CN110350178A - A kind of preparation method of lithium ion battery composite graphite negative electrode material - Google Patents
A kind of preparation method of lithium ion battery composite graphite negative electrode material Download PDFInfo
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- CN110350178A CN110350178A CN201910631639.2A CN201910631639A CN110350178A CN 110350178 A CN110350178 A CN 110350178A CN 201910631639 A CN201910631639 A CN 201910631639A CN 110350178 A CN110350178 A CN 110350178A
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- 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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Abstract
The invention discloses a kind of preparation methods of lithium ion battery composite graphite negative electrode material, it is related to lithium ion battery negative material field, using carbon product waste material, spherical natural graphite as raw material, carbon product waste material is crushed, shaping classification, carbon product waste material graphite powder is made except magnetic, carbon product waste material graphite powder, the spherical natural graphite are mixed in certain mass ratio, lithium ion battery composite graphite negative electrode material is obtained after screening.The present invention combine natural graphite high compacted density, high lithium storage content and the excellent cycle performance of carbon product waste material, it is at low cost the advantages that, lithium storage content, first charge-discharge efficiency, cycle performance and the processing performance that ensure that material, improve the cost performance of material.
Description
Technical field
The present invention relates to lithium ion battery negative material field, specially a kind of lithium ion battery composite graphite negative electrode material
Preparation method.
Background technique
Although the graphite cathode material of lithium ion battery has been commercialized, there is also some weakness for being difficult to overcome, exploitations
The more excellent negative electrode material of performance is still the important topic of Study on Li-ion batteries.The cathode of lithium ion battery is by cathode
Active material carbon material or non-carbon material, adhesive, additive are mixed and made into paste binder and are coated uniformly on copper foil, through dry
It is dry, roll.It is made to lithium ion battery success, can key be prepare the negative of reversibly de-/embedding lithium ion
Pole material.The selection of negative electrode material directly affects the performance of lithium ion battery.
Though natural graphite has higher specific capacity, compacted density in Carbon Materials, it is easy to react with electrolyte, makes
The removing that solvent molecule was embedded in altogether and caused graphite linings is obtained, the reversible capacity of battery reduces, under the cycle performance of lithium ion battery
Drop.And one of graphite type material artificial graphite is due to firm structural stability, excellent embedding lithium characteristic and long circulating
The advantages that service life, excellent pole piece processing performance, obtains extensive affirmative and use in the industry.But simultaneously its that there are capacity is relatively low, compacting
The disadvantages of density is relatively low limits its extensive use in lithium ion battery negative material.Therefore, how to develop one kind has
High lithium storage content, high compacted density, high first charge-discharge efficiency, high circulation service life, have both existing artificial graphite and natural graphite
Advantage, cost performance is high and can be used as the negative electrode material of lithium ion battery, be that the technology urgently to be resolved of this field one is asked
Topic.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of lithium ion battery composite graphite negative electrode material, to solve
The problem of be make negative electrode material have higher lithium storage content, better first charge-discharge efficiency and cycle performance, higher pressure
Real density meets requirement of the high performance lithium ion battery especially power lithium-ion battery to negative electrode material, while making material
Preparation is simpler, and cost is less expensive, easy to industrialized production.
In order to solve the above-mentioned technical problems, the present invention provides a kind of lithium ion battery composite graphite negative electrode materials, with charcoal
Cellulose product waste material, spherical natural graphite as raw material, crushed by carbon product waste material, shaping classification, except magnetic after with spherical day
For right graphite in being made after the mixing screening of certain mass ratio, lithium ion battery composite graphite negative electrode material average grain diameter is 12~20
μm。
Optionally, the lithium ion battery composite graphite negative electrode material average grain diameter is 14~18 μm, and tap density is big
In or equal to 1.05g/cm3, specific surface area is less than or equal to 3.0m2/g。
Optionally, the lithium ion battery composite graphite negative electrode material iron-content is less than or equal to 50ppm.
Optionally, the spherical natural graphite average grain diameter is 15~20 μm, and tap density is more than or equal to 1.10g/
cm3, specific surface area is less than or equal to 2.0m2/g。
Optionally, the preparation method of the lithium ion battery composite graphite negative electrode material, comprising the following steps:
S1, carbon product waste material is crushed, shaping is classified to obtain carbon product waste material graphite powder;
S2, carbon product waste material graphite powder is added to electromagnetism except in chinaware, carrying out except magnetic, so that carbon product waste material stone
The iron-content of ink powder is less than or equal to 80ppm, obtains carbon product waste material graphite powder;
S3, carbon product waste material graphite powder and spherical natural graphite are mixed in a high speed mixer in certain mass ratio
It closes, gets lithium ion battery composite graphite negative electrode material using sifted.
Optionally, carbon product waste material described in the step S1 includes graphite jig, graphite brake block, nuclear graphite.
Optionally, carbon product waste material graphite powder average grain diameter described in the step S2 is 12~18 μm, tap density
For 0.85~1.15g/cm3, specific surface area is 2~5m2/g。
Optionally, carbon product waste material graphite powder/spherical natural graphite=1/4~2/ in mass ratio described in step S3
3。
Optionally, in the step S2, electromagnetism is 25000~30000Gs, carbon product waste material stone except the magnetic flux of chinaware
The speed that ink powder adds is 20~40kg/min.
Optionally, in the step S3, the revolving speed of high-speed mixer is 300~500r/min, when stirring a length of 4h~8h,
Sifted subhead number is 250~400 mesh.
Compared with prior art, the beneficial effects of the present invention are: the present invention to provide a kind of lithium ion battery composite graphite negative
The preparation method of pole material will solve the problems, such as it is to make cathode material using carbon product waste material, spherical natural graphite as raw material
Material has higher lithium storage content, better first charge-discharge efficiency and cycle performance, and higher compacted density meets high-performance
Requirement of the lithium ion battery especially power lithium-ion battery to negative electrode material, while keeping the preparation of material simpler, cost is more
It is cheap, it is easy to industrialized production.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
The present invention provides a kind of preparation method of lithium ion battery composite graphite negative electrode material, with carbon product waste material, ball
Shape natural graphite is raw material, and carbon product waste material is crushed, shaping classification, carbon product waste material graphite powder is made except magnetic
Material, which is mixed in certain mass ratio, obtained after screening lithium from
Sub- battery composite graphite negative electrode material.Wherein, the average grain diameter of lithium ion battery composite graphite negative electrode material of the present invention be 12~
20μm.Lithium ion battery composite graphite negative electrode material average grain diameter preferably of the invention is 14~18 μm;Its tap density is
More than or equal to 1.05g/cm3, specific surface area is less than or equal to 3.0m2/g。
Carbon product waste material be the used waste materials of carbon industry carbon product, it is cheap, degree of graphitization compared with
Height, stable structure.It is used as the raw material of lithium ion battery negative material, not only can be salvaged, reduce cost, also as
Lack graphitization process section, reduces discharge, the protection environment of pollutant.
The granularity of carbon product waste material graphite powder, tap density compare table in lithium ion battery composite graphite negative electrode material
Area, all can structure, pattern, compacted density to obtained lithium ion battery negative material produce a very large impact, thus shadow
Ring its cycle life, compacted density.
In lithium ion battery composite graphite negative electrode material the content of spherical natural graphite influence its lithium storage content, compacting it is close
Degree.Spherical natural graphite content is too low, and the lithium storage content of lithium ion battery, compacted density can reduce;Spherical natural graphite content
It is excessively high, the increased costs of lithium ion battery.
Correspondingly, the present invention also provides a kind of preparation sides of lithium ion battery composite graphite negative electrode material described above
Method, comprising the following steps:
S1, carbon product waste material is crushed, shaping is classified to obtain carbon product waste material graphite powder;
S2, carbon product waste material graphite powder is added to electromagnetism except in chinaware, carrying out except magnetic, so that carbon product waste material stone
The iron-content of ink powder is less than or equal to 80ppm, obtains carbon product waste material graphite powder;
S3, carbon product waste material graphite powder and spherical natural graphite are mixed in a high speed mixer in certain mass ratio
It closes, gets lithium ion battery composite graphite negative electrode material using sifted.
Carbon product waste material graphite powder average grain diameter is 12~18 μm, and tap density is 0.85~1.15g/cm3, compare table
Area is 2~5m2/g.If size distribution, tap density and specific surface area are more than this range, the cyclicity of lithium ion battery
Energy, compacted density can reduce.
Spherical natural graphite average grain diameter of the invention is 15~20 μm, and tap density is more than or equal to 1.10g/cm3,
Specific surface area is less than or equal to 2.0m2/g;Mass ratio is --- carbon product waste material graphite powder/spherical natural graphite=
1/4 to 2/3.
Electromagnetism except chinaware magnetic flux be 25000~30000Gs, the speed that carbon product waste material graphite powder adds be 20~
40kg/min。
The revolving speed of fast mixing machine is 300~500r/min, when stirring a length of 4h~8h, sifted subhead number is 250~
400 mesh.
Resulting lithium ion battery is prepared using lithium ion battery composite graphite negative electrode material of the present invention, for the first time reversible specific volume
Amount reaches 355mAh/g, and up to 92.5% or more, 500 weeks reversible capacities of circulation remain to be maintained at 410mAh/g first charge-discharge efficiency
More than, compacted density is up to 1.65~1.70g/cm3。
Below will with specific embodiment come the present invention is further explained.
Embodiment 1
S1, carbon product waste material is crushed, shaping is classified to obtain carbon product waste material graphite powder;
S2, carbon product waste material graphite powder is added to electromagnetism except in chinaware, carrying out except magnetic, electromagnetism removes the magnetic flux of chinaware
The speed that adds for 25000Gs, carbon product waste material graphite powder is 30kg/min, so that the iron content of carbon product waste material graphite powder
Amount is less than 80ppm, obtains carbon product waste material graphite powder, and carbon product waste material graphite powder average grain diameter is 14.57 μm, vibration
Real density is 0.95g/cm3, specific surface area 4.0m2/g。
S3, by carbon product waste material graphite powder and spherical natural graphite example in mass ratio --- carbon product waste material graphite
Powder/spherical natural graphite=1/4, mixes in a high speed mixer, and it is compound to get lithium ion battery using sifted
Graphite cathode material, the revolving speed 400/min of high-speed mixer, when stirring a length of 8h, sifted subhead number is 325 mesh;It is spherical
Natural graphite average grain diameter is 17.98 μm,;Tap density is 1.16g/cm3, specific surface area 1.6m2/g。
The average grain diameter of lithium ion battery composite graphite negative electrode material is 15.84 μm, tap density 1.06g/cm3, than
Surface area is 2.9m2/ g, iron-content≤50ppm.
Embodiment 2
S1, carbon product waste material is crushed, shaping is classified to obtain carbon product waste material graphite powder;
S2, carbon product waste material graphite powder is added to electromagnetism except in chinaware, carrying out except magnetic, so that carbon product waste material stone
The iron-content of ink powder is less than 80ppm, obtains carbon product waste material graphite powder, carbon product waste material graphite powder average grain diameter is
16.17 μm, tap density 1.05g/cm3, specific surface area 3.2m2/g。
S3, by carbon product waste material graphite powder and spherical natural graphite example in mass ratio --- carbon product waste material graphite
Powder/spherical natural graphite=1/4, mixes in a high speed mixer, and it is compound to get lithium ion battery using sifted
Graphite cathode material carbon product waste material, the revolving speed 400/min of high-speed mixer, when stirring a length of 8h, sifted subhead number
For 325 mesh;Spherical natural graphite average grain diameter is 17.98 μm, tap density 1.16g/cm3, specific surface area 1.6m2/g。
The size distribution of lithium ion battery composite graphite negative electrode material is that average grain diameter is 16.89 μm, and tap density is
1.08g/cm3, specific surface area 2.6m2/ g, iron-content≤50ppm.
Embodiment 3
S1, carbon product waste material is crushed, shaping is classified to obtain carbon product waste material graphite powder;
S2, carbon product waste material graphite powder is added to electromagnetism except in chinaware, carrying out except magnetic, so that carbon product waste material stone
The iron-content of ink powder is less than 80ppm, obtains carbon product waste material graphite powder, carbon product waste material graphite powder average grain diameter is
16.17 μm, tap density 1.10g/cm3, specific surface area 3.2m2/g。
S3, by carbon product waste material graphite powder and spherical natural graphite example in mass ratio --- carbon product waste material graphite
Powder/spherical natural graphite=2/3, mixes in a high speed mixer, and it is compound to get lithium ion battery using sifted
The revolving speed 400/min of graphite cathode material high-speed mixer, when stirring a length of 8h, sifted subhead number is 325 mesh;Spherical day
Right graphite average grain diameter is 17.98 μm, tap density 1.16g/cm3, specific surface area 1.6m2/g。
The average grain diameter of lithium ion battery composite graphite negative electrode material is 17.21 μm, tap density 1.13g/cm3, than
Surface area is 2.5m2/ g, iron-content≤50ppm.
Identical lithium ion is made to the lithium ion battery composite graphite negative electrode material of embodiment 1, embodiment 2, embodiment 3
Battery, wherein performance of lithium ion battery is as follows:
As can be seen from the above table, resulting lithium-ion electric is prepared using lithium ion battery composite graphite negative electrode material of the present invention
Reversible specific capacity reaches 355mAh/g for the first time in pond, and up to 92.5% or more, 500 weeks reversible capacities of circulation remain to first charge-discharge efficiency
It is maintained at 410mAh/g or more, compacted density is up to 1.65~1.70g/cm3;Therefore obtained lithium ion battery through the invention
Composite graphite negative electrode material is applied to have excellent electrochemical performance in lithium ion battery.
It is born in conclusion the present invention is used as using cheap carbon product waste material as lithium ion battery composite graphite
The raw material of pole material.General artificial graphite will pass through graphitization and the material in carbon product waste material production process does not have to again
Graphitization, reduces process, reduces costs.In addition, the present invention is designed the granularity of carbon product waste material graphite powder,
So that its size distribution is in certain range, with improve lithium ion battery composite graphite negative electrode material first charge-discharge efficiency and
Cycle performance.Its simple production process, high production efficiency is at low cost, and process safety can be used for industrialized production, effectively
Reduce the cost of lithium ion battery.
The present invention mixes spherical natural graphite with carbon product waste material graphite powder, utilizes the Gao Rong of spherical natural graphite
Amount, high compacted density, to improve lithium storage content, the compacted density of lithium ion battery composite graphite negative electrode material.And it is existing
Spherical natural graphite is separately as lithium ion battery negative material, since spherical natural graphite surface group is easy to be total to electrolyte
Insertion causes its cycle performance, electrolyte compatibility that will be deteriorated, and such disadvantage is then not present in artificial plumbago negative pole material,
Therefore spherical natural graphite of the present invention and carbon product waste material graphite powder are mixed with extremely excellent cycle performance and electrolysis
Liquid compatibility.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any label in claim should not be construed as limiting the claims involved.
Claims (10)
1. a kind of preparation method of lithium ion battery composite graphite negative electrode material, it is characterised in that: by carbon product waste material through powder
Broken, shaping classification, except mixing after sieving after magnetic with spherical natural graphite, screening is obtained, lithium ion battery composite graphite negative electrode material
Average grain diameter is 12~20 μm.
2. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to claim 1, it is characterised in that:
Lithium ion battery composite graphite negative electrode material average grain diameter is 14~18 μm, and tap density is more than or equal to 1.05g/cm3, than
Surface area is less than or equal to 3.0m2/g。
3. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to claim 1, it is characterised in that:
Lithium ion battery composite graphite negative electrode material iron-content is less than or equal to 50ppm.
4. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to claim 1, it is characterised in that:
The spherical natural graphite average grain diameter is 15~20 μm, and tap density is more than or equal to 1.10g/cm3, surface area be less than
Or it is equal to 2.0m2/g。
5. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to any one of claims 1 to 4,
It is characterized in that, comprising the following steps:
S1, carbon product waste material is crushed, shaping is classified to obtain carbon product waste material graphite powder;
S2, carbon product waste material graphite powder is added to electromagnetism except in chinaware, carrying out except magnetic, so that carbon product waste material graphite powder
Iron-content be less than or equal to 80ppm, obtain carbon product waste material graphite powder;
S3, carbon product waste material graphite powder and spherical natural graphite are mixed in a high speed mixer in certain mass ratio,
Get lithium ion battery composite graphite negative electrode material using sifted.
6. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to claim 5, it is characterised in that:
Carbon product waste material described in step S1 includes graphite jig, graphite brake block, nuclear graphite.
7. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to claim 5, it is characterised in that:
Carbon product waste material graphite powder average grain diameter described in step S2 is 12~18 μm, and tap density is 0.85~1.15g/cm3,
Specific surface area is 2~5m2/g。
8. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to claim 5, it is characterised in that:
Carbon product waste material graphite powder/spherical natural graphite=1/4~2/3 in mass ratio described in step S3.
9. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to claim 5, it is characterised in that:
In the step S2, carbon product waste material graphite powder is added to electromagnetism except in chinaware, electromagnetism is 25000 except the magnetic flux of chinaware
The speed that adds of~30000Gs, carbon product waste material graphite powder are 20~40kg/min.
10. a kind of preparation method of lithium ion battery composite graphite negative electrode material according to claim 5, feature exist
In: the revolving speed of the step S3 high speed mixing machine be 300~500r/min, when stirring a length of 4~8h, sifted subhead number
For 250~400 mesh.
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Cited By (4)
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CN110729455A (en) * | 2019-10-24 | 2020-01-24 | 石家庄尚太科技有限公司 | Preparation method of lithium ion negative electrode material and lithium ion negative electrode material |
CN112652767A (en) * | 2020-12-03 | 2021-04-13 | 上海杉杉科技有限公司 | Preparation method of soft carbon negative electrode material of lithium ion battery |
CN112670504A (en) * | 2020-12-25 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Modified resistance material, graphite negative electrode material containing modified resistance material, and preparation method and application of graphite negative electrode material |
CN113422025A (en) * | 2021-06-25 | 2021-09-21 | 洛阳月星新能源科技有限公司 | Natural graphite composite material and preparation method thereof |
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