CN102674330A - Method for preparing structured graphene on SiC substrate based on Cu film annealing - Google Patents
Method for preparing structured graphene on SiC substrate based on Cu film annealing Download PDFInfo
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Abstract
The invention discloses a method for preparing structured graphene on a SiC substrate based on Cu film annealing, and mainly solves the problems that the surface of the graphene prepared by using the prior art is unsmooth, low in continuity and non-uniform in layer number and the problem that the electronic mobility of the graphene is reduced because of a photoetching process during manufacture of a device. The method comprises the following steps of: (1) performing standard cleaning on a SiC sample; (2) depositing a layer of SiO2 on the surface of the SiC sample, and etching a graphical window on the SiO2; (3) putting the sample with the window into a quartz pipe, and reacting gaseous CC14 with exposed SiC at the temperature of between 800 and 1,100 DEG C so as to generate a double-layer carbon film; (4) putting the generated double-layer carbon film into a buffering hydrofluoric acid solution, and removing the SiO2 outside the window; and (5) putting the sample subjected to SiO2 removal on a Cu film, putting in argon (Ar), and annealing at the temperature of between 900 and 1,100 DEG C for 15 to 25 minutes so as to generate the double-layer structured graphene at the window. The method has the advantages that the process is simple, the safety is high, the surface of the double-layer structured graphene is smooth, the continuity is good, and the porosity is low; and the double-layer structured graphene can be applied to manufacture of microelectronic devices.
Description
Technical field
The invention belongs to microelectronics technology, relate to semiconductor film material and preparation method thereof, specifically be based on structurizing graphene preparation method on the Cu film annealed SiC substrate.
Technical background
It is in 2004 that Graphene appears in the laboratory, and at that time, two scientist An Delie Jim of Univ Manchester UK and the Ke Siteyanuowo Lip river husband that disappears found that they can obtain more and more thinner graphite flake with a kind of very simple method.They separate graphite flake from graphite, the two sides with thin slice is bonded on a kind of special adhesive tape then, tears adhesive tape, just can be divided into two graphite flake.Operation so constantly, last so thin slice is more and more thinner, they have obtained the thin slice that only is made up of one deck carbon atom, Here it is Graphene.From now on, the novel method of preparation Graphene emerges in an endless stream, but uses maximum mainly contain following two kinds:
The one, chemical Vapor deposition process provides a kind of effective ways of controlled preparation Graphene; It is with planar substrates; Place the decomposable presoma of high temperature like mf, metal single crystal etc.; In atmosphere such as methane, ethene, make carbon atom be deposited on substrate surface through high temperature annealing and form Graphene, at last with obtaining independently graphene film after the chemical corrosion method removal metal base.The growth of the adjustable Graphenes of parameter such as flow of the type through selecting substrate, the temperature of growth, presoma; Like growth velocity, thickness, area etc.; The maximum shortcoming of this method is that the Graphene lamella and the substrate that obtain interact strong; Lost the character of many single-layer graphenes, and the continuity of Graphene not fine.
The 2nd, thermolysis SiC method: to remove Si through lip-deep SiC is decomposed, residual subsequently carbon forms Graphene with the monocrystal SiC heating.Yet the monocrystal SiC that uses in the SiC thermolysis is very expensive, and the Graphene that grows out is island and distributes, and hole is many, and the number of plies is inhomogeneous, and when making device because photoetching process can make the electronic mobility of Graphene reduce, thereby influenced device performance.
Existing preparation method of graphene; Like application number is " method of process for preparing graphenes by chemical vapour deposition " patent of 200810113596.0, and disclosed method is: at first prepare catalyzer, carry out high temperature chemical vapor deposition then; The substrate that will have catalyzer is put into anoxic reactor; Make substrate reach 500-1200 ℃, feed the carbon containing source of the gas again and carry out electroless plating and obtain Graphene, then Graphene is purified; Promptly use s.t. or evaporation under low pressure, high temperature, to remove catalyzer.The main drawback of this method is: complex process, need the special catalyzer of removing, and energy consumption is big, and production cost is high.
Summary of the invention
The objective of the invention is to deficiency to above-mentioned prior art; Propose a kind of based on structurizing graphene preparation method on the Cu film annealed SiC substrate; To improve Graphene surface flatness and continuity, to reduce porosity; And exempt the technological process that in follow-up manufacturing device process, will carry out etching to Graphene, and guarantee that the electronic mobility of Graphene is stable, improve device performance.
For realizing above-mentioned purpose, preparation method of the present invention may further comprise the steps:
(1) the SiC print is cleaned, to remove surface contaminant;
(2) the thick SiO of SiC print surface by utilizing plasma enhanced chemical vapor deposition PECVD deposit one deck 0.5-1 μ m after cleaning
2, as mask;
(3) be coated with one deck photoresist material in mask surface, on mask, carve the identical window of substrate shape with the device of required making again, expose SiC, form structured graphics;
(4) print after will windowing places silica tube, and connects each device, again silica tube is heated to 800-1000 ℃;
(5) to CCl is housed
4The there-necked flask of liquid is heated to 60-80 ℃, in there-necked flask, feeds Ar gas again, utilizes Ar gas to carry CCl
4Steam gets in the silica tube, makes CCl
4SiC reaction 30-120min with exposed generates double-deck carbon film;
The double-deck carbon film print that (6) will generate places buffered hydrofluoric acid solution to remove the SiO beyond the window
2
(7) will remove SiO
2After double-deck carbon film print place on the Cu film; Again they are together placed Ar gas; Be 900-1100 ℃ in temperature and annealed 15-25 minute down, make double-deck carbon film reconstitute the bilayer structure Graphene, again the Cu film is taken away from bilayer structure Graphene print at the window's position.
The present invention compared with prior art has following advantage:
1. the present invention is owing to utilize SiC and CCl
4Gas reaction, thereby the double-layer graphite alkene smooth surface that generates, porosity is low.
2. the present invention anneals owing to being utilized on the Cu film, thereby the easier reconstruct of the carbon film that generates forms continuity structurizing Graphene preferably.
3. the present invention is because the structure fossil China ink alkene of optionally having grown, thereby no longer needs photoetching when making device, makes that the electronic mobility in the Graphene can not reduce, and the device performance of solid making is guaranteed.
4. the method technology of the present invention's use is simple, and save energy is safe.
Description of drawings
Fig. 1 is the device synoptic diagram that the present invention prepares Graphene;
Fig. 2 is the schema that the present invention prepares Graphene.
Embodiment
With reference to Fig. 1, preparation equipment of the present invention is mainly by three-way valve 3, there-necked flask 8, and water-bath 9, silica tube 5, resistance furnace 6 is formed; Three-way valve 3 links to each other with silica tube 5 through first channel 1, link to each other with the left side mouth of there-necked flask 8 through second passage 2, and the right side mouth of there-necked flask 8 links to each other with silica tube 5, and CCl is housed in the there-necked flask
4Liquid, and it is placed in the water-bath 9, and silica tube 5 is placed in the resistance furnace 6.Three-way valve 3 is provided with inlet mouth 4, is used in equipment, feeding gas.
With reference to Fig. 2, making 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 sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue;
(1.2) the 6H-SiC print that will remove behind the surperficial organic residue re-uses HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, 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 plasma enhanced chemical vapor deposition 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 the PECVD system, feed the SiH that flow velocity is respectively 30sccm, 60sccm and 200sccm
4, N
2O and N
2, and lasting 30min, make SiH
4And N
2O reacts, thereby at the thick SiO of 6H-SiC print surface deposition one deck 0.5 μ m
2
Step 3: at SiO
2Carve graphical window on the layer.
(3.1) at SiO
2Spin coating one deck photoresist material on the layer;
(3.2) according to make device substrate shape process reticle, and then carry out photoetching, with figure transfer on the reticle to SiO
2On the layer;
(3.3) corrode SiO with buffered hydrofluoric acid
2Etch graphical window, expose 6H-SiC, form structured graphics.
Step 4: the silica tube of packing into of the print after will windowing, and exhaust heating.
(4.1) print after will windowing is put into silica tube 5, and places resistance furnace 6 to silica tube; Again with CCl
4Liquid is packed in the there-necked flask 10, and there-necked flask is put into water-bath 11, according to Fig. 1 silica tube is connected with there-necked flask then;
(4.2) the inlet mouth 4 feeding flow velocitys from three-way valve 3 are the Ar gas of 80ml/min, and utilize three-way valve 3 control Ar gas to get into from first channel 1 silica tube was carried out emptying 30 minutes, make air 7 discharges from the air outlet in the silica tube;
(4.3) open the resistance furnace power switch, silica tube is warming up to 800 ℃.
Step 5: the double-deck carbon film of growing.
(5.1) the fetch boiling water power supply of bath 9 is to being equipped with CCl
4The there-necked flask 8 of liquid is heated to 65 ℃;
(5.2) after resistance furnace reaches 800 ℃ of setting, the swivel tee valve, making flow velocity is that the Ar gas of 50ml/min flows into there-necked flasks from second passage 2, and carries CCl
4Steam gets into silica tube, makes gaseous state CCl
4In silica tube, reacted 20 minutes with exposed 6H-SiC, generate double-deck carbon film.
Step 6: remove remaining SiO
2
The double-deck carbon film print that generates is taken out and places hydrofluoric acid and water proportioning from silica tube is the buffered hydrofluoric acid solution of 1:10, to remove the SiO beyond the window
2
Step 7: reconstitute the bilayer structure Graphene.
(7.1) will remove SiO
2After double-deck carbon film print to place thickness be on the Cu film of 250nm;
(7.2) double-deck carbon film print and Cu film integral body being placed flow velocity is the Ar gas of 20ml/min, is 900 ℃ of annealing 25 minutes down in temperature, makes carbon film reconstitute successive structurizing Graphene at the window's position;
(7.3) the Cu film is taken away from bilayer structure Graphene print, obtain bilayer structure Graphene print.
Step 1: clean the 4H-SiC print, to remove surface contaminant.
The 4H-SiC substrate base is used NH earlier
4OH+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove ionic contamination.
Step 2: at 4H-SiC print surface deposition one deck SiO
2
4H-SiC print after cleaning is put into plasma enhanced chemical vapor deposition 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, feed 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 4H-SiC print surface deposition one deck 0.8 μ m
2
Step 3: at SiO
2Carve graphical window on the layer.
At SiO
2Spin coating one deck photoresist material on the layer; According to make device substrate shape process reticle, and then carry out photoetching, with figure transfer on the reticle to SiO
2On the layer; Corrode SiO with buffered hydrofluoric acid
2Etch graphical window, expose 4H-SiC, form structured graphics.
Step 4: the silica tube of packing into of the print after will windowing, and exhaust heating.
Print after windowing is placed silica tube 5, and place resistance furnace 6 to silica tube; Again with CCl
4Liquid is packed in the there-necked flask 10, and there-necked flask is put into water-bath 11, according to Fig. 1 silica tube is connected with there-necked flask then; From the inlet mouth 4 feeding flow velocitys of three-way valve 3 is the Ar gas of 80ml/min, and utilizes three-way valve 3 control Ar gas to get into from first channel 1 silica tube was carried out emptying 30 minutes, makes air 7 discharges from the air outlet in the silica tube; Open the resistance furnace power switch, silica tube is warming up to 900 ℃.
Step 5: the double-deck carbon film of growing.
Bath 9 power supplys of fetching boiling water are to being equipped with CCl
4The there-necked flask 8 of liquid is heated to 70 ℃; Reach 900 ℃ of setting when resistance furnace after, the swivel tee valve, making flow velocity is that the Ar gas of 60ml/min flows into there-necked flasks from second passage 2, and carries CCl
4Steam gets into silica tube, makes gaseous state CCl
4In silica tube, reacted 60 minutes with exposed 4H-SiC, generate double-deck carbon film.
Step 6: identical with the step 6 of embodiment 1.
Step 7: reconstitute the bilayer structure Graphene.
To remove SiO
2After double-deck carbon film print to place thickness be on the Cu film of 280nm; Again they together being placed flow velocity is the Ar gas of 60ml/min; Being 1000 ℃ in temperature annealed 20 minutes down; Make carbon film reconstitute successive structurizing Graphene, again the Cu film is taken away from bilayer structure Graphene print, obtain bilayer structure Graphene print at the window's position.
Embodiment 3
Steps A: the 6H-SiC substrate base is carried out cleaning surfaces handle, promptly use NH earlier
4OH+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove the sample surfaces organic residue; Re-use HCl+H
2O
2Reagent soaked sample 10 minutes, took out the back oven dry, to remove ionic contamination.
Step B: the 6H-SiC print after will cleaning is put into plasma enhanced chemical vapor deposition 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, feed the SiH that flow velocity is respectively 30sccm, 60sccm and 200sccm
4, N
2O and N
2, the time length is 100min, makes SiH
4And N
2O reacts, thereby at the thick SiO of 6H-SiC print surface deposition one deck 1 μ m
2
Step C: identical with the step 3 of embodiment 1.
Step D: the print after will windowing places silica tube 5, and places resistance furnace 6 to silica tube; Again with CCl
4Liquid is packed in the there-necked flask 10, and there-necked flask is put into water-bath 11, according to Fig. 1 silica tube is connected with there-necked flask then; From the inlet mouth 4 feeding flow velocitys of three-way valve 3 is the Ar gas of 80ml/min, and utilizes three-way valve 3 control Ar gas to get into from first channel 1 silica tube was carried out emptying 30 minutes, makes air 7 discharges from the air outlet in the silica tube; Open the resistance furnace power switch, silica tube is warming up to 1100 ℃.
Step e: bath 9 power supplys of fetching boiling water, to CCl is housed
4The there-necked flask 8 of liquid is heated to 80 ℃; Reach 1100 ℃ of setting when resistance furnace after, the swivel tee valve, making flow velocity is that the Ar gas of 80ml/min flows into there-necked flasks from second passage 2, and carries CCl
4Steam gets into silica tube, makes gaseous state CCl
4In silica tube, reacted 120 minutes with exposed 6H-SiC, generate double-deck carbon film.
Step F: identical with the step 6 of embodiment 1.
Step G: will remove SiO
2After double-deck carbon film print to place thickness be on the Cu film of 300nm; Again they together being placed flow velocity is the Ar gas of 100ml/min; Being 1100 ℃ in temperature annealed 15 minutes down; Make carbon film reconstitute successive structurizing Graphene, again the Cu film is taken away from bilayer structure Graphene print, obtain bilayer structure Graphene print at the window's position.
Claims (8)
1. one kind based on structurizing graphene preparation method on the Cu film annealed SiC substrate, may further comprise the steps:
(1) the SiC print is cleaned, to remove surface contaminant;
(2) the thick SiO of SiC print surface by utilizing plasma enhanced chemical vapor deposition PECVD deposit one deck 0.4-1.2 μ m after cleaning
2, as mask;
(3) be coated with one deck photoresist material in mask surface, on mask, carve the identical window of substrate shape with the device of required making again, expose SiC, form structured graphics;
(4) print after will windowing places silica tube, and connects each device, again silica tube is heated to 800-1000 ℃;
(5) to CCl is housed
4The there-necked flask of liquid is heated to 60-80 ℃, in there-necked flask, feeds Ar gas again, utilizes Ar gas to carry CCl
4Steam gets in the silica tube, makes CCl
4SiC reaction 30-120min with exposed generates double-deck carbon film;
The double-deck carbon film print that (6) will generate places buffered hydrofluoric acid solution to remove the SiO beyond the window
2
(7) will remove SiO
2After double-deck carbon film print place on the Cu film; Again they are together placed Ar gas; Be 900-1100 ℃ in temperature and annealed 15-25 minute down, make double-deck carbon film reconstitute the bilayer structure Graphene, again the Cu film is taken away from bilayer structure Graphene print at the window's position.
2. according to claim 1 based on structurizing graphene preparation method on the Cu film annealed SiC substrate, it is characterized in that said step (1) cleans the SiC print, be to use NH earlier
4OH+H
2O
2Reagent soaked the SiC print 10 minutes, took out the back oven dry, to remove print surface organic residue; Re-use HCl+H
2O
2Reagent soaked print 10 minutes, took out the back oven dry, to remove ionic contamination.
3. according to claim 1 based on structurizing graphene preparation method on the Cu film annealed SiC substrate, it is characterized in that utilizing in the said step (2) PECVD deposit SiO
2, its processing condition 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 ℃,
Deposition time is 30-100min.
4. according to claim 1 based on structurizing graphene preparation method on the Cu film annealed SiC substrate, it is characterized in that the Ar gas velocity is 50-80ml/min in the said step (5).
5. according to claim 1 based on structurizing graphene preparation method on the Cu film annealed SiC substrate, it is characterized in that buffered hydrofluoric acid solution is that hydrofluoric acid and water ratio are 1:10 in the said step (6).
6. according to claim 1 based on structurizing graphene preparation method on the Cu film annealed SiC substrate, the flow velocity of Ar gas is 25-100ml/min when it is characterized in that said step (7) annealing.
7. according to claim 1 based on structurizing graphene preparation method on the Cu film annealed SiC substrate, it is characterized in that the Cu film thickness in the said step (7) is 250-300nm.
8. according to claim 1 based on structurizing graphene preparation method on the Cu film annealed SiC substrate, it is characterized in that the crystal formation of said SiC print adopts 4H-SiC or 6H-SiC.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102938367A (en) * | 2012-11-22 | 2013-02-20 | 西安电子科技大学 | SiC-substrate patterned graphene preparation method based on Cu film 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 |
| 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 |
| 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 |
| CN103183335A (en) * | 2013-03-12 | 2013-07-03 | 西安电子科技大学 | Cu film annealing based method for preparing large-area graphene on SiC substrate |
| CN104425215A (en) * | 2013-09-10 | 2015-03-18 | 三菱电机株式会社 | Method for manufacturing SiC semiconductor device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102938367A (en) * | 2012-11-22 | 2013-02-20 | 西安电子科技大学 | SiC-substrate patterned graphene preparation method based on Cu film 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 |
| 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 |
| 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 |
| CN103183335A (en) * | 2013-03-12 | 2013-07-03 | 西安电子科技大学 | Cu film annealing based method for preparing large-area graphene on SiC substrate |
| CN104425215A (en) * | 2013-09-10 | 2015-03-18 | 三菱电机株式会社 | Method for manufacturing SiC semiconductor device |
| CN104425215B (en) * | 2013-09-10 | 2017-05-10 | 三菱电机株式会社 | Method for manufacturing SiC semiconductor device |
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Application publication date: 20120919 |