CN102674333B - Method for preparing structured graphene based on reaction of Cl2 and Ni film annealing - Google Patents
Method for preparing structured graphene based on reaction of Cl2 and Ni film annealing Download PDFInfo
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- CN102674333B CN102674333B CN2012101623852A CN201210162385A CN102674333B CN 102674333 B CN102674333 B CN 102674333B CN 2012101623852 A CN2012101623852 A CN 2012101623852A CN 201210162385 A CN201210162385 A CN 201210162385A CN 102674333 B CN102674333 B CN 102674333B
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Abstract
The invention discloses a method for preparing structured graphene based on reaction of Cl2 and Ni film annealing, mainly aiming at solving the problems that the graphene prepared by the prior art is poor in continuity and uneven in the number of layers. The realization process of the method comprises the steps of: (1) leading a carbide layer to grow on a Si substrate for transition; (2) leading a 3C-SiC film to grow at the temperature of 1200-1300 DEG C; (3) depositing a layer of SiO2 on the surface of the 3C-SiC film, and carving a graphic window; (4) after the graphic window is formed, leading the exposed 3C-SiC to have reaction with Cl2 at the temperature of 700-1100 DEG C, and generating a carbon film; (5) then, putting the generated carbon film sample piece into a buffer hydrofluoric acid solution, and removing the SiO2 outside the window; (6) after that, depositing a layer of Ni film on another Si sample piece by electron beams; and (7) arranging the carbon film sample piece without SiO2 on the Ni film, and arranging in Ar gas; and carrying out annealing at 900-1100 DEG C for 15-30minutes, and generating the structured graphene at the position of the window of the carbon film. The structured graphene prepared by the invention is smooth in the surface, good in continuity and low in porosity, thus being used for making a microelectronic device.
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 annealing of Ni film and Cl
2The structuring graphene preparation method of reaction.
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 with a kind of very simple method.They,, from graphite, separating graphite flake, then are bonded at the two sides of thin slice on a kind of special adhesive tape, tear adhesive tape, just can be divided into two graphite flake.Constantly operation like this, so thin slice is more and more thinner, last, they have obtained the thin slice that only consists of one deck carbon atom, Here it is Graphene.After this, the new method for preparing Graphene emerges in an endless stream.Present preparation method mainly contains two kinds:
The first thermal decomposition SiC method, the method is by the monocrystal SiC heating to remove Si by lip-deep SiC is decomposed, and residual carbon forms Graphene subsequently.Yet the monocrystal SiC that uses in the SiC thermal decomposition is very expensive, and the Graphene that grows out is island and distributes, and the number of plies is inhomogeneous, and because photoetching process can make the electron mobility of Graphene, reduces while making device, thereby has affected device performance.
The second chemical vapour deposition technique, the method provides a kind of controlled effective ways that prepare Graphene, it is by planar substrates, as metallic film, metal single crystal etc., be placed in the decomposable presoma of high temperature, in the atmosphere such as methane, ethene, by high annealing, make carbon atom be deposited on substrate surface and form Graphene, finally with after chemical corrosion method removal metallic substrates, obtaining independently graphene film.By the type of selecting substrate, the temperature of growth, the parameters such as flow of presoma, can regulate and control the growth of Graphene, as growth rate, thickness, area etc., it is strong that the shortcoming of the method maximum is that the graphene sheet layer that obtains and substrate interact, lost the character of many single-layer graphenes, and the continuity of Graphene not fine.
Summary of the invention
The object of the invention is to for above-mentioned the deficiencies in the prior art, propose a kind of based on the annealing of Ni film and Cl
2The structuring graphene preparation method of reaction, with Cost reduction, improve Graphene surface flatness and continuity, reduction porosity, realization growth structure functionalized graphene optionally on the 3C-SiC substrate, to exempt, in follow-up manufacture device process, to carry out to Graphene the technical process of etching, the electron 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 carried out to standard cleaning;
(2) the Si substrate base after cleaning is put into CVD system response chamber, and reative cell is vacuumized and reaches 10
-7The mbar rank;
(3) at H
2In the situation of protection, make reative cell progressively be warming up to 900 ℃-1200 ℃ of carburizing 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) reative cell is warming up to 1200 ℃-1300 ℃ of growth temperatures, 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
2Under protection, progressively be cooled to room temperature, complete the growth of 3C-SiC film;
(5) at the 3C-SiC film surface of having grown, utilize plasma enhanced chemical vapor deposition PECVD method, the thick SiO of deposit one deck 0.5-1 μ m
2Mask layer;
(6) on mask layer surface, be coated with one deck photoresist, and carve the window identical with the substrate shape of the device of required making, expose 3C-SiC, form structured graphics;
(7) print after windowing is placed in quartz ampoule, is heated to 700-1100 ℃;
(8) in quartz ampoule, pass into Ar gas and Cl
2The mist of gas, continue 3-5min, makes Cl
2With exposed 3C-SiC, react, generate carbon film;
(9) the carbon film print of generation is placed in to buffered hydrofluoric acid solution to remove the SiO outside window
2
(10) the thick Ni film of electron beam deposition 300-500nm on another sheet Si print;
(11) will remove SiO
2After the carbon film print be placed on the Ni film, then they together are placed in to Ar gas, in temperature, be annealing 15-30 minute under 900-1100 ℃, make carbon film reconstitute Graphene at the window's position, then the Ni film taken away from the Graphene print.
The present invention compared with prior art has following advantage:
1. the present invention anneals on the Ni film owing to utilizing, thereby the carbon film that generates more easily reconstitutes continuity Graphene preferably.
2. the present invention is due to the structure functionalized graphene of optionally having grown, and while on this Graphene, making device, without Graphene is carried out to etching, thereby the electron mobility in Graphene can not reduce, and guaranteed the device performance of making.
3. 3C-SiC and Cl in the present invention
2Can under lower temperature and normal pressure, react, and reaction rate is fast.
4. the present invention is owing to utilizing 3C-SiC and Cl
2Solid/liquid/gas reactions, thereby the Graphene smooth surface that generates, voidage is low, and thickness is easily controlled.
The present invention due to growth during 3C-SiC first 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 due to the 3C-SiC heteroepitaxial growth on the Si disk, thereby low with the method growth structure functionalized graphene cost.
The accompanying drawing explanation
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 resistance furnace 2.
With reference to Fig. 2, manufacture method of the present invention provides following three kinds of embodiment.
Embodiment 1
Step 1: remove the sample surfaces pollutant.
Si substrate base to 4 inches carries out the cleaning surfaces processing, namely first uses 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: the Si substrate base is put into to CVD system response chamber, reative cell is vacuumized and reaches 10
-7The mbar rank.
Step 3: growth carburization zone.
At H
2In the situation of protection, reaction chamber temperature is risen to the carburizing temperature of 900 ℃, then to reative cell, pass into the C that flow is 30sccm
3H
8, at Si Grown one deck carburization zone, growth time is 10min.
Step 4: growth 3C-SiC film on carburization zone.
Reaction chamber temperature is risen to rapidly to the growth temperature of 1200 ℃, pass into the SiH that flow is respectively 20sccm and 40sccm
4And C
3H
8, carrying out the 3C-SiC thin film heterogeneity epitaxial growth, growth time is 60min; Then at H
2Under protection, progressively be cooled to room temperature, complete the growth of 3C-SiC film.
Step 5: the 3C-SiC film surface deposit one deck SiO that is growing
2Mask layer.
(5.1) the 3C-SiC film print of having grown is put into to the 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 the PECVD system, pass into the SiH that flow velocity is respectively 30sccm, 60sccm and 200sccm
4, N
2O and N
2, continue 30min, make SiH
4And N
2O reacts, thereby at the thick SiO of 3C-SiC film surface deposit one deck 0.5 μ m
2Mask layer.
Step 6: at SiO
2On mask layer, carve graphical window.
At SiO
2On mask layer, carve graphical window.
(6.1) at SiO
2Spin coating one deck photoresist on mask layer;
(6.2) according to the substrate shape that will make device, make reticle, and then carry out photoetching, figure on reticle is transferred to SiO
2On mask layer;
(6.3) with buffered hydrofluoric acid, corrode SiO
2Mask layer, etch graphical window, exposes 3C-SiC, forms structured graphics.
Step 7: the quartz ampoule of packing into of the print after windowing, and exhaust heating.
(7.1) during the print after windowing is packed quartz ampoule 1 into, quartz ampoule is placed in to resistance furnace 2;
(7.2) from air inlet 3 to quartz ampoule, passing into flow velocity is the Ar gas of 80sccm, to quartz ampoule carry out 10 minutes emptying, gas 4 is discharged from gas outlet;
(7.3) open the resistance furnace mains switch, quartz ampoule is heated to 700 ℃.
Step 8: generate carbon film
To quartz ampoule, pass into Ar gas and the Cl that flow velocity is respectively 98sccm and 2sccm
2Gas, continue 5 minutes, makes Cl
23C-SiC reaction with exposed, generate carbon film.
Step 9: remove remaining SiO
2.
By the carbon film print of generation, from quartz ampoule, taking out and be placed in hydrofluoric acid and water proportioning is that the buffered hydrofluoric acid solution of 1:10 is removed the SiO outside window
2.
Step 10: deposit Ni film on the Si print.
Get another Si print and put on the slide of electron beam evaporation deposition machine, the adjustment 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, the thick Ni film of deposition one deck 300nm on the Si print.
Step 11: reconstitute Graphene.
(11.1) will remove SiO
2After the carbon film print be placed on the Ni film;
(11.2) carbon film print and Ni film integral body being placed in to the Ar gas that flow velocity is 90sccm, is to anneal 15 minutes under 1100 ℃ in temperature, makes carbon film reconstitute continuous structuring Graphene at the window's position;
(11.3) the Ni film is taken away from the structuring Graphene, obtain structuring Graphene print.
Embodiment 2
Step 1: remove the sample surfaces pollutant.
Si substrate base to 8 inches carries out the cleaning surfaces processing, namely first uses 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: 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 carburizing temperatures, then to reative cell, pass into the C that flow is 30sccm
3H
8, at Si Grown one deck carburization zone, growth time is 7min.
Step 4: growth 3C-SiC film on carburization zone.
Reaction chamber temperature is risen to rapidly to 1200 ℃ of growth temperatures, pass into the SiH that flow is respectively 25sccm and 50sccm
4And C
3H
8, carrying out the 3C-SiC thin film heterogeneity epitaxial growth, growth time is 45min; Then at H
2Under protection, progressively be cooled to room temperature, complete the growth of 3C-SiC film.
Step 5: the 3C-SiC film surface deposit one deck SiO that is growing
2.
The 3C-SiC film print of having grown is put into to 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 the SiH that flow velocity is respectively 30sccm, 60sccm and 200sccm
4, N
2O and N
2, continue 75min, make SiH
4And N
2O reacts, thereby at the thick SiO of 3C-SiC print surface deposition one deck 0.8 μ m
2Mask layer.
Step 6: identical with the step 6 of embodiment 1.
Step 7: the quartz ampoule of packing into of the print after windowing, and exhaust heating.
Print after windowing is placed in to quartz ampoule 1, quartz ampoule is placed in to resistance furnace 2; From air inlet 3 to quartz ampoule, passing into flow velocity is the Ar gas of 80sccm, to quartz ampoule carry out 10 minutes emptying, gas 4 is discharged from gas outlet; Open again the resistance furnace mains switch, quartz ampoule is heated to 1000 ℃.
Step 8: generate carbon film
To quartz ampoule, pass into Ar gas and the Cl that flow velocity is respectively 97sccm and 3sccm
2Gas, continue 4 minutes, makes Cl
23C-SiC reaction with exposed, generate carbon film.
Step 9: identical with the step 9 of embodiment 1.
Step 10: deposit Ni film on the Si print.
Get another Si print and put on the slide of electron beam evaporation deposition machine, slide is adjusted to 50cm to the distance of target, and reative cell pressure is evacuated to 5 * 10
-4Pa, the adjusting line is 40mA, evaporation 15min, the thick Ni film of deposition one deck 400nm on the Si print.
Step 11: reconstitute Graphene.
To remove SiO
2After the carbon film print be placed on the Ni film; Carbon film print and Ni film integral body are placed in to the Ar gas that flow velocity is 55sccm, are to anneal 20 minutes under 1000 ℃ in temperature, make carbon film reconstitute continuous structuring Graphene at the window's position; The Ni film is taken away from the structuring Graphene, obtain structuring Graphene print.
Embodiment 3
Steps A: the Si substrate base to 12 inches carries out the cleaning surfaces processing, namely first uses 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: 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 carburizing temperatures, then to reative cell, pass into 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 ℃ of growth temperatures, 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
2Under protection, progressively be cooled to room temperature.
Step e: the 3C-SiC print of having grown is put into to 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 the SiH that flow velocity is respectively 30sccm, 60sccm 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 μ m
2Mask layer.
Step F: identical with the step 6 of embodiment 1.
Step G: the print after windowing is placed in quartz ampoule 1, and quartz ampoule is placed in to resistance furnace 2; From air inlet 3 to quartz ampoule, passing into flow velocity is the Ar gas of 80sccm, to quartz ampoule carry out 10 minutes emptying, gas 4 is discharged from gas outlet; Open again the resistance furnace mains switch, quartz ampoule is heated to 1100 ℃.
Step H: pass into Ar gas and the Cl that flow velocity is respectively 95sccm and 5sccm in quartz ampoule
2Gas, the duration is 3 minutes, makes Cl
23C-SiC reaction with exposed, generate carbon film.
Step I: identical with the step 9 of embodiment 1.
Step J: get another Si print and put on the slide of electron beam evaporation deposition machine, 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, the thick Ni film of deposition one deck 500nm on the Si print.
Step K: will remove SiO
2After the carbon film print be placed on the Ni film; Carbon film print and Ni film integral body are placed in to the Ar gas that flow velocity is 30sccm, are to anneal 30 minutes under 900 ℃ in temperature, make carbon film reconstitute continuous structuring Graphene at the window's position; The Ni film is taken away from the structuring Graphene, obtain structuring Graphene print.
Claims (7)
1. based on the Ni film, anneal and Cl for one kind
2The structuring graphene preparation method of reaction comprises the following steps:
(1) the Si substrate base of 4-12 inch carried out to standard cleaning, namely first use 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;
(2) the Si substrate base after cleaning is put into CVD system response chamber, and reative cell is vacuumized and reaches 10
-7The Mbar rank;
(3) at H
2In the situation of protection, make reative cell progressively be warming up to 900 ℃-1200 ℃ of carburizing 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) reative cell is warming up to 1200 ℃-1300 ℃ of growth temperatures, 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
2Under protection, progressively be cooled to room temperature, complete the growth of 3C-SiC film;
(5) at the 3C-SiC film surface of having grown, utilize plasma enhanced chemical vapor deposition PECVD method, the thick SiO of deposit one deck 0.5-1 μ m
2Mask layer;
(6) on mask layer surface, be coated with one deck photoresist, and carve the window identical with the substrate shape of the device of required making, expose 3C-SiC, form structured graphics;
(7) print after windowing is placed in quartz ampoule, is heated to 700-1100 ℃;
(8) in quartz ampoule, pass into Ar gas and Cl
2The mist of gas, continue 3-5min, makes Cl
2With exposed 3C-SiC, react, generate carbon film;
(9) the carbon film print of generation is placed in to buffered hydrofluoric acid solution to remove the SiO outside window
2
(10) the thick Ni film of electron beam deposition 300-500nm on another sheet Si print;
(11) will remove SiO
2After the carbon film print be placed on the Ni film, then they together are placed in to Ar gas, in temperature, be annealing 15-30 minute under 900-1100 ℃, make carbon film reconstitute Graphene at the window's position, then the Ni film taken away from the Graphene print.
2. according to claim 1 based on the annealing of Ni film and Cl
2The structuring graphene preparation method of reaction, 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. according to claim 1 based on the annealing of Ni film and Cl
2The structuring graphene preparation method of reaction, what it is characterized in that described step (5) utilizes PECVD deposit SiO
2, its process conditions are: SiH
4, N
2O and N
2Flow velocity be respectively 30sccm, 60sccm 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. according to claim 1 based on the annealing of Ni film and Cl
2The structuring graphene preparation method of reaction, 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. according to claim 1 based on the annealing of Ni film and Cl
2The structuring graphene preparation method of reaction, is characterized in that buffered hydrofluoric acid solution in described step (9), is to be that hydrofluoric acid and the water of 1:10 is formulated with ratio.
6. according to claim 1 based on the annealing of Ni film and Cl
2The structuring graphene preparation method of reaction is characterized in that the condition of electron beam deposition in described step (10) is: substrate is 50cm to the distance of target, and reative cell pressure is 5 * 10
-4Pa, line are 40mA, and evaporation time is 10-20min.
7. according to claim 1 based on the annealing of Ni film and Cl
2The structuring graphene preparation method of reaction, while it is characterized in that described step (11) annealing, the flow velocity of Ar gas is 30-90sccm.
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| CN102931060A (en) * | 2012-11-23 | 2013-02-13 | 西安电子科技大学 | Ni film annealing graphical graphene preparation method on basis of reaction of SiC and chlorine |
| CN103165468A (en) * | 2013-01-31 | 2013-06-19 | 西安电子科技大学 | Preparing method of side grid graphene transistor through reaction of silicon carbide (SiC) and chlorine gas (Cl2) based on copper (Cu) membrane annealing |
| CN103151265A (en) * | 2013-01-31 | 2013-06-12 | 西安电子科技大学 | Manufacturing method of silicon (Si) substrate upper side grid grapheme field effect tube based on copper (Cu) film annealing |
| CN103165470A (en) * | 2013-01-31 | 2013-06-19 | 西安电子科技大学 | Preparing method of side grid graphene transistor based on copper (Cu) membrane annealing and chlorine (Cl2) reaction |
| 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 |
| CN103311104B (en) * | 2013-06-13 | 2016-01-27 | 苏州大学 | A kind of preparation method of Graphene |
| CN107381542A (en) * | 2017-09-07 | 2017-11-24 | 蚌埠玻璃工业设计研究院 | A kind of preparation facilities of graphene film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101285175A (en) * | 2008-05-29 | 2008-10-15 | 中国科学院化学研究所 | Process for preparing graphenes by chemical vapour deposition method |
| CN101602503A (en) * | 2009-07-20 | 2009-12-16 | 西安电子科技大学 | The method of 4H-SiC silicon face extending and growing graphene |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101285175A (en) * | 2008-05-29 | 2008-10-15 | 中国科学院化学研究所 | Process for preparing graphenes by chemical vapour deposition method |
| CN101602503A (en) * | 2009-07-20 | 2009-12-16 | 西安电子科技大学 | The method of 4H-SiC silicon face extending and growing graphene |
Non-Patent Citations (3)
| Title |
|---|
| "Painted graphitic carbon films formed underneath Ni templates";Meng-Yu Lin et al.;《Physica Status Solidi C》;20111227;第9卷(第2期);第179-182页 * |
| Meng-Yu Lin et al.."Painted graphitic carbon films formed underneath Ni templates".《Physica Status Solidi C》.2011,第9卷(第2期),第179-182页. |
| Zhen-Yu Juang et al.."Synthesis of graphene on silicon carbide substrates at low temperature".《Carbon》.2009,第47卷第2026-2031页. |
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