CN105140480A - Preparation method of high-capacity tin-carbon anode material - Google Patents
Preparation method of high-capacity tin-carbon anode material Download PDFInfo
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- CN105140480A CN105140480A CN201510480854.9A CN201510480854A CN105140480A CN 105140480 A CN105140480 A CN 105140480A CN 201510480854 A CN201510480854 A CN 201510480854A CN 105140480 A CN105140480 A CN 105140480A
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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
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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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- 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
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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
- H01M4/621—Binders
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a preparation method of a high-capacity tin-carbon anode material. According to the method, after a cladding material precursor is subjected to composite treatment, firstly, a certain amount of resin curing agent is added and then is mixed with tin powder evenly; the composite cladding material completely covers the tin powder through atomization and carbonization treatment; secondly, the resin can play a framework support role after being cured; and the phenomenon that breaking treatment on the material is needed due to asphalt melting in the carbonization process and adhesive agglomeration after material carbonization, so that a cladding layer is destroyed is prevented. By the method disclosed by the invention, the mixing uniformity of a plurality of cladding material precursors is ensured; the method is simple in process and low in cost; and industrial production is easy to realize.
Description
Technical field
The present invention relates to field of lithium ion battery, be specially a kind of preparation method of the tin carbon negative pole material for lithium ion battery negative, the composite material that tin carbon negative pole material prepared by the method adopts pitch and resin to be formed carries out coated process to glass putty, to improve its cycle performance.
Background technology
Since nineteen ninety Sony corporation of Japan take the lead in succeeding in developing lithium ion battery and by its commercialization since, lithium ion battery obtains fast development.Nowadays lithium ion battery has been widely used in civilian and military every field.Along with the continuous progress of science and technology, the performance of people to battery proposes more higher requirements: the miniaturization of electronic equipment and individualized development, and the specific energy needing battery to have less volume and Geng Gao exports; Aero-Space energy requirements battery has cycle life, the security performance of better low temperature charge-discharge performance and Geng Gao; Electric automobile needs the battery of Large Copacity, low cost, high stability and security performance.
What current commercial Li-ion battery negative material adopted is graphite-like material with carbon element, and having lower lithium embedding/deintercalation current potential, suitable reversible capacity and aboundresources, the advantage such as cheap, is more satisfactory lithium ion battery negative material.But its theoretical specific capacity only has 372mAh/g, thus limit the further raising of lithium ion battery specific energy, the demand of growing high-energy Portable power source can not be met.Meanwhile, when graphite is as negative material, in first charge-discharge process, form one deck solid electrolyte film (SEI) on its surface.Solid electrolyte film is the formation that react to each other such as electrolyte, negative material and lithium ion, irreversibly consumes lithium ion, is to form the main factor of of irreversible capacity; It two is in the process of Lithium-ion embeding, electrolyte easily and its be embedded in the process of moving out altogether, electrolyte is reduced, the gaseous product generated causes graphite flake layer to peel off, especially containing in the electrolyte of PC, graphite flake layer comes off new for formation interface, causes further SEI to be formed, irreversible capacity increases, and cyclical stability declines simultaneously.And the degree of order of the amorphous carbon formed after resin polymers pyrolysis is low, structure comparison is loose, and lithium ion can embed relatively freely wherein and deviate from and can not produce large impact to its structure.
In addition, tin is a kind of negative material being hopeful to replace material with carbon element most, this is because tin has the height gram specific capacity up to 994mAh/g; And there is the stable discharge platform being similar to graphite.People have carried out this kind of material and have studied widely in recent years, and make some progress.But in reversible lithium storage process, metallic tin volumetric expansion is remarkable, and cause cycle performance to be deteriorated, capacity is decayed rapidly, is therefore difficult to the requirement meeting large-scale production.For this reason, by introducing the nonmetalloids such as carbon, carrying out stable metal tin in the mode of alloying or compound, slowing down the volumetric expansion of tin.Carbon can stop the direct contact between tin particles, suppresses the reunion of tin particles and grows up, playing the effect of resilient coating.These methods can improve the cycle performance of tin really to a certain extent, but the limitation improved, the cycle performance of material still can not be satisfied the demand.
More than show, at present in the coating modification process of material, all only hard charcoal precursor of independent resin-coated class or pitch class soft charcoal precursor.Adopt resinae as clad material, major advantage is resin good fluidity at low temperatures, can not only clad surface, and penetrate into material granule inside easily via micropore, useful to the tap density and electronic conductivity that improve material, can also by heating, introduce the solidification of the method such as catalyst or Ultraviolet radiation, distortion can not be melted in resin pyrolytic process, also obvious expansion can not be produced, but also there are some problems, mainly contain: the Carbon Materials yield obtained by resin pyrolysis is on the low side, enbrittle, in resin pyrolytic process, fugitive constituent is many, specific area is higher, the cohesive force of resin is stronger, be easy to cause coated particle to bond together, the destruction of coating layer is easily caused when pulverizing after heat treatment.These problems above, have impact on the compressibility of the cycle efficieny of resin-coating material, cyclical stability and electrode.Adopt pitch, petroleum tar, coal tar or their mixture as clad material, the asphalt pyrolysis charcoal specific area more coated than From Resin Char is little, to get well with the affinity of material, structure is more firm, but pitch-coating is out of shape because of fusing in heating process, consumption too much also easily causes the mutually bonding of clad material particle, consumption is very few easily cause coated uneven, and be easy in heating process expand, affect the electrical property of material.
Summary of the invention
Technical problem solved by the invention is the preparation method providing a kind of high-capacity Sn carbon negative pole material, to solve the problem proposed in above-mentioned background technology.
A preparation method for high-capacity Sn carbon negative pole material, its preparation process is as follows:
1, the pitch of softening point between 100 DEG C ~ 300 DEG C and the resin of softening point between 50 DEG C ~ 150 DEG C are joined by the weight ratio of 1:1.5 ~ 4 in the kneading still with heating and agitating device, be heated to pitch with the speed of 10 ~ 40 DEG C/min and resin is all fused into liquid;
2, then add the curing agent accounting for amount of resin 2% ~ 5%, under inert gas shielding, be constantly stirred to various component and mix;
3, according to resin and pitch total weight: glass putty: the weight of dispersion solvent is that the ratio of 1:0.05 ~ 0.15:0.2 ~ 0.6 takes glass putty and dispersion solvent, glass putty is joined in dispersion solvent, and ultrasonic disperse evenly after join in step 2 mixing material, be stirred to each component and mix;
4, cooled by atomising device atomization by the liquid mixed in step 3, then collect the powder of atomization gained and carry out classification process, obtain the powder of average grain diameter between 5 ~ 30 μm, now resin completes solidification;
5, by the powder that obtains in step 4 under the protection of inert gas, be warming up to 700 ~ 900 DEG C with the speed of 1 ~ 10 DEG C/min, then be incubated 1 ~ 5h, Temperature fall, after cooling, namely obtain high-capacity Sn carbon negative pole material.
In the present invention, the pitch described in step 1 comprises one or more the mixture in coal tar pitch, petroleum asphalt, modified coal tar pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier, and softening point is more than 100 DEG C.
In the present invention, the resin described in step 1 is thermoplastic resin, comprises one or more the mixture in furane resins, Lauxite, ethyl-amine resin, phenolic resins, epoxy resin and polyformaldehyde methacrylate resin.
In the present invention, the time of the stirring described in step 1 is 80 ~ 130min, and the final temperature of heating is higher 30 ~ 40 DEG C than the most high softening-point of component medium pitch and resin.
In the present invention, the curing agent described in step 2 is hexamethylenetetramine, diethyl amino propylamine, trimethylhexamethylenediamine, two base triamine, one or more the mixture had in the thermosetting resin of solidification.
In the present invention, the average grain diameter≤100nm of the glass putty described in step 3.
In the present invention, the dispersion solvent described in step 3 is ethanol, isopropyl alcohol, carbon disulfide, toluene, dimethylbenzene or with the one in the distilled water of decentralized medium.
In the present invention, what in step 4, atomization adopted is utilize the one in the atomising device of ultrasonic atomizatio, centrifugal atomizing, the work of high-pressure atomization principle.
In the present invention, what in step 4, classification process adopted is carries out cyclonic separation to powder, a kind of or both combination of sieving in process.
In above-mentioned preparation method, described inert gas is one or both the gaseous mixture in nitrogen, argon gas, helium.
With prior art, the invention has the beneficial effects as follows:
1, the innovative point that the present invention is the most outstanding is by after clad material presoma Combined Processing, more coated glass putty; Ensure that the uniformity that multiple clad material presoma mixes, simultaneously without any need for solvent, environmentally friendly; In addition, technique is simple, and cost is low, easy suitability for industrialized production;
2, the present invention is by adding a certain amount of resin curing agent to composite material, resin is after overcuring, skeletal support effect can be played, prevent carbonisation medium pitch from melting and powder occurs that adhesion is lumpd after causing carbonization, and need to carry out to it phenomenon that break process causes material coating layer to destroy;
3, the amorphous carbon that formed after high temperature cabonization of resin, to electrolyte, there is stronger corrosion resistance ability, simultaneously, the interlamellar spacing of amorphous carbon is larger, lithium ion can pass in and out fast, meet the requirement of lithium ion battery high power charging-discharging, the bulk effect that glass putty produces when discharge and recharge can be cushioned in the hole secondly formed after resin carbonation and space, ensures the overall stability of material;
4, the present invention and the hard charcoal precursor of independent resin-coated class or pitch class soft charcoal precursor as compared with clad material, there is obvious superiority, together with asphalt carbon and resin carbon are pinned at mutually, complementary not enough, effectively can improve the intensity of coating layer, ensure the cyclical stability of tin carbon composite.
Embodiment
Reaching object to make technological means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, setting forth the present invention further below.
Embodiment 1
By mesophase pitch (softening point 250 DEG C) and phenolic resins (softening point 110 DEG C) according to 1:3(3.5Kg with 10.5Kg) ratio together with join in the kneading still of 20L, start intensification and be heated to 300 DEG C, after pitch and resin are all fused into liquid, then add the curing agent-hexamethylenetetramine of 0.315Kg according to the ratio of weight resin 3%, be constantly stirred to each component and mix, according to pitch and total resin weight: glass putty: the weight of dispersion solvent is the alcoholic solution that the ratio of 1:0.1:0.3 takes glass putty that 1.4Kg average grain diameter is 50nm and 5.2 kilograms, after glass putty is joined alcoholic solution, disperseed by ultrasonic unit, after dispersion all has, add the pitch mixed, resin, in the mixing material of curing agent, cooling is sprayed by ultrasonic atomizing device after stirring 120min, and by the powder of cyclone collection average grain diameter between 5 ~ 30 μm, then 850 DEG C are heated under nitrogen protection, be incubated 3 hours, then room temperature is cooled to, finally obtain high-capacity Sn carbon battery negative material.
The performance of inspection embodiment 1 lithium ion battery negative material, test by half-cell method of testing, lithium ion battery negative material with prepared by embodiment 1: acetylene black: PVDF(Kynoar) weight ratio is 93:3:4, add appropriate NMP(N-methyl pyrrolidone) furnishing pulpous state, coat on Copper Foil, within 8 hours, make negative plate through vacuum 110 DEG C of dryings; Be to electrode with metal lithium sheet, electrolyte is the LiPF6/EC+DEC+DMC=1:1:1 of 1mol/L, and microporous polypropylene membrane is barrier film, is assembled into battery.Charging/discharging voltage is 0 ~ 2.0V, and charge-discharge velocity is 0.2C, and carry out testing to battery performance, the discharge capacity first of this electrode material reaches 445mAh/g, and the capacity after 100 circulations still has 412mAh/g, and conservation rate is 92.6%.
Embodiment 2
By mesophase pitch (softening point 250 DEG C) and phenolic resins (softening point 110 DEG C) according to 1:4(3Kg with 12Kg) ratio together with join in the kneading still of 20L, start intensification and be heated to 300 DEG C, after pitch and resin are all fused into liquid, then add the curing agent-hexamethylenetetramine of 0.48Kg according to the ratio of weight resin 4%, be constantly stirred to each component and mix, according to pitch and total resin weight: glass putty: the weight of dispersion solvent is the xylene solution that the ratio of 1:0.09:0.27 takes glass putty that 1.35Kg average grain diameter is 50nm and 4.05 kilograms, after glass putty is joined xylene solution, disperseed by ultrasonic unit, after dispersion all has, add the pitch mixed, resin, in the mixing material of curing agent, cooling is sprayed by centrifugal atomization apparatus after stirring 150min, and by the powder of cyclone collection average grain diameter between 5 ~ 30 μm, then 850 DEG C are heated under nitrogen protection, be incubated 3 hours, then room temperature is cooled to, finally obtain high-capacity Sn carbon battery negative material.
The performance of inspection embodiment 2 lithium ion battery negative material, adopt the identical detection method of embodiment 1 to detect, the discharge capacity first of this motor material reaches 416mAh/g, and the capacity after 100 circulations still has 379mAh/g, and conservation rate is 91.1%.
More than show and describe general principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (9)
1. a preparation method for high-capacity Sn carbon negative pole material, its preparation process is as follows:
(1) pitch of softening point between 100 DEG C ~ 300 DEG C and the resin of softening point between 50 DEG C ~ 150 DEG C are joined by the weight ratio of 1:1.5 ~ 4 in the kneading still with heating and agitating device, be heated to pitch with the speed of 10 ~ 40 DEG C/min and resin is all fused into liquid;
(2) then add the curing agent accounting for amount of resin 2% ~ 5%, under inert gas shielding, be constantly stirred to various component and mix;
(3) according to resin and pitch total weight: glass putty: the weight of dispersion solvent is that the ratio of 1:0.05 ~ 0.15:0.2 ~ 0.6 takes glass putty and dispersion solvent, glass putty is joined in dispersion solvent, and ultrasonic disperse evenly after join in step 2 mixing material, be stirred to each component and mix;
(4) cooled by atomising device atomization by the liquid mixed in step (3), then collect the powder of atomization gained and carry out classification process, obtain average grain diameter between the powder between 5 ~ 30 μm, now resin completes solidification;
(5) by the powder that obtains in step (4) under the protection of inert gas, be warming up to 700 ~ 900 DEG C with the speed of 1 ~ 10 DEG C/min, then be incubated 1 ~ 5h, Temperature fall, after cooling, namely obtain high-capacity Sn carbon negative pole material.
2. the preparation method of a high-capacity Sn carbon negative pole material, it is characterized in that: the pitch described in step (1) comprises one or more the mixture in coal tar pitch, petroleum asphalt, modified coal tar pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier, and softening point is more than 100 DEG C.
3. the preparation method of a high-capacity Sn carbon negative pole material, it is characterized in that: the resin described in step (1) is thermoplastic resin, comprise one or more the mixture in furane resins, Lauxite, ethyl-amine resin, phenolic resins, epoxy resin and polyformaldehyde methacrylate resin.
4. a preparation method for high-capacity Sn carbon negative pole material, is characterized in that: the time of the stirring described in step (1) is 80 ~ 130min, and the final temperature of heating is higher 30 ~ 40 DEG C than the most high softening-point of component medium pitch and resin.
5. a preparation method for high-capacity Sn carbon negative pole material, is characterized in that: the curing agent described in step (2) is hexamethylenetetramine, diethyl amino propylamine, trimethylhexamethylenediamine, two base triamine, one or more the mixture had in the thermosetting resin of solidification.
6. a preparation method for high-capacity Sn carbon negative pole material, is characterized in that: the average grain diameter≤100nm of the glass putty described in step (3).
7. a preparation method for high-capacity Sn carbon negative pole material, is characterized in that: the dispersion solvent described in step (3) is ethanol, isopropyl alcohol, carbon disulfide, toluene, dimethylbenzene or with the one in the distilled water of decentralized medium.
8. a preparation method for high-capacity Sn carbon negative pole material, is characterized in that: what in step (4), atomization adopted is utilize the one in the atomising device of ultrasonic atomizatio, centrifugal atomizing, the work of high-pressure atomization principle.
9. a preparation method for high-capacity Sn carbon negative pole material, is characterized in that: what classification process adopted in step (4) is carries out cyclonic separation to powder, sieve a kind of in process or both combinations.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510480854.9A CN105140480A (en) | 2015-08-07 | 2015-08-07 | Preparation method of high-capacity tin-carbon anode material |
| PCT/CN2016/086703 WO2017024898A1 (en) | 2015-08-07 | 2016-06-22 | Preparation method for high capacity tin-carbon negative electrode material |
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| CN201510480854.9A CN105140480A (en) | 2015-08-07 | 2015-08-07 | Preparation method of high-capacity tin-carbon anode material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017024898A1 (en) * | 2015-08-07 | 2017-02-16 | 田东 | Preparation method for high capacity tin-carbon negative electrode material |
| CN117711833A (en) * | 2024-02-01 | 2024-03-15 | 山西三元炭素有限责任公司 | Manufacturing method of super-capacitor carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113956053A (en) * | 2021-09-29 | 2022-01-21 | 大同新成新材料股份有限公司 | Kneading preparation process of isostatic pressing graphite |
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| CN101017893A (en) * | 2006-02-08 | 2007-08-15 | 深圳市比克电池有限公司 | A tin carbon compound electrode material for lithium ion battery cathode and preparing method |
| CN101202340A (en) * | 2007-12-07 | 2008-06-18 | 广西师范大学 | Tin carbon nanometer compound material for lithium ion battery and method for making same |
| CN103594691A (en) * | 2012-12-14 | 2014-02-19 | 深圳市斯诺实业发展有限公司永丰县分公司 | Preparation method of high-volume silicon-carbon negative electrode material |
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| CN100338796C (en) * | 2004-05-26 | 2007-09-19 | 中国科学院金属研究所 | Process for modifying negative electrode material of lithium ion cell |
| CN102030326B (en) * | 2010-11-22 | 2012-03-21 | 中科恒达石墨股份有限公司 | Preparation method of graphite cathode material |
| CN105140480A (en) * | 2015-08-07 | 2015-12-09 | 田东 | Preparation method of high-capacity tin-carbon anode material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017893A (en) * | 2006-02-08 | 2007-08-15 | 深圳市比克电池有限公司 | A tin carbon compound electrode material for lithium ion battery cathode and preparing method |
| CN101202340A (en) * | 2007-12-07 | 2008-06-18 | 广西师范大学 | Tin carbon nanometer compound material for lithium ion battery and method for making same |
| CN103594691A (en) * | 2012-12-14 | 2014-02-19 | 深圳市斯诺实业发展有限公司永丰县分公司 | Preparation method of high-volume silicon-carbon negative electrode material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017024898A1 (en) * | 2015-08-07 | 2017-02-16 | 田东 | Preparation method for high capacity tin-carbon negative electrode material |
| CN117711833A (en) * | 2024-02-01 | 2024-03-15 | 山西三元炭素有限责任公司 | Manufacturing method of super-capacitor carbon |
| CN117711833B (en) * | 2024-02-01 | 2024-04-30 | 山西三元炭素有限责任公司 | Manufacturing method of super-capacitor carbon |
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Application publication date: 20151209 |