CN102082272A - Hard carbon coated lithium ion battery anode material and preparation method thereof - Google Patents
Hard carbon coated lithium ion battery anode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hard carbon coated lithium ion battery anode material and a preparation method thereof. The anode material is characterized in that the coating material is formed by a heteroatom modifier, a hard carbon precursor material and a soft carbon precursor material, wherein the weight ratio of the heteroatom modifier to the hard carbon precursor to the soft carbon precursor is 1:(2-3.3):(3-9). The preparation method is mainly characterized by comprising the following steps: fully mixing graphite and the coating material, and then carrying out heat treatment on the mixture under the protection of inert atmosphere; preserving the temperature for 0.5-6 hours, and then cooling; and carrying out secondary high-temperature graphitization treatment under the protection of inert atmosphere. The heteroatom modifier can change the structure of the hard carbon in the coating material, and the hard carbon precursor has the characteristics of dissolvability and condensation polymerization with the soft carbon precursor asphalt, thus improving the uniformity and operability of the coated graphite particles; and the ratio of the heteroatom modifier to the hard carbon precursor to the soft carbon precursor has an important effect on the performance of the three. By optimizing the ratio of the heteroatom to the hard carbon precursor to the soft carbon precursor in the coated graphite material, the aims of increasing the capacity of the anode material and improving the cycle performance of the anode material are achieved.
Description
Technical field
The present invention relates to a kind of lithium ion battery cathode material and its preparation method that hard carbon coats that contains.
Background technology
Lithium ion battery has advantages such as operating voltage height, specific energy is big, security performance is good, is widely used in mobile communication, notebook computer lamp field, also has wide application prospect in following electric automobiles.
Having lower lithium as the graphite type material of negative material and embed/take off embedding current potential, suitable reversible capacity and aboundresources, advantage such as cheap, is comparatively ideal lithium ion battery negative material.But it also exists, and discharging efficiency is low first, cycle performance is poor, to shortcomings such as electrolyte selectivity height, graphite material is used is restricted, need carry out modification to graphite material.
Usually the method that adopts is that carbon coats method at present.He Ming etc. are at " resin carbon coats the preparation and the chemical property thereof of micro crystal graphite " (" battery ", 2003,3 (5): coat one deck resin carbon at natural micro crystal graphite microparticle surfaces 281-284), coat and handle the irreversible capacity first that can reduce natural micro crystal graphite, adopt and mix the method coated graphite that disperses then, inside is natural micro crystal graphite, and the outside is the phenolic resins pyrolysis carbon-coating of 1-2 μ m.The irreversible capacity that the lithium ion Experimental cell records natural micro crystal graphite is 14%, and the irreversible capacity of coated graphite is 7%.Coat and handle the irreversible capacity that can reduce natural micro crystal graphite to a great extent.Yang Ruizhi etc. are at " the resin carbon coated graphite is as the research of lithium ion battery negative electrode " (" Journal of Inorganic Materials, 2000,15 (4): coat phenolic resins with the liquid impregnation method on the natural flake graphite surface 712-718), utilization constant current charge and discharge method, the powder microelectrode cyclic voltammetry has been investigated the charge and discharge performance.Experimental result shows that higher through the discharge capacity of heat treated phenolic resins carbon coated graphite material, cycle life is longer, can be used as the negative material of high-performance file ion battery.Zhou Defeng etc. are at " preparation of boronation phenolic resin-carbon material and embedding lithium performance " (" chemistry world ", 2006 (5): prepared boracic phenolic resins pyrolysis raw material of wood-charcoal material 260-263), the doping that has contrasted boron is to raw material of wood-charcoal material microstructure and embedding lithium Effect on Performance, and the result shows, H
3BO
3Adding can improve the degree of graphitization of raw material of wood-charcoal material, the first charge-discharge specific capacity of boracic raw material of wood-charcoal material and efficiency for charge-discharge are higher than pure raw material of wood-charcoal material.Yin Ge equality " preparation of boron-doping phenolic resins pyrolysis carbon and embedding lithium performance study " (" high-tech communication ", 2001 (3): 98-100) with thermosetting phenolic resin and H
3BO
3Dissolving also mixes, and obtains containing boron bakelite resin, makes the boron-doping hard carbon material through further charing, discharge and recharge the result and show, the doping of boron makes that the embedding of lithium/taking off capacity obviously improves, and the embedding current potential that takes off that 1V is following simultaneously reduces, and the current potential stationarity makes moderate progress, and XRD analysis shows, makes the d of hard carbon after the boron-doping
002Obviously reduce, promptly the ordering degree of carbon structure improves.
In at present the modification of graphite material being handled, only resin-coated class hard carbon presoma, not good with the adhesion of graphite material, and hard carbon presoma degree of graphitization is lower, though can improve the cycle performance of material, bigger to the first charge-discharge performance impact of material.The Chinese patent CN101604743A heteroatomic resinae macromolecule RESEARCH OF PYROCARBON coated graphite material that mixes, significantly improve the electrical property of graphite, but also had some problems, relatively poor as the compatibility of resinous material and graphite, volatile matter is many in the resin pyrolytic process, and specific surface is higher.Chinese patent CN101162775A mixes the coating graphite material with resin with pitch, this method also has some shortcomings in actual applications, and the carbonization degree of resin is low, has influenced the final efficient first of material.
Summary of the invention
The object of the present invention is to provide a kind of lithium ion battery cathode material and its preparation method that hard carbon coats that contains.
A kind of lithium ion battery negative material that contains the hard carbon coating provided by the present invention has following characteristic: the graphite surface clad material is formed hetero-atom modifier by hetero-atom modifier, hard carbon persursor material and soft carbon matrix precursor material: the hard carbon presoma: soft carbon matrix precursor weight ratio is 1: (2-3.3): (3-9); Described hetero-atom modifier is selected from boric acid or diboron trioxide; The hard carbon presoma is selected wherein one or more of phenolic resins, furfural resin, epoxy resin, furane resins, polyvinyl alcohol or polyacrylonitrile for use; Soft carbon matrix precursor is selected pitch for use.
In the lithium ion battery negative material provided by the invention, graphite is natural or/and Delanium, and its granularity is 5-70 μ m, and degree of graphitization 〉=80%, graphite account for the 150-900% of clad material mass percent.
The invention provides the above-mentioned preparation method who contains the lithium ion battery negative material of hard carbon coating.
Method of the present invention is hetero-atom modifier, the hard carbon presoma, and soft carbon matrix precursor proportionally adds in the mixing and blending machine and mixes, and mixes 1-5h.In mixer, add the graphite that takes by weighing by mass percentage again, continue to mix 1-5h.
Method of the present invention with graphite with after clad material fully mixes, at inert gas N
2Perhaps the Ar protection 100 ℃ of-300 ℃ of cured, is incubated 1-3h down; Rise to 800 ℃-1200 ℃ with 1-10 ℃/min speed after the cured, insulation 0.5-6h is cooled to below 200 ℃; Behind the crushing screening, carry out the secondary high temperature graphitization and handle, rise to 2800 ℃-3200 ℃ with 1-10 ℃/min speed, insulation 0.5-6h, cooling back crushing screening both must contain the lithium ion battery negative material that hard carbon coats.
The present invention implements hetero-atom at graphite surface, the hard carbon presoma, soft carbon matrix precursor mixes coating, adopt hard carbon presoma, soft carbon matrix precursor to mix and coat graphite granule, both advantages have not only been utilized, and selected hard carbon presoma have dissolving and with the feature of pitch generation polycondensation reaction, not only improved uniformity, the operability of coated graphite particle, and improved the comprehensive electrochemical properties of coated graphite particle; Heteroatomic introducing can change the structure of hard carbon, and the change of this structure has improved the efficient of enclosed pasture first of hard carbon in the negative material; And hetero-atom, the hard carbon presoma, the triangular formula rate of soft carbon matrix precursor has determined the important parameter of negative materials such as the final specific area of structure, negative material, the final compacted density of negative material of coating layer, thereby influences the final chemical property of negative material greatly.Therefore, preparation method of the present invention has not only improved the cycle performance of graphite, and has further improved the efficient of enclosed pasture first of negative material, is that a kind of technology is simple, the method for easy operating.
Description of drawings:
Fig. 1 is the electromicroscopic photograph (300 times) of the lithium ion battery negative material that contains the hard carbon coating of the embodiment of the invention 1;
Fig. 2 is the electromicroscopic photograph (1000 times) of the lithium ion battery negative material that contains the hard carbon coating of the embodiment of the invention 1;
Fig. 3 is the XRD figure of the lithium ion battery negative material that contains the hard carbon coating of the embodiment of the invention 1.
Specific embodiment
In order further to understand summary of the invention of the present invention and characteristics, enumerate following example, but these examples do not comprise or limit the full content of inventive concept.
Embodiment 1
Take by weighing 10g boric acid; 33g hot shortness phenolic resins; 67g pitch joins in the mixing and blending machine; mix under the room temperature and stir 1h; add average grain diameter 18 μ m; the native graphite micro mist 890g of degree of graphitization 〉=80%; continue to stir 2h; mixture packed into put into board-like kiln in the ceramic crucible; under the nitrogen atmosphere protection, rise to 150 ℃, insulation 2h with the speed of 1.5 ℃/min; speed with 2 ℃/min rises to 1100 ℃ again; naturally cool to below 200 ℃ behind the insulation 4h and take out material, through pulverizing; after the screening, the speed with 3 ℃/min is warming up to 2850 ℃ under nitrogen atmosphere protection again; naturally cool to below 200 ℃ behind the insulation 3h and take out material, through pulverizing; be lithium ion battery negative material after the screening.
Take by weighing 10g boric acid; 25g epoxy resin; 75g pitch joins in the mixing and blending machine; mix under the room temperature and stir 1.5h; add average grain diameter 18 μ m; the native graphite micro mist 890g of degree of graphitization 〉=80%; continue to stir 2h; mixture packed into put into board-like kiln in the ceramic crucible, under the nitrogen atmosphere protection, rise to 180 ℃ with the speed of 3 ℃/min; insulation 2h; speed with 1.5 ℃/min rises to 1100 ℃ again, naturally cools to below 200 ℃ behind the insulation 4h and takes out material, is lithium ion battery negative material after pulverizing, sieving.
Embodiment 3
Take by weighing the 15g diboron trioxide; 50g hot shortness phenolic resins; 50g pitch joins in the mixing and blending machine; mix under the room temperature and stir 2.5h; add average grain diameter 18 μ m; the native graphite micro mist 885g of degree of graphitization 〉=80%; continue to stir 2h; mixture packed into put into board-like kiln in the ceramic crucible, under the nitrogen atmosphere protection, rise to 160 ℃ with the speed of 2.5 ℃/min; insulation 2h; speed with 2 ℃/min rises to 1080 ℃ again, insulation 4h, after naturally cool to below 200 ℃ and take out material; through pulverizing; after the screening; speed with 2.5 ℃/min is warming up to 3000 ℃ under nitrogen atmosphere protection again, naturally cools to below 200 ℃ behind the insulation 5h and takes out material, through pulverizing; be lithium ion battery negative material after the screening.
Embodiment 4
Take by weighing 10g boric acid; the 30g furane resins; 90g pitch joins in the mixing and blending machine; mix under the room temperature and stir 1h; add average grain diameter 18 μ m; the native graphite micro mist 870g of degree of graphitization 〉=80%; continue to stir 3h; mixture packed into put into board-like kiln in the ceramic crucible, under the nitrogen atmosphere protection, rise to 260 ℃ with the speed of 3 ℃/min; insulation 2.5h; speed with 2 ℃/min rises to 1150 ℃ again, insulation 3.5h, after naturally cool to below 200 ℃ and take out material; through pulverizing; after the screening; speed with 4 ℃/min is warming up to 2900 ℃ under nitrogen atmosphere protection again, naturally cools to below 200 ℃ behind the insulation 3h and takes out material, through pulverizing; be lithium ion battery negative material after the screening.
Embodiment 5
Take by weighing the 10g diboron trioxide; the 20g furfural resin; 80g pitch joins in the mixing and blending machine; mix under the room temperature and stir 1.5h; add average grain diameter 18 μ m; the native graphite micro mist 900g of degree of graphitization 〉=80%; continue to stir 2.5h; mixture packed into put into board-like kiln in the ceramic crucible, under the nitrogen atmosphere protection, rise to 190 ℃ with the speed of 3 ℃/min; insulation 3h; speed with 2 ℃/min rises to 1050 ℃ again, insulation 4h, after naturally cool to below 200 ℃ and take out material; through pulverizing; after the screening; speed with 3 ℃/min is warming up to 2850 ℃ under nitrogen atmosphere protection again, naturally cools to below 200 ℃ behind the insulation 3.5h and takes out material, through pulverizing; be lithium ion battery negative material after the screening.
Comparative example 1
Take by weighing 40g hot shortness phenolic resins; 80g pitch joins in the mixing and blending machine; mix under the room temperature and stir 2h; add average grain diameter 18 μ m; the native graphite micro mist 880g of degree of graphitization 〉=80%; continue to stir 2h; mixture packed into put into board-like kiln in the ceramic crucible; under the nitrogen atmosphere protection; speed with 1.5 ℃/min rises to 200 ℃, insulation 2.5h, and the speed with 2.5 ℃/min rises to 1100 ℃ again; insulation 4h; after naturally cool to below 200 ℃ and take out material, through pulverizing; after the screening, the speed with 3 ℃/min is warming up to 2850 ℃ under nitrogen atmosphere protection again; naturally cool to below 200 ℃ behind the insulation 5h and take out material, through pulverizing; be lithium ion battery negative material after the screening.
Comparative example 2
Take by weighing 20g boric acid; the 80g furfural resin joins in the mixing and blending machine; mix under the room temperature and stir 1h; add average grain diameter 18 μ m; the native graphite micro mist 900g of degree of graphitization 〉=80%; continue to stir 2.5h; mixture packed into put into board-like kiln in the ceramic crucible; under the nitrogen atmosphere protection; speed with 2.5 ℃/min rises to 150 ℃, insulation 2h, and the speed with 2 ℃/min rises to 1100 ℃ again; insulation 4h; after naturally cool to below 200 ℃ and take out material, through pulverizing; after the screening, the speed with 3 ℃/min is warming up to 3000 ℃ under nitrogen atmosphere protection again; naturally cool to below 200 ℃ behind the insulation 3h and take out material, through pulverizing; be lithium ion battery negative material after the screening.
Comparative example 3
Take by weighing the 60g diboron trioxide; 40g hot shortness phenolic resins; 10g pitch joins in the mixing and blending machine; mix under the room temperature and stir 1.5h; add average grain diameter 18 μ m; the native graphite micro mist 879g of degree of graphitization 〉=80%; continue to stir 2h; mixture packed into put into board-like kiln in the ceramic crucible, under the nitrogen atmosphere protection, rise to 270 ℃ with the speed of 3 ℃/min; insulation 3h; speed with 2 ℃/min rises to 1050 ℃ again, insulation 5h, after naturally cool to below 200 ℃ and take out material; through pulverizing; after the screening; speed with 5 ℃/min is warming up to 2850 ℃ under nitrogen atmosphere protection again, naturally cools to below 200 ℃ behind the insulation 4h and takes out material, through pulverizing; be lithium ion battery negative material after the screening.
Electrochemical property test
For detecting the performance that the present invention contains the lithium ion battery negative material of hard carbon coating, test with the half-cell method of testing, negative material with above embodiment and comparative example: SBR (solid content 50%): CMC=96.5: 1.8: 1.7 (weight ratio), add appropriate amount of deionized water and reconcile into pulpous state, coat on the Copper Foil and and made negative plate in 12 hours in the vacuum drying chamber inner drying; Use LiCoO
2Be positive electrode active materials, mix according to 94: 3 (weight ratio), add an amount of NMP, be coated on the aluminium foil, and make positive plate in the vacuum drying chamber inner drying as dispersant furnishing slurry with binding agent PVDF; Electrolyte is 1M LiPF
6/ EC+DEC+DMC=1: 1: 1, microporous polypropylene membrane was a barrier film, is assembled into battery.Cycle performance test uses having put of 300mA to carry out the constant current charge-discharge experiment, and charging/discharging voltage is limited in 4.2-3.0V, and that computerizeds control discharges and recharges collection and the control that cabinet carries out data.
The negative material performance that table 1 has been listed different embodiment and comparative example compares.
The negative material performance relatively in different embodiment of table 1 and the comparative example
From the result of table 1 as can be seen, hetero-atom, hard carbon presoma, soft carbon matrix precursor are indispensable in the modification of graphite is handled, and the coating in the present invention uses formula range is handled, and can improve the efficient first and the cycle performance of negative material.
Claims (4)
1. one kind contains the lithium ion battery negative material that hard carbon coats, it is characterized in that: the graphite surface clad material is formed hetero-atom modifier by hetero-atom modifier, hard carbon persursor material and soft carbon matrix precursor material: the hard carbon presoma: soft carbon matrix precursor weight ratio is 1: (2--3.3): (3-9); Hetero-atom modifier is boracic modified dose, is selected from boric acid, diboron trioxide; The hard carbon presoma is selected wherein one or more of phenolic resins, furfural resin, epoxy resin, furane resins, polyvinyl alcohol or polyacrylonitrile for use; Soft carbon matrix precursor is selected pitch for use.
2. a kind of lithium ion battery negative material that hard carbon coats that contains according to claim 1, it is characterized in that: graphite is natural or/and Delanium, its granularity is 5-70 μ m, and degree of graphitization 〉=80%, graphite account for the 150-900% of clad material mass percent.
3. preparation method who contains the lithium ion battery negative material that hard carbon coats, it is characterized in that: with hetero-atom modifier, the hard carbon presoma, soft carbon matrix precursor, proportionally add in the mixing and blending machine and mix, after mixing 1-5h, in mixer, add the graphite that takes by weighing by mass percentage again, continue to mix 1-5h; Hetero-atom modifier wherein: the hard carbon presoma: soft carbon matrix precursor weight ratio is 1: (2-3.3): (3-9).
4. a kind of preparation method who contains the lithium ion battery negative material that hard carbon coats according to claim 3 is characterized in that: with graphite with after clad material fully mixes, at inert gas N
2Perhaps the Ar protection 100 ℃ of-300 ℃ of cured, is incubated 1-3h down; Rise to 800 ℃-1200 ℃ with 1-10 ℃/min speed after the cured, insulation 0.5-6h is cooled to below 200 ℃; Behind the crushing screening, carry out the secondary high temperature graphitization and handle, rise to 2800 ℃-3200 ℃ with 1-10 ℃/min speed, insulation 0.5-6h, cooling back crushing screening both must contain the lithium ion battery negative material that hard carbon coats.
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