CN101931076A - Method for preparing silicon carbide composite particles and application thereof as cathode material of lithium ion battery - Google Patents
Method for preparing silicon carbide composite particles and application thereof as cathode material of lithium ion battery Download PDFInfo
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Abstract
The invention discloses a method for preparing silicon carbide composite particles and application thereof as a cathode material of a lithium ion battery. The method for preparing silicon carbide composite particles comprises the following steps: 1) performing electrostatic spraying on solution containing a silicon source and a carbon source so as to obtain spherical particles, wherein the carbon source is a carbon-containing high-molecular polymer; and 2) sintering the spherical particles in a non-oxidizing atmosphere to obtain the silicon carbide particles. The method enables one-step forming without needing a template and has high practicality; and moreover, the obtained silicon carbide composite particle integrates the advantages of the silicon carbide composite material with the advantages of a porous material, and improves the problems of weak cyclicity and low coulombic efficiency of using silicon-based material as the cathode material of the lithium ion battery.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide composite particles and as the application of lithium ion battery negative material.
Background technology
Lithium ion battery is because of it has operating voltage height, specific energy height, capacity is big, self discharge is little, cyclicity is good, the ideal source of long service life, in light weight, outstanding advantage becomes portable electric appts such as mobile phone, notebook computer such as volume is little.In order to satisfy instructions for use, high power capacity, extended-life lithium ion battery become an important research direction of lithium ion battery development.Because the specific capacity of positive electrode is relatively low, the room for promotion of capacity is little, so the development work of high-capacity lithium ion cell mainly concentrates on negative material.The existing commercial negative material that uses is material with carbon element, and its theoretical specific capacity only has 372mAh/g, and therefore seeking the high power capacity negative material that substitutes carbon becomes an important research direction.
Because silicon has high theoretical specific capacity (4200mAh/g) and lower embedding lithium current potential, and in the earth abundant, lower, the environmental sound of cost of reserves, be a kind of promising negative material.Yet in charge and discharge process, the removal lithium embedded process of silicon is followed 310% change in volume, causes that electrode cracking and active material come off from collector, and structure is destroyed gradually, and capacity constantly descends in cyclic process repeatedly.At this shortcoming, mainly improve the cyclicity of silicon materials in recent years by the following aspects:
1, nano silicon material
In order to improve the cycle performance of elemental silicon, the silicon nanometer can be reduced the change in volume of silicon to a certain extent, reduce electrode interior stress.The contraction although silicon nanowires, nano-tube volume in charge and discharge process can expand, length and diameter also can change, but the variation that the space that silicon nanowires or pipe oldered array exist can buffer volumes, make that structure is not broken in the repeated charge process, electronics can flow to nano wire or pipe from collector effectively simultaneously, and the electrolyte that permeates between nano wire or pipe array has shortened the path of lithium ion diffusion, makes it have good cyclicity and high-multiplying power discharge.Although the cyclicity of silicon nanowires, nano-tube is better, its preparation process complexity yields poorly, and is difficult to large-scale industrialization production, and degree of being practical is low.
In the whole bag of tricks of preparation nano material, but, be widely used in preparing the nano material of multiple structures such as nano thin-film, nanofiber, nanotube, nano/micron packing, quantum dot owing to static fluidics one-step shaping, need not template.But static fluidics liquid droplets shape or fibrous material, be called electrostatic spray (abbreviation EFI) and electrostatic spinning (abbreviation electrospinning), wherein, utilize the nano/micron packing of electrostatic spray preparation to have the dispersion unicity of height, and the institute of embedding well carrier material, electrostatic spray is mainly used in the preparation medicament slow release preparation at present.
2, silicon based composite material
Study more silicon based composite material and mainly contain the silico-carbo composite material.Flexibility, good electron conductivity, less density, smaller volume expand (10%) because carbon has preferably, therefore become the active matrix of silicon-based anode material.Carry out after carbon coats at silicon face, help contacting of isolated silicon and electrolyte, reduce surface area, reduce irreversible capacity, also prevent the reunion and the growth of silicon grain in the charge and discharge process simultaneously, thereby improve the capacity maintenance performance of silicon-based anode material.But also there are some problems in Si-C composite material, adopts pyrolysismethod, ball-milling method, vapour deposition process and polymerization-pyrolysismethod etc. during preparation usually, and the material homogeneity that these methods obtain is relatively poor, and silicon is dispersed bad in carbon matrix, and the interface contact of silicon-carbon is relatively poor.
Except adopting above-mentioned composite material, discover recently, a large amount of hole and the electron channels of design in silicon based composite material, can alleviate the destruction that the silicon materials change in volume causes the electrode material structure in charge and discharge process, keep the good electron migrating channels, make silicon based composite material have good capacity hold facility and high-multiplying power discharge.
Summary of the invention
The purpose of this invention is to provide a kind of silicon carbide composite particles and preparation method thereof.
Silicon carbide composite particles provided by the present invention is to prepare according to the method that comprises the steps:
1) solution that will contain silicon source and carbon source carries out electrostatic spray, obtains spheric granules; Wherein, described carbon source is the high molecular polymer of carbon containing;
2) described spheric granules is carried out sintering under non-oxidizing atmosphere, obtain described silicon carbide composite particles.
Wherein, the source of silicon described in the step 1) can be selected from following at least a: silicon quantum dot, silica flour and silicon monoxide.Described carbon source can be the synthesising macromolecule copolymer and/or the natural polymers of carbon containing; Described synthesising macromolecule copolymer specifically can be at least a in the following substances: phenolic resins, polyvinylidene fluoride (PVDF), polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyethylene glycol oxide (PEO), polyvinyl chloride (PVC), polyacrylonitrile (PAN); Described natural polymers specifically can be at least a in the following substances: glucan, starch, gelatin, shitosan, sodium carboxymethylcellulose and alginic acid.
The mass ratio of source of silicon described in the step 1) and carbon source can be (0.1～20): (1～50) is preferably (0.1-1): (1～50) specifically can be 0.1: 50,0.1: 20,0.1: 1,1: 1; The mass concentration sum of silicon source and carbon source can be 1～50% in the described solution.
Electrostatic spray described in the step 1) adopts the static fluidic device to carry out; Described static fluidic device comprises at least: high voltage source, syringe, nozzle and receiving system, and wherein, the port of export of syringe connects nozzle, and the output of high voltage source is connected on the nozzle, and receiving system is positioned at the nozzle below and keeps certain distance with nozzle.The voltage of described high voltage source is 30～300KV, specifically can be 150KV, and the distance in described nozzle and the receiving system between the collecting board is 10～50cm, specifically can be 20cm.
Step 2) non-oxidizing atmosphere described in is provided by following at least a gas: nitrogen, argon gas, hydrogen, helium and carbon dioxide.
The condition of sintering step 2) is: be warming up to 300～1000 ℃ of sintering temperatures by room temperature, keep described sintering temperature 1～30h, be cooled to room temperature; The speed of described intensification is 1～20 ℃/min.
The particle diameter of silicon carbide composite particles provided by the present invention is nanoscale or micron order: the carbon in the described silicon carbide composite particles exists with the form of amorphous carbon and/or graphitized carbon; Described silicon carbide composite particles inside is the skeleton structure of porous carbon.
Further object of the present invention provides the application of described silicon carbide composite particles.
Application provided by the present invention is the application of silicon carbide composite particles as battery electrode material, particularly as the application of lithium ion battery negative material.
The present invention also provides a kind of energy storage elements, and described energy storage elements contains described silicon carbide composite particles, this energy storage elements preferred lithium ion battery.
The present invention also provides a kind of portable electric appts, and this electronic equipment uses above-mentioned energy storage elements, the preferred mobile phone of this portable electric appts, camera, video camera, MP3, MP4, notebook computer.
Compared with prior art, but preparation method's one-step shaping provided by the invention, need not template, the degree of being practical height, and the advantage of the silicon carbide composite particles that obtains is integrated Si-C composite material and porous material has improved that silica-base material is poor as the cyclicity that lithium ion battery negative material exists, the inefficient problem of enclosed pasture.
Description of drawings
Fig. 1 is the structural representation of the static fluidic device of the present invention's use.
The electron scanning micrograph of the silicon carbide composite particles that Fig. 2 obtains for embodiment 1.
X-ray diffraction (XRD) collection of illustrative plates of the silicon carbide composite particles that Fig. 3 obtains for embodiment 1.
Fig. 4 is a negative material for the silicon carbide composite particles that obtains with embodiment 4, the charging and discharging curve under 50mA/g constant current charge-discharge condition.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but the present invention is not limited to following examples.
Experimental technique described in the following embodiment if no special instructions, is conventional method; Described reagent and material if no special instructions, all can obtain from commercial channels.
Used static fluidic device among the following embodiment, its structural representation as shown in Figure 1, comprise: high voltage source, syringe, shower nozzle and receiving system, wherein, the solution that contains silicon source and carbon source is housed in the syringe, the port of export of syringe connects nozzle, and the output of high voltage source is connected on the nozzle, and receiving system is positioned at the nozzle below and keeps certain distance with nozzle.
The preparation of embodiment 1, silicon carbide composite particles and electrochemical property test thereof
By shitosan (weight average molecular weight is 89000): the mass ratio of silicon quantum dot=50: 0.1 mixes, and is solvent with water, at room temperature stirs more than the 24h, and the mass concentration sum that obtains shitosan and silicon quantum dot is 1% solution.Polymer solution is injected the syringe of static fluidic device, and shower nozzle is apart from collecting board 20cm, and voltage is 150kV; carry out electrostatic spray; the particle speed with 10 ℃/min under nitrogen protection that obtains is risen to 800 ℃ by room temperature, naturally cool to room temperature behind the constant temperature 6h, obtain silicon carbide composite particles.
The sign of silicon carbide composite particles:
With the particle diameter and the particle size distribution of the silicon carbide composite particles that obtains under the above-mentioned condition of NEC ESEM (JEOL-6700F) detection, the result shows that the particle size distribution of silicon carbide composite particles is more even, and particle diameter is (see figure 2) between 10～100 microns.
With powder x-ray diffraction (Rigaku DmaxrB, CuK
αRay) as can be seen from Figure 3, there is not impurity peaks in the crystal structure of analysis silicon carbide composite particles in the spectrogram, and the product purity height is described; Because the carbon of gained is noncrystalline structure, so there is not its diffraction maximum.
The chemical property of silicon carbide composite particles characterizes:
Silicon carbide composite particles, acetylene black and the Kynoar (binding agent) that prepare among the embodiment 1 are made into slurry with mass ratio mixing in 80: 10: 10, are coated to equably on the Copper Foil collector and obtain cathode membrane.As positive pole, microporous polypropylene membrane (Celgard 2400) is as barrier film with metal lithium sheet, 1mol/L LiPF
6(solvent is that volume ratio is 1: 1 ethylene carbonate and a dimethyl carbonate mixed liquor) is assembled into the Swagelok pattern and intends battery as electrolyte in the glove box of argon shield.
The battery of above-mentioned assembling is carried out the constant current charge-discharge test on Arbin BT2000 charge-discharge test instrument, charge-discharge magnification is 50mA/g, and the charging/discharging voltage interval is 0～2.0V, and charging and discharging curve is seen Fig. 4.The composition of the silicon carbide composite particles for preparing in the present embodiment and simulated battery test result are listed in table 1.
The preparation of embodiment 2, silicon carbide composite particles and electrochemical property test thereof
By shitosan (weight average molecular weight is 89000): the mass ratio of silica flour=20: 0.1 mixes, and is solvent with water, at room temperature stirs more than the 24h, and the mass concentration sum that obtains shitosan and silica flour is 5% solution.Polymer solution is injected the syringe of static fluidic device; shower nozzle is apart from collecting board 20cm; high pressure is 150kV; carry out electrostatic spray; the particle speed with 15 ℃/min under nitrogen protection that obtains is risen to 300 ℃ by room temperature; reduce to room temperature with the speed of 10 ℃/min behind the constant temperature 6h, obtain silicon carbide composite particles.
The positive pole of simulated battery, negative pole, electrolyte and battery assembling are identical with embodiment 1, and the composition of gained silicon carbide composite particles reaches and lists in table 1 in the test result of simulated battery.
The preparation of embodiment 3, silicon carbide composite particles and electrochemical property test thereof
In sodium carboxymethylcellulose (weight average molecular weight is 250000): the ratio (mass ratio) of silicon monoxide=1: 0.1 is mixed, with water is solvent, at room temperature stir more than the 24h, the mass concentration sum that obtains sodium carboxymethylcellulose and silicon monoxide is 50% solution.Polymer solution is injected the syringe of static fluidic device, and shower nozzle is apart from collecting board 20cm, and high pressure is 150kV; carry out electrostatic spray; the particle speed with 20 ℃/min under nitrogen protection that obtains is risen to 1000 ℃ by room temperature, naturally cool to room temperature behind the constant temperature 6h, obtain silicon carbide composite particles.
The positive pole of simulated battery, negative pole, electrolyte and battery assembling are identical with embodiment 1, and the composition of gained silicon carbide composite particles reaches and lists in table 1 in the test result of simulated battery.
The preparation of embodiment 4, silicon carbide composite particles and electrochemical property test thereof
In starch (weight average molecular weight is 300000): the ratio (mass ratio) of silicon monoxide=1: 1 is mixed, and is solvent with water, at room temperature stirs more than the 24h, obtains starch and silicon monoxide mass concentration sum and be 20% solution.Polymer solution is injected the syringe of static fluidic device; shower nozzle is apart from collecting board 20cm; high pressure is 150kV; carry out electrostatic spray; the particle speed with 10 ℃/min under nitrogen protection that obtains is risen to 1000 ℃ by room temperature; reduce to room temperature with the speed of 10 ℃/min behind the constant temperature 6h, obtain silicon carbide composite particles.
The positive pole of simulated battery, negative pole, electrolyte and battery assembling are identical with embodiment 1, and the composition of gained silicon carbide composite particles reaches and lists in table 1 in the test result of simulated battery.
The composition of table 1, silicon carbide composite particles reaches the test result of constant current charge-discharge under the 50mA/g condition
From the result of table 1 as can be seen, the silicon carbide composite particles discharge capacity of the present invention's preparation can reach more than the 1000mAh/g, and enclosed pasture efficient can reach more than 90%, has improved poor, the inefficient problem of enclosed pasture of cycle performance that the silicon-based anode material exists to a great extent.
Claims (10)
1. method for preparing silicon carbide composite particles may further comprise the steps:
1) solution that will contain silicon source and carbon source carries out electrostatic spray, obtains particle; Wherein, described carbon source is the high molecular polymer of carbon containing;
2) described particle is carried out sintering under non-oxidizing atmosphere, obtain described silicon carbide composite particles.
2. method according to claim 1 is characterized in that: the source of silicon described in the step 1) is selected from following at least a: silicon quantum dot, silica flour and silicon monoxide.
3. method according to claim 1 and 2 is characterized in that: carbon source described in the step 1) is the synthesising macromolecule copolymer and/or the natural polymers of carbon containing; Described synthesising macromolecule copolymer is preferably at least a in the following substances: phenolic resins, polyvinylidene fluoride, polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol oxide, polyvinyl chloride and polyacrylonitrile; Described natural polymers is preferably at least a in the following substances: glucan, starch, gelatin, shitosan, sodium carboxymethylcellulose and alginic acid.
4. according to arbitrary described method among the claim 1-3, it is characterized in that: the mass ratio of source of silicon described in the step 1) and carbon source is (0.1～20): (1～50); The mass concentration sum of silicon source and carbon source is 1～50% in the described solution.
5. according to arbitrary described method among the claim 1-4, it is characterized in that: electrostatic spray described in the step 1) adopts the static fluidic device to carry out; Described static fluidic device comprises at least: high voltage source, syringe, nozzle and receiving system; The voltage of described high voltage source is 30～300KV, and the distance in described nozzle and the receiving system between the collecting board is 10～50cm.
6. according to arbitrary described method among the claim 1-5, it is characterized in that: step 2) described in non-oxidizing atmosphere provide by following at least a gas: nitrogen, argon gas, hydrogen, helium and carbon dioxide;
The condition of sintering step 2) is: be warming up to 300～1000 ℃ of sintering temperatures by room temperature, keep described sintering temperature 1～30h, be cooled to room temperature; The speed of described intensification is 1～20 ℃/min.
7. the silicon carbide composite particles that arbitrary described method prepares among the claim 1-6.
8. the described silicon carbide composite particles of claim 7 is as the application of battery electrode material, particularly as the application of lithium ion battery negative material.
9. an energy storage elements is characterized in that: contain the described silicon carbide composite particles of claim 7.
10. a portable electric appts is characterized in that: use the described energy storage elements of claim 9.
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| CN102299306A (en) * | 2011-07-15 | 2011-12-28 | 中国科学院广州能源研究所 | Nano-silicon composite lithium ion battery cathode material with poly (3,4-ethylenedioxythiophene) as coating and carbon source and preparation method thereof |
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| CN103187556A (en) * | 2011-12-27 | 2013-07-03 | 宁波杉杉新材料科技有限公司 | Lithium ion battery and anode material thereof, preparation method |
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| CN111326720A (en) * | 2018-12-14 | 2020-06-23 | 天津师范大学 | Silicon-carbon composite material and preparation method and application thereof |
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| CN109950546B (en) * | 2019-03-24 | 2021-04-13 | 湖北中一科技股份有限公司 | Copper foil manufacturing process and negative current collector |
| CN116454543A (en) * | 2023-06-16 | 2023-07-18 | 深圳海辰储能控制技术有限公司 | Diaphragm, preparation method thereof, energy storage device and electric equipment |
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