CN102214817A - Carbon/silicon/carbon nano composite structure cathode material and preparation method thereof - Google Patents
Carbon/silicon/carbon nano composite structure cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a carbon/silicon/carbon nano composite structure cathode material and a preparation method thereof, belonging to the technical field of electrochemical power supply technologies. The cathode material consists of a carbon-based conductive substrate, nano silicon and a nano carbon coating layer, wherein the nano silicon is uniformly distributed on the carbon-based conductive substrate; the nano carbon coating layer is arranged on the surface of the nano silicon; the carbon-based conductive substrate is porous carbon, a carbon nanotube or graphene; the nano silicon exists in the state of nanoparticles or nano films; the weight percentage of the nano silicon in the cathode material is 10-90 percent; and the thickness of the nano carbon coating layer is 0.1-10 nanometers. The preparation method comprises the following steps of: depositing nano silicon on the carbon substrate in a reaction space in oxygen-free atmosphere by adopting a chemical vapor deposition process; and coating nano carbon on the surface of the nano silicon by adopting the chemical vapor deposition process. In the obtained carbon/silicon/carbon composite cathode material, the volume change of a silicon electrode material is controlled effectively in the charging and discharging processes, the electrode structure is kept complete, the circulation volume is large, the circulation service life is long, and the electrochemical performance is high.
Description
Technical field
The invention belongs to the electrochemical power source technical field, particularly a kind of carbon/silicon/carbon nano composite structure negative material and preparation method thereof.
Background technology
Lithium ion battery is as the green high-capacity battery, it is the ideal source of portable electric appts and electric automobile, exploration specific energy height, fail safe new material good and cheap and easy to get are the core contents in present Study on Li-ion batteries using field, and the research of novel negative material is significant to the development of lithium ion battery of new generation.
Silicon has high theoretical specific capacity (4200mAh/g), lower storage lithium response voltage platform (0.1V vs.Li/Li
+), and silicon is very wide in the distribution of occurring in nature, and the content in the earth's crust is only second to oxygen, so silicium cathode is the novel high-energy negative pole that a class has development prospect.But the electronic conductivity and the lithium ion conductivity of silicon are lower, cause the dynamic performance of its electrochemical reaction relatively poor.And phase transformation and volumetric expansion (400%) the meeting generation bigger stress of silicon in the lithiumation process, cause lead rupture efflorescence, resistance increase, cycle performance rapid drawdown.Nearest discovers that the compatibility of silicon and electrolyte is relatively poor, and the surface functional group of silicon and the reaction of electrolyte can cause the silicium cathode surface to be difficult to form stable, thin and fine and close solid electrolyte film, cause the electrode cycle performance to descend gradually.
Research to silicium cathode mainly is silica flour and carbon source material to be carried out ball milling mix the back pyrolysis at present, with preparation silico-carbo composite material.Because ball-milling method is difficult to effectively regulate and control particle diameter, pattern, the orientation of silicon nanoparticle, and be difficult to realize single, the even dispersion of silicon nanoparticle in carbon carrier, so the silico-carbo composite material cycle performance of Prepared by Ball Milling is relatively poor.Recently, people are by preparation silicon nanowires (Candace K.Chan, HailinPeng, Gao Liu, Yi Cui.Nat.Nanotechnol., 2008,3 (1): 31-35; Li-Feng Cui, Riccardo Ruffo, Candace K.Chan, Yi Cui.Nano Letters, 2009,9 (1): 491-495), nano-tube (Mi-Hee Park, M in Gyu Kim, Jaeb um Joo.Nano Letters, 2009,9 (11): 3844-3847), three-dimensional porous silicon grain (Hyunjung Kim, Byunghee Han, Jaebum Choo, Jaephil Cho.Angew.Chem.Int.Ed.2008,47 (52), 10151-10154), significantly improved the cyclical stability of silicon materials.Reason is all to exist a large amount of spaces in these structures, can hold the volumetric expansion in the silicon storage lithium process, thereby eliminate the stress that produces in the lithium insertion process.But owing to do not contain the carrier of high conductivity in these materials, and silicon often directly contacts with electrolyte, so material polarizes greatlyyer under the high current charge-discharge condition, and the cyclical stability under the high magnification is relatively poor, has limited its practical application.
Summary of the invention
The objective of the invention is to weak point, silica-based composite negative pole material of lithium ion battery that provide a kind of specific capacity height, have extended cycle life, the kinetics performance is good and preparation method thereof at existing silica-based negative material of lithium ion battery and preparation method thereof.
A kind of carbon/silicon/carbon nano composite structure negative material that the present invention proposes is characterized in that: this negative material by the carbon back conducting base, be evenly distributed on nano-silicon on the carbon back conducting base and the nano-sized carbon coating layer on nano-silicon surface is formed.
Described carbon back conducting base is at least a in porous carbon, carbon nano-tube, the Graphene.
Nano-silicon exists with the state of nano particle or nano thin-film in the described negative material.
The thickness of the nano-sized carbon coating layer on described nano-silicon surface is 0.1～10nm.
The percentage by weight of described nano-silicon in negative material is 10～90%.
The preparation method of a kind of carbon/silicon/carbon nano composite structure negative material that the present invention proposes, it is characterized in that: in the reaction compartment of no oxygen atmosphere, adopt chemical vapor deposition method depositing nano silicon on carbon base body, again by chemical vapor deposition method at nano-silicon surface coating nano carbon, comprise the steps:
(1) with the gaseous silane being the silicon source, is carrier gas with inert gas or hydrogen, reacts in chemical vapor deposition stove, and constant temperature is 10 minutes～100 hours under 500～1200 ℃ of temperature, nano-silicon is deposited to the surface and the interior void of carbon back conducting base;
(2) with the hydrocarbon being carbon source, is carrier gas with inert gas or hydrogen, reacts in chemical vapor deposition stove, and constant temperature is 10 minutes～100 hours under 500～1200 ℃ of temperature, nano-sized carbon is deposited on the surface of nano-silicon.
Described gaseous silane is selected from SiH
4, Si
2H
6, ClSiH
3, Cl
2SiH
2, Cl
3SiH, SiCl
4, Si
2Cl
6In at least a.
Described hydrocarbon is selected from aliphatic hydrocarbon or aromatic hydrocarbon.Wherein, aliphatic hydrocarbon preferably contains the saturated or unsaturated hydrocarbons of short chain of no more than 4 carbon atoms usually, comprises ethene, acetylene, propylene, ethane, propane, and ethene and acetylene are most preferred; Aromatic hydrocarbon preferably contains the aromatic hydrocarbon of 6-20 carbon atom, as benzene, naphthalene or alkyl-substituted derivatives such as toluene, dimethylbenzene, isopropyl alcohol benzene or ethylbenzene.
Described chemical vapor deposition stove is horizontal type stove or shaft (tower) furnace.
Described inert gas is nitrogen or argon gas.
Use said method can obtain " carbon/silicon/carbon " of the present invention nano composite material, it be at carbon back conductive carrier particle surface and inner hole loaded with nano silicon grain or Nano thin film, and at the composite material of receiving of the surperficial clad nano carbon-coating of silicon materials.This " carbon/silicon/carbon " nano composite material, utilized the high conductivity of carbon-based supports material on the one hand, make it can remedy the problem of silicon materials poorly conductive, on the other hand because the silicon nanometer shortens electronics, ion transport path greatly, increase the electrochemical reaction interface, thereby improve the electrochemical reaction dynamic performance of material, and the superplastic ability of nano material discharges the stress that the lithiumation process produces preferably, thereby improve the cycle performance of electrode; At last at nano-silicon coated with uniform nanometer carbon-coating, can improve the surface chemical structure of nano-silicon, reducing it contacts with the direct of electrolyte, promotion forms stable, thin and fine and close solid electrolyte film at electrode surface, improve the electrode/electrolyte interface compatibility, thereby improve the cycle performance of electrode.
Preparation method provided by the invention is also advantageous in that: depositing nano silicon that can be controlled on carbon-based supports and nano-sized carbon coating layer, the temperature and time of the weight percent of nano-silicon kind, flow, different carrier gas components in proportions and reaction that when the thickness of nano-sized carbon coating layer all can be by the source of the gas that adopts of control chemical vapour deposition (CVD) is regulated and control in the composite material.And technology provided by the invention is simple, and good reproducibility, required instrument and equipment all are chemistry and material industry equipment commonly used.The product purity height that the present invention prepares, geometry is controlled, and material is stable." carbon/silicon/carbon " provided by the invention nano composite material can be used as the negative material of lithium ion battery.
Embodiment
Can further understand the present invention from following examples, but the present invention not only is confined to following examples:
Embodiment 1
The porous carbon particle that takes by weighing 1g is placed in the quartz boat, the horizontal type of packing into tube furnace, and quartz boat is placed on the middle part of tube furnace, (9/1, v/v), total flow is 100sccm to feed the mixed air of argon gas and hydrogen then, after the temperature programming to 1000 ℃, begin to feed SiCl
4, flow is 20sccm, and vacuumizes at an end of gas outlet, constant temperature naturally cooled to room temperature after 60 minutes.In tube furnace, feed argon gas again, flow is 20sccm, and temperature programming to 950 ℃ is converted to gas the mixed air of benzene and argon gas, its ratio is 1/20 (v/v), total flow is 300sccm, and constant temperature was converted to argon gas with gas after 20 minutes, naturally cool to room temperature, products therefrom is nano-sized carbon/nano-silicon/porous carbon composite material, and wherein the percentage by weight of silicon in composite material is 40%, and the thickness of nano-sized carbon coating layer is 5nm.
Embodiment 2
The multi-wall carbon nano-tube tube particle that takes by weighing 1g is packed in the vertical tube furnace, and (95/5, v/v), total flow is 200sccm, makes the multi-walled carbon nano-tubes particle fluidization in the stove to feed the mixed air of argon gas and hydrogen.After the temperature programming to 900 ℃, begin to feed SiH
4, flow is 40sccm, and vacuumizes at an end of gas outlet, constant temperature naturally cooled to room temperature after 60 minutes.In tube furnace, feed argon gas again, flow is 200sccm, makes the fluidization of stove endoparticle, temperature programming to 1000 ℃, gas is converted to acetylene, flow is 100sccm, and constant temperature was converted to argon gas with gas after 10 minutes, naturally cool to room temperature, products therefrom is nano-sized carbon/nano-silicon/multi-wall carbon nano-tube composite material, and wherein the percentage by weight of silicon in composite material is 60%, and the thickness of nano-sized carbon coating layer is 3nm.
Embodiment 3
The Graphene particle that takes by weighing 1g is placed in the quartz boat, the horizontal type of packing into tube furnace, and quartz boat is placed on the middle part of tube furnace, (9/1, v/v), total flow is 150sccm to feed the mixed air of argon gas and hydrogen then, after the temperature programming to 900 ℃, begin to feed HSiCl
3, flow is 50sccm, and vacuumizes at an end of gas outlet, constant temperature 2 hours naturally cools to room temperature.In tube furnace, feed argon gas again, flow is 20sccm, and temperature programming to 950 ℃ is converted to gas the mixed air of benzene and argon gas, its ratio is 1/10 (v/v), total flow is 300sccm, and constant temperature was converted to argon gas with gas after 20 minutes, naturally cool to room temperature, products therefrom is nano-sized carbon/nano-silicon/graphene composite material, and wherein the percentage by weight of silicon in composite material is 80%, and the thickness of nano-sized carbon coating layer is 4nm.
Embodiment 4
The Graphene particle that takes by weighing 1g is packed in the vertical tube furnace, and (95/5, v/v), total flow is 200sccm, makes the Graphene particle fluidization in the stove to feed the mixed air of argon gas and hydrogen.After the temperature programming to 1000 ℃, begin to feed SiCl
4, flow is 40sccm, and vacuumizes at an end of gas outlet, constant temperature naturally cooled to room temperature after 60 minutes.Feed argon gas again in tube furnace, flow is 200sccm, makes the fluidization of stove endoparticle, temperature programming to 1000 ℃, gas is converted to the mixed air of benzene and argon gas, and its ratio is 1/10 (v/v), and total flow is 300sccm, behind the constant temperature 20 minutes, gas is converted to argon gas, naturally cools to room temperature, products therefrom is nano-sized carbon/nano-silicon/graphene composite material, wherein the percentage by weight of silicon in composite material is 50%, and the thickness of nano-sized carbon coating layer is 1nm.
Embodiment 5
The composite material of gained among the embodiment 1 negative material as lithium ion battery is used.The preparation method of electrode is described below: nano-sized carbon/nano-silicon/porous carbon composite material, carbon black mixes the formation slurry at normal temperatures and pressures with the N-methyl pyrrolidone solution of Kynoar, evenly be coated on the Copper Foil as collector, the percentage by weight of composite material, carbon black and Kynoar is 80: 10: 10, with the film of gained behind 120 ℃ of following vacuum dryings, at 20Kg/cm
2Pressure under compress, then film is reduced for area be 1cm
2Thin rounded flakes as electrode.Do electrode with lithium metal, electrolyte is 1mol LiPF
6Be dissolved in the mixed solvent of 1L EC and EMC (volume ratio 3: 7), barrier film is a microporous polypropylene membrane, is assembled into Experimental cell in being full of the glove box of argon gas.
Experimental cell is tested by being subjected to computer-controlled auto charge and discharge instrument to carry out charge and discharge cycles, and discharge cut-off voltage is 0.005V, and the charging cut-ff voltage is 2.0V.Described nano-sized carbon/nano-silicon/porous carbon composite material is 1200mAh/g at the reversible capacity of 0.1C, and 50 times circulation back capacity still surpass 1000mAh/g.
Embodiment 6
The composite material of gained among the embodiment 2 negative material as lithium ion battery is used.The preparation process of electrode is with embodiment 5.Described nano-sized carbon/nano-silicon/multi-wall carbon nano-tube composite material is 1800mAh/g at the reversible capacity of 0.1C, and 50 times circulation back capacity still surpass 1700mAh/g.
Embodiment 7
The composite material of gained among the embodiment 3 negative material as lithium ion battery is used.The preparation process of electrode is with embodiment 5.Described nano-sized carbon/nano-silicon/graphene composite material is 2200mAh/g at the reversible capacity of 0.1C, and 50 times circulation back capacity still surpass 2000mAh/g.
Embodiment 8
The composite material of gained among the embodiment 4 negative material as lithium ion battery is used.The preparation process of electrode is with embodiment 5.Described nano-sized carbon/nano-silicon/graphene composite material is 1500mAh/g at the reversible capacity of 0.1C, and 50 times circulation back capacity still surpass 1400mAh/g.
Claims (10)
1. carbon/silicon/carbon nano composite structure negative material is characterized in that: this negative material by the carbon back conducting base, be evenly distributed on nano-silicon on the carbon back conducting base and the nano-sized carbon coating layer on nano-silicon surface is formed.
2. a kind of carbon/silicon according to claim 1/carbon nano composite structure negative material is characterized in that: described carbon back conducting base is at least a in porous carbon, carbon nano-tube, the Graphene.
3. a kind of carbon/silicon according to claim 1/carbon nano composite structure negative material, it is characterized in that: nano-silicon exists with the state of nano particle or nano thin-film in the described negative material.
4. a kind of carbon/silicon according to claim 1/carbon nano composite structure negative material is characterized in that: the thickness of the nano-sized carbon coating layer on described nano-silicon surface is 0.1～10nm.
5. a kind of carbon/silicon according to claim 1/carbon nano composite structure negative material is characterized in that: the percentage by weight of described nano-silicon in negative material is 10～90%.
6. the preparation method of carbon/silicon/carbon nano composite structure negative material is characterized in that: comprise the steps:
(1) with the gaseous silane being the silicon source, is carrier gas with inert gas or hydrogen, reacts in chemical vapor deposition stove, and constant temperature is 10 minutes～100 hours under 500～1200 ℃ of temperature, nano-silicon is deposited to the surface and the interior void of carbon back conducting base;
(2) with the hydrocarbon being carbon source, is carrier gas with inert gas or hydrogen, reacts in chemical vapor deposition stove, and constant temperature is 10 minutes～100 hours under 500～1200 ℃ of temperature, nano-sized carbon is deposited on the surface of nano-silicon.
7. the preparation method of a kind of carbon/silicon according to claim 6/carbon nano composite structure negative material, it is characterized in that: described gaseous silane is selected from SiH
4, Si
2H
6, ClSiH
3, Cl
2SiH
2, Cl
3SiH, SiCl
4, Si
2Cl
6In at least a.
8. the preparation method of a kind of carbon/silicon according to claim 6/carbon nano composite structure negative material, it is characterized in that: described hydrocarbon is selected from aliphatic hydrocarbon or aromatic hydrocarbon.
9. the preparation method of a kind of carbon/silicon according to claim 8/carbon nano composite structure negative material, it is characterized in that: described aliphatic hydrocarbon is selected from the saturated or unsaturated hydrocarbons of the short chain that contains no more than 4 carbon atoms, and described aromatic hydrocarbon is selected from the aromatic hydrocarbon that contains 6-20 carbon atom.
10. the preparation method of a kind of carbon/silicon according to claim 6/carbon nano composite structure negative material is characterized in that: described chemical vapor deposition stove is horizontal type stove or shaft (tower) furnace.
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