CN105274489B - 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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- CN105274489B CN105274489B CN201410498442.3A CN201410498442A CN105274489B CN 105274489 B CN105274489 B CN 105274489B CN 201410498442 A CN201410498442 A CN 201410498442A CN 105274489 B CN105274489 B CN 105274489B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 56
- 239000002135 nanosheet Substances 0.000 title claims abstract description 39
- 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 104
- 239000010453 quartz Substances 0.000 claims abstract description 77
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 32
- 239000002210 silicon-based material Substances 0.000 claims abstract description 24
- 229910052786 argon Inorganic materials 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 16
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 16
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 16
- 238000005019 vapor deposition process Methods 0.000 claims abstract description 14
- 239000000376 reactant Substances 0.000 claims abstract description 8
- 238000005336 cracking Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 110
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 79
- 229910021389 graphene Inorganic materials 0.000 claims description 56
- 229910052751 metal Inorganic materials 0.000 claims description 39
- 239000003708 ampul Substances 0.000 claims description 38
- 239000002184 metal Substances 0.000 claims description 34
- 230000015572 biosynthetic process Effects 0.000 claims description 33
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- 229910052710 silicon Inorganic materials 0.000 claims description 22
- 239000010703 silicon Substances 0.000 claims description 22
- 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 16
- 150000001336 alkenes Chemical class 0.000 claims description 14
- 239000000919 ceramic Substances 0.000 claims description 12
- 229910052802 copper Inorganic materials 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 10
- -1 polydimethylsiloxane Polymers 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 7
- 229920002521 macromolecule Polymers 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 5
- 239000010962 carbon steel Substances 0.000 claims description 5
- 239000011247 coating layer Substances 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 238000002955 isolation Methods 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 150000001299 aldehydes Chemical class 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 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
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 239000002064 nanoplatelet Substances 0.000 abstract 2
- 238000000034 method Methods 0.000 description 36
- 229910052799 carbon Inorganic materials 0.000 description 24
- 238000005229 chemical vapour deposition Methods 0.000 description 22
- 238000001237 Raman spectrum Methods 0.000 description 15
- 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
- 229910052814 silicon oxide Inorganic materials 0.000 description 12
- 239000004575 stone Substances 0.000 description 10
- 239000010410 layer Substances 0.000 description 8
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- 150000003377 silicon compounds Chemical class 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 238000003763 carbonization Methods 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
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- 238000001069 Raman spectroscopy Methods 0.000 description 4
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- 150000002739 metals Chemical class 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910021332 silicide Inorganic materials 0.000 description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
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- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
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- 125000001339 silanediyl group Chemical group [H][Si]([H])(*)* 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
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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 present invention relates to a kind of formation flaky nanometer structure network preparation method on base material, especially with regard to one kind
Forming flaky nanometer structure network method on base material and surface by vapor deposition processes has flaky nanometer structure network
Base material application.The carbide covalently bonded for having bond intensity high between the flaky nanometer structure network and base material.Secondly,
The flaky nanometer structure network is class graphene nano sheet structural network, so with good corrosion resistance, low friction system
Several, good thermal conductivity and Effective Conductivity and optical property.Furthermore the property that should have the base material of flaky nanometer structure network can
Regulate and control by gas phase composition used in vapor deposition processes is changed, reach the mesh in various industries using the base material whereby
's.
Background technology
The allotrope (allotropes) of carbon includes fullerene, carbon nanotubes, graphene, graphite and diamond,
Wherein graphene is especially paid attention to by researcher when with unique two-dimensional structure.Graphene is arranged by carbon atom
The flaky nanometer structure that formed shape is hexangle type and thickness is an atom, since this unique two-dimensional structure leads to graphene
With outstanding electrical conductance (8x 105S/m), high heat conduction property (about 5300W m-1K-1), excellent mechanical strength
(tensile strength of 130GPa and Young ' s modulus of 1TPa), low-friction coefficient and good anti-
Corrosion matter.
Generally using known techniques prepare graphene be using graphite as raw material, sequentially through peroxidating intercalation, dial from reduction journey
Sequence and obtain graphene.In high molecular material usually the modification of high molecular material is carried out by addition graphene.It is however, right
For ceramics, glass, metal and semi-conducting material, since the operation temperature of the materials such as above-mentioned ceramics is typically larger than 400 DEG C, but
It is that graphene is poor in 400 DEG C or more of stable at high temperature, structure is more easily damaged, therefore in practical industry using upper, use
The mode of addition graphene can not simultaneously obtain expected effect to carry out the modification of ceramics, glass, metal and semi-conducting material etc..
On the other hand, though graphene coating can be fixed on ceramics, glass, metal and semiconductor material by mode then
The surface of material etc., but graphene surface is very inert, so graphene layer is easy to from the surface of above-mentioned ceramic material
Stripping.And for being coated with the usual non-refractory of fixed solid.It is original excellent also to reduce change graphene for solid simultaneously
Heterogeneity.Therefore, such mode is not particularly suited for ceramics, glass, metal and semi-conducting material etc..
Yuegang Zhang et al. are disclosed in Nano Lett.2010,10,1542-1548 and a kind of are deposited graphene
Method on the dielectric material；This method is that the film being made of copper is previously deposited on the surface of dielectric material, secondly
The structure of graphene is formed on the above-mentioned film being made of copper by vapour deposition process again, it is thin finally to remove this
Film and obtain surface have graphene-structured dielectric material.Thus between the obtained graphene-structured of method and dielectric material
There is no the presence of covalently bonded.Therefore, the stability of high temperature is poor, and manufacturing method is cumbersome, can not be in direct on material surface
Form graphene laminated structure.
The method that 20110070146 A1 of U.S. Patent Publication case US disclose another manufacture graphene；This method packet
Contain：Hydrophily oxide layer is initially formed on base material；Secondly, hydrophobic metals catalyst layer is re-formed in the hydrophily oxide layer,
Then in forming graphene-structured on the hydrophobic metals catalyst layer；Finally, the hydrophobic metals catalyst layer is detached to be had
There is the base material of graphene-structured.In this method, manufacturing step is considerably complicated, and needs to remove metal solvent with etching program
Layer, this etching program can generate a large amount of acid waste liquids, therefore the manufacturing method is for environmental protection and unfriendly, and the manufacturer
Method equally directly can not form graphene laminated structure in material surface.
In conclusion graphene nano sheet is formed on the substrate surface of ceramics, glass, metal and semi-conducting material etc.
The process technique of structural network is that there is an urgent need for research and developments and the subject broken through for current industrial circle.
Invention content
In view of above-mentioned background of invention, in order to meet the demand in industry, the purpose of the present invention is to provide a kind of formation
Flaky nanometer structure network preparation method on base material and surface have the base material of flaky nanometer structure network, current to solve
Problem encountered in industry, while promote the technology of the surfaction of ceramics, metal and semi-conducting material etc..
The purpose of the present invention is what is realized using following technical scheme.The present invention provides a kind of formation flaky nanometer structure
Network preparation method on base material, this method comprise the steps of：Base material and silicon-containing compound are provided；In isolation air and temperature
Degree cracks the silicon-containing compound in the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace and is formed with forming gas；
Enter the stone of high temperature furnace or high temperature furnace of the above-mentioned temperature between 500 to 1500 DEG C by the steam of argon gas transmission hydrocarbon
The gas composition that the silicon-containing compound of Ying Guanzhong, the steam of the hydrocarbon and above-mentioned cracking is formed is mixed to form reaction
Object；And make in the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace by vapor deposition processes in above-mentioned temperature
The reactant forms flaky nanometer structure network on the base material, has altogether between the flaky nanometer structure network and the base material
Valence link knot.
The purpose of the present invention also can be used following technical measures and further realize.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned base material include ceramics,
Quartz, glass, Silicon Wafer or metal.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned metal include carbon steel,
Copper, titanium or its alloy.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned metallic surface has
The coating layer of silica.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned silicon-containing compound is selected from
One or a combination set of following group：Silica gel, polydimethylsiloxane, organosilicon, Silane Grafted macromolecule, siliceous metallocene macromolecule
And methyl trichlorosilane.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned silicon-containing compound more wraps
Containing charges, gold, copper halide or metallocene compound.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned temperature is 750 to 950
Between DEG C.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned hydrocarbon includes
Ketone, aldehydes, esters, alkanes, alkenes or acetylenic.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned alkenes are selected from following group
One or a combination set of group：Naphthalene, benzene,toluene,xylene and ethylene.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned flaky nanometer structure net
Network is class graphene nano sheet structural network.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned covalently bonded is carbonization
Object is bonded.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned carbide bond is selected from
One or a combination set of following group：Carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-to-nitrogen
Bond and carbon-to-nitrogen-metal bond.
What the purpose of the present invention was also realized using following technical scheme.The present invention provides another formation nano-sheet knot
Network forming network preparation method on base material, this method comprise the steps of：Base material is placed in high temperature furnace or the quartz ampoule of high temperature furnace
In interior；Performing temperature program makes the temperature of the quartz ampoule of the high temperature furnace or high temperature furnace reach between 500 to 1500 DEG C；By argon gas
Transmit vapor composition enter above-mentioned temperature in the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace, the steam into
Divide and be made of hydrocarbon and silicon compound；And high temperature furnace or high temperature furnace in above-mentioned temperature between 500 to 1500 DEG C
Quartz ampoule in, by vapor deposition processes make the vapor composition formed flaky nanometer structure network on the base material, this is received
There is covalently bonded between rice laminated structure network and the base material.
The purpose of the present invention also can be used following technical measures and further realize.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned base material include ceramics,
Quartz, glass, Silicon Wafer or metal.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned metal include carbon steel,
Copper, titanium or its alloy.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned metallic surface has
The coating layer of silica.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned temperature is 750 to 950
Between DEG C.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned hydrocarbon is selected from
One or a combination set of following group：Benzene, toluene and dimethylbenzene.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned silicon compound is four alkane
Radical silicide.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned silicon compound is tetrem
Radical silicide.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned silicon compound further includes
Charges, gold, copper halide or metallocene compound.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned flaky nanometer structure net
Network is class graphene nano sheet structural network.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned covalently bonded is carbonization
Object is bonded.
Aforementioned formation flaky nanometer structure network preparation method on base material, wherein above-mentioned carbide bond is selected from
One of following group and combinations thereof：Carbon-oxygen-silicon bound knot or carbon-silicon bond.
What the purpose of the present invention was realized again using following technical scheme.The present invention, which provides a kind of surface, has nanostructured
The base material of network, the nanostructured network are fixed on the surface by carbide bond.The Raman of above-mentioned nanostructured network
Spectrum is in 1594 ± 5cm-1There are G broadbands and 1338 ± 5cm in place-1There are D broadbands at place, due to the Raman spectrum of the nanostructured network
Very similar to the Raman spectrum of graphene nano sheet structure, so the nanostructured network is class graphene nano sheet structure
Network has the similar quality of graphene-structured, such as outstanding electrical conductance, high heat conduction property, excellent mechanical strength, low friction
Coefficient and good corrosion protection property；Meanwhile the nanostructured network is fixed on carbide bond on substrate surface again, it is above-mentioned
Carbide bond is selected from one or a combination set of following group：Carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-
Metal bond, carbon-to-nitrogen bond and carbon-to-nitrogen-metal bond.Therefore, the peace of the base material on the surface with above-mentioned nanostructured network
It is qualitative excellent, Different Industries field can be widely used in.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And it can be implemented in accordance with the contents of the specification, and in order to allow the above and other objects, features and advantages of the present invention can
It is clearer and more comprehensible, special below to lift preferred embodiment, and coordinate attached drawing, detailed description are as follows.
Description of the drawings
Fig. 1 (a) is the photograph of quartz plate；Fig. 1 (b) is to be prepared into surface using naphthalene as carbon source and with chemical vapour deposition technique
The photograph of quartz plate with class graphene nano sheet structural network.
Fig. 2 is the comparison figure of the class graphene nano sheet structural network of scanning electron microscope.
Fig. 3 (a) is the Raman spectrum of quartz；Fig. 3 (b) is the Raman spectrum of commercialized graphene；Fig. 3 (c) is quartz
Surface is with the Raman spectrum of class graphene nano sheet structural network and the structural network with carbonization key；Fig. 3 (d) is quartz
Surface is with the Raman spectrum of class graphene nano sheet structural network but the structural network not with carbonization key.
Fig. 4 (a) is the photograph of Silicon Wafer；Fig. 4 (b) is to be prepared into surface using naphthalene as carbon source and with chemical vapour deposition technique
The photograph of Silicon Wafer with class graphene nano sheet structural network.
Fig. 5 is to be prepared into surface with class graphene nano sheet structure using benzene as carbon source and with chemical vapour deposition technique
The photograph of the quartz plate of network.
Fig. 6 is to be prepared into surface with class graphene nano sheet knot using ethylene as carbon source and with chemical vapour deposition technique
The photograph of the quartz plate of network forming network.
Specific embodiment
The technological means and effect taken further to illustrate the present invention to reach predetermined goal of the invention, below in conjunction with
Attached drawing and preferred embodiment, to a kind of formation flaky nanometer structure network preparation method on base material proposed according to the present invention
And its specific embodiment, structure, feature and its effect of base material, it is described in detail as after.
What the present invention was inquired at this is a kind of formation flaky nanometer structure network preparation method on base material and surface
Base material with flaky nanometer structure network.In order to thoroughly understand the present invention, will be proposed in following description detailed
Raw material, step and application.It is apparent that the execution of the present invention is not limited to the specific details that the those skilled in the art in the field is familiar with.
On the other hand, well-known raw material or step are not described in details, to avoid the unnecessary limitation of the present invention is caused.This
The example of invention will be described in detail it is as follows, however in addition to these detailed description other than, the present invention can also widely be implemented in it
In his example, and the scope of the present invention is not limited, the scope of the claims being subject to later.
According to the first embodiment of the invention, it is on base material to provide a kind of formation flaky nanometer structure network by the present invention
Preparation method, this method comprise the steps of：Base material and silicon-containing compound are provided；In isolation air and temperature 500 to 1500
High temperature furnace between DEG C cracks the silicon-containing compound and is formed with forming gas in the quartz ampoule of high temperature furnace；Carbon is transmitted by argon gas
The steam of hydrogen compound enters above-mentioned temperature in the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace, this is hydrocarbon
The gas composition that the steam of compound and the silicon-containing compound of above-mentioned cracking are formed is mixed to form reactant；With in above-mentioned temperature
In the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace, reactant formation is made to receive by vapor deposition processes
Rice laminated structure network has covalently bonded on the base material between the flaky nanometer structure network and the base material.
In an embodiment, the base material includes ceramics, quartz, glass, Silicon Wafer or metal.
In another embodiment, the metal includes carbon steel, copper, titanium or its alloy.
In order to which vapor deposition processes is made to reach preferable effect on metal base, the surface of metal base usually all can be into
Row coating modification.
In an embodiment, metallic surface has the coating layer of silica.
In order to reach the purpose between flaky nanometer structure network and base material with covalently bonded, silicon-containing compound or contain
Nitrogen compound is necessary raw material in preparation method provided by the present invention.
In an embodiment, silicon-containing compound is selected from one or a combination set of following group：It is silica gel, polydimethylsiloxane, organic
Silicon, Silane Grafted macromolecule, siliceous metallocene macromolecule and methyl trichlorosilane.
In another embodiment, silicon-containing compound further includes charges, gold, copper halide or metallocene compound.
In an embodiment, nitrogenous compound is selected from one or a combination set of following group：Polypropylene is fine
(polyacrylonitrile), cyano macromolecule, nitrogen heterocyclic ring family macromolecule.
It is in the preparation method step：Completely cut off the high temperature furnace or high temperature of air and temperature between 500 to 1500 DEG C
The silicon-containing compound is cracked in the quartz ampoule of stove to form to form gas.
In a preferred embodiment, above-mentioned temperature is between 750 to 950 DEG C.
In an embodiment, by the environment for being continually fed into argon gas and creating isolation air.
It is in the preparation method step：Steam by argon gas transmission hydrocarbon enters above-mentioned temperature 500
High temperature furnace between to 1500 DEG C or in the quartz ampoule of high temperature furnace, the siliceous chemical combination of the steam of the hydrocarbon and above-mentioned cracking
The gas composition that object is formed is mixed to form reactant；And high temperature furnace or high temperature in above-mentioned temperature between 500 to 1500 DEG C
In the quartz ampoule of stove, the reactant is made to form flaky nanometer structure network on the base material by vapor deposition processes, this is received
There is covalently bonded between rice laminated structure network and the base material.
In an embodiment, the hydrocarbon as carbon source needed for vapor deposition processes includes ketone, aldehydes, esters, alkane
Class, alkenes or acetylenic.
In another embodiment, above-mentioned alkenes are selected from one or a combination set of following group：Naphthalene, benzene,toluene,xylene and second
Alkene.
In order to achieve the purpose that there is covalently bonded, the operation temperature of preparation method between flaky nanometer structure network and base material
Degree needs to control between 500 to 1500 DEG C.
In a preferred embodiment, above-mentioned temperature is between 750 to 950 DEG C.
The flaky nanometer structure network formed according to preparation method provided by the present invention is class graphene nano sheet
Structural network.
The covalently bonded having between above-mentioned flaky nanometer structure network and base material is carbide covalently bonded.
In an embodiment, the carbide covalently bonded is selected from one or a combination set of following group：Carbon-oxygen-silicon bound knot,
Carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-to-nitrogen bond and carbon-to-nitrogen-metal bond.
Second embodiment of the invention, the present invention provides another flaky nanometer structure network that formed on base material
Preparation method, this method comprises the steps of:Base material is placed in in the quartz ampoule of high temperature furnace or high temperature furnace；Perform heating journey
Sequence makes the temperature of the quartz ampoule of the high temperature furnace or high temperature furnace reach between 500 to 1500 DEG C；By argon gas transmit vapor composition into
Enter above-mentioned temperature in the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace, which is by nytron
Object and silicon compound are formed；And it is borrowed in the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace in above-mentioned temperature
The vapor composition is made to form flaky nanometer structure network on the base material by vapor deposition processes, the flaky nanometer structure network
There is covalently bonded between the base material.
In an embodiment, the base material includes ceramics, quartz, glass, Silicon Wafer or metal.
In another embodiment, the metal includes carbon steel, copper, titanium or its alloy.
In order to which vapor deposition processes is made to reach preferable effect on metal base, the surface of metal base usually all can be into
Row coating modification.
In an embodiment, metallic surface has the coating layer of silica.
It is in the preparation method step：Performing temperature program reaches the temperature of the quartz ampoule of the high temperature furnace or high temperature furnace
To between 500 to 1500 DEG C；By argon gas transmission vapor composition enter high temperature furnace of the above-mentioned temperature between 500 to 1500 DEG C or
In the quartz ampoule of high temperature furnace, which is made of hydrocarbon and silicon compound；With above-mentioned temperature 500 to
High temperature furnace between 1500 DEG C or in the quartz ampoule of high temperature furnace, makes the vapor composition form nano-sheet by vapor deposition processes
Structural network has covalently bonded on the base material between the flaky nanometer structure and the base material.
In order to achieve the purpose that there is covalently bonded, the operation temperature of preparation method between flaky nanometer structure network and base material
Degree needs to control between 500 to 1500 DEG C.
In a preferred embodiment, above-mentioned operation temperature is between 750 to 950 DEG C.
In an embodiment, by the environment for being continually fed into argon gas and creating isolation air.
In an embodiment, the hydrocarbon as carbon source needed for vapor deposition processes is selected from one of following group or its group
It closes：Benzene, toluene and dimethylbenzene.
In another embodiment, in order to reach the purpose between flaky nanometer structure network and base material with covalently bonded, contain
Silicon compound is tetraalkyl silicon compound.
In a preferred embodiment, silicon-containing compound is silicon tetraethyl compound.
In another embodiment, silicon-containing compound further includes charges, gold, copper halide or metallocene compound.
The flaky nanometer structure network formed according to preparation method provided by the present invention is class graphene nano sheet
Structural network.
The covalently bonded having between above-mentioned flaky nanometer structure network and base material is carbide covalently bonded.
In an embodiment, the carbide covalently bonded is selected from one or a combination set of following group：Carbon-oxygen-silicon bound knot
With carbon-silicon bond.
The formation nano-sheet knot that third embodiment of the present invention is provided by above-mentioned first or second embodiment
Network forming network preparation method on base material, which further provides for surface, has the base material of nanostructured network, which is
It is fixed in the substrate surface that (carbide bond) is bonded by carbide.The Raman spectrum of wherein above-mentioned nanostructured network
In 1594 ± 5cm-1There are G broadbands and 1338 ± 5cm in place-1There are D broadbands at place.
In an embodiment, above-mentioned carbide is bonded (carbide bond) selected from one or a combination set of following group：Carbon-
Oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal bond, carbon-metal bond, carbon-to-nitrogen bond and carbon-to-nitrogen-metal bond.
Since the Raman spectrum of above-mentioned nanostructured network is very similar to the Raman light of graphene nano sheet structure
Spectrum so the nanostructured network is class graphene nano sheet structural network, has and is similar to graphene nano sheet structure
The property of network, such as outstanding electrical conductance, high heat conduction property, excellent mechanical strength, low-friction coefficient and good corrosion protection
Matter；Meanwhile the nanostructured network is bonded (carbide bond) with carbide again and is fixed on substrate surface, therefore, has
The stability of the base material on the surface of above-mentioned nanostructured network is excellent, can be widely used in Different Industries.
In an embodiment, above-mentioned surface has the component composition that the base material of nanostructured network is used as solar cell.
In an embodiment, above-mentioned surface has the component composition that the base material of nanostructured network is used as semiconductor.
In an embodiment, above-mentioned surface has the component composition that the base material of nanostructured network is used as optical module.
In an embodiment, above-mentioned surface has the component composition that the base material of nanostructured network is used as anticorrosion material.
In an embodiment, above-mentioned surface has the composition that the base material of nanostructured network is used as non-stick cooker.
In an embodiment, above-mentioned surface has the component composition that the base material of nanostructured network is used as radiating module.
The present invention is illustrated further following with example, the implementation state of the present invention is merely illustrative of herein, is familiar with
This technology person can carry out various equivalent changes or modification, but the scope of the present invention is with aftermentioned according to these embodiments and example
Request range on the basis of, be not limited to these embodiments and example.
One, of example prepares a kind of surface with chemical vapour deposition technique has the class stone of silicon carbide (silicon oxide carbide) covalently bonded
The quartz plate of black alkene flaky nanometer structure network.
Class graphene-structured is formed using solid naphthalene (purity 99% is purchased to Aldrich) as chemical vapour deposition technique to exist
Carbon source on base material.First, it is quartz plate and silicon-containing compound that 1/16 inch of size is 1 inch of 1 inch of x by two panels thickness
(1 gram) is put into the quartz ampoule of high temperature furnace, is passed through argon gas after ten minutes, heats the quartz ampoule of high temperature furnace to 750 DEG C of temperature.With argon
The steam of gas transmission naphthalene enters quartz ampoule of the temperature at 750 DEG C, carries out chemical vapour deposition procedure after 50 minutes, cools down quartz ampoule
Quartz plate is taken out after returning to room temperature.Fig. 1 (a) is the photograph of quartz plate；Fig. 1 (b) is as carbon source and with chemical vapor deposition using naphthalene
Area method is prepared into the quartz plate of class graphene nano sheet structural network of the surface with silicon carbide (silicon oxide carbide) covalently bonded.
When quartz ampoule temperature reaches 500 DEG C or more, silicon-containing compound can occur thermal cracking and generate including Si (CH3)-
OH、H2Si(CH3)2、CH4, CO and O2Gas, above-mentioned gas can be with class graphene nano sheet structural network edge
Carbon atom reacts to form silicon carbide covalently bonded and silicon oxide carbide covalently bonded.Because quartz plate is mainly by silicon, carbon, oxygen and nitrogen etc.
Element is formed, so when quartz plate is at 750 DEG C or more, this temperature condition can make quartz plate and class graphene nano sheet
Silicon carbide covalently bonded and silicon oxide carbide covalently bonded are generated between structural network.
Class graphene nano sheet structural network figures of the Fig. 2 for scanning electron microscope, class graphene nano sheet
The thickness of structural network is about 3 μm.
Surface prepared by above-mentioned example one has the stone of the class graphene nano sheet structural network of silicon carbide covalently bonded
English plate, the resistance of the quartz plate is about in 12-24K Ω；In addition, the class graphene-structured network layer of the quartz plate surface can not be with strong
Acid or other physics strength remove, and when temperature is at 450 DEG C the quartz plate surface class graphene nano sheet Structure Network
Network layers still have good thermal stability.Its Young ' s modulus (Young's modulus) is further analyzed as 170GPa with AFM,
And Hertzian hardness (hardness of hertz) are 22.5GPa.
Since Raman spectrum is very sensitive for the electronic structure variation of carbon material, with Raman spectrum analysis stone
Black alkene and associated carbon element material can obtain highly useful information；Raman spectrum analysis instrument is used in this experimental analysis
Renishaw 1000microspectrometer, the wavelength used are 514.5nm.Fig. 3 (a) show the Raman light of quartz
Spectrum, as experimental comparison group；Fig. 3 (b) is the Raman spectrum of graphene commercially produced, which is by graphene oxide
It restores and is made, Raman spectrum is shown in 1586cm-1There are G broadbands (G band) and 1348cm-1There are D broadbands (D band), and
In 2703cm-1There are 2D broadbands, in addition in 2934cm-1There is the combination broadband of D+G.Fig. 3 (c) has class graphene for quartz surfaces
Flaky nanometer structure network and the structural network have the Raman spectrum of carbonization key.Fig. 3 (d) has class graphene for quartz surfaces
Flaky nanometer structure network but the structural network do not have the Raman spectrum of carbonization key, can clear view by Fig. 3 (c) and Fig. 3 (d)
To the presence of G broadbands (G band) and D broadbands (D band), and also there is the combination broadband of broad D+G, this Raman light simultaneously
Spectrum proves that the quartz surfaces have class graphene nano sheet structural network really.
Example two prepares a kind of class stone of surface with silicon carbide (silicon oxide carbide) covalently bonded with chemical vapour deposition technique
The Silicon Wafer of black alkene flaky nanometer structure network.
For preparation method as described in example one, base material is changed to Silicon Wafer by quartz plate, finally obtains surface with silicon carbide (carbon
Silica) covalently bonded class graphene nano sheet structural network Silicon Wafer, shown in finished product such as Fig. 4 (b), i.e., Fig. 4 (a) is
The photograph of Silicon Wafer；Fig. 4 (b) is to be prepared into surface with class graphene nano using naphthalene as carbon source and with chemical vapour deposition technique
The photograph of the Silicon Wafer of laminated structure network..
Example three prepares a kind of class stone of surface with silicon carbide (silicon oxide carbide) covalently bonded with chemical vapour deposition technique
The quartz plate of black alkene flaky nanometer structure network.
Class graphene-structured is formed in base as chemical vapour deposition technique using benzene (purity 99.9% is purchased to Aldrich)
Carbon source on material.First, it is that the quartz plate that 1/16 inch of size is 1 inch of 3 inches of x is put into the stone of high temperature furnace by two panels thickness
Ying Guanzhong is passed through argon gas after ten minutes, heats the quartz ampoule of high temperature furnace to 950 DEG C of temperature.Benzene and tetramethylsilane are transmitted with argon gas
The steam of compound (Tetramethylorthosilicate) enters quartz ampoule of the temperature at 950 DEG C, carries out chemical vapor deposition
After sixty minutes, cooling quartz ampoule takes out quartz plate to product program after returning to room temperature.It obtains using benzene as carbon source and with chemical gaseous phase
Sedimentation is prepared into the quartz of class graphene nano sheet structural network of the surface with silicon carbide (silicon oxide carbide) covalently bonded
Plate, finished product are as shown in Figure 5.
Example four prepares a kind of class stone of surface with silicon carbide (silicon oxide carbide) covalently bonded with chemical vapour deposition technique
The quartz plate of black alkene flaky nanometer structure network.
Class graphene-structured carbon source on base material is formed using ethylene (purity 99.5%) as chemical vapour deposition technique.
First, it is that quartz plate that 1/8 inch of size is 1 inch of 1 inch of x and silicon-containing compound (1 gram) are put into high temperature furnace by two panels thickness
Quartz ampoule in, be passed through argon gas after ten minutes, heat the quartz ampoule of high temperature furnace to 950 DEG C of temperature.Ethylene gas is transmitted with argon gas
Enter quartz ampoule of the temperature at 950 DEG C together, carry out chemical vapour deposition procedure after 50 minutes, after cooling quartz ampoule returns to room temperature
Take out quartz plate.It is i.e. available to be prepared into surface with silicon carbide (carbon oxygen using ethylene as carbon source and with chemical vapour deposition technique
SiClx) covalently bonded class graphene nano sheet structural network quartz plate.Finished product is as shown in Figure 6.
Example five prepares a kind of class stone of surface with silicon carbide (silicon oxide carbide) covalently bonded with chemical vapour deposition technique
The steel plate of black alkene flaky nanometer structure network.
Preparation method is as described in example one, and base material is changed to by quartz plate through the processed steel plate of silica-coating, finally
Obtain the steel plate of class graphene nano sheet structural network of the surface with silicon carbide (silicon oxide carbide) covalently bonded.
Example six prepares a kind of class stone of surface with silicon carbide (silicon oxide carbide) covalently bonded with chemical vapour deposition technique
The steel plate of black alkene flaky nanometer structure network.
Class graphene-structured is formed using toluene (purity 99.8% is purchased to Aldrich) as chemical vapour deposition technique to exist
Carbon source on base material.First, two panels is put into through the processed steel plate of silica-coating in the quartz ampoule of high temperature furnace, is passed through argon
Gas after ten minutes, heats the quartz ampoule of high temperature furnace to 850 DEG C of temperature.Toluene and silicon tetraethyl compound are transmitted with argon gas
(Tetraethylorthosilicate) steam enters quartz ampoule of the temperature at 850 DEG C, carries out chemical vapour deposition procedure 60
After minute, cooling quartz ampoule takes out quartz plate after returning to room temperature.It obtains using toluene as carbon source and with chemical vapour deposition technique
It is prepared into the steel plate of class graphene nano sheet structural network of the surface with silicon carbide (silicon oxide carbide) covalently bonded.
The above described is only a preferred embodiment of the present invention, not make limitation in any form to the present invention, though
So the present invention is disclosed above with preferred embodiment, however is not limited to the present invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, technical spirit according to the present invention
To any simple modification, equivalent change and modification that above example is made, in the range of still falling within technical solution of the present invention.
Claims (11)
- A kind of 1. formation flaky nanometer structure network preparation method on base material, it is characterised in that the formation flaky nanometer structure Network preparation method on base material includes:Base material and silicon-containing compound are provided；The siliceous chemical combination is cracked in the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace in isolation air and temperature Object is formed with forming gas；Steam by argon gas transmission hydrocarbon enters high temperature furnace or high temperature furnace of the above-mentioned temperature between 500 to 1500 DEG C Quartz ampoule in, gas composition that the silicon-containing compound of the steam of the hydrocarbon and above-mentioned cracking is formed is mixed to form anti- Answer object；AndIn above-mentioned temperature in the high temperature furnace between 500 to 1500 DEG C or the quartz ampoule of high temperature furnace, make by vapor deposition processes The reactant forms flaky nanometer structure network on the base material, has altogether between the flaky nanometer structure network and the base material Valence link knot, and above-mentioned flaky nanometer structure network is class graphene nano sheet structural network.
- 2. flaky nanometer structure network preparation method on base material is formed as described in claim 1, it is characterised in that wherein Above-mentioned base material includes ceramics, quartz, glass, Silicon Wafer or metal.
- 3. flaky nanometer structure network preparation method on base material is formed as claimed in claim 2, it is characterised in that wherein Above-mentioned metal includes carbon steel, copper, titanium or its alloy.
- 4. flaky nanometer structure network preparation method on base material is formed as claimed in claim 2, it is characterised in that wherein Above-mentioned metallic surface has the coating layer of silica.
- 5. flaky nanometer structure network preparation method on base material is formed as described in claim 1, it is characterised in that wherein Above-mentioned silicon-containing compound is selected from one or a combination set of following group：Silica gel, polydimethylsiloxane, organosilicon, Silane Grafted are high Molecule, siliceous metallocene macromolecule and methyl trichlorosilane.
- 6. flaky nanometer structure network preparation method on base material is formed as described in claim 1, it is characterised in that wherein Above-mentioned silicon-containing compound further includes charges, gold, copper halide or metallocene compound.
- 7. flaky nanometer structure network preparation method on base material is formed as described in claim 1, it is characterised in that wherein Above-mentioned temperature is between 750 to 950 DEG C.
- 8. flaky nanometer structure network preparation method on base material is formed as described in claim 1, it is characterised in that wherein Above-mentioned hydrocarbon includes ketone, aldehydes, esters, alkanes, alkenes or acetylenic.
- 9. flaky nanometer structure network preparation method on base material is formed as claimed in claim 8, it is characterised in that wherein Above-mentioned alkenes are selected from one or a combination set of following group：Naphthalene, benzene,toluene,xylene and ethylene.
- 10. flaky nanometer structure network preparation method on base material is formed as described in claim 1, it is characterised in that wherein Above-mentioned covalently bonded is carbide bond.
- 11. flaky nanometer structure network preparation method on base material is formed as claimed in claim 10, it is characterised in that its In above-mentioned carbide bond selected from one or a combination set of following group：Carbon-oxygen-silicon bound knot, carbon-silicon bond, carbon-oxygen-metal Bond, carbon-metal bond, carbon-to-nitrogen bond and carbon-to-nitrogen-metal bond.
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