CN102560414A - Method for preparing graphene on 3C-SiC substrate - Google Patents
Method for preparing graphene on 3C-SiC substrate Download PDFInfo
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- CN102560414A CN102560414A CN2012100076853A CN201210007685A CN102560414A CN 102560414 A CN102560414 A CN 102560414A CN 2012100076853 A CN2012100076853 A CN 2012100076853A CN 201210007685 A CN201210007685 A CN 201210007685A CN 102560414 A CN102560414 A CN 102560414A
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Abstract
The invention discloses a method for preparing graphene on a 3C-SiC substrate, which mainly solves the problems that the graphene prepared by prior technology has small area and uneven layer numbers. The steps include: developing a layer of carbonization layer as a transition on a 4 to 12 inches of Si substrate base piece, performing a development of a 3C-SiC hetero-epitaxy film at the temperature between 1150 DEG C and 1300 DEG C, having C3H8 and SiH4 as development gas sources, subjecting the 3C-SiC at the temperature between 800 DEG C and 1000 DEG C and CCl4 in gas state to a reaction so as to produce a double layer carbon film, producing a double layer grapheme by annealing the double layer carbon film for 10 to 20 minutes in the Ar gas at the temperature between 1000 DEG C to 1100 DEG C. The method for preparing graphene on the 3C-SiC substrate has the advantages that the double layer graphene has a large area, smooth surface and low void ratio, and can be used for sealing gas and liquid.
Description
Technical field
The invention belongs to microelectronics technology, relate to a kind of semiconductor film material and preparation method thereof, specifically is the method for substrate preparation Graphene with 3C-SiC.
Technical background
It is in 2004 that Graphene appears in the laboratory, and at that time, two scientist An Delie Jim of Univ Manchester UK and the Ke Siteyanuowo Lip river husband that disappears found that they can obtain more and more thinner graphite flake with a kind of very simple method.They separate graphite flake from graphite, the two sides with thin slice is bonded on a kind of special adhesive tape then, tears adhesive tape, just can be divided into two graphite flake.Operation so constantly, last so thin slice is more and more thinner, they have obtained the thin slice that only is made up of one deck carbon atom, Here it is Graphene.From now on, the novel method of preparation Graphene emerges in an endless stream, but uses maximum mainly contain following two kinds:
1. micromechanics is peeled off method: directly graphene platelet is cut down from bigger crystal.Novoselovt in 2004 etc. have prepared single-layer graphene in this way; And can be at stable existence under the external environment; See document " K.S.Novoselovt, science, (2004) " Electric field effect in atomically thin carbon films " ".The typical case preparation method is that the pyrolytic graphite of or introducing defective expanded with other a kind of material rubs, and the surface of body phase graphite can produce the flaky crystal of wadding, in these wad a quilt with cotton flaky crystal, contains the Graphene of individual layer.But shortcoming is this method is the graphene platelet that the thin slice that utilizes the friction graphite surface to obtain filters out individual layer, and its size is wayward, and factory length is enough supplied the graphene platelet of usefulness reliably.
2. thermolysis SiC method: to remove Si through lip-deep SiC is decomposed, residual subsequently carbon forms Graphene with the monocrystal SiC heating.Yet the monocrystal SiC that uses in the SiC thermolysis is very expensive, and the Graphene that grows out is island and distributes, and the number of plies is inhomogeneous, and size is less, is difficult to large-area manufacturing Graphene.
Summary of the invention
The objective of the invention is to avoid the deficiency of above-mentioned prior art, propose a kind of method that on the 3C-SiC substrate, prepares Graphene,, be implemented in large-area manufacturing Graphene on the 3C-SiC substrate to improve surface flatness, reduce porosity, to reduce cost.
For realizing above-mentioned purpose, preparation method of the present invention may further comprise the steps:
(1) the Si substrate base to the 4-12 inch carries out standard cleaning;
(2) the Si substrate base after will cleaning is put into CVD system response chamber, reaction chamber is vacuumized reach 10
-7The mbar rank;
(3) at H
2Progressively be warming up to 950 ℃-1150 ℃ of carbonization temperatures under the situation of protection, feeding flow is the C of 30ml/min
3H
8, substrate is carried out carbonization 3-7min, growth one deck carburization zone;
(4) be warming up to 1150 ℃-1300 ℃ of growth temperatures rapidly, feed C
3H
8And SiH
4, carry out 3C-SiC hetero epitaxy growth for Thin Film, the time is 36-60min, then at H
2Protection progressively is cooled to room temperature down, accomplishes the growth of 3C-SiC epitaxial film;
(5) the good 3C-SiC print of will growing places silica tube, is heated to 800-1000 ℃;
(6) heating CCl
4To 60-80 ℃, utilize Ar gas to carry CCl
4Steam gets in the silica tube and reacts with 3C-SiC, generates double-deck carbon film, and the Ar gas velocity is 50-80ml/min, and the reaction times is 30-120min;
(7) after reaction finishes, place Ar gas to be 1000-1100 ℃ the double-deck carbon film print that generates and annealed 10-20 minute down, reconstitute double-layer graphite alkene in temperature.
The present invention compared with prior art has following advantage:
The present invention since growth during 3C-SiC earlier on the Si substrate growth one deck carburization zone as transition, and then growth 3C-SiC, thereby the 3C-SiC quality of growth is high.
But the present invention since the 3C-SiC heteroepitaxial growth on the Si disk, and Si disk size can reach 12 inches, thus with this method can growing large-area Graphene, and low price.
3. the present invention is owing to utilize 3C-SiC and CCl
4Gas reaction, thereby the double-layer graphite alkene smooth surface that generates, porosity is low, can be used for the sealing to gas and liquid.
Description of drawings
Fig. 1 is the device synoptic diagram that the present invention prepares Graphene;
Fig. 2 is the schema that the present invention prepares Graphene.
Embodiment
With reference to Fig. 1, preparation equipment of the present invention is mainly by three-way valve 3, there-necked flask 10, and water-bath 11, silica tube 5, resistance furnace 6 is formed; Three-way valve 3 links to each other with silica tube 5 through first channel 1, link to each other with the left side mouth of there-necked flask 10 through second passage 2, and the right side mouth of there-necked flask 10 links to each other with silica tube 5, and CCl is housed in the there-necked flask
4Liquid, and it is placed in the water-bath 11, and silica tube 5 is placed in the resistance furnace 6.
With reference to Fig. 2, making method of the present invention provides following three kinds of embodiment.
Embodiment 1
Step 1: remove the sample surfaces pollutent.
4 inches Si substrate bases are carried out cleaning surfaces handle, promptly use NH earlier
4OH+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove ionic contamination.
Step 2: the Si substrate base is put into CVD system response chamber, reaction chamber is vacuumized reach 10
-7The mbar rank.
Step 3: growth carburization zone.
Under the situation of H2 protection, reaction chamber temperature is risen to 950 ℃ of carbonization temperatures, feeding flow to reaction chamber then is the C of 30ml/min
3H
8, growth one deck carburization zone on the Si substrate, growth time is 7min.
Step 4: growth 3C-SiC epitaxial film on carburization zone.
Reaction chamber temperature is risen to 1150 ℃ of growth temperatures rapidly, feed the SiH that flow is respectively 15ml/min and 30ml/min
4And C
3H
8, carrying out 3C-SiC hetero epitaxy growth for Thin Film, growth time is 60min; Then at H
2Protection progressively is cooled to room temperature down, accomplishes the growth of 3C-SiC epitaxial film.
Step 5: with the 3C-SiC print silica tube of packing into, and the exhaust heating.
(5.1) the good 3C-SiC epitaxial film print of will growing takes out from CVD system response chamber and is placed on the silica tube 5, places silica tube the thermal site that receives of resistance furnace 6;
(5.2) resistance to air loss of the whole preparation equipment of inspection, feeding flow velocitys from inlet mouth 4 is the Ar gas of 80ml/min, and utilizes three-way valve 3 control Ar gas to get into from first channel 1 silica tube was carried out emptying 30 minutes, and air in the silica tube 7 is discharged from the air outlet;
(5.3) open the resistance furnace power switch, be warming up to 800 ℃.
Step 6: the double-deck carbon film of growing.
(6.1) bath 11 power supplys of fetching boiling water are to being equipped with CCl
4The there-necked flask 10 of liquid is heated to 60 ℃;
(6.2) after resistance furnace reaches 800 ℃ of setting, the swivel tee valve, making flow velocity is that the Ar gas of 50ml/min flows into there-necked flasks from second passage 2, and carries CCl
4Steam gets into silica tube, makes gaseous state CCl
4React in silica tube with 3C-SiC, generate double-deck carbon film, the reaction times is 30 minutes.
Step 7: the double-deck carbon film of generation reconstitutes double-layer graphite alkene.
(7.1) after reaction finished, the swivel tee valve made Ar gas turn to first channel to get into silica tube rapidly, and the flow velocity of Ar gas is adjusted into 25ml/min from 50ml/min;
(7.2) resistance furnace temperature is risen to 1000 ℃ rapidly, the double-deck carbon film of generation was annealed 20 minutes, reconstitute double-layer graphite alkene; Close resistance furnace power supply and water-bath power supply then, make double-layer graphite alkene under the Ar gas shiled, be cooled to room temperature, and the bath water port 9 of fetching boiling water, behind the hot water of draining, introduce cold water from water-in 8, make CCl
4The liquid fast cooling.
Embodiment 2
Step 1: remove the sample surfaces pollutent.
8 inches Si substrate bases are carried out cleaning surfaces handle, promptly use NH earlier
4OH+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove ionic contamination.
Step 2: the Si substrate base is put into CVD system response chamber, reaction chamber is vacuumized reach 10
-7The mbar rank.
Step 3: growth carburization zone.
At H
2Under the situation of protection reaction chamber temperature is risen to 1050 ℃ of carbonization temperatures, feeding flow to reaction chamber then is the C of 30ml/min
3H
8, growth one deck carburization zone on the Si substrate, growth time is 5min.
Step 4: growth 3C-SiC epitaxial film on carburization zone.
Reaction chamber temperature is risen to 1200 ℃ of growth temperatures rapidly, feed the SiH that flow is respectively 20ml/min and 40ml/min
4And C
3H
8, carrying out 3C-SiC hetero epitaxy growth for Thin Film, growth time is 45min; Then at H
2Protection progressively is cooled to room temperature down, accomplishes the growth of 3C-SiC epitaxial film.
Step 5: with the 3C-SiC print silica tube of packing into, and the exhaust heating.
The 3C-SiC epitaxial film print that growth is good takes out from CVD system response chamber and is placed on the silica tube 5, places silica tube the thermal site that receives of resistance furnace 6; Check the resistance to air loss of whole preparation equipment, feeding flow velocity from inlet mouth 4 is the Ar gas of 80ml/min, and utilizes three-way valve 3 control Ar gas to get into from first channel 1 silica tube was carried out emptying 30 minutes, makes air 7 discharges from the air outlet in the silica tube; Open the resistance furnace power switch, be warming up to 900 ℃.
Step 6: the double-deck carbon film of growing.
Step 7: the double-deck carbon film of generation reconstitutes double-layer graphite alkene.
After reaction finished, the swivel tee valve made Ar gas turn to first channel to get into silica tube rapidly, and the flow velocity of Ar gas is adjusted into 80ml/min from 60ml/min; Resistance furnace temperature is risen to 1050 ℃ rapidly, the double-deck carbon film of generation was annealed 15 minutes, reconstitute double-layer graphite alkene; Close resistance furnace power supply and water-bath power supply then, make double-layer graphite alkene under the Ar gas shiled, be cooled to room temperature, and the bath water port 9 of fetching boiling water, behind the hot water of draining, introduce cold water from water-in 8, make CCl
4The liquid fast cooling.
Embodiment 3
Steps A: 12 inches Si substrate bases are carried out cleaning surfaces handle, promptly use NH earlier
4OH+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove ionic contamination.
Step B: the Si substrate base is put into CVD system response chamber, reaction chamber is vacuumized reach 10
-7The mbar rank.
Step C: at H
2Under the situation of protection reaction chamber temperature is risen to 1150 ℃ of carbonization temperatures, feeding flow to reaction chamber then is the C of 30ml/min
3H
8, continue 3min, with growth one deck carburization zone on the Si substrate.
Step D: reaction chamber temperature is risen to 1300 ℃ of growth temperatures rapidly, feed the SiH that flow is respectively 25ml/min and 50ml/min
4And C
3H
8, carry out 3C-SiC hetero epitaxy growth for Thin Film 36min; Then at H
2Protection progressively is cooled to room temperature down.
Step e: the good 3C-SiC epitaxial film print of will growing takes out from CVD system response chamber and is placed on the silica tube 5, places silica tube the thermal site that receives of resistance furnace 6; Check the resistance to air loss of whole preparation equipment, feeding flow velocity from inlet mouth 4 is the Ar gas of 80ml/min, and utilizes three-way valve 3 control Ar gas to get into from first channel 1 silica tube was carried out emptying 30 minutes, makes air 7 discharges from the air outlet in the silica tube; Open the resistance furnace power switch, be warming up to 1000 ℃.
Step F: bath 11 power supplys of fetching boiling water, to CCl is housed
4The there-necked flask 10 of liquid is heated to 70 ℃; Reach 1000 ℃ of setting when resistance furnace after, the swivel tee valve, making flow velocity is that the Ar gas of 80ml/min flows into there-necked flasks from second passage 2, and carries CCl
4Steam gets into silica tube, makes gaseous state CCl
4In silica tube, reacted 120 minutes with 3C-SiC, generate double-deck carbon film.
Step G: after reaction finished, the swivel tee valve made Ar gas turn to first channel to get into silica tube rapidly, and the flow velocity of Ar gas is adjusted into 100ml/min from 80ml/min; Resistance furnace temperature is risen to 1100 ℃ rapidly, the double-deck carbon film of generation was annealed 10 minutes, reconstitute double-layer graphite alkene; Close resistance furnace power supply and water-bath power supply then, make double-layer graphite alkene under the Ar gas shiled, be cooled to room temperature, and the bath water port 9 of fetching boiling water, behind the hot water of draining, introduce cold water from water-in 8, make CCl
4The liquid fast cooling.
Claims (3)
1. method that on the 3C-SiC substrate, prepares Graphene may further comprise the steps:
(1) the Si substrate base to the 4-12 inch carries out standard cleaning;
(2) the Si substrate base after will cleaning is put into CVD system response chamber, reaction chamber is vacuumized reach 10
-7The mbar rank;
(3) at H
2Progressively be warming up to 950 ℃-1150 ℃ of carbonization temperatures under the situation of protection, feeding flow is the C of 30ml/min
3H
8, substrate is carried out carbonization 3-7min, growth one deck carburization zone;
(4) be warming up to 1150 ℃-1300 ℃ of growth temperatures rapidly, feed C
3H
8And SiH
4, carry out 3C-SiC hetero epitaxy growth for Thin Film, the time is 36-60min, then at H
2Protection progressively is cooled to room temperature down, accomplishes the growth of 3C-SiC epitaxial film;
(5) the good 3C-SiC print of will growing places silica tube, is heated to 800-1000 ℃;
(6) heating CCl
4To 60-80 ℃, utilize Ar gas to carry CCl
4Steam gets in the silica tube and reacts with 3C-SiC, generates double-deck carbon film, and the Ar gas velocity is 50-80ml/min, and the reaction times is 30-120min;
(7) after reaction finishes, place Ar gas to be 1000-1100 ℃ the double-deck carbon film print that generates and annealed 10-20 minute down, reconstitute double-layer graphite alkene in temperature.
2. the method that on the 3C-SiC substrate, prepares Graphene according to claim 1 is characterized in that the SiH of the said feeding of step (4)
4And C
3H
8, its flow is respectively 15-25ml/min and 30-50ml/min.
3. the method that on the 3C-SiC substrate, prepares Graphene according to claim 1, the flow velocity of Ar gas is 25-100ml/min when it is characterized in that said step (7) annealing.
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| CN102903616A (en) * | 2012-10-22 | 2013-01-30 | 西安电子科技大学 | ZnO substrate-based graphene CVD direct epitaxial growth method and manufactured device |
| CN102903617A (en) * | 2012-10-22 | 2013-01-30 | 西安电子科技大学 | GaN substrate-based graphene CVD direct epitaxial growth method and manufactured device |
| CN102903618A (en) * | 2012-10-22 | 2013-01-30 | 西安电子科技大学 | AlN substrate-based graphene CVD direct epitaxial growth method and manufactured device |
| CN104120402A (en) * | 2014-08-08 | 2014-10-29 | 苏州宏久航空防热材料科技有限公司 | Preparation method of graphene-SiC film |
| CN104217930B (en) * | 2013-06-05 | 2017-08-25 | 中芯国际集成电路制造(上海)有限公司 | A kind of forming method of graphene pattern |
| CN107845567A (en) * | 2017-09-25 | 2018-03-27 | 重庆文理学院 | Graphene double heterojunction and preparation method thereof |
| GB2572271A (en) * | 2015-08-14 | 2019-09-25 | Paragraf Ltd | A method of producing a two-dimensional material |
| CN110323126A (en) * | 2019-04-15 | 2019-10-11 | 武汉理工大学 | A kind of preparation method of Si/SiC/ grapheme material |
| CN116514112A (en) * | 2023-06-09 | 2023-08-01 | 中电科先进材料技术创新有限公司 | Preparation method of large-area graphene on silicon surface |
-
2012
- 2012-01-03 CN CN2012100076853A patent/CN102560414A/en active Pending
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| CN102903616A (en) * | 2012-10-22 | 2013-01-30 | 西安电子科技大学 | ZnO substrate-based graphene CVD direct epitaxial growth method and manufactured device |
| CN102903617A (en) * | 2012-10-22 | 2013-01-30 | 西安电子科技大学 | GaN substrate-based graphene CVD direct epitaxial growth method and manufactured device |
| CN102903618A (en) * | 2012-10-22 | 2013-01-30 | 西安电子科技大学 | AlN substrate-based graphene CVD direct epitaxial growth method and manufactured device |
| CN102903618B (en) * | 2012-10-22 | 2015-07-29 | 西安电子科技大学 | Based on the direct epitaxial growth method of Graphene CVD of AlN substrate and the device of manufacture |
| CN102903617B (en) * | 2012-10-22 | 2015-09-09 | 西安电子科技大学 | Based on the direct epitaxial growth method of Graphene CVD of GaN substrate and the device of manufacture |
| CN104217930B (en) * | 2013-06-05 | 2017-08-25 | 中芯国际集成电路制造(上海)有限公司 | A kind of forming method of graphene pattern |
| CN104120402A (en) * | 2014-08-08 | 2014-10-29 | 苏州宏久航空防热材料科技有限公司 | Preparation method of graphene-SiC film |
| GB2572271A (en) * | 2015-08-14 | 2019-09-25 | Paragraf Ltd | A method of producing a two-dimensional material |
| US10593546B2 (en) | 2015-08-14 | 2020-03-17 | Paragraf Ltd. | Method of producing a two-dimensional material |
| GB2572271B (en) * | 2015-08-14 | 2020-04-29 | Paragraf Ltd | A Doped Graphene Sheet |
| US11217447B2 (en) | 2015-08-14 | 2022-01-04 | Paragraf Ltd. | Method of producing a two-dimensional material |
| US11456172B2 (en) | 2015-08-14 | 2022-09-27 | Paragraf Ltd. | Method of producing a two-dimensional material |
| US11848206B2 (en) | 2015-08-14 | 2023-12-19 | Paragraf Ltd. | Method of producing a two-dimensional material |
| CN107845567A (en) * | 2017-09-25 | 2018-03-27 | 重庆文理学院 | Graphene double heterojunction and preparation method thereof |
| CN110323126A (en) * | 2019-04-15 | 2019-10-11 | 武汉理工大学 | A kind of preparation method of Si/SiC/ grapheme material |
| CN116514112A (en) * | 2023-06-09 | 2023-08-01 | 中电科先进材料技术创新有限公司 | Preparation method of large-area graphene on silicon surface |
| CN116514112B (en) * | 2023-06-09 | 2023-12-19 | 中电科先进材料技术创新有限公司 | Preparation method of large-area graphene on silicon surface |
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Application publication date: 20120711 |