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CN103107068A - Nickel (Ni) film annealing side gate graphene transistor preparation method based on reaction of silicon carbide (SiC) and chlorine gas - Google Patents

Nickel (Ni) film annealing side gate graphene transistor preparation method based on reaction of silicon carbide (SiC) and chlorine gas Download PDF

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CN103107068A
CN103107068A CN2013100398211A CN201310039821A CN103107068A CN 103107068 A CN103107068 A CN 103107068A CN 2013100398211 A CN2013100398211 A CN 2013100398211A CN 201310039821 A CN201310039821 A CN 201310039821A CN 103107068 A CN103107068 A CN 103107068A
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graphene
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郭辉
张晨旭
张玉明
张克基
雷天民
胡彦飞
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Xidian University
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Abstract

本发明公开了一种基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,主要解决现有技术制备的石墨烯晶体管栅介质导致沟道载流子迁移率降低以及不能有效控制电流传输特性的问题。其实现过程是:(1)清洗SiC样片;(2)在清洗后的SiC样片上淀积SiO2掩模,并在SiO2光刻出侧栅晶体管图形;(3)将光刻后的样片置于石英管中,与Cl2反应生成碳膜;(4)去除SiO2掩模;(5)在碳膜样片上电子束沉积一层Ni膜;(6)将碳膜样片置于Ar气中,退火生成侧栅石墨烯;(7)在石墨烯样片上淀积金属Pd/Au层并刻蚀成侧栅晶体管的金属接触。本发明制作的侧栅石墨烯晶体管载流子迁移率极高,能够精确控制单个晶体管沟道电流,并且避免顶栅石墨烯场效应管顶栅介质的散射效应。

Figure 201310039821

The invention discloses a method for preparing a Ni film annealed side-gate graphene transistor based on the reaction of SiC and chlorine gas, which mainly solves the problem that the gate dielectric of the graphene transistor prepared by the prior art reduces the channel carrier mobility and cannot effectively control the current transmission problem of characteristics. The realization process is: (1) cleaning the SiC sample; (2) depositing a SiO2 mask on the cleaned SiC sample, and photoetching the side gate transistor pattern on the SiO2 ; (3) taking the photoetched sample Place in a quartz tube and react with Cl to form a carbon film; (4) remove the SiO mask; (5) deposit a layer of Ni film on the carbon film sample by electron beam; (6) place the carbon film sample in Ar gas , annealing to generate side-gate graphene; (7) Deposit a metal Pd/Au layer on the graphene sample and etch to form the metal contact of the side-gate transistor. The carrier mobility of the side-gate graphene transistor produced by the invention is extremely high, the channel current of a single transistor can be precisely controlled, and the scattering effect of the top-gate dielectric of the top-gate graphene field effect transistor can be avoided.

Figure 201310039821

Description

Ni film annealing side grid Graphene transistor preparation method based on SiC and chlorine reaction
Technical field
The invention belongs to microelectronics technology, relate to the semiconductor device preparation method, specifically be based on the Ni film annealing side grid Graphene transistor preparation method of SiC and chlorine reaction.
Technical background
Along with people to high-performance, high reliability, the raising of low power consumption equipment demand becomes more to device property on integrated circuit and pays close attention to.Graphene, this material that is formed by two-dimensional hexagonal carbon lattice, after the Lip river husband that disappeared by two scientist An Delie Jim of Univ Manchester UK and Ke Siteyanuowo from 2004 due to its outstanding electricity structure characteristic finds to obtain, namely by as the candidate materials of making high performance device.
The preparation method of existing Graphene, it is " method of process for preparing graphenes by chemical vapour deposition " patent of 200810113596.0 as application number, disclosed method 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 evaporate under low pressure, high temperature, to remove catalyst.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.
Geim seminar in 2005 and Kim seminar find, under room temperature, Graphene has 10 times to the high carrier mobility of commercial silicon chip approximately 2 * 10 5cm 2/ Vs, and be subjected to the impact of temperature and doping effect very little, show the ballistic transport characteristic of room temperature submicron-scale, this be Graphene as the most outstanding advantage of nanometer electronic device, make the room temperature trajectory field effect transistor of electronic engineering field very attractive become possibility.Larger carrier mobility and low contact resistance help further to reduce the devices switch time, and the operation response characteristic of ultra-high frequency is another significant advantage of graphene-based electronic device.In addition, different from the silicon that uses in present electronic device and metal material, Graphene is reduced to same good stability and the electric property of keeping of nanoscale, makes the exploration single-electron device become possibility.Recently, Geim seminar utilizes the method for electron beam lithography and dry etching that same Graphene is processed into quantum dot, lead-in wire and grid, obtain manipulable graphene-based single electron field effect transistor under room temperature, solved the limited problem of operating temperature that present single electron field effect brings due to the nanoscale instability of material and structure.The Holland scientist has reported first graphene-based superconducting field-effect pipe, finds still can transmit certain electric current in the situation that charge density is zero Graphene, may be low energy consumption, and switching time, fast nanoscale superconductive electronic device brought breakthrough.
Recently the document about the device of Graphene emerges in multitude, and about Graphene, a lot of reports is being arranged aspect electric capacity, solar cell, transparency electrode.Being on the scene effect transistor FET application facet also has a lot of reports, as back of the body grid graphene field effect transistor BG-GFET, top grid graphene field effect transistor TG-GFET, double grid graphene field effect transistor DG-GFET etc.They have certain shortcoming, need the improvement in a nearly step, but this can not affect the prospect of nearly half application in Graphene being on the scene effect pipe aspect.In the preparation technology of existing GFET, Graphene need to deposit or transfer to as on Si or SiC substrate, substrate has played the effect of the back of the body grid that are similar in traditional double-gate structure, because the introducing of the top gate medium of top grid GFET can be introduced more scattering source, simultaneously, in the grid manufacturing process of top, graphene film also is easy to be damaged, and makes the mobility of top grid GFET significantly descend.
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 side grid Graphene transistor preparation method based on SiC and chlorine reaction is proposed, to improve the electron mobility of Graphene, can realize the single transistor electric current is accurately controlled by changing the side gate voltage, avoid the scattering effect of top grid graphene field effect pipe top gate medium.
For achieving the above object, preparation method of the present invention comprises the following steps:
(1) the SiC print is cleaned, to remove surface contaminant;
(2) the SiC print surface after cleaning utilizes plasma enhanced CVD PECVD method, the thick SiO of deposit one deck 0.5-1.0 μ m 2, as mask;
(3) photoetching side gate figure:
Be made into reticle according to the transistorized side grid G of side grid Graphene, source S, drain D, conducting channel position;
Be 3% acrylic resin PMMA solution in mask surface spin coating concentration, and put into baking oven, baking is 60 seconds under 180 ℃, and itself and mask are closely linked;
With electron beam, PMMA is exposed again, the figure on reticle is transferred to SiO 2On mask, and use buffered hydrofluoric acid to SiO 2Mask layer corrodes, and exposes SiC, forms the identical window of side gate transistor shape;
The print that (4) will form after window is placed in quartz ampoule, is heated to 700-1100 ℃;
(5) pass into Ar gas and Cl in quartz ampoule 2The mist of gas makes Cl 2SiC reaction 3-8min with exposed generates carbon film;
(6) the carbon film print that generates is placed in buffered hydrofluoric acid solution to remove the SiO outside window 2
(7) the thick Ni film of electron beam evaporation deposit 300-500nm on the carbon film print;
(8) will be deposited with the carbon film print of Ni film, and be placed in Ar gas, be the 10-30min that anneals under 1000-1200 ℃ in temperature, make carbon film reconstitute Graphene at the window's position, form simultaneously the transistorized side grid of side grid Graphene, source electrode, drain electrode and conducting channel;
(9) the Graphene print is placed in HCl and CuSO 4In mixed solution to remove the Ni film;
(10) the method depositing metal Pd/Au contact layer of deposited by electron beam evaporation on the Graphene print;
(11) photoetching metal electrode:
11a) according to side grid, source, leakage metal electrode position making reticle;
11b) with concentration be 7% PMMA solution spin coating metal Pd/Au contact layer on, then put into baking oven, baking is 80 seconds under 200 ℃, makes itself and metal level close contact;
11c) use electron beam exposure PMMA, the figure on reticle is transferred on metal contact layer, and use oxygen to carry out reactive ion etching RIE to metal contact layer, form side grid, source, the drain metal contact of side gate transistor;
(12) sample that uses acetone soln to soak to make took out post-drying to remove residual PMMA in 10 minutes, obtained side grid Graphene transistor.
The present invention compared with prior art has following advantage:
1. the present invention is owing to adopting side grid structure to produce the Graphene transistor, thereby can realize accurate control to the single transistor channel resistance by changing the side gate voltage, avoid the scattering effect of top grid graphene field effect pipe top gate medium.
2. the present invention is due to the Graphene of optionally having grown, and need not Graphene is carried out etching when making device on this Graphene, thereby the electron mobility in Graphene can not reduce, and guaranteed the device performance of making.
3. the present invention is owing to utilizing SiC and Cl 2Solid/liquid/gas reactions, thereby can react under lower temperature and normal pressure, and reaction rate is fast, the Graphene smooth surface of generation, and voidage is low, and thickness is easily controlled.
4. 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 that the present invention manufactures the transistorized flow chart of connecting-type side grid Graphene;
Fig. 3 is the transistorized domain schematic diagram of connecting-type side grid Graphene of the present invention;
Fig. 4 is that the present invention manufactures the transistorized flow chart of disconnected type side grid Graphene;
Fig. 5 is the transistorized domain schematic diagram of the disconnected type side of the present invention grid 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.
Also used etching system in the present invention, electron beam evaporation system, the plasma enhanced CVD PECVD of system, and the ripe microelectronic technique system such as reactive ion etching RIE.
Embodiment 1
With reference to Fig. 2, the transistorized step of making connecting-type side grid Graphene of the present invention is as follows:
Step 1: clean the 6H-SiC print, to remove surface contaminant, as Fig. 2 (a).
(1.1) the 6H-SiC substrate base is used NH 4OH+H 2O 2Reagent soaked sample 10 minutes, took out post-drying, to remove the sample surfaces organic remains;
(1.2) the 6H-SiC print that will remove after surperficial organic remains re-uses HCl+H 2O 2Reagent soaked sample 10 minutes, took out post-drying, to remove ionic contamination.
Step 2: at 6H-SiC print surface deposition one deck SiO 2, as Fig. 2 (b).
(2.1) the 6H-SiC print after 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) pass into the SiH that flow velocity is respectively 30sccm, 60sccm and 200sccm in system 4, N 2O and N 2, the duration is 30min, makes SiH 4And N 2The O reaction is at 6H-SiC print surface deposition one deck 0.5 thick SiO of μ m 2Mask layer.
Step 3: at SiO 2Carve graphical window on mask layer, as Fig. 2 (c).
(3.1) at SiO 2Mask layer spin coating concentration is 3% PMMA solution, and puts into baking oven and toast 60s under 180 ℃;
(3.2) make reticle according to the figure of side gate transistor as shown in Figure 3, with electron beam, PMMA is exposed, electron accelerating voltage is 100kV, and exposure intensity is 8000 μ C/cm 2, figure on reticle is transferred to SiO 2On mask;
(3.3) with buffered hydrofluoric acid to SiO 2Mask layer corrodes, and figure on reticle is transferred to SiO 2On mask layer, expose 6H-SiC, at the transistorized side grid of side grid Graphene, source, leakage and raceway groove position formation window.
Step 4: the print that will make window by lithography pack into quartz ampoule and exhaust heating.
The print that (4.1) will make window by lithography is put into quartz ampoule 1, and quartz ampoule is placed in 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: reaction generates carbon film, as Fig. 2 (d).
Pass into to quartz ampoule Ar gas and the Cl that flow velocity is respectively 98sccm and 2sccm 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 is placed in from quartz ampoule the buffered hydrofluoric acid solution that proportioning is 1:10, to remove the SiO outside window 2
Step 7: deposit Ni film on the carbon film print, as Fig. 2 (e).
The carbon film print is 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 8: reconstitute Graphene.
The carbon film print that deposits the Ni film is placed in the Ar gas that flow velocity is 100sccm, be to anneal 30 minutes under 1000 ℃ in temperature, make carbon film reconstitute continuous side grid structure Graphene at the window's position, form the transistorized side grid of side grid Graphene, source electrode, drain electrode and conducting channel.
Step 9: the Graphene print is placed in HCl and CuSO 4In mixed solution to remove the Ni film, as Fig. 2 (f).
Step 10: the depositing metal contact layer, as Fig. 2 (g).
(10.1) the method depositing metal Pd of deposited by electron beam evaporation on the Graphene print of removing the Ni film, thickness is 5nm;
(10.2) utilize the method depositing metal Au of electron beam evaporation on the metal Pd layer, thickness is 100nm.
Step 11: photoetching forms Metal Contact, as Fig. 2 (h).
(11.1) spin coating concentration is 7% PMMA solution on metal level, and puts into baking oven, toasts 80s under 200 ℃;
(11.2) according to side grid, source, leakage metal electrode position making reticle, use electron beam that PMMA is exposed, figure on reticle is transferred on metal contact layer;
(11.3) use oxygen to carry out reactive ion etching RIE to metal contact layer, form the transistorized side grid of side grid Graphene, source, drain metal contact.
Step 12: the sample that the immersion of use acetone soln is made took out post-drying to remove residual PMMA in 10 minutes, obtained side grid Graphene transistor.
Embodiment 2
With reference to Fig. 4, it is as follows that the present invention makes the transistorized step of disconnected type side grid Graphene:
Step 1: clean the 4H-SiC print, to remove surface contaminant, as Fig. 4 (a).
(1.1) the 4H-SiC substrate base is used NH 4OH+H 2O 2Reagent soaked sample 10 minutes, took out post-drying, to remove the sample surfaces organic remains;
(1.2) the 4H-SiC print that will remove after surperficial organic remains re-uses 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, as Fig. 4 (b).
(2.1) the 4H-SiC print after 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) pass into the SiH that flow velocity is respectively 30sccm, 60sccm and 200sccm in system 4, N 2O and N 2, the duration is 100min, makes SiH 4And N 2The O reaction is at 4H-SiC print surface deposition one deck 1.0 thick SiO of μ m 2Mask layer.
Step 3: at SiO 2Carve graphical window on mask layer, as Fig. 4 (c).
(3.1) at SiO 2Mask layer spin coating concentration is 3% PMMA solution, and puts into baking oven and toast 60s under 180 ℃;
(3.2) make reticle according to the figure of side gate transistor as shown in Figure 5, with electron beam, PMMA is exposed, electron accelerating voltage is 100kV, and dosage is 9000 μ C/cm 2, figure on reticle is transferred to SiO 2On mask layer;
(3.3) with buffered hydrofluoric acid to SiO 2Mask layer corrodes, and exposes 4H-SiC, at the transistorized side grid of side grid Graphene, source, leakage and raceway groove position formation window.
Step 4: the print that will make window by lithography pack into quartz ampoule and exhaust heating.
The print that (4.1) will make window by lithography is put into quartz ampoule 1, and quartz ampoule is placed in 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 1100 ℃.
Step 5: reaction generates carbon film, as Fig. 4 (d).
Pass into to quartz ampoule Ar gas and the Cl that flow velocity is respectively 95sccm and 5sccm 2Gas, the time is 3 minutes, makes Cl 24H-SiC reaction with exposed generates carbon film.
Step 6: remove remaining SiO 2
The carbon film print that generates is taken out and is placed in the buffered hydrofluoric acid solution of 1:10 from quartz ampoule, with the SiO outside the removal window 2
Step 7: deposit Ni film on the carbon film print, as Fig. 4 (e).
The carbon film print is 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 20min, the thick Ni film of deposition one deck 500nm on the Si print.
Step 8: reconstitute Graphene.
The carbon film print that deposits the Ni film is placed in the Ar gas that flow velocity is 25sccm, be to anneal 10 minutes under 1200 ℃ in temperature, make carbon film reconstitute continuous side grid structure Graphene at the window's position, form the transistorized side grid of side grid Graphene, source electrode, drain electrode and conducting channel.
Step 9: the Graphene print is placed in HCl and CuSO 4In mixed solution to remove the Ni film, as Fig. 4 (f).
Step 10: the depositing metal contact layer, as Fig. 4 (g).
(10.1) in the method for removing deposited by electron beam evaporation on the Graphene print of Ni film, deposition thickness is the Pd metal of 5nm;
(10.2) utilize the method for electron beam evaporation on the metal Pd layer, deposition thickness is the metal A u of 100nm.
Step 11: photoetching forms Metal Contact, as Fig. 4 (h).
(11.1) spin coating concentration is 7% PMMA solution on metal level, and puts into baking oven, toasts 80s under 200 ℃;
(11.2) according to side grid, source, leakage metal electrode position making reticle, use electron beam that PMMA is exposed, figure on reticle is transferred on metal contact layer;
(11.3) re-use oxygen metal contact layer is carried out reactive ion etching RIE, form the transistorized side grid of side grid Graphene, source, drain metal contact.
Step 12: the sample that the immersion of use acetone soln is made took out post-drying to remove residual PMMA in 10 minutes, obtained side grid Graphene transistor.
Embodiment 3
With reference to Fig. 4, the transistorized step of the disconnected type side of making of the present invention grid Graphene is as follows:
Steps A: the 6H-SiC substrate base is used NH 4OH+H 2O 2Reagent soaked sample 10 minutes, took out post-drying, to remove the sample surfaces organic remains; 6H-SiC print after the surperficial organic remains of removal is re-used HCl+H 2O 2Reagent soaked sample 10 minutes, took out post-drying, to remove ionic contamination, as Fig. 4 (a).
Step B: the 6H-SiC print after 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 ℃; Pass into the SiH that flow velocity is respectively 30sccm, 60sccm and 200sccm in system 4, N 2O and N 2, the duration is 60min, makes SiH 4And N 2The O reaction is at 6H-SiC print surface deposition one deck 0.8 thick SiO of μ m 2Mask layer is as Fig. 4 (b).
Step C: at SiO 2Mask layer spin coating concentration is 3% PMMA solution, and puts into baking oven and toast 60s under 180 ℃; Make reticle according to the figure of side gate transistor as shown in Figure 5, with electron beam, PMMA is exposed, electron accelerating voltage is 100kV, and exposure intensity is 8500 μ C/cm 2, figure on reticle is transferred on metal contact layer; With buffered hydrofluoric acid to SiO 2Mask layer corrodes, and exposes 6H-SiC, at the transistorized side grid of side grid Graphene, source, leakage and raceway groove position formation window, as Fig. 4 (c).
Step D: the print that will make window by lithography is put into quartz ampoule 1, and quartz ampoule is placed in 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 the resistance furnace mains switch, quartz ampoule is heated to 1000 ℃.
Step e: pass into Ar gas and the Cl that flow velocity is respectively 96sccm and 4sccm to quartz ampoule 2Gas, the time is 5 minutes, makes Cl 26H-SiC reaction with exposed generates carbon film, as Fig. 4 (d).
Step F: the carbon film print that generates is taken out and be placed in from quartz ampoule the buffered hydrofluoric acid solution that proportioning is 1:10, to remove the SiO outside window 2
Step G: the carbon film print is 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 15min, the thick Ni film of deposition one deck 400nm on the Si print is as Fig. 4 (e).
Step H: the carbon film print that will deposit the Ni film is placed in the Ar gas that flow velocity is 60sccm, be to anneal 20 minutes under 1100 ℃ in temperature, make carbon film reconstitute continuous side grid structure Graphene at the window's position, form the transistorized side grid of side grid Graphene, source electrode, drain electrode and conducting channel.
Step I: the Graphene print is placed in HCl and CuSO 4In mixed solution to remove the Ni film, as Fig. 4 (f).
Step J: the method deposition thickness of deposited by electron beam evaporation is the Pd metal of 5nm on the Graphene print that etches side gate transistor shape; The method deposition thickness of recycling electron beam evaporation is the metal A u of 100nm on the Pd metal level, as Fig. 4 (g).
Step K: spin coating concentration is 7% PMMA solution on metal level, and puts into baking oven, toasts 80s under 200 ℃; According to side grid, source, leakage metal electrode position making reticle, use electron beam that PMMA is exposed, the reticle figure is transferred on metal contact layer; Re-use oxygen metal contact layer is carried out reactive ion etching RIE, form the transistorized side grid of side grid Graphene, source, drain metal contact, as Fig. 4 (h).
Step L: the sample that the immersion of use acetone soln is made took out post-drying to remove residual PMMA in 10 minutes, obtained side grid Graphene transistor.

Claims (10)

1.一种基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,包括以下步骤:1. a Ni film annealing side gate graphene transistor preparation method based on SiC and chlorine reaction, comprises the following steps: (1)对SiC样片进行清洗,以去除表面污染物;(1) Clean the SiC sample to remove surface pollutants; (2)在清洗后的SiC样片表面利用等离子体增强化学气相淀积PECVD方法,淀积一层0.5-1.0μm厚的SiO2,作为掩膜;(2) Deposit a layer of SiO 2 with a thickness of 0.5-1.0 μm on the surface of the cleaned SiC sample using the plasma enhanced chemical vapor deposition PECVD method as a mask; (3)光刻侧栅图形:(3) Lithographic side gate pattern: 按照侧栅石墨烯晶体管的侧栅极G、源极S、漏极D、导电沟道位置制作成光刻版;Make a photolithographic plate according to the position of the side gate G, source S, drain D, and conductive channel of the side gate graphene transistor; 在掩膜表面旋涂浓度为3%的丙烯酸树脂PMMA溶液,并放入烘箱中,在180℃下烘烤60秒,使其与掩膜紧密结合在一起;Spin-coat an acrylic resin PMMA solution with a concentration of 3% on the surface of the mask, put it in an oven, and bake it at 180°C for 60 seconds to make it tightly bonded to the mask; 再用电子束对PMMA曝光,将光刻版上的图形转移到SiO2掩模上,并使用缓冲氢氟酸对SiO2掩膜层进行腐蚀,露出SiC,形成侧栅晶体管形状相同的窗口;Then use an electron beam to expose PMMA, transfer the pattern on the photolithography plate to the SiO 2 mask, and use buffered hydrofluoric acid to etch the SiO 2 mask layer to expose SiC and form a window with the same shape as the side gate transistor; (4)将形成窗口后的样片置于石英管中,加热至700-1100℃;(4) Place the sample with the window formed in a quartz tube and heat it to 700-1100°C; (5)向石英管中通入Ar气和Cl2气的混合气体,使Cl2与裸露的SiC反应3-8min,生成碳膜;(5) Introduce a mixed gas of Ar gas and Cl 2 gas into the quartz tube to make Cl 2 react with the exposed SiC for 3-8 minutes to form a carbon film; (6)将生成的碳膜样片置于缓冲氢氟酸溶液中以去除窗口之外的SiO2(6) Place the generated carbon film sample in buffered hydrofluoric acid solution to remove SiO 2 outside the window; (7)在碳膜样片上电子束蒸发淀积300-500nm厚的Ni膜;(7) Electron beam evaporation deposits a 300-500nm thick Ni film on the carbon film sample; (8)将淀积有Ni膜的碳膜样片,并置于Ar气中,在温度为1000-1200℃下退火10-30min,使碳膜在窗口位置重构成石墨烯,同时形成侧栅石墨烯晶体管的侧栅极、源极、漏极和导电沟道;(8) Place the carbon film sample with the Ni film deposited in Ar gas, and anneal at a temperature of 1000-1200°C for 10-30 minutes, so that the carbon film can be restructured into graphene at the window position, and at the same time form side gate graphite side gate, source, drain and conduction channel of the ene transistor; (9)将石墨烯样片置于HCl和CuSO4混合溶液中以去除Ni膜;(9) Place the graphene sample in a mixed solution of HCl and CuSO 4 to remove the Ni film; (10)在石墨烯样片上用电子束蒸发的方法淀积金属Pd/Au接触层;(10) Deposit a metal Pd/Au contact layer on the graphene sample by electron beam evaporation; (11)光刻金属电极:(11) Photolithographic metal electrodes: 11a)按照侧栅、源、漏金属电极位置制作光刻版;11a) Make a photolithography plate according to the positions of the side gate, source and drain metal electrodes; 11b)将浓度为7%的的PMMA溶液旋涂金属Pd/Au接触层上,再放入烘箱中,在200℃下烘烤80秒,使其与金属层紧密接触;11b) Spin-coat the PMMA solution with a concentration of 7% on the metal Pd/Au contact layer, then put it into an oven, and bake it at 200° C. for 80 seconds to make it closely contact with the metal layer; 11c)用电子束曝光PMMA,将光刻版上的图形转移到金属接触层上,并使用氧气对金属接触层进行反应离子刻蚀RIE,形成侧栅晶体管的侧栅、源、漏极金属接触;11c) Expose the PMMA with an electron beam, transfer the pattern on the photolithography plate to the metal contact layer, and use oxygen to perform reactive ion etching RIE on the metal contact layer to form the side gate, source and drain metal contacts of the side gate transistor ; (12)使用丙酮溶液浸泡制作好的样品10分钟以去除残留的PMMA,取出后烘干,获得侧栅石墨烯晶体管。(12) Soak the prepared sample in acetone solution for 10 minutes to remove residual PMMA, take it out and dry it to obtain a side-gate graphene transistor. 2.根据权利要求1所述的基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,其特征在于所述步骤(1)对SiC样片进行清洗,是先使用NH4OH+H2O2试剂浸泡SiC样片10分钟,取出后烘干,以去除样片表面有机残余物;再使用HCl+H2O2试剂浸泡样片10分钟,取出后烘干,以去除离子污染物。2. The method for preparing Ni film annealed side-gate graphene transistor based on the reaction of SiC and chlorine gas according to claim 1, characterized in that the step (1) to clean the SiC sample is first using NH 4 OH+H 2 Soak the SiC sample with O 2 reagent for 10 minutes, take it out and dry it to remove the organic residue on the surface of the sample; then use HCl+H 2 O 2 reagent to soak the sample for 10 minutes, take it out and dry it to remove ionic pollutants. 3.根据权利要求1所述的基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,其特征在于所述步骤(2)中利用PECVD淀积SiO2,其工艺条件为:3. The method for preparing Ni film annealed side-gate graphene transistor based on the reaction of SiC and chlorine gas according to claim 1, characterized in that in the step (2), SiO 2 is deposited by PECVD, and the process conditions are: SiH4流速为30sccm,N2O流速为60sccm,N2流速为200sccm,SiH 4 flow rate is 30 sccm, N 2 O flow rate is 60 sccm, N 2 flow rate is 200 sccm, 腔内压力为3.0Pa,The pressure in the cavity is 3.0Pa, 射频功率为100W,RF power is 100W, 淀积温度为150℃,The deposition temperature is 150°C, 淀积时间为30-100min。The deposition time is 30-100min. 4.根据权利要求1所述的基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,其特征在于所述步骤(3)中电子束对PMMA曝光,其工艺条件为:4. the Ni film annealing side gate graphene transistor preparation method based on SiC and chlorine reaction according to claim 1 is characterized in that electron beam is exposed to PMMA in described step (3), and its processing condition is: 电子加速电压:100kV,Electron acceleration voltage: 100kV, 曝光强度为:8000-9000μC/cm2Exposure intensity: 8000-9000μC/cm 2 . 5.根据权利要求1所述的基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,其特征在于所述步骤(5)中通入的Ar气和Cl2气,其流速分别为95-98sccm和5-2sccm。5. The Ni film annealing side-gate graphene transistor preparation method based on the reaction of SiC and chlorine gas according to claim 1, characterized in that the Ar gas and Cl gas introduced in the step (5) have a flow rate of 95-98sccm and 5-2sccm. 6.根据权利要求1所述的基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,其特征在于所述步骤(7)中电子束淀积,按如下工艺条件进行:6. the Ni film annealing side-gate graphene transistor preparation method based on SiC and chlorine reaction according to claim 1 is characterized in that electron beam deposition in the described step (7) is carried out according to the following process conditions: 基底到靶材的距离为50cm,The distance from substrate to target is 50cm, 反应室压强为5×10-4Pa,The reaction chamber pressure is 5×10 -4 Pa, 束流为40mA,The beam current is 40mA, 蒸发时间为10-20min。Evaporation time is 10-20min. 7.根据权利要求1所述的基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,其特征在于所述步骤(8)退火时Ar气的流速为25-100sccm。7. The method for preparing Ni film annealed side-gate graphene transistor based on the reaction of SiC and chlorine gas according to claim 1, characterized in that the flow rate of Ar gas during the annealing in the step (8) is 25-100 sccm. 8.根据权利要求1所述的基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,其特征在于所述步骤(10)电子束蒸发法淀积金属Pd/Au层,其Pd层的厚度为5nm,Au层的厚度为100nm。8. The Ni film annealing side-gate graphene transistor preparation method based on the reaction of SiC and chlorine gas according to claim 1, characterized in that the step (10) deposits a metal Pd/Au layer by electron beam evaporation, and the Pd layer The thickness of the Au layer is 5 nm, and the thickness of the Au layer is 100 nm. 9.根据权利要求1所述的基于Ni膜退火的SiC衬底上侧栅结构石墨烯晶体管制备方法,其特征在于步骤(11)中RIE刻蚀金属接触层,其工艺条件为:9. The method for preparing graphene transistors with side gate structures on SiC substrates based on Ni film annealing according to claim 1, characterized in that in step (11), RIE etches the metal contact layer, and the process conditions are: 功率为100W,The power is 100W, 氧气流量为20sccm,Oxygen flow rate is 20sccm, 刻蚀时间为60s。The etching time is 60s. 10.根据权利要求1所述的基于SiC与氯气反应的Ni膜退火侧栅石墨烯晶体管制备方法,其特征在于所述SiC样片的晶型采用4H-SiC或6H-SiC。10. The Ni film annealing side-gate graphene transistor preparation method based on the reaction of SiC and chlorine gas according to claim 1, characterized in that the crystal form of the SiC sample adopts 4H-SiC or 6H-SiC.
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Application publication date: 20130515