CN103682268B - The preparation method of the silicium cathode material of a kind of carbon, lithium titanate double-coated - Google Patents
The preparation method of the silicium cathode material of a kind of carbon, lithium titanate double-coated Download PDFInfo
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- CN103682268B CN103682268B CN201310639148.5A CN201310639148A CN103682268B CN 103682268 B CN103682268 B CN 103682268B CN 201310639148 A CN201310639148 A CN 201310639148A CN 103682268 B CN103682268 B CN 103682268B
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- 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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- 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 secondary lithium ion battery key material technical field, provide the preparation method of silicium cathode material of a kind of carbon, lithium titanate double-coated.Take chelating agent as carbon source, soluble T i compound is titanium source, nano-silicon source and various lithium compound be lithium source, adopt the silicon based anode material of two chelating agent sol-gal process synthesis carbon, lithium titanate double-coated.The advantage of lithium titanate and silicon materials combines by the present invention, and the lithium ion battery of preparation has height ratio capacity, excellent cyclical stability, high consistency, by height ratio capacity and high stability is organic gathers together, is with a wide range of applications.
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 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, speciality efficiently capable of circulation, becomes the object that numerous manufacturer selects first to consider during power.Develop the new type lithium ion battery that specific capacity is larger, cycle performance better, discharge and recharge is safer sooner, also become the target of numerous scientific worker 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 got most of the attention.But, silicon when discharge and recharge up to the change in volume of 300%, make its bear in charge and discharge cycles very large mechanicals efforts and gradually efflorescence cave in, lose electrical contact with collector, finally cause battery failure, show the cycle performance of extreme difference.For this problem, researcher proposes many solutions, such as, reduce silicium cathode material particle size, prepare loose structure silicon, and prepare silicon based composite material.
Spinel-type Li
4ti
5o
12be a kind of " zero strain " material, cell parameter changes hardly at Lithium-ion embeding with before and after deviating from, thus makes it have excellent cycle performance and stable discharge voltage.Therefore introduce lithium titanate and can provide good mechanical support for silicon, the violent change in volume that lithium titanate coating layer can suppress silicon to produce in de-lithium and embedding lithium process effectively, lower inner contact loss, and then improve the carrying out of internal resistance and de-/embedding lithium.
Silicon and lithium titanate have same shortcoming, and namely conductivity is not high, in charge and discharge process, easily 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 material that conductivity is not high, common way is that to carry out carbon coated, improves the electric conductivity on its surface.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention proposes the preparation method of 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) be distributed in absolute ethyl alcohol by lithium source, titanium source and chelating agent, magnetic agitation 12 ~ 18 hours, obtains colloidal sol at normal temperatures; Wherein involved charge ratio is mol ratio=(0.8 ~ 1.0) of Li:Ti: 1, chelating agent: mol ratio=(1.0 ~ 3.0) of metal ion: 1, Ti compound: volume ratio=1:(5 ~ 20 of alcohol);
(2) in the colloidal sol of step (1) gained, add silicon source, stir 3 ~ 4 hours at 60 ~ 80 DEG C of lower magnetic forces, obtain the gel that silicon source fully disperses; Wherein involved charge ratio is silicon: mol ratio=(0.05 ~ 0.3) of metal ion: 1;
(3) gained gel in step (2) be placed in convection oven dry 3 ~ 24 hours, obtain black lithium titanate coated Si presoma, the temperature told in baking oven be 150 ~ 250 DEG C;
(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) black presoma tiny for the particle of gained in step (4) is transferred in tube furnace calcines 5 ~ 15 hours, obtain finished product carbon, lithium titanate double-coated silicium cathode material, calcining heat is 650 ~ 850 DEG C, atmosphere of ventilating be x%Ar+ (1-x) %H
2.
Described lithium source is one 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 or its combination.
Described soluble T i compound is tetra-n-butyl titanate, tetraisopropyl titanate, the one in the chloride of titanium or its combination.
Described bi-component chelating agent is triethanolamine, acetic acid, laurate, tartaric acid, citric acid, oxalic acid, gluconic acid, 2, two kinds in 2'-bipyridine, 1,10-phenanthrolene, aminotriacetic acid, diethylene-triamine pentaacetic acid, ethylenediamine, ethylenediamine tetra-acetic acid.
Described silicon source is nano silica fume, or nanometer particle.
The present invention adopts bi-component chelating agent, can either make reactant Homogeneous phase mixing on a molecular scale, makes the final lithium titanate coating thickness uniformity formed, can form again the carbon source of carbon coating layer as pyrolysis.Meanwhile, the present invention strictly controls the selection that silicon source adds colloidal sol opportunity, avoids the possibility reunited in silicon source.In addition, the present invention, by controlling the size of the amount in the silicon source added in a certain amount of colloidal sol, controls the thickness of end-product coating layer, thus realizes by the change of carbon-lithium titanate mixed monolayer coated Si negative material to carbon, lithium titanate double-coated silicium cathode material.Also the ratio by changing chelating agent and metal ion changes 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 the advantage 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, prepare burden according to the mol ratio of Li:Ti=0.84:1, take the tetra-n-butyl titanate (analyzing pure) of 25.52g, the lithium carbonate (analyzing pure) of 2.33g, 20g ethylenediamine tetra-acetic acid and 30g citric acid join in 300ml absolute ethyl alcohol, to be stirred formation colloidal sol by magnetic force heating stirrer; Add 0.2g nano silica fume again, add thermal agitation at 80 DEG C, until obtain the gel that silicon source fully disperses; Dry in the convection oven of 240 DEG C, 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 presoma tiny for particle is put into tube furnace, pass to Ar gas, in 750 DEG C of calcining 5h, obtain finished product carbon, lithium titanate double-coated silicium cathode material.
Embodiment 2:
By the soluble compound compound of Li and Ti, prepare burden according to the mol ratio of Li:Ti=0.84:1, take the tetraisopropyl titanate (analyzing pure) of 21.31g, the lithium acetate (analyzing pure) of 6.43g, 20g ethylenediamine tetra-acetic acid and 40g citric acid join in 300ml absolute ethyl alcohol, to be stirred formation colloidal sol by magnetic force heating stirrer; Add 0.2g nanometer particle again, add thermal agitation at 80 DEG C, until obtain the gel that silicon source fully disperses; Dry in the convection oven of 240 DEG C, 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 presoma tiny for particle is put into tube furnace, pass to 95%Ar+5%H
2, in 750 DEG C 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, prepare burden according to the mol ratio of Li:Ti=0.88:1, take the tetra-n-butyl titanate (analyzing pure) of 25.52g, the lithium nitrate (analyzing pure) of 4.55g, 20g ethylenediamine tetra-acetic acid and 60g citric acid join in 300ml absolute ethyl alcohol, to be stirred formation colloidal sol by magnetic force heating stirrer; Add 0.6g nano silica fume again, add thermal agitation at 80 DEG C, until obtain the gel that silicon source fully disperses; Dry in the convection oven of 240 DEG C, 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 ~ 10h, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny; Finally presoma tiny for particle is put into tube furnace, pass to Ar gas, in 750 DEG C of calcining 5h, obtain finished product carbon, lithium titanate double-coated silicium cathode material.
Embodiment 4:
By the soluble compound compound of Li and Ti, prepare burden according to the mol ratio of Li:Ti=0.88:1, take the tetraisopropyl titanate (analyzing pure) of 21.31g, the lithium acetate (analyzing pure) of 6.74g, 30g ethylenediamine tetra-acetic acid and 50g citric acid join in 300ml absolute ethyl alcohol, to be stirred formation colloidal sol by magnetic force heating stirrer; Add 0.6g nanometer particle again, add thermal agitation at 80 DEG C, until obtain the gel that silicon source fully disperses; Dry in the convection oven of 240 DEG C, 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 presoma tiny for particle is put into tube furnace, pass to 95%Ar+5%H
2, in 750 DEG C 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, prepare burden according to the mol ratio of Li:Ti=4.6:5, take the tetraisopropyl titanate (analyzing pure) of 21.31g, the lithium oxalate (analyzing pure) of 3.52g, 20g ethylenediamine tetra-acetic acid and 50g citric acid join in 300ml absolute ethyl alcohol, to be stirred formation colloidal sol by magnetic force heating stirrer; Add 1.2g nano silica fume again, add thermal agitation at 80 DEG C, until obtain the gel that silicon source fully disperses; Dry in the convection oven of 240 DEG C, 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 ~ 10h, wherein the mass ratio of ball and material is 2:1, obtains the lithium titanate coated Si presoma that particle is tiny; Finally presoma tiny for particle is put into tube furnace, pass to Ar gas, in 750 DEG C 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) be distributed in absolute ethyl alcohol by lithium source, titanium source and two component chelating agent, magnetic agitation 12 ~ 18 hours, obtains colloidal sol at normal temperatures; Wherein involved charge ratio is mol ratio=(0.8 ~ 1.0) of Li:Ti: 1, two component chelating agent: mol ratio=(1.0 ~ 3.0) of metal ion: 1, titanium source: volume ratio=1:(5 ~ 20 of absolute ethyl alcohol);
(2) in the colloidal sol of step (1) gained, add silicon source, stir 3 ~ 4 hours at 60 ~ 80 DEG C of lower magnetic forces, obtain the gel that silicon source fully disperses; Wherein involved charge ratio is silicon: mol ratio=(0.05 ~ 0.3) of metal ion: 1;
(3) be placed in convection oven by gained gel in step (2) and dry 3 ~ 24 hours, obtain black lithium titanate coated Si presoma, the temperature in described convection oven is 150 ~ 250 DEG C;
(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) black presoma tiny for the particle of gained in step (4) is transferred in tube furnace, calcine 5 ~ 15 hours under certain atmosphere, obtain finished product carbon, lithium titanate double-coated silicium cathode material, calcining heat is 650 ~ 850 DEG C, and described atmosphere is 100%Ar or 95%Ar+5%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 one in lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate, isopropyl lithium alkoxide or its combination.
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 titanium source is one in the chloride of the tetra-n-butyl titanate of solubility, tetraisopropyl titanate or titanium or its combination.
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, two kinds in 2'-bipyridine, 1,10-phenanthrolene, aminotriacetic acid, diethylene-triamine pentaacetic acid, ethylenediamine, ethylenediamine tetra-acetic acid.
5. 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 silicon source is nano silica fume or nanometer particle.
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| CN102820461B (en) * | 2012-08-20 | 2014-10-15 | 上海交通大学 | Method for preparing carbon-coated nano-lithium titanate by ethylene diamine tetraacetic acid-citric acid (EDTA-CA) joint complexation |
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