CN107500560A - The method for preparing Graphene glass - Google Patents

The method for preparing Graphene glass Download PDF

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Publication number
CN107500560A
CN107500560A CN201710914397.9A CN201710914397A CN107500560A CN 107500560 A CN107500560 A CN 107500560A CN 201710914397 A CN201710914397 A CN 201710914397A CN 107500560 A CN107500560 A CN 107500560A
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glass
gas
graphene
carbon
graphene film
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邢飞
闫立群
磨玉茹
张同林
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Beijing Carbon Century Technology Co Ltd
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Beijing Carbon Century Technology Co Ltd
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Priority to CN201710914397.9A priority Critical patent/CN107500560A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/15Deposition methods from the vapour phase
    • C03C2218/152Deposition methods from the vapour phase by cvd
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/30Aspects of methods for coating glass not covered above
    • C03C2218/31Pre-treatment

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The method for preparing Graphene glass of the present invention, including:Step 1: glass cleaning, is cleaned by ultrasonic glass, cleaning 35 minutes, are dried up with nitrogen every time with water, ethanol, acetone, water, isopropanol, water successively respectively;Step 2: using glass as substrate, in a low pressure environment, environment temperature is warming up to 900 DEG C 1100 DEG C, it is passed through reducing atmosphere gas, then being passed through carbon-source gas according to the 200sccm of flow velocity 10 grows graphene film, and after certain time, environment temperature is down to room temperature naturally, obtain the graphene film on quartz glass, carbon-source gas be methanol gas, at least one of alcohol gas.Technical scheme provide it is a kind of using methanol or ethanol as carbon source prepare graphene film method, it is necessary to methanol or ethanol flow it is smaller, experimentation is very safe;Resulting graphene film thickness is uniform, is of high quality, and can obtain the different graphene film of thickness, can obtain and the excellent graphene film of quartz glass plate adhesive force.

Description

The method for preparing Graphene glass
Technical field
The present invention relates to the preparation of carbon, more particularly to a kind of method for preparing Graphene glass.
Background technology
Graphene is with sp by carbon atom2The individual layer two-dimensional atomic crystal that hybridized orbit is formed by honeycomb crystal lattice arrangement. Graphene is known most thin, most tough and tensile nano material, and its hardness exceedes diamond;Single-layer graphene is almost fully transparent, only 2.3% absorbance;Thermal conductivity factor is up to 5300W/mK, and resistivity only has 10-6 Ω cm, is most excellent heat and electricity Conductor.Graphene has important research and application value because of its excellent physicochemical property in many application fields.
Currently used method for preparing graphene membrane is mainly using chemical vapor deposition (CVD) technology in metal substrate Superficial growth graphene, such as copper-base graphite alkene, Ni-based graphene.CVD method, which prepares graphene, has that step is simple, quality The high, advantage such as controllability is strong, while metal has catalytic action to graphene forming core, growth, therefore CVD method turns into main flow One of method for preparing graphene membrane.But the metallic substrates graphene of high-quality growth typically can not be directly using, it is necessary to enter Row graphene transfer operation, is especially transferred graphene on the dielectrics such as glass, complex process be present, sample fold increases The problems such as more, defect increase, transfer medium residual destruction, cause graphene power, heat, light, electricity etc. property to be deteriorated, because This serious performance for restricting Graphene glass and application.
To solve the above problems, the technology for directly being prepared graphene in substrate of glass based on CVD method is arisen at the historic moment, equally Graphene film is prepared using CVD, by controlling the bars such as carbon source and content, reducing atmosphere and ratio, sintering temperature and time Part also can obtain the graphene film of function admirable.At present, the conventional carbon source that CVD method prepares Graphene glass is the hydrocarbon such as methane Class gas, and using the hydrogen of higher concentration as auxiliary atmosphere, in high-temperature sintering process, these flammable explosive gas have one Fixed potential safety hazard.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of using methanol or ethanol as carbon source, safer prepares stone The method of black alkene glass.
An object of the present invention is to provide a kind of using methanol or ethanol as the method for preparing graphene film of carbon source, replaces The hazardous gases such as methane are changed, the flow velocity of load carbon source argon gas is reduced and using low-pressure system, agraphitic carbon deposition is greatly decreased, obtains To high quality, uniform graphene film.
The second object of the present invention is to provide a kind of gas relatively low using density of hydrogen ratio as reducing atmosphere, experiment The very safe method for preparing graphene film of process.
The third object of the present invention is to extend graphene time in low pressure reducing atmosphere, increases graphene and glass substrate Adhesive force, and then improve Graphene glass anti-wiping performance.
The method for preparing Graphene glass of the present invention, including:
Step 1: glass cleaning, is cleaned by ultrasonic quartz glass with water, ethanol, acetone, water, isopropanol, water successively respectively, Every time cleaning 3-5 minutes, dried up with nitrogen;
Step 2: using the glass as substrate, in a low pressure environment, environment temperature is warming up to 900 DEG C -1100 DEG C, led to Enter reducing atmosphere gas, being then passed through carbon-source gas according to flow velocity 10-200sccm grows graphene film, after certain time, Stopping is passed through carbon-source gas and reducing atmosphere gas, and environment temperature is down to room temperature naturally, obtains the graphite on the quartz glass Alkene film, described carbon-source gas are at least one of methanol gas, alcohol gas.
The method for preparing Graphene glass of the present invention, wherein, the reducing atmosphere gas is the mixing of argon gas and hydrogen Gas, wherein hydrogen ratio are percent by volume 1%-10%.
The method for preparing Graphene glass of the present invention, wherein, wherein hydrogen ratio is percent by volume 5%.
The method for preparing Graphene glass of the present invention, wherein, described carbon source is at least one of methanol, ethanol.
The method for preparing Graphene glass of the present invention, wherein, it is described that environment temperature is warming up to 900 DEG C of -1100 DEG C of tools Body is that environment temperature is warming up into 1000 DEG C -1050 DEG C.
The method for preparing Graphene glass of the present invention, wherein, the carbon-source gas are carried by the use of argon gas as carrier gas, argon gas The flow of gas is 10-200sccm.
The method for preparing Graphene glass of the present invention, wherein, the flow of the argon carrier is 100sccm.
The method for preparing Graphene glass of the present invention, wherein, the vacuum of the environment under low pressure is 200-2000Pa.
The method for preparing Graphene glass of the present invention, wherein, the vacuum of environment under low pressure is 1000Pa.
The method for preparing Graphene glass of the present invention, wherein, the certain time is 10-600min.
The method for preparing Graphene glass of the present invention, wherein, the glass is quartz glass, thickness 0.1mm- 30mm。
The method for preparing Graphene glass of the present invention, including:
Step 1: glass cleaning, is cleaned by ultrasonic quartz glass with water, ethanol, acetone, water, isopropanol, water successively respectively, Every time cleaning 3-5 minutes, dried up with nitrogen;
Step 2: using the glass as substrate, in 200-2000Pa depositional environments, by environment temperature be warming up to 900 DEG C- 1100 DEG C of growth temperature, reducing atmosphere gas is passed through, being then passed through carbon-source gas according to flow velocity 10-200sccm makes graphene Film grows, and after depositing 10-600min, stopping is passed through carbon-source gas, obtains the graphene film on the glass, keeps growth Temperature and pressure, make the graphene film on glass continue to be located in reducing atmosphere, time 30min-240min, drop naturally Temperature, the reducing atmosphere are the gaseous mixture of argon gas and hydrogen, and wherein hydrogen ratio is percent by volume 1%-10%, the carbon source For at least one of methanol or ethanol, carrier gas is used as by the use of argon gas.
Technical scheme provide it is a kind of using methanol or ethanol as carbon source prepare graphene film method, it is necessary to Methanol or ethanol flow it is smaller, hydrogen proportion is very low in reducing atmosphere, and experimentation is very safe;Low discharge methanol Or ethanol is under low pressure, make that carbon source is less, more rapidly pass through glass surface, deposited so as to reduce amorphous carbon, it is resulting Graphene film thickness is uniform, is of high quality;By technique adjustment, the different graphene film of thickness is can obtain, is passed through simultaneously Adjusting process, it can obtain and the excellent graphene film of quartz glass plate adhesive force.
Brief description of the drawings
Fig. 1 is the CVD device schematic diagram prepared used in the method for Graphene glass of the present invention;
The Raman for the graphene that Fig. 2 is Reference Example 1, prepared by the embodiment 1 of the method for preparing Graphene glass of the present invention Spectrum;
Fig. 3 is the material object of Graphene glass prepared by the embodiment 22-26 of the method for preparing Graphene glass of the present invention Figure;
Fig. 4 is thickness and the suction of graphene prepared by the embodiment 22-26 of the method for preparing Graphene glass of the present invention Receive the graph of a relation with growth time;
Fig. 5 is the Graphene glass of the preparation of embodiment 24,27 of the method for preparing Graphene glass of the present invention with 1N's Power wipes front and rear optical imagery;
Fig. 6 is the Graphene glass of the preparation of embodiment 24 of the method for preparing Graphene glass of the present invention in different temperatures Resistance test figure after lower thermal annealing;
Fig. 7 is the Raman spectrum of graphene prepared by the embodiment 29 of the method for preparing Graphene glass of the present invention.
Embodiment
The method for preparing Graphene glass of the present invention, including:
Step 1: glass cleaning, is cleaned by ultrasonic glass, every time with water, ethanol, acetone, water, isopropanol, water successively respectively Clean 3-5 minutes and (take 18-30 minutes altogether), dried up with nitrogen;
Step 2: using the glass as substrate, in a low pressure environment, environment temperature is warming up to 900 DEG C -1100 DEG C, led to Enter reducing atmosphere gas, being then passed through carbon-source gas according to flow velocity 10-200sccm grows graphene film, after certain time, Stopping is passed through carbon-source gas and reducing atmosphere gas, and environment temperature is down to room temperature naturally, obtains the graphite on the quartz glass Alkene film, described carbon-source gas are at least one of methanol gas, alcohol gas.
The method for preparing Graphene glass of the present invention, wherein, the reducing atmosphere gas is the mixing of argon gas and hydrogen Gas, wherein hydrogen ratio are percent by volume 1%-10%.
The method for preparing Graphene glass of the present invention, wherein, wherein hydrogen ratio is percent by volume 5%.
The method for preparing Graphene glass of the present invention, wherein, described carbon source is at least one of methanol, ethanol.
The method for preparing Graphene glass of the present invention, wherein, it is described that environment temperature is warming up to 900 DEG C of -1100 DEG C of tools Body is that environment temperature is warming up into 1000 DEG C -1050 DEG C.
The method for preparing Graphene glass of the present invention, wherein, the carbon-source gas are carried by the use of argon gas as carrier gas, argon gas The flow of gas is 10-200sccm.
The method for preparing Graphene glass of the present invention, wherein, the flow of the argon carrier is 100sccm.
The method for preparing Graphene glass of the present invention, wherein, the vacuum of the environment under low pressure is 200-2000Pa.
The method for preparing Graphene glass of the present invention, wherein, the vacuum of environment under low pressure is 1000Pa.
The method for preparing Graphene glass of the present invention, wherein, the certain time is 10-600min.
The method for preparing Graphene glass of the present invention, wherein, the glass is quartz glass, thickness 0.1mm- 30mm。
The method for preparing Graphene glass of the present invention, including:
Step 1: glass cleaning, is cleaned by ultrasonic quartz glass with water, ethanol, acetone, water, isopropanol, water successively respectively, Every time cleaning 3-5 minutes, dried up with nitrogen;
Step 2: using the glass as substrate, in 200-2000Pa depositional environments, by environment temperature be warming up to 900 DEG C- 1100 DEG C of growth temperature, reducing atmosphere gas is passed through, being then passed through carbon-source gas according to flow velocity 10-200sccm makes graphene Film grows, and after depositing 10-600min, stopping is passed through carbon-source gas, obtains the graphene film on the glass, keeps growth Temperature and pressure, make the graphene film on glass continue to be located in reducing atmosphere, time 30min-240min, drop naturally Temperature, the reducing atmosphere are the gaseous mixture of argon gas and hydrogen, and wherein hydrogen ratio is percent by volume 1%-10%, the carbon source For at least one of methanol or ethanol, carrier gas is used as by the use of argon gas.
(1) methanol or ethanol that technical scheme passes through safety are carbon source, are mixed and reduced using low ratio hydrogen Gas, makes that the growth course of Graphene glass is safe and reliable, and danger coefficient is greatly reduced;
(2) technical scheme loads the flow velocity of carbon source argon gas by reducing and using low-pressure system, is greatly decreased Agraphitic carbon deposits, and obtains high quality, uniform graphene film, controllable by controlling technique to reach graphene film thickness;
(3) graphene film and the adhesion of quartz glass that generally CVD method obtains be not strong, and slight friction will make Graphene wears or peeled off, and to improve this shortcoming of Graphene glass, technical scheme grows in graphene film After the completion of, continue to carry out annealing certain time in original temperature and reducing atmosphere and environment under low pressure, this operation can So that adhesive force of the graphene on quartz glass is significantly increased, and then improve the anti-wiping performance of Graphene glass;
(4) graphene prepared by the present invention has certain heat endurance in atmosphere, and highest is resistant to 400 DEG C.
The method for preparing Graphene glass of the present invention is described in detail with specific embodiment below.
Reference Example 1:After quartz glass plate is cleaned by ultrasonic 3min with pure water, ethanol, acetone, water, isopropanol, water successively, nitrogen Air-blowing is done;Quartz glass after cleaning is put into the tube furnace in CVD system, the temperature of tube furnace is set to 1050 DEG C, will Tube furnace pressure is evacuated to below 10Pa, each leads into 700sccm high-purity argon gas and 700sccm high-purity hydrogens, after temperature stabilization, It is passed through 500sccm alcohol vapours into reaction chamber, controls in tube furnace pressure after 1500Pa or so, graphene growth 40min, Stopping is passed through carbon-source gas, hydrogen and argon gas, is naturally cooling to room temperature, it is 7.3nm to obtain graphene film thickness.
Embodiment 1:Quartz glass plate is cleaned by ultrasonic 3min using pure water, ethanol, acetone, water, isopropanol, water successively, uses Nitrogen dries up;Quartz glass after cleaning is put into the boiler tube of chemical gas-phase deposition system, tubular type furnace temperature is set to 1050 DEG C, After being evacuated to 10Pa or so, with the whole gas circuit of 500sccm argon purges, time 5min;Hydrogen is opened, sets argon gas and stream Speed is 475sccm, hydrogen flow rate 25sccm, and the volume ratio that the ratio of hydrogen accounts for argon hydrogen gaseous mixture is 5%;Open load ethanol Argon gas gas circuit, the flow velocity for adjusting argon gas is 100sccm, adjusts vavuum pump, tubular type furnace pressure is kept for 1000Pa or so Constant temperature grows 100min, and stopping is passed through carbon-source gas and reducing atmosphere gas, is then naturally cooling to room temperature, obtains institute of the present invention The Graphene glass of offer, quartz glass thickness 0.1mm-30mm, the graphene film thickness are 6.2nm.
The Raman spectrum of the graphene film of Reference Example 1 and the gained of embodiment 1 is as shown in Fig. 2 the gained graphene of Reference Example 1 Raman spectrum in D peaks (1350cm-1) and G peaks (1596cm-1) intensity rate ID/IGFor 0.73, the graphene film of comparative example 1 Intensity compares ID/IGFor 0.69, graphene film defect level prepared by two techniques is substantially close, the ethanol flow that comparative example 1 needs Smaller, hydrogen proportion is very low in reducing atmosphere, and experimentation is comparatively safe reliable.
For embodiment 2-13 according to the method, step and growth time of embodiment 1, fixed carbon source is ethanol, changes carbon source The ratio of gas flow rate and reducing gas, flow velocity, measurement thickness, the absorption under the irradiation of 550nm laser, and in Raman spectrum ID/IGAs shown in table 1,
Table 1
Embodiment 1-4 can control the thickness of graphene by changing carbon source flow velocity, from the intensity rate of Raman spectrum test ID/IGData are seen, when carbon source flow velocity is 100sccm, ID/IGRatio is minimum, minimum the defects of graphene film;Embodiment 1, The ratio of embodiment 5-9 fixed carbon source stream speed and argon gas hydrogen, change the flow velocity of reducing gas, it is smaller to can obtain thickness difference Graphene film, Raman test ID/IGRatio changes greatly, when the flow velocity of reducing gas is 500sccm, ID/IGRatio is most It is small;Embodiment 1, embodiment 10-13 are that reducing gas flow velocity is 500sccm, change H2Concentration ratio, obtained thickness basic one The graphene film of cause, in terms of absorption and Raman test result, H2When concentration ratio is 5%, the defects of graphene film is most It is few.
Embodiment 1-13 result shows that optimal conditions prepared by Graphene glass is respectively that carbon source flow velocity is 100sccm, Reducing gas flow velocity is 500sccm, and density of hydrogen is 5% in reducing atmosphere.
To find the optimal conditions of Graphene glass growth temperature and pressure, we change according to the method and step of embodiment 1 Become tube furnace sintering temperature and quartzy intraductal pressure, carry out embodiment 14-19 experiment, measure the graphene of preparation thickness, Absorption and Raman data, as shown in table 2
Table 2
Embodiment 1, embodiment 14-17 are the Graphene glass obtained by changing pressure in tube furnace, when pressure is During 1000Pa or so, Graphene glass best performance;Embodiment 1, embodiment 18-21 are to change the graphene that sintering temperature obtains Glass, with the rise of temperature, Graphene glass film defects gradually decrease, but when temperature is more than 1050 DEG C, graphene is thin Film defect is really increasing.
Graphene sintering temperature and the optimum condition of pressure are respectively 1050 DEG C and 1000Pa.
Embodiment 22-26 be according to above-mentioned optimum condition technique prepare Graphene glass, when deposited between be respectively When 10min, 20min, 30min, 60min, 120min, 360min, the Graphene glass material object design sketch of preparation as shown in figure 3, The Graphene glass uniformity of film of preparation is good, and surface is smooth, and with the increase of sedimentation time, thickness is also increasing with absorbing, Thickness is as shown in Figure 4 with the variation tendency of sedimentation time with absorbing.
The graphene film and the adhesion of quartz glass that usual CVD method obtains be not strong, and slight friction may can Graphene is set to wear or peel off, to improve this shortcoming of Graphene glass, technical scheme is given birth in graphene film After the completion of length, continue to carry out annealing certain time in original temperature and reducing atmosphere and environment under low pressure, this operation Adhesive force of the graphene on quartz glass can be significantly increased, and then improve the anti-wiping performance of Graphene glass.
Embodiment 27:According to the processing step of embodiment 24, after the completion of the time to be deposited is 30min, stopping is passed through carbon source Gas, the unobstructed of reducing gas is kept, keep pressure and temperature constant, anneal after 60min, Temperature fall obtains and quartz glass The strong graphene of piece adhesive force.
The Graphene glass 100 times that embodiment 24 and embodiment 27 obtain slowly is wiped with 1N power, obtained effect is such as Shown in Fig. 5, obvious abrasion mark can be observed in the Graphene glass surface of embodiment 24, and it, which absorbs, reduces 21.23%, implements Obvious abrasion mark is not observed on the Graphene glass surface of example 27, and absorption only reduces by 2.15%, therefore by increasing in low pressure The time of reducing atmosphere can increase the adhesive force of graphene and quartz glass plate.
Embodiment 28:By graphene prepared in embodiment 24 be separately heated in air ambient 100 DEG C, 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, its sheet resistance is measured, obtained curve is as shown in Figure 6.Before 400 DEG C, graphene sheet resistance is substantially not Become, graphene film shows good heat endurance.
Embodiment 29:According to the method and step of embodiment 1, carbon source is changed into methanol, growth time 10min, other Part is constant, and it is 0.82nm to obtain graphene film thickness, is absorbed as 5.51%, Raman test spectral is Fig. 7.
Fig. 7 represents that the graphene thickness that the graphene prepared under the same terms with methanol is prepared with ethanol differs greatly, and draws Defect level I is represented in graceful spectrumD/IGValue is basically identical with ethanol, then height can be equally obtained when illustrating methanol as carbon source The graphene of quality.
It the above is only the preferred embodiment of the present invention, it is noted that come for those skilled in the art Say, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should be regarded as Protection scope of the present invention.

Claims (10)

  1. A kind of 1. method for preparing Graphene glass, it is characterised in that including:
    Step 1: glass cleaning, is cleaned by ultrasonic glass, every time cleaning with water, ethanol, acetone, water, isopropanol, water successively respectively 3-5 minutes, dried up with nitrogen;
    Step 2: using the glass as substrate, in a low pressure environment, environment temperature is warming up to 900 DEG C -1100 DEG C, be passed through also Former atmosphere gas, being then passed through carbon-source gas according to flow velocity 10-200sccm grows graphene film, after certain time, stops Carbon-source gas and reducing atmosphere gas are passed through, environment temperature is down to room temperature naturally, obtains the graphene film on the glass, institute The carbon-source gas stated are at least one of methanol gas, alcohol gas.
  2. 2. the method as claimed in claim 1 for preparing Graphene glass, it is characterised in that the reducing atmosphere gas is argon gas With the gaseous mixture of hydrogen, wherein hydrogen ratio is percent by volume 1%-10%.
  3. 3. the method as claimed in claim 1 for preparing Graphene glass, it is characterised in that described carbon source is methanol, ethanol At least one of.
  4. 4. the method as claimed in claim 1 for preparing Graphene glass, it is characterised in that described to be warming up to environment temperature 900 DEG C -1100 DEG C are specially that environment temperature is warming up into 1000 DEG C -1050 DEG C.
  5. 5. the method as claimed in claim 3 for preparing Graphene glass, it is characterised in that the carbon-source gas are made with argon gas For carrier gas, the flow of argon carrier is 10-200sccm.
  6. 6. the as claimed in claim 5 method for preparing Graphene glass, it is characterised in that the flow of the argon carrier is 100sccm。
  7. 7. the as claimed in claim 1 method for preparing Graphene glass, it is characterised in that the vacuum of the environment under low pressure is 200-2000Pa。
  8. 8. the method as claimed in claim 1 for preparing Graphene glass, it is characterised in that the certain time is 10- 600min。
  9. 9. the method as claimed in claim 1 for preparing Graphene glass, it is characterised in that the glass is quartz glass, thick Spend for 0.1mm-30mm.
  10. A kind of 10. method for preparing Graphene glass, it is characterised in that including:
    Step 1: glass cleaning, is cleaned by ultrasonic quartz glass, every time with water, ethanol, acetone, water, isopropanol, water successively respectively 3-5 minutes are cleaned, are dried up with nitrogen;
    Step 2: using the glass as substrate, in 200-2000Pa depositional environments, environment temperature is warming up to 900 DEG C -1100 DEG C growth temperature, be passed through reducing atmosphere gas, being then passed through carbon-source gas according to flow velocity 10-200sccm makes graphene film Growth, after depositing 10-600min, stopping is passed through carbon-source gas, obtains the graphene film on the glass, keeps growth temperature And pressure, make the graphene film on glass continue to be located in reducing atmosphere, time 30min-240min, Temperature fall, The reducing atmosphere is the gaseous mixture of argon gas and hydrogen, and wherein hydrogen ratio is percent by volume 1%-10%, and the carbon source is At least one of methanol or ethanol, carrier gas is used as by the use of argon gas.
CN201710914397.9A 2017-09-30 2017-09-30 The method for preparing Graphene glass Pending CN107500560A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN108996916A (en) * 2018-09-05 2018-12-14 成都中建材光电材料有限公司 A kind of method of quartz inside pipe wall plated film
CN109399620A (en) * 2018-12-05 2019-03-01 中国电子科技集团公司第十三研究所 A method of preparing the silicon carbide-based grapheme material of high mobility
CN111302649A (en) * 2020-03-17 2020-06-19 中国建筑材料科学研究总院有限公司 Graphene conductive glass, preparation method, defrosting glass and electromagnetic shielding glass
CN111675209A (en) * 2020-06-02 2020-09-18 天津理工大学 Method for growing vertical graphene film by using nitrogen and ethanol

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CN106029080A (en) * 2014-02-18 2016-10-12 康宁股份有限公司 Metal-free cvd coating of graphene on glass and other dielectric substrates

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108996916A (en) * 2018-09-05 2018-12-14 成都中建材光电材料有限公司 A kind of method of quartz inside pipe wall plated film
CN108996916B (en) * 2018-09-05 2021-06-08 成都中建材光电材料有限公司 Method for coating inner wall of quartz tube
CN109399620A (en) * 2018-12-05 2019-03-01 中国电子科技集团公司第十三研究所 A method of preparing the silicon carbide-based grapheme material of high mobility
CN111302649A (en) * 2020-03-17 2020-06-19 中国建筑材料科学研究总院有限公司 Graphene conductive glass, preparation method, defrosting glass and electromagnetic shielding glass
CN111675209A (en) * 2020-06-02 2020-09-18 天津理工大学 Method for growing vertical graphene film by using nitrogen and ethanol

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