CN103241731A - Preparation method of compound graphite material for lithium ion secondary battery - Google Patents
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Abstract
The invention discloses a preparation method of a compound graphite material for a lithium ion secondary battery. The preparation method comprises the following steps of: firstly pouring natural graphite, a binding agent and a graphite catalyst which are taken as raw materials into a roller furnace, wherein the roller furnace rotates all the time in a raw material pouring process; then progressively heating the raw materials, namely heating the raw materials in the roller furnace by adopting a progressive heating mode while the roller furnace rotates in a heating process, and then carrying out natural cooling to normal temperature after the raw materials in the roller furnace are heated; and finally carrying out graphitizing treatment on the raw materials, thus the binding agent forms artificial graphite, and the artificial graphite forms a coating on natural graphite particles, so as to form a shell-core structure, and compound particles of the shell-core structure are further spliced to form compound graphite particles with the required grain diameter. The compound graphite material prepared by the invention is of the shell-core structure with the natural graphite as an inner core and an artificial graphite layer as a coating, and the compound graphite has good isotropy, high capacity, high compactness, excellent multiplying, low temperature and cyclic performances and low electrode expansion. The preparation method of the compound graphite material for the lithium ion secondary battery adopts a method that coating and splicing are carried out at the same time, the preparation method is simple and practicable, and the cost is low.
Description
Technical field
The present invention relates to lithium ion battery negative material preparation method field, a kind of secondary lithium battery composite graphite preparation methods particularly, graphite material by this method preparation forms a kind of nucleocapsid structure, and the nucleocapsid structure graphite granule is through isotropic composite graphite particles material of bonding formation.
Background technology
Because the development of advanced electronics, people increase day by day for small-sized, lightweight, portable electronics and need for equipment.Charging back requires longer duration of service, and therefore, the battery that need have a 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, bigger to the cell container contribution, the negative material of having studied at present comprises: graphite, hard carbon, soft carbon, silicon-base alloy, tin-based alloy etc.Be badly in need of improving the capacity of negative material, under the situation of retention, improve compacted density simultaneously.
Natural graphite have that cost is low, capacity is high (〉=360mAh/g), the characteristics of good processability, yet exist with the electrolytic solution consistency poor, the shortcoming that cycle performance is relatively poor.Simultaneously single graphite granule is generally 15-20um, and graphite granule is bigger, and graphite is laminated structure simultaneously, and high anisotropy makes that lithium ion takes off, the embedding path length, prepared battery multiplying power, poor performance at low temperatures.
For overcoming the above problems, improve circulation, multiplying power and the low-temperature performance of natural graphite, Japanese Patent JP2000-182617 is with natural graphite and pitch or other mixed with resin, through pulverizing, charing, greying, can improve the deficiency of natural graphite, improve the cycle performance of graphite.Japanese Patent JP2002-373656 mixes height-oriented Graphite Powder 99 with mesophase pitch, through pulverizing, classification, calcining, greying and make matrix material, combine the excellent properties of heavy body and intermediate phase, has improved efficient, circulation and compaction capacity.Japanese Patent JP2003-173778 mixes natural graphite mutually with pitch, carries out machinery, graphitization processing, prepares sphere or oval composite graphite, this graphite is kernel with the natural graphite, and synthetic graphite is shell, uses under high compacting, irreversible capacity reduces, and cycle performance improves.Kernel is combined with shell closely, is difficult for fragmentation under high compacting, and coating layer and electrolytic solution consistency are good simultaneously, thereby has excellent performance.
The material of above-mentioned patent preparation, graphite granule are easy to form orientation, especially after compacting, the graphite granule of flats is orientated at pole piece, lithium ion takes off, the embedding path length, and prepared battery multiplying power, low-temperature performance can not satisfy more and more higher requirement, and electrode expands bigger simultaneously.
In addition, the synthetic graphite Stability Analysis of Structures, good with the electrolytic solution consistency, multiplying power, low temperature and cycle performance excellence (after the circulation of 500 weeks, capability retention 〉=80%).For obtaining the graphite cathode material of capacity height, compacting height, multiplying power, low temperature and cycle performance excellence, need be in conjunction with the advantage of natural graphite and synthetic graphite.
Summary of the invention
Technical problem to be solved by this invention just is to provide a kind of secondary lithium battery composite graphite preparation methods, composite graphite material by this method preparation is exactly to be that kernel, synthetic graphite are the nucleocapsid structure material of coating layer with the natural graphite, this composite graphite material can provide heavy body (〉=360mAh/g), and the consistency that it can improve graphite and electrolytic solution provides excellent cycle performance.
For solving the problems of the technologies described above, the present invention has adopted following technical scheme, this this method may further comprise the steps: 1, raw material mixes: will drop in the rotary drum furnace as natural graphite, binding agent, the graphite catalyst of raw material, and raw material launch process intermediate roll keeps rotating state simultaneously; The mass percentage content of each composition is in the raw material: natural graphite: 70%～90%; Binding agent: 5%～30%; Graphite catalyst: 1%～5%; Wherein binding agent is the material that can form synthetic graphite after the greying; By stirring binding agent natural graphite is coated, realize the bonding of natural graphite again; 2, progressive heating: raw material in the stove is added the progressive heat temperature raising mode of thermal recovery, and heat-processed intermediate roll stove keeps rotation, and it comprises the following heating phase: the fs, and normal temperature to 200 ℃, the time is 0.5-10 hour; Subordinate phase, 200 ℃ to 400 ℃, the time is 1-10 hour; Phase III, 400 ℃ to 600 ℃, the time is 1-10 hour; The quadravalence section, 600 ℃ constant temperature 1-10 hour; 3, cooling: raw material naturally cools to normal temperature through after heating in the stove; 4, greying: raw material is carried out graphitization processing; The above-mentioned processing of process, binding agent forms synthetic graphite through handling, and synthetic graphite forms coating to natural graphite particles.
Furthermore, in the technique scheme, described natural graphite can be selected this area natural graphite commonly used for use, and its median size is 1-20um, preferred 5-15um.
Furthermore, in the technique scheme, described binding agent is a kind of or mixture of pitch, coal tar, resin.
Furthermore, in the technique scheme, describedly be pitch, coal tar, resin for what pitch, coal tar, resin can be selected this area all size for use.Particle diameter can be below the 100um, is preferably below the 15um.
Furthermore, in the technique scheme, the content of described graphite catalyst be natural graphite content 0.5%～10%.
Furthermore, in the technique scheme, described graphitization catalyst is oxide compound or the carbide of silicon, iron, tin.
Furthermore, in the technique scheme, described graphite catalyst is: a kind of or its mixture of SiO2, SiC, Fe2O3, SnO2.
Furthermore, in the technique scheme, described graphitization processing adopts the graphitization processing of purifying under purifying gas.
Furthermore, in the technique scheme, through handling the composite graphite material that finally obtains, its center is natural graphite, the natural graphite skin is coated by the synthetic graphite particle and forms nucleocapsid structure, core-shell structure particles further forms porous composite structure particle, and wherein the graphite small-particle of nucleocapsid structure has 2-20.
After the present invention adopts technique scheme, for further for improving the isotropy of graphite, under the prerequisite of guaranteed performance, obtain (〉=1.7g/cc) the negative material of high compacted density more, the present invention makes its particle diameter less by controlling the particle diameter of natural/artificial nuclear's shell structure composite graphite earlier, and then the graphite granule of the required particle diameter of the further bonding one-tenth of the less nucleocapsid structure composite particles of particle diameter, realize increasing the isotropy of graphite, increased the graphite internal void; Make lithium ion to be beneficial to electrolytic solution and to soak into to several direction motions, form more lithium ion migrating channels, migration path is shorter, has improved cycle performance, multiplying power, the low-temperature performance of graphite, and electrode expands littler.
For guaranteeing the performance of graphite under high pressure truth condition, the present invention introduces graphitization catalyst simultaneously, with in graphite pebbles surface pore-creating, improves the graphite specific surface.Realize electrode under high compacting (〉=1.7g/cc), also can keep enough electrolytic solution, increase the interfacial area of graphite and electrolytic solution simultaneously, further improve battery multiplying power, low temperature and cycle performance.
Marginal data
Fig. 1 is scanning electronic microscope (SEM) figure according to the composite graphite particles of the embodiment of the invention 1 preparation.
Fig. 2 is the first charge-discharge graphic representation according to the composite graphite particles of the embodiment of the invention 1 preparation.
Fig. 3 is the compaction capacity figure according to the electrode of the composite graphite particles preparation of the embodiment of the invention 1 preparation.
Fig. 4 is the absorbent figure according to the composite graphite particles of the embodiment of the invention 1 preparation.
Fig. 5 is the bounce-back scale map according to the composite graphite particles of the embodiment of the invention 1 preparation.
Fig. 6 is the cycle performance figure according to the composite graphite particles of the embodiment of the invention 1 preparation.
Fig. 7 is the high rate performance figure according to the composite graphite particles of the embodiment of the invention 1 preparation.
Fig. 8 is the cold cycle performance map according to the composite graphite particles of the embodiment of the invention 1 preparation.
Specific embodiment
Preparation method of the present invention may further comprise the steps:
(1) raw material mixes: will drop in the rotary drum furnace as natural graphite, binding agent, the graphite catalyst of raw material, and raw material launch process intermediate roll keeps rotating state simultaneously; The mass percentage content of each composition is in the raw material:
Natural graphite: 70%～90%;
Binding agent: 5%～30%;
Graphite catalyst: 1%～5%;
Wherein binding agent is the material that can form synthetic graphite after the greying; By stirring binding agent natural graphite is coated, realize the bonding of natural graphite again.
(2) progressive heating: raw material in the stove is added the progressive heat temperature raising mode of thermal recovery, and heat-processed intermediate roll stove keeps rotation, regulates drum rotational speed 10-100Hz.It comprises the following heating phase:
Fs, normal temperature to 200 ℃, the time is 0.5-10 hour;
Subordinate phase, 200 ℃ to 400 ℃, the time is 1-10 hour;
Phase III, 400 ℃ to 600 ℃, the time is 1-10 hour;
The quadravalence section, 600 ℃ constant temperature 1-10 hour.
(3) cooling: raw material naturally cools to normal temperature through after heating in the stove.
(4) greying: raw material is carried out graphitization processing.
The above-mentioned processing of process, binding agent forms synthetic graphite through handling, and synthetic graphite forms coating to natural graphite particles.
The described natural graphite of step 1 can be selected this area natural graphite commonly used for use, and its median size is 1-20um, preferred 5-15um.
The described caking agent of step 1 can be selected the caking agent commonly used of this area for use, and can form synthetic graphite after the greying, is generally a kind of or its mixture of pitch, coal tar, resin.Describedly be pitch, coal tar, resin for what pitch, coal tar, resin can be selected this area all size for use.Particle diameter can be below the 100um, is preferably below the 15um.
The described graphitization catalyst of step 1 can be selected oxide compound or the carbide of this area silicon commonly used, iron, tin for use, is preferably a kind of or its mixture of SiO2, SiC, Fe2O3, SnO2.
The described cylinder of step 1 is reinforced while rotating, can improve the mixed effect of graphite, caking agent and graphitization catalyst, allow the three mix fully, be beneficial to caking agent and graphitization catalyst to the coating of graphite, caking agent and graphitization catalyst coat more even effective.
Step 2 refers under heating condition, realizes graphite, caking agent and the more abundant mixing of graphitization catalyst by the rotation in the stove and stirring, is beneficial to the coating of natural graphite simultaneously, and prepared material circulation, multiplying power, low-temperature performance are better.Drum rotational speed is adjustable as 10-100H, is preferably 20-60Hz.The present invention mediates by heating and makes the less nucleocapsid structure primary particle of particle diameter in the one way or another arrangement of the composite graphite particles surface of the bonding one-tenth of institute, has high isotropy characteristics, has increased the graphite internal void simultaneously; Make lithium ion to be beneficial to electrolytic solution and to soak into to several direction motions, form more lithium ion migrating channels, migration path is shorter, has improved cycle performance, multiplying power, the low-temperature performance of graphite.The graphite linings orientation reduces simultaneously, and Graphite Electrodes expands littler.
The described normal temperature that is cooled to of step 3 is in order to cool off the mixture after heating is mediated, can to adopt the conventional method of cooling in this area.
The described catalyzed graphitization of step 4 can select for use this area to use the graphitization processing method always, specifically has to carry out high temperature graphitization processing and the graphitization processing of purifying under protection of inert gas under purifying gas.Because the purification graphitization processing, can more abundant removal impurity, the graphite purity of preparation is higher, so the present invention preferably proposes graphitization processing.
Embodiment 1
Natural graphite (D5015um) 222.5kg, coal-tar pitch (D5010um) 25kg and graphitization catalyst SiC2.5kg are thrown to rotary drum furnace, and cylinder is reinforced while rotating when feeding intake, and heats kneading after the end that feeds intake.Regulate drum rotational speed 30Hz, heating schedule is: normal temperature to 200 ℃ 1 hour, 200 ℃ to 400 ℃ 3 hours, 400 ℃ to 600 ℃ 3 hours, 600 ℃ of constant temperature 2 hours.Be cooled to normal temperature.Catalyzed graphitization is handled under 3000 ℃ and chlorine gas again.Material sieves after the gained greying, removes macrobead with 250 eye mesh screens, makes composite graphite particles (D5021.0um), capacity 362mAh/g, efficient 92.1%.
The composite graphite particles index that present embodiment makes such as following table 1:
See shown in Figure 1, through handling the composite graphite material that finally obtains, its center is natural graphite, the natural graphite skin is coated by the synthetic graphite particle, 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 preparation battery electrode that uses above-described embodiment to obtain, and it is carried out Performance Detection, shown in Fig. 2-8, specimen is carried out compaction capacity, absorbent, bounce-back ratio, cycle performance, high rate performance, the cold cycle performance of electrode and test, its result obviously is better than similar usual production at present.
Embodiment 2
Natural graphite (D5013um) 210kg, coal-tar pitch (D5012um) 37.5kg and graphitization catalyst SiO22.5kg are thrown to rotary drum furnace, and cylinder is reinforced while rotating when feeding intake, and heats kneading after the end that feeds intake.Regulate drum rotational speed 30Hz, heating schedule is: normal temperature to 200 ℃ 2 hours, 200 ℃ to 400 ℃ 5 hours, 400 ℃ to 600 ℃ 5 hours, 600 ℃ of constant temperature 3 hours.Be cooled to normal temperature.Catalyzed graphitization is handled under 3000 ℃ and chlorine gas again.Material sieves after the gained greying, removes macrobead with 250 eye mesh screens, makes composite graphite particles (D5020um), capacity 363mAh/g, efficient 92.4%.
Certainly, the above only is specific embodiments of the invention, be not to limit the scope of the present invention, all equivalences of doing according to the described structure of the present patent application claim, feature and principle change or modify, and all should be included in the present patent application claim.
Claims (9)
1. secondary lithium battery composite graphite preparation methods, it is characterized in that: this method may further comprise the steps:
(1) raw material mixes: will drop in the rotary drum furnace as natural graphite, binding agent, the graphite catalyst of raw material, and raw material launch process intermediate roll keeps rotating state simultaneously; The mass percentage content of each composition is in the raw material:
Natural graphite: 70%～90%;
Binding agent: 5%～30%;
Graphite catalyst: 1%～5%;
Wherein binding agent is the material that can form synthetic graphite after the greying, by stirring binding agent natural graphite is coated, and realizes coating the bonding of back nucleocapsid structure graphite again;
(2) progressive heating: raw material in the stove is added the progressive heat temperature raising mode of thermal recovery, and heat-processed intermediate roll stove keeps rotation, and it comprises the following heating phase:
Fs, normal temperature to 200 ℃, the time is 0.5-10 hour;
Subordinate phase, 200 ℃ to 400 ℃, the time is 1-10 hour;
Phase III, 400 ℃ to 600 ℃, the time is 1-10 hour;
The quadravalence section, 600 ℃ constant temperature 1-10 hour;
(3) cooling: raw material naturally cools to normal temperature through after heating in the stove;
(4) greying: raw material is carried out graphitization processing;
The above-mentioned processing of process, binding agent forms synthetic graphite through handling, and synthetic graphite realizes coating the bonding of back nucleocapsid structure graphite again to natural graphite particles formation coating.
2. secondary lithium battery according to claim 1 composite graphite preparation methods, it is characterized in that: described natural graphite, its median size are 5-15um.
3. secondary lithium battery according to claim 1 composite graphite preparation methods, it is characterized in that: described binding agent is a kind of or mixture of pitch, coal tar, resin.
4. secondary lithium battery according to claim 3 composite graphite preparation methods, it is characterized in that: the particle diameter of described binding agent is below the 15um.
5. secondary lithium battery according to claim 1 composite graphite preparation methods is characterized in that: the content of described graphite catalyst be natural graphite content 0.5%～10%.
6. secondary lithium battery according to claim 1 composite graphite preparation methods, it is characterized in that: described graphitization catalyst is oxide compound or the carbide of silicon, iron, tin.
7. secondary lithium battery according to claim 6 composite graphite preparation methods, it is characterized in that: described graphite catalyst is: a kind of or its mixture of SiO2, SiC, Fe2O3, SnO2.
8. secondary lithium battery according to claim 1 composite graphite preparation methods is characterized in that: the graphitization processing that described graphitization processing employing is purified under purifying gas.
9. secondary lithium battery according to claim 1 composite graphite preparation methods, it is characterized in that: through handling the composite graphite material that finally obtains, it is natural graphite by the center, the natural graphite skin is by bonding bonding the forming of nucleocapsid structure graphite granule that constitutes of synthetic graphite particle, form the composite graphite material of porous composite structure particle, wherein the graphite small-particle of nucleocapsid structure has 2-20.
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