CN102931060A - Ni film annealing graphical graphene preparation method on basis of reaction of SiC and chlorine - Google Patents

Ni film annealing graphical graphene preparation method on basis of reaction of SiC and chlorine Download PDF

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Publication number
CN102931060A
CN102931060A CN2012104845351A CN201210484535A CN102931060A CN 102931060 A CN102931060 A CN 102931060A CN 2012104845351 A CN2012104845351 A CN 2012104845351A CN 201210484535 A CN201210484535 A CN 201210484535A CN 102931060 A CN102931060 A CN 102931060A
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sic
film
print
annealing
patterned graphene
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郭辉
胡彦飞
张玉明
赵艳黎
雷天民
张克基
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Xidian University
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Xidian University
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Abstract

The invention discloses a Ni film annealing graphical preparation method on the basis of the reaction of SiC and chlorine, which mainly solves the problem that graphene prepared by the prior art needs to complete the shape clipping via electron beam etching before manufactured to elements. The implement process of the method comprises the following steps: standard cleaning of a SiC sample sheet is executed; a layer of SiO2 is deposited on the surface of the SiC sample sheet and a graph is chiseled; the graphic sample sheet is placed in a quartz tube to generate a carbon film under the temperature of 700-1,100 DEG C; the generated carbon sample sheet is placed in a buffer hydrofluoric acid solution to remove SiO2 outside the graph; and lastly, a layer of Ni film with a thickness of 350-600 nm is deposited on the carbon film by utilizing electron beam, the sample sheet deposited with the Ni film is placed in Ar, and a graphic graphene material is generated via 10-30 min annealing under the temperature of 900-1,100 DEG C. The electron mobility of the graphic graphene prepared by the method is stable, the continuity is good, etching is not required, and the graphene can be directly used for manufacturing basic elements.

Description

Ni film annealing patterned graphene preparation method based on SiC and chlorine reaction
Technical field
The invention belongs to microelectronics technology, relate to semiconductor film material and preparation method thereof, specifically be based on the Ni film annealing patterned graphene preparation method of SiC and chlorine reaction.
Technical background
In basis and applied science field, the research of carbon group material is the infusive thing of part always.Although carbon group material is used in industry very early such as graphite, until the electronic structure of graphite is just furtherd investigate about nineteen fifty.Along with the rise of nanosecond science and technology, other allotropes of carbon are constantly studied.The people such as Harold in 1985 have found the zero-dimension structural fullerene C of carbon 60, this discovery be nanosecond science and technology field development essential step so far people also exploring its character and electronic application.1991, the carbon nano-tube of one dimension was found by Ijima, because the physical property of its uniqueness becomes rapidly study hotspot.With sp 2The Two-dimensional Carbon film that hydridization forms is named as Graphene.Graphene only has an atomic layers thick, is to consist of above-mentioned other allotropic elementary cell.But once once thought most of physicists, all can not exist under finite temperature at any two dimensional crystal material under the thermodynamics fluctuation.Scientists makes great efforts to obtain the Graphene of two dimension always, but until 2004, Geim and Novoselov utilize the method for micromechanics glass highly oriented pyrolytic graphite just to obtain the two-dimensional material of a this atomic thickness.
From now on, the new method of preparation Graphene emerges in an endless stream, and mainly is chemical vapour deposition technique but use maximum.The 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 annealing and form Graphene, at last with obtaining independently graphene film after the chemical corrosion method removal metallic substrates.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 rate, thickness, area etc., the shortcoming of the method maximum is that the graphene sheet layer and the substrate that obtain interact strong, lost the character of many patterned graphenes, and the continuity of Graphene not fine.It is " method of process for preparing graphenes by chemical vapour deposition " patent application of 200810113596.0 such as application number, it is exactly a kind of method with process for preparing graphenes by chemical vapour deposition, its implementation procedure is: Kaolinite Preparation of Catalyst at first, then carry out high temperature chemical vapor deposition, to put into anoxic reactor with the substrate of catalyst, make substrate reach 500-1200 ℃, passing into the carbon containing source of the gas carries out chemical deposition and obtains Graphene again, then Graphene is purified, namely use acid treatment or in low pressure, evaporate Graphene under the high temperature, to remove the catalyst in the Graphene.The major defect of the method is: complex process, need the special catalyst of removing, and energy resource consumption is large, and production cost is high.
Graphene has been proved to be the preparation that can be applied to multiple electronic 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) 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;
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) photoetching process.The large tracts of land 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 technical process.
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 SiC and chlorine reaction is proposed, to improve Graphene surface flatness and continuity, reduction porosity, and release will be carried out to Graphene the technical process of etching in follow-up manufacturing device process, the electron 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 SiC print is cleaned, to remove surface contaminant;
(2) the SiC print surface after cleaning utilizes plasma enhanced chemical vapor deposition PECVD method, the thick SiO of deposit one deck 0.5-1.0 μ m 2, as mask;
(3) at SiO 2Mask surface is coated with one deck photoresist, carves the window identical with the substrate shape of the device of required making at mask again, exposes SiC, forms the figure identical with window shape;
(4) patterned print is placed quartz ampoule, be heated to 700-1100 ℃;
(5) in quartz ampoule, pass into Ar gas and Cl 2The mist of gas continues 3-8min, makes Cl 2Produce reaction with exposed SiC, generate carbon film;
(6) the carbon film print that generates is placed buffered hydrofluoric acid solution to remove the SiO outside the figure 2
(7) utilize the thick Ni film of electron beam deposition one deck 400-600nm at carbon film;
It is the Ar gas of 30-90sccm that the print that (8) will deposit the Ni film places flow velocity, is 1000-1200 ℃ of lower annealing 10-30 minute in temperature, makes carbon film reconstitute patterned graphene in graph position;
(9) print with the patterned graphene that generates places HCl and CuSO 4To remove the Ni film, obtain the patterned graphene material in the mixed solution.
The present invention compared with prior art has following advantage:
1. 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 electron mobility in the Graphene can not reduce, and guaranteed the device performance of making.
2. the present invention anneals at the Ni film owing to utilizing, thereby the easier reconstruct of the carbon film that generates forms preferably Graphene of continuity.
3. the present invention is owing to utilizing SiC and Cl 2Solid/liquid/gas reactions, thereby the patterned graphene smooth surface that generates, voidage is low, and thickness easily controls, and can be used for the sealing to gas and liquid.
4. SiC and Cl among the present invention 2Can under lower temperature and normal pressure, react, and reaction rate is fast.
5. the method technique of the present invention's use is simple, and energy savings is safe.
Description of drawings
Fig. 1 is the device schematic diagram that the present invention prepares Graphene;
Fig. 2 is the flow chart that the present invention prepares Graphene.
Embodiment
With reference to Fig. 1, Preparation equipment of the present invention mainly is comprised of quartz ampoule 1 and resistance furnace 2, and wherein quartz ampoule 1 is provided with air inlet 3 and gas outlet 4, and resistance furnace is 2 for the annular hollow structure, and quartz ampoule 1 is inserted in the resistance furnace 2.
With reference to Fig. 2, manufacture method of the present invention provides following three kinds of embodiment.
Embodiment 1
Step 1: clean the 6H-SiC print, to remove surface contaminant.
(1.1) the 6H-SiC substrate base is used NH 4OH+H 2O 2Reagent soaked 10 minutes, took out post-drying, to remove the sample surfaces organic remains;
(1.2) the 6H-SiC print that will remove behind the surperficial organic remains re-uses HCl+H 2O 2Reagent soaked 10 minutes, took out post-drying, to remove ionic contamination.
Step 2: at 6H-SiC print surface deposition one deck SiO 2
(2.1) the 6H-SiC print after will cleaning 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 ℃;
(2.2) in system, pass into the SiH that flow velocity is respectively 30sccm, 60sccm and 200sccm 4, N 2O and N 2, the duration is 30min, makes SiH 4And N 2The O reaction is at the thick SiO of 6H-SiC print surface deposition one deck 0.5 μ m 2Mask layer.
Step 3: at SiO 2Carve figure on the layer.
(3.1) at SiO 2Spin coating one deck photoresist on the layer;
(3.2) make reticle according to making device tpo substrate shape, and then carry out photoetching, figure on the reticle is transferred to SiO 2On the layer;
(3.3) corrode SiO with buffered hydrofluoric acid 2, expose 6H-SiC, form the figure on the reticle.
Step 4: with the patterned print quartz ampoule of packing into, and the exhaust heating.
(4.1) patterned print is put into quartz ampoule 1, quartz ampoule is placed resistance furnace 2;
(4.2) passing into flow velocity from air inlet 3 to quartz ampoule is the Ar gas of 80sccm, to quartz ampoule carry out 10 minutes emptying, air 4 is discharged from the gas outlet;
(4.3) open the resistance furnace mains switch, quartz ampoule is heated to 700 ℃.
Step 5: generate carbon film.
Pass into Ar gas and the Cl that flow velocity is respectively 98sccm and 2sccm to quartz ampoule 2Gas, the time is 8 minutes, makes Cl 26H-SiC reaction with exposed generates carbon film.
Step 6: 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 quartz ampoule 2
Step 7: electron beam deposition layer of Ni film.
To remove SiO 2After the carbon film print put on the slide of electron beam evaporation deposition machine, adjusting slide is 50cm to the distance of target, and reative cell pressure is evacuated to 5 * 10 -4Pa, the adjusting line is 40mA, evaporation 10min is at the thick Ni film of carbon film deposition one deck 400nm.
Step 8: reconstitute patterned graphene.
It is the Ar gas of 90sccm that the print that deposits the Ni film is placed flow velocity, is 1000 ℃ of lower annealing 30 minutes in temperature, makes carbon film reconstitute patterned graphene in graph position.
Step 9: 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 mixed solution.
Embodiment 2
Step 1: clean the 4H-SiC print, to remove surface contaminant.
The 4H-SiC substrate base is used first NH 4OH+H 2O 2Reagent soaked sample 10 minutes, took out post-drying, to remove the sample surfaces organic remains; Re-use HCl+H 2O 2Reagent soaked sample 10 minutes, took out post-drying, to remove ionic contamination.
Step 2: at 4H-SiC print surface deposition one deck SiO 2
4H-SiC print after cleaning is put into the PECVD system, internal system pressure is adjusted to 3.0Pa, radio-frequency power is adjusted to 100W, and temperature is adjusted to 150 ℃; In system, pass into SiH 4, N 2O and N 2, SiH 4Flow velocity is 30sccm, N 2The O flow velocity is 60sccm, N 2Flow velocity is 200sccm, makes SiH 4And N 2O reacts 70min, at the thick SiO of 4H-SiC print surface deposition one deck 0.8 μ m 2
Step 3: at SiO 2Carve figure on the layer.
At SiO 2Spin coating one deck photoresist on the layer; Make reticle according to making device tpo substrate shape, and then carry out photoetching, figure on the reticle is transferred to SiO 2On the layer; Corrode SiO with buffered hydrofluoric acid 2, expose 4H-SiC, form figure.
Step 4: with the patterned print quartz ampoule of packing into, and the exhaust heating.
Patterned print is placed quartz ampoule 1, quartz ampoule is placed resistance furnace 2; Passing into flow velocity from air inlet 3 to quartz ampoule is the Ar gas of 80sccm, to quartz ampoule carry out 10 minutes emptying, air 4 is discharged from the gas outlet; Open again the resistance furnace mains switch, quartz ampoule is heated to 1000 ℃.
Step 5: generate carbon film.
Pass into Ar gas and Cl to quartz ampoule 2In the gas, wherein the Ar flow velocity is 97sccm, Cl 2Flow velocity is 3sccm, makes Cl 2Reacted 5 minutes with exposed 4H-SiC, generate carbon film.
Step 6: identical with the step 6 of embodiment 1.
Step 7: electron beam deposition layer of Ni film.
To remove SiO 2After the carbon film print put on the slide of electron beam evaporation deposition machine, adjusting slide is 50cm to the distance of target, and reative cell 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 8: reconstitute patterned graphene.
It is the Ar gas of 75sccm that the print that deposits the Ni film is placed flow velocity, is 1200 ℃ of lower annealing 10 minutes in temperature, makes carbon film reconstitute patterned graphene in graph position.
Step 9: 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 mixed solution.
Embodiment 3
Steps A: the 6H-SiC substrate base is 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 remains; Re-use HCl+H 2O 2Reagent soaked sample 10 minutes, took out post-drying, to remove ionic contamination.
Step B: the 6H-SiC print after will cleaning 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 30sccm 4, flow velocity is the N of 60sccm 2O and flow velocity are the N of 200sccm 2, the duration is 90min, makes SiH 4And N 2The O reaction is at the thick SiO of 6H-SiC print surface deposition one deck 1.0 μ m 2
Step C: identical with the step 3 of embodiment 1.
Step D: the patterned print of shape is placed quartz ampoule 1, and quartz ampoule is placed resistance furnace 2; Passing into flow velocity from air inlet 3 to quartz ampoule is the Ar gas of 80sccm, to quartz ampoule carry out 10 minutes emptying, air 4 is discharged from the gas outlet; Open again the resistance furnace mains switch, quartz ampoule is heated to 1100 ℃.
Step e: passing into Ar gas and the flow velocity that flow velocity is 95sccm in the quartz ampoule is the Cl of 5sccm 2Gas, the time is 3 minutes, makes Cl 26H-SiC reaction with exposed generates carbon film.
Step F: identical with the step 6 of embodiment 1.
Step G: electron beam deposition layer of Ni film.
To remove SiO 2After the carbon film print put on the slide of electron beam evaporation deposition machine, adjusting slide is 50cm to the distance of target, and reative cell pressure is evacuated to 5 * 10 -4Pa, the adjusting line is 40mA, evaporation 30min is at the thick Ni film of carbon film deposition one deck 600nm.
Step H: reconstitute patterned graphene.
It is 1100 ℃ Ar gas that the print that deposits the Ni film is placed temperature, and the Ar gas velocity is 30sccm, anneals 20 minutes, makes carbon film reconstitute patterned graphene in graph position.
Step I: 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 mixed solution.

Claims (8)

1. one kind based on the Ni film of SiC and chlorine reaction annealing patterned graphene preparation method, may further comprise the steps:
(1) the SiC print is cleaned, to remove surface contaminant;
(2) the SiC print surface after cleaning utilizes plasma enhanced chemical vapor deposition PECVD method, the thick SiO of deposit one deck 0.5-1.0 μ m 2, as mask;
(3) at SiO 2Mask surface is coated with one deck photoresist, 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;
(4) patterned print is placed quartz ampoule, be heated to 700-1100 ℃;
(5) in quartz ampoule, pass into Ar gas and Cl 2The mist of gas continues 3-8min, makes Cl 2Produce reaction with exposed SiC, generate carbon film;
(6) the carbon film print that generates is placed buffered hydrofluoric acid solution to remove the SiO outside the figure 2
(7) utilize the thick Ni film of electron beam deposition one deck 400-600nm at carbon film;
It is the Ar gas of 30-90sccm that the print that (8) will deposit the Ni film places flow velocity, is 1000-1200 ℃ of lower annealing 10-30 minute in temperature, makes carbon film reconstitute patterned graphene in graph position;
(9) print with the patterned graphene that generates places HCl and CuSO 4To remove the Ni film, obtain the patterned graphene material in the mixed solution.
2. the method for preparing patterned graphene based on SiC and the chlorine reaction of Ni film annealing according to claim 1 is characterized in that described step (1) cleans the SiC print, is to use first NH 4OH+H 2O 2Reagent soaked the SiC print 10 minutes, took out post-drying, to remove print surface organic remains; Re-use HCl+H 2O 2Reagent soaked print 10 minutes, took out post-drying, to remove ionic contamination.
3. the method for preparing patterned graphene based on SiC and the chlorine reaction of the annealing of Ni film according to claim 1 is characterized in that utilizing in the described step (2) PECVD deposit SiO 2, its process conditions are:
SiH 4, N 2O and N 2Flow velocity is respectively 30sccm, 60sccm and 200sccm,
Cavity pressure is 3.0Pa,
Radio-frequency power is 100W,
Deposition temperature is 150 ℃,
Deposition time is 30-90min.
4. the Ni film annealing patterned graphene preparation method based on SiC and chlorine reaction according to claim 1 is characterized in that Ar gas and Cl that described step (5) passes into 2Gas, its flow velocity is respectively 95-98sccm and 5-2sccm.
5. the Ni film annealing patterned graphene preparation method based on SiC and chlorine reaction according to claim 1 is characterized in that buffered hydrofluoric acid solution in the described step (6), 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 SiC and chlorine reaction according to claim 1, the condition that it is characterized in that electron beam deposition in the described step (7) are substrate to the distance of target is 50cm, and reative cell pressure is 5 * 10 -4Pa, line are 40mA, and evaporation time is 10-30min.
7. the Ni film annealing patterned graphene preparation method based on SiC and chlorine reaction according to claim 1 is characterized in that the crystal formation of described SiC print adopts 4H-SiC.
8. the Ni film annealing patterned graphene preparation method based on SiC and chlorine reaction according to claim 1 is characterized in that the crystal formation of described SiC print is adopted or 6H-SiC.
CN2012104845351A 2012-11-23 2012-11-23 Ni film annealing graphical graphene preparation method on basis of reaction of SiC and chlorine Pending CN102931060A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103183524A (en) * 2013-03-12 2013-07-03 西安电子科技大学 Preparation method of large-area graphene on SiC substrate based on Ni film annealing

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CN102674331A (en) * 2012-05-23 2012-09-19 西安电子科技大学 Method for preparing structured graphene by reaction of SiC and Cl2 based on Ni film annealing
CN102674332A (en) * 2012-05-23 2012-09-19 西安电子科技大学 Method for preparing structured graphene by reaction of SiC and Cl2 based on Cu film annealing
CN102674333A (en) * 2012-05-23 2012-09-19 西安电子科技大学 Method for preparing structured graphene based on reaction of Cl2 and 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

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Publication number Priority date Publication date Assignee Title
WO2009129194A2 (en) * 2008-04-14 2009-10-22 Massachusetts Institute Of Technology Large-area single- and few-layer graphene on arbitrary substrates
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
CN102674331A (en) * 2012-05-23 2012-09-19 西安电子科技大学 Method for preparing structured graphene by reaction of SiC and Cl2 based on Ni film annealing
CN102674332A (en) * 2012-05-23 2012-09-19 西安电子科技大学 Method for preparing structured graphene by reaction of SiC and Cl2 based on Cu film annealing
CN102674333A (en) * 2012-05-23 2012-09-19 西安电子科技大学 Method for preparing structured graphene based on reaction of Cl2 and Ni film annealing

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103183524A (en) * 2013-03-12 2013-07-03 西安电子科技大学 Preparation method of large-area graphene on SiC substrate based on Ni film annealing

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Application publication date: 20130213