CN105274489A - Preparation method for forming nano sheet structure network on substrate and substrate - Google Patents
Preparation method for forming nano sheet structure network on substrate and substrate Download PDFInfo
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- CN105274489A CN105274489A CN201410498442.3A CN201410498442A CN105274489A CN 105274489 A CN105274489 A CN 105274489A CN 201410498442 A CN201410498442 A CN 201410498442A CN 105274489 A CN105274489 A CN 105274489A
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 46
- 239000000758 substrate Substances 0.000 title abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 160
- 239000010453 quartz Substances 0.000 claims abstract description 43
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007789 gas Substances 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 239000002210 silicon-based material Substances 0.000 claims abstract description 27
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- 238000010438 heat treatment Methods 0.000 claims description 70
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- 239000000377 silicon dioxide Substances 0.000 claims description 50
- 235000012239 silicon dioxide Nutrition 0.000 claims description 46
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- 239000002184 metal Substances 0.000 claims description 44
- 230000015572 biosynthetic process Effects 0.000 claims description 34
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- 238000001237 Raman spectrum Methods 0.000 claims description 20
- -1 polydimethylsiloxane Polymers 0.000 claims description 20
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
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- 239000011521 glass Substances 0.000 claims description 11
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- ADKPKEZZYOUGBZ-UHFFFAOYSA-N [C].[O].[Si] Chemical compound [C].[O].[Si] ADKPKEZZYOUGBZ-UHFFFAOYSA-N 0.000 claims description 9
- 229960001866 silicon dioxide Drugs 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 7
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 6
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- 150000001875 compounds Chemical class 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
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- 239000010931 gold Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 150000001299 aldehydes Chemical class 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
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- 150000002576 ketones Chemical class 0.000 claims description 3
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 3
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
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- 239000002064 nanoplatelet Substances 0.000 abstract 2
- 238000000034 method Methods 0.000 description 41
- 238000005229 chemical vapour deposition Methods 0.000 description 23
- 229910052799 carbon Inorganic materials 0.000 description 20
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 15
- 229910010271 silicon carbide Inorganic materials 0.000 description 15
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- NHDHVHZZCFYRSB-UHFFFAOYSA-N pyriproxyfen Chemical compound C=1C=CC=NC=1OC(C)COC(C=C1)=CC=C1OC1=CC=CC=C1 NHDHVHZZCFYRSB-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention relates to a preparation method for forming a nano sheet structure network on a substrate, which comprises the steps of providing a substrate and a silicon-containing compound; cracking the silicon-containing compound in a high temperature furnace or a quartz tube of a high temperature furnace insulated from air and having a temperature between 500 and 1500 ℃ to form a gas composition; delivering hydrocarbon vapor into the high temperature furnace or the quartz tube of the high temperature furnace at 500-1500 ℃ by argon gas, wherein the hydrocarbon vapor and the gas formed by the cracked silicon-containing compound are mixed to form a reactant; and in the high-temperature furnace or the quartz tube of the high-temperature furnace with the temperature of 500-1500 ℃, forming the reactant into a nano-sheet structure network on the substrate by a vapor deposition process, wherein covalent bonds are formed between the nano-sheet structure network and the substrate. Furthermore, the network of nano-platelet structures is a graphene-like network of nano-platelet structures.
Description
Technical field
The invention relates to and a kind ofly form the preparation method of flaky nanometer structure network on base material, particularly form by vapor deposition processes the application that the method for flaky nanometer structure network on base material and surface have the base material of flaky nanometer structure network about a kind of.There is between this flaky nanometer structure network and base material the carbide covalently bonded that bond intensity is high.Secondly, this flaky nanometer structure network is class graphene nano sheet structural network, so have good erosion resistance, low-friction coefficient, good thermal conductance and Effective Conductivity and optical property.Moreover the gas phase composition that this character with the base material of flaky nanometer structure network can use by change vapor deposition processes regulates and controls, and reaches the object of this base material of application in various industry whereby.
Background technology
The allotropic substance (allotropes) of carbon comprises soccerballene, CNT (carbon nano-tube), Graphene, graphite and diamond, and wherein Graphene is subject to the attention of researchist especially because having unique two-dirnentional structure.Graphene be by carbon atom rearrange shape and be hexangle type and thickness is the flaky nanometer structure of an atom, the two-dirnentional structure due to this uniqueness causes Graphene to have outstanding electric conductivity (8x105S/m), high thermal conductivity matter (about5300Wm
-1k
-1), excellent physical strength (tensilestrengthof130GPaandYoung ' smodulusof1TPa), low-friction coefficient and good corrosion protection character.
It is general that to prepare Graphene with known techniques be with graphite for raw material, sequentially through peroxidation intercalation, dial from reducing program and obtain Graphene.Usually carry out the upgrading of macromolecular material by interpolation Graphene in macromolecular material.But, for pottery, glass, metal and semiconductor material, because the service temperature of the materials such as above-mentioned pottery is greater than 400 DEG C usually, but the stable at high temperature of Graphene more than 400 DEG C is poor, structure is easily destroyed, therefore, in actual industry application, the mode of adding Graphene is adopted to carry out the upgrading of pottery, glass, metal and semiconductor material etc. and cannot expected effect be obtained.
On the other hand, though Graphene coating can be fixed on the surface of pottery, glass, metal and semiconductor material etc. by mode then, but graphenic surface is unusual inertia, so graphene layer is easy to the sur-face peeling from above-mentioned stupalith.And for being coated with the usual non-refractory of fixing solid.Solid also can reduce and change the original excellent properties of Graphene simultaneously.Therefore, this kind of mode be not suitable for pottery, glass, metal and semiconductor material etc.
The people such as YuegangZhang are at NanoLett.2010, and 10,1542 – 1548 disclose a kind of by Graphene deposition method on the dielectric material; The method deposits on the surface of dielectric materials the film be made up of copper in advance, by vapour deposition process, the structure of Graphene is formed on the above-mentioned film be made up of copper and then, finally removes this film and obtain the dielectric materials that surface has graphene-structured.Covalently bonded is not had thus between the graphene-structured that obtains of method and dielectric materials.Therefore, the poor stability of its high temperature, and manufacture method is loaded down with trivial details, directly cannot form Graphene sheet structure on material surface.
U.S. Patent Publication case US20110070146A1 discloses the another kind of method manufacturing Graphene; The method comprises: first form wetting ability zone of oxidation on base material; Secondly, then form hydrophobic metals catalyst layer in this wetting ability zone of oxidation, then on this hydrophobic metals catalyst layer, form graphene-structured; Finally, this hydrophobic metals catalyst layer is separated to obtain having the base material of graphene-structured.In this method; manufacturing step is quite complicated, and needs to remove metal solvent layer with etching program, and this etching program can produce a large amount of acid waste liquid; therefore this manufacture method is unfriendly for environment protection, and this manufacture method directly cannot form Graphene sheet structure in material surface equally.
In sum, the process technique substrate surface of pottery, glass, metal and semiconductor material etc. forming graphene nano sheet structural network is the problem that current industrial community needs researchdevelopment and breakthrough badly.
Summary of the invention
In view of above-mentioned background of invention, in order to meet the demand in industry, the object of the present invention is to provide and a kind ofly form the base material that the preparation method of flaky nanometer structure network on base material and surface have flaky nanometer structure network, to solve institute's problems faced in current industry, promote the technology of the surfaction of pottery, metal and semiconductor material etc. simultaneously.
The object of the invention is to realize by the following technical solutions.The invention provides and a kind ofly form the preparation method of flaky nanometer structure network on base material, the method comprises the following step: provide base material and silicon-containing compound; In the silica tube of High Temperature Furnaces Heating Apparatus between 500 to 1500 DEG C of isolated air and temperature or High Temperature Furnaces Heating Apparatus, this silicon-containing compound of cracking is to form gas composition; Transmit the steam of hydrocarbon polymer by argon gas to enter in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, the gas composition that the steam of this hydrocarbon polymer and the silicon-containing compound of above-mentioned cracking are formed is mixed to form reactant; And in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, make this reactant form flaky nanometer structure network on this base material by vapor deposition processes, between this flaky nanometer structure network and this base material, there is covalently bonded.
Object of the present invention also can be applied to the following technical measures to achieve further.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned base material comprises pottery, quartz, glass, Silicon Wafer or metal.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned metal comprises carbon steel, copper, titanium or its alloy.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned metallic surface has the coating layer of silicon-dioxide.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned silicon-containing compound is selected from following group one or a combination set of: silica gel, polydimethylsiloxane, organosilicon, Silane Grafted polymer, siliceous metallocene polymer and METHYL TRICHLORO SILANE.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned silicon-containing compound more comprises charges, gold, copper halide or metallocene compound.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned temperature is between 750 to 950 DEG C.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned hydrocarbon polymer comprises ketone, aldehydes, ester class, alkanes, alkene class or alkynes class.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned alkene class is selected from following group one or a combination set of: naphthalene, benzene,toluene,xylene and ethene.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned flaky nanometer structure network is class graphene nano sheet structural network.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned covalently bonded is carbide bond.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned carbide bond is selected from following group one or a combination set of: carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-nitrogen bond knot and carbon-nitrogen-metal bond.
Object of the present invention also realizes by the following technical solutions.The invention provides and another kind of form the preparation method of flaky nanometer structure network on base material, the method comprises the following step: insert base material in the silica tube of High Temperature Furnaces Heating Apparatus or High Temperature Furnaces Heating Apparatus in; Performing heating schedule makes the temperature of the silica tube of this High Temperature Furnaces Heating Apparatus or High Temperature Furnaces Heating Apparatus reach between 500 to 1500 DEG C; Transmit vapor composition by argon gas to enter in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, this vapor composition is made up of hydrocarbon polymer and silicon compound; And in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, make this vapor composition form flaky nanometer structure network on this base material by vapor deposition processes, between this flaky nanometer structure network and this base material, there is covalently bonded.
Object of the present invention also can be applied to the following technical measures to achieve further.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned base material comprises pottery, quartz, glass, Silicon Wafer or metal.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned metal comprises carbon steel, copper, titanium or its alloy.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned metallic surface has the coating layer of silicon-dioxide.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned temperature is between 750 to 950 DEG C.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned hydrocarbon polymer is selected from following group one or a combination set of: benzene, toluene and dimethylbenzene.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned silicon compound is tetraalkyl silicon compound.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned silicon compound is tetraethyl silicane compound.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned silicon compound more comprises charges, gold, copper halide or metallocene compound.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned flaky nanometer structure network is class graphene nano sheet structural network.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned covalently bonded is carbide bond.
The preparation method of aforesaid formation flaky nanometer structure network on base material, wherein above-mentioned carbide bond is selected from one of following group and combination thereof: carbon-oxygen-silicon bound knot or carbon-silicon bond.
Object of the present invention realizes again by the following technical solutions.The invention provides the base material that a kind of surface has nanostructured network, this nanostructured network is fixed on this surface by carbide bond.The Raman spectrum of above-mentioned nanostructured network is at 1594 ± 5cm
-1there are G broadband and 1338 ± 5cm in place
-1there is D broadband at place, due to the Raman spectrum of the Raman spectrum very similar graphene nano sheet structure of this nanostructured network, so this nanostructured network is class graphene nano sheet structural network, there is the similar quality of graphene-structured, as outstanding electric conductivity, high thermal conductivity matter, excellent physical strength, low-friction coefficient and good corrosion protection character; Simultaneously, this nanostructured network is fixed on substrate surface with carbide bond again, and above-mentioned carbide bond is selected from following group one or a combination set of: carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-nitrogen bond knot and carbon-nitrogen-metal bond.Therefore, the stability with the base material on the surface of above-mentioned nanostructured network is excellent, can be widely used in Different Industries field.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to technique means of the present invention can be better understood, and can be implemented according to the content of specification sheets, and can become apparent to allow above and other object of the present invention, feature and advantage, below especially exemplified by preferred embodiment, and coordinate accompanying drawing, be described in detail as follows.
Accompanying drawing explanation
The photograph that Fig. 1 (a) is quartz plate; Fig. 1 (b) is using naphthalene as carbon source and is prepared into chemical Vapor deposition process the photograph that surface has the quartz plate of class graphene nano sheet structural network.
Fig. 2 is the comparison diagram of the class graphene nano sheet structural network of sweep electron microscope.
Fig. 3 (a) is the Raman spectrum of quartz; Fig. 3 (b) is the Raman spectrum of business-like Graphene; Fig. 3 (c) has class graphene nano sheet structural network and this structural network has the Raman spectrum of carbonization key for quartz surfaces; Fig. 3 (d) has class graphene nano sheet structural network but this structural network does not have the Raman spectrum of carbonization key for quartz surfaces.
The photograph that Fig. 4 (a) is Silicon Wafer; Fig. 4 (b) is using naphthalene as carbon source and is prepared into chemical Vapor deposition process the photograph that surface has the Silicon Wafer of class graphene nano sheet structural network.
Fig. 5 is using benzene as carbon source and is prepared into chemical Vapor deposition process the photograph that surface has the quartz plate of class graphene nano sheet structural network.
Fig. 6 is using ethene as carbon source and is prepared into chemical Vapor deposition process the photograph that surface has the quartz plate of class graphene nano sheet structural network.
Embodiment
For further setting forth the present invention for the technique means reaching predetermined goal of the invention and take and effect, below in conjunction with accompanying drawing and preferred embodiment, to a kind of embodiment, structure, feature and the effect thereof forming the preparation method of flaky nanometer structure network on base material and base material thereof proposed according to the present invention, be described in detail as follows.
What the present invention inquired at this is a kind ofly form the base material that the preparation method of flaky nanometer structure network on base material and surface have flaky nanometer structure network.In order to the present invention can be understood up hill and dale, by following description, detailed raw material, step and application are proposed.Apparently, the specific details that the those skilled in the art that execution of the present invention is not defined in this field has the knack of.On the other hand, well-known raw material or step are not described in details, to avoid the restriction causing the present invention unnecessary.Example of the present invention can be described in detail as follows, but except these are described in detail, the present invention can also be implemented in other example widely, and scope of the present invention not circumscribed, it is as the criterion with the scope of the claims afterwards.
According to first embodiment of the invention, the invention provides and a kind ofly form the preparation method of flaky nanometer structure network on base material, the method comprises the following step: provide base material and silicon-containing compound; In the silica tube of High Temperature Furnaces Heating Apparatus between 500 to 1500 DEG C of isolated air and temperature or High Temperature Furnaces Heating Apparatus, this silicon-containing compound of cracking is to form gas composition; Transmit the steam of hydrocarbon polymer by argon gas to enter in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, the gas composition that the steam of this hydrocarbon polymer and the silicon-containing compound of above-mentioned cracking are formed is mixed to form reactant; And in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, make this reactant form flaky nanometer structure network on this base material by vapor deposition processes, between this flaky nanometer structure network and this base material, there is covalently bonded.
In an embodiment, described base material comprises pottery, quartz, glass, Silicon Wafer or metal.
In another embodiment, described metal comprises carbon steel, copper, titanium or its alloy.
In order to make vapor deposition processes reach preferably effect on metal base, coating upgrading all can be carried out usually in the surface of metal base.
In an embodiment, metallic surface has the coating layer of silicon-dioxide.
In order to reach the object between flaky nanometer structure network and base material with covalently bonded, silicon-containing compound or nitrogenous compound are necessary raw material in preparation method provided by the present invention.
In an embodiment, silicon-containing compound is selected from following group one or a combination set of: silica gel, polydimethylsiloxane, organosilicon, Silane Grafted polymer, siliceous metallocene polymer and METHYL TRICHLORO SILANE.
In another embodiment, silicon-containing compound more comprises charges, gold, copper halide or metallocene compound.
In an embodiment, nitrogenous compound is selected from following group one or a combination set of: polypropylene fine (polyacrylonitrile), cyano group polymer, nitrogen heterocyclic ring family macromolecule.
In described preparation method's step be: in the silica tube of High Temperature Furnaces Heating Apparatus between 500 to 1500 DEG C of isolated air and temperature or High Temperature Furnaces Heating Apparatus, this silicon-containing compound of cracking is to form gas composition.
In a preferred embodiment, above-mentioned temperature is between 750 to 950 DEG C.
In an embodiment, by continuing to pass into the environment that argon gas creates isolated air.
In described preparation method's step be: transmit the steam of hydrocarbon polymer by argon gas and enter in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, the gas composition that the steam of this hydrocarbon polymer and the silicon-containing compound of above-mentioned cracking are formed is mixed to form reactant; And in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, make this reactant form flaky nanometer structure network on this base material by vapor deposition processes, between this flaky nanometer structure network and this base material, there is covalently bonded.
In an embodiment, comprise ketone, aldehydes, ester class, alkanes, alkene class or alkynes class as the hydrocarbon polymer of carbon source needed for vapor deposition processes.
In another embodiment, above-mentioned alkene class is selected from following group one or a combination set of: naphthalene, benzene,toluene,xylene and ethene.
In order to reach the object between flaky nanometer structure network and base material with covalently bonded, the service temperature of preparation method needs to control between 500 to 1500 DEG C.
In a preferred embodiment, above-mentioned temperature is between 750 to 950 DEG C.
Class graphene nano sheet structural network according to the flaky nanometer structure network that preparation method provided by the present invention is formed.
The covalently bonded had between above-mentioned flaky nanometer structure network and base material is carbide covalently bonded.
In an embodiment, described carbide covalently bonded is selected from following group one or a combination set of: carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-nitrogen bond knot and carbon-nitrogen-metal bond.
Second embodiment of the invention, the invention provides and another kind of form the preparation method of flaky nanometer structure network on base material, the method comprises the following step: insert base material in the silica tube of High Temperature Furnaces Heating Apparatus or High Temperature Furnaces Heating Apparatus in; Performing heating schedule makes the temperature of the silica tube of this High Temperature Furnaces Heating Apparatus or High Temperature Furnaces Heating Apparatus reach between 500 to 1500 DEG C; Transmit vapor composition by argon gas to enter in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, this vapor composition is made up of hydrocarbon polymer and silicon compound; And in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, make this vapor composition form flaky nanometer structure network on this base material by vapor deposition processes, between this flaky nanometer structure network and this base material, there is covalently bonded.
In an embodiment, described base material comprises pottery, quartz, glass, Silicon Wafer or metal.
In another embodiment, described metal comprises carbon steel, copper, titanium or its alloy.
In order to make vapor deposition processes reach preferably effect on metal base, coating upgrading all can be carried out usually in the surface of metal base.
In an embodiment, metallic surface has the coating layer of silicon-dioxide.
In described preparation method's step be: perform heating schedule and make the temperature of the silica tube of this High Temperature Furnaces Heating Apparatus or High Temperature Furnaces Heating Apparatus reach between 500 to 1500 DEG C; Transmit vapor composition by argon gas to enter in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, this vapor composition is made up of hydrocarbon polymer and silicon compound; And in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, make this vapor composition form flaky nanometer structure network on this base material by vapor deposition processes, between this flaky nanometer structure and this base material, there is covalently bonded.
In order to reach the object between flaky nanometer structure network and base material with covalently bonded, the service temperature of preparation method needs to control between 500 to 1500 DEG C.
In a preferred embodiment, above-mentioned service temperature is between 750 to 950 DEG C.
In an embodiment, by continuing to pass into the environment that argon gas creates isolated air.
In an embodiment, be selected from following group one or a combination set of as the hydrocarbon polymer of carbon source needed for vapor deposition processes: benzene, toluene and dimethylbenzene.
In another embodiment, in order to reach the object between flaky nanometer structure network and base material with covalently bonded, silicon-containing compound is tetraalkyl silicon compound.
In a preferred embodiment, silicon-containing compound is tetraethyl silicane compound.
In another embodiment, silicon-containing compound more comprises charges, gold, copper halide or metallocene compound.
Class graphene nano sheet structural network according to the flaky nanometer structure network that preparation method provided by the present invention is formed.
The covalently bonded had between above-mentioned flaky nanometer structure network and base material is carbide covalently bonded.
In an embodiment, described carbide covalently bonded is selected from following group one or a combination set of: carbon-oxygen-silicon bound knot and carbon-silicon bond.
The preparation method of formation flaky nanometer structure network on base material that 3rd embodiment of the present invention provides by the above-mentioned first or second embodiment provides surface to have the base material of nanostructured network further, and this nanostructured network is fixed on this substrate surface by carbide bond (carbidebond).The Raman spectrum of wherein above-mentioned nanostructured network is at 1594 ± 5cm
-1there are G broadband and 1338 ± 5cm in place
-1there is D broadband at place.
In an embodiment, above-mentioned carbide bond (carbidebond) is selected from following group one or a combination set of: carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-nitrogen bond knot and carbon-nitrogen-metal bond.
Raman spectrum due to above-mentioned nanostructured network is very similar to the Raman spectrum of graphene nano sheet structure, so this nanostructured network is class graphene nano sheet structural network, there is the character similar in appearance to graphene nano sheet structural network, as outstanding electric conductivity, high thermal conductivity matter, excellent physical strength, low-friction coefficient and good corrosion protection character; Meanwhile, this nanostructured network is fixed on substrate surface with carbide bond (carbidebond) again, and therefore, the stability with the base material on the surface of above-mentioned nanostructured network is excellent, can be widely used in Different Industries.
In an embodiment, the base material that above-mentioned surface has a nanostructured network is used as the assembly composition of solar cell.
In an embodiment, the base material that above-mentioned surface has a nanostructured network is used as the assembly composition of semi-conductor.
In an embodiment, the base material that above-mentioned surface has a nanostructured network is used as the assembly composition of optical module.
In an embodiment, the base material that above-mentioned surface has a nanostructured network is used as the assembly composition of anticorrosion material.
In an embodiment, the base material that above-mentioned surface has a nanostructured network is used as the composition of non-stick cooker.
In an embodiment, the base material that above-mentioned surface has a nanostructured network is used as the assembly composition of radiating module.
Example is below utilized to illustrate further the present invention, only illustrate enforcement state of the present invention herein, haveing the knack of this operator can according to these embodiments and example, carry out various equivalence change or modify, but scope of the present invention be with request scope described later for benchmark, be not limited to these embodiments and example.
Example one. prepare with chemical Vapor deposition process the quartz plate that a kind of surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
Solid naphthalene (purity 99%, purchases to Aldrich) is used to form the carbon source of class graphene-structured on base material as chemical Vapor deposition process.First, the quartz plate of to be 1/16 inch of size by two panels thickness be 1 inch of x1 inch and silicon-containing compound (1 gram) put into the silica tube of High Temperature Furnaces Heating Apparatus, and pass into argon gas after 10 minutes, the silica tube of heating High Temperature Furnaces Heating Apparatus is to temperature 750 DEG C.The steam transmitting naphthalene with argon gas enters temperature at the silica tube of 750 DEG C, carries out chemical vapour deposition procedure after 50 minutes, takes out quartz plate after room temperature got back to by cooling silica tube.The photograph that Fig. 1 (a) is quartz plate; Fig. 1 (b) is using naphthalene as carbon source and is prepared into chemical Vapor deposition process the quartz plate that surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
When silica tube temperature reaches more than 500 DEG C, can there is thermo-cracking and produce to comprise Si (CH in silicon-containing compound
3)-OH, H
2si (CH
3)
2, CH
4, CO and O
2gas, above-mentioned gas can form silicon carbide covalently bonded and silicon oxide carbide covalently bonded with the reaction of the carbon atom at class graphene nano sheet structural network edge.Because quartz plate formed primarily of elements such as silicon, carbon, oxygen and nitrogen, so when quartz plate is at 750 DEG C or more, this temperature condition can make to produce silicon carbide covalently bonded and silicon oxide carbide covalently bonded between quartz plate and class graphene nano sheet structural network.
Fig. 2 is the class graphene nano sheet structural network figure of sweep electron microscope, and the thickness of its class graphene nano sheet structural network is about 3 μm.
Surface prepared by above-mentioned example one has the quartz plate of the class graphene nano sheet structural network of silicon carbide covalently bonded, and the resistance of this quartz plate is about 12-24K Ω; In addition, the class graphene-structured network layer on this quartz plate surface cannot remove with strong acid or other physics strength, and temperature at 450 DEG C time this quartz plate surface class graphene nano sheet structural network layer still there is good thermostability.Analyze its Young ' smodulus (Young's modulus) for 170GPa with AFM further, and Hertzianhardness (hardness of hertz) is 22.5GPa.
Because Raman spectrum is very sensitive for the electronic structure change of carbon material, therefore very useful information can be obtained with Raman spectrum analysis Graphene and associated carbon element material; The Raman spectrum analysis instrument that this experimental analysis uses is Renishaw1000microspectrometer, and the wavelength of use is 514.5nm.Fig. 3 (a) is depicted as the Raman spectrum of quartz, as experiment contrast group; The Raman spectrum of Graphene of Fig. 3 (b) for commercially producing, this Graphene is reduced by graphene oxide and makes, and its Raman spectrum is presented at 1586cm
-1there are G broadband (Gband) and 1348cm
-1there is D broadband (Dband), and at 2703cm
-1there is 2D broadband, this external 2934cm
-1have D+G in conjunction with broadband.Fig. 3 (c) has class graphene nano sheet structural network and this structural network has the Raman spectrum of carbonization key for quartz surfaces.Fig. 3 (d) has class graphene nano sheet structural network but this structural network does not have the Raman spectrum of carbonization key for quartz surfaces, by Fig. 3 (c) and Fig. 3 (d) can clear view to the existence of G broadband (Gband) and D broadband (Dband), and also have simultaneously broad D+G in conjunction with broadband, this Raman spectrum proves that this quartz surfaces has class graphene nano sheet structural network really.
Example two, prepare with chemical Vapor deposition process the Silicon Wafer that a kind of surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
Preparation method is as described in example one, base material changes Silicon Wafer into by quartz plate, finally obtain the Silicon Wafer that surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded, finished product as shown in Fig. 4 (b), i.e. Fig. 4 (a) photograph that is Silicon Wafer; Fig. 4 (b) is using naphthalene as carbon source and is prepared into chemical Vapor deposition process the photograph that surface has the Silicon Wafer of class graphene nano sheet structural network.。
Example three, prepare with chemical Vapor deposition process the quartz plate that a kind of surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
Benzene (purity 99.9%, purchases to Aldrich) is used to form the carbon source of class graphene-structured on base material as chemical Vapor deposition process.First, the quartz plate of to be 1/16 inch of size by two panels thickness be 1 inch of x3 inch puts into the silica tube of High Temperature Furnaces Heating Apparatus, and pass into argon gas after 10 minutes, the silica tube of heating High Temperature Furnaces Heating Apparatus is to temperature 950 DEG C.The steam transmitting benzene and tetramethylsilane compound (Tetramethylorthosilicate) with argon gas enters temperature at the silica tube of 950 DEG C, carries out chemical vapour deposition procedure after 60 minutes, takes out quartz plate after room temperature got back to by cooling silica tube.Namely obtain using benzene as carbon source and be prepared into chemical Vapor deposition process the quartz plate that surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded, finished product as shown in Figure 5.
Example four, prepare with chemical Vapor deposition process the quartz plate that a kind of surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
Ethene (purity 99.5%) is used to form the carbon source of class graphene-structured on base material as chemical Vapor deposition process.First, the quartz plate of to be 1/8 inch of size by two panels thickness be 1 inch of x1 inch and silicon-containing compound (1 gram) put into the silica tube of High Temperature Furnaces Heating Apparatus, and pass into argon gas after 10 minutes, the silica tube of heating High Temperature Furnaces Heating Apparatus is to temperature 950 DEG C.Transmit ethylene gas with argon gas and together enter temperature at the silica tube of 950 DEG C, carry out chemical vapour deposition procedure after 50 minutes, after room temperature got back to by cooling silica tube, take out quartz plate.Can obtain using ethene as carbon source and be prepared into chemical Vapor deposition process the quartz plate that surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.Finished product as shown in Figure 6.
Example five, prepare with chemical Vapor deposition process the steel plate that a kind of surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
Preparation method is as described in example one, and base material changes the steel plate through silica-coating process into by quartz plate, finally obtains the steel plate that surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
Example six, prepare with chemical Vapor deposition process the steel plate that a kind of surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
Toluene (purity 99.8%, purchases to Aldrich) is used to form the carbon source of class graphene-structured on base material as chemical Vapor deposition process.First, two panels is put into the silica tube of High Temperature Furnaces Heating Apparatus through the steel plate of silica-coating process, pass into argon gas after 10 minutes, the silica tube of heating High Temperature Furnaces Heating Apparatus is to temperature 850 DEG C.The steam transmitting toluene and tetraethyl silicane compound (Tetraethylorthosilicate) with argon gas enters temperature at the silica tube of 850 DEG C, carries out chemical vapour deposition procedure after 60 minutes, takes out quartz plate after room temperature got back to by cooling silica tube.Namely obtain using toluene as carbon source and be prepared into chemical Vapor deposition process the steel plate that surface has the class graphene nano sheet structural network of silicon carbide (silicon oxide carbide) covalently bonded.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but and be not used to limit the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (25)
1. form the preparation method of flaky nanometer structure network on base material, it is characterized in that the preparation method of this formation flaky nanometer structure network on base material comprises:
Base material and silicon-containing compound are provided;
In the silica tube of High Temperature Furnaces Heating Apparatus between 500 to 1500 DEG C of isolated air and temperature or High Temperature Furnaces Heating Apparatus, this silicon-containing compound of cracking is to form gas composition;
Transmit the steam of hydrocarbon polymer by argon gas to enter in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, the gas composition that the steam of this hydrocarbon polymer and the silicon-containing compound of above-mentioned cracking are formed is mixed to form reactant; And
In the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, make this reactant form flaky nanometer structure network on this base material by vapor deposition processes, between this flaky nanometer structure network and this base material, there is covalently bonded.
2. the preparation method of formation flaky nanometer structure network as claimed in claim 1 on base material, is characterized in that wherein above-mentioned base material comprises pottery, quartz, glass, Silicon Wafer or metal.
3. the preparation method of formation flaky nanometer structure network as claimed in claim 2 on base material, is characterized in that wherein above-mentioned metal comprises carbon steel, copper, titanium or its alloy.
4. the preparation method of formation flaky nanometer structure network as claimed in claim 2 on base material, is characterized in that wherein above-mentioned metallic surface has the coating layer of silicon-dioxide.
5. the preparation method of formation flaky nanometer structure network as claimed in claim 1 on base material, is characterized in that wherein above-mentioned silicon-containing compound is selected from following group one or a combination set of: silica gel, polydimethylsiloxane, organosilicon, Silane Grafted polymer, siliceous metallocene polymer and METHYL TRICHLORO SILANE.
6. the preparation method of formation flaky nanometer structure network as claimed in claim 1 on base material, is characterized in that wherein above-mentioned silicon-containing compound more comprises charges, gold, copper halide or metallocene compound.
7. the preparation method of formation flaky nanometer structure network as claimed in claim 1 on base material, is characterized in that wherein above-mentioned temperature is between 750 to 950 DEG C.
8. the preparation method of formation flaky nanometer structure network as claimed in claim 1 on base material, is characterized in that wherein above-mentioned hydrocarbon polymer comprises ketone, aldehydes, ester class, alkanes, alkene class or alkynes class.
9. the preparation method of formation flaky nanometer structure network as claimed in claim 8 on base material, is characterized in that wherein above-mentioned alkene class is selected from following group one or a combination set of: naphthalene, benzene,toluene,xylene and ethene.
10. the preparation method of formation flaky nanometer structure network as claimed in claim 1 on base material, is characterized in that wherein above-mentioned flaky nanometer structure network is class graphene nano sheet structural network.
11. form the preparation method of flaky nanometer structure network on base material as claimed in claim 1, it is characterized in that wherein above-mentioned covalently bonded is carbide bond.
12. form the preparation method of flaky nanometer structure network on base material as claimed in claim 11, it is characterized in that wherein above-mentioned carbide bond is selected from following group one or a combination set of: carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-nitrogen bond knot and carbon-nitrogen-metal bond.
13. 1 kinds form the preparation method of flaky nanometer structure network on base material, it is characterized in that the preparation method of this formation flaky nanometer structure network on base material comprises:
Insert base material in the silica tube of High Temperature Furnaces Heating Apparatus or High Temperature Furnaces Heating Apparatus in;
Performing heating schedule makes the temperature of the silica tube of this High Temperature Furnaces Heating Apparatus or High Temperature Furnaces Heating Apparatus reach between 500 to 1500 DEG C;
Transmit vapor composition by argon gas to enter in the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, this vapor composition is made up of hydrocarbon polymer and silicon compound; And
In the silica tube of the High Temperature Furnaces Heating Apparatus of said temperature between 500 to 1500 DEG C or High Temperature Furnaces Heating Apparatus, make this vapor composition form flaky nanometer structure network on this base material by vapor deposition processes, between this flaky nanometer structure network and this base material, there is covalently bonded.
14. form the preparation method of flaky nanometer structure network on base material as claimed in claim 13, it is characterized in that wherein above-mentioned base material comprises pottery, quartz, glass, Silicon Wafer or metal.
15. form the preparation method of flaky nanometer structure network on base material as claimed in claim 14, it is characterized in that wherein above-mentioned metal comprises carbon steel, copper, titanium or its alloy.
16. form the preparation method of flaky nanometer structure network on base material as claimed in claim 14, it is characterized in that wherein above-mentioned metallic surface has the coating layer of silicon-dioxide.
17. form the preparation method of flaky nanometer structure network on base material as claimed in claim 13, it is characterized in that wherein above-mentioned temperature is between 750 to 950 DEG C.
18. form the preparation method of flaky nanometer structure network on base material as claimed in claim 13, it is characterized in that wherein above-mentioned hydrocarbon polymer is selected from following group one or a combination set of: benzene, toluene and dimethylbenzene.
19. form the preparation method of flaky nanometer structure network on base material as claimed in claim 13, it is characterized in that wherein above-mentioned silicon compound is tetraalkyl silicon compound.
20. form the preparation method of flaky nanometer structure network on base material as claimed in claim 13, it is characterized in that wherein above-mentioned silicon compound is tetraethyl silicane compound.
21. form the preparation method of flaky nanometer structure network on base material as claimed in claim 13, it is characterized in that wherein above-mentioned silicon compound more comprises charges, gold, copper halide or metallocene compound.
22. form the preparation method of flaky nanometer structure network on base material as claimed in claim 13, it is characterized in that wherein above-mentioned flaky nanometer structure network is class graphene nano sheet structural network.
23. form the preparation method of flaky nanometer structure network on base material as claimed in claim 13, it is characterized in that wherein above-mentioned covalently bonded is carbide bond.
24. form the preparation method of flaky nanometer structure network on base material as claimed in claim 23, it is characterized in that wherein above-mentioned carbide bond is selected from one of following group and combination thereof: carbon-oxygen-silicon bound knot or carbon-silicon bond.
25. 1 kinds of surfaces have the base material of nanostructured network, and it is characterized in that this nanostructured network is fixed on this surface by carbide bond, the Raman spectrum of wherein above-mentioned nanostructured network is at 1594 ± 5cm
-1there are G broadband and 1338 ± 5cm in place
-1there is D broadband at place, and wherein above-mentioned carbide bond is selected from following group one or a combination set of: carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-nitrogen bond knot and carbon-nitrogen-metal bond.
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| JP2002538301A (en) * | 1999-03-05 | 2002-11-12 | レステック・コーポレーション | Surface modification of solid support through thermal decomposition and functionalization of silane |
| CN1735710A (en) * | 2002-12-20 | 2006-02-15 | 应用材料有限公司 | A method and apparatus for forming a high quality low temperature silicon nitride layer |
| CN102268653A (en) * | 2011-06-24 | 2011-12-07 | 北京科技大学 | Preparation method of hard alloy tool diamond interlayer |
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| US9593413B2 (en) * | 2011-05-04 | 2017-03-14 | Uchicago Argonne, Llc | Composite materials for battery applications |
| EP2744751A4 (en) * | 2011-08-15 | 2015-08-05 | Purdue Research Foundation | Methods and apparatus for the fabrication and use of graphene petal nanosheet structures |
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| JP2002538301A (en) * | 1999-03-05 | 2002-11-12 | レステック・コーポレーション | Surface modification of solid support through thermal decomposition and functionalization of silane |
| CN1735710A (en) * | 2002-12-20 | 2006-02-15 | 应用材料有限公司 | A method and apparatus for forming a high quality low temperature silicon nitride layer |
| CN102268653A (en) * | 2011-06-24 | 2011-12-07 | 北京科技大学 | Preparation method of hard alloy tool diamond interlayer |
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Granted publication date: 20180619 Termination date: 20200925 |
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| CF01 | Termination of patent right due to non-payment of annual fee |