CN105047867A - Preparation method of high power capacity lithium titanate negative electrode material - Google Patents
Preparation method of high power capacity lithium titanate negative electrode material Download PDFInfo
- Publication number
- CN105047867A CN105047867A CN201510331370.8A CN201510331370A CN105047867A CN 105047867 A CN105047867 A CN 105047867A CN 201510331370 A CN201510331370 A CN 201510331370A CN 105047867 A CN105047867 A CN 105047867A
- Authority
- CN
- China
- Prior art keywords
- preparation
- lithium titanate
- ball
- ball milling
- simple substance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
- H01M4/626—Metals
-
- 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 relates to a preparation method of a high power capacity lithium titanate negative electrode material. According to the negative electrode material, silicon is combined with metal, carbon and lithium titanate to form a multiphase compound system, which not only ensures the high power capacity of the material, but also relieves the volume expansion and shrinkage effect in a charge-discharge process. The silicon and the metal are dispersed in a cracking carbon and lithium titanate system, so the metal has the effect of improving electrical conductivity, and the silicon plays the role of high power capacity, and the cracking carbon and the lithium titanate provide a structure of mechanically supporting and stabilizing material. The lithium titanate negative electrode material of the invention has high compaction density, excellent processing performance, high electrical conductivity, high initial efficiency and excellent cycling stability. The negative electrode material provided by the invention is simple in preparation technology, low in material cost, environmentally friendly, pollution-free 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 titanate anode material, be specifically related to the heterogeneous composite negative pole material of a kind of lithium titanate doping metals tin and agraphitic carbon.
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.Li
4ti
5o
12as a kind of novel ion secondary battery cathode material lithium, compared with other business-like material, advantages such as having good cycle, do not react with electrolyte, security performance is high, charge and discharge platform is steady is one of the most excellent lithium ion battery negative material received much concern in recent years.Compared with carbon negative electrode material, lithium titanate has a lot of advantages, wherein, the deintercalation of lithium ion in lithium titanate is reversible, and lithium ion is embedding or is deviating from the process of lithium titanate, its crystal formation does not change, change in volume is less than 1%, therefore be called as " zero strain material ", can avoid causing structural damage due to the flexible back and forth of electrode material in charge and discharge cycles, thus improve cycle performance and the useful life of electrode, decrease and increase with cycle-index and bring specific capacity significantly to decay, there is the cycle performance more excellent than Carbon anode; But, because lithium titanate is a kind of insulating material, its conductivity is low, thus cause the application in lithium electricity to there is the poor problem of high rate performance, lithium titanate material theoretical specific capacity is 175mAh/g simultaneously, and actual specific capacity is greater than 160mAh/g, has the shortcomings such as gram volume is lower, therefore, it is very necessary for carrying out modification for lithium titanate.
And silicon-based anode has unique advantage and potential, silicium cathode material is in charge and discharge process, the alloys such as Li12Si7, Li13Si4, Li7Si3, Li15Si4, Li22Si5 can be formed with lithium, have high power capacity (Li22Si5, the highest 4200mAh/g), removal lithium embedded voltage low, with electrolyte reactivity is low, security performance is good etc. advantage.But violent volumetric expansion (0 ~ 300%) can occur silicon in removal lithium embedded course of reaction, thus causes destruction and the efflorescence of material structure, causes capacity to be decayed rapidly, cycle performance worsens.In addition, also there is the defects such as conductivity is low, and high rate performance is not good enough, and coulombic efficiency is lower in silicium cathode.
Research show metal dust and silica flour and lithium titanate compound to prepare obtain the performance that negative material can greatly improve lithium titanate anode material.The advantages such as metal itself has good ductility, high conductivity, and mechanical strength is high, therefore select suitable metal and silicon to form silicon-carbon, effectively can overcome the bulk effect of silicon in charge and discharge process, improve the cyclical stability of material, conductivity is also necessarily improved.But current existing silicon-carbon cathode material capacity and head are imitated generally on the low side, and the material consistency of preparation is poor.
Therefore, the lithium titanate composite anode material 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 titanate anode 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 titanate anode material, comprising the following steps:
(1) metal dust is mixed with silica flour, carbon source presoma, titanium dioxide, lithium carbonate, ball-milling, mix mutually to each;
(2) step (1) gained powder is sintered under inert gas shielding, obtain composite negative pole material;
(3) composite material step (2) obtained is pulverized, is sieved and remove magnetic, obtains the lithium titanate anode material that particle diameter D50 is 1.0 ~ 10 μm.
Further, step (1) metal dust: the weight ratio of silica flour is 1:0.1 ~ 2, titanium dioxide: the weight ratio of lithium carbonate is the total weight of 100:38 ~ 40, titanium dioxide and lithium titanate: the total weight of metal dust and silica flour: the weight ratio of carbon source presoma is 1:0.01 ~ 0.1:0.05 ~ 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 silica flour, carbon source presoma, titanium dioxide, lithium carbonate and ball milling pearl are loaded in ball milling cavity, then pass into protective gas, carry out ball milling, obtain silicon-carbon powder.
Preferably, the step of described wet ball grinding is: in metal dust and the silica flour of mixing, carbon source presoma, titanium dioxide, lithium carbonate, add solvent, stirring, obtains mixed-powder slurry; Mixed-powder slurry and ball milling pearl are loaded in ball milling cavity and carries out ball milling, dry, obtain silicon-carbon powder.
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, Antaciron, silicotitanium, magnesium antimony alloy, aluminium-antimony alloy, almag and Si-Mg 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 Si 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 silicon 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 silicon and metal dispersion in cracking carbon system, metal plays the effect improving conductivity, and silicon plays the characteristic of high power capacity, and cracking carbon provides mechanical support, the structure of stabilizing material.Lithium titanate anode material 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 silica flour of 3 μm, by weight Fe:Si=1:2, carry out proportioning, simultaneously in titanium dioxide: the weight ratio of lithium carbonate is the ratio of 100:40, finally in the total weight of titanium oxide and lithium titanate: the total weight of metal dust and silica flour: the weight ratio of carbon source presoma is that the ratio of 1:0.01:0.05 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 lithium titanate anode material 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 silica flour of 0.05 μm, by weight Cu:Si=2:1, carry out proportioning, simultaneously in titanium dioxide: the weight ratio of lithium carbonate is the ratio of 100:39, finally in the total weight of titanium oxide and lithium titanate: the total weight of metal dust and silica flour: the weight ratio of carbon source presoma is that the ratio of 1:0.05:0.1 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 lithium titanate anode material that particle diameter D50 is 1.0-10 μm.
Embodiment 3
(1) by the silicotitanium powder of median particle diameter 0.1 μm and median particle diameter be the silica flour of 30 μm, by weight Ti-Si:Si=2:1, carry out proportioning, simultaneously in titanium dioxide: the weight ratio of lithium carbonate is the ratio of 100:38, finally in the total weight of titanium oxide and lithium titanate: the total weight of metal dust and silica flour: the weight ratio of carbon source presoma is that the ratio of 1:0.1:0.15 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, obtain silicotitanium 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 lithium titanate anode material that particle diameter D50 is 1.0-10 μm.
Embodiment 4
(1) by the Antaciron powder of median particle diameter 10 μm and median particle diameter be the silica flour of 5 μm, by weight Fe-Si:Si=3:1, carry out proportioning
Simultaneously in titanium dioxide: the weight ratio of lithium carbonate is the ratio of 100:40, finally in the total weight of titanium oxide and lithium titanate: the total weight of metal dust and silica flour: the weight ratio of carbon source presoma is that the ratio of 1:0.08:0.12 takes pitch, be scattered in tetrahydrofuran solvent, then dropped in sand mill by slurry 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, obtains Antaciron 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 lithium titanate anode material that particle diameter D50 is 1.0-10 μm.
Comparative example 1
Lithium titanate anode material is prepared according to method substantially the same manner as Example 1, difference is: directly silica flour 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 lithium titanate anode material 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, silicon-carbon cathode material prepared by the method for the invention is not more that the negative material of silicon-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 titanate anode material, comprises the following steps:
(1) metal dust is mixed with silica flour, carbon source presoma, titanium dioxide, lithium carbonate, ball-milling, mix mutually to each;
(2) step (1) gained powder is sintered under inert gas shielding, obtain composite negative pole material;
(3) composite material step (2) obtained is pulverized, is sieved and remove magnetic, obtains the lithium titanate anode material that particle diameter D50 is 1.0 ~ 10 μm.
2. preparation method according to claim 1, it is characterized in that, step (1) metal dust: the weight ratio of silica flour is 1:0.1 ~ 2, titanium dioxide: the weight ratio of lithium carbonate is the total weight of 100:38 ~ 40, titanium dioxide and lithium titanate: the total weight of metal dust and silica flour: the weight ratio of carbon source presoma is 1:0.01 ~ 0.1:0.05 ~ 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 silica flour, carbon source presoma, titanium dioxide, lithium carbonate and ball milling pearl are loaded in ball milling cavity, then pass into protective gas, carry out ball milling, obtain silicon-carbon powder;
Preferably, the step of described wet ball grinding is: in metal dust and the silica flour of mixing, carbon source presoma, titanium dioxide, lithium carbonate, add solvent, stirring, obtains mixed-powder slurry; Mixed-powder slurry and ball milling pearl are loaded in ball milling cavity and carries out ball milling, dry, obtain silicon-carbon powder.
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, Antaciron, silicotitanium, magnesium antimony alloy, aluminium-antimony alloy, almag and Si-Mg 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 Si 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510331370.8A CN105047867A (en) | 2015-06-13 | 2015-06-13 | Preparation method of high power capacity lithium titanate negative electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510331370.8A CN105047867A (en) | 2015-06-13 | 2015-06-13 | Preparation method of high power capacity lithium titanate negative electrode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105047867A true CN105047867A (en) | 2015-11-11 |
Family
ID=54454246
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510331370.8A Pending CN105047867A (en) | 2015-06-13 | 2015-06-13 | Preparation method of high power capacity lithium titanate negative electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105047867A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108365195A (en) * | 2018-02-06 | 2018-08-03 | 深圳市普锐能源科技有限公司 | A kind of lithium ion battery nucleocapsid negative material and preparation method thereof |
| CN108682832A (en) * | 2018-06-11 | 2018-10-19 | 四会市恒星智能科技有限公司 | Lithium battery composite negative pole material and preparation method thereof |
| CN109216695A (en) * | 2018-08-17 | 2019-01-15 | 安徽赛尔新能源科技有限公司 | A method of 1.55V lithium titanate battery capacity is improved by solid phase reaction |
| CN109301236A (en) * | 2018-08-17 | 2019-02-01 | 中北润良新能源汽车(徐州)股份有限公司 | A kind of solid reaction process improving 1.55V lithium titanate battery capacity |
| CN110739454A (en) * | 2019-09-26 | 2020-01-31 | 山东玉皇新能源科技有限公司 | negative electrode materials and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103326009A (en) * | 2013-06-05 | 2013-09-25 | 深圳市斯诺实业发展有限公司永丰县分公司 | Process for preparing high capacity lithium titanate anode 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 |
-
2015
- 2015-06-13 CN CN201510331370.8A patent/CN105047867A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103326009A (en) * | 2013-06-05 | 2013-09-25 | 深圳市斯诺实业发展有限公司永丰县分公司 | Process for preparing high capacity lithium titanate anode 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108365195A (en) * | 2018-02-06 | 2018-08-03 | 深圳市普锐能源科技有限公司 | A kind of lithium ion battery nucleocapsid negative material and preparation method thereof |
| CN108682832A (en) * | 2018-06-11 | 2018-10-19 | 四会市恒星智能科技有限公司 | Lithium battery composite negative pole material and preparation method thereof |
| CN109216695A (en) * | 2018-08-17 | 2019-01-15 | 安徽赛尔新能源科技有限公司 | A method of 1.55V lithium titanate battery capacity is improved by solid phase reaction |
| CN109301236A (en) * | 2018-08-17 | 2019-02-01 | 中北润良新能源汽车(徐州)股份有限公司 | A kind of solid reaction process improving 1.55V lithium titanate battery capacity |
| CN110739454A (en) * | 2019-09-26 | 2020-01-31 | 山东玉皇新能源科技有限公司 | negative electrode materials and preparation method thereof |
| CN110739454B (en) * | 2019-09-26 | 2021-04-02 | 山东玉皇新能源科技有限公司 | Negative electrode material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104900843A (en) | Preparation method of silicon carbon composite anode material | |
| CN104617269B (en) | A kind of silicon alloy composite negative pole material, preparation method and lithium ion battery | |
| CN102931409B (en) | A kind of used as negative electrode of Li-ion battery polyaniline/silicon composite preparation method of nucleocapsid structure | |
| CN105070894B (en) | A kind of lithium ion battery porous silicon-base composite negative pole material, Preparation method and use | |
| CN102983313B (en) | Si-C composite material and preparation method thereof, lithium ion battery | |
| CN104638252B (en) | Silicon composited negative electrode material, preparation method of silicon composited negative electrode material and lithium ion battery | |
| CN107275606B (en) | Carbon-coated spinel lithium manganate nanocomposite and preparation method and application thereof | |
| CN103346324B (en) | Lithium ion battery cathode material and its preparation method | |
| CN102306759B (en) | Silicon monoxide composite cathode material for lithium ion battery, and preparation method thereof | |
| CN103236534B (en) | A kind of preparation method of lithium ion battery silicon oxide/carbon composite negative pole material | |
| CN103545497B (en) | The lithium ion battery cathode material and its preparation method of a kind of bivalve Rotating fields | |
| CN105047867A (en) | Preparation method of high power capacity lithium titanate negative electrode material | |
| CN101908627B (en) | Cathode material of lithium ion secondary battery and preparation method thereof | |
| CN102664262A (en) | Method for preparing lithium ferrous silicate or carbon ferrous silicate cathode material for lithium ion battery | |
| CN104009218B (en) | The preparation method of lithium ion battery negative material tin/lithium titanate composite electrode material | |
| CN109103438A (en) | A kind of lithium ion battery core-shell structure negative electrode material and preparation method thereof | |
| CN108365194A (en) | A kind of preparation method of composite negative electrode material of lithium ion battery | |
| CN103326009A (en) | Process for preparing high capacity lithium titanate anode material | |
| CN110336035B (en) | Tin dioxide/aluminum oxide doped carbon composite material and preparation method thereof | |
| CN102104149A (en) | Lithium iron phosphate composite anode material in lithium-ion battery and preparation method thereof | |
| CN101834287B (en) | Preparation method of anode material of lithium ion battery | |
| CN104916835A (en) | Preparation method of lithium titanate silicon-based composite anode material | |
| CN104701500A (en) | Preparation method of lithium ion battery composite cathode material, cathode material and battery | |
| CN103000863B (en) | Sn-Co/C alloy cathode material of lithium ion battery and preparation method thereof | |
| CN105047868A (en) | Preparation method of high-capacity lithium battery anode material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20151111 |
|
| RJ01 | Rejection of invention patent application after publication |