CN106119967A - Continuous two steps prepare the method for monocrystalline silicon carbide/Graphene composite nano fiber - Google Patents
Continuous two steps prepare the method for monocrystalline silicon carbide/Graphene composite nano fiber Download PDFInfo
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- CN106119967A CN106119967A CN201610447943.8A CN201610447943A CN106119967A CN 106119967 A CN106119967 A CN 106119967A CN 201610447943 A CN201610447943 A CN 201610447943A CN 106119967 A CN106119967 A CN 106119967A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
Abstract
The invention discloses a kind of method that continuous two steps prepare monocrystalline silicon carbide/Graphene composite nano fiber.The step of the method is as follows: be to prepare carbon containing gel by sol-gal process, by pyrocarbon thermal reduction synthetizing silicon carbide nano fiber in high temperature；At high temperature heat, the desiliconization of silicon carbide fibre surface, prepare monocrystalline silicon carbide/Graphene composite nano fiber.The method utilizes the high-specific surface area carborundum nanofiber prepared, and prepares the monocrystalline silicon carbide/Graphene composite nano fiber of same high-specific surface area.The performance of excellent properties and carborundum semiconductor material with wide forbidden band that monocrystalline silicon carbide/Graphene composite nano fiber combines Graphene is also demonstrated by the performance of nanofiber one-dimensional nano structure material, has that preparation technology is simple, product is pollution-free, product purity advantages of higher.The present invention is with a wide range of applications in fields such as nano photoelectronic devices, flexible electronic, lithium ion battery electrode material, energy storage and nano composite materials.
Description
Technical field
The present invention relates to the preparation method of Graphene, especially relate to a kind of two-step method continuously and prepare monocrystalline silicon carbide/stone
Ink alkene composite nano fiber.
Background technology
Graphene (Graphene) be a kind of by carbon atom withsp 2 Mode hydridization composition hexangle type is the plane of honeycomb lattice
Thin film, it is steady that Novoselov of Manchester university in 2004 et al. uses Scotch adhesive tape to be obtained by micromechanics stripping method
Fixed, self-existent single-layer graphene, first is found that real two dimensional crystal, finds to attract the scientific research of each field the most always
Worker puts into wherein, starts the research climax of Graphene.
In Graphene, each carbon atom has four valency electron, each of which carbon atom with three covalent bonds with another
Outer three atoms are connected to form three σ keys, and six carbon atom defines orthohexagonal ring in approximately the same plane and stretches formation
Lamellar two-dimension plane structure, each on the direction be perpendicular to graphite linings still remaining one2pTrack and a valency electron
The big π key through whole graphite linings is formed with neighbour's atomic interaction.Covalent bond between carbon atom, bond distance belongs to atomic bond
Long scope, belongs to atomic crystal, thus Graphene has big elastic modelling quantity and intensity.Columbia University Changgu Lee
Et al. find that the elastic modelling quantity of Graphene and tensile strength are respectively 1.1 TPa and 125 GPa；The most each surplus one of carbon atomPRail
Road, and overlapped, form a big π key, unusual electronic structure makes it have the electrical properties of uniqueness, and electronics is at stone
Fermi velocity in ink alkene is 106 The 1/300 of m/s, the about light velocity, and do not rely on energy or momentum, Graphene also uniqueness
Optical characteristics and the thermal property of high heat conductance.
From the discovery of Graphene so far, researchers have developed many methods preparing Graphene, such as: machinery stripping
From method, CVD growth method, silicon carbide epitaxial growth method, chemical method etc..Wherein silicon carbide epitaxial growth method is in silicon carbide substrates
Upper growth Graphene, maximum advantage be by relatively simple method can prepare large-area graphene (in principle size by
Substrate size determines).Make monocrystalline silicon carbide (0001) emaciated face remove silicon by high-temperature heating, thus obtain the stone of its surface extension
Ink alkene.
It is saturated that manufacturing silicon carbide semiconductor material has indirect broad stopband, big breakdown electric field, high thermal conductivity and high electronics
The features such as drift velocity.Monocrystalline silicon carbide/Graphene composite nano fiber combines excellent properties and the carborundum half of Graphene
The performance of conductor material is also demonstrated by the excellent properties of nanofiber one-dimensional nano structure material, and monocrystalline silicon carbide/Graphene is multiple
The preparation process technique of conjunction nanofiber is simple, product is pollution-free, product purity advantages of higher.SiC nano fiber/graphite
Alkene composite nano fiber is at nano photoelectronic devices, flexible electronic, lithium ion battery electrode material, energy storage and nano combined
The fields such as material are with a wide range of applications.
At present, if both at home and abroad independent of the relevant report of preparation of SiC nano fiber/Graphene composite nano fiber.
Summary of the invention
It is an object of the invention to provide the method that continuous two steps prepare monocrystalline silicon carbide/ink alkene composite nano fiber, even
Continuous two-step method prepares monocrystalline silicon carbide/Graphene composite nano fiber, first first step pyrocarbon thermal reduction synthesizing silicon carbide
Nanofiber；Second step uses silicon sublimed method to make silicon carbide desiliconization by high-temperature heating, it is thus achieved that monocrystalline silicon carbide/Graphene
Composite nano fiber.
The step of the technical solution used in the present invention is as follows:
Step 1) prepared by pyrocarbon thermal reduction synthetizing silicon carbide nano fiber: it is to prepare carbon containing by sol-gel process to coagulate
Glue, after drying, grinds to form the dry gel powder of carbon containing, and described dry gel powder is placed in bottom corundum crucible, puts into high temperature process furnances,
Evacuation is filled with protective gas；Heat temperature raising, heat preservation sintering is cooled to room temperature, and blow-on covers with green silicon carbide in finding crucible
Nanofiber, through characterizing the SiC nano fiber that this product is zincblende lattce structure cube；
Step 2) use silicon sublimed method make the desiliconization of SiC nano fiber surface by high-temperature heating: be by step 1) in carbon
SiClx nanofiber heat temperature raising again, is incubated under hot environment, continues evacuation, at Gao Zhen with high reliability vacuum pump simultaneously
Under reciprocal of duty cycle, hot environment, SiC nano fiber surface removing silicon, prepare monocrystalline silicon carbide/Graphene composite nano fiber.
Described sol-gel process prepares the step of carbon containing gel: be dissolved in dehydrated alcohol by tetraethyl orthosilicate, adds
Oxalic acid is to accelerate teos hydrolysis, and oxalic acid is diluted to 0.01 mol/L, tetraethyl orthosilicate, dehydrated alcohol, water and oxalic acid
Mol ratio is 1:0.86:4:7.2 × 10-4, it is subsequently adding expansible graphite, magnetic agitation preparation carbon containing gel；Wherein positive silicic acid
Ethyl ester and expansible graphite ratio, it is ensured that carbon is 1:1 with the mol ratio of silicon, become gel to be dried in being placed on baking oven.
Described step 1) in heat temperature raising be 1500 DEG C, heat preservation sintering 2 ~ 6 h.
Described step 2) again heat temperature raising be 1200 ~ 1500 DEG C, under hot environment, temperature retention time is 0.5 ~ 2 h, very
Reciprocal of duty cycle is maintained at 1 P ~ 1 × 10-2 MP。
The present invention is compared with background technology, and have has the advantages that:
SiC nano fiber/Graphene composite nano fiber compared with the Graphene of bulk single crystal silicon carbide epitaxial growth method, by
In prepared SiC nano fiber, there is high-specific surface area, same with the Graphene that SiC nano fiber goes out for substrate epitaxial
Having high-specific surface area, monocrystalline silicon carbide/Graphene composite nano fiber combines excellent properties and the carborundum half of Graphene
The performance of conductor material is also demonstrated by the excellent properties of nanofiber one-dimensional nano structure material, simultaneously monocrystalline silicon carbide/graphite
The preparation process technique of alkene composite nano fiber is simple, product is pollution-free, product purity advantages of higher.SiC nano fiber/
Graphene composite nano fiber is in nano photoelectronic devices, flexible electronic, lithium ion battery electrode material, energy storage and nanometer
The fields such as composite are with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the Raman collection of illustrative plates of the product monocrystalline silicon carbide/Graphene composite nano fiber of the embodiment of the present invention 6.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
The method step that a kind of continuous two steps of the present embodiment prepare monocrystalline silicon carbide/Graphene composite nano fiber is as follows:
Tetraethyl orthosilicate is dissolved in dehydrated alcohol by step a., and addition oxalic acid is to accelerate teos hydrolysis, and oxalic acid dilutes
To 0.01 mol/L, the mol ratio of tetraethyl orthosilicate, dehydrated alcohol, water and oxalic acid is 1:0.86:4:7.2 × 10-4, it is subsequently adding
Expansible graphite, magnetic agitation preparation carbon containing gel；Wherein tetraethyl orthosilicate and expansible graphite ratio, it is ensured that carbon rubs with silicon
Your ratio is 1:1, becomes gel to be dried in being placed on baking oven；
After step b. carbon containing gel drying, the dry gel powder grinding to form powdery is placed in bottom corundum crucible, and puts into high-temperature tubular
In stove, evacuation is also filled with protective gas argon, heat temperature raising 1500 DEG C, and heat preservation sintering 2 h is cooled to room temperature, and blow-on obtains
SiC nano fiber to zincblende lattce structure cube；
The SiC nano fiber that step c. prepares is heated to 1200 DEG C the most again, is incubated, uses simultaneously under hot environment
High reliability vacuum pump continues evacuation 2 h, and vacuum is maintained at 1 × 10-2 MP, under condition of high vacuum degree, hot environment, carbonization
Silica fibre surface removing silicon.
Embodiment 2:
Step a is identical with embodiment 1 step a；
After step b. carbon containing gel drying, the dry gel powder grinding to form powdery is placed in bottom corundum crucible, and puts into high-temperature tubular
In stove, evacuation is also filled with protective gas argon, heat temperature raising 1500 DEG C, and heat preservation sintering 4h is cooled to room temperature, and blow-on obtains
The SiC nano fiber of zincblende lattce structure cube；
The SiC nano fiber that step c. prepares is heated to 1400 DEG C the most again, is incubated, uses simultaneously under hot environment
High reliability vacuum pump continues evacuation 1 h, and vacuum is maintained at 1 × 10-3 MP, under condition of high vacuum degree, hot environment, carbonization
Silica fibre surface removing silicon.
Embodiment 3:
Step a is identical with embodiment 1 step a；
After step b. carbon containing gel drying, the dry gel powder grinding to form powdery is placed in bottom corundum crucible, and puts into high-temperature tubular
In stove, evacuation is also filled with protective gas argon, heat temperature raising 1500 DEG C, and heat preservation sintering 4 h is cooled to room temperature, and blow-on obtains
SiC nano fiber to zincblende lattce structure cube；
The SiC nano fiber that step c. prepares is heated to 1400 DEG C the most again, is incubated, uses simultaneously under hot environment
High reliability vacuum pump continues evacuation 0.5 h, and vacuum is maintained at 1 P, and under condition of high vacuum degree, hot environment, carborundum is fine
Dimension table emaciated face removes silicon.
Embodiment 4:
Step a is identical with embodiment 1 step a；
After step b. carbon containing gel drying, the dry gel powder grinding to form powdery is placed in bottom corundum crucible, and puts into high-temperature tubular
In stove, evacuation is also filled with protective gas argon, heat temperature raising 1500 DEG C, and heat preservation sintering 4 h is cooled to room temperature, and blow-on obtains
SiC nano fiber to zincblende lattce structure cube；
The SiC nano fiber that step c. prepares is heated to 1500 DEG C the most again, is incubated, uses simultaneously under hot environment
High reliability vacuum pump continues evacuation 1h, and vacuum is maintained at 1 × 10-2 MP, under condition of high vacuum degree, hot environment, carborundum
Fiber surface removing silicon.
Embodiment 5:
Step a is identical with embodiment 1 step a；
After step b. carbon containing gel drying, the dry gel powder grinding to form powdery is placed in bottom corundum crucible, and puts into high-temperature tubular
In stove, evacuation is also filled with protective gas argon, heat temperature raising 1500 DEG C, and heat preservation sintering 4h is cooled to room temperature, and blow-on obtains
The SiC nano fiber of zincblende lattce structure cube；
The SiC nano fiber that step c. prepares is heated to 1500 DEG C the most again, is incubated, uses simultaneously under hot environment
High reliability vacuum pump continues evacuation 0.5 h, and vacuum is maintained at 1 × 10-3 MP, under condition of high vacuum degree, hot environment, carbon
SiClx fiber surface removing silicon.
Embodiment 6:
Step a is identical with embodiment 1 step a；
After step b. carbon containing gel drying, the dry gel powder grinding to form powdery is placed in bottom corundum crucible, and puts into high-temperature tubular
In stove, evacuation is also filled with protective gas argon, heat temperature raising 1500 DEG C, and heat preservation sintering 4h is cooled to room temperature, and blow-on obtains
The SiC nano fiber of zincblende lattce structure cube；
The SiC nano fiber that step c. prepares is heated to 1500 DEG C the most again, is incubated, uses simultaneously under hot environment
High reliability vacuum pump continues evacuation 0.5 h, and vacuum is maintained at 1 P, and under condition of high vacuum degree, hot environment, carborundum is fine
Dimension table emaciated face removes silicon.Fig. 1 is the Raman collection of illustrative plates of the product monocrystalline silicon carbide/Graphene composite nano fiber of the present embodiment, from Fig. 1
In it can be seen that in 1349cm-1、1579 cm-1、2699 cm-1There is the characteristic peak of Graphene in place.
Embodiment 7:
Step a is identical with embodiment 1 step；
After step b. carbon containing gel drying, the dry gel powder grinding to form powdery is placed in bottom corundum crucible, and puts into high-temperature tubular
In stove, evacuation is also filled with protective gas argon, heat temperature raising 1500 DEG C, and heat preservation sintering 6h is cooled to room temperature, and blow-on obtains
The SiC nano fiber of zincblende lattce structure cube；
The SiC nano fiber that step c. prepares is heated to 1500 DEG C the most again, is incubated, uses simultaneously under hot environment
High reliability vacuum pump continues evacuation 0.5 h, and vacuum is maintained at 1 P, and under condition of high vacuum degree, hot environment, carborundum is fine
Dimension table emaciated face removes silicon.
Claims (4)
- The most continuous two steps prepare the method for monocrystalline silicon carbide/Graphene composite nano fiber, it is characterised in that:Step 1) prepared by pyrocarbon thermal reduction synthetizing silicon carbide nano fiber: it is to prepare carbon containing by sol-gel process to coagulate Glue, after drying, grinds to form the dry gel powder of carbon containing, and described dry gel powder is placed in bottom corundum crucible, puts into high temperature process furnances, Evacuation is filled with protective gas；Heat temperature raising, heat preservation sintering is cooled to room temperature, and blow-on covers with green silicon carbide in finding crucible Nanofiber, through characterizing the SiC nano fiber that this product is zincblende lattce structure cube；Step 2) use silicon sublimed method make the desiliconization of SiC nano fiber surface by high-temperature heating: be by step 1) in carbon SiClx nanofiber heat temperature raising again, is incubated under hot environment, continues evacuation, at Gao Zhen with high reliability vacuum pump simultaneously Under reciprocal of duty cycle, hot environment, SiC nano fiber surface removing silicon, prepare monocrystalline silicon carbide/Graphene composite nano fiber.
- The method that continuous two steps the most according to claim 1 prepare monocrystalline silicon carbide/Graphene composite nano fiber, it is special Levy and be: described sol-gel process is prepared the step of carbon containing gel and is: be dissolved in dehydrated alcohol by tetraethyl orthosilicate, add Oxalic acid is to accelerate teos hydrolysis, and oxalic acid is diluted to 0.01 mol/L, tetraethyl orthosilicate, dehydrated alcohol, water and oxalic acid Mol ratio is 1:0.86:4:7.2 × 10-4, it is subsequently adding expansible graphite, magnetic agitation preparation carbon containing gel；Wherein positive silicic acid Ethyl ester and expansible graphite ratio, it is ensured that carbon is 1:1 with the mol ratio of silicon, become gel to be dried in being placed on baking oven.
- The method that continuous two steps the most according to claim 1 prepare monocrystalline silicon carbide/Graphene composite nano fiber, it is special Levy and be: described step 1) in heat temperature raising be 1500 DEG C, heat preservation sintering 2 ~ 6 h.
- The method that continuous two steps the most according to claim 1 prepare monocrystalline silicon carbide/Graphene composite nano fiber, it is special Levy and be: described step 2) again heat temperature raising be 1200 ~ 1500 DEG C, under hot environment, temperature retention time is 0.5 ~ 2 h, very Reciprocal of duty cycle is maintained at 1 P ~ 1 × 10-2 MP。
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| CN110028070A (en) * | 2019-05-09 | 2019-07-19 | 清芯未来(北京)科技有限公司 | Monocrystalline silicon carbide/graphene nuclear shell structure nano fiber and its preparation method and application |
| CN111943713A (en) * | 2020-08-19 | 2020-11-17 | 龚俊琼 | Environment-friendly heat-preservation and heat-insulation material and preparation method thereof |
| CN111943703A (en) * | 2020-08-10 | 2020-11-17 | 西北工业大学 | Method for preparing silicon carbide fiber reinforced graphite preform through silicon aerogel |
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Application publication date: 20161116 |