CN105633374A - Preparation method of silicon-carbon-graphite composite anode material - Google Patents
Preparation method of silicon-carbon-graphite composite anode material Download PDFInfo
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Abstract
The invention relates to a preparation method of a silicon-carbon-graphite composite anode material. The method comprises the following steps of carrying out carbon coating on nanosilicon dioxide powder; with magnesium powder as a reducing agent, reducing carbon-coated nanosilicon dioxide into carbon-coated nanosilicon through magnesiothermic reduction; and with the carbon-coated nanosilicon as a raw material, fully mixing the carbon-coated nanosilicon with graphite powder at a certain mass ratio to prepare the silicon-carbon-graphite composite anode material. The required reduction temperature is low; the preparation technology is simple; mass production is easy to achieve; and the prepared composite material has excellent cycle performance and relatively high first cycle columbic efficiency when applied to a positive electrode of a lithium-ion battery.
Description
Technical field
The present invention relates to the use of magnesium reduction process and prepare the nano-silicon of carbon cladding, and be mixed with silico-carbo-graphite composite material by a certain percentage with graphite as lithium ion battery negative material, belong to field of functional materials.
Background technology
As lithium ion battery negative material, the theoretical specific capacity of silicon reaches 4200mAh/g, thus causes and extensively pay attention to and research. But the poorly conductive of silicon, circulation coulombic efficiency is low first, there is violent change in volume (> 300% in charge and discharge process simultaneously) so that the easy efflorescence of silicon materials, intergranular electrical contact performance declines, and causes that its cycle performance is not good. In order to reduce the impact of this change in volume, method of modifying conventional at present includes, by silicon nanorize, preparing silicon materials and the doped metallic elements etc. of carbon cladding, and these methods have been demonstrated effectively to improve the cycle performance of silicon.
The negative material of current commercial Li-ion battery is mainly graphite-like material with carbon element, and its volumetric expansion is little, initial coulomb efficiency higher (more than 90%), therefore, graphite and nano-silicon compound can be effectively improved the initial coulomb efficiency of material. And graphite has the electric conductivity of excellence, it is also beneficial to improve the composite charge-discharge performance when high current density. The preparation method that patent of invention " a kind of lithium ion battery silicon/carbon graphite composite negative pole material and preparation method thereof " (patent publication No.: CN1761089N) discloses a kind of silicon/carbon graphite mixed powder material, it is characterized in that the silica flour after by ball milling and graphite add in carbohydrate saturated solution, add concentrated sulphuric acid after drying, utilize the dehydration carbonization of concentrated sulphuric acid to prepare the electrode material of silicon, graphite, amorphous carbon mixing. The cycle performance of this silicon/carbon graphite material preferably, but circulates coulombic efficiency first and only has about 70%, it is difficult to meet practical requirement.
At present, industrial preparing polysilicon typically by carbothermic method, reaction generates thick silicon and byproducts of carbon monoxide gas. Thick silicon reacts with chlorine and hydrogen more successively under the high temperature conditions, finally obtains pure silicon. The method reduction temperature higher (more than 2000 DEG C), energy consumption is higher, and by-product silicon grain that is many and that obtain is of a size of micron order, is not suitable for lithium ion battery negative material. Magnesium is a kind of active metal, magnesiothermic reduction is exothermic reaction, it is silicon hence with magnesium reduction process by reducing silica, reaction temperature can be greatly reduced, thus suppressing the particle growth caused because of high temperature, finally give nano level silicon materials, and the by-product of this reaction only has magnesium oxide, it is easy to remove.
Summary of the invention
It is desirable to provide the preparation method of a kind of silico-carbo-composite cathode material of silicon/carbon/graphite. First the nano silicon SiO of carbon cladding is prepared2/ C, then utilizes magnesium reduction process by SiO2/ C is reduced to nano-silicon Si/C, the Si/C of carbon cladding and then mixes than with graphite powder according to certain mass, prepares the silico-carbo-graphite composite material negative material as lithium ion battery. This preparation method has that reduction temperature is relatively low, energy consumption is relatively low, simple process and be prone to industrialization and convert the feature produced, and this composite for lithium ion battery time there is the cycle performance of excellence and high coulombic efficiency.
A kind of method preparing above-mentioned silico-carbo-composite cathode material of silicon/carbon/graphite, comprises the following steps that:
(1) by SiO2Nano-powder and carbon source are according to certain mass than mix homogeneously, and its additional proportion is: 1:0.5��SiO2: carbon source mass ratio��1:5; Then under inert gas shielding, temperature is increased to 700��1100 DEG C of constant temperature 1��5 hour, is finally cooled to room temperature; Carbon source is generally adopted Colophonium, phenolic resin, starch.
(2) magnesium powder and the obtained carbon coated silica SiO of above-mentioned steps (1) are weighed2/ C, according to mol ratio Mg:SiO2=2:1 weighs bi-material mix homogeneously respectively, reacts 2��8 hours in 600��800 DEG C under inert atmosphere protection. Naturally cool to after room temperature until it, put in dilute acid soln and stir, and with ethanol and deionized water filtration washing, obtain the nano Si of carbon cladding.
The principle of above-mentioned reaction is:
2Mg+SiO2/C��2MgO+Si/C��
(3) being mixed homogeneously than with graphite powder according to certain mass by the nano-silicon of carbon cladding obtained for step (2), its mass ratio is: 1:0.2��Si/C: graphite��1:5, obtains silico-carbo-composite cathode material of silicon/carbon/graphite.
Compared with prior art, the present invention possesses advantages below:
1. the preparation temperature of the present invention is low, energy consumption is little, low for equipment requirements.
2. the preparation method condition of the present invention is moderate, and technological process is simple, it is easy to industrialized production.
3. silico-carbo-the graphite composite material prepared by the present invention for lithium ion battery negative time there is cycle performance and the stability of excellence, and initial coulomb efficiency is high, it is possible to meet practical requirement, is the modified effective ways of silicon based anode material.
Accompanying drawing explanation
Fig. 1 (a) and (b) nano silicon SiO respectively2And carbon coated silica SiO2The stereoscan photograph of/C; C () and (d) is magnesiothermic reduction SiO respectively2The transmission electron microscope photo of the carbon coated Si Si/C that/C obtains and X-ray diffraction spectrum.
The stereoscan photograph that Fig. 2 (a) is graphite powder; B () and (c) is stereoscan photograph and the X-ray diffraction spectrum of Si/C and the mixed silico-carbo-composite cathode material of silicon/carbon/graphite of graphite powder 1:5 in mass ratio respectively; D () is 0.1mA/cm2Charge-discharge performance under current density condition.
Fig. 3 (a), (b) and (c) are Si/C and the mixed silico-carbo of graphite powder 1:2.5 in mass ratio-composite cathode material of silicon/carbon/graphite stereoscan photograph, X-ray diffraction spectrum and 0.1mA/cm respectively2Charge-discharge performance under current density condition.
Fig. 4 (a), (b) and (c) are Si/C and the mixed silico-carbo of graphite powder 1:1 in mass ratio-composite cathode material of silicon/carbon/graphite stereoscan photograph, X-ray diffraction spectrum and 0.1mA/cm respectively2Charge-discharge performance under current density condition.
Fig. 5 (a), (b) and (c) are Si/C and the mixed silico-carbo of graphite powder 1:0.2 in mass ratio-composite cathode material of silicon/carbon/graphite stereoscan photograph, X-ray diffraction spectrum and 0.1mA/cm respectively2Charge-discharge performance under current density condition.
Detailed description of the invention
Embodiment 1
Fig. 1 (a) is silicon dioxide SiO2The stereoscan photograph of nano-powder, SiO2Size between 10��20nm. By SiO2Nano-powder is mixed homogeneously according to mass ratio 1:0.5 with carbon source Colophonium, then in 700 DEG C of constant temperature 5 hours under argon atmosphere, is finally cooled to room temperature, obtains the silicon dioxide SiO of carbon cladding2/ C, as shown in Fig. 1 (b). It can be seen that SiO2/ C also presents powder shaped, and its size compares SiO2Nano-powder increases, average 20nm. According to Mg:SiO2Mol ratio be that 2:1 weighs SiO respectively2/ C nano powder body and magnesium powder (wherein SiO2SiO in/C2Mass content be tested to be 70%), and be sufficiently mixed uniformly, react 8 hours in 600 DEG C under argon atmosphere. Naturally cool to after room temperature until it, put in dilute hydrochloric acid solution and stir, and with ethanol and deionized water filtration washing, obtain the nano Si/C of carbon cladding. Fig. 1 (c) is the transmission electron microscope photo of Si/C, it can be seen that at the Surface coating carbon-coating of silicon nanoparticle. Fig. 1 (d) is corresponding X-ray diffraction spectrum, is consistent completely with the standard X-ray diffraction card PDF#27-1402 of silicon, it was demonstrated that obtained is silicon, and carbon presents unformed shape, and X-ray diffraction cannot differentiate agraphitic carbon.
Fig. 2 (a) is the stereoscan photograph of graphite composite powder, it can be seen that the size of graphite granule is at about 10 ��m. Fig. 2 (b) is according to mass ratio Si/C: graphite is 1:5, bi-material is sufficiently mixed the stereoscan photograph after uniformly, it can be seen that nano level Si/C powder body sticks to the surface of graphite composite powder. Fig. 2 (c) is the X-ray diffraction spectrum of this material, it is seen then that it is by graphite and two kinds of phase compositions of silicon. Fig. 2 (d) is that this silico-carbo-graphite composite material is at 0.1mA/cm2Charge-discharge performance under current density condition, the specific capacity of its charged/discharged first is 611.6/554.3mAh/g, and circulation coulombic efficiency is up to 90.6% first. After 100 circulations, reversible charging capacity is 509.5mAh/g, thus capability retention is up to 91.9%.
Embodiment 2
By SiO2Nano-powder is mixed homogeneously according to mass ratio 1:1 with carbon source phenolic resin, then in 800 DEG C of constant temperature 4 hours under argon atmosphere, is finally cooled to room temperature, obtains the silicon dioxide SiO of carbon cladding2/ C. According to Mg:SiO2Mol ratio be that 2:1 weighs SiO respectively2/ C nano powder body and magnesium powder, and it is sufficiently mixed uniformly, react 5 hours in 650 DEG C under argon atmosphere. Naturally cool to after room temperature until it, put in dilution heat of sulfuric acid and stir, and with ethanol and deionized water filtration washing, obtain the nano Si/C of carbon cladding. Fig. 3 (a) is according to mass ratio Si/C: graphite is 1:2.5, bi-material is sufficiently mixed the stereoscan photograph after uniformly, it can be seen that nano level Si/C powder body sticks to the surface of graphite composite powder. Fig. 3 (b) is the X-ray diffraction spectrum of this material, it is seen then that it is by graphite and two kinds of phase compositions of silicon, and the ratio of the diffraction peak intensity of silicon and graphite diffraction peak intensity increases relative to Fig. 2 (c), it was demonstrated that in composite, the content of silicon improves. Fig. 3 (c) is that this silico-carbo-graphite composite material is at 0.1mA/cm2Charge-discharge performance under current density condition, the specific capacity of its charged/discharged first is 728.6/662.4mAh/g, and circulation coulombic efficiency is up to 90.9% first. After 100 circulations, reversible charging capacity is 601.3mAh/g, thus capability retention is up to 90.8%.
Embodiment 3
By SiO2Nano-powder is mixed homogeneously according to mass ratio 1:2.5 with carbon source starch, then in 900 DEG C of constant temperature 3 hours under nitrogen protection atmosphere, is finally cooled to room temperature, obtains the silicon dioxide SiO of carbon cladding2/ C. According to Mg:SiO2Mol ratio be that 2:1 weighs SiO respectively2/ C nano powder body and magnesium powder, and it is sufficiently mixed uniformly, react 3 hours in 700 DEG C under nitrogen protection atmosphere. Naturally cool to after room temperature until it, put in dilute nitric acid solution and stir, and with ethanol and deionized water filtration washing, obtain the nano Si/C of carbon cladding. Fig. 4 (a) is according to mass ratio Si/C: graphite is 1:1, bi-material is sufficiently mixed the stereoscan photograph after uniformly, it can be seen that nano level Si/C powder body sticks to the surface of graphite composite powder. Fig. 4 (b) is the X-ray diffraction spectrum of this material, visible, it is by graphite and two kinds of phase compositions of silicon, and the ratio of the diffraction peak intensity of silicon and graphite diffraction peak intensity increases relative to Fig. 3 (b), it was demonstrated that in composite, the content of silicon improves further. Fig. 4 (c) is that this silico-carbo-graphite composite material is at 0.1mA/cm2Charge-discharge performance under current density condition, the specific capacity of its charged/discharged first is 763.6/676.3mAh/g, and circulation coulombic efficiency is 88.6% first. After 100 circulations, reversible charging capacity is 501.6mAh/g, thus capability retention is 74.2%.
Embodiment 4
By SiO2Nano-powder is mixed homogeneously according to mass ratio 1:5 with carbon source Colophonium, then in 1000 DEG C of constant temperature 2 hours under nitrogen protection atmosphere, is finally cooled to room temperature, obtains the silicon dioxide SiO of carbon cladding2/ C. According to Mg:SiO2Mol ratio be that 2:1 weighs SiO respectively2/ C nano powder body and magnesium powder, and it is sufficiently mixed uniformly, react 2 hours in 800 DEG C under nitrogen protection atmosphere. Naturally cool to after room temperature until it, put in dilute hydrochloric acid solution and stir, and with ethanol and deionized water filtration washing, obtain the nano Si/C of carbon cladding. Fig. 5 (a) is according to mass ratio Si/C: graphite is 1:0.2, bi-material is sufficiently mixed the stereoscan photograph after uniformly, it can be seen that nano level Si/C powder body sticks to the surface of graphite composite powder. Fig. 5 (b) is the X-ray diffraction spectrum of this material, prove that composite is by graphite and two kinds of phase compositions of silicon, and the ratio of the diffraction peak intensity of silicon and graphite diffraction peak intensity increases relative to Fig. 4 (b), it was demonstrated that in composite, the content of silicon improves further. Fig. 5 (c) is that this silico-carbo-graphite composite material is at 0.1mA/cm2Charge-discharge performance under current density condition, the specific capacity of its charged/discharged first is 802.8/698.0mAh/g, and circulation coulombic efficiency is 86.9% first. After 100 circulations, reversible charging capacity is 476.2mAh/g, thus capability retention is 68.2%.
Claims (4)
1. the preparation method of silico-carbo-composite cathode material of silicon/carbon/graphite, it is characterised in that preparation process includes following series of steps: (1) selects Colophonium, phenolic resin or starch as carbon source respectively, first to nano silicon SiO2Powder body carries out carbon cladding, and its ratio is: 1:0.5��SiO2: carbon source mass ratio��1:5; By bi-material mix homogeneously, then in 700��1100 DEG C of constant temperature 1��5 hour under inert gas shielding, it is subsequently cooled to room temperature, obtains the silicon dioxide SiO of carbon cladding2/ C powder body; (2) silicon of carbon cladding is prepared using magnesium powder as reducing agent; According to mol ratio Mg:SiO2=2:1 weighs magnesium powder and SiO respectively2Then two kinds of powder body are sufficiently mixed uniformly by/C powder body, react 2��8 hours in 600��800 DEG C under inert protective atmosphere; Naturally cool to after room temperature until it, put in dilute acid soln and stir, and with ethanol and deionized water filtration washing, obtain the nano Si/C of carbon cladding; (3) being mixed homogeneously according to certain mass ratio with graphite powder by Si/C, its mass ratio is: 1:0.2��Si/C: graphite��1:5, obtains silico-carbo-composite cathode material of silicon/carbon/graphite.
2. the preparation method of a kind of silico-carbo-composite cathode material of silicon/carbon/graphite as claimed in claim 1, it is characterised in that: described silicon dioxide is nano-powder, and it is carried out carbon cladding.
3. the preparation method of a kind of silico-carbo-composite cathode material of silicon/carbon/graphite as claimed in claim 1, it is characterised in that: described inert atmosphere is argon or nitrogen.
4. the preparation method of a kind of silico-carbo-composite cathode material of silicon/carbon/graphite as claimed in claim 1, it is characterised in that: described olefin(e) acid is dilute hydrochloric acid, dust technology or dilute sulfuric acid.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106159229A (en) * | 2016-07-28 | 2016-11-23 | 深圳市贝特瑞新能源材料股份有限公司 | Silicon based composite material, preparation method and comprise the lithium ion battery of this composite |
| CN107492649A (en) * | 2017-08-25 | 2017-12-19 | 南陵县生产力促进中心 | A kind of silicon carbon material for cathode of lithium battery and preparation method thereof |
| CN107611417A (en) * | 2017-08-28 | 2018-01-19 | 上海大学 | Volume-controllable silicon substrate lithium ion battery negative material and preparation method thereof |
| CN108598381A (en) * | 2018-03-02 | 2018-09-28 | 合肥国轩高科动力能源有限公司 | A kind of carbon-coated nano silicon materials and its preparation method and application |
| CN109148871A (en) * | 2018-09-30 | 2019-01-04 | 东莞市三臻科技发展有限公司 | A kind of negative electrode material and lithium ion battery based on SiC |
| CN109216683A (en) * | 2018-09-20 | 2019-01-15 | 天津师范大学 | A kind of synthetic method of lithium ion battery high-capacity cathode material |
| CN109659514A (en) * | 2018-11-21 | 2019-04-19 | 郑州中科新兴产业技术研究院 | A kind of silicon-carbon cathode material and preparation method thereof based on mesocarbon microspheres |
| CN109755482A (en) * | 2017-11-01 | 2019-05-14 | 同济大学 | Silicon/carbon composite and preparation method thereof |
| CN109841814A (en) * | 2019-02-19 | 2019-06-04 | 深圳市斯诺实业发展有限公司 | A kind of preparation method of silicon-carbon cathode material |
| CN111193020A (en) * | 2020-01-17 | 2020-05-22 | 昆明理工大学 | Preparation method of silicon cathode composite material of lithium ion battery |
| CN111785969A (en) * | 2020-07-08 | 2020-10-16 | 吴耀帮 | Preparation method of porous nano Si-SiO2-C @ graphite composite lithium ion battery cathode powder and lithium ion battery |
| CN112768672A (en) * | 2021-02-05 | 2021-05-07 | 昆明理工大学 | Method for preparing graphite-based Si @ C negative electrode material by taking micro silicon powder as Si source |
| CN112897536A (en) * | 2021-03-02 | 2021-06-04 | 南京邮电大学 | Carbon-coated hollow silicon dioxide composite material and preparation method thereof |
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| CN106159229A (en) * | 2016-07-28 | 2016-11-23 | 深圳市贝特瑞新能源材料股份有限公司 | Silicon based composite material, preparation method and comprise the lithium ion battery of this composite |
| CN107492649A (en) * | 2017-08-25 | 2017-12-19 | 南陵县生产力促进中心 | A kind of silicon carbon material for cathode of lithium battery and preparation method thereof |
| CN107611417A (en) * | 2017-08-28 | 2018-01-19 | 上海大学 | Volume-controllable silicon substrate lithium ion battery negative material and preparation method thereof |
| CN107611417B (en) * | 2017-08-28 | 2020-11-24 | 上海大学 | Capacity-controllable silicon-based lithium ion battery cathode material and preparation method thereof |
| CN109755482B (en) * | 2017-11-01 | 2021-08-10 | 同济大学 | Silicon/carbon composite material and preparation method thereof |
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| CN109841814A (en) * | 2019-02-19 | 2019-06-04 | 深圳市斯诺实业发展有限公司 | A kind of preparation method of silicon-carbon cathode material |
| CN111193020A (en) * | 2020-01-17 | 2020-05-22 | 昆明理工大学 | Preparation method of silicon cathode composite material of lithium ion battery |
| CN111785969A (en) * | 2020-07-08 | 2020-10-16 | 吴耀帮 | Preparation method of porous nano Si-SiO2-C @ graphite composite lithium ion battery cathode powder and lithium ion battery |
| CN112768672A (en) * | 2021-02-05 | 2021-05-07 | 昆明理工大学 | Method for preparing graphite-based Si @ C negative electrode material by taking micro silicon powder as Si source |
| CN112897536A (en) * | 2021-03-02 | 2021-06-04 | 南京邮电大学 | Carbon-coated hollow silicon dioxide composite material and preparation method thereof |
| CN113479890A (en) * | 2021-06-30 | 2021-10-08 | 松山湖材料实验室 | Silicon-based negative electrode material and preparation method and application thereof |
| CN113479890B (en) * | 2021-06-30 | 2022-12-27 | 松山湖材料实验室 | Silicon-based negative electrode material and preparation method and application thereof |
| CN113942991A (en) * | 2021-09-13 | 2022-01-18 | 惠州市贝特瑞新材料科技有限公司 | Silicon carbon-graphite composite negative electrode material and preparation method thereof |
| CN115425212A (en) * | 2022-09-29 | 2022-12-02 | 安徽科达新材料有限公司 | Method for preparing high-first-efficiency silicon monoxide through low-temperature reduction and application thereof |
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