric acid vanadium lithium quality
Property agent poly- dioctyl sodium sulfosuccinate 0.170g, control solution in vanadium ion concentration be 0.06mol/L, adjust pH value with ammonia
For 5, use magnetic stirrer 10h, obtain uniform solution clear solution；Obtained transparent and homogeneous solution is transferred to high pressure
In reactor, it is passed through protective gas, with the speed of 800rpm, 240 DEG C of temperature, react 25h, scrubbed, filter, be dried
Afterwards, grind, obtain LiFePO4-phosphoric acid vanadium lithium composite material precursor powder；By the precursor powder of gained, non-oxidizable
In 700 DEG C of roasting 18h under atmosphere, obtain LiFePO4-phosphoric acid vanadium lithium composite positive pole.
The assembling of battery：Weigh the LiFePO4-phosphoric acid vanadium lithium of 0.4g gained, add 0.05g acetylene black make conductive agent and
0.05g NMP（N-Methyl pyrrolidone）Make binding agent, be coated in after mix homogeneously on aluminium foil and make positive plate, in vacuum glove box
In with metal lithium sheet as negative pole, with Celgard 2300 as barrier film, 1mol/L LiPF6/EC∶DMC（Volume ratio 1: 1）For electrolysis
Liquid, can be assembled into the button cell of CR2025, and 0.1C first discharge specific capacity is 138.9mAh/g, and 1C first discharge specific capacity is
130.6mAh/g, 10C first discharge specific capacity is 119.8mAh/g.
Embodiment 3
Weigh sodium vanadate 16.55g（0.09mol）, ferric nitrate 18.18g（0.045mol）, lithium dihydrogen phosphate 18.71g
（0.18mol）, sucrose 5.78g（0.017mol）, it is 2 by vanadium atom, iron atom, phosphorus atoms, lithium atom, carbon atom mol ratio:
1:4:4:4.5 are dissolved in deionized water, more pungent by 5% addition surfactant of theoretical gained LiFePO4-phosphoric acid vanadium lithium quality
Base phenyl polyvinylether 1.27g, controls vanadium ion concentration in solution to be 0.09mol/L, adjusting pH value with ammonia is 7, uses magnetic force
Agitator stirs 12h, obtains uniform solution clear solution；Obtained transparent and homogeneous solution is transferred in autoclave,
Be passed through protective gas, with the speed of 1000rpm, 260 DEG C of temperature, react 15h, scrubbed, filter, be dried after, grind, obtain
To LiFePO4-phosphoric acid vanadium lithium composite material precursor powder；By gained precursor powder, in 780 under non-oxidizing atmosphere
DEG C roasting 15h, obtains LiFePO4-phosphoric acid vanadium lithium composite positive pole.
The assembling of battery：Weigh the LiFePO4-phosphoric acid vanadium lithium of 0.4g gained, add 0.05g acetylene black make conductive agent and
0.05g NMP（N-Methyl pyrrolidone）Make binding agent, be coated in after mix homogeneously on aluminium foil and make positive plate, in vacuum glove box
In with metal lithium sheet as negative pole, with Celgard 2300 as barrier film, 1mol/L LiPF6/EC∶DMC（Volume ratio 1: 1）For electrolysis
Liquid, can be assembled into the button cell of CR2025, and 0.1C first discharge specific capacity is 135.9mAh/g, and 1C first discharge specific capacity is
128.6mAh/g, 10C first discharge specific capacity is 115.8mAh/g.
Claims (9)
1. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium is it is characterised in that comprise the following steps：
（1）By vanadium source, source of iron, phosphorus source, lithium source, organic carbon source, rub by vanadium atom, iron atom, phosphorus atoms, lithium atom, carbon atom
That ratio is 2:1:4:4:3～5 ratio is dissolved in deionized water, then by theoretical gained LiFePO4-phosphoric acid vanadium lithium quality 1～
5% addition surfactant, controls vanadium ion concentration in solution to be 0.05～0.1mol/L, adjusting pH value with ammonia is 2～8, stirs
Mix, obtain transparent and homogeneous solution；
（2）By step（1）The transparent and homogeneous solution of gained is transferred in autoclave, is passed through protective gas, with 200～
The speed of 1200rpm, 200～300 DEG C of temperature, react 10～30h, scrubbed, filter, be dried after, grind, obtain iron phosphate
Lithium-phosphoric acid vanadium lithium composite material precursor powder；
（3）By step（2）The precursor powder of gained, in 600～800 DEG C of roasting 10～20h under non-oxidizing atmosphere, obtains
LiFePO4-phosphoric acid vanadium lithium composite positive pole.
2. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium according to claim 1, its feature exists
In step（1）In, described vanadium source be vanadic anhydride, sodium vanadate, ammonium metavanadate, Vanadium sesquioxide, ammonium vanadate, vanadic acid sodium,
One or more of vanadyl oxalate.
3. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium according to claim 1 and 2, it is special
Levy and be, step（1）In, described source of iron is ferroso-ferric oxide, iron sesquioxide, ferrous chloride, ferric nitrate, Ferrox., sulfur
One or more of sour ferrous ammonium.
4. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium according to claim 1 and 2, it is special
Levy and be, step（1）In, phosphorus source is monoammonium phosphate, ammonium dihydrogen phosphate, ammonium phosphate, lithium phosphate, lithium dihydrogen phosphate, phosphorus
One or more of sour trisodium, triethyl phosphate, tributyl phosphate, phosphate ester.
5. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium according to claim 1 and 2, it is special
Levy and be, step（1）In, described lithium source is lithium oxalate, lithium dihydrogen phosphate, Lithium hydrate, lithium acetate, lithium carbonate, lithium phosphate, chlorine
Change one or more of lithium, lithium nitrate.
6. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium according to claim 1 and 2, it is special
Levy and be, step（1）In, described organic carbon source be sucrose, shitosan, lactic acid, glucose, malic acid, acetic acid, phenolic resin,
One or more of acrylic resin, epoxy resin, oxalic acid, citric acid.
7. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium according to claim 1 and 2, it is special
Levy and be, step（1）In, described surfactant is dioctyl sodium sulfosuccinate, sodium lauryl sulphate, cetyl three
One or more of methyl bromide ammonium, octyl phenyl polyvinylether, Macrogol 4000, sorbester p17.
8. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium according to claim 1 and 2, it is special
Levy and be, step（2）In, described protective atmosphere is one of argon, nitrogen, helium or several.
9. the preparation method of lamellar composite positive pole LiFePO4-phosphoric acid vanadium lithium according to claim 1 and 2, it is special
Levy and be, step（3）In, described non-oxidizing atmosphere is one of argon, nitrogen, hydrogen, carbon dioxide or carbon monoxide
Or it is several.
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Cited By (8)
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| CN110294466A (en) * | 2019-08-19 | 2019-10-01 | 四川轻化工大学 | A kind of preparation method of nano-sheet ferric phosphate |
| CN110416503A (en) * | 2019-07-01 | 2019-11-05 | 齐鲁工业大学 | A kind of soft carbon cladding titanium phosphate sodium mesoporous composite material and the preparation method and application thereof |
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| CN112216825A (en) * | 2020-08-31 | 2021-01-12 | 合肥国轩高科动力能源有限公司 | Preparation method of nitrogen-doped lithium vanadate/lithium iron phosphate composite material |
| CN113054176A (en) * | 2021-03-16 | 2021-06-29 | 河北九丛科技有限公司 | Phosphate ternary salt positive electrode material and synthetic method |
| CN113299889A (en) * | 2021-04-27 | 2021-08-24 | 合肥国轩电池材料有限公司 | Lithium battery positive electrode material and preparation method and application thereof |
| CN113582149A (en) * | 2021-05-31 | 2021-11-02 | 佛山市德方纳米科技有限公司 | Preparation method of flaky lithium iron phosphate material |
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|---|---|---|---|---|
| CN108199028A (en) * | 2018-01-10 | 2018-06-22 | 中南大学 | A kind of NaVPO4F/C composite materials and preparation method thereof |
| CN110416503A (en) * | 2019-07-01 | 2019-11-05 | 齐鲁工业大学 | A kind of soft carbon cladding titanium phosphate sodium mesoporous composite material and the preparation method and application thereof |
| CN110294466A (en) * | 2019-08-19 | 2019-10-01 | 四川轻化工大学 | A kind of preparation method of nano-sheet ferric phosphate |
| CN110294466B (en) * | 2019-08-19 | 2020-11-17 | 四川轻化工大学 | Preparation method of nano flaky iron phosphate |
| CN111422852A (en) * | 2020-04-18 | 2020-07-17 | 蒋央芳 | Preparation method of iron vanadium phosphate |
| CN112216825A (en) * | 2020-08-31 | 2021-01-12 | 合肥国轩高科动力能源有限公司 | Preparation method of nitrogen-doped lithium vanadate/lithium iron phosphate composite material |
| CN112216825B (en) * | 2020-08-31 | 2022-04-12 | 合肥国轩高科动力能源有限公司 | Preparation method of nitrogen-doped lithium vanadate/lithium iron phosphate composite material |
| CN113054176A (en) * | 2021-03-16 | 2021-06-29 | 河北九丛科技有限公司 | Phosphate ternary salt positive electrode material and synthetic method |
| CN113299889A (en) * | 2021-04-27 | 2021-08-24 | 合肥国轩电池材料有限公司 | Lithium battery positive electrode material and preparation method and application thereof |
| CN113582149A (en) * | 2021-05-31 | 2021-11-02 | 佛山市德方纳米科技有限公司 | Preparation method of flaky lithium iron phosphate material |
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