CN103137954B - Novel carbon-carbon nanotube lithium ion battery cathode material and preparation method thereof - Google Patents
Novel carbon-carbon nanotube lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- CN103137954B CN103137954B CN201310061495.4A CN201310061495A CN103137954B CN 103137954 B CN103137954 B CN 103137954B CN 201310061495 A CN201310061495 A CN 201310061495A CN 103137954 B CN103137954 B CN 103137954B
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Abstract
The invention discloses a novel carbon-carbon nanotube lithium ion battery cathode material and a preparation method thereof, and belongs to the technical field of lithium ion batteries and the nanometer technology field. The novel carbon-carbon nanotube lithium ion battery cathode material is characterized in that the novel carbon-carbon nanotube lithium ion battery cathode material is formed by spherical graphite and a cladding material wrapped on the surface of the spherical graphite, and the cladding material accounts for 8-12% of the total weight of the spherical graphite and the cladding material; and the cladding material is prepared through mixing carbon nanotubes with organic carbon powder, and the weight ratio of the carbon nanotubes to the organic carbon powder is 3:7. The novel carbon-carbon nanotube lithium ion battery cathode material prepared in the invention can well solve the carbon nanotube agglomeration phenomenon through multi-time grading diffusion, the cladding material is wrapped on the surface of the spherical graphite, and the carbon nanotubes generate a pompon-like grid structure on the surface of the spherical graphite, so the surface strength is enhanced, the conductive performance and the anti-damping performance are substantially improved, and the first discharge capacity is substantially improved.
Description
Technical field
The present invention relates to a kind of lithium ion battery cathode material and its preparation method, especially a kind of Novel carbon-carbon nanotube lithium ion battery cathode material and preparation method thereof, belongs to technical field of lithium ion and field of nanometer technology.
Background technology
Because lithium ion battery has the important advantage of high voltage, high power capacity, and have extended cycle life, security performance is good, makes it be with a wide range of applications in the field such as portable electric appts and electric automobile.Spherical natural graphite has higher lithium storage content, good voltage platform, and cheap, is one of negative material common on Vehicles Collected from Market.But spherical graphite is as lithium ion battery negative material, the SEI film formed in charge-discharge process is constantly avalanche easily, affects serviceability and the life-span of battery, need to modify and shaping its surface, after modification, surface strength is low, easily peels off, destroys in charge and discharge process.Be point cantact between spheroidal graphite particles simultaneously, poorly conductive.
The interlamellar spacing of carbon nano-tube is slightly larger than the interlamellar spacing of spherical graphite, and the tubular structure of carbon nano-tube can not subside after the circulation of repeatedly charge-discharge, good cycle, carbon nano-tube has larger draw ratio and good axial one-dimensional electric ability simultaneously, is considered to desirable electric conducting material.But the irreversible capacity of carbon nano-tube is also comparatively large, and cycle efficieny is low first, does not have obvious charge-discharge platform.In addition, because its diameter is little, draw ratio is large, very easily reunites, is not easy to be disperseed, affects the performance of its physics and chemical property.
Therefore, in the urgent need to providing, a kind of lithium storage content is high, voltage platform good, the lithium ion battery negative material of good cycle.
Summary of the invention
The object of the invention is for above-mentioned the deficiencies in the prior art, there is provided that a kind of lithium storage content is high, voltage platform be good, the Novel carbon-carbon nanotube lithium ion battery cathode material of good cycle and preparation method thereof, the present invention utilizes nanometer-material-modified lithium ion battery negative material greatly can improve the properties of lithium ion battery.
The object of the invention is to be achieved through the following technical solutions: Novel carbon-carbon nanotube lithium ion battery cathode material, it is characterized in that, be made up of spherical graphite and the clad material that is wrapped in spherical graphite surface, described clad material accounts for the 8-12% of spherical graphite and clad material total weight; Described clad material mixes obtained by carbon nano-tube and organic carbon dust, and wherein the weight ratio of carbon nano-tube and organic carbon dust is 3:7.
The particle diameter of described clad material is 2-6 μm.
The preparation method of Novel carbon-carbon nanotube lithium ion battery cathode material, is characterized in that, comprises the following steps:
1) raw material is got ready: spherical graphite, carbon nano-tube, organic carbon dust;
2) carbon nano-tube of step 1), organic carbon dust are put into ball mill in batches and carried out multiple fractionation mixing, when putting in batches, wherein a kind of material is disposable puts into, another kind of material average mark is put into for five times, the interval time of at every turn putting into is 1-2 hour, total incorporation time is 10-12 hour, obtains clad material, and the particle diameter of clad material is 2-6 μm; The weight ratio of described carbon nano-tube and organic carbon dust is 3:7;
3) by the spherical graphite of step 1) and step 2) obtained clad material carries out stirring makes it fully mix, and the time of being uniformly mixed is 1-3 hour, makes clad material evenly be wrapped in spherical graphite surface; Described clad material accounts for the 8-12% of spherical graphite and clad material total weight;
4) spherical graphite being wrapped in clad material step 3) obtained carries out adding gentle isothermal holding, clad material melting is made to be wrapped in spherical graphite surface, and the organic principle in clad material is volatilized, stable sizing carbon coating layer is formed on spherical graphite surface, and carbon nano-tube forms network distribution on spherical graphite surface, obtains semifinished material; Wherein heating-up temperature is 500-800 DEG C, and the time controling of temperature-rise period is at 6-8 hour, and temperature retention time controls at 2-5 hour;
5) semifinished material step 4) obtained carries out high temperature graphitization process, carbon nano-tube and spherical graphite is made to form organic combination, even carbon nanotube dispersion, be wrapped in spherical graphite surface and spherical graphite surface formed grid structure, carbon nano-tube directly and spherical graphite form entirety, generate class bobbles shape, obtained Novel carbon-carbon nanotube lithium ion battery cathode material; The described high temperature graphitization processing time is 4-7 days, and temperature is 2800-3000 DEG C, and the temperature-rise period time is 8-12 hour, and the insulating process time is 2-5 hour.
The Novel carbon-carbon nanotube lithium ion battery cathode material that the present invention obtains, spread through multiple fractionation, solve the agglomeration of carbon nano-tube well, clad material is wrapped in spherical graphite surface, carbon nano-tube is in the grid structure of spherical graphite Surface Creation class bobbles shape, enhance surface strength, substantially improve electric conductivity, anti-decay property, discharge capacity has had significant raising especially first.Spherical graphite has higher lithium storage content, good voltage platform, and cheap, is one of negative material common on Vehicles Collected from Market.The interlamellar spacing of carbon nano-tube is slightly larger than the interlamellar spacing of spherical graphite, and the tubular structure of carbon nano-tube can not subside after the circulation of repeatedly charge-discharge, good cycle, carbon nano-tube has larger draw ratio and good axial one-dimensional electric ability simultaneously, is considered to desirable electric conducting material.The present invention is by improving spherical graphite surface, uniform coating layer is formed at graphite surface, carbon nano-tube is made to be wrapped in spherical graphite surface, grid structure is formed on spherical graphite surface, generate class bobbles shape, strengthen surface strength, and give full play to the premium properties of carbon nano-tube, improve the conductivity of negative material, gram specific capacity, anti-decay property and excellent multiplying power property, discharge capacity can reach 390mAh/g first.The present invention makes advantages of simple, and lithium storage content is high, and voltage platform is good, cheap, can not subside after repeatedly charge-discharge circulation, good cycle.
Embodiment
Novel carbon-carbon nanotube lithium ion battery cathode material, be made up of spherical graphite and the clad material that is wrapped in spherical graphite surface, described clad material accounts for the 8-12% of spherical graphite and clad material total weight; Described clad material mixes obtained by carbon nano-tube and organic carbon dust, and wherein the weight ratio of carbon nano-tube and organic carbon dust is 3:7.The particle diameter of clad material is 2-6 μm.
The preparation method of Novel carbon-carbon nanotube lithium ion battery cathode material, comprises the following steps:
1) raw material is got ready: spherical graphite, carbon nano-tube, organic carbon dust;
2) carbon nano-tube of step 1), organic carbon dust are put into ball mill in batches and carried out multiple fractionation mixing, when putting in batches, wherein a kind of material is disposable puts into, another kind of material average mark is put into for five times, the interval time of at every turn putting into is 1-2 hour, total incorporation time is 10-12 hour, obtains clad material, and the particle diameter of clad material is 2-6 μm; The weight ratio of described carbon nano-tube and organic carbon dust is 3:7;
3) by the spherical graphite of step 1) and step 2) obtained clad material carries out stirring makes it fully mix, and the time of being uniformly mixed is 1-3 hour, makes clad material evenly be wrapped in spherical graphite surface; Described clad material accounts for the 8-12% of spherical graphite and clad material total weight;
4) spherical graphite being wrapped in clad material step 3) obtained carries out adding gentle isothermal holding, clad material melting is made to be wrapped in spherical graphite surface, and the organic principle in clad material is volatilized, stable sizing carbon coating layer is formed on spherical graphite surface, and carbon nano-tube forms network distribution on spherical graphite surface, obtains semifinished material; Wherein heating-up temperature is 500-800 DEG C, and the time controling of temperature-rise period is at 6-8 hour, and temperature retention time controls at 2-5 hour;
5) semifinished material step 4) obtained carries out high temperature graphitization process, carbon nano-tube and spherical graphite is made to form organic combination, even carbon nanotube dispersion, be wrapped in spherical graphite surface and spherical graphite surface formed grid structure, carbon nano-tube directly and spherical graphite form entirety, generate class bobbles shape, obtained Novel carbon-carbon nanotube lithium ion battery cathode material; The described high temperature graphitization processing time is 4-7 days, and temperature is 2800-3000 DEG C, and the temperature-rise period time is 8-12 hour, and the insulating process time is 2-5 hour.
Embodiment 1
The preparation method of Novel carbon-carbon nanotube lithium ion battery cathode material, comprises the following steps:
1) spherical graphite of 10KG is got ready as forming core matrix and carbon nano-tube, organic carbon dust;
2) carbon nano-tube of step 1), organic carbon dust are put into ball mill in batches and carried out multiple fractionation mixing, first carbon nano-tube is all put into ball mill, again organic carbon dust average mark is put into for five times, the interval time of at every turn putting into is 1.5 hours, total incorporation time is 10 hours, obtain clad material 0.87KG, the particle diameter of clad material is 2 μm; The weight ratio of described carbon nano-tube and organic carbon dust is 3:7;
3) spherical graphite of 10KG and the clad material of 0.87KG are carried out in agitating device fully stir 1 hour, make clad material evenly be wrapped in spherical graphite surface; Described clad material accounts for 8% of spherical graphite and clad material total weight;
4) spherical graphite being wrapped in clad material step 3) obtained carries out adding gentle isothermal holding, heating-up temperature linearly rises, within 6 hours, be warmed up to 500 DEG C, and keep the temperature 2 hours of 500 DEG C, make clad material melting be wrapped in spherical graphite surface, and the organic principle in clad material is volatilized, formed stable sizing carbon coating layer on spherical graphite surface, and carbon nano-tube forms network distribution on spherical graphite surface, obtains semifinished material;
5) semifinished material step 4) obtained high temperature graphitization process 4 days under the high temperature of 2800 DEG C, the temperature-rise period time is 8 hours, the insulating process time is 2 hours, carbon nano-tube and spherical graphite is made to form organic combination, even carbon nanotube dispersion, be wrapped in spherical graphite surface and spherical graphite surface formed grid structure, carbon nano-tube directly and spherical graphite form entirety, generate class bobbles shape, be beneficial to the conductivity, gram specific capacity, the anti-decay property that improve negative material, obtained Novel carbon-carbon nanotube lithium ion battery cathode material.
Embodiment 2
The preparation method of Novel carbon-carbon nanotube lithium ion battery cathode material, comprises the following steps:
1) spherical graphite of 10KG is got ready as forming core matrix and carbon nano-tube, organic carbon dust;
2) carbon nano-tube of step 1), organic carbon dust are put into ball mill in batches and carried out multiple fractionation mixing, first organic carbon dust is all put into ball mill, again carbon nano-tube average mark is put into for five times, the interval time of at every turn putting into is 1 hour, total incorporation time is 10 hours, obtain clad material 1.11KG, the particle diameter of clad material is 3 μm; The weight ratio of described carbon nano-tube and organic carbon dust is 3:7;
3) spherical graphite of 10KG and the clad material of 1.11KG are carried out in agitating device fully stir 1.5 hours, make clad material evenly be wrapped in spherical graphite surface; Described clad material accounts for 10% of spherical graphite and clad material total weight;
4) spherical graphite being wrapped in clad material step 3) obtained carries out adding gentle isothermal holding, heating-up temperature linearly rises, within 7 hours, be warmed up to 700 DEG C, and keep the temperature 3 hours of 700 DEG C, make clad material melting be wrapped in spherical graphite surface, and the organic principle in clad material is volatilized, formed stable sizing carbon coating layer on spherical graphite surface, and carbon nano-tube forms network distribution on spherical graphite surface, obtains semifinished material;
5) semifinished material step 4) obtained high temperature graphitization process 5 days under the high temperature of 2800 DEG C, the temperature-rise period time is 9 hours, the insulating process time is 3 hours, carbon nano-tube and spherical graphite is made to form organic combination, even carbon nanotube dispersion, be wrapped in spherical graphite surface and spherical graphite surface formed grid structure, carbon nano-tube directly and spherical graphite form entirety, generate class bobbles shape, be beneficial to the conductivity, gram specific capacity, the anti-decay property that improve negative material, obtained Novel carbon-carbon nanotube lithium ion battery cathode material.
Embodiment 3
The preparation method of Novel carbon-carbon nanotube lithium ion battery cathode material, comprises the following steps:
1) spherical graphite of 10KG is got ready as forming core matrix and carbon nano-tube, organic carbon dust;
2) carbon nano-tube of step 1), organic carbon dust are put into ball mill in batches and carried out multiple fractionation mixing, first carbon nano-tube is all put into ball mill, again organic carbon dust average mark is put into for five times, the interval time of at every turn putting into is 1.5 hours, total incorporation time is 12 hours, obtain clad material 1.11KG, the particle diameter of clad material is 4 μm; The weight ratio of described carbon nano-tube and organic carbon dust is 3:7;
3) spherical graphite of 10KG and the clad material of 1.11KG are carried out in agitating device fully stir 2 hours, make clad material evenly be wrapped in spherical graphite surface; Described clad material accounts for 10% of spherical graphite and clad material total weight;
4) spherical graphite being wrapped in clad material step 3) obtained carries out adding gentle isothermal holding, heating-up temperature linearly rises, within 7 hours, be warmed up to 800 DEG C, and keep the temperature 4 hours of 800 DEG C, make clad material melting be wrapped in spherical graphite surface, and the organic principle in clad material is volatilized, formed stable sizing carbon coating layer on spherical graphite surface, and carbon nano-tube forms network distribution on spherical graphite surface, obtains semifinished material;
5) semifinished material step 4) obtained high temperature graphitization process 6 days under the high temperature of 3000 DEG C, the temperature-rise period time is 10 hours, the insulating process time is 4 hours, carbon nano-tube and spherical graphite is made to form organic combination, even carbon nanotube dispersion, be wrapped in spherical graphite surface and spherical graphite surface formed grid structure, carbon nano-tube directly and spherical graphite form entirety, generate class bobbles shape, be beneficial to the conductivity, gram specific capacity, the anti-decay property that improve negative material, obtained Novel carbon-carbon nanotube lithium ion battery cathode material.
Embodiment 4
The preparation method of Novel carbon-carbon nanotube lithium ion battery cathode material, comprises the following steps:
1) spherical graphite of 10KG is got ready as forming core matrix and carbon nano-tube, organic carbon dust;
2) carbon nano-tube of step 1), organic carbon dust are put into ball mill in batches and carried out multiple fractionation mixing, first organic carbon dust is all put into ball mill, again carbon nano-tube average mark is put into for five times, the interval time of at every turn putting into is 1.5 hours, total incorporation time is 12 hours, obtain clad material 1.24KG, the particle diameter of clad material is 2 μm; The weight ratio of described carbon nano-tube and organic carbon dust is 3:7;
3) spherical graphite of 10KG and the clad material of 1.24KG are carried out in agitating device fully stir 3 hours, make clad material evenly be wrapped in spherical graphite surface; Described clad material accounts for 11% of spherical graphite and clad material total weight;
4) spherical graphite being wrapped in clad material step 3) obtained carries out adding gentle isothermal holding, heating-up temperature linearly rises, within 7 hours, be warmed up to 800 DEG C, and keep the temperature 5 hours of 800 DEG C, make clad material melting be wrapped in spherical graphite surface, and the organic principle in clad material is volatilized, formed stable sizing carbon coating layer on spherical graphite surface, and carbon nano-tube forms network distribution on spherical graphite surface, obtains semifinished material;
5) semifinished material step 4) obtained high temperature graphitization process 7 days under the high temperature of 3000 DEG C, the temperature-rise period time is 10 hours, the insulating process time is 4 hours, carbon nano-tube and spherical graphite is made to form organic combination, even carbon nanotube dispersion, be wrapped in spherical graphite surface and spherical graphite surface formed grid structure, carbon nano-tube directly and spherical graphite form entirety, generate class bobbles shape, be beneficial to the conductivity, gram specific capacity, the anti-decay property that improve negative material, obtained Novel carbon-carbon nanotube lithium ion battery cathode material.
Embodiment 5
The preparation method of Novel carbon-carbon nanotube lithium ion battery cathode material, comprises the following steps:
1) spherical graphite of 10KG is got ready as forming core matrix and carbon nano-tube, organic carbon dust;
2) carbon nano-tube of step 1), organic carbon dust are put into ball mill in batches and carried out multiple fractionation mixing, first carbon nano-tube is all put into ball mill, again organic carbon dust average mark is put into for five times, the interval time of at every turn putting into is 2 hours, total incorporation time is 12 hours, obtain clad material 1.36KG, the particle diameter of clad material is 6 μm; The weight ratio of described carbon nano-tube and organic carbon dust is 3:7;
3) spherical graphite of 10KG and the clad material of 1.36KG are carried out in agitating device fully stir 3 hours, make clad material evenly be wrapped in spherical graphite surface; Described clad material accounts for 12% of spherical graphite and clad material total weight;
4) spherical graphite being wrapped in clad material step 3) obtained carries out adding gentle isothermal holding, heating-up temperature linearly rises, within 8 hours, be warmed up to 800 DEG C, and keep the temperature 4 hours of 800 DEG C, make clad material melting be wrapped in spherical graphite surface, and the organic principle in clad material is volatilized, formed stable sizing carbon coating layer on spherical graphite surface, and carbon nano-tube forms network distribution on spherical graphite surface, obtains semifinished material;
5) semifinished material step 4) obtained high temperature graphitization process 7 days under the high temperature of 2900 DEG C, the temperature-rise period time is 10 hours, the insulating process time is 4 hours, carbon nano-tube and spherical graphite is made to form organic combination, even carbon nanotube dispersion, be wrapped in spherical graphite surface and spherical graphite surface formed grid structure, carbon nano-tube directly and spherical graphite form entirety, generate class bobbles shape, be beneficial to the conductivity, gram specific capacity, the anti-decay property that improve negative material, obtained Novel carbon-carbon nanotube lithium ion battery cathode material.
Below be only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (1)
1. a preparation method for Novel carbon-carbon nanotube lithium ion battery cathode material, is characterized in that, comprises the following steps:
1) raw material is got ready: spherical graphite, carbon nano-tube, organic carbon dust;
2) by step 1) carbon nano-tube, organic carbon dust put into ball mill in batches and carry out multiple fractionation mixing, when putting in batches, wherein a kind of material is disposable puts into, another kind of material average mark is put into for five times, the interval time of at every turn putting into is 1-2 hour, total incorporation time is 10-12 hour, obtains clad material, and the particle diameter of clad material is 2-6 μm; The weight ratio of described carbon nano-tube and organic carbon dust is 3:7;
3) by step 1) spherical graphite and step 2) obtained clad material carries out stirring makes it fully mix, the time of being uniformly mixed is 1-3 hour, makes clad material evenly be wrapped in spherical graphite surface; Described clad material accounts for the 8-12% of spherical graphite and clad material total weight;
4) by step 3) spherical graphite being wrapped in clad material that obtains carries out adding gentle isothermal holding, clad material melting is made to be wrapped in spherical graphite surface, and the organic principle in clad material is volatilized, stable sizing carbon coating layer is formed on spherical graphite surface, and carbon nano-tube forms network distribution on spherical graphite surface, obtains semifinished material; Wherein heating-up temperature is 500-800 DEG C, and the time controling of temperature-rise period is at 6-8 hour, and temperature retention time controls at 2-5 hour;
5) by step 4) semifinished material that obtains carries out high temperature graphitization process, carbon nano-tube and spherical graphite is made to form organic combination, even carbon nanotube dispersion, be wrapped in spherical graphite surface and spherical graphite surface formed grid structure, carbon nano-tube directly and spherical graphite form entirety, generate class bobbles shape, obtained Novel carbon-carbon nanotube lithium ion battery cathode material; The described high temperature graphitization processing time is 4-7 days, and wherein warm temperature is 2800-3000 DEG C, and the temperature-rise period time is 8-12 hour, and the insulating process time is 2-5 hour.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106532045A (en) * | 2015-09-15 | 2017-03-22 | 宁德新能源科技有限公司 | Graphite negative electrode material of lithium ion battery and preparation method for graphite negative electrode material |
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| CN107845794A (en) * | 2017-10-31 | 2018-03-27 | 湖南国盛石墨科技有限公司 | A kind of preparation method of the spherical micro crystal graphite negative material of CNT/Lauxite carbon coating |
| CN111313012A (en) * | 2020-03-30 | 2020-06-19 | 江西远东电池有限公司 | Multiwalled carbon nanotube graphite lithium ion battery negative electrode material and preparation method thereof |
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| CN1373526A (en) * | 2002-01-04 | 2002-10-09 | 华南理工大学 | Lithium-bearing composite nano carbon tube-graphite material and its preparing process |
| CN1567617A (en) * | 2003-06-20 | 2005-01-19 | 比亚迪股份有限公司 | Method for preparing a carbon cathode material of lithium ion battery |
| CN102832378A (en) * | 2012-08-28 | 2012-12-19 | 浙江瓦力新能源科技有限公司 | Carbon anode material for lithium ion battery and preparation method for carbon anode material |
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| CN1373526A (en) * | 2002-01-04 | 2002-10-09 | 华南理工大学 | Lithium-bearing composite nano carbon tube-graphite material and its preparing process |
| CN1567617A (en) * | 2003-06-20 | 2005-01-19 | 比亚迪股份有限公司 | Method for preparing a carbon cathode material of lithium ion battery |
| CN102832378A (en) * | 2012-08-28 | 2012-12-19 | 浙江瓦力新能源科技有限公司 | Carbon anode material for lithium ion battery and preparation method for carbon anode material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106532045A (en) * | 2015-09-15 | 2017-03-22 | 宁德新能源科技有限公司 | Graphite negative electrode material of lithium ion battery and preparation method for graphite negative electrode material |
| CN106532045B (en) * | 2015-09-15 | 2019-10-29 | 宁德新能源科技有限公司 | Graphite negative material of lithium ion battery and preparation method thereof |
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