CN103618086A - Positive material of lithium ion battery - Google Patents
Positive material of lithium ion battery Download PDFInfo
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- CN103618086A CN103618086A CN201310588814.7A CN201310588814A CN103618086A CN 103618086 A CN103618086 A CN 103618086A CN 201310588814 A CN201310588814 A CN 201310588814A CN 103618086 A CN103618086 A CN 103618086A
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- base material
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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
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- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion batteries, and in particular relates to a positive material of a lithium ion battery. The positive material comprises graphite and a silicon-based material, wherein the surface of the silicon-based material is coated with amorphous carbon; the median particle size of the graphite is 2 to 10 microns; the median particle size of the silicon-based material is 2 to 10 microns; the mass of the silicon-based material accounts for 10 to 30 percent of the total mass of the positive material; the mass of the amorphous carbon accounts for 5 to 20 percent of the total mass of the positive material. Compared with the prior art, the positive material has the advantages that the volume expansion of the silicon-based material can be effectively suppressed by coating the amorphous carbon on the surface of the silicon-based material, so that the problem of battery deformation caused by the expansion of the silicon-based material is eliminated; meanwhile, active substances are prevented from falling from a collector, and thus the cycling performance of the battery is improved; the silicon-based material is mixed with the graphite, so that the volume per gram of the positive material can be greatly improved and is obviously higher than that of the graphite, and thus the cycling performance of the positive material is greatly improved compared with that of the silicon-based material.
Description
Technical field
The invention belongs to technical field of lithium ion, relate in particular 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 to be subject to showing great attention to of people in its capacity and useful life.And along with miniaturization and the microminiaturization of all kinds of consumer electronics products, its space of leaving lithium ion battery for is more and more limited, for this reason, just need to improve the capacity of battery, say more accurately the energy density that improves battery, just seem particularly important.Improve the energy density of battery, the gram volume of the improvement on battery structure, the gram volume that improves positive electrode and raising negative material is all considerable directions, but the improvement on battery structure, as reduce the thickness of packaging film or lug is processed, can only improve slightly the energy density of battery; And the raising of the gram volume of positive electrode is limited, the gram volume of negative material promotes 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 372 mAh/g, and it cannot meet the energy density requirement of current high-end electronic product.Therefore researcher has been done extensive and deep research to the negative material of high-energy-density, and it is most promising that wherein researcher is generally acknowledged is exactly silica-base material.The theoretical gram volume of silicon is up to 4200 mAh/g, far above theoretical gram volume 372 mAh/g of graphite.But silicon also has very large shortcoming: the volumetric expansion after silicon embedding lithium can reach 300%-400% more than.Its violent expansion easily causes active material and collector come off and declined electrode life rapidly.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, and provide a kind of energy density that can effectively improve battery, can effectively 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 of described silica-base material is coated with amorphous carbon, the median particle diameter of described graphite is 2-10 μ m, the median particle diameter of silica-base material is 2-10 μ m, 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.
On the surface of silica-base material, coated amorphous carbon, can effectively suppress the volumetric expansion of silica-base material, and the mixing of silica-base material and graphite, gram volume that can anode material, the energy density of raising battery.In the present invention, the median particle diameter of graphite and silica-base material is all less, for graphite and silica-base material can evenly be mixed, further to cushion the volumetric expansion of silica-base material, 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, thereby greatly extended the useful life of battery.
As a kind of improvement of lithium ion battery anode material of the present invention, the quality of described silica-base material accounts for the 15-25% of described anode material gross mass, and this is preferred scope.
As a kind of improvement of lithium ion battery anode material of the present invention, the quality of described silica-base material accounts for 20% of described anode material gross mass, and this is preferably to select.
As a kind of improvement of lithium ion battery anode material of the present invention, the quality of described amorphous carbon accounts for the 10-15% of described anode material gross mass, and this is preferred scope.
As a kind of improvement of lithium ion battery anode material of the present invention, the quality of described amorphous carbon accounts for 12% of described anode material gross mass, and this is preferably to select.
As a kind of improvement of lithium ion battery anode material of the present invention, described silica-base material is at least one in silicon, silicon monoxide and silicon dioxide.
As a kind of improvement of lithium ion battery anode material of the present invention, described graphite is at least one in native graphite, Delanium and carbonaceous mesophase spherules.
As a kind of improvement of lithium ion battery anode material of the present invention, the preparation method of described anode material comprises the following steps:
The first step, silica-base material is placed in to high mixer, rotating speed with 100-450r/min stirs, then organic carbon presoma is made to 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 μ m, after sprinkling completes, continuation is stirred 30min-3h with the rotating speed of 100-450r/min, dries at 110-150 ℃, obtains coated silica-base material;
Second step, coated silica-base material and pitch that graphite and the first step are obtained add high mixer, after stirring, obtain mixture, and described pitch accounts for the 1-8% of described mixture;
The 3rd step, the mixture that second step is obtained adds in high temperature furnace, and the speed with 10-50 ℃/min under inert atmosphere is warming up to 1000-1700 ℃, and high temperature sintering 1-10h, after natural cooling down, grinds, and sieves, and makes anode material.
As a kind of improvement of lithium ion battery anode material of the present invention, described organic carbon presoma is at least one in glucose, sucrose and polyvinyl alcohol, and oxygen content and the hydrogen content of these several materials are higher, is easy to form the coating layer of open structure.
As a kind of improvement of lithium ion battery anode material of the present invention, 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, make organic carbon presoma can be coated on equably the surface of silica-base material powder, 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 obtaining after high temperature sintering has loose structure, thereby 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.
Adding of pitch is in order to increase silica-base material after coated and the adhesion between graphite, and silica-base material and graphite all to select more tiny particle be in order to increase the uniformity of the two mixing, after fully mixing, under pitch bonding, coated silica-base material is together with joining of graphite, after high temperature sintering, pitch changes into amorphous carbon, is dispersed in the particle of anode material.After grinding, just comprised 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.
With respect to prior art, the present invention is by the coated amorphous carbon in the surface at silica-base material, can effectively suppress the volumetric expansion of silica-base material, thereby eliminate the battery problem on deformation that expands and cause due to silica-base material, suppress active material simultaneously and come off from collector, improve the cycle performance of battery; Silica-base material is mixed with graphite, can greatly improve again the gram volume of anode material, its gram volume is apparently higher than the gram volume of graphite, and cycle performance greatly improves compared with silica-base material.
Embodiment
Below in conjunction with instantiation, describe the present invention in detail, but protection scope of the present invention is also not only confined to the described content of 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 of silica-base material is coated with amorphous carbon, the median particle diameter of graphite is 5 μ m, the median particle diameter of silica-base material is 5 μ m, 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 to high mixer, rotating speed with 300r/min stirs, then by the glucose solution of making soluble in water, this solution is added in sprayer, make solution with the form of the drop of 1 μ m to silicon-dioxide powdery surface sprinkling, after sprinkling completes, continuation is stirred 1h with the rotating speed of 300r/min, dries at 120 ℃, obtains coated silica-base material;
Second step, coated silica-base material and bitumen that native graphite and the first step are obtained add high mixer, after stirring, obtain mixture, and described bitumen accounts for 4% of described mixture;
The 3rd step, the mixture that second step is obtained adds in high temperature furnace, and the speed with 30 ℃/min under nitrogen atmosphere is warming up to 1200 ℃, and high temperature sintering 5h, after natural cooling down, grinds, and sieves, and makes 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 of silica-base material is coated with amorphous carbon, the median particle diameter of graphite is 8 μ m, the median particle diameter of silica-base material is 3 μ m, 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 to high mixer, rotating speed with 200r/min stirs, then by the sucrose solution of making soluble in water, this solution is added in sprayer, make solution with the form of the drop of 2 μ m to silicon powder surface sprinkling, after sprinkling completes, continuation is stirred 2h with the rotating speed of 200r/min, dries at 130 ℃, obtains coated silica-base material;
Second step, coated silica-base material and petroleum asphalt that Delanium and the first step are obtained add high mixer, after stirring, obtain mixture, and described petroleum asphalt accounts for 5% of described mixture;
The 3rd step, the mixture that second step is obtained adds in high temperature furnace, and the speed with 40 ℃/min under argon gas atmosphere is warming up to 1300 ℃, and high temperature sintering 7h, after natural cooling down, grinds, and sieves, and makes 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 of silica-base material is coated with amorphous carbon, the median particle diameter of graphite is 10 μ m, the median particle diameter of silica-base material is 6 μ m, 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 to high mixer, rotating speed with 400r/min stirs, then by the polyvinyl alcohol solution of making soluble in water, this solution is added in sprayer, solution is sprayed to silicon monoxide powder surface with the form of the drop of 2.5 μ m, after sprinkling completes, continuation is stirred 30min with the rotating speed of 400r/min, dries at 150 ℃, obtains coated silica-base material;
Second step, coated silica-base material and shale tar pitch that carbonaceous mesophase spherules and the first step are obtained add high mixer, after stirring, obtain mixture, and described shale tar pitch accounts for 3% of described mixture;
The 3rd step, the mixture that second step is obtained adds in high temperature furnace, and the speed with 20 ℃/min under argon gas atmosphere is warming up to 1100 ℃, and high temperature sintering 10h, after natural cooling down, grinds, and sieves, and makes 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 of silica-base material is coated with amorphous carbon, the median particle diameter of graphite is 3 μ m, the median particle diameter of silica-base material is 8 μ m, 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 to high mixer, rotating speed with 100r/min stirs, then by the glucose solution of making soluble in water, this solution is added in sprayer, make solution with the form of the drop of 0.5 μ m to silicon powder surface sprinkling, after sprinkling completes, continuation is stirred 3h with the rotating speed of 100r/min, dries at 110 ℃, obtains coated silica-base material;
Second step, coated silica-base material and coal tar asphalt that native graphite and the first step are obtained add high mixer, after stirring, obtain mixture, and described coal tar asphalt accounts for 8% of described mixture;
The 3rd step, the mixture that second step is obtained adds in high temperature furnace, and the speed with 50 ℃/min under nitrogen atmosphere is warming up to 1700 ℃, and high temperature sintering 1h, after natural cooling down, grinds, and sieves, and makes 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 Super P respectively, wherein, the mass ratio of anode material and sodium carboxymethylcellulose, butadiene-styrene rubber and Super P is followed successively by 96:1:1:2, after stirring, make anode slurry, this slurry is coated on collector, dry, after colding pressing, make anode strip, be numbered respectively A1-A4 and C1, C2.
Above-mentioned anode strip is assembled into lithium ion battery with same lithium cobaltate cathode sheet, polypropylene diaphragm and electrolyte respectively, is numbered respectively B1-B4 and D1, D2.
To being numbered the battery of B1-B4 and D1, D2, test as follows:
1, battery performance test.
To being numbered the lithium ion battery of B1-B4 and D1, D2, carry out charge-discharge test, the discharge capacity first of battery relatively, test condition: first battery is changed into, at 45 ℃ 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 standing 5min, with 0.2C, is discharged to 3.0V, records discharge capacity, and acquired results is in Table 1.
2,25 ℃ of cycle performance tests of battery.
To being numbered the lithium ion battery of B1-B4 and D1, D2, carry out cycle performance test: at 25 ℃, to 4.2V, constant voltage is to 0.05C with 1C constant current charge, and after standing 30min, to 3.0V, standing 30min, circulates 400 weeks successively with 1C constant-current discharge.Discharge capacity * 100% of discharge capacity/the first of the capability retention of battery=400th week week, meanwhile, tests the one-tenth-value thickness 1/10 d of each battery
end, after assembled battery (also change into etc. operation before), also to first test the one-tenth-value thickness 1/10 d of initial cells
just, then calculate the expansion rate of battery.The expansion rate of battery=(d
end-d
just)/d
just* 100%, acquired results is in Table 1.
Table 1: the performance test results that is numbered the lithium-ion-power cell of B1-B4 and D1, D2.
As can be seen from Table 1: than graphite, anode material of the present invention has higher specific capacity, can meet the miniaturization requirement 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 of use graphite, therefore has great application prospect.
The explanation of book according to the above description, under the present invention, the personnel in field can also carry out suitable change and modification 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 to modifications and changes more of the present invention.In addition,, although used some specific terms in this specification, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (10)
1. a lithium ion battery anode material, it is characterized in that: described anode material comprises graphite and silica-base material, the surface of described silica-base material is coated with amorphous carbon, the median particle diameter of described graphite is 2-10 μ m, the median particle diameter of silica-base material is 2-10 μ m, 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.
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, Delanium and carbonaceous mesophase spherules.
8. according to the lithium ion battery anode material described in claim 1 to 7 any one, it is characterized in that, the preparation method of described anode material comprises the following steps:
The first step, silica-base material is placed in to high mixer, rotating speed with 100-450r/min stirs, then organic carbon presoma is made to 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 μ m, after sprinkling completes, continuation is stirred 30min-3h with the rotating speed of 100-450r/min, dries at 110-150 ℃, obtains coated silica-base material;
Second step, coated silica-base material and pitch that graphite and the first step are obtained add high mixer, after stirring, obtain mixture, and described pitch accounts for the 1-8% of described mixture;
The 3rd step, the mixture that second step is obtained adds in high temperature furnace, and the speed with 10-50 ℃/min under inert atmosphere is warming up to 1000-1700 ℃, and high temperature sintering 1-10h, after natural cooling down, grinds, and sieves, and makes anode material.
9. lithium ion battery anode material according to claim 8, is characterized in that: described organic carbon presoma is at least one in glucose, sucrose and polyvinyl alcohol.
10. lithium ion battery anode material according to claim 8, 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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| 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 |
| CN110311130A (en) * | 2019-05-25 | 2019-10-08 | 浙江锋锂新能源科技有限公司 | A kind of titanium niobate negative electrode material and preparation method thereof |
| 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 |
| CN113013390A (en) * | 2021-02-20 | 2021-06-22 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery |
| 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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