CN104966821A - Preparation method for graphite-doped negative electrode material - Google Patents
Preparation method for graphite-doped negative electrode material Download PDFInfo
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- CN104966821A CN104966821A CN201510305058.1A CN201510305058A CN104966821A CN 104966821 A CN104966821 A CN 104966821A CN 201510305058 A CN201510305058 A CN 201510305058A CN 104966821 A CN104966821 A CN 104966821A
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- graphite
- modification liquid
- cathode material
- ball milling
- negative electrode
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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
- 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
- H01M4/387—Tin or alloys based on tin
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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
- H01M4/58—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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- 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 discloses a preparation method for a graphite-doped negative electrode material. The preparation method comprises the following steps: (1) preparing a graphite negative electrode material; (2) preparing a modification solution; and (3) modifying the graphite negative electrode material. According to the modified graphite negative electrode material prepared in the invention, tin and nickel are compounded on a graphite material so as to enable the graphite material to have much higher specific capacity compared with a pure carbon material; and the graphite material is modified, so expansion of the material when used as a negative electrode is effectively inhibited, and cycle stability of the material is improved; thus, the negative electrode material has high energy density and good cycle stability when used for a lithium ion battery.
Description
Technical field
The present invention relates to a kind of preparation method of doped graphite negative material, be specifically related to a kind of preparation method being mixed with the graphite cathode material of metallic nickel and metallic tin.
Background technology
It is little that lithium ion battery has volume, and still maintain the advantages such as high reserve of electricity and high discharge capacity under long-time use, is thus used in widely in the equipment such as communication, electronics." graphite material ", based on its fail safe and cost viewpoint, becomes the raw material main flow of lithium ion battery negative material already; And the various lithium ion battery negative material that is raw material with graphite material, and relevant preparation method, be also developed gradually.
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.
Due to the limitation of graphite cathode material, therefore very necessary to the exploitation of Novel anode material.Novel negative material has alloy material, silicon-base oxide material etc.Although alloy material can provide higher reversible capacity, its cycle performance is not ideal enough.Although silicon-base 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.Research finds, during negative material as lithium ion battery of metallic nickel and oxide thereof, have higher specific capacity, the ductility of metallic nickel tool is good in addition, and electrode material expansion rate in the embedding de-process of lithium can be made greatly to reduce.But the conductance of nickel oxide is low, have impact on the charge-discharge performance of battery.
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.
For solving the problem, usually adopt the method for composite material, tin-based material and graphite are carried out compound, and the tin/graphite composite material of gained possesses the long circulating performance of graphite and the high power capacity feature of tin, and this does not also have similar report in industry.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of preparation method of graphite cathode material, using negative material prepared by the method, when having high power capacity, material self has high conductivity, also has good electrochemical cycle stability simultaneously.
1) graphite cathode material is prepared
Prepare burden by following weight portion:
Graphite 35-45
Nickel powder 20-25
Glass putty 15-20
Pitch 10-15
Glass putty and nickel powder are added suitable alcohols high-energy mechanical ball milling 12-16h according to mass ratio, the alloy powder obtained by above-mentioned mechanical ball milling mixes with graphite and adds alcohol and continues high-energy mechanical ball milling 8-10h, take out above-mentioned tin-nickel alloy graphite composite material suction filtration and remove alcohol, then baking oven vacuumize 6-10h is put into, then under argon shield, carry out high-temperature heat treatment, programming rate is 2-5 DEG C/min, is warmed up to 700-900 DEG C, constant temperature 4-6h, then drops to normal temperature naturally;
The tin-nickel alloy graphite composite material of preparation is taken out after cooling, add pitch, then add alcohol and continue high-energy mechanical ball milling, ball milling method is the grinding of speed change alternate intermittent, that is: operate 2min, 1000-1200rpm of 600-800rpm to operate 3min, after circulation 4-5 time, interval 10min, accumulative milling time 4-5h; Take out the dry 10-15h of suction filtration final vacuum, then high-temperature heat treatment is carried out under nitrogen protection, programming rate is 2-5 DEG C/min, after being warming up to 400-600 DEG C, constant temperature 4-7h, then continue to be warmed up to 900-1200 DEG C with 4-8 DEG C/min, constant temperature 5-8h, finally naturally cool to normal temperature and obtain graphite cathode material;
2) modification liquid is prepared
Be that modification liquid prepared by solvent with deionized water, this modification liquid of every 1L has following component: modification liquid is dissolved with the sub-nickel of fluoboric acid of 0.05-0.2mol, the thiocarbamide of 0.1-0.5mol, the stannous sulfate of 0.15-0.3mol, the potassium hydroxide of 0.2-0.4mol, and the potassium oxalate of 0.1-0.15mol;
3) modification is carried out to graphite cathode material
Above-mentioned graphite cathode material is immersed in above-mentioned modification liquid, in the modification liquid of every liter, the incorporation of this graphite cathode material is 100-250g, after mixing mixing, carries out ultrasonic process, this ultrasonic process carries out at 65-95 DEG C, ultrasonic time is 10-15min, after sonication techniques, is taken out by modified graphite cathode material, under vacuo, carry out drying in 50-120 DEG C temperature range, obtain product.
Modified graphite cathode material prepared by the present invention, compound tin and nickel on graphite material, make material possess higher specific capacity far above pure material with carbon element, material carried out modification simultaneously, effectively inhibit this material as expansion during negative pole, improve the cyclical stability of material.Therefore make this negative material when for lithium ion battery, there is higher energy density and good cyclical stability.
Embodiment
Embodiment one
Prepare burden by following weight portion:
Graphite 35
Nickel powder 20
Glass putty 15
Pitch 10.
Glass putty and nickel powder are added suitable alcohols high-energy mechanical ball milling 12h according to mass ratio, the alloy powder obtained by above-mentioned mechanical ball milling mixes with graphite and adds alcohol and continues high-energy mechanical ball milling 8h, take out above-mentioned tin-nickel alloy graphite composite material suction filtration and remove alcohol, then baking oven vacuumize 6h is put into, then under argon shield, carry out high-temperature heat treatment, programming rate is 2 DEG C/min, is warmed up to 700 DEG C, constant temperature 6h, then drops to normal temperature naturally;
Take out the tin-nickel alloy graphite composite material of preparation after cooling, add pitch, then add alcohol and continue high-energy mechanical ball milling, ball milling method is the grinding of speed change alternate intermittent, that is: 600rpm running 2min, 1000rpm running 3min, circulate after 5 times, interval 10min, accumulative milling time 5h; Take out the dry 10h of suction filtration final vacuum, then carry out high-temperature heat treatment under nitrogen protection, programming rate is 2 DEG C/min; after being warming up to 400 DEG C, constant temperature 7h, then continues to be warmed up to 900 DEG C with 4 DEG C/min; constant temperature 8h, finally naturally cools to normal temperature and obtains graphite cathode material.
Be that modification liquid prepared by solvent with deionized water, this modification liquid of every 1L has following component: modification liquid is dissolved with the sub-nickel of fluoboric acid of 0.05mol, the thiocarbamide of 0.1mol, the stannous sulfate of 0.15mol, the potassium hydroxide of 0.2mol, and the potassium oxalate of 0.1mol.
Above-mentioned graphite cathode material is immersed in above-mentioned modification liquid, in the modification liquid of every liter, should in the modification liquid of every liter, the incorporation of this graphite cathode material is 100g, after mixing mixing, carry out ultrasonic process, this ultrasonic process carries out at 65 DEG C, and ultrasonic time is 15min, after sonication techniques, by modified graphite cathode material take out, under vacuo, 50 DEG C carry out drying, obtain product.
Embodiment two
Prepare burden by following weight portion:
Graphite 45
Nickel powder 25
Glass putty 20
Pitch 15.
Glass putty and nickel powder are added suitable alcohols high-energy mechanical ball milling 16h according to mass ratio, the alloy powder obtained by above-mentioned mechanical ball milling mixes with graphite and adds alcohol and continues high-energy mechanical ball milling 10h, take out above-mentioned tin-nickel alloy graphite composite material suction filtration and remove alcohol, then baking oven vacuumize 10h is put into, then under argon shield, carry out high-temperature heat treatment, programming rate is 5 DEG C/min, is warmed up to 900 DEG C, constant temperature 4h, then drops to normal temperature naturally;
Take out the tin-nickel alloy graphite composite material of preparation after cooling, add pitch, then add alcohol and continue high-energy mechanical ball milling, ball milling method is the grinding of speed change alternate intermittent, that is: 800rpm running 2min, 1200rpm running 3min, circulate after 4 times, interval 10min, accumulative milling time 4h; Take out the dry 15h of suction filtration final vacuum, then carry out high-temperature heat treatment under nitrogen protection, programming rate is 5 DEG C/min; after being warming up to 600 DEG C, constant temperature 4h, then continues to be warmed up to 1200 DEG C with 8 DEG C/min; constant temperature 5h, finally naturally cools to normal temperature and obtains graphite cathode material.
Be that modification liquid prepared by solvent with deionized water, this modification liquid of every 1L has following component: modification liquid is dissolved with the sub-nickel of fluoboric acid of 0.2mol, the thiocarbamide of 0.5mol, the stannous sulfate of 0.3mol, the potassium hydroxide of 0.4mol, and the potassium oxalate of 0.15mol.
Above-mentioned graphite cathode material is immersed in above-mentioned modification liquid, in the modification liquid of every liter, should in the modification liquid of every liter, the incorporation of this graphite cathode material is 250g, after mixing mixing, carry out ultrasonic process, this ultrasonic process carries out at 95 DEG C, and ultrasonic time is 10min, after sonication techniques, by modified graphite cathode material take out, under vacuo, 120 DEG C carry out drying, obtain product.
Comparative example
Be 400 orders by granularity, purity be 99.5% glass putty and granularity be 300 orders, purity is that the nickel powder of 99.5% is according to than 1: 1 mixing, ball-milling treatment is carried out in planetary ball mill, rotational speed of ball-mill is 400 revs/min, and ball material weight ratio is set to 300: 1, and the time is 30 hours.Then heat-treat under helium protection in high temperature furnace, treatment temperature is 400 DEG C, and the time is 10 hours, obtains alloy material.Preparation 200mL ethanol water; the volume ratio of ethanol and water is 1: 4; add 40g sucrose to be stirred to and to dissolve completely; add the alloy material 35 grams of tin obtained above and nickel in the solution; stir, 100 DEG C are dried 10 hours in an oven, 900 DEG C of heat treatment 10 hours under helium protection in high temperature furnace after taking-up; then be 300: 1 in ball material weight ratio, rotating speed is the planetary ball mill ball-milling treatment 15 hours of 200 revs/min.45 grams of composite material of lithium ion battery cathodes are obtained after crossing 300 mesh sieves.
Above-described embodiment one, two and comparative example products therefrom are made same size experimental cell pole piece.Be to electrode with lithium sheet, electrolyte is EC/DMC (Vol 1:1) solution of the LiPF6 of 1M, and barrier film is polyethylene, polypropylene composite materials barrier film, and cut-off charging/discharging voltage is 0V-1.5V.At probe temperature is 25 DEG C, carry out electric performance test, after tested this embodiment one with two material compared with the product of comparative example, specific capacity improve more than 20%, bring up to more than 1.5 times useful life.
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 (1)
1. a preparation method for doped graphite negative material, comprises the steps:
(1) graphite cathode material is prepared
Prepare burden by following weight portion:
Graphite 35-45
Nickel powder 20-25
Glass putty 15-20
Pitch 10-15
Glass putty and nickel powder are added suitable alcohols high-energy mechanical ball milling 12-16h according to mass ratio, the alloy powder obtained by above-mentioned mechanical ball milling mixes with graphite and adds alcohol and continues high-energy mechanical ball milling 8-10h, take out above-mentioned tin-nickel alloy graphite composite material suction filtration and remove alcohol, then baking oven vacuumize 6-10h is put into, then under argon shield, carry out high-temperature heat treatment, programming rate is 2-5 DEG C/min, is warmed up to 700-900 DEG C, constant temperature 4-6h, then drops to normal temperature naturally;
The tin-nickel alloy graphite composite material of preparation is taken out after cooling, add pitch, then add alcohol and continue high-energy mechanical ball milling, ball milling method is the grinding of speed change alternate intermittent, that is: operate 2min, 1000-1200rpm of 600-800rpm to operate 3min, after circulation 4-5 time, interval 10min, accumulative milling time 4-5h;
Take out the dry 10-15h of suction filtration final vacuum, then high-temperature heat treatment is carried out under nitrogen protection, programming rate is 2-5 DEG C/min, after being warming up to 400-600 DEG C, constant temperature 4-7h, then continue to be warmed up to 900-1200 DEG C with 4-8 DEG C/min, constant temperature 5-8h, finally naturally cool to normal temperature and obtain graphite cathode material;
(2) modification liquid is prepared
Be that modification liquid prepared by solvent with deionized water, this modification liquid of every 1L has following component: modification liquid is dissolved with the sub-nickel of fluoboric acid of 0.05-0.2mol, the thiocarbamide of 0.1-0.5mol, the stannous sulfate of 0.15-0.3mol, the potassium hydroxide of 0.2-0.4mol, and the potassium oxalate of 0.1-0.15mol;
(3) modification is carried out to graphite cathode material
Above-mentioned graphite cathode material is immersed in above-mentioned modification liquid, in the modification liquid of every liter, should in the modification liquid of every liter, the incorporation of this graphite cathode material is 100-250g, after mixing mixing, carry out ultrasonic process, this ultrasonic process carries out at 65-95 DEG C, and ultrasonic time is 10-15min, after sonication techniques, modified graphite cathode material is taken out, under vacuo, carries out drying in 50-120 DEG C temperature range, obtain product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108963258A (en) * | 2018-07-11 | 2018-12-07 | 大同新成新材料股份有限公司 | A kind of porous carbon-based negative electrode material of surface low-level oxidation and preparation method thereof |
| CN109148866A (en) * | 2018-09-10 | 2019-01-04 | 澳洋集团有限公司 | A kind of preparation method of graphene doped alloys lithium cell cathode material |
| CN109546099A (en) * | 2018-10-16 | 2019-03-29 | 中航锂电（洛阳）有限公司 | A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery |
| CN113636546A (en) * | 2021-07-19 | 2021-11-12 | 西安交通大学 | Composite graphite material and preparation method and application thereof |
| CN114122392A (en) * | 2021-11-10 | 2022-03-01 | 云南中晟新材料有限责任公司 | High-capacity quick-charging graphite composite material and preparation method thereof |
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| CN102054967A (en) * | 2009-10-28 | 2011-05-11 | 深圳市贝特瑞新能源材料股份有限公司 | Tin-nickel-carbon alloy composite material for lithium ion battery and preparation method thereof |
| CN104505503A (en) * | 2015-01-09 | 2015-04-08 | 高淑萍 | Method for preparing modified carbon-based negative electrode material |
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2015
- 2015-06-05 CN CN201510305058.1A patent/CN104966821A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102054967A (en) * | 2009-10-28 | 2011-05-11 | 深圳市贝特瑞新能源材料股份有限公司 | Tin-nickel-carbon alloy composite material for lithium ion battery and preparation method thereof |
| CN104505503A (en) * | 2015-01-09 | 2015-04-08 | 高淑萍 | Method for preparing modified carbon-based negative electrode material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108963258A (en) * | 2018-07-11 | 2018-12-07 | 大同新成新材料股份有限公司 | A kind of porous carbon-based negative electrode material of surface low-level oxidation and preparation method thereof |
| CN109148866A (en) * | 2018-09-10 | 2019-01-04 | 澳洋集团有限公司 | A kind of preparation method of graphene doped alloys lithium cell cathode material |
| CN109546099A (en) * | 2018-10-16 | 2019-03-29 | 中航锂电（洛阳）有限公司 | A kind of composite cathode material of silicon/carbon/graphite and preparation method thereof, lithium ion battery |
| CN109546099B (en) * | 2018-10-16 | 2021-08-31 | 中航锂电（洛阳）有限公司 | Graphite composite negative electrode material, preparation method thereof and lithium ion battery |
| CN113636546A (en) * | 2021-07-19 | 2021-11-12 | 西安交通大学 | Composite graphite material and preparation method and application thereof |
| CN114122392A (en) * | 2021-11-10 | 2022-03-01 | 云南中晟新材料有限责任公司 | High-capacity quick-charging graphite composite material and preparation method thereof |
| CN114122392B (en) * | 2021-11-10 | 2024-03-29 | 云南中晟新材料有限责任公司 | High-capacity quick-charging graphite composite material and preparation method thereof |
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