CN102600775A - SiC-graphene nano-composite and preparation method thereof - Google Patents
SiC-graphene nano-composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a SiC-graphene nano-composite and a preparation method thereof. The SiC-graphene nano-composite has a core-shell structure with the core covered with the shell, wherein the core is made of SiC nano particles, and the shell is made of nano graphite composed of the graphene. The preparation method includes steps of (1) precursor pyrolysis: heating and pyrolyzing the polymer pyrolysis into SiC nano particles at the inert gas atmosphere in a chemical gas-phase deposition furnace; (2), chemical gas-phase deposition: heating continuously until silicon atoms on surfaces of the SiC nano particles are sublimed and escape, forming graphite fragments by means of recombination of the residual carbon atoms, and finally obtaining the SiC-graphene nano-composite by deposition and growth of the graphite fragments. The SiC-graphene nano-composite has the advantages of excellent physical and chemical properties and mechanical properties, simplicity in preparation process, low cost and wide application range.
Description
Technical field
The present invention relates to field of nanocomposite materials, relate in particular to a kind of SiC-graphene nano composite and preparation method thereof.
Background technology
Graphene is the tightly packed revolutionary new carbon that forms of monolayer carbon atom, and thickness has only 0.335 nanometer, is the thinnest in the world present two-dimensional material, also is to construct other material with carbon elements such as C60, CNT, graphite and adamantine construction unit.Graphene has the lattice structure that bi-dimensional cellular shape form is arranged, and fundamental structural unit is stable carbon hexatomic ring, combines with the powerful carbon-carbon bond of active force between the atom, so graphene-structured is highly stable.The stable lattice structure of Graphene makes it have very excellent electric conductivity.When the electronics in the Graphene moves in track, can or not introduce foreign atom and scattering takes place because of lattice defect.Because active force is very strong between atom, at normal temperatures, even carbon atom pushes on every side, the interference that electronics receives in the Graphene is also very little.Another characteristic of Graphene is that wherein electronic motion speed has reached 1/300 of the light velocity, considerably beyond the movement velocity of electronics in general conductor.On the other hand, Graphene is that energy gap is zero semiconductor, and its carrier presents linear dispersion relation near fermi level.Because these excellent electric performance, Graphene is considered to the desirable semi-conducting material of integrated circuit of future generation.Simultaneously, Graphene also has good mechanical, optics and thermal property, has electron mobility (15000cm at a high speed under outstanding heat conductivility (3000W/ (mK)) and mechanical property (1060GPa) and the room temperature
2/ (VS)).Graphene is real superficiality solid, and desirable single-layer graphene has the specific area of super large, and its theoretical specific area is up to 2066m
2/ g substantially exceeds the specific area of the activated carbon that is applied to electrochemical capacitor in double electrode layer at present.Graphene and graphene-based nano composite material are because electricity, optics, calorifics and the mechanical property of above-mentioned excellence are expected to be applied to numerous areas, like integrated circuit, MEMS, electrochemical catalyst, super capacitor, field emmision material etc.
At present; Graphene preparation method mainly contains mechanical stripping method, crystal epitaxy and chemical vapour deposition technique etc.; These preparation methods generally prepare the single or multiple lift Graphene to study its electric property at semiconductor substrate such as SiC single crystal ingot surface, develop IC semiconductor material of future generation.The graphene oxide reducing process of latest developments prepares Graphene can prepare multiple graphene-based composite; To be applied to fields such as electrochemical catalyst, super capacitor and field emmision material; But this method comprises processes such as preparing graphene oxide and the reduction of subsequent oxidation Graphene in advance, technology more complicated.And the method for preparing Graphene and graphene-based nano composite material simply, reliably still remains to be continued research and development.
Summary of the invention
Technical problem to be solved by this invention is: to the problem that prior art exists, the present invention provides a kind of SiC-graphene nano composite of core/shell structure; And a kind of technology is simple and the preparation method that is fit to produce in batches, adopt the graphene-based nano composite material that precursor conversion method and chemical vapour deposition technique combine.
For solving the problems of the technologies described above; The present invention adopts a kind of SiC-graphene nano of following technical scheme composite; Said SiC-graphene nano composite is the hud typed structure that shell coats kernel, and said kernel is the SiC nano particle, and said shell is the nano-graphite that Graphene is formed.
In the above-mentioned SiC-graphene nano composite, Graphene is preferably 8 layers～15 layers in the said nano-graphite, and the radially growth of the said SiC nano particle in edge.
In the above-mentioned SiC-graphene nano composite, said SiC-graphene nano composite is preferably diameter 100 nm～300nm and the surface is penniform spherical particle.
As a total technical conceive, the present invention also provides a kind of preparation method of above-mentioned SiC-graphene nano composite, may further comprise the steps:
(1) precursor cracking: in chemical vapor deposition stove, under the inert gas atmosphere; The polymeric preceramic body is heated to 800 ℃～1200 ℃ with the speed of heating of 5 ℃/s～10 ℃/s; Keeping inert gas flow in the heating process is 30 sccm～50 sccm; To temperature back insulation 10 minutes～50 minutes, form the SiC nano particle behind the heating pyrolyze;
(2) chemical vapour deposition (CVD): continue heating temperature is risen to 1300 ℃～1500 ℃, inert gas flow was decreased to 5 sccm～10 sccm, to temperature back insulation 10 minutes～60 minutes; Under inert gas atmosphere, be cooled to room temperature at last, it is 5 sccm～10 sccm that cooling procedure keeps inert gas flow, obtains SiC-graphene nano composite.
Above-mentioned preparation method's cardinal principle is that the distillation of SiC nano grain surface silicon atom is overflowed, and remaining carbon atom reorganization forms the Graphene fragment; The Graphene fragment is grown up through chemical vapour deposition (CVD) and is obtained SiC-graphene nano composite.
Among the above-mentioned preparation method, said polymeric preceramic body is preferably Polycarbosilane.
Among the above-mentioned preparation method, said Polycarbosilane molecular formula is: [SiH (CH
3) CH
2]
n, molecular weight is 2000, softening point is 180 ℃～220 ℃.
Among the above-mentioned preparation method, said inert gas is preferably high pure nitrogen.
Compared with prior art, the invention has the advantages that:
1, SiC-graphene nano composite of the present invention is hud typed structure; Kernel is the SiC nano particle; Shell is the nano-graphite that Graphene is formed, and it has stable physics and chemical constitution and character, has huge specific area; Can be applied to electrode of lithium cell, super capacitor, fields such as filed emission cathode material, electrochemical catalyst and composite material reinforcement body.
2, the preparation method of SiC-graphene nano composite of the present invention adopts Stainless Steel via Precursor Pyrolysis SiC nano particle earlier; Combine chemical vapour deposition technique can prepare the graphene-based nano composite material of SiC/ again; Processing step is very simple; Low production cost need not to adopt special equipment, is applicable to continuously and large-scale production.
Description of drawings
Fig. 1 is the structural representation of the preparation facilities of SiC-graphene nano composite of the present invention.
Fig. 2 is the stereoscan photograph of the SiC-graphene nano composite that makes of embodiments of the invention 1.
Fig. 3 is the stereoscan photograph of the SiC-graphene nano composite that makes of embodiments of the invention 2.
The transmission electron microscope photo of the SiC-graphene nano composite that Fig. 4 makes for embodiments of the invention 2.
Fig. 5 is the high-resolution-ration transmission electric-lens photo of the top layer nano-graphite of the SiC-graphene nano composite that makes of embodiments of the invention 2.
Fig. 6 is the stereoscan photograph of the SiC-graphene nano composite that Comparative Examples makes in the specific embodiment of the invention.
Marginal data:
1, tubular type chemical vapor deposition stove; 11, air inlet; 12, gas outlet; 2, alumina crucible; 3, graphite boat; 4, graphite substrate.
The specific embodiment
Below will combine Figure of description and specific embodiment that the present invention is explained further details.
Embodiment 1:
A kind of SiC-graphene nano composite of the present invention, it is the hud typed structure of shell coating kernel, and kernel is the SiC nano particle, and shell is the nano-graphite that Graphene is formed.It is that 100 nm～300 nm and surface are penniform spherical particle that SiC-graphene nano composite totally is diameter.Graphene is 8 layers～15 layers in the nano-graphite, and along the radially growth of SiC nano particle.
Above-mentioned SiC-graphene nano composite prepares through following steps:
(1) preparation:
A. preparatory technology device: as shown in Figure 1; Prepare the tubular type chemical vapor deposition stove 1 that two ends are established air inlet 11 and gas outlet 12 respectively; In tubular type chemical vapor deposition stove 1, place graphite boat 3, graphite boat 3 upper edge airflow directions are placed alumina crucible 2 that is used for ccontaining raw material and the graphite substrate 4 (being provided with of graphite substrate mainly is to be convenient to collect product) that is used to collect product successively.The graphite flake that graphite substrate 4 is crossed with acetone for a slice.Among Fig. 1, the direction of hollow arrow is an airflow direction.
B. 5 gram Polycarbosilanes are put into alumina crucible 2, in the present embodiment, Polycarbosilane is selected PCS (National University of Defense technology's space flight and Materials Academy CFC key lab are synthetic) for use, and technical parameter is following: molecular formula: [SiH (CH
3) CH
2]
nMolecular weight: 2000; Softening point: 180 ℃～220 ℃.
(2) precursor cracking:
C. in tubular type chemical vapor deposition stove 1, import high pure nitrogen, 2～3 times repeatedly, with the emptying of stove air.
D. the speed that heats with 10 ℃/s is heated to 1100 ℃ with tubular type chemical vapor deposition stove 1; Keeping nitrogen flow in the heating process is 30 sccm～50 sccm; To temperature back insulation 30 minutes; The PCS pyrolysis product comprises gases such as silane fragment, hydrocarbon, under nitrogen stream delivery effect, arrives on the graphite substrate, and heating pyrolyze forms the SiC nano particle.
(3) chemical vapour deposition (CVD):
E. continue heating temperature is risen to 1300 ℃, nitrogen flow was decreased to 5 sccm～10 sccm, to temperature back insulation 10 minutes; Under nitrogen atmosphere, be cooled to room temperature then, it is 5 sccm～10 sccm that cooling procedure keeps nitrogen flow, on graphite substrate, collects at last and obtains SiC-graphene nano composite.
F. close nitrogen, take out graphite boat 3, on graphite substrate 4, collect pulverous product.
The above-mentioned product that makes is carried out electron-microscope scanning, and the gained photo is as shown in Figure 2.Visible by Fig. 2, product is the spherical of diameter 100 nm～300 nm, and energy spectrum analysis shows that these products are the SiC particle; Wherein visible part SiC particle surface is coarse; Be coated with the featheriness material, X-ray diffraction analysis shows that it is a SiC-graphene nano composite of the present invention, and is visible by stereoscan photograph; Graphene is approximately 8 layers～15 layers in the nano-graphite, and along the radially growth of SiC nano particle.
Embodiment 2:
A kind of SiC-graphene nano composite of the present invention, it is the hud typed structure of shell coating kernel, and kernel is the SiC nano particle, and shell is the nano-graphite that Graphene is formed.It is that 100 nm～200 nm and surface are penniform spherical particle that SiC-graphene nano composite totally is diameter.Graphene is 8 layers～15 layers in the nano-graphite, and along the radially growth of SiC nano particle.
The SiC-graphene nano composite of present embodiment prepares through following steps:
(1) preparation: identical with embodiment 1.
(2) precursor cracking:
C. in tubular type chemical vapor deposition stove 1, import high pure nitrogen, 2～3 times repeatedly, with the emptying of stove air.
D. the speed that heats with 8 ℃/s is heated to 800 ℃ with tubular type chemical vapor deposition stove 1, and keeping nitrogen flow in the heating process is 30 sccm～50 sccm, to temperature back insulation 50 minutes, polymeric preceramic body Polycarbosilane heating pyrolyze is formed the SiC nano particle.
(3) chemical vapour deposition (CVD):
E. continue heating temperature is risen to 1400 ℃, nitrogen flow was decreased to 5 sccm～10 sccm, to temperature back insulation 60 minutes; Under inert gas atmosphere, be cooled to room temperature then, it is 5 sccm～10 sccm that cooling procedure keeps nitrogen flow, and continuing heating is that the distillation of SiC nano grain surface silicon atom is overflowed, and remaining carbon atom reorganization forms the Graphene fragment; The Graphene fragment is grown up through chemical vapour deposition (CVD) and is obtained SiC-graphene nano composite.
F. close nitrogen, take out graphite boat 3, on graphite substrate 4, collect pulverous product.
The above-mentioned product that makes is carried out electron-microscope scanning, gained photo such as Fig. 3, Fig. 4, shown in Figure 5.Visible by Fig. 3, product is the spherical of diameter 100 nm～300nm, and rough surface is coated with the featheriness material, and X-ray diffraction analysis shows that product is made up of SiC and graphite.Visible by Fig. 4, product is the SiC-graphene nano composite with core/shell structure, and core is the SiC particle, diameter 100 nm～200 nm, and skin is the featheriness nano-graphite, the featheriness nano-graphite is radially growth at the SiC particle surface.Fig. 5 is the high-resolution-ration transmission electric-lens photo of nano-graphite, and visible nano-graphite is made up of the multi-layer graphene that freely distributes, and each sheet nano-graphite is made up of 8 layers～15 layer graphenes.
Comparative Examples:
The SiC-graphene nano composite of this Comparative Examples prepares through following steps:
(1) preparation: identical with embodiment 1.
(2) precursor cracking:
C. in tubular type chemical vapor deposition stove 1, import high pure nitrogen, 2～3 times repeatedly, with the emptying of stove air.
D. with the speed that heats tubular type chemical vapor deposition stove 1 is heated to 1100 ℃ less than 10 ℃/s; Keeping nitrogen flow in the heating process is 30 sccm～50 sccm; To temperature back insulation 5 minutes, polymeric preceramic body Polycarbosilane heating pyrolyze is formed the SiC nano particle.
(3) chemical vapour deposition (CVD):
E. continue heating temperature is risen to 1400 ℃, nitrogen flow was decreased to 5 sccm～10 sccm, to temperature back insulation 90 minutes; Be cooled to room temperature, it is 5 sccm～10 sccm that cooling procedure keeps nitrogen flow.
F. close nitrogen, take out graphite boat 3, on graphite substrate 4, collect pulverous product.
The above-mentioned product that makes is carried out electron-microscope scanning, and the gained photo is as shown in Figure 6.Visible by Fig. 6; Product is the spherical of ribbon and diameter 50 nm～100 nm, surperficial smoother, and energy spectrum analysis shows that these products are SiC; It is thus clear that product is made up of the SiC nano particle; Do not form nano-graphite, its reason possibly mainly be because heat time heating time or temperature retention time do not control effectively, and makes the SiC nanoparticle growth become the SiC nanofiber.It is thus clear that in preparation technology of the present invention, control of process parameters is quite crucial and important.
To sum up, employing Stainless Steel via Precursor Pyrolysis SiC nano particle of the present invention can prepare the graphene-based nano composite material of SiC/ in conjunction with chemical vapour deposition technique, and low production cost need not to adopt special equipment, is applicable to continuously and large-scale production.The SiC-graphene nano composite that makes can be applicable to electrode of lithium cell, super capacitor, fields such as filed emission cathode material, electrochemical catalyst and composite material reinforcement body.
Below only be preferred implementation of the present invention, protection scope of the present invention also not only is confined to the foregoing description, and the various process programs of conceiving no substantial differences with the present invention are all in protection scope of the present invention.
Claims (7)
1. a SiC-graphene nano composite is characterized in that, said SiC-graphene nano composite is the hud typed structure that shell coats kernel, and said kernel is the SiC nano particle, and said shell is the nano-graphite that Graphene is formed.
2. SiC-graphene nano composite according to claim 1 is characterized in that, Graphene is 8 layers～15 layers in the said nano-graphite, and the radially growth of the said SiC nano particle in edge.
3. SiC-graphene nano composite according to claim 1 and 2 is characterized in that, said SiC-graphene nano composite is that diameter 100 nm～300nm and surface are penniform spherical particle.
4. preparation method like each described SiC-graphene nano composite in the claim 1～3 may further comprise the steps:
(1) precursor cracking: in chemical vapor deposition stove, under the inert gas atmosphere; The polymeric preceramic body is heated to 800 ℃～1200 ℃ with the speed of heating of 5 ℃/s～10 ℃/s; Keeping inert gas flow in the heating process is 30 sccm～50 sccm; To temperature back insulation 10 minutes～50 minutes, form the SiC nano particle behind the heating pyrolyze;
(2) chemical vapour deposition (CVD): continue heating temperature is risen to 1300 ℃～1500 ℃, inert gas flow was decreased to 5 sccm～10 sccm, to temperature back insulation 10 minutes～60 minutes; Under inert gas atmosphere, be cooled to room temperature at last, it is 5 sccm～10 sccm that cooling procedure keeps inert gas flow, obtains SiC-graphene nano composite.
5. preparation method according to claim 4 is characterized in that, said polymeric preceramic body is a Polycarbosilane.
6. preparation method according to claim 5 is characterized in that, said Polycarbosilane molecular formula is: [SiH (CH
3) CH
2]
n, molecular weight is 2000, softening point is 180 ℃～220 ℃.
7. according to claim 4 or 5 or 6 described preparation methods, it is characterized in that said inert gas is a high pure nitrogen.
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| US20130184143A1 (en) * | 2011-07-29 | 2013-07-18 | The Arizona Board Of Regents, On Behalf Of The University Of Arizona | Graphene-Reinforced Ceramic Composites and Uses Therefor |
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| CN104120402A (en) * | 2014-08-08 | 2014-10-29 | 苏州宏久航空防热材料科技有限公司 | Preparation method of graphene-SiC film |
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| CN102343239A (en) * | 2011-05-20 | 2012-02-08 | 四川大学 | Oxidized graphene or graphene/inorganic particle core/shell material and preparation method thereof |
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| US20130184143A1 (en) * | 2011-07-29 | 2013-07-18 | The Arizona Board Of Regents, On Behalf Of The University Of Arizona | Graphene-Reinforced Ceramic Composites and Uses Therefor |
| US8962504B2 (en) * | 2011-07-29 | 2015-02-24 | Arizona Board Of Regents On Behalf Of The University Of Arizona | Graphene-reinforced ceramic composites and uses therefor |
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| CN109160804A (en) * | 2018-10-26 | 2019-01-08 | 武汉大学 | A kind of preparation method of height endurability nanometer phase graphene composite ceramics |
| CN110229709A (en) * | 2019-06-28 | 2019-09-13 | 中国人民解放军空军勤务学院 | SiC adulterates the preparation and application of onion shape graphitization carbon ball nanocomposite |
| CN110229709B (en) * | 2019-06-28 | 2022-01-28 | 中国人民解放军空军勤务学院 | Preparation and application of SiC-doped onion-shaped graphitized carbon sphere nano composite material |
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| KR102513770B1 (en) | 2020-12-24 | 2023-03-24 | (주)다다코리아 | Method for manufacturing graphite coated silicon carbide particles |
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