CN105070918A - Graphite anode material for lithium ion battery and preparation method of graphite anode material - Google Patents
Graphite anode material for lithium ion battery and preparation method of graphite anode material Download PDFInfo
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- CN105070918A CN105070918A CN201510395791.7A CN201510395791A CN105070918A CN 105070918 A CN105070918 A CN 105070918A CN 201510395791 A CN201510395791 A CN 201510395791A CN 105070918 A CN105070918 A CN 105070918A
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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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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a graphite anode material for a lithium ion battery. The graphite anode material comprises a graphite material, wherein the surface of the graphite material is coated with a conductive network membrane which is composed of plant nanofibers and carbon nanotubes; the mass of the conductive network membrane is 0.01%-10% of total mass of the graphite anode material; and the preparation method of the anode material comprises the following steps: mixing a dispersed medium, graphite powder, the plant nanofibers and the carbon nanotubes; drying the mixture into a material block; and baking and cooling the material block to form the graphite anode material. Through the method, the surface of the graphite material is coated with the conductive network membrane which is composed of plant nanofiber pyrolytic carbon and the carbon nanotubes; the interface interaction of the conductive network membrane and the graphite anode material is strong; overpotential between two phases is low; and strong chemical bonding interaction exists, so that the electronic conductivity can be greatly improved; polarization of the graphite anode material is lowered; the internal resistance of the material is reduced; and the high multiplying power, the cycle performance and the charge-discharge specific capacity of the lithium ion battery are improved.
Description
Technical field
The invention belongs to technical field of lithium ion, be specially a kind of lithium ion battery graphite cathode material and preparation method thereof.
Background technology
Along with the miniaturization of electronic product and the development of removableization, and the fast development of electric tool, electric motorcycle and Prospect of EVS Powered with Batteries, high power and high-capacity lithium ion cell have become the focus that countries in the world are competitively developed.As the negative material of one of the four large main materials of lithium ion battery, and at present the negative material of commercialization and result of use the best be graphite Carbon Materials, mainly comprise Delanium and native graphite two class.
Delanium has graphous graphite powder, MCMB and intermediate-phase carbon fiber, the Delanium shortcoming that tap density is low owing to existing, specific area is high is not suitable for directly as negative material, the advantage that irreversible capacity is low, cycle life is good although MCMB and intermediate-phase carbon fiber have, but its high temperature graphitization costly, cause this material cost too high, limit the extensive use of material.Although native graphite cost of material is low, there is higher embedding lithium ability, but through the natural graphite negative electrode material of modification, irreversible capacity loss is very not high first, during high-multiplying power discharge, capacity declines very fast, embed altogether due to solvent can be there is in cyclic process, the problem such as cause capacity attenuation very fast, is not suitable for directly as negative material.
The improvement of researcher to graphite proposes a lot of method, and current Surface coating is widely used in graphite Carbon Materials study on the modification as effective and the most cheap means.Although at present carrying out surface coating modification to graphite cathode material has much with the patent and bibliographical information that improve the high rate capability of graphite cathode material, cycle performance and reversible capacity, but to the raising of graphite cathode material performance, the special improvement for being high rate during charging-discharging is not remarkable very especially, so that graphite cathode material is subject to a definite limitation in the application of high-end lithium battery.
Summary of the invention
The object of the invention is, in order to solve the problem mentioned in above-mentioned background technology, to provide a kind of lithium ion battery graphite cathode material and preparation method thereof.
To achieve these goals, technical scheme of the present invention is as follows:
A kind of lithium ion battery graphite cathode material, comprise graphite material, described graphite material Surface coating is by the conductive network film be made up of plant nanometer fiber and carbon nano-tube, and the quality of described conductive network film is 0.01 ~ 10% of described graphite cathode material gross mass.
Further, described conductive network film quality is 0.01 ~ 5% of described graphite cathode material gross mass.
A preparation method for lithium ion battery graphite cathode material, comprises the steps:
A1, decentralized medium, graphite powder, plant nanometer fiber, carbon nano-tube to be mixed according to following weight fraction meter, decentralized medium 100-200 part, graphite powder 80-99 part, plant nanometer fiber 0.05-10 part, carbon nano-tube 0.05-10 part;
A2, the compound of step 1 gained is dried into material block;
After a3, the material block obtained by step a2 are placed in sintering kiln roasting, cooling obtains graphite cathode material.
Further, in described step a3, dry the material block obtained and be placed in sintering furnace, in inert atmosphere or reduction mixed atmosphere, heat up with 5 ~ 30 DEG C/min rate of heat addition, constant temperature calcining 3-15 hour at 260-1250 DEG C, then heat up with 5 ~ 30 DEG C/min rate of heat addition, constant temperature calcining 5 ~ 26 hours at 650 ~ 1250 DEG C.
Further, in described step a3, the material block obtained through step a2, after sintering kiln roasting terminates, is cooled to room temperature with 3 ~ 30 DEG C/min rate of temperature fall.
Further, in described step a2, the compound obtained by a1 is dried under being placed in 100 DEG C of-200 DEG C of temperature environments.
Further, step a2 is dried after the material block obtained cuts into sheet/round shape/spherical, be placed in sintering kiln roasting.
Further, described plant nanometer fiber is one or more in seed nanofiber, tough bark nano, leaf nanofiber, fruit nanofiber, root nanofiber, cob nanofiber, timber nanofiber, stem stalk nanofiber.
Further, described carbon nano-tube is single-walled pipe or multi-walled pipes.
Further, described decentralized medium is one or more in water, methyl alcohol, ethanol, benzene, toluene, acetone, organic acid and organic ester.
Compared with prior art, beneficial effect of the present invention is as follows;
1. lithium ion battery graphite cathode material disclosed by the invention, its graphite material Surface coating is by the conductive network film be made up of plant nanometer fiber and carbon nano-tube, the quality of conductive network film is 0.01 ~ 10% of graphite cathode material gross mass, the conductive network film that in the present invention, plant nanometer fiber RESEARCH OF PYROCARBON and carbon nano-tube are formed and the interface interaction of graphite cathode material strong, two alternate overpotentials are low and there is strong chemical bond, thus electronic conductivity can be improved widely, reduce the polarization of graphite cathode material, reduce the internal resistance of material, the high power improving lithium ion battery is forthright, cycle performance and charging and discharging capacity.
2. in the present invention, conductive network film is mainly made up of plant carbide fiber and carbon nano-tube, thus can hinder the common embedding of electrolyte solvent and lithium ion, reduces the irreversible capacity of graphite cathode material, thus increases the reversible capacity of graphite cathode material.
3. the preparation method of lithium ion battery graphite cathode material of the present invention, comprises the steps: that decentralized medium, graphite powder, plant nanometer fiber, carbon nano-tube mix, compound is dried in material block, the roasting of material block, graphite cathode material is formed after cooling, pass through the method, its plant nanometer fiber is in heat treatment process, gas can at the uniform velocity spread, make solid phase reaction more even, plant nanometer fiber, carbon nano-tube and decentralized medium (electrolytic solution) compatibility better, graphite powder material is fully contacted with decentralized medium (electrolytic solution), in heat treatment process, gas can at the uniform velocity spread, make solid phase reaction more even, thus form at graphite powder material surface the conductive network film that one deck is made up of plant nanometer fiber and carbon nano-tube, its conductive network film formed compensate for lithium ion and deviates from/telescopiny in charge balance, and then improve the chemical property of graphite cathode material.
4. material block is made sheet, column, spherical or other geometries, can high temperature solid state reaction be accelerated, shorten the high temperature solid state reaction time, energy savings.
5. low, the environmental protection and energy saving of the inventive method cost, technique are simple, easily large-scale production, the graphite cathode material excellent electrochemical performance of preparation.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
A kind of lithium ion battery graphite cathode material, comprise graphite material, described graphite material Surface coating is by the conductive network film be made up of plant nanometer fiber and carbon nano-tube, and the quality of described conductive network film is 0.01 ~ 10% of described graphite cathode material gross mass.
Preferred in above-mentioned graphite cathode material, the quality of described conductive network film is 0.01 ~ 5.00% of graphite cathode material quality.
As a total technical conceive: a kind of preparation method of lithium ion battery graphite cathode material, concrete steps are as follows:
1. graphite powder, plant nanometer fiber are mixed in decentralized medium with carbon nano-tube, decentralized medium, graphite powder, plant nanometer fiber, carbon nano-tube mix according to following weight fraction meter, decentralized medium 100-200 part, graphite powder 80-99 part, plant nanometer fiber 0.05-10 part, carbon nano-tube 0.05-10 part.
2. obtained compound is dried into material block,
3, expect that block is placed in sintering furnace, in inert atmosphere or reduction mixed atmosphere, heat up with 5 ~ 30 DEG C/min rate of heat addition, constant temperature calcining 3 ~ 15 hours at 260 ~ 550 DEG C, heat up with 5 ~ 30 DEG C/min rate of heat addition again, constant temperature calcining 5 ~ 26 hours at 650 ~ 1250 DEG C, is then cooled to room temperature with 3 ~ 30 DEG C/min rate of temperature fall, obtains the graphite cathode material that Surface coating one deck plants thing nanofiber RESEARCH OF PYROCARBON and carbon nano-tube.
In above-mentioned preparation method, preferred plant nanometer fiber is described plant nanometer fiber is that seed nanofiber is (as: cotton, kapok etc.), tough bark nano (as: flax, ramie, jute, bamboo fibre etc.), leaf nanofiber (as: sisal hemp, abaca etc.), fruit nanofiber (as: cocoanut fiber etc.), root nanofiber (as: Radix Glycyrrhizae etc.), cob nanofiber (as: Chinese sorghum etc.), timber nanofiber (as: pine, China fir, press), stem stalk nanofiber (as: corn, rice, wheat etc.) in one or more.
Carbon nano-tube is single-walled pipe (, at 0.6-2nm, draw ratio is between 20:1 ~ 1000:1 for diameter) or multi-walled pipes (, at 2-100nm, draw ratio is between 20:1 ~ 1000:1 for diameter).
Decentralized medium is one or more in water, methyl alcohol, ethanol, benzene, toluene, acetone, organic acid and organic ester, carries out ultrasonic process or ball-milling treatment when mixing in decentralized medium simultaneously.
In its preparation methods steps 1 by graphite powder, plant nanometer fiber with the concrete operations that carbon nano-tube mixes in decentralized medium be: first plant nanometer fiber and carbon nano-tube are dissolved in decentralized medium by proportioning and obtain finely disseminated mixed liquor, then graphite powder is joined in aforementioned mixed liquor by proportioning mix.
It is carry out at 100 DEG C ~ 200 DEG C temperature that preferred step a2 is dried.
Step a2 is dried after the material block obtained cuts into sheet/round shape/spherical, is placed in sintering kiln roasting.
In above-mentioned preparation method, in preferred described step a3 at 350 ~ 500 DEG C constant temperature calcining 4 ~ 10 hours, constant temperature calcining 10 ~ 18 hours at 750 ~ 900 DEG C.
The specific embodiment 1 of this preparation method:
By 200mg plant nanometer fiber and 100mg carbon nano-tube, be dissolved in 100mL water, ultrasonic echography process 2h.Again 5g graphite powder is joined in plant nanometer fiber and the finely disseminated mixed liquor of oxide/carbon nanometer tube, continue ultrasonic agitation 1h, slowly dry at 120 DEG C, it is powder that material after oven dry is put into the ball mill container ball milling filling hydrogen or nitrogen atmosphere, on tablet press machine, above-mentioned powder is made sheet again, be incorporated with in the sintering vessel of lid.Then the sintering vessel that material is housed is placed in sintering furnace, in argon gas, nitrogen or reduction mixed atmosphere, heat up with the 5 DEG C/min rate of heat addition, constant temperature calcining 6h at 400 DEG C, heat up with the 5 DEG C/min rate of heat addition, constant temperature calcining 10h at 1050 DEG C, is then cooled to room temperature with 10 DEG C/min rate of temperature fall again, the broken classification of product, obtains the graphite shell core negative material of the conductive network film that Surface coating one deck is made up of plant nanometer fiber RESEARCH OF PYROCARBON and carbon nano-tube.
Through test, the conductance of the graphite cathode material of coated front and back brings up to the 10-2S/cm order of magnitude from l0-6S/cm, and tap density brings up to 1.70g/cm3 by 1.60g/cm3.
At 25 scholar 2 DEG C, in 0.001V ~ 3.0V voltage range, constant current charge-discharge test is carried out to the lithium ion battery of the present embodiment graphite cathode material, with reversible specific capacity during 0.2C multiplying power discharging up to 390mAh/g, exceed the theoretical specific capacity of graphite.382,378 and 357mAh/g is respectively with its specific capacity during 1C, 5C and 10C multiplying power discharging.
Embodiment 2
By 300mg plant nanometer fiber and 100mg carbon nano-tube, be dissolved in 100mL water, ultrasonic echography process 2h.Again 8g graphite powder is joined in plant nanometer fiber and the finely disseminated mixed liquor of oxide/carbon nanometer tube, continue ultrasonic agitation 1.5h, slowly dry at 150 DEG C, it is powder that material after oven dry is put into the ball mill container ball milling filling hydrogen or nitrogen atmosphere, on tablet press machine, above-mentioned powder is made sheet again, be incorporated with in the sintering vessel of lid.Then the sintering vessel that material is housed is placed in sintering furnace, in argon gas, nitrogen or reduction mixed atmosphere, heat up with the 10 DEG C/min rate of heat addition, constant temperature calcining 6h at 500 DEG C, heat up with the 10 DEG C/min rate of heat addition, constant temperature calcining 10h at 1110 DEG C, is then cooled to room temperature with 20 DEG C/min rate of temperature fall again, the broken classification of product, obtains the graphite shell core negative material of the conductive network film that Surface coating one deck is made up of plant nanometer fiber RESEARCH OF PYROCARBON and carbon nano-tube.
Through test, the conductance of the graphite cathode material of coated front and back brings up to the 10-1S/cm order of magnitude from l0-6S/cm, and tap density brings up to 1.90g/cm3 by 1.60g/cm3.
At 25 scholar 2 DEG C, in 0.001V ~ 3.0V voltage range, constant current charge-discharge test is carried out to the lithium ion battery of the present embodiment graphite cathode material, with reversible specific capacity during 0.2C multiplying power discharging up to 390mAh/g, exceed the theoretical specific capacity of graphite.382,378 and 357mAh/g is respectively with its specific capacity during 1C, 5C and 10C multiplying power discharging.
Embodiment 3
By 250mg plant nanometer fiber and 150mg carbon nano-tube, be dissolved in 100mL water, ultrasonic echography process 2h.Again 5g graphite powder is joined in plant nanometer fiber and the finely disseminated mixed liquor of oxide/carbon nanometer tube, continue ultrasonic agitation 1h, slowly dry at 120 DEG C, it is powder that material after oven dry is put into the ball mill container ball milling filling hydrogen or nitrogen atmosphere, on tablet press machine, above-mentioned powder is made sheet again, be incorporated with in the sintering vessel of lid.Then the sintering vessel that material is housed is placed in sintering furnace, in argon gas, nitrogen or reduction mixed atmosphere, heat up with the 5 DEG C/min rate of heat addition, constant temperature calcining 6h at 400 DEG C, heat up with the 5 DEG C/min rate of heat addition, constant temperature calcining 10h at 1050 DEG C, is then cooled to room temperature with 10 DEG C/min rate of temperature fall again, the broken classification of product, obtains the graphite shell core negative material of the conductive network film that Surface coating one deck is made up of plant nanometer fiber RESEARCH OF PYROCARBON and carbon nano-tube.
Through test, the conductance of the graphite cathode material of coated front and back brings up to the 10-1S/cm order of magnitude from l0-6S/cm, and tap density brings up to 1.860g/cm3 by 1.60g/cm3.
At 25 scholar 2 DEG C, in 0.001V ~ 3.0V voltage range, constant current charge-discharge test is carried out to the lithium ion battery of the present embodiment graphite cathode material, with reversible specific capacity during 0.2C multiplying power discharging up to 390mAh/g, exceed the theoretical specific capacity of graphite.382,378 and 357mAh/g is respectively with its specific capacity during 1C, 5C and 10C multiplying power discharging.
Embodiment 4
By 200mg plant nanometer fiber and 100mg carbon nano-tube, be dissolved in 100mL water, ultrasonic echography process 2h.Again 8g graphite powder is joined in plant nanometer fiber and the finely disseminated mixed liquor of oxide/carbon nanometer tube, continue ultrasonic agitation 1h, slowly dry at 150 DEG C, it is powder that material after oven dry is put into the ball mill container ball milling filling hydrogen or nitrogen atmosphere, on tablet press machine, above-mentioned powder is made sheet again, be incorporated with in the sintering vessel of lid.Then the sintering vessel that material is housed is placed in sintering furnace, in argon gas, nitrogen or reduction mixed atmosphere, heat up with the 5 DEG C/min rate of heat addition, constant temperature calcining 6h at 500 DEG C, heat up with the 5 DEG C/min rate of heat addition, constant temperature calcining 10h at 1110 DEG C, is then cooled to room temperature with 10 DEG C/min rate of temperature fall again, the broken classification of product, obtains the graphite shell core negative material of the conductive network film that Surface coating one deck is made up of plant nanometer fiber RESEARCH OF PYROCARBON and carbon nano-tube.
Through test, the conductance of the graphite cathode material of coated front and back brings up to the 10-2S/cm order of magnitude from l0-6S/cm, and tap density brings up to 1.650g/cm3 by 1.60g/cm3.
At 25 scholar 2 DEG C, in 0.001V ~ 3.0V voltage range, constant current charge-discharge test is carried out to the lithium ion battery of the present embodiment graphite cathode material, with reversible specific capacity during 0.2C multiplying power discharging up to 390mAh/g, exceed the theoretical specific capacity of graphite.382,378 and 357mAh/g is respectively with its specific capacity during 1C, 5C and 10C multiplying power discharging.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments, equivalent replacement etc. done in protection scope of the present invention, all should be included within protection scope of the present invention.
Claims (10)
1. a lithium ion battery graphite cathode material, comprise graphite material, it is characterized in that, described graphite material Surface coating is by the conductive network film be made up of plant nanometer fiber and carbon nano-tube, and the quality of described conductive network film is 0.01 ~ 10% of described graphite cathode material gross mass.
2. lithium ion battery graphite cathode material according to claim 1, is characterized in that, described conductive network film quality is 0.01 ~ 5% of described graphite cathode material gross mass.
3. a preparation method for lithium ion battery graphite cathode material, is characterized in that, comprises the steps:
A1, decentralized medium, graphite powder, plant nanometer fiber, carbon nano-tube to be mixed according to following weight fraction meter, decentralized medium 100-200 part, graphite powder 80-99 part, plant nanometer fiber 0.05-10 part, carbon nano-tube 0.05-10 part;
A2, the compound of step 1 gained is dried into material block;
After a3, the material block obtained by step a2 are placed in sintering kiln roasting, cooling obtains graphite cathode material.
4. the preparation method of lithium ion graphite cathode material according to claim 3, it is characterized in that, in described step a3, dry the material block obtained and be placed in sintering furnace, in inert atmosphere or reduction mixed atmosphere, heat up with 5 ~ 30 DEG C/min rate of heat addition, constant temperature calcining 3-15 hour at 260-1250 DEG C, heat up with 5 ~ 30 DEG C/min rate of heat addition again, constant temperature calcining 5 ~ 26 hours at 650 ~ 1250 DEG C.
5. the preparation method of lithium ion graphite cathode material according to claim 4, is characterized in that, in described step a3, the material block obtained through step a2, after sintering kiln roasting terminates, is cooled to room temperature with 3 ~ 30 DEG C/min rate of temperature fall.
6. the preparation method of lithium ion graphite cathode material according to claim 3, is characterized in that, in described step a2, the compound obtained by a1 is dried under being placed in 100 DEG C of-200 DEG C of temperature environments.
7. the preparation method of lithium ion graphite cathode material according to claim 6, is characterized in that, is dried by step a2 after the material block obtained cuts into sheet/round shape/spherical, is placed in sintering kiln roasting.
8. according to the preparation method of the lithium ion graphite cathode material in claim 3-7 described in any one, it is characterized in that, described plant nanometer fiber is one or more in seed nanofiber, tough bark nano, leaf nanofiber, fruit nanofiber, root nanofiber, cob nanofiber, timber nanofiber, stem stalk nanofiber.
9. according to the preparation method of the lithium ion graphite cathode material in claim 3-7 described in any one, it is characterized in that, described carbon nano-tube is single-walled pipe or multi-walled pipes.
10. according to the preparation method of the lithium ion graphite cathode material in claim 3-7 described in any one, it is characterized in that, described decentralized medium is one or more in water, methyl alcohol, ethanol, benzene, toluene, acetone, organic acid and organic ester.
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| CN101969112A (en) * | 2010-09-30 | 2011-02-09 | 湛江市聚鑫新能源有限公司 | Anode material and cathode material for lithium ion battery and modifying method thereof |
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