CN105717724A - Application of super graphene glass - Google Patents
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- CN105717724A CN105717724A CN201410725858.4A CN201410725858A CN105717724A CN 105717724 A CN105717724 A CN 105717724A CN 201410725858 A CN201410725858 A CN 201410725858A CN 105717724 A CN105717724 A CN 105717724A
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Abstract
The invention discloses application of super graphene glass. The application of super graphene glass refers to the application in preparation of conductive devices, or conductive devices containing the super graphene glass. The conductive devices may be transparent circuit boards, bottom plates of resistance-type touch screens, electrical heating elements or electrochromic electrode elements. Each performance index of the super graphene glass can vary in a relatively large range, the light transmissivity of the super graphene glass (wave length being 55nm) can vary from about 10% to 97%, and the surface resistivity can vary from 80 omega/sq to 20 k omega/sq. The super graphene glass has simple structure, low cost, relatively excellent performance, and wide application rang, and is applicable to transparent printed circuit base boards, bottom plates of resistance-type touch screens, heating parts of electrical heaters, or the like.
Description
Technical field
The invention belongs to Material Field, relate to the application of a kind of superior graphite alkene glass.
Background technology
Graphene is a kind of material with carbon element emerging in recent years, there is extremely excellent character, including high mechanical strength, high carrier mobility, significantly high light transmission rate, chemical stability, heat conductivity etc., Nobel Prize in physics in 2010 is won in the discovery of its performance.Due to the character that these are outstanding, Graphene electronics device, transparent conductive film, etc. many fields have extensive and important application prospect, be increasingly subject to people's attention.
Glass is a kind of ancient and apply extremely wide material.It is of a great variety, and cost is generally extremely cheap.As a kind of transparent material coming into and being known most in popular life, it also has better mechanical property concurrently, is prone to the outstanding qualities such as processing.But it is a kind of insulant, does not have electric conductivity, thus obtains more and more wide variety of today at electric power, the application of glass receives a definite limitation.Therefore, combine glass with the advantage of Graphene to be formed with low cost, be prone to processing, mechanical performance is outstanding, have the transparency new material with electric conductivity concurrently, is one of the emphasis of association area research.
Existing general graphene conductive method for glass preparation includes: 1) graphene film prepared by chemical vapour deposition technique is covered on the glass substrate by the method shifted.The flatness of base material is had higher requirements by the method, complex steps, thus high expensive, also cannot obtain the electro-conductive glass on rough surface (such as clouded glass surface).2) solution adopting powder body Graphene or reduction graphite oxide is coated with on the glass substrate.Used by the method, Graphene performance is generally poor, and electrical conductivity is relatively low, is difficult to meet requirement for some occasions, also cannot avoid loaded down with trivial details solution phase processor process simultaneously.
Summary of the invention
It is an object of the invention to provide the application of a kind of superior graphite alkene glass (namely Graphene glass).
The application of superior graphite alkene glass provided by the invention, for the application in preparing conductive devices of the superior graphite alkene glass and the conductive devices containing superior graphite alkene glass.
Wherein, described conductive devices is transparent circuit board, the base plate of resistive touch screen, electrical heating elements or electrochromic electrode element.
Above-mentioned superior graphite alkene glass is made up of glass and the Graphene being positioned in described substrate of glass as substrate；And described Graphene is positioned at the one or both sides of described substrate of glass.
In above-mentioned superior graphite alkene glass, described glass at least one in white glass, smalt, green glass, brown glass, quartz glass, sapphire glass, blue cobalt glass, ito glass, FTO glass, AZO glass, soda-lime glass, Pyrex, flexible micarex, borate glass and phosphate glass；
Wherein, the thickness of described white glass, smalt, green glass, brown glass and quartz glass is 1mm-10mm, is specially 4mm；
The thickness of described Graphene is 1-100 atomic layer.
Described superior graphite alkene glass is alternatively the product obtained according to the preparation of following method provided by the invention.
Described Graphene glass is obtain according to the method preparation comprised the steps:
With foregoing glass for substrate, in chemical gas-phase deposition system, pass into carbon source and carry out chemical vapour deposition (CVD), deposit and complete be cooled to room temperature, obtain described superior graphite alkene glass.
The method uses the method for direct growth to be prepared, it is thus possible to avoid the impurity such as the introduced water layer of common transfer method or polymeric membrane residue.
Said method also comprises the steps:, before described chemical vapor deposition step, to be carried out drying by described substrate；
In described cleaning step, abluent used is specially ultra-pure water, isopropanol and acetone；The method cleaned is specially ultrasonic cleaning；Ultrasonic power is specially 70-90W, more specifically 80W；
Described cleaning-drying more specifically comprises the steps: with ultra-pure water, isopropanol, acetone and ultra-pure water, described substrate is respectively cleaned 3-5min successively, then dries up with nitrogen.
In described chemical vapor deposition step, carbon source at least one in methane and ethylene；
Depositing temperature is 400 DEG C-1100 DEG C, is specially 1000 DEG C-1020 DEG C；
Sedimentation time is 30min-480min；
Described cooling step is programme-control cooling or Temperature fall；
In described Programmed freezing step, it is Temperature fall by depositing temperature to 600 DEG C, process conditions according to glass cools molding, set and delay the temperature-fall period at 600 DEG C-450 DEG C, in this interval, temperature fall time is set to 2 hours (being generally 20 minutes), as may be set to 1 DEG C/min-1.5 DEG C/min by the rate of temperature fall of 600 DEG C to 450 DEG C so that it is the better molding of glass, surface smooths, it is suppressed that the generation of sample interior and blibbing and crackle in Liquid-solid Transition process.It is Temperature fall by 450 DEG C to room temperature
In described chemical vapor deposition step, the method for deposition at least one in normal pressure thermal chemical vapor deposition method (APCVD), melting heat chemical vapour deposition technique (molten-stateAPCVD) and plasma enhanced chemical vapor deposition method (PECVD)；
When the softening temperature of described glass is not higher than 630 DEG C, the method for described deposition is chosen in particular from least one in melting heat chemical vapour deposition technique (molten-stateAPCVD) and plasma enhanced chemical vapor deposition method (PECVD)；
When the softening temperature of described glass is higher than 900 DEG C, the method for described deposition is specially normal pressure thermal chemical vapor deposition method (APCVD).
The concrete steps of described normal pressure thermal chemical vapor deposition method (APCVD) including: substrate of glass is put in conventional quartz pipe, carrier gas is passed under atmospheric pressure environment, substrate is warming up to setting furnace temperature, carbon-source gas is then passed into when keeping carrier gas to pass into, under high temperature, carbon-source gas is cracked into active group, deposit at substrate surface, it is achieved the direct growth of Graphene；
Concrete, in described normal pressure thermal chemical vapor deposition method (APCVD), depositional environment is 1 atmospheric pressure；Carrier gas is the gaseous mixture being made up of argon and hydrogen；Depositing temperature is 950 DEG C-1100 DEG C, it is preferable that 1000 DEG C-1050 DEG C, is specially 1020 DEG C；Sedimentation time is 60min-480min, it is preferable that 180min；The flow of argon is 50-500sccm, it is preferable that 100sccm；The flow of hydrogen is 50-200sccm；The flow-rate ratio of argon and hydrogen is 2:0.5-1.5, it is preferable that 2:1；The flow of carbon source is 1-50sccm, is specially 7sccm；
The concrete steps of described melting heat chemical vapour deposition technique (molten-stateAPCVD) including: is placed in the smooth graphite jig of speciality by the substrate of glass of well cutting, then whole mould is put in conventional quartz pipe, substrate is warming up to setting furnace temperature, glass hot mastication in mould is fused solution, then pass into carbon-source gas, at high temperature it is cracked into active group, and the glass of molten condition is beneficial to the migration of carbon active specy, temperature-fall period takes Programmed freezing pattern, it is achieved that Graphene is in the direct growth of melten glass substrate；
In described melting heat chemical vapour deposition technique (molten-stateAPCVD), carrier gas is the gaseous mixture being made up of argon and hydrogen；Depositing temperature is 1000 DEG C-1100 DEG C, it is preferable that 1000 DEG C；Sedimentation time is 30min-480min, it is preferable that 120min；The flow of-argon is 50-500sccm, it is preferable that 150sccm；The flow of hydrogen is 2-100sccm, is specially 20sccm；The flow-rate ratio of argon and hydrogen is 1-100:1, it is preferable that 7.5:1；The flow of carbon source is 1-20sccm, it is preferable that 6sccm；
The concrete steps of described plasma enhanced chemical vapor deposition method (PECVD) including: substrate of glass is put in plasma enhanced chemical vapor deposition cavity, it is evacuated to the environment (being specially 1Pa) of 0.4-170Pa, passing into carbon-source gas, substrate is warmed up to setting furnace temperature；Then open plasma electrical source, make Hydrocarbon ionization be cracked into active group, react at substrate surface, it is achieved the direct growth of Graphene.
In described plasma enhanced chemical vapor deposition method (PECVD), depositional environment is vacuum is the environment of 0.4-170Pa, and vacuum is specially 1Pa；Depositing temperature is 400 DEG C-600 DEG C；The power of plasma electrical source is 40-100W, it is preferable that 80W；The flow of carbon source is 2-7sccm, it is preferable that 5.5sccm；Sedimentation time is 30-120min, it is preferable that 60min.
In the above-mentioned method preparing superior graphite alkene glass, reaction unit used is conventional tube stove, concretely quartz capsule pipe-type stove, in quartz capsule pipe-type stove used, and the diameter of quartz ampoule concretely 1-3 inch, it is preferable that 3 inches, it is beneficial to the growth of large scale sample.It addition, in preparation process, substrate of glass need to be kept to be positioned at the point midway of reaction unit such as tube furnace.
Owing in the present invention, the property indices of graphene conductive glass can change in a big way, especially, its light transmission rate (wavelength 550nm place) can from about 10% to 97%, and surface resistivity can from 80 Ω sq-1To 20k Ω sq-1.This graphene conductive glass structure is simple, and with low cost, performance is comparatively excellent, applied widely, can be applicable to transparent tellite, resistive touch panel substrate, electric heater heating parts, the parts etc. of electrochromism window.
Accompanying drawing explanation
Fig. 1 is structural representation and the preparation method schematic diagram of graphene conductive glass of the present invention.
Fig. 2 is the pictorial diagram of part graphene conductive glass sample.
Fig. 3 is the sample characterization of the superior graphite alkene glass obtained by the growth of normal pressure thermal chemical vapor deposition.
Fig. 4 is the resistive touch screen pictorial diagram using graphene conductive glass.
Fig. 5 is the sample characterization of the superior graphite alkene glass obtained by normal pressure molten chemical vapor deposition growth.
Fig. 6 is the pictorial diagram of the simple printed circuit using superior graphite alkene glass.
Fig. 7 is the sample characterization of the superior graphite alkene glass obtained by plasma auxiliary chemical vapor deposition growth.
Fig. 8 is the pictorial diagram of the electric heater using superior graphite alkene glass.
Fig. 9 is the visual illustration figure of the electrochromism window using superior graphite alkene glass.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following example.Described method is conventional method if no special instructions.Described raw material if no special instructions all can from being openly either commercially available.
The schematic diagram of the direct growth method of superior graphite alkene glass provided by the invention and growth sample Graphene coverage characterize as it is shown in figure 1, numbering 1 is substrate of glass, and numbering 2 is tube furnace, and numbering 3 is quartz ampoule.
Wherein, the chemical gas-phase deposition system that Fig. 1 (a) uses for growth superior graphite alkene glass；
Fig. 1 (b) is the Graphene growth process at glass basic surface, and carbon atom is connected to edge, Graphene island by edge-diffusion, and then Graphene island is spliced into graphene film；
The graphene growth process that Fig. 1 (c) characterizes for scanning electron microscope (SEM) and optical microscope (OM), by the graphene film of subband structures to the graphene film expiring layer, it is shown that the ability of regulation and control that Graphene is grown on the glass substrate.Fig. 1 (d) is for growing the structural representation of obtained superior graphite alkene glass.
Fig. 2 is the photo in kind of part superior graphite alkene glass sample.Wherein a to be common white glass, b be common color glass, c are flexible micarex, d is cobalt glass and pyroceram, e be boron glass, f are quartz glass.
Embodiment 1:
With quartz glass for substrate, utilize normal pressure thermal chemical vapor deposition method (APCVD) to prepare superior graphite alkene glass, then make touch screen sample, show its working condition.
1) quartz glass substrate (length is 10cm, and width is 5cm, and thickness is 1mm) ultrasonic cleaning in ultra-pure water, isopropanol, acetone and ultra-pure water (ultra sonic bath) each 5min successively, the ultrasonic power of ultra sonic bath is 80W.Quartz glass substrate after ultra sonic bath uses high pure nitrogen to dry up, and obtains quartz glass substrate, standby.
2) the quartz glass substrate obtained after cleaning is put in APCVD cavity, by Ar and H2Gas flowmeter is respectively set as 100sccm and 50sccm, opens Ar and H2Valve, carries out gas scrubbing, it is therefore an objective to drive away the H in reaction chamber2O and O2, the persistent period is 10min.After gas washing, the air pressure of APCVD cavity is 1 atmospheric pressure, and quartz glass substrate is warming up to 1020 DEG C, keeps Ar and H in temperature-rise period2Flow velocity is constant.After furnace temperature rises to 1020 DEG C, stablize 30min, it is therefore an objective to be annealed sample while stablizing furnace temperature processing, set CH therebetween4Flow is calculated as 7sccm, later on CH4Gas valve, the response time is 180min, at the quartz glass substrate surface of 1020 DEG C, CH4Thermal cracking is carbon active group, carries out chemical vapour deposition (CVD), Temperature fall after deposition, obtains superior graphite alkene glass.
The sign of the superior graphite alkene glass sample that this embodiment obtains is as shown in Figure 3.Wherein, Fig. 3 (a) is the x-ray photoelectron power spectrum C of growth sample1sNarrow spectrum (XPSC1sSpectrum), it was shown that sp in Graphene2Carbon constituent content is high, it does not have oxy radical, the purity of prominent CVD growth sample.The surface resistivity that Fig. 3 (b) is growth sample characterizes, the surface resistivity average out to 500 Ω sq of this sample as seen from the figure-1, and it is distributed visibly homogeneous.Fig. 3 (c) is the curve of the light transmission rate growing sample under such condition of a part, and the surface resistivity participating in diagram sample is shown in the lower right corner of picture.As seen from the figure, by controlling growth temperature, growth time or carbon source concentration, the light transmission rate of superior graphite alkene glass and surface resistivity can be carried out controllable adjustment.
Using this superior graphite alkene glass as base plate, copper sheet is pasted as extraction electrode using conducting resinl in both sides in its longitudinal direction；Commodity in use ITO-PET thin film as teleblem, both sides making electrode same as above in the width direction, then that conducting surface is relative, bond with double faced adhesive tape, by each electrode extraction wire, is obtained simplest four-wire resistance type touch screen sample.This sample is shown in Fig. 4 (a).The wiring schematic diagram of sample is shown in Fig. 4 (b).
With universal test software Touchkit it tested and write, this touch screen can works fine, its PKU printed words write are shown in Fig. 4 (c).As seen from the figure, this embodiment gained superior graphite alkene glass can use as the base plate of resistive touch screen.
Embodiment 2:
With common white glass for substrate, utilize melting heat chemical vapour deposition technique (molten-stateAPCVD) to prepare Graphene glass, show its conductive characteristic.
1) according to the method for embodiment 1 step 1, the common white substrate of glass (length is 5cm, and width is 5cm, and thickness is 4mm) of cleaning is obtained.
2) put in square graphite crucible at the bottom of the common white glass basis obtained after cleaning, then crucible is put in APCVD cavity, by Ar and H2Gas flowmeter is respectively set as 150sccm and 20sccm, opens Ar and H2Valve, carries out gas scrubbing, it is therefore an objective to drive away the H in reaction chamber2O and O2, the persistent period is 10min.After gas washing, the air pressure of APCVD cavity is 1 atmospheric pressure, and common white substrate of glass is warming up to 1000 DEG C, keeps Ar and H in temperature-rise period2Flow velocity is constant.After furnace temperature rises to 1000 DEG C, stablizing 30min, it is therefore an objective to be annealed sample while stablizing furnace temperature processing, now white glass is softened for liquid, but owing to the protective effect of graphite crucible will not be overflowed.Set CH therebetween4Flow is calculated as 4sccm, later on CH4Gas valve, the response time is 120min, at the melten glass substrate surface of 1000 DEG C, CH4Thermal cracking is carbon active group, reacts, direct growth Graphene.The substrate of molten state can promote the migration of active material.After reacted, stove elder generation Temperature fall to 600 DEG C, and the step of Programmed freezing is taked in 600 DEG C of-450 DEG C of intervals, temperature fall time is extended to 2 hours in this interval, rate of temperature fall may be set to 1 DEG C/min-1.5 DEG C/min, purpose is to avoid glass cools to turn the generation of bubble and crackle in solid phase procedures, finally naturally cools to room temperature again, obtains superior graphite alkene glass provided by the invention.
The sign of the superior graphite alkene glass sample that this embodiment obtains is as shown in Figure 5.Wherein, Fig. 5 (a) be the ultraviolet-visible of sample through spectrum, be transferred to for the Graphene of growth and the quartz substrate of 1cm × 1cm record, it was shown that the Graphene thickness obtained is 1 atomic layer (550nm place transmitance is 97.1%)；Fig. 5 (b) is representational SEM picture；Fig. 5 (c) is representational atomic force microscope (AFM) photo, and thickness data shown in figure is about 0.5 nanometer, it is known that the thickness of this Graphene is 1 atomic layer.In addition, due also to single-layer graphene thickness (0.7-1 nanometer) prepared by the more usual transfer method of this thickness is for low, and closer to Graphene atomic layer level thickness in theory (0.3 nanometer), prove that this sample surfaces is compared with Graphene glass prepared by usual transfer method, the not impurity such as water-bearing layer or polymeric membrane residue.
This superior graphite alkene glass-cutting is become 1cm × 2cm, and with icking tool, pattern shown in Fig. 6 (a) cuts out circuit patterns (blue portion is for carving except part) in its surface.Then with conducting resinl paster LED is pasted onto according to the such as position shown in Fig. 6 (a) and do not carve on the Graphene except part, namely complete a simple all-transparent circuit.Except above method, it is also possible to used the method for plasma etching to make circuit patterns by template.
Using the D.C. regulated power supply of commercialization, be energized in the position shown in Fig. 6 (a) by alligator clamp, voltage 3-5V, paster LED gets final product normal luminous, illustrates that this circuit is working properly, and photo is such as shown in Fig. 6 (b).As seen from the figure, this embodiment gained superior graphite alkene glass can use as transparent circuit board.
Embodiment 3:
With quartz glass for substrate, utilize plasma enhanced chemical vapor deposition method (PECVD) to prepare Graphene glass, then make electric heater.
1) according to the method for embodiment 1 step 1, the quartz glass substrate (length is 4cm, and width is 6cm, and thickness is 1mm) of cleaning is obtained.
2) the quartz glass substrate obtained after cleaning is put in PECVD cavity, be evacuated to 1Pa, pass into CH4Gas (5.5sccm), common white substrate of glass is warming up to 600 DEG C, controls the air pressure of gas less than 40Pa.When after system stability, open plasma electrical source power 80W, react 1 hour, methane ionization is cracked into active group, reacts at the substrate surface active groups of 600 DEG C, carbon carbon Cheng Jian, direct growth Graphene, close plasma electrical source, then Temperature fall after having reacted, obtain superior graphite alkene glass provided by the invention.
The sign of the superior graphite alkene glass sample that this embodiment obtains is as shown in Figure 7.Wherein, Fig. 7 (a) is representational SEM picture, Fig. 7 (b) is the measurement result of sample surface resistance, and Fig. 7 (c) is the Raman spectrum photo of the PECVD superior graphite alkene glass prepared, and wherein blue spectral line is the spectral line growing sample under this condition.In this spectral line, the peak intensity ratio of 2D/G is about 2, it is known that the thickness of this Graphene is 1-2 atomic layer；Then for Graphene that thickness is 10-100 atomic layer shown in red spectral line.
Brush the contact of a small amount of conductive silver glue auxiliary electrode in these superior graphite alkene sheet glass both sides, namely become simplest electric boiling plate.Taking a small amount of temperature induced color changing dyestuff (reversible color temperature is 60 degree, and red and white change, purchased from Shenzhen thousand complexion changed Dye Co., Ltd), directly dropping is on this superior graphite alkene glass heater, as shown in Figure 8.Then, using the D.C. regulated power supply of commercialization, by alligator clamp in elargol covering place (now resistance is about thousands of Europe), energising, voltage 30-50V, after hanging on, dyestuff is become white from redness.Prove that superior graphite alkene glass heater can normal heating, it is possible to use as electrical heating elements.
Embodiment 4: the performance of the electrochromism window of embodiment 3 gained superior graphite alkene sheet glass
First two panels equivalently-sized embodiment 3 gained superior graphite alkene glass is taken, strip is cut into another block simple glass, then the window-like of hollow it is bonded into Commercial epoxy glue (AB glue), as it is shown in figure 9, a hole injecting liquid need to be reserved during bonding.
Then, commercially available hydroxypropyl methyl cellulose (HPMC), sodium chloride (NaCl) and water are prepared mixed solution, its mass ratio is 2:5:100, is slowly injected in the hollow window that two-layer superior graphite alkene glass is formed by this solution with syringe.Finally, at superior graphite alkene glass both sides conducting resinl bond wire extraction electrode.Now, resistance about tens of kilo-ohms between this two electrode, light transmission rate is about 77%.
Two wires are accessed civil power (alternating current), after hanging on, owing to energising causes that solution temperature rises, coacervation process occurs so that this window becomes opaque.After stopping energising, it being cooled down, window recovers again transparent, as shown in Figure 9 (for being not powered on state, right side is "on" position in left side).Prove the electrochromism window be made up of this embodiment 3 gained superior graphite alkene glass can works fine, namely this embodiment 3 gained superior graphite alkene glass can use as electrochromic electrode element.
Claims (10)
1. Graphene glass application in preparing conductive devices.
2. contain the conductive devices of Graphene glass.
3. the conductive devices described in application according to claim 1 or claim 2, it is characterised in that: described conductive devices is transparent circuit board, the base plate of resistive touch screen, electrical heating elements or electrochromic electrode element.
4. the application according to claim 1 or 3 or the conductive devices described in Claims 2 or 3, it is characterised in that: described Graphene glass forms by substrate with being positioned at described suprabasil Graphene；
Wherein, described substrate is glass；Described Graphene is positioned at the one or both sides of described substrate；
The thickness of described Graphene is 1-100 atomic layer.
5. the conductive devices described in application according to claim 4 or Claims 2 or 3, it is characterised in that: described glass at least one in white glass, smalt, green glass, brown glass, quartz glass, sapphire glass, blue cobalt glass, ito glass, FTO glass, AZO glass, soda-lime glass, Pyrex, flexible micarex, borate glass and phosphate glass；
The thickness of described white glass, smalt, green glass, brown glass and quartz glass is 1mm-10mm.
6. the application according to claim 1 or 3 or 4 or 5 or the conductive devices described in Claims 2 or 3 or 4 or 5, it is characterised in that: described Graphene glass obtains according to the method preparation comprised the steps:
With glass described in claim 5 for substrate, in chemical gas-phase deposition system, pass into carbon source and carry out chemical vapour deposition (CVD), deposit and complete be cooled to room temperature, obtain described Graphene glass.
7. application according to claim 6 or conductive devices, it is characterised in that: in described chemical vapor deposition step, carbon source at least one in methane and ethylene；
Depositing temperature is 400 DEG C-1100 DEG C；
Sedimentation time is 30min-480min；
Described cooling step is programme-control cooling or Temperature fall；
In described programme-control cooling, depositing temperature to 600 DEG C it is Temperature fall, the rate of temperature fall of 600 DEG C to 450 DEG C is 1 DEG C/min-1.5 DEG C/min, be Temperature fall by 450 DEG C to room temperature.
8. the method according to claim 6 or 7, it is characterised in that: in described chemical vapor deposition step, the method for deposition at least one in normal pressure thermal chemical vapor deposition method, melting heat chemical vapour deposition technique and plasma enhanced chemical vapor deposition method.
9. method according to claim 8, it is characterised in that: in described normal pressure thermal chemical vapor deposition method, depositional environment is 1 atmospheric pressure；Carrier gas is the gaseous mixture being made up of argon and hydrogen；Depositing temperature is 950 DEG C-1100 DEG C；Sedimentation time is 60min-480min；The flow-rate ratio of argon and hydrogen is 2:0.5-1.5；
In described melting heat chemical vapour deposition technique, carrier gas is the gaseous mixture being made up of argon and hydrogen；Depositing temperature is 1000 DEG C-1100 DEG C；Sedimentation time is 30min-480min；The flow-rate ratio of argon and hydrogen is 1-100:1:1；
In described plasma enhanced chemical vapor deposition method, depositional environment is vacuum is the environment of 0.4Pa-170Pa；Depositing temperature is 400 DEG C-600 DEG C；The power of plasma electrical source is 40W-100W；The flow of carbon source is 2-7sccm；Sedimentation time is 30min-120min.
10. method according to claim 9, it is characterised in that: in described normal pressure thermal chemical vapor deposition method, the flow of argon is 50-500sccm；The flow of hydrogen is 50-200sccm；The flow of carbon source is 1-50sccm；
In described melting heat chemical vapour deposition technique, the flow of argon is 50-500sccm；The flow of hydrogen is 2-100sccm；The flow of carbon source is 1-20sccm.
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| CN107311467A (en) * | 2017-05-27 | 2017-11-03 | 北京大学 | A kind of preparation method, Graphene glass and the photo-thermal conversion device of the photo-thermal conversion device based on Graphene glass |
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| CN107689323A (en) * | 2017-08-11 | 2018-02-13 | 北京大学 | A kind of graphene Sapphire Substrate for being applied to III group-III nitride epitaxial growth |
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