CN104085887B - A kind of process for preparing graphenes by chemical vapour deposition - Google Patents
A kind of process for preparing graphenes by chemical vapour deposition Download PDFInfo
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Abstract
The present invention provides a kind of process for preparing graphenes by chemical vapour deposition, including: step 1, employing copper, the double; two target magnetic control co-sputtering method of nickel prepare corronil thin film at monocrystalline silicon surface；Step 2, by surface deposition have the monocrystal silicon substrate of corronil thin film to be transferred in the reacting furnace of chemical vapour deposition (CVD), in described reacting furnace, pass into helium, drain the air in described reacting furnace；Step 3, substrate is risen in 20～40min 400～600 DEG C, pass into helium afterwards, make in reacting furnace pressure within the scope of 5～10Torr；Step 4, in described reacting furnace, pass into hydrogen, then to benzene injection in reacting furnace；In step 5, maintenance reacting furnace, pressure is within the scope of 5～10Torr, after benzene has been injected, stop passing into hydrogen, helium is passed into again in reacting furnace, deposition has the monocrystal silicon substrate of corronil thin film to be down to room temperature with 20 DEG C/min speed, is continually fed into helium 10min step 6 afterwards, takes out growth and have the substrate of graphene film.
Description
Technical field
The present invention relates to a kind of method preparing Graphene, adopt process for preparing graphenes by chemical vapour deposition particularly to one.
Background technology
Graphene, the i.e. monoatomic layer of graphite are carbon atoms by the two-dimensional structure of honeycomb arrangement, are also the elementary cells constituting other low dimensional material with carbon elements such as fullerene, CNT.According to the number of plies, Graphene can be divided into single-layer graphene, bilayer graphene, few layer graphene.The research of Graphene is long-standing, but the Graphene of real independent stable existence is then peeled off high starch breeding by the Geim of Univ Manchester UK etc. by adhesive tape to obtain.After Graphene is found, owing to the performance of its excellence and huge application prospect have caused the research boom in the field such as physics and material science.But the grapheme material problem that controlledly synthesis has specific morphology is not still solved.Based on this, the research of Graphene remains in basic research field, and the large-scale application of distance still has a segment distance.
But the preparation realizing too busy to get away high-quality, low cost, extensive Graphene of Graphene physical property and potential application.The main method currently preparing Graphene has: micromechanics stripping method, chemical vapour deposition technique, surface of SiC graphitization method, organic molecule dispersion method, ion insertion method, solvent-thermal method, oxidation-reduction method, C doping deposition method etc..Micromechanics stripping method is to adopt ion beam that material surface is etched, and by mechanical force, material surface is carried out stripping and prepare Graphene.But due to complex process, the Graphene productivity of preparation is low, it is impossible to meet industrialization demand, limits large-scale production to a certain extent.Chemical vapour deposition technique is to utilize chemical reaction to form the film growth method of graphene film at substrate surface, has and passes through CH4Decompose, reduction CO generates gaseous carbon atom, and product deposition, at substrate surface, generates two-dimensional graphene thin film.Due to CH4Decomposition temperature is significantly high, and this method may be only available for resistant to elevated temperatures a few materials substrate.Surface of SiC graphitization method is, under ultrahigh vacuum, 4H-SiC or 6H-SiC is heated to more than 1300 DEG C, and after the Si atom on SiC crystal surface is evaporated, carbon atom reconstructs, it is possible to generate two-dimensional graphene thin film on single crystalline Si face.The graphene film thickness that this method prepares is only 1～2 carbon atomic layer, has high carrier mobility.But not observing quantum hall effect in the Graphene that profit prepares in this way, and the electronic property of graphenic surface is very big by the impact of SiC substrate, research is still underway further.Graphite ultrasonic disperse in organic solvent is obtained a kind of method of Graphene by organic molecule dispersion method, and the Graphene defect that this method obtains is few, but concentration is not high.First ion insertion method prepares compound between graphite layers, and then Graphene is prepared in dispersion in organic solvent, and it is relatively low that this method prepares graphene dispersion degree.Solvent-thermal method is that reactant is added solvent, utilizes solvent higher than under critical temperature and critical pressure, it is possible to dissolve the character of most material, it is possible to be that the reaction that can not occur under normal condition under high pressure can carry out with relatively low temperature, or acceleration.This method development time is short, and present stage, many theory and technology problems still can not break through, and needs to be explored further.Oxidation-reduction method is that graphite oxidation obtains scattered graphene oxide in the solution, then prepares Graphene with reducing agent reduction；Its cost is low, productivity is high, but the graphite that strong oxidizer complete oxidation is crossed is difficult to reduce completely, causes the performances such as some of physics, chemistry, especially electric conductivity loss of energy.C doping deposition method is to utilize the MBE GaAs material growing C doping, makes GaAs decompose by improving temperature, and wherein C atom precipitates out formation Graphene, and this method controllability is very low, and the Graphene mass ratio of generation is relatively low, is still within the stage of fumbling.This level just requiring to improve existing preparation technology, the preparation of current Graphene remains the technical barrier in this field.
Chemical vapour deposition (CVD) is a kind of deposition technique the most frequently used in semi-conductor industry.This side's ratio juris is the mode by chemical reaction, utilizes the various energy such as heating, plasma excitation or light radiation, makes the chemical substance of gaseous state or steam condition form the technology of solid deposited thing in gas phase or gas-solid interface through chemical reaction in reactor.
Summary of the invention
The invention provides a kind of process for preparing graphenes by chemical vapour deposition, by provide a kind of copper nickel with 53: 47 be ratio corronil substrate to improve Graphene in the suprabasil speed of growth.The preparation of Graphene is broadly divided into two kinds: 1 from growth mechanism) carburizing analysis charcoal mechanism: nickel etc. is had to the metallic substrates of higher molten carbon amounts, the carbon atom that carbon source cracking produces penetrates into when high temperature in metallic substrates, cooling time again from it inside precipitate out nucleation, and then growth Graphene；2) superficial growth mechanism: copper etc. is had to the metallic substrates of relatively low molten carbon amounts, the carbon atom that under high temperature, gaseous carbon source cracking generates is adsorbed on metal surface, and then nucleating growth becomes " Graphene island ", and obtain continuous print graphene film by the two dimension on " Graphene island " merging of growing up.In this case, the temperature of corronil substrate is within the scope of 400～600 DEG C, superficial growth mechanism is deferred in the growth of Graphene, and with adopt fine copper thin film as compared with substrate, when adopting that in substrate, the ratio of corronil is 53: 47, the speed of growth of graphene film is the fastest.Nickel serves the effect promoting graphene growth in graphene growth process.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of process for preparing graphenes by chemical vapour deposition, it is by following technological process:
Step 1, selection monocrystal silicon are substrate, adopt sputtering power respectively 120～200W, the 80～100W of copper target and nickel target to prepare thickness for 3～5 μm of corronil thin film with copper, the double; two target magnetic control co-sputtering method of nickel at monocrystalline silicon surface；
Step 2, by surface deposition have in the reacting furnace that the monocrystal silicon substrate of corronil thin film is transferred to chemical vapour deposition (CVD) (CVD), the helium that flow velocity is 500sccm is passed in described reacting furnace, it is continually fed into 10min, drains the air in described reacting furnace；
Step 3, substrate is risen in 20～40min 400～600 DEG C, backward described reacting furnace in continue to pass into helium, control the pressure in described reacting furnace within the scope of 5～10Torr；
In step 4, maintenance CVD, the pressure of reacting furnace is within the scope of 5～10Torr, base reservoir temperature at 400～600 DEG C, backward described reacting furnace in pass into hydrogen, the flow of hydrogen is 200～300sccm, benzene injection in described reacting furnace, the injection speed of benzene is 100～150 μ l/min；
In step 5, maintenance CVD, the pressure of reacting furnace is within the scope of 5～10Torr, after benzene has been injected, stop pass into hydrogen, backward described reacting furnace in pass into helium, deposition has the monocrystal silicon substrate of corronil thin film to be down to room temperature with 20 DEG C/min speed, is continually fed into helium 10min afterwards；
Step 6, taking-up growth have the substrate of graphene film.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, described step 1 monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries in a nitrogen environment.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, in described step 1, the sputtering power of copper target is preferably 120～150W, and the sputtering power of nickel target is preferably 90～100W.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, copper in described step 1, the double; two target magnetic control co-sputtering method of nickel deposit the condition of corronil at monocrystalline silicon surface, and design parameter is as follows: sputtering chamber back end vacuum is 5.0 × 10-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, in described step 3, the temperature of corronil substrate is 400～500 DEG C.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, in described step 4, the injection speed of benzene is constant speed, and the injection speed of benzene is preferably 120 μ l/min.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, it is 400～600sccm that described step 5 passes into the flow of helium, it is preferred that 450～500sccm.
Preferably, described process for preparing graphenes by chemical vapour deposition, wherein, shifts in described step 6 method of graphene film in corronil substrate:
Step one, polymethyl methacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface；
Step 2, drip have the sample of PMMA to put into FeCl3In solution, after the corronil of sample erodes, the Graphene sample scribbling PMMA swims in FeCl3On solution；
Step 3, the graphene film scribbling PMMA are put in acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, picks up with copper mesh or transfers in other substrates to be measured.
A kind of process for preparing graphenes by chemical vapour deposition provided by the invention; its beneficial effect includes: this preparation method technological process is simple; Productive statistics cost is low; base reservoir temperature is relatively low, expends little energy, selects the copper nickel substrate of proper ratio to improve the speed of growth of graphene film; suitable for scale production; and the graphene product prepared: Area comparison is big, and quality purity is higher, and light transmittance is high.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, to make those skilled in the art can implement according to this with reference to description word.
Embodiment 1
The present embodiment provides a kind of process for preparing graphenes by chemical vapour deposition, through the following steps that prepare:
Step 1, selection monocrystal silicon are substrate, and monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries in a nitrogen environment, and the double; two target magnetic control co-sputtering method of copper, nickel is 5.0 × 10 in sputtering chamber back end vacuum-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa, and copper target sputtering power is that to prepare thickness at monocrystalline silicon surface when being 90W be 4 μm of corronil thin film for 120W, nickel target sputtering power；
Step 2, by surface deposition have in the reacting furnace that the monocrystal silicon substrate of corronil thin film is transferred to chemical vapour deposition (CVD) (CVD), the helium that flow velocity is 500sccm is passed in described reacting furnace, it is continually fed into 10min, drains the air in described reacting furnace；
Step 3, substrate is risen in 20min 400 DEG C, backward described reacting furnace in continue to pass into helium, control the pressure in described reacting furnace at 10Torr；
Step 4, keep in CVD the pressure of reacting furnace at 10Torr, base reservoir temperature at 400 DEG C, backward described reacting furnace in pass into hydrogen, the flow of hydrogen is 200sccm, benzene injection in described reacting furnace, and the injection speed of benzene is 120 μ l/min；
In step 5, maintenance CVD, the pressure of reacting furnace is within the scope of 10Torr, after benzene has been injected, stop passing into hydrogen, backward described reacting furnace in pass into helium, the flow of helium is 500sccm, deposition has the monocrystal silicon substrate of corronil thin film to be down to room temperature with 20 DEG C/min speed, is continually fed into helium 10min afterwards；
Step 6, taking-up growth have the substrate of graphene film.
Step 7, to graphene film not damaged shift: 1) polymethyl methacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface,
2) drip and have the sample of PMMA to put into FeCl3In solution, after the corronil of sample erodes, the Graphene sample scribbling PMMA swims in FeCl3On solution,
3) graphene film scribbling PMMA is put in acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, picks up with copper mesh or transfers in other substrates to be measured.
Embodiment 2
The present embodiment provides a kind of process for preparing graphenes by chemical vapour deposition, through the following steps that prepare:
Step 1, selection monocrystal silicon are substrate, and monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries in a nitrogen environment, and the double; two target magnetic control co-sputtering method of copper, nickel is 5.0 × 10 in sputtering chamber back end vacuum-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa, and copper target sputtering power is that to prepare thickness at monocrystalline silicon surface when being 90W be 4 μm of corronil thin film for 135W, nickel target sputtering power；
Step 2, by surface deposition have in the reacting furnace that the monocrystal silicon substrate of corronil thin film is transferred to chemical vapour deposition (CVD) (CVD), the helium that flow velocity is 500sccm is passed in described reacting furnace, it is continually fed into 10min, drains the air in described reacting furnace；
Step 3, substrate is risen in 20min 400 DEG C, backward described reacting furnace in continue to pass into helium, control the pressure in described reacting furnace at 10Torr；
Step 4, keep in CVD the pressure of reacting furnace at 10Torr, base reservoir temperature at 400 DEG C, backward described reacting furnace in pass into hydrogen, the flow of hydrogen is 200sccm, benzene injection in described reacting furnace, and the injection speed of benzene is 120 μ l/min；
In step 5, maintenance CVD, the pressure of reacting furnace is within the scope of 10Torr, after benzene has been injected, stop passing into hydrogen, backward described reacting furnace in pass into helium, the flow of helium is 500sccm, deposition has the monocrystal silicon substrate of corronil thin film to be down to room temperature with 20 DEG C/min speed, is continually fed into helium 10min afterwards；
Step 6, taking-up growth have the substrate of graphene film.
Step 7, to graphene film not damaged shift: 1) polymethyl methacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface,
2) drip and have the sample of PMMA to put into FeCl3In solution, after the corronil of sample erodes, the Graphene sample scribbling PMMA swims in FeCl3On solution,
3) graphene film scribbling PMMA is put in acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, picks up with copper mesh or transfers in other substrates to be measured.
Embodiment 3
The present embodiment provides a kind of process for preparing graphenes by chemical vapour deposition, through the following steps that prepare:
Step 1, selection monocrystal silicon are substrate, and monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries in a nitrogen environment, and the double; two target magnetic control co-sputtering method of copper, nickel is 5.0 × 10 in sputtering chamber back end vacuum-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa, and copper target sputtering power is that to prepare thickness at monocrystalline silicon surface when being 90W be 4 μm of corronil thin film for 150W, nickel target sputtering power；
Step 2, by surface deposition have in the reacting furnace that the monocrystal silicon substrate of corronil thin film is transferred to chemical vapour deposition (CVD) (CVD), the helium that flow velocity is 500sccm is passed in described reacting furnace, it is continually fed into 10min, drains the air in described reacting furnace；
Step 3, substrate is risen in 20min 400 DEG C, backward described reacting furnace in continue to pass into helium, control the pressure in described reacting furnace at 10Torr；
Step 4, keep in CVD the pressure of reacting furnace at 10Torr, base reservoir temperature at 400 DEG C, backward described reacting furnace in pass into hydrogen, the flow of hydrogen is 200sccm, benzene injection in described reacting furnace, and the injection speed of benzene is 120 μ l/min；
In step 5, maintenance CVD, the pressure of reacting furnace is within the scope of 10Torr, after benzene has been injected, stop passing into hydrogen, backward described reacting furnace in pass into helium, the flow of helium is 500sccm, deposition has the monocrystal silicon substrate of corronil thin film to be down to room temperature with 20 DEG C/min speed, is continually fed into helium 10min afterwards；
Step 6, taking-up growth have the substrate of graphene film.
Step 7, to graphene film not damaged shift: 1) polymethyl methacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface,
2) drip and have the sample of PMMA to put into FeCl3In solution, after the corronil of sample erodes, the Graphene sample scribbling PMMA swims in FeCl3On solution,
3) graphene film scribbling PMMA is put in acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, picks up with copper mesh or transfers in other substrates to be measured.
The corronil component that in above three embodiment, different sputtering powers obtain is in Table 1:
Graphene product index prepared by above-mentioned 3 embodiments is shown in table 2 below
Although embodiment of the present invention are disclosed as above, but listed utilization that it is not restricted in description and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, it is easily achieved other amendment, therefore, under the general concept limited without departing substantially from claim and equivalency range, the present invention is not limited to specific details and shown here as the embodiment with description.
Claims (5)
1. a process for preparing graphenes by chemical vapour deposition, it is characterised in that including:
Step 1, selection monocrystal silicon are substrate, and monocrystal silicon substrate is each ultrasonic cleaning 18～20min in acetone, dehydrated alcohol, deionized water successively, then dries in a nitrogen environment, and the double; two target magnetic control co-sputtering method of copper, nickel is 5.0 × 10 in sputtering chamber back end vacuum-4, argon flow amount is 20sccm, and sputtering time is 30min, and sputtering pressure is 1.0Pa；
The sputtering power of copper target be 135W, nickel target sputtering power when being 90W monocrystalline silicon surface prepare thickness be 4 μm, copper nickel is with the 53:47 corronil thin film being ratio；
Step 2, by surface deposition have in the reacting furnace that the monocrystal silicon substrate of corronil thin film is transferred to chemical vapour deposition (CVD) (CVD), the helium that flow velocity is 500sccm is passed in described reacting furnace, it is continually fed into 10min, drains the air in described reacting furnace；
Step 3, substrate is risen in 20～40min 400～600 DEG C, backward described reacting furnace in continue to pass into helium, control the pressure in described reacting furnace within the scope of 5～10Torr；
In step 4, maintenance CVD, the pressure of reacting furnace is within the scope of 5～10Torr, base reservoir temperature at 400～600 DEG C, backward described reacting furnace in pass into hydrogen, the flow of hydrogen is 200～300sccm, benzene injection in described reacting furnace, the injection speed of benzene is 100～150 μ l/min；
In step 5, maintenance CVD, the pressure of reacting furnace is within the scope of 5～10Torr, after benzene has been injected, stop pass into hydrogen, backward described reacting furnace in pass into helium, deposition has the monocrystal silicon substrate of corronil thin film to be down to room temperature with 20 DEG C/min speed, is continually fed into helium 10min afterwards；
Step 6, taking-up growth have the substrate of graphene film.
2. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, it is characterised in that in described step 3, the temperature of corronil substrate is 400～500 DEG C.
3. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, it is characterised in that in described step 4, the injection speed of benzene is constant speed.
4. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, it is characterised in that it is 400～600sccm that described step 5 passes into the flow of helium.
5. process for preparing graphenes by chemical vapour deposition as claimed in claim 1, it is characterised in that shift in described step 6 method of graphene film in corronil substrate:
Step one, polymethyl methacrylate (PMMA) is dissolved in trace acetone solution, be then coated onto graphene film surface；
Step 2, drip have the sample of PMMA to put into FeCl3In solution, after the corronil of sample erodes, the Graphene sample scribbling PMMA swims in FeCl3On solution；
Step 3, the graphene film scribbling PMMA are put in acetone soln, and after PMMA dissolves, Graphene sample swims in acetone soln, picks up with copper mesh or transfers in other substrates to be measured.
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| CN104328389B (en) * | 2014-10-24 | 2016-08-03 | 中国科学院合肥物质科学研究院 | The preparation method of graphene nano net |
| CN104779015B (en) * | 2015-05-06 | 2017-03-15 | 南京汉能薄膜太阳能有限公司 | The preparation method of transparent graphene conductive film |
| CN106706710A (en) * | 2015-11-11 | 2017-05-24 | 中国科学院上海微***与信息技术研究所 | Nitrogen oxide gas sensor based on sulphur-doped graphene, and preparation method thereof |
| CN106024111A (en) * | 2016-06-24 | 2016-10-12 | 成都天航智虹企业管理咨询有限公司 | Preparation method of conductive thin film |
| CN106158145A (en) * | 2016-06-24 | 2016-11-23 | 成都天航智虹企业管理咨询有限公司 | A kind of preparation method of graphene conductive film |
| CN108033439B (en) * | 2018-01-02 | 2021-02-05 | 电子科技大学 | Graphene low-temperature preparation method for plasma-assisted sputtering of solid carbon source |
| CN114867549A (en) * | 2019-12-19 | 2022-08-05 | 海科材料有限公司 | Method for preparing porous graphene membrane and membrane prepared using same |
| CN113148992B (en) * | 2021-03-31 | 2022-10-25 | 哈尔滨金纳科技有限公司 | Preparation method of small-size graphene |
| CN114107914A (en) * | 2021-11-12 | 2022-03-01 | 航天特种材料及工艺技术研究所 | Preparation method and application of graphene/metal film composite material |
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| CN102050442A (en) * | 2009-11-10 | 2011-05-11 | 三星电子株式会社 | Methods of fabricating graphene using alloy catalyst |
| CN102161482A (en) * | 2011-01-25 | 2011-08-24 | 中国科学院化学研究所 | Method for preparing graphene |
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| CN102050442A (en) * | 2009-11-10 | 2011-05-11 | 三星电子株式会社 | Methods of fabricating graphene using alloy catalyst |
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Address after: 223900 Sihong Province Economic Development Zone, West Ocean Road, No. 6, No. Patentee after: Jiangsu Stick new materials Polytron Technologies Inc Address before: 215400 Taicang Economic Development Zone, Jiangsu, Qingdao West Road, No. 11, No. Patentee before: Suzhou Sidike New Material Science & Technology Co., Ltd. |