CN103618086B - A kind of lithium ion battery anode material - Google Patents
A kind of lithium ion battery anode material Download PDFInfo
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- CN103618086B CN103618086B CN201310588814.7A CN201310588814A CN103618086B CN 103618086 B CN103618086 B CN 103618086B CN 201310588814 A CN201310588814 A CN 201310588814A CN 103618086 B CN103618086 B CN 103618086B
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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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- 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
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 belongs to technical field of lithium ion, particularly relate to a kind of lithium ion battery anode material, described anode material comprises graphite and silica-base material, the Surface coating of silica-base material has amorphous carbon, the median particle diameter of graphite is 2-10 μm, the median particle diameter of silica-base material is 2-10 μm, and the quality of silica-base material accounts for the 10-30% of described anode material gross mass, and the quality of amorphous carbon accounts for the 5-20% of described anode material gross mass.Relative to prior art, the present invention is by the Surface coating amorphous carbon at silica-base material, effectively can suppress the volumetric expansion of silica-base material, thus eliminate because silica-base material expands the cell deformation problem caused, inhibit activities material comes off from collector simultaneously, improves the cycle performance of battery; Silica-base material is mixed with graphite, greatly can improve again the gram volume of anode material, its gram volume apparently higher than the gram volume of graphite, cycle performance then comparatively silica-base material greatly improve.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to a kind of lithium ion battery anode material.
Background technology
Along with the variation of consumer electronics product function, lithium ion battery, as the supply energy of electronic product, starts in its capacity and useful life to be subject to showing great attention to of people.And along with the miniaturization of all kinds of consumer electronics product and microminiaturization, its space leaving lithium ion battery for is more and more limited, for this reason, just need the capacity improving battery, be the energy density improving battery more precisely, just seem particularly important.Improve the energy density of battery, the gram volume of the improvement on battery structure, raising positive electrode and the gram volume of raising negative material are all considerable directions, but the improvement on battery structure, as reduced the thickness of packaging film or processing lug, the energy density of battery can only be improved slightly; And the gram volume of positive electrode improves limited, the gram volume of negative material promotes then also has very large space.
Now widely used negative material mainly comprises native graphite, Delanium, carbonaceous mesophase spherules and their mixture.As everyone knows, the theoretical gram volume of graphite is 372mAh/g, and it cannot meet the energy density requirement of current high-end electronic product.Therefore the negative material of researcher to high-energy-density has done extensive and deep research, wherein researcher generally acknowledge most promising be exactly silica-base material.The theoretical gram volume of silicon up to 4200mAh/g, far above the theoretical gram volume 372mAh/g of graphite.But silicon also has very large shortcoming: the volumetric expansion after the embedding lithium of silicon can reach more than 300%-400%.Its violent expansion easily causes active material and collector come off and electrode life is declined rapidly.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, and a kind of energy density that effectively can improve battery is provided, effectively can solve again the lithium ion battery anode material of the expansion issues of silica-base material.
In order to achieve the above object, the present invention adopts following technical scheme: a kind of lithium ion battery anode material, described anode material comprises graphite and silica-base material, the Surface coating of described silica-base material has amorphous carbon, the median particle diameter of described graphite is 2-10 μm, the median particle diameter of silica-base material is 2-10 μm, and the quality of described silica-base material accounts for the 10-30% of described anode material gross mass, and the quality of described amorphous carbon accounts for the 5-20% of described anode material gross mass.
At the Surface coating amorphous carbon of silica-base material, effectively can suppress the volumetric expansion of silica-base material, and the mixing of silica-base material and graphite, then can the gram volume of anode material, improve the energy density of battery.In the present invention, the median particle diameter of graphite and silica-base material is all less, to enable graphite and silica-base material Homogeneous phase mixing, to cushion the volumetric expansion of silica-base material further, the content of silica-base material is in the scope of 10-30%, not only can meet the demand of electronic product to energy density and high power capacity, and the expansion of anode material is less, thus greatly extended in the useful life of battery.
One as lithium ion battery anode material of the present invention is improved, and the quality of described silica-base material accounts for the 15-25% of described anode material gross mass, and this is preferred scope.
One as lithium ion battery anode material of the present invention is improved, and the quality of described silica-base material accounts for 20% of described anode material gross mass, and this preferably selects.
One as lithium ion battery anode material of the present invention is improved, and the quality of described amorphous carbon accounts for the 10-15% of described anode material gross mass, and this is preferred scope.
One as lithium ion battery anode material of the present invention is improved, and the quality of described amorphous carbon accounts for 12% of described anode material gross mass, and this preferably selects.
One as lithium ion battery anode material of the present invention is improved, and described silica-base material is at least one in silicon, silicon monoxide and silicon dioxide.
One as lithium ion battery anode material of the present invention is improved, and described graphite is at least one in native graphite, Delanium and carbonaceous mesophase spherules.
One as lithium ion battery anode material of the present invention is improved, and the preparation method of described anode material comprises the following steps:
The first step, silica-base material is placed in high mixer, stir with the rotating speed of 100-450r/min, then organic carbon presoma is made solution, this solution is added in sprayer, solution is sprayed to silica-base material powder surface with the form of the drop of 0.5-3 μm, after sprinkling completes, dry at continuing to stir 30min-3h, 110-150 DEG C with the rotating speed of 100-450r/min, obtain coated silica-base material;
Second step, coated silica-base material graphite and the first step obtained and pitch add high mixer, obtain mixture after stirring, and described pitch accounts for the 1-8% of described mixture;
3rd step, the mixture obtained by second step adds in high temperature furnace, is warming up to 1000-1700 DEG C under inert atmosphere with the speed of 10-50 DEG C/min, high temperature sintering 1-10h, and after Temperature fall cooling, grinding, sieves, obtained anode material.
One as lithium ion battery anode material of the present invention is improved, and described organic carbon presoma is at least one in glucose, sucrose and polyvinyl alcohol, and oxygen content and the hydrogen content of this several material are higher, is easy to the coating layer forming open structure.
One as lithium ion battery anode material of the present invention is improved, and described pitch is at least one in bitumen, petroleum asphalt, shale tar pitch and coal tar asphalt.
Inert atmosphere wherein such as nitrogen atmosphere, argon gas atmosphere etc.
The method is by the mode of spraying, organic carbon presoma is enable to be coated on the surface of silica-base material powder equably, form organic carbon matrix precursor coating layer, this coating layer, after high temperature sintering, forms amorphous carbon coating layer, and organic carbon presoma is wherein preferably containing oxygen and the more organic substance of hydrogen, the amorphous carbon coating layer obtained after high temperature sintering has loose structure, thus not only can suppress the expansion of silica-base material, and when the expansion of silica-base material is larger, can also be its headspace.
Pitch add be in order to increase coated after silica-base material and graphite between adhesion, and silica-base material and graphite all select more tiny particle to be the uniformity mixed to increase the two, after abundant mixing, pitch bonding under, coated silica-base material is together with joining of graphite, after high temperature sintering, bitumen conversion becomes amorphous carbon, is dispersed in the particle of anode material.After grinding, just contain silica-base material, graphite and amorphous carbon in anode material particle, wherein, the surface of silica-base material is also uniformly coated with the amorphous carbon with open structure.
Relative to prior art, the present invention is by the Surface coating amorphous carbon at silica-base material, effectively can suppress the volumetric expansion of silica-base material, thus eliminate because silica-base material expands the cell deformation problem caused, inhibit activities material comes off from collector simultaneously, improves the cycle performance of battery; Silica-base material is mixed with graphite, greatly can improve again the gram volume of anode material, its gram volume apparently higher than the gram volume of graphite, cycle performance then comparatively silica-base material greatly improve.
Embodiment
Describe the present invention in detail below in conjunction with instantiation, but protection scope of the present invention is also not only confined to the content described by case study on implementation.
Embodiment 1
A kind of lithium ion battery anode material that the present embodiment provides, comprise graphite and silica-base material, the Surface coating of silica-base material has amorphous carbon, the median particle diameter of graphite is 5 μm, the median particle diameter of silica-base material is 5 μm, the quality of silica-base material accounts for 15% of anode material gross mass, and the quality of amorphous carbon accounts for 8% of anode material gross mass, and graphite accounts for 77% of anode material gross mass.
Wherein, graphite is specially native graphite, and silica-base material is specially silicon dioxide.
Its preparation method comprises the following steps:
The first step, silicon dioxide is placed in high mixer, stir with the rotating speed of 300r/min, then make solution by soluble in water for glucose, this solution is added in sprayer, make solution with the form of the drop of 1 μm to silicon-dioxide powdery surface sprinkling, after sprinkling completes, continue to stir 1h with the rotating speed of 300r/min, dry at 120 DEG C, obtain coated silica-base material;
Second step, coated silica-base material native graphite and the first step obtained and bitumen add high mixer, obtain mixture after stirring, and described bitumen accounts for 4% of described mixture;
3rd step, the mixture obtained by second step adds in high temperature furnace, is warming up to 1200 DEG C under nitrogen atmosphere with the speed of 30 DEG C/min, high temperature sintering 5h, and after Temperature fall cooling, grinding, sieves, obtained anode material.
Embodiment 2
A kind of lithium ion battery anode material that the present embodiment provides, comprise graphite and silica-base material, the Surface coating of silica-base material has amorphous carbon, the median particle diameter of graphite is 8 μm, the median particle diameter of silica-base material is 3 μm, the quality of silica-base material accounts for 20% of anode material gross mass, and the quality of amorphous carbon accounts for 10% of anode material gross mass, and graphite accounts for 70% of anode material gross mass.
Wherein, graphite is specially Delanium, and silica-base material is specially silicon.
Its preparation method comprises the following steps:
The first step, silicon is placed in high mixer, stir with the rotating speed of 200r/min, then make solution by soluble in water for sucrose, this solution is added in sprayer, make solution with the form of the drop of 2 μm to silicon powder surface sprinkling, after sprinkling completes, continue to stir 2h with the rotating speed of 200r/min, dry at 130 DEG C, obtain coated silica-base material;
Second step, coated silica-base material Delanium and the first step obtained and petroleum asphalt add high mixer, obtain mixture after stirring, and described petroleum asphalt accounts for 5% of described mixture;
3rd step, the mixture obtained by second step adds in high temperature furnace, is warming up to 1300 DEG C under argon gas atmosphere with the speed of 40 DEG C/min, high temperature sintering 7h, and after Temperature fall cooling, grinding, sieves, obtained anode material.
Embodiment 3
A kind of lithium ion battery anode material that the present embodiment provides, comprise graphite and silica-base material, the Surface coating of silica-base material has amorphous carbon, the median particle diameter of graphite is 10 μm, the median particle diameter of silica-base material is 6 μm, the quality of silica-base material accounts for 25% of anode material gross mass, and the quality of amorphous carbon accounts for 12% of anode material gross mass, and graphite accounts for 63% of anode material gross mass.
Wherein, graphite is specially carbonaceous mesophase spherules, and silica-base material is specially silicon monoxide.
Its preparation method comprises the following steps:
The first step, silicon monoxide is placed in high mixer, stir with the rotating speed of 400r/min, then make solution by soluble in water for polyvinyl alcohol, this solution is added in sprayer, solution is sprayed to silicon monoxide powder surface with the form of the drop of 2.5 μm, after sprinkling completes, continue to stir 30min with the rotating speed of 400r/min, dry at 150 DEG C, obtain coated silica-base material;
Second step, coated silica-base material carbonaceous mesophase spherules and the first step obtained and shale tar pitch add high mixer, obtain mixture after stirring, and described shale tar pitch accounts for 3% of described mixture;
3rd step, the mixture obtained by second step adds in high temperature furnace, is warming up to 1100 DEG C under argon gas atmosphere with the speed of 20 DEG C/min, high temperature sintering 10h, and after Temperature fall cooling, grinding, sieves, obtained anode material.
Embodiment 4
A kind of lithium ion battery anode material that the present embodiment provides, comprise graphite and silica-base material, the Surface coating of silica-base material has amorphous carbon, the median particle diameter of graphite is 3 μm, the median particle diameter of silica-base material is 8 μm, the quality of silica-base material accounts for 10% of anode material gross mass, and the quality of amorphous carbon accounts for 5% of anode material gross mass, and graphite accounts for 85% of anode material gross mass.
Wherein, graphite is specially native graphite, and silica-base material is specially silicon.
Its preparation method comprises the following steps:
The first step, silicon is placed in high mixer, stir with the rotating speed of 100r/min, then make solution by soluble in water for glucose, this solution is added in sprayer, make solution with the form of the drop of 0.5 μm to silicon powder surface sprinkling, after sprinkling completes, continue to stir 3h with the rotating speed of 100r/min, dry at 110 DEG C, obtain coated silica-base material;
Second step, coated silica-base material native graphite and the first step obtained and coal tar asphalt add high mixer, obtain mixture after stirring, and described coal tar asphalt accounts for 8% of described mixture;
3rd step, the mixture obtained by second step adds in high temperature furnace, is warming up to 1700 DEG C under nitrogen atmosphere with the speed of 50 DEG C/min, high temperature sintering 1h, and after Temperature fall cooling, grinding, sieves, obtained anode material.
Comparative example 1
The anode material that this comparative example provides is commercially available native graphite.
Comparative example 2
The anode material that comparative example provides is commercially available elementary silicon.
The anode material of embodiment 1 to 4 and comparative example 1 and 2 is added in distilled water with sodium carboxymethylcellulose, butadiene-styrene rubber and SuperP respectively, wherein, the mass ratio of anode material and sodium carboxymethylcellulose, butadiene-styrene rubber and SuperP is followed successively by 96:1:1:2, obtained anode slurry after stirring, by the coating of this slurry on a current collector, drying, after colding pressing, obtained anode strip, is numbered A1-A4 and C1, C2 respectively.
Above-mentioned anode strip is assembled into lithium ion battery with same lithium cobaltate cathode sheet, polypropylene diaphragm and electrolyte respectively, is numbered B1-B4 and D1, D2 respectively.
To being numbered B1-B4 and D1, the battery of D2 tests as follows:
1, battery performance test.
To being numbered B1-B4 and D1, the lithium ion battery of D2 carries out charge-discharge test, compares the discharge capacity first of battery, test condition: first change into battery, at 45 DEG C first with 0.01C constant current charge to 3.4V, then with 0.2C constant current charge to 3.8V; Then at normal temperatures, with 0.2C size of current constant current charge to 4.2V, then constant voltage is to 0.05C, after leaving standstill 5min, is discharged to 3.0V with 0.2C, and record discharge capacity, acquired results is in table 1.
2, battery 25 DEG C of cycle performance tests.
To being numbered B1-B4 and D1, the lithium ion battery of D2 carries out cycle performance test: at 25 DEG C, with 1C constant current charge to 4.2V, after constant voltage to 0.05C, after leaving standstill 30min, with 1C constant-current discharge to 3.0V, leave standstill 30min, circulate 400 weeks successively.Discharge capacity × 100% of discharge capacity/the first of capability retention=400th of battery week week, meanwhile, tests the one-tenth-value thickness 1/10 d of each battery
end, after assembled battery (also do not carry out change into etc. operation before), also first to test the one-tenth-value thickness 1/10 d of initial cells
just, then calculate the expansion rate of battery.Expansion rate=(the d of battery
end-d
just)/d
just× 100%, acquired results is in table 1.
Table 1: the performance test results of lithium-ion-power cell being numbered B1-B4 and D1, D2.
As can be seen from Table 1: compared to graphite, anode material of the present invention has higher specific capacity, can meet the small form factor requirements of current consumer electronics product; Compared to silicon, the present invention has better cycle performance and lower cell expansion rate, and adopts the expansion rate of battery of the present invention suitable with the expansion rate of the battery using graphite, therefore has great application prospect.
The explanation of book according to the above description, the personnel in field belonging to the present invention can also carry out suitable change and amendment to above-mentioned execution mode.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection range of claim of patent of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this specification, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (9)
1. a lithium ion battery anode material, it is characterized in that: described anode material comprises graphite and silica-base material, the Surface coating of described silica-base material has amorphous carbon, the median particle diameter of described graphite is 2-10 μm, the median particle diameter of silica-base material is 2-10 μm, the quality of described silica-base material accounts for the 10-30% of described anode material gross mass, and the quality of described amorphous carbon accounts for the 5-20% of described anode material gross mass;
The preparation method of described anode material comprises the following steps:
The first step, silica-base material is placed in high mixer, stir with the rotating speed of 100-450r/min, then organic carbon presoma is made solution, this solution is added in sprayer, solution is sprayed to silica-base material powder surface with the form of the drop of 0.5-3 μm, after sprinkling completes, dry at continuing to stir 30min-3h, 110-150 DEG C with the rotating speed of 100-450r/min, obtain coated silica-base material;
Second step, coated silica-base material graphite and the first step obtained and pitch add high mixer, obtain mixture after stirring, and described pitch accounts for the 1-8% of described mixture;
3rd step, the mixture obtained by second step adds in high temperature furnace, is warming up to 1000-1700 DEG C under inert atmosphere with the speed of 10-50 DEG C/min, high temperature sintering 1-10h, and after Temperature fall cooling, grinding, sieves, obtained anode material.
2. lithium ion battery anode material according to claim 1, is characterized in that: the quality of described silica-base material accounts for the 15-25% of described anode material gross mass.
3. lithium ion battery anode material according to claim 2, is characterized in that: the quality of described silica-base material accounts for 20% of described anode material gross mass.
4. lithium ion battery anode material according to claim 1, is characterized in that: the quality of described amorphous carbon accounts for the 10-15% of described anode material gross mass.
5. lithium ion battery anode material according to claim 4, is characterized in that: the quality of described amorphous carbon accounts for 12% of described anode material gross mass.
6. lithium ion battery anode material according to claim 1, is characterized in that: described silica-base material is at least one in silicon, silicon monoxide and silicon dioxide.
7. lithium ion battery anode material according to claim 1, is characterized in that: described graphite is at least one in native graphite and Delanium.
8. lithium ion battery anode material according to claim 1, is characterized in that: described organic carbon presoma is at least one in glucose, sucrose and polyvinyl alcohol.
9. lithium ion battery anode material according to claim 1, is characterized in that: described pitch is at least one in bitumen, petroleum asphalt, shale tar pitch and coal tar asphalt.
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| CN103915629A (en) * | 2014-03-25 | 2014-07-09 | 湖南立方新能源科技有限责任公司 | Preparation method of cladding material of lithium ion battery |
| CN104409709B (en) * | 2014-11-27 | 2016-09-21 | 中航锂电（江苏）有限公司 | A kind of lithium ion battery negative material, preparation method and lithium ion battery |
| CN107046125B (en) * | 2017-02-22 | 2020-08-04 | 深圳市金润能源材料有限公司 | Composite negative electrode, preparation method thereof and lithium ion battery |
| CN108123117A (en) * | 2017-11-20 | 2018-06-05 | 深圳市斯诺实业发展股份有限公司 | A kind of preparation method of SiO/ carbon graphites composite material |
| CN111244400B (en) * | 2018-11-28 | 2021-09-10 | 上海杉杉科技有限公司 | Silicon-oxygen-carbon composite material, lithium ion battery, and preparation method and application of silicon-oxygen-carbon composite material |
| CN111834612A (en) * | 2019-04-23 | 2020-10-27 | 四川佰思格新能源有限公司 | Hard carbon-silicon carbon composite material, preparation method thereof and lithium ion battery |
| CN110311130B (en) * | 2019-05-25 | 2022-02-18 | 浙江锋锂新能源科技有限公司 | Titanium niobate negative electrode material and preparation method thereof |
| CN110571424A (en) * | 2019-09-23 | 2019-12-13 | 七台河万锂泰电材有限公司 | Flake graphite silicon carbon composite negative electrode material and preparation method thereof |
| CN113013390B (en) * | 2021-02-20 | 2022-07-22 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery |
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| US20080286657A1 (en) * | 2007-05-16 | 2008-11-20 | Sanyo Electric Co., Ltd. | Non-aqueous electrolyte secondary battery |
| CN102332569A (en) * | 2011-03-22 | 2012-01-25 | 东莞新能源科技有限公司 | Lithium ion battery and negative electrode active material thereof |
| CN103219504A (en) * | 2013-03-28 | 2013-07-24 | 深圳市贝特瑞新能源材料股份有限公司 | Silicon monoxide composite cathode material for lithium ion battery, and preparation method thereof |
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