CN101931076B - 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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- CN101931076B CN101931076B CN201010241963.2A CN201010241963A CN101931076B CN 101931076 B CN101931076 B CN 101931076B CN 201010241963 A CN201010241963 A CN 201010241963A CN 101931076 B CN101931076 B CN 101931076B
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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 has the ideal source that the outstanding advantages such as operating voltage is high, specific energy is high, capacity is large, self discharge is little, cyclicity is good, long service life, lightweight, volume is little become the portable electric appts such as mobile phone, notebook computer because of it.In order to meet 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, therefore the development work of high-capacity lithium ion cell mainly concentrates on negative material.The negative material of existing commercial use is material with carbon element, and its theoretical specific capacity only has 372mAh/g, and the high power capacity negative material of therefore finding alternative carbon becomes an important research direction.
Because silicon has higher theoretical specific capacity (4200mAh/g) and lower embedding lithium current potential, and reserves are abundant, cost is lower, environmental sound, is a kind of promising negative material in the earth.Yet in charge and discharge process, the removal lithium embedded process of silicon is followed 310% change in volume, cause that electrode cracking and active material come off from collector, structure is destroyed gradually, and in cyclic process repeatedly, capacity constantly declines.For this shortcoming, mainly by the following aspects, improve in recent years the cyclicity of silicon materials:
1, nano silicon material
In order to improve the cycle performance of elemental silicon, silicon nanometer can be reduced to a certain extent to the change in volume of silicon, reduce electrode interior stress.Although silicon nanowires, nano-tube be volume meeting dilation in charge and discharge process, length and diameter also can change, but the variation that the space that silicon nanowires or pipe oldered array exist can buffer volumes, structure in repeated charge process is not broken, electronics can flow to nano wire or pipe from collector effectively simultaneously, and the electrolyte permeating 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 is complicated, yields poorly, and is difficult to large-scale industrialization and produces, and degree of being practical is low.
In the whole bag of tricks of preparation nano material, due to static fluidics can one-step shaping, without template, be widely used in preparing the nano material of the various structures such as nano thin-film, nanofiber, nanotube, nano/micron packing, quantum dot.Static fluidics can liquid droplets shape or fibrous material, be called electrostatic spray (abbreviation EFI) and electrostatic spinning (abbreviation electrospinning), wherein, utilize nano/micron packing prepared by electrostatic spray to there is dispersion unicity highly, and the institute of embedding well carrier material, electrostatic spray is mainly for the preparation of medicament slow release preparation at present.
2, silicon based composite material
Study more silicon based composite material and mainly contain silico-carbo composite material.Because carbon has good flexibility, good electron conduction, less density, less volumetric expansion (10%), therefore become the active matrix of silicon based anode material.Silicon face carry out carbon coated after, be conducive to contacting of isolated silicon and electrolyte, reduce surface area, reduce irreversible capacity, also prevent reunion and the growth of silicon grain in charge and discharge process simultaneously, thereby the Capacitance reserve performance of raising silicon based anode material.But also there are some problems in Si-C composite material, during preparation, conventionally adopt pyrolysismethod, ball-milling method, vapour deposition process and polymerization-pyrolysismethod etc., the material homogeneity that these methods obtain is poor, and silicon is dispersed bad in carbon matrix, and the interface contact of silicon-carbon is poor.
Except adopting above-mentioned composite material, research is recently found, in silicon based composite material, design a large amount of holes and electron channel, can alleviate the destruction that silicon materials change in volume causes electrode material structure in charge and discharge process, keep good electron transfer passage, make silicon based composite material there is good Capacitance reserve ability and high-multiplying power discharge.
Summary of the invention
The object 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 comprising the steps:
1) solution that contains silicon source and carbon source is carried out to electrostatic spray, obtain spheric granules; Wherein, the high molecular polymer that described carbon source is carbon containing;
2) described spheric granules is carried out under non-oxidizing atmosphere to sintering, obtain described silicon carbide composite particles.
Wherein, silicon source step 1) can be selected from following at least one: silicon quantum dot, silica flour and silicon monoxide.Described carbon source can be synthesising macromolecule copolymer and/or the natural polymers of carbon containing; Described synthesising macromolecule copolymer specifically can be at least one in 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 one in following substances: glucan, starch, gelatin, shitosan, sodium carboxymethylcellulose and alginic acid.
The mass ratio of the source of silicon 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; In described solution, the mass concentration sum of silicon source and carbon source can be 1～50%.
Step 1) electrostatic spray described in adopts static fluidic device to carry out; Described static fluidic device at least comprises: 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 nozzle, and receiving system is positioned at 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 receiving system between collecting board is 10～50cm, specifically can be 20cm.
Step 2) non-oxidizing atmosphere described in is provided by following at least one gas: nitrogen, argon gas, hydrogen, helium and carbon dioxide.
The condition of sintering step 2) is: by room temperature, be warming up to 300～1000 ℃ of sintering temperatures, 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 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 is to provide the application of described silicon carbide composite particles.
Application provided by the present invention is that silicon carbide composite particles is as the application of 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, preparation method provided by the invention can one-step shaping, without template, degree of being practical is high, and the advantage of the silicon carbide composite particles obtaining is integrated Si-C composite material and porous material, has improved that the cyclicity that silica-base material exists as lithium ion battery negative material is poor, coulomb inefficient problem.
Accompanying drawing explanation
Fig. 1 is the structural representation of the static fluidic device that uses of the present invention.
Fig. 2 is the electron scanning micrograph of the silicon carbide composite particles that obtains of embodiment 1.
Fig. 3 is X-ray diffraction (XRD) collection of illustrative plates of the silicon carbide composite particles that obtains of embodiment 1.
Fig. 4 is negative material for take the silicon carbide composite particles that embodiment 4 obtains, the charging and discharging curve under 50mA/g constant current charge-discharge condition.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but the present invention is not limited to following examples.
Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Static fluidic device used in 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 syringe, the port of export of syringe connects nozzle, and the output of high voltage source is connected on nozzle, and receiving system is positioned at 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): silicon quantum dot=50: 0.1 mass ratio mixes, and take water as solvent, more than at room temperature stirring 24h, the solution that the mass concentration sum that obtains shitosan and silicon quantum dot is 1%.Polymer solution is injected to the syringe of static fluidic device, shower nozzle is apart from collecting board 20cm, and voltage is 150kV; carry out electrostatic spray; the particle obtaining speed with 10 ℃/min under nitrogen protection is risen to 800 ℃ by room temperature, after constant temperature 6h, naturally cool to room temperature, obtain silicon carbide composite particles.
The sign of silicon carbide composite particles:
With NEC ESEM (JEOL-6700F), detect particle diameter and the particle size distribution of the silicon carbide composite particles obtaining under above-mentioned condition, result shows that the particle size distribution of silicon carbide composite particles is more even, and particle diameter (is shown in Fig. 2) between 10～100 microns.
With powder x-ray diffraction (Rigaku DmaxrB, CuK
αray) analyze the crystal structure of silicon carbide composite particles, as can be seen from Figure 3, in spectrogram, do not have impurity peaks, illustrate that product purity is high; Because the carbon of gained is noncrystalline structure, so there is no its diffraction maximum.
The Electrochemical Characterization of silicon carbide composite particles:
The silicon carbide composite particles preparing in embodiment 1, acetylene black and Kynoar (binding agent) are mixed and are made into slurry with mass ratio at 80: 10: 10, be coated to equably on Copper Foil collector and obtain cathode membrane.Using metal lithium sheet as positive pole, and microporous polypropylene membrane (Celgard 2400) is as barrier film, 1mol/L LiPF
6(solvent is that volume ratio is ethylene carbonate and the dimethyl carbonate mixed liquor of 1: 1), as electrolyte, is assembled into Swagelok type simulated battery in the glove box of argon shield.
The battery of above-mentioned assembling is carried out to constant current charge-discharge test on Arbin BT2000 charge-discharge test instrument, and charge-discharge magnification is 50mA/g, and charging/discharging voltage interval is 0～2.0V, and charging and discharging curve is shown in Fig. 4.The composition of the silicon carbide composite particles 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): silica flour=20: 0.1 mass ratio mixes, and take water as solvent, more than at room temperature stirring 24h, the solution that the mass concentration sum that obtains shitosan and silica flour is 5%.Polymer solution is injected to the syringe of static fluidic device; shower nozzle is apart from collecting board 20cm; high pressure is 150kV; carry out electrostatic spray; the particle obtaining speed with 15 ℃/min under nitrogen protection is risen to 300 ℃ by room temperature; after constant temperature 6h, with the speed of 10 ℃/min, be down to room temperature, obtain silicon carbide composite particles.
The positive pole of simulated battery, negative pole, electrolyte and battery assembling are identical with embodiment 1, the composition of gained silicon carbide composite particles and list 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): silicon monoxide=1: 0.1 ratio (mass ratio) is mixed, take water as solvent, more than at room temperature stirring 24h, the solution that the mass concentration sum that obtains sodium carboxymethylcellulose and silicon monoxide is 50%.Polymer solution is injected to the syringe of static fluidic device, shower nozzle is apart from collecting board 20cm, and high pressure is 150kV; carry out electrostatic spray; the particle obtaining speed with 20 ℃/min under nitrogen protection is risen to 1000 ℃ by room temperature, after constant temperature 6h, naturally cool to room temperature, obtain silicon carbide composite particles.
The positive pole of simulated battery, negative pole, electrolyte and battery assembling are identical with embodiment 1, the composition of gained silicon carbide composite particles and list 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): silicon monoxide=1: 1 ratio (mass ratio) is mixed, and take water as solvent, more than at room temperature stirring 24h, obtains the solution that starch and silicon monoxide mass concentration sum are 20%.Polymer solution is injected to the syringe of static fluidic device; shower nozzle is apart from collecting board 20cm; high pressure is 150kV; carry out electrostatic spray; the particle obtaining speed with 10 ℃/min under nitrogen protection is risen to 1000 ℃ by room temperature; after constant temperature 6h, with the speed of 10 ℃/min, be down to room temperature, obtain silicon carbide composite particles.
The positive pole of simulated battery, negative pole, electrolyte and battery assembling are identical with embodiment 1, the composition of gained silicon carbide composite particles and list in table 1 in the test result of simulated battery.
The composition of table 1, silicon carbide composite particles and under 50mA/g condition the test result of constant current charge-discharge
From the results shown in Table 1, more than silicon carbide composite particles discharge capacity prepared by the present invention can reach 1000mAh/g, and coulomb efficiency can reach more than 90%, improved to a great extent that the cycle performance that silicon based anode material exists is poor, coulomb inefficient problem.
Claims (6)
1. a method of preparing silicon carbide composite particles, comprises the following steps:
1) solution that contains silicon source and carbon source is carried out to electrostatic spray, obtain particle;
2) described particle is carried out under non-oxidizing atmosphere to sintering, obtain described silicon carbide composite particles;
Wherein, electrostatic spray step 1) adopts static fluidic device to carry out; Described static fluidic device at least comprises: 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 receiving system between collecting board is 10～50cm;
Step 1) described carbon source is sodium carboxymethylcellulose and alginic acid, and described silicon source is silicon monoxide; The mass ratio of described silicon source and carbon source is (0.1～20): (1～50); In described solution, the mass concentration sum of silicon source and carbon source is 1～50%.
2. method according to claim 1, is characterized in that: step 2) described in non-oxidizing atmosphere by following at least one gas, provided: nitrogen, argon gas, hydrogen, helium and carbon dioxide; The condition of sintering step 2) is: by room temperature, be warming up to 300～1000 ℃ of sintering temperatures, keep described sintering temperature 1～30h, be cooled to room temperature; The speed of described intensification is 1～20 ℃/min.
3. the silicon carbide composite particles that in claim 1-2, arbitrary described method prepares.
4. silicon carbide composite particles claimed in claim 3 is as the application of battery electrode material, and described battery electrode material is lithium ion battery negative material.
5. an energy storage elements, is characterized in that: contain lithium ion battery negative material claimed in claim 4.
6. a portable electric appts, is characterized in that: right to use requires the energy storage elements described in 5.
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| CN102299306B (en) * | 2011-07-15 | 2015-01-21 | 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 |
| KR101708360B1 (en) * | 2011-10-05 | 2017-02-21 | 삼성에스디아이 주식회사 | Negative active material and lithium battery containing the material |
| CN103187556B (en) * | 2011-12-27 | 2017-07-28 | 宁波杉杉新材料科技有限公司 | Lithium ion battery and its negative material, preparation method |
| KR101615439B1 (en) * | 2014-07-17 | 2016-05-13 | 오씨아이 주식회사 | Manufacturing mehtod of carbon-silicon composite |
| CN104852027B (en) * | 2015-04-09 | 2017-09-01 | 江西师范大学 | A kind of preparation method of the Si/C composites with three-dimensional caged dodecahedron structure |
| KR102368307B1 (en) * | 2015-09-16 | 2022-03-02 | 삼성전자주식회사 | Electrode active material, electrode and secondary battery including the same, and method of preparing the electrode active material |
| CN106876665B (en) * | 2015-12-14 | 2019-08-02 | 中国科学院苏州纳米技术与纳米仿生研究所 | Silicon carbide composite particles, preparation method and application |
| CN107170980A (en) * | 2016-08-01 | 2017-09-15 | 深圳市比克动力电池有限公司 | A kind of silicon based anode material, lithium battery cathode plate of its application and preparation method thereof |
| CN106898755B (en) * | 2017-04-24 | 2019-08-16 | 广东烛光新能源科技有限公司 | The preparation method of silicon-carbon cathode material and the silicon-carbon cathode material being prepared using this method |
| CN106876687B (en) * | 2017-04-28 | 2020-03-31 | 无锡德碳科技股份有限公司 | Preparation method of carbon-coated silicon quantum dot composite lithium ion battery negative electrode material |
| CN108365188B (en) * | 2018-01-17 | 2020-12-15 | 上海大学 | Preparation method of SiO/C composite negative electrode material for lithium ion battery |
| CN108987685A (en) * | 2018-06-11 | 2018-12-11 | 浙江衡远新能源科技有限公司 | A kind of preparation method of the three-dimensional porous silicon substrate carbon compound film negative electrode material of lithium ion battery |
| CN109092240A (en) * | 2018-09-17 | 2018-12-28 | 佛山皖和新能源科技有限公司 | A kind of preparation method of porous magnetic hydroxylapatite microballoon |
| CN111326720A (en) * | 2018-12-14 | 2020-06-23 | 天津师范大学 | Silicon-carbon composite material and preparation method and application thereof |
| 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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