CN103241731B - The preparation method of compound graphite material for lithium ion secondary battery - Google Patents
The preparation method of compound graphite material for lithium ion secondary battery Download PDFInfo
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- 239000007770 graphite material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 15
- 150000001875 compounds Chemical class 0.000 title claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 61
- 239000010439 graphite Substances 0.000 claims abstract description 61
- 229910021382 natural graphite Inorganic materials 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 238000005087 graphitization Methods 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000011230 binding agent Substances 0.000 claims abstract description 20
- 229910021383 artificial graphite Inorganic materials 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 238000012545 processing Methods 0.000 claims abstract description 15
- 230000000750 progressive effect Effects 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011280 coal tar Substances 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000011246 composite particle Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000012946 outsourcing Methods 0.000 abstract 1
- 239000011295 pitch Substances 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000008151 electrolyte solution Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000005056 compaction Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000006664 bond formation reaction Methods 0.000 description 2
- 239000011294 coal tar pitch Substances 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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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Abstract
The invention discloses a kind of preparation method of compound graphite material for lithium ion secondary battery, first the method drops into as the natural graphite of raw material, binding agent, graphite catalyst in rotary drum furnace, and raw material launch process intermediate roll keeps rotating state simultaneously; Then carry out progressive heating to raw material: adopt progressive heat temperature raising mode to heating raw materials in stove, heat-processed intermediate roll stove keeps rotating, and then in stove, raw material, after heating, naturally cools to normal temperature; Finally graphitization processing is carried out to raw material; Through above-mentioned process, binding agent forms synthetic graphite, and synthetic graphite is formed coated to natural graphite particles, and then forms nucleocapsid structure, simultaneously the composite graphite particles of particle diameter needed for the further bonding one-tenth of nucleocapsid structure composite particles.By the composite graphite material that the present invention makes, using natural graphite as kernel, the nucleocapsid structure of outsourcing rostone layer of ink, this composite graphite isotropy is good, capacity is high, compacting is high, multiplying power, low temperature and cycle performance excellent, electrode expansion is low.Manufacture method of the present invention adopts coated and bonding method of simultaneously carrying out, and prepare simple, cost is low.
Description
Technical field
The present invention relates to lithium ion battery negative material preparation method field, particularly a kind of preparation method of compound graphite material for lithium ion secondary battery, the graphite material prepared by the method forms a kind of nucleocapsid structure, and nucleocapsid structure graphite granule is through isotropic composite graphite particles material of bonding formation.
Background technology
Due to the development of the electronics of advanced person, people increase day by day for the demand of small-sized, lightweight, portable electronics and device.Require longer duration of service after charging, therefore, the battery needing to have high-energy-density provides the energy for this equipment and device.
Lithium ion battery negative material, as the important component part of lithium ion battery, comparatively large to cell container contribution, the negative material studied at present comprises: graphite, hard carbon, soft carbon, silicon-base alloy, tin-based alloy etc.Be badly in need of the capacity improving negative material, simultaneously when retention, improve compacted density.
Natural graphite has that cost is low, capacity is high (>=360mAh/g), the feature of good processability, however exist with compatibility of electrolyte poor, the shortcoming that cycle performance is poor.Simultaneously single graphite granule is generally 15-20 micron, and graphite granule is comparatively large, and graphite is laminated structure simultaneously, high anisotropy, makes that lithium ion is de-, embedding path length, prepared battery multiplying power, poor performance at low temperatures.
For overcoming the above problems, improve the circulation of natural graphite, multiplying power and low-temperature performance, Japanese Patent JP2000-182617 by natural graphite and pitch or other mixed with resin, through pulverizing, charing, greying, the deficiency of natural graphite can be improved, improve the cycle performance of graphite.Height-oriented Graphite Powder 99 mixes with mesophase pitch by Japanese Patent JP2002-373656, through pulverizing, classification, calcining, greying and obtained matrix material, combines the excellent properties of heavy body and mesophase spherule, improves efficiency, circulation and compaction capacity.Natural graphite mixes with pitch by Japanese Patent JP2003-173778 mutually, carries out machinery, graphitization processing, prepares spherical or oval composite graphite, this graphite take natural graphite as kernel, and synthetic graphite is shell, uses under high-pressure solid, irreversible capacity reduces, and cycle performance improves.Kernel is combined with shell closely, and not easily broken under high-pressure solid, coating layer is good with compatibility of electrolyte simultaneously, thus has the performance of excellence.
The material that above-mentioned patent system is standby, graphite granule is easy to form orientation, especially after compaction, graphite granule orientation on pole piece of flats, lithium ion is de-, embedding path length, and prepared battery multiplying power, low-temperature performance can not meet more and more higher requirement, and electrode expansion is larger simultaneously.
In addition, synthetic graphite Stability Analysis of Structures, good with compatibility of electrolyte, multiplying power, low temperature and cycle performance excellence (after circulation in 500 weeks, capability retention >=80%).For obtaining that capacity is high, compacting is high, the graphite cathode material of multiplying power, low temperature and cycle performance excellence, need the advantage in conjunction with natural graphite and synthetic graphite.
Summary of the invention
Technical problem to be solved by this invention is just the preparation method providing a kind of compound graphite material for lithium ion secondary battery, the Core-shell structure material that the composite graphite material prepared by the method is exactly take natural graphite as kernel, synthetic graphite is coating layer, this composite graphite material can provide heavy body (>=360mAh/g), and it can improve the consistency of graphite and electrolytic solution, provide excellent cycle performance.
For solving the problems of the technologies described above, present invention employs following technical scheme, this the method comprises the following steps: 1, raw material mixing: drop into as the natural graphite of raw material, binding agent, graphite catalyst in rotary drum furnace, and raw material launch process intermediate roll keeps rotating state simultaneously; In raw material, the mass percentage content of each composition is: natural graphite: 70% ~ 90%; Binding agent: 5% ~ 30%; Graphite catalyst: 1% ~ 5%; Wherein binding agent is the material that can form synthetic graphite after greying; Carrying out coated by stirring binding agent to natural graphite, realizing again the bonding of natural graphite; 2, progressive heating: progressive heat temperature raising mode is adopted to heating raw materials in stove, heat-processed intermediate roll stove keeps rotating, and it comprises the following heating phase: the first stage, normal temperature to 200 DEG C, and the time is 0.5-10 hour; Subordinate phase, 200 DEG C to 400 DEG C, the time is 1-10 hour; Phase III, 400 DEG C to 600 DEG C, the time is 1-10 hour; Fourth stage, 600 DEG C of constant temperature 1-10 hour; 3, cool: in stove, raw material is after heating, naturally cools to normal temperature; 4, greying: graphitization processing is carried out to raw material; Through above-mentioned process, binding agent forms synthetic graphite through process, and synthetic graphite is formed coated to natural graphite particles.
Furthermore, in technique scheme, the natural graphite that described natural graphite can select this area conventional, its median size is 1-20 micron, preferred 5-15 micron.
Furthermore, in technique scheme, described binding agent is pitch, coal tar, the one of resin or mixture.
Furthermore, in technique scheme, described what can select this area all size for pitch, coal tar, resin is pitch, coal tar, resin.Particle diameter can be less than 100 microns, is preferably less than 15 microns.
Furthermore, in technique scheme, the content of described graphite catalyst is 0.5% ~ 10% of the content of natural graphite.
Furthermore, in technique scheme, described graphitization catalyst is silicon, iron, the oxide compound of tin or carbide.
Furthermore, in technique scheme, described graphite catalyst is: SiO
2, SiC, Fe
2o
3, SnO
2one or its mixture.
Furthermore, in technique scheme, described graphitization processing adopts the graphitization processing of carrying out purifying under purifying gas.
Furthermore, in technique scheme, through processing the composite graphite material finally obtained, its center is natural graphite, natural graphite skin forms nucleocapsid structure by synthetic graphite particles is coated, core-shell structure particles forms porous composite structure particle further, and wherein the graphite small-particle of nucleocapsid structure has 2-20.
After the present invention adopts technique scheme, in order to be the isotropy of raising graphite further, under the prerequisite of guaranteed performance, obtain the negative material of more high compacted density (>=1.7g/cc), the present invention, by first controlling the particle diameter of natural/artificial nuclear's shell structure composite graphite, makes its particle diameter less, and then the graphite granule of particle diameter needed for further for nucleocapsid structure composite particles less for particle diameter bonding one-tenth, achieve the isotropy increasing graphite, add graphite internal void; Lithium ion can be moved to several direction, and be beneficial to electrolytic solution and infiltrate, form more lithium ion mobility passages, migration path is shorter, and improve the cycle performance of graphite, multiplying power, low-temperature performance, electrode expansion is less.
For ensureing the performance of graphite in high-pressure solid situation, the present invention introduces graphitization catalyst simultaneously, with in graphite pebbles surface pore-creating, improves graphite specific surface.Realize electrode (>=1.7g/cc) under high-pressure solid, also can keep enough electrolytic solution, increase the interfacial area of graphite and electrolytic solution simultaneously, improve battery multiplying power, low temperature and cycle performance further.
Marginal data
Fig. 1 is scanning electronic microscope (SEM) figure of the composite graphite particles according to the embodiment of the present invention 1 preparation.
Fig. 2 is the first charge-discharge graphic representation of the composite graphite particles according to the embodiment of the present invention 1 preparation.
Fig. 3 is the compaction capacity figure of electrode prepared by the composite graphite particles prepared according to the embodiment of the present invention 1.
Fig. 4 is the absorbent figure of the composite graphite particles according to the embodiment of the present invention 1 preparation.
Fig. 5 is the bounce-back scale map of the composite graphite particles according to the embodiment of the present invention 1 preparation.
Fig. 6 is the cycle performance figure of the composite graphite particles according to the embodiment of the present invention 1 preparation.
Fig. 7 is the high rate performance figure of the composite graphite particles according to the embodiment of the present invention 1 preparation.
Fig. 8 is the cold cycle performance map of the composite graphite particles according to the embodiment of the present invention 1 preparation.
Specific embodiment
Preparation method of the present invention comprises the following steps:
(1) raw material mixing: drop into as the natural graphite of raw material, binding agent, graphite catalyst in rotary drum furnace, and raw material launch process intermediate roll keeps rotating state simultaneously; In raw material, the mass percentage content of each composition is:
Natural graphite: 70% ~ 90%;
Binding agent: 5% ~ 30%;
Graphite catalyst: 1% ~ 5%;
Wherein binding agent is the material that can form synthetic graphite after greying; Carrying out coated by stirring binding agent to natural graphite, realizing again the bonding of natural graphite.
(2) progressive heating: adopt progressive heat temperature raising mode to heating raw materials in stove, heat-processed intermediate roll stove keeps rotating, regulating rotation speed of drum 10-100Hz.It comprises the following heating phase:
First stage, normal temperature to 200 DEG C, the time is 0.5-10 hour;
Subordinate phase, 200 DEG C to 400 DEG C, the time is 1-10 hour;
Phase III, 400 DEG C to 600 DEG C, the time is 1-10 hour;
Fourth stage, 600 DEG C of constant temperature 1-10 hour.
(3) cool: in stove, raw material is after heating, naturally cools to normal temperature.
(4) greying: graphitization processing is carried out to raw material.
Through above-mentioned process, binding agent forms synthetic graphite through process, and synthetic graphite is formed coated to natural graphite particles.
The natural graphite that natural graphite described in step 1 can select this area conventional, its median size is 1-20 micron, preferred 5-15 micron.
Caking agent described in step 1 can select the conventional caking agent of this area, and can form synthetic graphite after greying, is generally pitch, coal tar, the one of resin or its mixture.It is described that what can select this area all size for pitch, coal tar, resin is pitch, coal tar, resin.Particle diameter can be less than 100 microns, is preferably less than 15 microns.
Silicon, iron, the oxide compound of tin or carbide that graphitization catalyst described in step 1 can select this area to commonly use, be preferably SiO
2, SiC, Fe
2o
3, SnO
2one or its mixture.
Feed in raw material in rotation limit, cylinder limit described in step 1, the mixed effect of graphite, caking agent and graphitization catalyst can be improved, allow three mix fully, be beneficial to coated to graphite of caking agent and graphitization catalyst, caking agent and graphitization catalyst coated evenly effectively.
Step 2 refers in a heated condition, and realize graphite, caking agent and graphitization catalyst by the rotation in stove and stirring and more fully mix, be beneficial to the coated of natural graphite simultaneously, prepared material circulation, multiplying power, low-temperature performance are better.Drum rotational speed is adjustable as 10-100Hz, is preferably 20-60Hz.The present invention by heating mediate make particle diameter less nucleocapsid structure primary particle institute bonding one-tenth composite graphite particles surface one way or another arrange, there is high isotropy feature, add graphite internal void simultaneously; Lithium ion can be moved to several direction, and be beneficial to electrolytic solution and infiltrate, form more lithium ion mobility passages, migration path is shorter, improves the cycle performance of graphite, multiplying power, low-temperature performance.Graphite linings orientation reduces simultaneously, and Graphite Electrodes expands less.
Be cooled to normal temperature described in step 3, be the mixture in order to cool after heating kneading, this area conventional chilling method can be adopted.
Catalyzed graphitization described in step 4 can select this area to commonly use graphitization processing method, specifically has and under protection of inert gas, to carry out high temperature graphitization process and carry out purification graphitization processing under purifying gas.Due to purification graphitization processing, more fully can remove impurity, the graphite purity of preparation is higher, so the present invention preferably proposes graphitization processing.
Embodiment 1
Natural graphite (D5015 micron) 222.5kg, coal-tar pitch (D5010 micron) 25kg and graphitization catalyst SiC2.5kg are thrown in rotary drum furnace, and when feeding intake, feed in raw material in rotation limit, cylinder limit, feeds intake after terminating and carry out heating kneading.Regulating rotation speed of drum 30Hz, heating schedule is: normal temperature to 200 DEG C 1 hour, 200 DEG C to 400 DEG C 3 hours, 400 DEG C to 600 DEG C 3 hours, 600 DEG C of constant temperature 2 hours.Be cooled to normal temperature.Catalyzed graphitization process under 3000 DEG C and chlorine gas again.After gained greying, material sieves, and removes macrobead with 250 eye mesh screens, obtained composite graphite particles (D5021.0 micron), capacity 362mAh/g, efficiency 92.1%.
The composite graphite particles index that the present embodiment obtains is as following table 1:
As shown in Figure 1, through processing the composite graphite material finally obtained, its center is natural graphite, natural graphite is outer coated by synthetic graphite particles, and then formation nucleocapsid structure, the composite graphite material of the further bonding formation porous composite structure particle of nucleocapsid structure composite particles, wherein the graphite small-particle of this nucleocapsid structure has 2-20.
The composite graphite material using above-described embodiment to obtain prepares battery electrode, and Performance Detection is carried out to it, as illustrated in figs. 2 through 8, carry out the compaction capacity of electrode to test sample, absorbent, bounce-back ratio, cycle performance, high rate performance, cold cycle performance test, its result is obviously better than usual production similar at present.
Embodiment 2
Natural graphite (D5013 micron) 210kg, coal-tar pitch (D5012 micron) 37.5kg and graphitization catalyst SiO
22.5kg throws in rotary drum furnace, and when feeding intake, feed in raw material in rotation limit, cylinder limit, feeds intake after terminating and carries out heating kneading.Regulating rotation speed of drum 30Hz, heating schedule is: normal temperature to 200 DEG C 2 hours, 200 DEG C to 400 DEG C 5 hours, 400 DEG C to 600 DEG C 5 hours, 600 DEG C of constant temperature 3 hours.Be cooled to normal temperature.Catalyzed graphitization process under 3000 DEG C and chlorine gas again.After gained greying, material sieves, and removes macrobead with 250 eye mesh screens, obtained composite graphite particles (D5020 micron), capacity 363mAh/g, efficiency 92.4%.
Certainly, the foregoing is only specific embodiments of the invention, be not limit the scope of the present invention, all equivalences done according to structure, feature and principle described in the present patent application the scope of the claims change or modify, and all should be included in the present patent application the scope of the claims.
Claims (1)
1. a preparation method for compound graphite material for lithium ion secondary battery, is characterized in that: the method comprises the following steps:
(1) raw material mixing: drop into as the natural graphite of raw material, binding agent, graphite catalyst in rotary drum furnace, and raw material launch process intermediate roll keeps rotating state simultaneously; In raw material, the mass percentage content of each composition is:
Natural graphite: 70% ~ 90%;
Binding agent: 5% ~ 30%;
Graphite catalyst: 1% ~ 5%;
In above-mentioned raw materials, the quality of each composition is 100% than summation;
Wherein binding agent is the material that can form synthetic graphite after greying, carrying out coated, realizing again the bonding of coated rear nucleocapsid structure graphite by stirring binding agent to natural graphite;
(2) progressive heating: progressive heat temperature raising mode is adopted to heating raw materials in stove, heat-processed intermediate roll stove keeps rotating, and it comprises the following heating phase:
First stage, normal temperature to 200 DEG C, the time is 0.5-10 hour;
Subordinate phase, 200 DEG C to 400 DEG C, the time is 1-10 hour;
Phase III, 400 DEG C to 600 DEG C, the time is 1-10 hour;
Fourth stage, 600 DEG C of constant temperature 1-10 hour;
(3) cool: in stove, raw material is after heating, naturally cools to normal temperature;
(4) greying: graphitization processing is carried out to raw material;
Through above-mentioned process, binding agent forms synthetic graphite through process, and synthetic graphite is formed coated to natural graphite particles, realizes again the bonding of coated rear nucleocapsid structure graphite;
Through processing the composite graphite material finally obtained, it is natural graphite by center, natural graphite skin forms by the bonding nucleocapsid structure graphite granule formed of synthetic graphite particles is bonding, form the composite graphite material of porous composite structure particle, wherein the graphite small-particle of nucleocapsid structure has 2-20;
Described natural graphite, its median size is 5-15 micron;
Described binding agent is pitch, coal tar, the one of resin or mixture;
The particle diameter of described binding agent is less than 15 microns;
Described graphite catalyst is: SiO
2, SiC, Fe
2o
3, SnO
2one or its mixture;
Described graphitization processing adopts the graphitization processing of carrying out purifying under purifying gas.
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| CN201310111645.8A CN103241731B (en) | 2013-04-01 | 2013-04-01 | The preparation method of compound graphite material for lithium ion secondary battery |
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