CN102936011A - Ni film annealing patterned graphene preparation method based on 3C-SiC/chlorine gas reaction - Google Patents
Ni film annealing patterned graphene preparation method based on 3C-SiC/chlorine gas reaction Download PDFInfo
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- CN102936011A CN102936011A CN2012104845328A CN201210484532A CN102936011A CN 102936011 A CN102936011 A CN 102936011A CN 2012104845328 A CN2012104845328 A CN 2012104845328A CN 201210484532 A CN201210484532 A CN 201210484532A CN 102936011 A CN102936011 A CN 102936011A
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Abstract
The invention discloses an Ni film annealing patterned graphene preparation method based on 3C-SiC/chlorine gas reaction, which mainly solves the problem that the graphene prepared by the prior art can cause damage and result in electron mobility reduction when being used for photoetching technology as a transistor channeling material. The preparation method comprises the following steps: (1) growing a carbonization layer on an Si substrate as a transition layer; (2) growing a 3C-SiC film on the carbonization layer; (3) depositing SiO2 on the surface of the 3C-SiC film, and etching a pattern on the SiO2; (4) reacting the patterned sample wafer with Cl2 to generate a carbon film; (5) removing the SiO2 except the pattern; (6) depositing an Ni film on the carbon film by using an electron beam; and (7) putting the sample wafer with the deposited Ni film in Ar gas, and annealing for 15-30 minutes so that the carbon film reconstitutes the patterned graphene in the pattern position. The invention has the advantages of simple technique and high safety; the graphene can be directly used as a conducting channel without photoetching when making a transistor on the graphene; and the graphene can be used for making graphene transistors with superhigh mobility.
Description
Technical field
The invention belongs to microelectronics technology, relate to a kind of semiconductor film material and preparation method thereof, specifically be based on the Ni film annealing patterned graphene preparation method of 3C-SiC and chlorine reaction.
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, then the two sides with thin slice is bonded on a kind of special adhesive tape, tears adhesive tape, just can be divided into two graphite flake.Constantly like this operation, last so thin slice is more and more thinner, they have obtained the thin slice that only is made of one deck carbon atom, Here it is Graphene.After this, the novel method of preparation Graphene emerges in an endless stream.Present preparation method mainly contains two kinds:
The first thermolysis SiC method, to remove Si by lip-deep SiC is decomposed, residual carbon forms Graphene to this method subsequently 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 when making device because photoetching process can make the electronic mobility of Graphene reduce, thereby affected device performance.
The second chemical Vapor deposition process, this method provides a kind of effective ways of controlled preparation Graphene, it is with planar substrates, place the decomposable presoma of high temperature such as metallic film, metal single crystal etc., in the atmosphere such as methane, ethene, make carbon atom be deposited on substrate surface by high temperature annealing and form Graphene, at last with obtaining independently graphene film after the chemical corrosion method removal metal base.Can regulate and control the growth of Graphene by the type of selecting substrate, the temperature of growth, the parameters such as flow of presoma, such as growth velocity, thickness, area etc., the shortcoming of this method maximum is that the graphene sheet layer and the substrate that obtain interact strong, lost the character of many Graphenes, and the continuity of Graphene not fine.
Graphene has been proved to be the preparation that can be applied to multiple electron device, such as molecule sensor, field-effect transistor, solar cell etc.Based on the preparation of micro-nano device, usually need to carry out graphically Graphene, Graphene graphic method commonly used has at present:
1) photolithography.The big area Graphene is carried out photoetching, ion etching technique, obtain patterned Graphene, the graphical precision of this method is high, but technology difficulty is large, easily Graphene is polluted and damages in the technological process;
2) direct growth method.Transfer to the components and parts substrate at the patterned Graphene of metallic film base growth, this method need not to use follow-up photoengraving technique, but can't accurately navigate to Graphene on the substrate again;
3) nano impression method.Have the place of figure to impress out Graphene at needs, this method is convenient and simple, but can't obtain comparatively complicated figure, and the template preparation cost is also very high.
Summary of the invention
The object of the invention is to for above-mentioned the deficiencies in the prior art, a kind of Ni film annealing patterned graphene preparation method based on 3C-SiC and chlorine reaction is proposed, to realize on the 3C-SiC of Si substrate epitaxial film optionally Fast Growth patterned graphene, make the technological process that does not need to carry out etching in the follow-up manufacturing device process, avoided Graphene is polluted and damages, thereby the electronic mobility that guarantees Graphene is stable, improves device performance.
For achieving the above object, preparation method of the present invention may further comprise the steps:
(1) the Si substrate base of 4-12 inch carried 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
2Protection is lower, makes reaction chamber progressively be warming up to 900 ℃-1200 ℃ of carbonization temperatures, passes into the C that flow is 30sccm
3H
8, substrate is carried out carbonization 5-10min, growth one deck carburization zone;
(4) reaction chamber is warming up to 1200 ℃-1300 ℃, passes into C
3H
8And SiH
4, carrying out the 3C-SiC thin film heterogeneity epitaxial growth, growth time is 30-60min, then at H
2Protection is lower progressively to be cooled to room temperature, finishes the growth of 3C-SiC film;
(5) utilize plasma enhanced chemical vapor deposition PECVD method, the thick SiO of deposit one deck 0.5-1.2 μ m at the good 3C-SiC film surface of growth
2Mask layer;
(6) at SiO
2Mask surface is coated with one deck photoresist material, carves the window identical with the substrate shape of the device of required making at mask again, exposes 3C-SiC, forms the figure identical with window shape;
(7) patterned print is placed silica tube, be heated to 700-1100 ℃;
(8) in silica tube, pass into Ar gas and Cl
2The mixed gas of gas continues 3-5min, makes Cl
2React with exposed 3C-SiC, generate carbon film;
(9) the carbon film print that generates is placed buffered hydrofluoric acid solution to remove the SiO outside the figure
2
(10) utilize the thick Ni film of electron beam deposition one deck 300-500nm at carbon film;
It is the Ar gas of 30-90sccm that the print that (11) will deposit the Ni film places flow velocity, is 900-1100 ℃ of lower annealing 15-30 minute in temperature, makes carbon film reconstitute patterned graphene in graph position;
(12) print with the patterned graphene that generates places HCl and CuSO
4To remove the Ni film, obtain the patterned graphene material in the mixing solutions.
The present invention compared with prior art has following advantage:
1. the present invention anneals at the Ni film owing to utilizing, thereby the carbon film that generates more easily reconstitutes preferably Graphene of continuity.
2. the present invention is because the patterned graphene of having grown optionally need not Graphene is carried out etching when this Graphene is made device, thereby the electronic mobility in the Graphene can not reduce, and guaranteed the device performance of making.
The present invention since growth during 3C-SiC first on the Si substrate growth one deck carburization zone as transition, then at the carburization zone 3C-SiC that grows, effectively reduced 3C-SiC lattice mismatch and dislocation, thereby the Graphene smooth surface of the generation of growth thereon, voidage is low, and thickness is easily controlled.
4. the present invention is owing to adopting 3C-SiC and Cl
2Reaction has not only improved speed of reaction, and can react under lower temperature and normal pressure.
But the present invention since the 3C-SiC heteroepitaxial growth on the Si disk, thereby low with this method growth patterned graphene cost.
Description of drawings
Fig. 1 is the device schematic 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 mainly is comprised of silica tube 1 and resistance furnace 2, and wherein silica tube 1 is provided with inlet mouth 3 and air outlet 4, and resistance furnace is 2 for the annular hollow structure, and silica tube 1 is inserted in the resistance furnace 2.
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 process, namely use first NH
4OH+H
2O
2Reagent soaked sample 10 minutes, took out post-drying, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out post-drying, 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
2Protection is lower, reaction chamber temperature is risen to 900 ℃ carbonization temperature, then passes into the C that flow is 30sccm to reaction chamber
3H
8, at Si Grown one deck carburization zone, growth time is 10min.
Step 4: at carburization zone growth 3C-SiC film.
Reaction chamber temperature is risen to rapidly 1200 ℃, pass into reactant gases SiH
4And C
3H
8, flow is respectively 20sccm and 40sccm, carries out the 3C-SiC thin film heterogeneity epitaxial growth, and growth time is 60min; Then at H
2The lower room temperature that progressively is cooled to of protection.
Step 5: at the good 3C-SiC film surface deposit one deck SiO of growth
2Mask layer.
(5.1) the good 3C-SiC film print of will growing is put into the PECVD system, and internal system pressure is adjusted to 3.0Pa, and radio frequency power is adjusted to 100W, and temperature is adjusted to 150 ℃;
(5.2) in the PECVD system, pass into SiH
4, N
2O and N
2, flow velocity is respectively 35sccm, 70sccm and 200sccm, continues 30min, makes SiH
4And N
2O reacts, thereby at the thick SiO of 3C-SiC film surface deposit one deck 0.4 μ m
2Mask layer.
Step 6: at SiO
2Carve figure on the layer.
(6.1) at SiO
2Spin coating one deck photoresist material on the layer;
(6.2) carve the window identical with the substrate shape of the device of required making at mask, expose 3C-SiC, form figure;
(6.3) corrode SiO with buffered hydrofluoric acid
2, expose 3C-SiC, form the figure on the reticle.
Step 7: with the patterned print silica tube of packing into, and the exhaust heating.
(7.1) patterned print is packed in the silica tube 1, silica tube is placed resistance furnace 2;
(7.2) passing into flow velocity from inlet mouth 3 to silica tube is the Ar gas of 80sccm, to silica tube carry out 10 minutes emptying, gas 4 is discharged from the air outlet;
(7.3) open the resistance furnace power switch, silica tube is heated to 700 ℃.
Step 8: generate carbon film.
Pass into Ar gas and Cl to silica tube
2Gas, flow velocity are respectively 98sccm and 2sccm, continue 5 minutes, make Cl
23C-SiC reaction with exposed generates carbon film.
Step 9: remove remaining SiO
2
The carbon film print that generates is taken out and places buffered hydrofluoric acid solution to remove SiO outside the figure from silica tube
2, this solution by hydrofluoric acid and water in proportion 1: 10 formulated.
Step 10: electron beam deposition layer of Ni film.
To remove SiO
2After the carbon film print put on the slide glass of electron beam evaporation deposition machine, adjusting slide glass is 50cm to the distance of target, and reaction chamber pressure is evacuated to 5 * 10
-4Pa, the setting line is 40mA, evaporation 10min is at the thick Ni film of carbon film deposition one deck 300nm.
Step 11: reconstitute patterned graphene.
The print that deposits the Ni film is placed Ar gas, and flow velocity is 90sccm, is 1100 ℃ of lower annealing 15 minutes in temperature, makes carbon film reconstitute patterned graphene in graph position.
Step 12: remove the Ni film.
The print of the patterned graphene that generates is placed HCl and CuSO
4To remove the Ni film, obtain the patterned graphene material in the mixing solutions.
Step 1: remove the sample surfaces pollutent.
8 inches Si substrate bases are carried out cleaning surfaces process, namely use first NH
4OH+H
2O
2Reagent soaked sample 10 minutes, took out post-drying, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out post-drying, to remove ionic contamination.
Step 2: identical with the step 2 of embodiment 1.
Step 3: growth carburization zone.
At H
2In the situation of protection, reaction chamber temperature is risen to 1050 ℃ of carbonization temperatures, then pass into C3H8 gas to reaction chamber, its flow is 30sccm, and at Si Grown one deck carburization zone, growth time is 7min.
Step 4: at carburization zone growth 3C-SiC film.
Reaction chamber temperature is risen to rapidly 1250 ℃, pass into respectively the SiH that flow is 25sccm
4With flow be the C of 50sccm
3H
8, reaction 45min, heteroepitaxial growth 3C-SiC film on carburization zone; Then at H
2The lower room temperature that progressively is cooled to of protection.
Step 5: at 3C-SiC film surface deposit one deck SiO
2
3C-SiC film print is put into the PECVD system, and the initialization system internal pressure is 3.0Pa, and radio frequency power is 100W, and temperature is 150 ℃; In system, pass into SiH
4, N
2O and N
2,SiH wherein
4Flow velocity is 35sccm, N
2The O flow velocity is 70sccm, N
2Flow velocity is 200sccm; Make SiH
4And N
2O reacts 75min, thereby at the thick SiO of 3C-SiC print surface deposition one deck 0.8 μ m
2Mask layer.
Step 6: at SiO
2Carve figure on the layer.
Identical with the step 6 of embodiment 1.
Step 7: with the patterned print silica tube of packing into, and the exhaust heating.
Patterned print is placed silica tube 1, silica tube is placed resistance furnace 2; Passing into flow velocity from inlet mouth 3 to silica tube is the Ar gas of 80sccm, to silica tube carry out 10 minutes emptying, gas 4 is discharged from the air outlet; Open again the resistance furnace power switch, silica tube is heated to 1100 ℃.
Step 8: generate carbon film.
Passing into respectively Ar gas that flow velocity is 97sccm and flow velocity to silica tube is 3sccm's and Cl
2Gas,, make Cl
2Reacted 4 minutes with exposed 3C-SiC, generate carbon film.
Step 9: remove remaining SiO
2
Identical with the step 9 of embodiment 1.
Step 10: electron beam deposition layer of Ni film.
To remove SiO
2After the carbon film print put on the slide glass of electron beam evaporation deposition machine, adjusting slide glass is 50cm to the distance of target, and reaction chamber pressure is evacuated to 5 * 10
-4Pa, the adjusting line is 40mA, evaporation 15min, at carbon film deposition layer of Ni film, thickness is 400nm.
Step 11: reconstitute patterned graphene.
It is under 1000 ℃ that the print that deposits the Ni film is placed at temperature, and flow velocity is in the Ar gas of 55sccm, anneals 20 minutes, makes carbon film reconstitute patterned graphene in graph position.
Step 12: remove the Ni film.
The print of the patterned graphene that generates is placed HCl and CuSO
4To remove the Ni film, obtain the patterned graphene material in the mixing solutions.
Steps A: 12 inches Si substrate bases are carried out cleaning surfaces process, namely use first NH
4OH+H
2O
2Reagent soaked sample 10 minutes, took out post-drying, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out post-drying, to remove ionic contamination.
Step B: identical with the step 2 of embodiment 1.
Step C: at H
2In the situation of protection reaction chamber temperature is risen to 1200 ℃ of carbonization temperatures, then pass into the C that flow is 30sccm to reaction chamber
3H
8, continue 5min, with at Si Grown one deck carburization zone.
Step D: reaction chamber temperature is risen to rapidly 1300 ℃, pass into the SiH that flow is respectively 30sccm and 60sccm
4And C
3H
8, carry out 3C-SiC thin film heterogeneity epitaxial growth 30min, then at H
2The lower room temperature that progressively is cooled to of protection.
Step e: the good 3C-SiC print of will growing is put into the PECVD system, and internal system pressure is adjusted to 3.0Pa, and radio frequency power is adjusted to 100W, and temperature is adjusted to 150 ℃; In system, pass into the SiH that flow velocity is respectively 35sccm, 70sccm and 200sccm
4, N
2O and N
2, continue 100min, make SiH
4And N
2O reacts, at the thick SiO of 3C-SiC print surface deposition one deck 1.2 μ m
2Mask layer.
Step F: identical with the step 6 of embodiment 1.
Step G: the print after will windowing places silica tube 1, and silica tube is placed resistance furnace 2; Passing into flow velocity from inlet mouth 3 to silica tube is the Ar gas of 80sccm, to silica tube carry out 10 minutes emptying, gas 4 is discharged from the air outlet; Open again the resistance furnace power switch, silica tube is heated to 1000 ℃.
Step H: in silica tube, pass into Ar gas and the Cl that flow velocity is respectively 95sccm and 5sccm
2Gas, the time length is 3 minutes, makes Cl
23C-SiC reaction with exposed generates carbon film.
Step I: identical with the step 9 of embodiment 1.
Step J: electron beam deposition layer of Ni film.
To remove SiO
2After the carbon film print put on the slide glass of electron beam evaporation deposition machine, adjusting slide glass is 50cm to the distance of target, and reaction chamber pressure is evacuated to 5 * 10
-4Pa, the adjusting line is 40mA, evaporation 20min is at the thick Ni film of carbon film deposition one deck 500nm.
Step K: reconstitute patterned graphene.
It is the Ar gas of 30sccm that the print that deposits the Ni film is placed flow velocity, is 900 ℃ of lower annealing 30 minutes in temperature, makes carbon film reconstitute patterned graphene in graph position.
Step L: remove the Ni film.
The print of the patterned graphene that generates is placed HCl and CuSO
4To remove the Ni film, obtain the patterned graphene material in the mixing solutions.
Claims (6)
1. one kind based on the Ni film of 3C-SiC and chlorine reaction annealing patterned graphene preparation method, may further comprise the steps:
(1) the Si substrate base of 4-12 inch carried 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
2Protection is lower, makes reaction chamber progressively be warming up to 900 ℃-1200 ℃ of carbonization temperatures, passes into the C that flow is 30sccm
3H
8, substrate is carried out carbonization 5-10min, growth one deck carburization zone;
(4) reaction chamber is warming up to 1200 ℃-1300 ℃, passes into C
3H
8And SiH
4, carrying out the 3C-SiC thin film heterogeneity epitaxial growth, growth time is 30-60min, then at H
2Protection is lower progressively to be cooled to room temperature, finishes the growth of 3C-SiC film;
(5) utilize plasma enhanced chemical vapor deposition PECVD method, the thick SiO of deposit one deck 0.4-1.2 μ m at the good 3C-SiC film surface of growth
2Mask layer;
(6) at SiO
2Mask surface is coated with one deck photoresist material, carves the window identical with the substrate shape of the device of required making at mask again, exposes 3C-SiC, forms the figure identical with window shape;
(7) patterned print is placed silica tube, be heated to 700-1100 ℃;
(8) in silica tube, pass into Ar gas and Cl
2The mixed gas of gas continues 3-5min, makes Cl
2React with exposed 3C-SiC, generate the individual layer carbon film;
(9) the carbon film print that generates is placed buffered hydrofluoric acid solution to remove the SiO outside the figure
2
(10) utilize the thick Ni film of electron beam deposition one deck 300-500nm at carbon film;
It is the Ar gas of 30-90sccm that the print that (11) will deposit the Ni film places flow velocity, is 900-1100 ℃ of lower annealing 15-30 minute in temperature, makes carbon film reconstitute patterned graphene in graph position;
(12) print with the patterned graphene that generates places HCl and CuSO
4To remove the Ni film, obtain grapheme material in the mixing solutions.
2. the Ni film annealing patterned graphene preparation method based on 3C-SiC and chlorine reaction according to claim 1 is characterized in that the SiH that described step (4) passes into
4And C
3H
8, its flow is respectively 20-30sccm and 40-60sccm.
3. the Ni film annealing patterned graphene preparation method based on 3C-SiC and chlorine reaction according to claim 1, what it is characterized in that described step (5) utilizes PECVD deposit SiO
2, its processing condition are: SiH
4, N
2O and N
2Flow velocity be respectively 35sccm, 70sccm and 200sccm, the reaction chamber internal pressure is 3.0Pa, radio frequency power is 100W,
Deposition temperature is 150 ℃, and deposition time is 30-100min.
4. the Ni film annealing patterned graphene preparation method based on 3C-SiC and chlorine reaction according to claim 1 is characterized in that Ar gas and Cl that described step (8) passes into
2Gas, its flow velocity is respectively 95-98sccm and 5-2sccm.
5. the Ni film annealing patterned graphene preparation method based on 3C-SiC and chlorine reaction according to claim 1 is characterized in that buffered hydrofluoric acid solution in the described step (9), is to be that 1: 10 hydrofluoric acid and water is formulated with ratio.
6. the Ni film annealing patterned graphene preparation method based on 3C-SiC and chlorine reaction according to claim 1, the condition that it is characterized in that electron beam deposition in the described step (10) is: substrate is 50cm to the distance of target, and reaction chamber pressure is 5 * 10
-4Pa, line are 40mA, and evaporation time is 10-20min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183338A (en) * | 2013-03-12 | 2013-07-03 | 西安电子科技大学 | Preparation method of large-area graphene based on Ni film annealing and chlorine reaction |
| CN112542464A (en) * | 2020-12-09 | 2021-03-23 | 长江存储科技有限责任公司 | Manufacturing method of three-dimensional memory |
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| CN102674328A (en) * | 2012-05-22 | 2012-09-19 | 西安电子科技大学 | Preparation method of structured graphene based on Cu film annealing |
| CN102674329A (en) * | 2012-05-22 | 2012-09-19 | 西安电子科技大学 | Preparation method of structured graphene based on Cl2 reaction |
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| CN102674328A (en) * | 2012-05-22 | 2012-09-19 | 西安电子科技大学 | Preparation method of structured graphene based on Cu film annealing |
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| CN103183338A (en) * | 2013-03-12 | 2013-07-03 | 西安电子科技大学 | Preparation method of large-area graphene based on Ni film annealing and chlorine reaction |
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