CN103086370A - Method for preparing graphene strip by adopting low-temperature chemical vapour deposition - Google Patents
Method for preparing graphene strip by adopting low-temperature chemical vapour deposition Download PDFInfo
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- CN103086370A CN103086370A CN2013100214203A CN201310021420A CN103086370A CN 103086370 A CN103086370 A CN 103086370A CN 2013100214203 A CN2013100214203 A CN 2013100214203A CN 201310021420 A CN201310021420 A CN 201310021420A CN 103086370 A CN103086370 A CN 103086370A
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Abstract
The invention belongs to the field of preparation of semiconductor materials and in particular relates to a method for preparing a graphene strip by adopting low-temperature chemical vapour deposition. The method provided by the invention comprises the following steps of: firstly carrying out electrolytic polishing on a copper foil, then placing the copper foil into a quartz tube reactor, annealing under the condition of hydrogen, and then adjusting flow velocity of the hydrogen to be 2.4-3.0sccm and introducing a liquid carbon source at the temperature of 500-580 DEG C, and growing a graphene strip on the copper foil while pressure is controlled to be 2.0-10.0Torr and growth time is controlled to be 10-50 minutes, so that the graphene strip growing on the copper foil is obtained. According to the method, the copper foil subjected to electrolytic polishing is adopted, so that chemical activity of the surface of the copper foil is higher; and the adopted carbon source is a carbon-containing organic solvent which has the characteristics of aromatic compounds and aliphatic compounds and the characteristics between the characteristics of the aromatic compounds and the characteristics of the aliphatic compounds, and compared with a gas carbon source commonly used in the prior art such as methane, the carbon-containing organic solvent is more beneficial to low-temperature growth of the graphene strip.
Description
Technical field
The invention belongs to the semiconductor material preparation field, be specifically related to a kind of low temperature chemical vapor deposition preparation method of Graphene band.
Background technology
Graphene (graphene) is the material by the two-dimentional honeycomb structure of the tightly packed one-tenth of monolayer carbon atom, the semiconductor material that its unique crystalline structure becomes mono-layer graphite and has zero band gap represents, wherein single-layer graphene nanometer band is because having quantum confined effect and fringing effect, and make the Graphene band can realize adjusting to band gap being expected to be used to transistor device of making high electron mobility and high switching speed etc.
At present, the typical method of preparation Graphene band comprises both at home and abroad: electron beam lithography, chemical method and epitaxial growth method etc., but these methods exist such as: can't accurately control Graphene band cutting ruler cun, can't avoid the problems such as defect and impurity in prepared Graphene band, particularly adopt the growth temperature of the prepared Graphene of vapor growth method higher, its typical growth temperature brings difficulty for manufacture and the application of Graphene even higher than 1000 ℃.
Summary of the invention
Problem for the prior art existence, the invention provides a kind of low temperature chemical vapor deposition (CVD) preparation method of Graphene band, purpose is under lower than the condition of 1000 ℃, directly prepares the smooth of the edge, has regular rectangular single-layer graphene band.
Realize that the technical scheme of the object of the invention carries out according to following steps:
(1) electropolishing Copper Foil: with polished Copper Foil as anode, copper coin is made negative electrode, be inserted into simultaneously two electrodes in electrolytic polishing liquid, controlling current constant is 1.0 ~ 1.5 A, switched on 70 ~ 120 seconds, Copper Foil is carried out electropolishing, and then the Copper Foil after cleaning polishing, dry up standby with nitrogen;
(2) copper foil annealing: the Copper Foil that dries up is put into quartz tube reactor, and be placed in horizontal process furnace flat-temperature zone, an end of quartz tube reactor is connected with the liquid carbon source container with hydrogen cylinder, and the other end is connected with vacuum pump, will be evacuated to 10 in quartz tube reactor
-2Torr passes into the hydrogen that flow velocity is 4.0 ~ 10.0 sccm, adopts simultaneously horizontal process furnace with the speed intensification heating of 5 ~ 50 ℃/min, when being heated to 500 ~ 950 ℃, and insulation 30 ~ 60 min annealing;
(3) Graphene band low-temperature epitaxy: controlling furnace temperature after annealing is 500 ~ 580 ℃, the flow velocity of regulating simultaneously hydrogen is 2.4 ~ 3.0 sccm, pass into the liquid carbon source, enter in reactor with gaseous form under the suction function of liquid carbon source in quartz tube reactor, growing graphene band on Copper Foil, control the quartz tube reactor internal pressure between 2.0 ~ 10.0 Torr, controlling growth time is 10 ~ 50 min;
(4) after growth finished, under vacuum condition, stove was chilled to room temperature, obtains being grown in the Graphene band on Copper Foil.
The formula of described electrolytic polishing liquid is: deionized water 1000 ml, phosphoric acid 500 ml, dehydrated alcohol 500 ml, Virahol 100 ml, urea 9 g.
Described liquid carbon source is to have aromatic series, fatty compounds feature and the carbon containing organic solvent between aromatic series and fatty compounds feature.
Hydrogen is both as reducing gas, again as carrier gas and diluent gas.
Compared with prior art, characteristics of the present invention and beneficial effect are:
(1) growth temperature of the Graphene band of the inventive method is lower than the temperature of CVD method growing graphene of the prior art;
(2) the Graphene band for preparing of the inventive method itself has the rectangle of more level and smooth edge and rule mostly, need not to carry out shape and cuts out;
(3) the black alkene band for preparing of the inventive method is the single-layer graphene band;
(4) in the inventive method, the catalyst substrate material as the Graphene growth is the Copper Foil through electropolishing, makes copper foil surface smoothly and has higher chemical mobility of the surface; The carbon source that adopts is to have aromatic series and fatty compounds feature and the carbon containing organic solvent between aromatic series and fatty compounds feature, compare with the gaseous carbon sources methane that generally adopts in existing CVD technology etc., this class I liquid I is conducive to the low-temperature epitaxy of Graphene band.
Description of drawings
Fig. 1 is the device schematic diagram that low temperature of the present invention prepares the Graphene band;
In figure, 1: horizontal process furnace; 2: quartz tube reactor; 3: the Copper Foil of electropolishing; 4: the liquid carbon source; 5: carbon source is controlled vacuum valve; 6: vacuumometer; 7: ball valve; 8: vacuum pump; 9: hydrogen cylinder.
Fig. 2 is SEM photo and the Raman spectrogram of the Graphene band of the embodiment of the present invention 1 preparation;
Wherein (a) is the SEM photo of the Graphene band of low-temperature epitaxy on the electropolishing Copper Foil;
(b) the typical Laser Raman spectrogram of single-layer graphene band.
Embodiment
Below in conjunction with drawings and Examples in detail the present invention is described in detail.
the device schematic diagram that low temperature chemical vapor deposition of the present invention prepares the Graphene band as shown in Figure 1, comprise horizontal process furnace 1, quartz tube reactor 2, the Copper Foil 3 of electropolishing, liquid carbon source 4, vacuum valve 5, vacuumometer 6, ball valve 7, vacuum pump 8 and hydrogen cylinder, wherein quartz tube reactor 2 is as the reaction growth chamber of Graphene band, be placed in horizontal process furnace 1, the Copper Foil 3 of electropolishing is placed in quartz tube reactor 2, and be advanced in the isothermal reaction district of horizontal process furnace 1, one end of quartz tube reactor 2 is connected by ball valve 7 with vacuum pump 8, the other end is connected with hydrogen cylinder 9 with liquid carbon source 4.
In the embodiment of the present invention, Copper Foil used is that purity is that the thickness that 99.8% Copper Foil U.S. Alfa-Aesar company produces is the Copper Foil of 25 μ m, and cuts into the rectangle that is of a size of 2 cm * 1 cm;
In the embodiment of the present invention, the power supply model of electropolishing is Hewlett Packard 6612 type direct supplys.
Embodiment 1
(1) electropolishing Copper Foil: with polished Copper Foil as anode, thickness is that the copper coin of 1mm is made negative electrode, two electrodes is inserted into composition simultaneously is: deionized water 1000 ml, ortho-phosphoric acid 500 ml, dehydrated alcohol 500 ml, Virahol 100 ml, in the electrolytic polishing liquid of urea 9 g, the control current constant is 1.0A, switched on 120 seconds, Copper Foil is carried out electropolishing, and then the Copper Foil after cleaning polishing, dry up standby with nitrogen;
(2) copper foil annealing: the Copper Foil that dries up is put into quartz tube reactor, and be placed in horizontal process furnace flat-temperature zone, one end of quartz tube reactor is connected with the container that fills liquid carbon source dehydrated alcohol with hydrogen cylinder, and the other end is connected with vacuum pump, will be evacuated to 9 * 10 in quartz tube reactor
-3Torr passes into the hydrogen that flow velocity is 5.8 sccm, adopts simultaneously horizontal process furnace with the speed intensification heating of 20 ℃/min, when being heated to 950 ℃, and insulation 30 min annealing;
(3) Graphene band low-temperature epitaxy: controlling furnace temperature after annealing is 550 ℃, the flow velocity of regulating simultaneously hydrogen is 3.0 sccm, pass into liquid carbon source dehydrated alcohol, enter in reactor with gaseous form under the suction function of dehydrated alcohol in quartz tube reactor, growing graphene band on Copper Foil, control the quartz tube reactor internal pressure at 7.8 Torr, controlling growth time is 30 min;
(4) after growth finished, under vacuum condition, stove was chilled to room temperature, obtains being grown in the Graphene band on Copper Foil.
Adopt FEI Quanta-600 environmental scanning electronic microscope to carry out electron-microscope scanning to the graphene strips band that is grown on Copper Foil, obtain the SEM photo as shown in Fig. 2 (a), the simple spectrum spectrogram of its laser co-focusing Raman spectrum is as shown in Fig. 2 (b), can find out that from Fig. 2 (a) and Fig. 2 (b) the Graphene band of preparing is single-layer graphene, have regular shape.
Embodiment 2
(1) electropolishing Copper Foil: with polished Copper Foil as anode, thickness is that the copper coin of 1mm is made negative electrode, two electrodes is inserted into composition simultaneously is: deionized water 1000 ml, ortho-phosphoric acid 500 ml, dehydrated alcohol 500 ml, Virahol 100 ml, in the electrolytic polishing liquid of urea 9 g, the control current constant is 1.2A, switched on 90 seconds, Copper Foil is carried out electropolishing, and then the Copper Foil after cleaning polishing, dry up standby with nitrogen;
(2) copper foil annealing: the Copper Foil that dries up is put into quartz tube reactor, and be placed in horizontal process furnace flat-temperature zone, one end of quartz tube reactor is connected with the container that fills liquid carbon source tetrahydrofuran (THF) with hydrogen cylinder, and the other end is connected with vacuum pump, will be evacuated to 10 in quartz tube reactor
-2Torr passes into the hydrogen that flow velocity is 4.0sccm, adopts simultaneously horizontal process furnace with the speed intensification heating of 5 ℃/min, when being heated to 500 ℃, and insulation 60 min annealing;
(3) Graphene band low-temperature epitaxy: controlling furnace temperature after annealing is 500 ℃, the flow velocity of regulating simultaneously hydrogen is 2.4 sccm, pass into liquid carbon source tetrahydrofuran (THF), enter in reactor with gaseous form under the suction function of liquid carbon source tetrahydrofuran (THF) in quartz tube reactor, growing graphene band on Copper Foil, control the quartz tube reactor internal pressure at 10.0 Torr, controlling growth time is 50 min;
(4) after growth finished, under vacuum condition, stove was chilled to room temperature, obtains being grown in the Graphene band on Copper Foil, and after testing, the Graphene band of preparing is single-layer graphene, has regular shape.
Embodiment 3
(1) electropolishing Copper Foil: with polished Copper Foil as anode, thickness is that the copper coin of 1mm is made negative electrode, two electrodes is inserted into composition simultaneously is: deionized water 1000 ml, ortho-phosphoric acid 500 ml, dehydrated alcohol 500 ml, Virahol 100 ml, in the electrolytic polishing liquid of urea 9 g, the control current constant is 1.5A, switched on 70 seconds, Copper Foil is carried out electropolishing, and then the Copper Foil after cleaning polishing, dry up standby with nitrogen;
(2) copper foil annealing: the Copper Foil that dries up is put into quartz tube reactor, and be placed in horizontal process furnace flat-temperature zone, one end of quartz tube reactor is connected with the container that fills liquid carbon source dimethylbenzene with hydrogen cylinder, and the other end is connected with vacuum pump, will be evacuated to 8 * 10 in quartz tube reactor
-3Torr passes into the hydrogen that flow velocity is 10.0sccm, adopts simultaneously horizontal process furnace with the speed intensification heating of 50 ℃/min, when being heated to 800 ℃, and insulation 45 min annealing;
(3) Graphene band low-temperature epitaxy: controlling furnace temperature after annealing is 580 ℃, the flow velocity of regulating simultaneously hydrogen is 2.8 sccm, pass into liquid carbon source dimethylbenzene, enter in reactor with gaseous form under the suction function of liquid carbon source dimethylbenzene in quartz tube reactor, growing graphene band on Copper Foil, control the quartz tube reactor internal pressure at 2.0 Torr, controlling growth time is 10 min;
(4) after growth finished, under vacuum condition, stove was chilled to room temperature, obtains being grown in the Graphene band on Copper Foil, and the Graphene band of preparing is single-layer graphene, has regular shape.
Claims (3)
1. the low temperature chemical vapor deposition preparation method of a Graphene band is characterized in that carrying out according to following steps:
(1) electropolishing Copper Foil: with polished Copper Foil as anode, copper coin is made negative electrode, be inserted into simultaneously two electrodes in electrolytic polishing liquid, controlling current constant is 1.0 ~ 1.5 A, switched on 70 ~ 120 seconds, Copper Foil is carried out electropolishing, and then the Copper Foil after cleaning polishing, dry up standby with nitrogen;
(2) copper foil annealing: the Copper Foil that dries up is put into quartz tube reactor, and be placed in horizontal process furnace flat-temperature zone, an end of quartz tube reactor is connected with the liquid carbon source container with hydrogen cylinder, and the other end is connected with vacuum pump, will be evacuated to 10 in quartz tube reactor
-2Torr passes into the hydrogen that flow velocity is 4.0 ~ 10.0 sccm, adopts simultaneously horizontal process furnace with the speed intensification heating of 5 ~ 50 ℃/min, when being heated to 500 ~ 950 ℃, and insulation 30 ~ 60 min annealing;
(3) Graphene band low-temperature epitaxy: controlling furnace temperature after annealing is 500 ~ 580 ℃, the flow velocity of regulating simultaneously hydrogen is 2.4 ~ 3.0 sccm, pass into the liquid carbon source, enter in reactor with gaseous form under the suction function of liquid carbon source in quartz tube reactor, growing graphene band on Copper Foil, control the quartz tube reactor internal pressure between 2.0 ~ 10.0 Torr, controlling growth time is 10 ~ 50 min;
(4) after growth finished, under vacuum condition, stove was chilled to room temperature, obtains being grown in the Graphene band on Copper Foil.
2. the low temperature chemical vapor deposition preparation method of a kind of Graphene band according to claim 1, the formula that it is characterized in that described electrolytic polishing liquid is: with deionized water 1000 ml, and phosphoric acid 500 ml, dehydrated alcohol 500 ml, Virahol 100 ml, urea 9 g mix.
3. the low temperature chemical vapor deposition preparation method of a kind of Graphene band according to claim 2, is characterized in that described liquid carbon source is to have aromatic series, fatty compounds feature and the carbon containing organic solvent between aromatic series and fatty compounds feature.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211054A (en) * | 2014-09-09 | 2014-12-17 | 中国科学院化学研究所 | Method for controllably preparing graphene |
| CN104773725A (en) * | 2015-04-09 | 2015-07-15 | 厦门大学 | Method for preparing graphene by using low-temperature plasmas |
| CN105439126A (en) * | 2014-09-01 | 2016-03-30 | 华北电力大学 | Simple preparation method of millimeter level monocrystalline graphene |
| CN105803602A (en) * | 2015-01-02 | 2016-07-27 | 中原工学院 | Method for preparing graphene fiber through graphene film twisting forming method |
| CN105928365A (en) * | 2016-05-05 | 2016-09-07 | 武汉拓材科技有限公司 | Quartz vessel carburizing device and method used for preparation of high-purity material |
| CN107815664A (en) * | 2017-10-24 | 2018-03-20 | 中国科学技术大学 | Chemical vapor depsotition equipment, method and purposes |
| CN108211811A (en) * | 2017-12-29 | 2018-06-29 | 广东工业大学 | A kind of graphene oxide filters film manufacturing method |
| CN109444202A (en) * | 2018-09-13 | 2019-03-08 | 江苏大学 | A kind of experimental detection device and method preparing graphene using laser |
| CN109455704A (en) * | 2018-12-07 | 2019-03-12 | 四川聚创石墨烯科技有限公司 | A kind of graphene continuous process system |
| CN111517309A (en) * | 2020-04-29 | 2020-08-11 | 吴琼 | Method and system for growing large-area few-layer graphene by using small molecules |
| CN111826712A (en) * | 2019-04-15 | 2020-10-27 | 中国科学院化学研究所 | Method for preparing wafer-level uniform hexagonal boron nitride film |
| CN112661140A (en) * | 2020-12-11 | 2021-04-16 | 上海交通大学 | Preparation method of novel graphene nano narrow band |
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Cited By (17)
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| CN105439126A (en) * | 2014-09-01 | 2016-03-30 | 华北电力大学 | Simple preparation method of millimeter level monocrystalline graphene |
| CN105439126B (en) * | 2014-09-01 | 2017-12-22 | 华北电力大学 | A kind of grade single crystal graphene preparation method |
| CN104211054A (en) * | 2014-09-09 | 2014-12-17 | 中国科学院化学研究所 | Method for controllably preparing graphene |
| CN105803602A (en) * | 2015-01-02 | 2016-07-27 | 中原工学院 | Method for preparing graphene fiber through graphene film twisting forming method |
| CN105803602B (en) * | 2015-01-02 | 2018-03-09 | 中原工学院 | The method that the graphene film twisting method of forming prepares graphene fiber |
| CN104773725A (en) * | 2015-04-09 | 2015-07-15 | 厦门大学 | Method for preparing graphene by using low-temperature plasmas |
| CN105928365A (en) * | 2016-05-05 | 2016-09-07 | 武汉拓材科技有限公司 | Quartz vessel carburizing device and method used for preparation of high-purity material |
| CN105928365B (en) * | 2016-05-05 | 2017-12-12 | 武汉拓材科技有限公司 | A kind of silica ware cementing plant prepared for high-purity material and method |
| CN107815664A (en) * | 2017-10-24 | 2018-03-20 | 中国科学技术大学 | Chemical vapor depsotition equipment, method and purposes |
| CN108211811A (en) * | 2017-12-29 | 2018-06-29 | 广东工业大学 | A kind of graphene oxide filters film manufacturing method |
| CN109444202A (en) * | 2018-09-13 | 2019-03-08 | 江苏大学 | A kind of experimental detection device and method preparing graphene using laser |
| CN109455704A (en) * | 2018-12-07 | 2019-03-12 | 四川聚创石墨烯科技有限公司 | A kind of graphene continuous process system |
| CN109455704B (en) * | 2018-12-07 | 2021-01-22 | 四川聚创石墨烯科技有限公司 | Graphene continuous production system |
| CN111826712A (en) * | 2019-04-15 | 2020-10-27 | 中国科学院化学研究所 | Method for preparing wafer-level uniform hexagonal boron nitride film |
| CN111517309A (en) * | 2020-04-29 | 2020-08-11 | 吴琼 | Method and system for growing large-area few-layer graphene by using small molecules |
| CN111517309B (en) * | 2020-04-29 | 2023-07-14 | 吴琼 | Method and system for growing large-area few-layer graphene by using small molecules |
| CN112661140A (en) * | 2020-12-11 | 2021-04-16 | 上海交通大学 | Preparation method of novel graphene nano narrow band |
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Application publication date: 20130508 |