CN101916844A - Torispherical cathode material for lithium ion battery and preparation method thereof - Google Patents
Torispherical cathode material for lithium ion battery and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a torispherical cathode material for a lithium ion battery, which has a 'shell-core' graphite composite microstructure, wherein an inner core may be spherical natural graphite, spherical artificial graphite, a mesocarbon microbead or a mixture of the three; a shell is a graphitized product of asphalt; an interlayer distance between the inner core and the shell ranges from 0.3360 to 0.3390nm; and the torispherical cathode material has a mesoporous structure with an aperture of 10 to 50nm, and the ratio of granular length to granular width of the graphite composite ranges from 1.0 to 2.0. The torispherical cathode material for the lithium ion battery has the advantages that: 1, the high-rate performance of the electrode material is improved; and the discharge capacitance of the electrode material still reaches 320 to 340mAh/g after 300 times of circulation at a 5C rate; 2, preparation cost is low and atmosphere pollution is avoided; and 3, the shape of the graphite raw material used by the invention is torispherical and favorable for the cladding uniformity of the asphalt and can better strengthen the structural stability of the composite.
Description
Technical field
The present invention relates to a kind of lithium ion battery with negative material and preparation method thereof, relate in particular to a kind of Torispherical cathode material for lithium ion battery and preparation method thereof.
Background technology
Along with the active demand of present people to electric automobile, electrokinetic cell and high magnification electrode material all become the research and development focus of field of power supplies.With graphite type material as lithium ion battery negative material have embedding, take off the lithium good reversibility, advantage such as the current potential platform is low and cycle performance is good, its theoretical specific capacity is up to 372mAh/g, far above the specific capacity of positive electrodes such as LiCoO2.Yet lithium ion is less at the diffusion coefficient of graphite layers, is seriously restricting the raising of lithium ion battery high-rate charge-discharge capability.In addition, the graphite material of high graphitization degree and the compatibility of electrolyte are relatively poor, thus must by further improve with the high rate performance that improves the graphite-like negative material and with the compatibility of electrolyte.
The used graphite modified method of forefathers is broadly divided into three classes: surface oxidation or reduction are handled, are mixed and coat, and for suitability for industrialized production, then mainly use the raw material of wood-charcoal material package to cover modified technique.Employing spray granulations such as the Shen Wanci of Tsing-Hua University and Kang Feiyu make phenolic resins and coat spherical graphite composite material, make pyrolytic carbon through charing again and coat spherical graphite composite material, compare with spherical graphite, the efficient of enclosed pasture first of this composite graphite material obviously improves, cycle performance obviously prolongs, the compatibility of electrolyte such as electrode material and PC is also obviously improved [CN, 02125715.9]; China Electronics Technology Group Corporation No.18 Institute once carried out surface treatment (be mainly charcoal and coat processing) to graphite, and the gained material is irreversible capacity less [CN, 03144278.1] first.Yet above-mentioned two patents only limit to the low range lithium ion battery negative material, do not relate to improving the improvement of graphite material high rate performance.Recently, Shenzhen company once coated length than (length-width ratio) almost spherical Delanium [CN between 1.5～4 with pyrolytic carbon, 200710075897.4], find that this composite sample not only has good low range charge and discharge performance, its high magnification charge and discharge performance is also comparatively desirable.
Summary of the invention
The object of the present invention is to provide a kind of Torispherical cathode material for lithium ion battery and preparation method thereof, this method adopts simple solid phase cladding process to make the torispherical graphite composite material of length-width ratio between 1.0-2, in order to reduce the adverse effect of coating layer to the lithium ion diffusion, this method is by having added a certain amount of pore creating material in raw material, in product, increased a large amount of lithium ion migrating channels, can shorten the evolving path of lithium ion at material internal.
The present invention is achieved like this, a kind of Torispherical cathode material for lithium ion battery, it is characterized in that this negative material has " shell-nuclear " type microstructure, its kernel is the material that mixes mutually between a kind of or three in spherical natural graphite, spherical Delanium, the MCMB, shell is the graphitization product of pitch, and the interlamellar spacing of kernel and shell is 0.3360-0.3390nm.Composite cathode material of silicon/carbon/graphite has the microcosmic meso-hole structure, and pore diameter range is 10-50nm, and this material granule approaches sphere, and the particle length-width ratio is between 1.0-2.0.
The preparation method of described a kind of Torispherical cathode material for lithium ion battery is characterized in that method step is:
The first step: raw material mixed processes: at ambient temperature, graphite raw material after the shaping, pore-creating additive are mixed with the abundant mechanical ball milling of pitch, the mass ratio of graphite raw material, pore-creating additive and pitch is 100: (1-5): (15-35), drum's speed of rotation is 1000-3000rpm, and the ball milling time is 1-3h;
Second step: charing-trimming: the prepared mixed material of the first step is changed in the reactor, in inert atmosphere, stir 1-3h in 200-300 ℃, then continue heat treatment and be warming up to 700-1200 ℃, obtain the charing material, then handle through pulverizing, screening and shaping again and obtain spherical charing material, the specific area of gained charing material powder is 2.5-4.5, and pore diameter range is 10-50nm;
The 3rd step: graphitization process: place graphitizing furnace to carry out the graphitization purification process spherical charing material, make Torispherical cathode material for lithium ion battery, the graphitization processing temperature is in 2500-3000 ℃ of scope.
Described pore-creating additive is selected from a kind of in the following material: silica flour, gelatin, citric acid, polyvinyl alcohol or three block macromolecular surfactants; Described pitch is selected from hard pitch, and softening point 200-300 ℃, coking rate 60-90%.
Advantage of the present invention is: 1. graphite surface of the present invention improves technology, not only can significantly improve the efficient of enclosed pasture first of material, prolong the cycle life of electrode, can also shorten the evolving path of lithium ion in graphite linings, improve the high rate capability of electrode material; The present invention relates to the torispherical composite cathode material of silicon/carbon/graphite and carry out the constant current charge-discharge test under the multiplying power of 0.1C, find that its reversible capacity can reach 350-360mAh/g, 300 its discharge capacities that circulate of experience still can reach 320-340mAh/g under 5C multiplying power condition.
2. the solid phase cladding process of the present invention's employing makes the torispherical graphite composite material, compares with atomizing granulating technology with the liquid impregnation cladding process, and the solid phase cladding process is avoided with an organic solvent, and preparation cost is low and pollution-free to atmosphere.
3. the pattern of the used graphite raw material of the present invention is a torispherical, and this shape helps the uniformity of pitch-coating, better the structural stability of reinforced composite.
Description of drawings
Fig. 1 is button cell charging and discharging curve figure of the present invention.
Fig. 2 is a sem photograph of the present invention (* 1000).
Embodiment
Embodiment 1
1, the spherical Delanium of 50kg is pulverized the Delanium D50:17-20um. after the pulverizing through pulverizer
2, will pulverize orthopedic Delanium and add pitch coke, pore creating material, the proportion of Delanium, silica flour and pitch coke is 100: 5: 10, stirs under 210 ℃, and mixing time is 2h.
3, then the material that stirs is handled processing time 5h in 900 ℃ of following charings of nitrogen protection.
4, charing is good material is sent in 2600 ℃ of high temperature furnaces graphitization under nitrogen protection.
5, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P:3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
The part testing result sees Table one
Embodiment 2
1, with the 50kg spherical natural graphite: spherical Delanium weight ratio is that 1: 1 mixed material is pulverized the Delanium D50:17-20um. after the pulverizing through pulverizer
2, will pulverize orthopedic mixed material and add pitch coke, pore creating material, the proportion of Delanium, silica flour and pitch coke is 100: 2: 15, stirs under 260 ℃, and mixing time is 2h.
3, then the material that stirs is handled processing time 6h in 900 ℃ of following charings of nitrogen protection.
4, charing is good material is sent in 2600 ℃ of high temperature furnaces graphitization under nitrogen protection.
5, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P:3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
The part testing result sees Table two
Embodiment 3
1, the 50kg MCMB is pulverized the Delanium D50:17-20um. after the pulverizing through pulverizer
2, will pulverize orthopedic MCMB and add pitch coke, pore creating material, the proportion of Delanium, silica flour and pitch coke is 100: 5: 10, stirs under 230 ℃, and mixing time is 2h.
3, then with the material that stirs at 900 ℃ of following carbonization treatment of nitrogen protection, processing time 5h.
4, carbonization is good material is sent in 2600 ℃ of high temperature furnaces graphitization under nitrogen protection.
5, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P:3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
The part testing result sees Table three
Embodiment 4
1, be that 1: 1: 1 compound is pulverized the Delanium D50:17-20um. after the pulverizing through pulverizer with the spherical Delanium of 50kg, spherical natural graphite, MCMB weight ratio
2, will pulverize orthopedic compound and add pitch coke, pore creating material, the proportion of compound, silica flour and pitch coke is 100: 5: 10, stirs under 280 ℃, and mixing time is 2h.
3, then with the material that stirs at 900 ℃ of following carbonization treatment of nitrogen protection, processing time 5h.
4, carbonization is good material is sent in 2600 ℃ of high temperature furnaces graphitization under nitrogen protection.
5, the making of button cell and detection
1), electrolyte: 1M-LiPF6 EC/DMC/EMC
2), binding agent: LA-133:3%
3), conductive agent: Super-P:3%
4), to electrode: pour lithium slice
5), discharge and recharge system
(A) constant-current discharge (0.2mA, 0.001V)
(B) leave standstill (1min)
(C) constant current charge (0.2mA, 2.000V)
The part testing result sees Table four
As shown in Figure 1, as can be seen from the figure, the graphite composite material that the present invention is made is assembled into button cell, and this material charge and discharge platform is stable, and the discharge gram volume is more than 365mAh/g.As shown in Figure 2, as can be seen from the figure, the present invention makes graphite composite material and has the torispherical structure, and the particle length and width of this material are between 1.0-2.0.
Table one
Table two
Table three
Table four
Claims (3)
1. lithium ion battery composite cathode material of silicon/carbon/graphite, it is characterized in that this negative material has " shell-nuclear " type microstructure, its kernel is the material that mixes mutually between a kind of or three in spherical natural graphite, spherical Delanium, the MCMB, shell is the graphitization product of pitch, the interlamellar spacing of kernel and shell is 0.3360-0.3390nm, composite cathode material of silicon/carbon/graphite has the microcosmic meso-hole structure, pore diameter range is 10-50nm, this material granule approaches sphere, and the particle length-width ratio is between 1.0-2.0.
2. the preparation method of the described a kind of Torispherical cathode material for lithium ion battery of claim 1 is characterized in that method step is:
The first step: raw material mixed processes: at ambient temperature, graphite raw material after the shaping, pore-creating additive are mixed with the abundant mechanical ball milling of pitch, the mass ratio of graphite raw material, pore-creating additive and pitch is 100: (1-5): (15-35), drum's speed of rotation is 1000-3000rpm, and the ball milling time is 1-3h;
Second step: charing-trimming: the prepared mixed material of the first step is changed in the reactor, in inert atmosphere, stir 1-3h in 200-300 ℃, then continue heat treatment and be warming up to 700-1200 ℃, obtain the charing material, then handle through pulverizing, screening and shaping again and obtain spherical charing material, the specific area of gained charing material powder is 2.5-4.5, and pore diameter range is 10-50nm;
The 3rd step: graphitization process: place graphitizing furnace to carry out the graphitization purification process spherical charing material, make Torispherical cathode material for lithium ion battery, the graphitization processing temperature is in 2500-3000 ℃ of scope.
3. the preparation method of a kind of Torispherical cathode material for lithium ion battery according to claim 2 is characterized in that described pore-creating additive is selected from a kind of in the following material: silica flour, gelatin, citric acid, polyvinyl alcohol or three block macromolecular surfactants; Described pitch is selected from hard pitch, and softening point 200-300 ℃, coking rate 60-90%.
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