CN103579596A - Preparation method of lithium ion battery cathode material - Google Patents
Preparation method of lithium ion battery cathode material Download PDFInfo
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- CN103579596A CN103579596A CN201310556327.2A CN201310556327A CN103579596A CN 103579596 A CN103579596 A CN 103579596A CN 201310556327 A CN201310556327 A CN 201310556327A CN 103579596 A CN103579596 A CN 103579596A
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a lithium ion battery cathode material. The preparation method comprises the following steps: firstly carrying out acid washing on rice husks, then carrying out high-temperature pyrolysis on the rice husks after the acid washing to obtain solid products, fully mixing the obtained solid products and reducible metallic powder, carrying out high-temperature reducing reaction under the protection of inert gases to obtain products, and carrying out suction filtration drying after carrying out the acid washing on the products so as to obtain a porous silicon-carbon composite material which can be taken as the lithium ion battery cathode material. The used raw materials are widely in source and low in cost; the obtained porous silicon-carbon as the lithium battery cathode material has the advantages of large capacity density, high first charging and discharging coulomb efficiency, good cycle performance and the like.
Description
Technical field
The present invention relates to electrode material manufacturing process technology field, relate in particular to a kind of preparation method of lithium ion battery negative material.
Background technology
Compare with the secondary cell that plumbic acid, NI-G, ni-mh etc. are traditional, lithium ion battery has that operating voltage is high, volume is little, quality is light, capacity density is high, memory-less effect, pollution-free, and self discharge is little, the advantage such as have extended cycle life.Nineteen ninety, Japanese Sony company produces first lithium ion battery, has started the commercialization tide of lithium ion battery.
The negative material using in lithium ion battery is at present all material with carbon elements, comprises native graphite, Delanium and MCMB (MCMB) etc.These carbon negative poles have voltage stabilization in charge and discharge process, the advantages such as good cycle.But the theoretical capacity of graphite material is only 372mAh/g, be difficult to meet the people pursuit to lithium ion cell high-capacity, the especially electric automobile needs to high-performance lithium battery, an urgent demand exploitation has the negative material of high capacity density.Compare with material with carbon element, the theoretical capacity density of silicon can reach 4200mAh/g, as Novel anode material, has bright prospects.But in the embedding/de-embedding process of lithium, there is serious bulk effect in silicon, and material efflorescence is serious, causes capacity attenuation very fast, and cycle performance is poor.In recent years, researcher is that negative material has carried out study on the modification to silicon, comprises that nanometer, the carbon to silicon is coated and prepares silicon alloy etc., has improved to a certain extent the cycle performance of silicon based material.It is the precursor of negative material as silicon that the present invention selects rice husk, utilize its pyrolysis solid product and metal powder generation reduction reaction, formation has the silico-carbo composite material of loose structure, this porous material is as the negative pole of lithium ion battery, there is capacity density higher, first the advantage such as the high and good cycle of coulomb efficiency.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of lithium ion battery negative material.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: the preparation method of lithium ion battery negative material, comprises the following steps:
1) rice husk is carried out to pickling to remove alkali metal impurity wherein, being washed with water to subsequently pH is 6～7, dry;
2) to step 1) gained rice husk carries out pyrolysis, to decompose lignin and cellulose wherein, obtains pyrolysis solid product;
3) to step 2) dioxide-containing silica in thermal decomposition product detects, and according to its content, adds by a certain percentage reducing metal powder, mixes, and carries out high temperature reduction reaction under the protection of inert gas;
To step 3) gained reduzate first carries out pickling, and being then washed to pH is 6～8, and suction filtration is dry, obtains porous silicon-carbon composite.
As preferably, step 1) the pickling acid used in is HCl or HNO
3or HF or H
2sO
4, concentration is 10wt%～40wt%, pickling time is 2h～4h.
As preferably, step 1) washing in is deionized water washing.
As preferably, step 1) drying process in is 80 ℃～120 ℃ oven drying 24h～48h.
As preferably, step 2) condition of described pyrolysis is: pyrolysis protection gas is nitrogen or argon gas or helium, 500 ℃～650 ℃ of pyrolysis temperatures, and pyrolysis time is 3h～6h.
As preferably, step 3) method that detects silicone content in is elemental microanalysis method.
As preferably, step 3) in, the mol ratio of reducing metal powder and silicon dioxide is 1.5～2.5.
As preferably, step 3) in, reducing metal powder is magnesium powder or aluminium powder or glass putty or iron powder.
As preferably, step 3) in, inert gas is nitrogen or argon gas or helium.
As preferably, step 3) temperature of described high temperature reduction reaction is 800 ℃～900 ℃, and the reaction time is 3h～5h.
As preferably, step 4) pickling in is be first 20wt%～40wt% by concentration HCl or HNO
3or H
2sO
4washing, the rear HF solution washing with 20wt%～40wt% to pH be 6～8.
The invention has the beneficial effects as follows:
By rice husk is carried out to a series of processing and reaction, obtain having the silico-carbo composite material of loose structure.Its preparation technology is simple, easy to operate, and raw material sources are extensive, with low cost; The silico-carbo composite material obtaining can be used as the negative pole of lithium ion battery, has that capacity density is high, a feature such as good cycle and chemical property excellence, is conducive to the preparation of high performance lithium ion battery.
Embodiment
Below by embodiment, the present invention will be further described, but embodiment does not limit the scope of the invention.
Embodiment 1
1) rice husk is soaked in to 4h in the HCl solution of 10wt%, carries out pickling to remove alkali metal impurity wherein, then with deionized water washing, suction filtration 3 times, to pH be 6,80 ℃ of dry 48h;
2) to step 1) gained rice husk is under nitrogen protection, and 500 ℃ of pyrolysis 5h, to decompose lignin and cellulose wherein, obtain pyrolysis solid product;
3) elemental microanalysis method records step 2) molal quantity of silicon dioxide in thermal decomposition product, add metal magnesium powder, the mol ratio of magnesium powder and silicon dioxide is 2, mixes, and carries out the high temperature reduction reaction 4h of 800 ℃ under the protection of argon gas;
4) to step 3) gained reduzate first carries out the HCl solution washing of 30wt%, and then to pH, be 7 with the HF solution washing of 30wt%, finally, with deionized water washing, suction filtration 3 times, in 80 ℃ of baking ovens, dry 48h, obtains porous silicon-carbon composite.
5) using the porous silicon-carbon composite of preparation as lithium ion battery negative material, and it is carried out to charging and discharging capacity and cycle performance test: silico-carbo porous material and conductive agent, binding agent in mass ratio 8:1:1 are mixed and made into electrode slice as work electrode, lithium metal is as to electrode, electrolyte is that EC is molten with mixing of DEC, the volume ratio of the two is 1:1, LiFP
6as electrolyte lithium salt, concentration is 1mol/L, and barrier film used is PP (Celgard2400), in argon gas atmosphere glove box, assembles button cell, and make-up electricity carries out charge-discharge test, and voltage range is 0.01-1.0V (vs.Li
+/ Li), current density is 0.1C (1C:2000mA/g).
Test result: porous silicon-carbon negative pole material charging and discharging capacity under 0.1C is respectively 724mAh/g, 609mAh/g, coulomb efficiency is 84.2% first, circulate after 200 weeks, charge/discharge capacity is respectively 654mAh/g, 630mAh/g, coulomb efficiency is 96.3%, capacity attenuation is 9.6%, shows excellent cycle performance.
Embodiment 2
1) rice husk is soaked in to 3h in the HCl solution of 20wt%, carries out pickling to remove alkali metal impurity wherein, to pH be 7, then with deionized water washing, suction filtration 3 times, 100 ℃ of dry 36h;
2) to step 1) gained rice husk is under argon shield, and 550 ℃ of pyrolysis 3h, to decompose lignin and cellulose wherein, obtain pyrolysis solid product;
3) elemental microanalysis method records step 2) molal quantity of silicon dioxide in thermal decomposition product, add metallic aluminium powder, the mol ratio of aluminium powder and silicon dioxide is 1.5, mixes, and carries out the high temperature reduction reaction 3h of 850 ℃ under the protection of argon gas;
4) to step 3) gained reduzate first carries out the HCl solution washing of 20wt%, and then to pH, be 7 with the HF solution washing of 40wt%, finally, with deionized water washing, suction filtration 3 times, in 120 ℃ of baking ovens, dry 24h, obtains porous silicon-carbon composite.
5) using the porous silicon-carbon composite of preparation as lithium ion battery negative material, and it is carried out to charging and discharging capacity and cycle performance test: silico-carbo porous material and conductive agent, binding agent in mass ratio 8:1:1 is mixed and made into electrode slice as work electrode, lithium metal is as to electrode, electrolyte is the mixed solution of EC and DEC, the volume ratio of the two is 1:1, LiFP6 is as electrolyte lithium salt, concentration is 1mol/L, barrier film used is PP (Celgard2400), in argon gas atmosphere glove box, assemble button cell, and make-up electricity carries out charge-discharge test, voltage range is 0.01-1.0V (vs.Li
+/ Li), current density is 0.1C (1C:2000mA/g).
Test result: porous silicon-carbon negative pole material charging and discharging capacity under 0.1C is respectively 709mAh/g, 583mAh/g, coulomb efficiency is 82.3% first, circulate after 200 weeks, charge/discharge capacity is respectively 638mAh/g, 601mAh/g, coulomb efficiency is 94.2%, capacity attenuation is 10%, shows excellent cycle performance.
Embodiment 3
1) rice husk is soaked in to 2h in the HCl solution of 30wt%, carries out pickling to remove alkali metal impurity wherein, to pH be 7, then with deionized water washing, suction filtration 3 times, 120 ℃ of dry 24h;
2) to step 1) gained rice husk is under nitrogen protection, and 600 ℃ of pyrolysis 3h, to decompose lignin and cellulose wherein, obtain pyrolysis solid product;
3) elemental microanalysis method records step 2) molal quantity of silicon dioxide in thermal decomposition product, add metal iron powder, the mol ratio of iron powder and silicon dioxide is 1.5, mixes, and carries out the high temperature reduction reaction 3h of 850 ℃ under the protection of argon gas;
4) to step 3) gained reduzate first carries out the HCl solution washing of 30wt%, and then to pH, be 7 with the HF solution washing of 30wt%, finally, with deionized water washing, suction filtration 3 times, in 120 ℃ of baking ovens, dry 24h, obtains porous silicon-carbon composite.
5) using the porous silicon-carbon composite of preparation as lithium ion battery negative material, and it is carried out to charging and discharging capacity and cycle performance test: silico-carbo porous material and conductive agent, binding agent in mass ratio 8:1:1 are mixed and made into electrode slice as work electrode, lithium metal is as to electrode, electrolyte is the mixed solution of EC and DEC, the volume ratio of the two is 1:1, LiFP
6as electrolyte lithium salt, concentration is 1mol/L, and barrier film used is PP (Celgard2400), in argon gas atmosphere glove box, assembles button cell, and make-up electricity carries out charge-discharge test, and voltage range is 0.01-1.0V (vs.Li
+/ Li), current density is 0.1C (1C:2000mA/g).
Test result: porous silicon-carbon negative pole material charging and discharging capacity under 0.1C is respectively 715mAh/g, 608mAh/g, coulomb efficiency is 85.1% first, circulate after 200 weeks, charge/discharge capacity is respectively 648mAh/g, 615mAh/g, coulomb efficiency is 95%, capacity attenuation is 9.4%, shows excellent cycle performance.
Embodiment 4
1) rice husk is soaked in to 2h in the HCl solution of 40wt%, carries out pickling to remove alkali metal impurity wherein, to pH be 6, then with deionized water washing, suction filtration 3 times, 120 ℃ of dry 24h;
2) to step 1) gained rice husk is under nitrogen protection, and 650 ℃ of pyrolysis 3h, to decompose lignin and cellulose wherein, obtain pyrolysis solid product;
3) elemental microanalysis method records step 2) molal quantity of silicon dioxide in thermal decomposition product, add metallic tin powder, the mol ratio of glass putty and silicon dioxide is 2.5, mixes, and carries out the high temperature reduction reaction 3h of 850 ℃ under the protection of argon gas;
4) to step 3) gained reduzate first carries out the HCl solution washing of 20wt%, and then to pH, be 8 with the HF solution washing of 30wt%, finally, with deionized water washing, suction filtration 3 times, in 120 ℃ of baking ovens, dry 24h, obtains porous silicon-carbon composite.
5) using the porous silicon-carbon composite of preparation as lithium ion battery negative material, and it is carried out to charging and discharging capacity and cycle performance test: silico-carbo porous material and conductive agent, binding agent in mass ratio 8:1:1 are mixed and made into electrode slice as work electrode, lithium metal is as to electrode, electrolyte is the mixed solution of EC and DEC, the volume ratio of the two is 1:1, LiFP
6as electrolyte lithium salt, concentration is 1mol/L, and barrier film used is PP (Celgard2400), in argon gas atmosphere glove box, assembles button cell, and make-up electricity carries out charge-discharge test, and voltage range is 0.01-1.0V (vs.Li
+/ Li), current density is 0.1C (1C:2000mA/g).
Test result: porous silicon-carbon negative pole material charging and discharging capacity under 0.1C is respectively 698mAh/g, 591mAh/g, coulomb efficiency is 84.7% first, circulate after 200 weeks, charge/discharge capacity is respectively 614mAh/g, 590mAh/g, coulomb efficiency is 96.1%, capacity attenuation is 12%, shows excellent cycle performance.
Embodiment 5
1) rice husk is soaked in to 2h in the HCl solution of 30wt%, carries out pickling to remove alkali metal impurity wherein, to pH be 6, then with deionized water washing, suction filtration 3 times, 100 ℃ of dry 24h;
2) to step 1) gained rice husk is under argon shield, and 550 ℃ of pyrolysis 3h, to decompose lignin and cellulose wherein, obtain pyrolysis solid product;
3) elemental microanalysis method records step 2) molal quantity of silicon dioxide in thermal decomposition product, add metal magnesium powder, the mol ratio of magnesium powder and silicon dioxide is 2.5, mixes, and carries out the high temperature reduction reaction 3h of 800 ℃ under the protection of nitrogen;
4) to step 3) gained reduzate first carries out the HCl solution washing of 20wt%, and then to pH, be 7 with the HF solution washing of 20wt%, finally, with deionized water washing, suction filtration 3 times, in 120 ℃ of baking ovens, dry 24h, obtains porous silicon-carbon composite.
5) using the porous silicon-carbon composite of preparation as lithium ion battery negative material, and it is carried out to charging and discharging capacity and cycle performance test: silico-carbo porous material and conductive agent, binding agent in mass ratio 8:1:1 are mixed and made into electrode slice as work electrode, lithium metal is as to electrode, electrolyte is the mixed solution of EC and DEC, the volume ratio of the two is 1:1, LiFP
6as electrolyte lithium salt, concentration is 1mol/L, and barrier film used is PP (Celgard2400), in argon gas atmosphere glove box, assembles button cell, and make-up electricity carries out charge-discharge test, and voltage range is 0.01-1.0V (vs.Li
+/ Li), current density is 0.1C (1C:2000mA/g).
Test result: porous silicon-carbon negative pole material charging and discharging capacity under 0.1C is respectively 721mAh/g, 585mAh/g, coulomb efficiency is 81.2% first, circulate after 200 weeks, charge/discharge capacity is respectively 645mAh/g, 601mAh/g, coulomb efficiency approaches 93.2%, capacity attenuation is 10.5%, shows excellent cycle performance.
Embodiment 6
1) rice husk is soaked in to the H of 20wt%
2sO
43h in solution, carries out pickling to remove alkali metal impurity wherein, to pH be 7, then with deionized water washing, suction filtration 3 times, 80 ℃ of dry 48h;
2) to step 1) gained rice husk is under nitrogen protection, and 500 ℃ of pyrolysis 4h, to decompose lignin and cellulose wherein, obtain pyrolysis solid product;
3) elemental microanalysis method records step 2) molal quantity of silicon dioxide in thermal decomposition product, add metal magnesium powder, the mol ratio of magnesium powder and silicon dioxide is 2.2, mixes, and carries out the high temperature reduction reaction 3h of 850 ℃ under the protection of nitrogen;
4) to step 3) gained reduzate first carries out the H of 20wt%
2sO
4solution washing, and then to pH, be 8 with the HF solution washing of 20wt%, finally, with deionized water washing, suction filtration 3 times, in 80 ℃ of baking ovens, dry 48h, obtains porous silicon-carbon composite.
5) using the porous silicon-carbon composite of preparation as lithium ion battery negative material, and it is carried out to charging and discharging capacity and cycle performance test: silico-carbo porous material and conductive agent, binding agent in mass ratio 8:1:1 are mixed and made into electrode slice as work electrode, lithium metal is as to electrode, electrolyte is the mixed solution of EC and DEC, the volume ratio of the two is 1:1, LiFP
6as electrolyte lithium salt, concentration is 1mol/L, and barrier film used is PP (Celgard2400), in argon gas atmosphere glove box, assembles button cell, and make-up electricity carries out charge-discharge test, and voltage range is 0.01-1.0V (vs.Li
+/ Li), current density is 0.1C (1C:2000mA/g).
Test result: porous silicon-carbon negative pole material charging and discharging capacity under 0.1C is respectively 714mAh/g, 576mAh/g, coulomb efficiency is 80.7% first, circulate after 200 weeks, charge/discharge capacity is respectively 633mAh/g, 599mAh/g, coulomb efficiency is 94.6%, capacity attenuation is 11.3%, shows excellent cycle performance.
Above-described embodiment is only example character.For those skilled in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and sex change to these embodiment, scope of the present invention is claims and equivalent restriction thereof again.
Claims (10)
1. a preparation method for lithium ion battery negative material, is characterized in that comprising the following steps:
1) rice husk is carried out to pickling to remove alkali metal impurity wherein, being washed with water to subsequently pH is 6～7, dry;
2) to step 1) gained rice husk carries out pyrolysis, to decompose lignin and cellulose wherein, obtains pyrolysis solid product;
3) to step 2) dioxide-containing silica in thermal decomposition product detects, and according to its content, adds by a certain percentage reducing metal powder, mixes, and carries out high temperature reduction reaction under the protection of inert gas;
To step 3) gained reduzate first carries out pickling, and being then washed to pH is 6～8, and suction filtration is dry, obtains porous silicon-carbon composite.
2. method as claimed in claim 1, is characterized in that: step 1) in pickling acid used be HCl or HNO
3or HF or H
2sO
4, concentration is 10wt%～40wt%, and pickling time is 2h～4h, and washing is deionized water washing.
3. method as claimed in claim 1, is characterized in that: step 1) in drying process be 80 ℃～120 ℃ oven drying 24h～48h.
4. method as claimed in claim 1, is characterized in that: step 2) condition of described pyrolysis is: pyrolysis protection gas is nitrogen or argon gas or helium, 500 ℃～650 ℃ of pyrolysis temperatures, pyrolysis time is 3h～6h.
5. method as claimed in claim 1, is characterized in that: step 3) in detect silicone content method be elemental microanalysis method.
6. method as claimed in claim 1, is characterized in that: step 3) in the mol ratio of reducing metal powder and silicon dioxide be 1.5～2.5.
7. method as claimed in claim 1, is characterized in that: step 3) in reducing metal powder be magnesium powder or aluminium powder or glass putty or iron powder.
8. method as claimed in claim 1, is characterized in that: step 3) in inert gas be nitrogen or argon gas or helium.
9. method as claimed in claim 1, is characterized in that: step 3) temperature of described high temperature reduction reaction is 800 ℃～900 ℃, the reaction time is 3h～5h.
10. method as claimed in claim 1, is characterized in that: step 4) in pickling be first 20wt%～40wt% by concentration HCl or HNO
3or H
2sO
4washing, the rear HF solution washing with 20wt%～40wt% to pH be 6～8.
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Cited By (16)
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| CN104009235A (en) * | 2014-05-13 | 2014-08-27 | 昆明理工大学 | Preparation method of porous silicon/graphene composite material |
| CN104518209A (en) * | 2014-12-09 | 2015-04-15 | 江西正拓新能源科技股份有限公司 | Lithium ion battery silicon composite material and preparation method thereof |
| CN104577045A (en) * | 2014-12-20 | 2015-04-29 | 江西正拓新能源科技股份有限公司 | Silicon-carbon composite material of lithium ion battery and preparation method of silicon-carbon composite material |
| CN104617275A (en) * | 2015-02-11 | 2015-05-13 | 武汉科技大学 | Method for preparing silicon-carbon compound from silicon-containing biomass as raw material as well as prepared silicon-carbon compound and application thereof |
| CN105417543A (en) * | 2015-10-26 | 2016-03-23 | 河北民族师范学院 | Process for preparing nano porous silicon electrode material |
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| CN106430213A (en) * | 2016-09-07 | 2017-02-22 | 扬州大学 | Low-temperature preparation method of rice-hull-based porous silicon material |
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| US10941273B2 (en) | 2015-11-20 | 2021-03-09 | Jinan Shengquan Group Share Holding Co., Ltd. | Graphene-containing modified latex as well as preparation method therefor and application thereof |
| US11306416B2 (en) | 2015-11-26 | 2022-04-19 | Jinan Shengquan Group Share Holding Co., Ltd. | Functional regenerated viscose fiber |
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