CN105047868A - Preparation method of high-capacity lithium battery anode material - Google Patents
Preparation method of high-capacity lithium battery anode material Download PDFInfo
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- CN105047868A CN105047868A CN201510331371.2A CN201510331371A CN105047868A CN 105047868 A CN105047868 A CN 105047868A CN 201510331371 A CN201510331371 A CN 201510331371A CN 105047868 A CN105047868 A CN 105047868A
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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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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- 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
- H01M4/387—Tin or alloys based on tin
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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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
- 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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- H—ELECTRICITY
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- 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
- H01M4/626—Metals
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a preparation method of a high-capacity lithium battery anode material. In the anode material, tin is combined with metal and carbon to form a multi-phase composite system, so that high capacity of the material is ensured; and the volume expansion and contraction effect in charging and discharging processes can also be relieved. The tin and metal are dispersed into a cracking carbon system; the metal plays a role in improving the conductivity; the characteristic of high capacity of the tin is put into play; a mechanical support is provided by cracking carbon; and the structure of the material is stabilized. The tin-carbon composite anode material provided by the invention has high compaction density, good processability, high conductivity, high first efficiency and excellent cycling stability. The anode material provided by the invention is simple in preparation technology, low in raw material cost, friendly to environment, free of pollution and suitable for industrial production.
Description
Technical field
The invention belongs to lithium ion battery negative material field, particularly a kind of preparation method of high-capacity lithium battery negative material, be specifically related to a kind of preparation method of tin carbon compound cathode materials.
Background technology
At present continuous deterioration with climatic environment in short supply along with global petroleum resources, human social development is faced with stern challenge.The new-energy automobile of development clean energy-saving is subject to the great attention of countries in the world.The development of new-energy automobile, crucial in its electrical source of power.Lithium ion battery has the advantages such as energy density is large, self discharge is little, memory-less effect, operating voltage range are wide, long service life, non-environmental-pollution, is the main electrical source of power of current new-energy automobile.And the crucial electrode material of lithium ion battery is the final deciding factor of battery performance, wherein the raising of negative material to performance of lithium ion battery plays vital effect.Therefore, high-performance, cheap negative material is developed to promoting that the development of new-energy automobile and relevant new industry has great importance.
Current negative material is mainly graphite, and its specific capacity, close to the theoretical value of 372mAh/g, is difficult to have the space of lifting again, and therefore finding the height ratio capacity negative material substituting carbon becomes an important developing direction.Due to the limitation of graphite cathode material, therefore very necessary to the exploitation of Novel anode material.Novel negative material has alloy material, tin-based oxide material etc.Although alloy material can provide higher reversible capacity, its cycle performance is not ideal enough.Although tin-based oxide material has higher reversible capacity and good cycle performance, its shortcoming is the irreversible capacity loss comparatively large (being often greater than 50%) that circulates first.
The theoretical specific capacity (994mAh/g) of tin base cathode material for the twice of graphite cathode material (372mAh/g) many, intercalation potential is moderate simultaneously, tin base cathode material is become be worth studying and has the lithium ion battery negative material of development potentiality.But the Volumetric expansion that tin-based material is huge causes, and its cycle performance is lower and irreversible capacity is larger.
Research shows metal dust and glass putty compound to prepare the performance that tin carbon negative pole material can greatly improve tin negative pole material.The advantages such as metal itself has good ductility, high conductivity, and mechanical strength is high, therefore select suitable metal and tin to form tin carbon, effectively can overcome the bulk effect of tin in charge and discharge process, improve the cyclical stability of material, conductivity is also necessarily improved.But current existing tin carbon negative pole material capacity and head are imitated generally on the low side, and the material consistency of preparation is poor.
Therefore, the tin carbon compound cathode materials developing a kind of high conductivity, high power capacity, high first charge-discharge efficiency and good cycling stability is the technical barrier of field of lithium ion battery.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is the preparation method providing a kind of high-capacity lithium battery negative material, described negative material good conductivity, and capacity and first coulombic efficiency are high, simultaneously Stability Analysis of Structures, and cycle performance is excellent.
For reaching above-mentioned purpose, the invention provides a kind of preparation method of high-capacity lithium battery negative material, comprising the following steps:
(1) metal dust is mixed with glass putty, carbon source presoma, ball-milling, prepare tin carbon;
(2) step (1) gained tin carbon is sintered under inert gas shielding, obtain tin carbon compound cathode materials;
(3) composite material step (2) obtained is pulverized, is sieved and remove magnetic, obtains the tin carbon compound cathode materials that particle diameter D50 is 1.0 ~ 10 μm.
Further, step (1) metal dust: glass putty weight ratio is 1:0.1 ~ 2, carbon source presoma: the weight ratio of metal dust and glass putty total weight is 1:0.01 ~ 0.15.
Further, ball-milling described in step (1) adopts dry ball milling or wet ball grinding.
Preferably, the step of described dry ball milling is: the mixed-powder of metal dust and glass putty, carbon source presoma and ball milling pearl are loaded in ball milling cavity, then pass into protective gas, carry out ball milling, obtain tin carbon dust.
Preferably, the step of described wet ball grinding is: mixing metal dust and glass putty, add solvent in carbon source presoma, stir, obtain mixed-powder slurry; Mixed-powder slurry and ball milling pearl are loaded in ball milling cavity and carries out ball milling, dry, obtain tin carbon dust.
Further, described in step (1), solvent is preferably organic solvent and/or water.
Preferably, described organic solvent is oxolane, acid amides, 1 kind in alcohol and ketone or the combination of at least 2 kinds, be preferably oxolane, dimethylacetylamide, 1 kind in C1-C6 alcohol and C3-C8 ketone or the combination of at least 2 kinds, more preferably methyl alcohol, ethanol, ethylene glycol, propyl alcohol, isopropyl alcohol, 1, 2-propylene glycol, 1, ammediol, glycerol, n-butanol, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, n-amyl alcohol and 2-hexanol, acetone, methyl ethyl ketone, methyl propyl ketone, 1-METHYLPYRROLIDONE, ethyl propyl ketone, methyl butyl ketone, ethyl n-butyl ketone, 1 kind in methyl amyl ketone and methyl hexyl ketone or the combination of at least 2 kinds.
Further, the ball-grinding machine described in step (1) is any one in high-speed stirred mill, planetary ball mill, tube mill, type taper grinder, rod mill and sand mill, is preferably planetary ball mill.
Preferably, described ball milling bead diameter is 0.1 ~ 20mm, and ratio of grinding media to material is 10 ~ 200:1.
Preferably, the rotating speed of described ball milling is 100 ~ 3000rpm, and Ball-milling Time is 5 ~ 120h.
Preferably, the material of described ball milling pearl is stainless steel, agate, pottery, zirconia, aluminium oxide, the one in carbide alloy.
Further, described in step (1), metal dust is elemental metals and/or metal alloy compound, is preferably tin simple substance, antimony simple substance, iron simple substance, germanium simple substance, aluminium simple substance, magnesium simple substance, zinc simple substance, sows the combination of in simple substance, cadmium simple substance, titanium simple substance, tin pewter, tin ferroalloy, tin titanium alloy, magnesium antimony alloy, aluminium-antimony alloy, almag and tin magnesium alloy a kind or at least 2 kinds.
Preferably, the median particle diameter of described metal dust is 0.1 ~ 100 μm, is preferably 0.5 ~ 50 μm, more preferably 1.0 ~ 15 μm.
Preferably, the median particle diameter of described tin powder is 0.05 ~ 30 μm, more preferably 0.1 ~ 10 μm, is particularly preferably 0.2 ~ 5 μm.
Further, carbon source presoma described in step (1) is the combination of in polymer, carbohydrate, organic acid, pitch and macromolecular material a kind or at least 2 kinds, is preferably the combination of in epoxy resin, phenolic resins, furfural resin, Lauxite, polyvinyl alcohol, polyvinyl chloride, polyethylene glycol, poly(ethylene oxide), Kynoar, acrylic resin and polyacrylonitrile a kind or at least 2 kinds.
Further, step (2) described inert gas is the combination of in nitrogen, helium, neon, argon gas, Krypton and xenon a kind or at least 2 kinds.
Further, step (2) described sintering temperature is 600 ~ 1200 DEG C.
Preferably, described heating rate 0.5 ~ 10 DEG C/min, temperature retention time is insulation 1 ~ 5h.
Compared with prior art, negative material of the present invention to be combined with metal, carbon by tin and to form heterogeneous compound system, not only ensure that the high power capacity of material, can also alleviate in charge and discharge process, volumetric expansion blockage effect.By tin and metal dispersion in cracking carbon system, metal plays the effect improving conductivity, and tin plays the characteristic of high power capacity, and cracking carbon provides mechanical support, the structure of stabilizing material.Tin carbon compound cathode materials compacted density of the present invention is high, processing characteristics is good, conductivity is high, efficiency is high first, cyclical stability is excellent.The preparation technology of negative material provided by the invention is simple, low raw-material cost, and environmental friendliness is pollution-free, is applicable to suitability for industrialized production.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment only understands the present invention for helping, and should not be considered as concrete restriction of the present invention.
Embodiment 1
(1) to be the Fe powder of 10 μm and median particle diameter by median particle diameter the be glass putty of 3 μm, by weight Fe:Si=1:2, carry out proportioning, simultaneously in Fe powder and glass putty total weight: the ratio of carbon source presoma=0.1:1 takes phenolic resins, and ball milling 50h is to mixing;
(2) powder obtained in step (1) is placed in box type furnace, passes into argon gas, be warming up to 1050 DEG C with 10 DEG C/min heating rate, insulation 10h, naturally cools to room temperature;
(3) powder obtained in step (2) is pulverized, sieved and remove magnetic, obtain the tin carbon compound cathode materials that particle diameter D50 is 1.0-10 μm.
Embodiment 2
(1) by the Cu powder of median particle diameter 10 μm and median particle diameter be the glass putty of 0.05 μm, by weight Cu:Si=2:1, carry out proportioning, simultaneously in Cu powder and glass putty total weight: the ratio of carbon source presoma=0.5:1 takes epoxy resin, and ball milling 40h is to mixing;
(2) powder obtained in step (1) is placed in box type furnace, passes into argon gas, be warming up to 900 DEG C with 10 DEG C/min heating rate, insulation 10h, naturally cools to room temperature;
(3) powder obtained in step (2) is pulverized, sieved and remove magnetic, obtain the tin carbon compound cathode materials that particle diameter D50 is 1.0-10 μm.
Embodiment 3
(1) by the tin titanium alloy powder of median particle diameter 0.1 μm and median particle diameter be the glass putty of 30 μm, by weight Ti-Si:Si=2:1, carry out proportioning, simultaneously in tin titanium alloy powder and glass putty total weight: the ratio of carbon source presoma=0.5:1 takes phenolic resins, be scattered in alcohol solvent, then slurry is dropped in sand mill and carry out ball milling, wherein, ball is 0.1mm zirconium ball, drum's speed of rotation is 1500r/min, the mass ratio of ball and powder is 10:1, after ball milling 5h, obtains tin titanium alloy slurry;
(2) powder obtained in step (1) is placed in box type furnace, passes into argon gas, be warming up to 800 DEG C with 10 DEG C/min heating rate, insulation 2h, naturally cools to room temperature;
(3) powder obtained in step (2) is pulverized, sieved and remove magnetic, obtain the tin carbon compound cathode materials that particle diameter D50 is 1.0-10 μm.
Embodiment 4
(1) by the tin ferroalloy powder of median particle diameter 10 μm and median particle diameter be the glass putty of 5 μm, by weight Fe-Si:Si=3:1, carry out proportioning simultaneously in tin ferroalloy powder and glass putty total weight: the ratio of carbon source presoma=0.5:1 takes pitch, be scattered in tetrahydrofuran solvent, then slurry is dropped in sand mill and carry out ball milling, wherein, ball is 0.2mm zirconium ball, drum's speed of rotation is 3000r/min, the mass ratio of ball and powder is 20:1, after ball milling 6h, obtain tin ferroalloy slurry;
(2) powder obtained in step (1) is placed in box type furnace, passes into argon gas, be warming up to 1000 DEG C with 10 DEG C/min heating rate, insulation 10h, naturally cools to room temperature;
(3) powder obtained in step (2) is pulverized, sieved and remove magnetic, obtain the tin carbon compound cathode materials that particle diameter D50 is 1.0-10 μm.
Comparative example 1
Tin carbon compound cathode materials is prepared according to method substantially the same manner as Example 1, difference is: directly glass putty and phenolic resins are carried out ball milling according to the weight ratio of 0.1:1, powder after ball milling is sintered, then pulverize, sieve and remove magnetic, obtain the tin carbon compound cathode materials that particle diameter D50 is 1.0-10 μm.
By the negative material that above-described embodiment and comparative example obtain, adopt following methods test electrochemistry cycle performance: by negative material, conductive agent and binding agent by mass percentage 94:1:5 they dissolved mix in a solvent, control solid content 50%, be coated in copper foil current collector, vacuum drying, obtained cathode pole piece; LiPF6/EC+DMC+EMC (v/v=1:1:1) electrolyte of the tertiary cathode pole piece then prepared by traditional maturation process, 1mol/L, Celgard2400 barrier film, shell adopt conventional production process to assemble 18650 cylinder cells.The charge-discharge test of cylindrical battery carries out on battery test system, normal temperature condition, and 0.2C constant current charge-discharge, charging/discharging voltage is limited in 2.75 ~ 4.2V.
The performance test data of embodiment 1-4 and comparative example 1 is listed in table 1.
Table 1
As can be seen from Table 1, tin carbon negative pole material prepared by the method for the invention is not more that the negative material of tin carbon has more excellent chemical property, and circulation is more stable.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (9)
1. a preparation method for high-capacity lithium battery negative material, comprises the following steps:
(1) metal dust is mixed with glass putty, carbon source presoma, ball-milling, prepare tin carbon;
(2) step (1) gained tin carbon is sintered under inert gas shielding, obtain tin carbon compound cathode materials;
(3) composite material step (2) obtained is pulverized, is sieved and remove magnetic, obtains the tin carbon compound cathode materials that particle diameter D50 is 1.0 ~ 10 μm.
2. preparation method according to claim 1, is characterized in that, metal dust in step (1): glass putty weight ratio is 1:0.1 ~ 2, carbon source presoma: the weight ratio of metal dust and glass putty total weight is 1:0.01 ~ 0.15.
3. preparation method according to claim 1, is characterized in that, ball-milling described in step (1) adopts dry ball milling or wet ball grinding;
Preferably, the step of described dry ball milling is: the mixed-powder of metal dust and glass putty, carbon source presoma and ball milling pearl are loaded in ball milling cavity, then pass into protective gas, carry out ball milling, obtain tin carbon dust;
Preferably, the step of described wet ball grinding is: mixing metal dust and glass putty, add solvent in carbon source presoma, stir, obtain mixed-powder slurry; Mixed-powder slurry and ball milling pearl are loaded in ball milling cavity and carries out ball milling, dry, obtain tin carbon dust.
4. preparation method according to claim 1, is characterized in that, described in step (1), solvent is preferably organic solvent and/or water;
Preferably, described organic solvent is oxolane, acid amides, 1 kind in alcohol and ketone or the combination of at least 2 kinds, be preferably oxolane, dimethylacetylamide, 1 kind in C1-C6 alcohol and C3-C8 ketone or the combination of at least 2 kinds, more preferably methyl alcohol, ethanol, ethylene glycol, propyl alcohol, isopropyl alcohol, 1, 2-propylene glycol, 1, ammediol, glycerol, n-butanol, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, n-amyl alcohol and 2-hexanol, acetone, methyl ethyl ketone, methyl propyl ketone, 1-METHYLPYRROLIDONE, ethyl propyl ketone, methyl butyl ketone, ethyl n-butyl ketone, 1 kind in methyl amyl ketone and methyl hexyl ketone or the combination of at least 2 kinds.
5. preparation method according to claim 1, it is characterized in that, ball-grinding machine described in step (1) is any one in high-speed stirred mill, planetary ball mill, tube mill, type taper grinder, rod mill and sand mill, is preferably planetary ball mill;
Preferably, described ball milling bead diameter is 0.1 ~ 20mm, and ratio of grinding media to material is 10 ~ 200:1;
Preferably, the rotating speed of described ball milling is 100 ~ 3000rpm, and Ball-milling Time is 5 ~ 120h;
Preferably, the material of described ball milling pearl is stainless steel, agate, pottery, zirconia, aluminium oxide, the one in carbide alloy.
6. preparation method according to claim 1 and 2, it is characterized in that, described in step (1), metal dust is elemental metals and/or metal alloy compound, is preferably tin simple substance, antimony simple substance, iron simple substance, germanium simple substance, aluminium simple substance, magnesium simple substance, zinc simple substance, sows the combination of in simple substance, cadmium simple substance, titanium simple substance, tin pewter, tin ferroalloy, tin titanium alloy, magnesium antimony alloy, aluminium-antimony alloy, almag and tin magnesium alloy a kind or at least 2 kinds;
Preferably, the median particle diameter of described metal dust is 0.1 ~ 100 μm, is preferably 0.5 ~ 50 μm, more preferably 1.0 ~ 15 μm;
Preferably, the median particle diameter of described tin powder is 0.05 ~ 30 μm, more preferably 0.1 ~ 10 μm, is particularly preferably 0.2 ~ 5 μm.
7. preparation method according to claim 1, it is characterized in that, carbon source presoma described in step (1) is the combination of in polymer, carbohydrate, organic acid, pitch and macromolecular material a kind or at least 2 kinds, is preferably the combination of in epoxy resin, phenolic resins, furfural resin, Lauxite, polyvinyl alcohol, polyvinyl chloride, polyethylene glycol, poly(ethylene oxide), Kynoar, acrylic resin and polyacrylonitrile a kind or at least 2 kinds.
8. preparation method according to claim 1, is characterized in that, step (2) described inert gas is the combination of in nitrogen, helium, neon, argon gas, Krypton and xenon a kind or at least 2 kinds.
9. preparation method according to claim 1, is characterized in that, step (2) described sintering temperature is 600 ~ 1200 DEG C;
Preferably, described heating rate 0.5 ~ 10 DEG C/min, temperature retention time is insulation 1 ~ 5h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105449214A (en) * | 2016-01-12 | 2016-03-30 | 广西师范大学 | Lithium ion battery cathode material of which nano particles embedded into carbon nanosheet and preparation method of lithium ion battery cathode material |
| CN106876678A (en) * | 2017-03-30 | 2017-06-20 | 苏州载物强劲新材料科技有限公司 | A kind of metal and its oxide and carbon composite production technology |
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| CN102340001A (en) * | 2011-08-26 | 2012-02-01 | 奇瑞汽车股份有限公司 | Method for preparing high-specific-capacity silicon carbon and tin carbon composite anode material |
| CN104577079A (en) * | 2014-12-22 | 2015-04-29 | 江西正拓新能源科技股份有限公司 | Method for preparing tin-carbon composite negative electrode material |
| CN104617269A (en) * | 2015-01-23 | 2015-05-13 | 深圳市贝特瑞新能源材料股份有限公司 | Silicon alloy composite anode material, preparation method and lithium ion battery |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102340001A (en) * | 2011-08-26 | 2012-02-01 | 奇瑞汽车股份有限公司 | Method for preparing high-specific-capacity silicon carbon and tin carbon composite anode material |
| CN104577079A (en) * | 2014-12-22 | 2015-04-29 | 江西正拓新能源科技股份有限公司 | Method for preparing tin-carbon composite negative electrode material |
| CN104617269A (en) * | 2015-01-23 | 2015-05-13 | 深圳市贝特瑞新能源材料股份有限公司 | Silicon alloy composite anode material, preparation method and lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105449214A (en) * | 2016-01-12 | 2016-03-30 | 广西师范大学 | Lithium ion battery cathode material of which nano particles embedded into carbon nanosheet and preparation method of lithium ion battery cathode material |
| CN106876678A (en) * | 2017-03-30 | 2017-06-20 | 苏州载物强劲新材料科技有限公司 | A kind of metal and its oxide and carbon composite production technology |
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Application publication date: 20151111 |