CN103682268A - Preparation method of carbon-lithium titanate double-layer coated silicon negative electrode material - Google Patents
Preparation method of carbon-lithium titanate double-layer coated silicon negative electrode material Download PDFInfo
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- CN103682268A CN103682268A CN201310639148.5A CN201310639148A CN103682268A CN 103682268 A CN103682268 A CN 103682268A CN 201310639148 A CN201310639148 A CN 201310639148A CN 103682268 A CN103682268 A CN 103682268A
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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
- H01M4/366—Composites as layered products
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- 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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Abstract
The invention belongs to the secondary lithium ion battery key material technical field, and provides a method for preparing a carbon-lithium titanate double-layer coated silicon negative electrode material. With chelating agents as carbon sources, a soluble Ti compound as a titanium source, a nano silicon source and various lithium compounds as lithium sources, the carbon-lithium titanate double-layer coated silicon negative electrode material is synthesized by a double-chelating-agent sol-gel method. Through combination of advantages of lithium titanate and the silicon material, a prepared lithium ion battery has high specific capacity, excellent cycling stability and quite high consistency, allows the high specific capacity and the high stability to be organically gathered together, and has wide application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of cell negative electrode material, be specifically related to the preparation method of the silicium cathode material of a kind of carbon, lithium titanate double-coated.
Background technology
In current environmental pollution, under the background of energy scarcity, lithium ion battery, because of its cleanliness without any pollution, efficient speciality capable of circulation, becomes the object of first considering when power is selected by numerous manufacturers.Develop that specific capacity is larger, cycle performance better, discharge and recharge faster safer new type lithium ion battery, also become numerous scientific workers target of unremitting effort for it.
Silicon has theoretical specific capacity (3572mAh/g) maximum in known lithium ion battery negative material, and when room temperature lower de-lithium current potential (< 0.5V), now become the negative pole candidate material of the high capacity cell of future generation getting most of the attention.Yet, silicon when discharging and recharging up to 300% change in volume, make its in charge and discharge cycles, bear very large mechanicals efforts and gradually efflorescence cave in, lose and electrically contact with collector, finally cause battery failure, show the cycle performance of extreme difference.For this problem, researcher has proposed many solutions, for example, reduce silicium cathode material granule size, prepares loose structure silicon, and prepares silicon based composite material.
Spinel-type Li
4ti
5o
12be a kind of " zero strain " material, cell parameter changes hardly before and after lithium ion embeds and deviates from, thereby makes it have good cycle performance and discharge voltage stably.Therefore introducing lithium titanate can provide good mechanical support for silicon, and lithium titanate coating layer can suppress the violent change in volume that silicon produces in de-lithium and embedding lithium process effectively, lowers inner contact loss, and then improves the carrying out of internal resistance and de-/embedding lithium.
Silicon and lithium titanate have same shortcoming, and conductivity is not high, easily in charge and discharge process, cause the enrichment of electronics, hinder the embedding of lithium ion and deviate from, and affect the battery performance of battery under high magnification.For the not high material of conductivity, common way is to carry out carbon to be coated, and improves its surperficial electric conductivity.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention proposes the preparation method of the silicium cathode material of a kind of carbon, lithium titanate double-coated.
A preparation method for the silicium cathode material of carbon, lithium titanate double-coated, is characterized in that, the concrete steps of the method are:
(1) lithium source, titanium source and chelating agent are distributed in absolute ethyl alcohol, magnetic agitation is 12～18 hours at normal temperatures, obtains colloidal sol; The mol ratio that wherein related charge ratio is Li:Ti=(0.8～1.0): 1, chelating agent: the mol ratio of metal ion=(1.0～3.0): 1, Ti compound: volume ratio=1:(5～20 of alcohol);
(2) in the colloidal sol of step (1) gained, add silicon source, at 60～80 ℃ of lower magnetic forces, stir 3～4 hours, obtain the gel that silicon source fully disperses; Wherein related charge ratio is silicon: the mol ratio of metal ion=(0.05～0.3): 1;
(3) gained gel in step (2) is placed in convection oven and is dried 3～24 hours, obtain black lithium titanate coated Si presoma, the temperature of being told in baking oven is 150～250 ℃;
(4) the black presoma of gained in step (3) is put into high energy ball mill ball milling 1～10 hour, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny;
(5) the tiny black presoma of particle of gained in step (4) is transferred in tube furnace and is calcined 5～15 hours, obtain finished product carbon, lithium titanate double-coated silicium cathode material, calcining heat is 650～850 ℃, and the atmosphere of ventilating is x%Ar+ (1-x) %H
2.
Described lithium source is a kind of or its combination in lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate, isopropyl lithium alkoxide, long-chain or short-chain alkyl lithium.
Described soluble T i compound is tetra-n-butyl titanate, tetraisopropyl titanate, a kind of or its combination in the chloride of titanium.
Described bi-component chelating agent is triethanolamine, acetic acid, laurate, tartaric acid, citric acid, oxalic acid, gluconic acid, 2,2'-bipyridine, 1, in 10-phenanthrolene, aminotriacetic acid, diethylene-triamine pentaacetic acid, ethylenediamine, ethylenediamine tetra-acetic acid two kinds.
Described silicon source is nano silica fume, or mesoporous silicon nano particle.
The present invention adopts bi-component chelating agent, can either make reactant evenly mix on molecular level, makes the final lithium titanate coating thickness uniformity forming, and can form as pyrolysis the carbon source of carbon coating layer again.Meanwhile, the present invention strictly controls silicon source and adds the colloidal sol selection on opportunity, the possibility of avoiding silicon source to reunite.In addition, the present invention can control the thickness of end-product coating layer by controlling the size of the amount in the silicon source adding in a certain amount of colloidal sol, thereby realizes the variation to carbon, lithium titanate double-coated silicium cathode material by carbon-lithium titanate mixed monolayer coated Si negative material.Also can change by changing the ratio of chelating agent and metal ion the ratio of carbon coating layer and lithium titanate coating layer.Product carbon of the present invention, lithium titanate double-coated silicium cathode material have advantages of large specific capacity, long circulation life, and have superior fast charging and discharging ability.
Accompanying drawing explanation
The schematic flow sheet of Fig. 1 embodiment of the present invention.
Embodiment
The present invention is described in detail below by instantiation, but protection scope of the present invention is not limited to these examples of implementation.
Embodiment 1:
By the soluble compound compound of Li and Ti, mol ratio according to Li:Ti=0.84:1 is prepared burden, take the tetra-n-butyl titanate (analyzing pure) of 25.52g, the lithium carbonate of 2.33g (analyzing pure), 20g ethylenediamine tetra-acetic acid and 30 g citric acids join in 300ml absolute ethyl alcohol, by the magnetic force heating stirrer formation colloidal sol that stirs; Add again 0.2g nano silica fume, at 80 ℃, add thermal agitation, until obtain the gel that silicon source fully disperses; In the convection oven of 240 ℃, dry, obtain the lithium titanate coated Si presoma that black is fluffy; Then presoma is put into high energy ball mill ball milling 1 ~ 10h, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny; Finally the tiny presoma of particle is put into tube furnace, pass to Ar gas, in 750 ℃ of calcining 5 h, obtain finished product carbon, lithium titanate double-coated silicium cathode material.
Embodiment 2:
By the soluble compound compound of Li and Ti, mol ratio according to Li:Ti=0.84:1 is prepared burden, take the tetraisopropyl titanate (analyzing pure) of 21.31 g, the lithium acetate of 6.43g (analyzing pure), 20g ethylenediamine tetra-acetic acid and 40g citric acid join in 300ml absolute ethyl alcohol, by the magnetic force heating stirrer formation colloidal sol that stirs; Add again 0.2g mesoporous silicon nano particle, at 80 ℃, add thermal agitation, until obtain the gel that silicon source fully disperses; In the convection oven of 240 ℃, dry, obtain the lithium titanate coated Si presoma that black is fluffy; Then presoma is put into high energy ball mill ball milling 1 ~ 10h, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny; Finally the tiny presoma of particle is put into tube furnace, pass to 95%Ar+5%H
2, in 750 ℃ of calcining 5h, obtain finished product carbon, lithium titanate double-coated silicium cathode material.
Embodiment 3:
By the soluble compound compound of Li and Ti, mol ratio according to Li:Ti=0.88:1 is prepared burden, take the tetra-n-butyl titanate (analyzing pure) of 25.52 g, the lithium nitrate of 4.55g (analyzing pure), 20g ethylenediamine tetra-acetic acid and 60g citric acid join in 300ml absolute ethyl alcohol, by the magnetic force heating stirrer formation colloidal sol that stirs; Add again 0.6g nano silica fume, at 80 ℃, add thermal agitation, until obtain the gel that silicon source fully disperses; In the convection oven of 240 ℃, dry, obtain the lithium titanate coated Si presoma that black is fluffy; Then lithium titanate precursor is put into high energy ball mill ball milling 1 ~ 10 h, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny; Finally the tiny presoma of particle is put into tube furnace, pass to Ar gas, in 750 ℃ of calcining 5 h, obtain finished product carbon, lithium titanate double-coated silicium cathode material.
Embodiment 4:
By the soluble compound compound of Li and Ti, mol ratio according to Li:Ti=0.88:1 is prepared burden, take the tetraisopropyl titanate (analyzing pure) of 21.31 g, the lithium acetate of 6.74g (analyzing pure), 30g ethylenediamine tetra-acetic acid and 50 g citric acids join in 300ml absolute ethyl alcohol, by the magnetic force heating stirrer formation colloidal sol that stirs; Add again 0.6g mesoporous silicon nano particle, at 80 ℃, add thermal agitation, until obtain the gel that silicon source fully disperses; In the convection oven of 240 ℃, dry, obtain the lithium titanate coated Si presoma that black is fluffy; Then presoma is put into high energy ball mill ball milling 1 ~ 10 h, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny; Finally the tiny presoma of particle is put into tube furnace, pass to 95%Ar+5%H
2, in 750 ℃ of calcining 5h, obtain finished product carbon, lithium titanate double-coated silicium cathode material.
Embodiment 5:
By the soluble compound compound of Li and Ti, mol ratio according to Li:Ti=4.6:5 is prepared burden, take the tetraisopropyl titanate (analyzing pure) of 21.31 g, the lithium oxalate of 3.52 g (analyzing pure), 20 g ethylenediamine tetra-acetic acids and 50 g citric acids join in 300ml absolute ethyl alcohol, by the magnetic force heating stirrer formation colloidal sol that stirs; Add again 1.2g nano silica fume, at 80 ℃, add thermal agitation, until obtain the gel that silicon source fully disperses; In the convection oven of 240 ℃, dry, obtain the lithium titanate coated Si presoma that black is fluffy; Then lithium titanate precursor is put into high energy ball mill ball milling 1 ~ 10 h, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny; Finally the tiny presoma of particle is put into tube furnace, pass to Ar gas, in 750 ℃ of calcining 5h, obtain finished product carbon, lithium titanate double-coated silicium cathode material.
Claims (5)
1. a preparation method for the silicium cathode material of carbon, lithium titanate double-coated, is characterized in that, the concrete steps of the method are:
(1) lithium source, titanium source and chelating agent are distributed in absolute ethyl alcohol, magnetic agitation is 12～18 hours at normal temperatures, obtains colloidal sol; The mol ratio that wherein related charge ratio is Li:Ti=(0.8～1.0): 1, chelating agent: the mol ratio of metal ion=(1.0～3.0): 1, Ti compound: volume ratio=1:(5～20 of alcohol);
(2) in the colloidal sol of step (1) gained, add silicon source, at 60～80 ℃ of lower magnetic forces, stir 3～4 hours, obtain the gel that silicon source fully disperses; Wherein related charge ratio is silicon: the mol ratio of metal ion=(0.05～0.3): 1;
(3) gained gel in step (2) is placed in convection oven and is dried 3～24 hours, obtain black lithium titanate coated Si presoma, the temperature of being told in baking oven is 150～250 ℃;
(4) the black presoma of gained in step (3) is put into high energy ball mill ball milling 1～10 hour, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny;
(5) the tiny black presoma of particle of gained in step (4) is transferred in tube furnace and is calcined 5～15 hours, obtain finished product carbon, lithium titanate double-coated silicium cathode material, calcining heat is 650～850 ℃, and the atmosphere of ventilating is x%Ar+ (1-x) %H
2.
2. the preparation method of the silicium cathode material of a kind of carbon, lithium titanate double-coated according to claim 1, it is characterized in that, described lithium source is a kind of or its combination in lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate, isopropyl lithium alkoxide, long-chain or short-chain alkyl lithium.
3. the preparation method of the silicium cathode material of a kind of carbon, lithium titanate double-coated according to claim 1, is characterized in that, described soluble T i compound is tetra-n-butyl titanate, tetraisopropyl titanate, a kind of or its combination in the chloride of titanium.
4. the preparation method of the silicium cathode material of a kind of carbon, lithium titanate double-coated according to claim 1, it is characterized in that, described bi-component chelating agent is triethanolamine, acetic acid, laurate, tartaric acid, citric acid, oxalic acid, gluconic acid, 2,2'-bipyridine, 1, in 10-phenanthrolene, aminotriacetic acid, diethylene-triamine pentaacetic acid, ethylenediamine, ethylenediamine tetra-acetic acid two kinds.
5. the preparation method of the silicium cathode material of a kind of carbon, lithium titanate double-coated according to claim 1, is characterized in that, described silicon source is nano silica fume, or mesoporous silicon nano particle.
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| CN104319366A (en) * | 2014-10-09 | 2015-01-28 | 奇瑞汽车股份有限公司 | Silicon/graphite/lithium titanate composite anode material and preparation method thereof |
| CN106328900A (en) * | 2016-10-09 | 2017-01-11 | 珠海格力电器股份有限公司 | Lithium titanate and carbon double-layer cladded silicon compound material, preparation method and application |
| CN107959012A (en) * | 2017-11-17 | 2018-04-24 | 力信（江苏）能源科技有限责任公司 | A kind of individual layer/double-coating Si oxide composite negative pole material and preparation method thereof |
| CN108232175A (en) * | 2018-02-06 | 2018-06-29 | 安徽科达铂锐能源科技有限公司 | A kind of lithium ion battery graphite/lithium titanate composite anode material and preparation method |
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| CN109786665A (en) * | 2018-12-20 | 2019-05-21 | 上海力信能源科技有限责任公司 | A kind of silicon-carbon composite cathode pole piece and preparation method thereof |
| CN109713271A (en) * | 2018-12-27 | 2019-05-03 | 山东精工电子科技有限公司 | The synthetic method of the carbon composite of high-energy density three-dimensional texture |
| CN110931761A (en) * | 2019-12-20 | 2020-03-27 | 江苏厚生新能源科技有限公司 | Lithium battery negative electrode material with double-layer coating layer and preparation method thereof |
| CN111342020A (en) * | 2020-03-11 | 2020-06-26 | 中国科学院宁波材料技术与工程研究所 | Silicon-based negative electrode material, preparation method thereof and lithium ion battery |
| CN115799492A (en) * | 2023-02-02 | 2023-03-14 | 河北格力钛新能源有限公司 | Method for preparing modified silicon-carbon composite material and modified silicon-carbon composite material |
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