CN102936011B - 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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- CN102936011B CN102936011B CN201210484532.8A CN201210484532A CN102936011B CN 102936011 B CN102936011 B CN 102936011B CN 201210484532 A CN201210484532 A CN 201210484532A CN 102936011 B CN102936011 B CN 102936011B
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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, the specifically annealing of the Ni film based on 3C-SiC and chlorine reaction patterned graphene preparation method.
Technical background
It is in 2004 that Graphene appears in 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 by a kind of very simple method.They separate graphite flake from graphite, then the two sides of thin slice are bonded on a kind of special adhesive tape, tear adhesive tape, just graphite flake can be divided into two.Constantly operation like this, so thin slice is more and more thinner, last, they have obtained the thin slice being only made up of one deck carbon atom, Here it is Graphene.After this, the novel method of preparing Graphene emerges in an endless stream.Current preparation method mainly contains two kinds:
The first thermolysis SiC method, this method is by monocrystal SiC heating to remove Si by lip-deep SiC is decomposed, and residual carbon forms Graphene subsequently.But the monocrystal SiC using in SiC thermolysis is very expensive, and the Graphene growing out is island and distributes, and the number of plies is inhomogeneous, and reduces because photoetching process can make the electronic mobility of Graphene while making device, thereby has affected device performance.
The second chemical Vapor deposition process, this method provides a kind of controlled effective ways of preparing Graphene, it is by planar substrates, as metallic film, metal single crystal etc. are placed in the decomposable presoma of high temperature, in the atmosphere such as methane, ethene, make carbon atom be deposited on substrate surface by high temperature annealing and form Graphene, finally with obtaining independently graphene film after chemical corrosion method removal metal base.By selecting the type of substrate, the parameter such as temperature, the flow of presoma of growth can regulate and control the growth of Graphene, 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, as molecule sensor, field-effect transistor, solar cell etc.Based on the preparation of micro-nano device, conventionally need to carry out graphically Graphene, conventional Graphene graphic method has at present:
1) photolithography.Big area Graphene is carried out to photoetching, ion etching technique, obtain patterned Graphene, the graphical precision of this method is high, but technology difficulty is large, in technological process, easily Graphene is polluted and is damaged;
2) direct growth method.The patterned Graphene of growing in metallic film base is transferred to components and parts substrate again, and this method, without using follow-up photoengraving technique, still cannot accurately navigate to Graphene on substrate;
3) nano impression method.Impress out Graphene in the place that need to have figure, this method is convenient and simple, but cannot obtain comparatively complicated figure, and 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 Fast Growth patterned graphene optionally on the 3C-SiC of Si substrate epitaxial film, make not need to carry out in follow-up manufacture device process the technological process of etching, avoid Graphene to pollute and damage, thereby the electronic mobility that guarantees Graphene is stable, improves device performance.
For achieving the above object, preparation method of the present invention comprises the following steps:
(1) the Si substrate base of 4-12 inch is carried out to standard cleaning;
(2) the Si substrate base after cleaning is put into CVD system response chamber, reaction chamber is vacuumized and reaches 10
-7mbar rank;
(3) at H
2under protection, make reaction chamber progressively be warming up to 900 ℃-1200 ℃ of carbonization temperatures, pass into the C that flow is 30sccm
3h
8, substrate is carried out to 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 3C-SiC thin film heterogeneity epitaxial growth, growth time is 30-60min, then at H
2under protection, be progressively cooled to room temperature, complete the growth of 3C-SiC film;
(5) utilize plasma enhanced chemical vapor deposition PECVD method at the 3C-SiC film surface of having grown, the thick SiO of deposit one deck 0.5-1.2 μ m
2mask layer;
(6) at SiO
2mask surface is coated with one deck photoresist material, then on mask, carves the window identical with the substrate shape of the device of required making, exposes 3C-SiC, forms the figure identical with window shape;
(7) patterned print is placed in to silica tube, is 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 of generation is placed in to buffered hydrofluoric acid solution to remove the SiO outside figure
2;
(10) on carbon film, utilize the Ni film that electron beam deposition one deck 300-500nm is thick;
(11) print that deposits Ni film being placed in to the Ar gas that flow velocity is 30-90sccm, is the 15-30 minute that anneals at 900-1100 ℃ in temperature, makes carbon film reconstitute patterned graphene in graph position;
(12) print of the patterned graphene of generation is placed in to HCl and CuSO
4in mixing solutions, to remove Ni film, obtain patterned graphene material.
The present invention compared with prior art tool has the following advantages:
1. the present invention anneals on Ni film owing to utilizing, thereby the carbon film generating more easily reconstitutes the good Graphene of continuity.
2. the present invention is due to the patterned graphene of optionally having grown, and make device on this Graphene time, without Graphene is carried out to etching, thereby electronic mobility in Graphene can not reduce, and guaranteed the device performance of making.
3. the present invention is owing to first growing up one deck carburization zone as transition on Si substrate in the time growing 3C-SiC, then the 3C-SiC that grows on carburization zone, has 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 under lower temperature and normal pressure, react.
The present invention due to 3C-SiC can heteroepitaxial growth on Si disk, thereby low with this method growth patterned graphene cost.
Accompanying drawing explanation
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 is mainly made up 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 annular hollow structure, and silica tube 1 is inserted in 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 sample surfaces pollutent.
Si substrate base to 4 inches carries out surface cleaning processing, first uses NH
4oH+H
2o
2reagent soaks sample 10 minutes, takes out post-drying, to remove sample surfaces organic residue; Re-use HCl+H
2o
2reagent soaks sample 10 minutes, takes out post-drying, to remove ionic contamination.
Step 2: Si substrate base is put into CVD system response chamber, reaction chamber is vacuumized and reaches 10
-7mbar rank.
Step 3: growth carburization zone.
At H
2under protection, reaction chamber temperature is risen to the carbonization temperature of 900 ℃, then pass into reaction chamber the C that flow is 30sccm
3h
8, at Si Grown one deck carburization zone, growth time is 10min.
Step 4: the 3C-SiC film of growing on carburization zone.
Reaction chamber temperature is risen to rapidly to 1200 ℃, pass into reactant gases SiH
4and C
3h
8, flow is respectively 20sccm and 40sccm, carries out 3C-SiC thin film heterogeneity epitaxial growth, and growth time is 60min; Then at H
2under protection, be progressively cooled to room temperature.
Step 5: the 3C-SiC film surface deposit one deck SiO growing
2mask layer.
(5.1) the 3C-SiC film print of having grown is put into PECVD system, internal system pressure is adjusted to 3.0Pa, radio frequency power is adjusted to 100W, and temperature is adjusted to 150 ℃;
(5.2) in 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
2on layer, carve figure.
(6.1) at SiO
2spin coating one deck photoresist material on layer;
(6.2) on mask, carve the window identical with the substrate shape of the device of required making, expose 3C-SiC, form figure;
(6.3) corrode SiO with buffered hydrofluoric acid
2, expose 3C-SiC, form the figure in reticle.
Step 7: pack patterned print into silica tube, and exhaust heating.
(7.1) patterned print is packed in silica tube 1, silica tube is placed in to resistance furnace 2;
(7.2) from inlet mouth 3 to silica tube, passing into flow velocity is the Ar gas of 80sccm, to silica tube carry out 10 minutes emptying, gas is discharged from air outlet 4;
(7.3) open 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 is respectively 98sccm and 2sccm, continues 5 minutes, makes Cl
2react with exposed 3C-SiC, generate carbon film.
Step 9: remove remaining SiO
2.
The carbon film print of generation is taken out and be placed in buffered hydrofluoric acid solution from silica tube and remove the SiO outside figure
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 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, setting line is 40mA, evaporation 10min deposits the Ni film that one deck 300nm is thick on carbon film.
Step 11: reconstitute patterned graphene.
The print that deposits Ni film is placed in to Ar gas, and flow velocity is 90sccm, is at 1100 ℃, to anneal 15 minutes in temperature, makes carbon film reconstitute patterned graphene in graph position.
Step 12: remove Ni film.
The print of the patterned graphene of generation is placed in to HCl and CuSO
4in mixing solutions, to remove Ni film, obtain patterned graphene material.
Step 1: remove sample surfaces pollutent.
Si substrate base to 8 inches carries out surface cleaning processing, first uses NH
4oH+H
2o
2reagent soaks sample 10 minutes, takes out post-drying, to remove sample surfaces organic residue; Re-use HCl+H
2o
2reagent soaks sample 10 minutes, takes 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: the 3C-SiC film of growing on carburization zone.
Reaction chamber temperature is risen to rapidly to 1250 ℃, pass into respectively the SiH that flow is 25sccm
4with the flow C that is 50sccm
3h
8, reaction 45min, heteroepitaxial growth 3C-SiC film on carburization zone; Then at H
2under protection, be progressively cooled to room temperature.
Step 5: at 3C-SiC film surface deposit one deck SiO
2.
3C-SiC film print is put into PECVD system, and 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,wherein SiH
4flow velocity is 35sccm, N
2o 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
2on layer, carve figure.
Identical with the step 6 of embodiment 1.
Step 7: pack patterned print into silica tube, and exhaust heating.
Patterned print is placed in to silica tube 1, silica tube is placed in to resistance furnace 2; From inlet mouth 3 to silica tube, passing into flow velocity is the Ar gas of 80sccm, to silica tube carry out 10 minutes emptying, gas is discharged from air outlet 4; Open again 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
2react 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 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, adjusting line is 40mA, and evaporation 15min deposits layer of Ni film on carbon film, and thickness is 400nm.
Step 11: reconstitute patterned graphene.
It is at 1000 ℃ that the print that deposits Ni film is placed to temperature, in the Ar gas that flow velocity is 55sccm, anneals 20 minutes, makes carbon film reconstitute patterned graphene in graph position.
Step 12: remove Ni film.
The print of the patterned graphene of generation is placed in to HCl and CuSO
4in mixing solutions, to remove Ni film, obtain patterned graphene material.
Steps A: the Si substrate base to 12 inches carries out surface cleaning processing, is first used NH
4oH+H
2o
2reagent soaks sample 10 minutes, takes out post-drying, to remove sample surfaces organic residue; Re-use HCl+H
2o
2reagent soaks sample 10 minutes, takes 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 reaction chamber the C that flow is 30sccm
3h
8, continue 5min, with at Si Grown one deck carburization zone.
Step D: reaction chamber temperature is risen to rapidly to 1300 ℃, pass into flow and be respectively the SiH of 30sccm and 60sccm
4and C
3h
8, carry out 3C-SiC thin film heterogeneity epitaxial growth 30min, then at H
2under protection, be progressively cooled to room temperature.
Step e: the 3C-SiC print of having grown is put into PECVD system, internal system pressure is adjusted to 3.0Pa, radio frequency power is adjusted to 100W, temperature is adjusted to 150 ℃; To the SiH that passes into flow velocity in system and be 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 windowing is placed in to silica tube 1, silica tube is placed in to resistance furnace 2; From inlet mouth 3 to silica tube, passing into flow velocity is the Ar gas of 80sccm, to silica tube carry out 10 minutes emptying, gas is discharged from air outlet 4; Open again resistance furnace power switch, silica tube is heated to 1000 ℃.
Step H: to the Ar gas and the Cl that pass into flow velocity in silica tube and be respectively 95sccm and 5sccm
2gas, the time length is 3 minutes, makes Cl
2react with exposed 3C-SiC, generate 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 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, adjusting line is 40mA, evaporation 20min deposits the Ni film that one deck 500nm is thick on carbon film.
Step K: reconstitute patterned graphene.
The print that deposits Ni film is placed in to the Ar gas that flow velocity is 30sccm, is at 900 ℃, to anneal 30 minutes in temperature, makes carbon film reconstitute patterned graphene in graph position.
Step L: remove Ni film.
The print of the patterned graphene of generation is placed in to HCl and CuSO
4in mixing solutions, to remove Ni film, obtain patterned graphene material.
Claims (6)
1. the annealing of the Ni film based on a 3C-SiC and chlorine reaction patterned graphene preparation method, comprises the following steps:
(1) the Si substrate base of 4-12 inch is carried out to standard cleaning;
(2) the Si substrate base after cleaning is put into CVD system response chamber, reaction chamber is vacuumized and reaches 10
-7mbar rank;
(3) at H
2under protection, make reaction chamber progressively be warming up to 900 ℃-1200 ℃ of carbonization temperatures, pass into the C that flow is 30sccm
3h
8, substrate is carried out to 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 3C-SiC thin film heterogeneity epitaxial growth, growth time is 30-60min, then at H
2under protection, be progressively cooled to room temperature, complete the growth of 3C-SiC film;
(5) utilize plasma enhanced chemical vapor deposition PECVD method at the 3C-SiC film surface of having grown, the thick SiO of deposit one deck 0.4-1.2 μ m
2mask layer;
(6) at SiO
2mask surface is coated with one deck photoresist material, then on mask, carves the window identical with the substrate shape of the device of required making, exposes 3C-SiC, forms the figure identical with window shape;
(7) patterned print is placed in to silica tube, is heated to 700-1100 ℃;
(8) in silica tube, pass into Ar and Cl
2mixed gas, continue 3-5min, make Cl
2react with exposed 3C-SiC, generate individual layer carbon film;
(9) the carbon film print of generation is placed in to buffered hydrofluoric acid solution to remove the SiO outside figure
2;
(10) on carbon film, utilize the Ni film that electron beam deposition one deck 300-500nm is thick;
(11) print that deposits Ni film being placed in to the Ar that flow velocity is 30-90sccm, is the 15-30 minute that anneals at 900-1100 ℃ in temperature, makes carbon film reconstitute patterned graphene in graph position;
(12) print of the patterned graphene of generation is placed in to HCl and CuSO
4in mixing solutions, to remove Ni film, obtain grapheme material.
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. Ni film based on 3C-SiC and chlorine reaction annealing patterned graphene preparation method according to claim 1, is characterized in that utilizing in described step (5) plasma enhanced chemical vapor deposition PECVD method deposit SiO
2, its processing condition are: SiH
4, N
2o and N
2flow velocity be respectively 35sccm, 70sccm and 200sccm, reaction chamber internal pressure is 3.0Pa, radio frequency power is 100W, deposition temperature is 150 ℃, 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 and Cl that described step (8) passes into
2, its flow velocity is respectively 95-98sccm and 5-2sccm.
5. Ni film based on 3C-SiC and chlorine reaction annealing patterned graphene preparation method according to claim 1, is characterized in that buffered hydrofluoric acid solution in described step (9), is to be 1:10 by ratio hydrofluoric acid and water are formulated.
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 described step (10) is: substrate is 50cm to the distance of target, and reaction chamber pressure is 5 × 10
-4pa, line is 40mA, evaporation time is 10-20min.
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US6896706B2 (en) * | 2002-01-17 | 2005-05-24 | Korea Institute Of Science And Technology | Carbonaceous materials coated with a metal or metal oxide, a preparation method thereof, and a composite electrode and lithium secondary battery comprising the same |
CN102653401A (en) * | 2012-05-22 | 2012-09-05 | 西安电子科技大学 | Structural graphene preparation method based on Ni 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 |
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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US6896706B2 (en) * | 2002-01-17 | 2005-05-24 | Korea Institute Of Science And Technology | Carbonaceous materials coated with a metal or metal oxide, a preparation method thereof, and a composite electrode and lithium secondary battery comprising the same |
CN102653401A (en) * | 2012-05-22 | 2012-09-05 | 西安电子科技大学 | Structural graphene preparation method based on Ni 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 |
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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