CN102936009A - Method for manufacturing low layer number graphene film on silicon carbide substrate - Google Patents
Method for manufacturing low layer number graphene film on silicon carbide substrate Download PDFInfo
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- CN102936009A CN102936009A CN2012103836660A CN201210383666A CN102936009A CN 102936009 A CN102936009 A CN 102936009A CN 2012103836660 A CN2012103836660 A CN 2012103836660A CN 201210383666 A CN201210383666 A CN 201210383666A CN 102936009 A CN102936009 A CN 102936009A
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Abstract
The present invention relates to a method for manufacturing a low layer number graphene film on a silicon carbide substrate. The method comprises the following process steps: 1) selecting a silicon surface silicon carbide substrate, and placing on a graphite base having a tantalum carbide coating; 2) carrying out system heating; 3) reducing a reaction chamber temperature to less than 1200 DEG C; 4) increasing argon flow; 5) carrying out system heating; 6) reducing argon flow, and reducing reaction chamber pressure to 0-1 mbar; 7) continuously adopting a mechanical pump to control a reaction chamber vacuum degree; 8) adopting a molecular pump to control the reaction chamber vacuum degree, and starting a carbonization process; 9) closing heating, and introducing argon; 10) reducing the reaction chamber temperature to 1000 DEG C, and closing argon; and 11) reducing the reaction chamber temperature, introducing argon to the reaction chamber to achieve atmospheric pressure, opening the chamber, and taking the sheet. The method has the following advantages that: graphene film formation can be promoted, sublimation of silicon atoms in the SiC substrate during heating and cooling processes can be effectively inhibited, and the carbonization process is easily controlled so as to achieve low layer number graphene film preparation.
Description
Technical field
What the present invention proposed is a kind of method of making low number of plies graphene film in silicon carbide substrates, low by the graphene film number of plies of the method preparation, and good reproducibility, stablizes controlled.Belong to technical field of semiconductor.
Background technology
Graphene is the monoatomic layer graphite crystal film that Geim seminar of Univ Manchester UK found in 2004, it is the bi-dimensional cellular shape material that the carbon atom by sp2 hydridization consists of, it is the elementary cell that makes up other dimension carbon material, can wrap up the soccerballene that forms zero dimension, roll the carbon nanotube that forms one dimension, pile up layer by layer the graphite that forms three-dimensional.Graphene C-C bond distance is about 0.142nm, and perfectly Graphene is two-dimentional, includes only hexagonal cellular (isogonism hexagon), is the human two dimensional crystal of finding first.
Graphene film has many excellent specific properties, for example: under the room temperature up to 200000 cm
2The intrinsic electronic mobility of/Vs (silicon 140 times); The mean free path of micron order electronics; Current density (108A/cm than high two orders of magnitude of copper
2); Good thermal conductivity [5000W/ (mK)], (adamantine 5 times); Specific surface area (the 2630m of high strength (1060GPa) and super large
2/ g).
Electronics can not be scattered in Graphene and transmits, and is less with the transistor size of its preparation, speed is faster, and energy consumption is lower.Simultaneously graphene device technique also with traditional CMOS process compatible, can utilize the planar light lithography to prepare graphene device and circuit, Graphene is the first-selection of the update of device critical material.The achievement in research of scholarly forecast Graphene will produce to the innovation and development of high-end military systems surging force difficult to the appraisal, comprise supercomputer, the accurate imaging system of millimeter wave, millimeter wave ultra-wideband communication system, radar and electronic warfare system etc.At present, the working speed of silicon device can reach the GHz scope, and the operating frequency of graphene device can reach THz.If can further develop, its meaning is self-evident.
The at present preparation of grapheme material mainly contains following several: mechanically peel method, SiC thermal decomposition method, CVD (Chemical Vapor Deposition) method, molecular beam epitaxy and chemical dispersion method.The SiC thermal decomposition method is more suitable in other graphene film preparation of wafer level.The reasons are as follows: at first from the angle of element manufacturing, can directly prepare graphene/carbon SiClx structure by the SiC thermal decomposition method, need not to add the operation that graphene film shifts to device substrate, simplification of flowsheet, reduce the course of processing to the disadvantageous effect of film performance, therefore can provide more believable quality and interface, thereby have good producibility and repeatability.
The performance of graphene film and the number of plies have very large relation.The SiC thermal decomposition method makes the carbonization of SiC substrate by the Siliciumatom in the distillation SiC substrate, and carbon atom remaining after the Siliciumatom distillation forms Graphene in substrate surface absorption nucleation.Different with epitaxy, the SiC thermal decomposition method can't pass into by adjusting time and the control of the flow realization graphene film number of plies in source.How to control effective carbonization time of SiC substrate, how to suppress to reach before the carbonization temperature and finish in the carbonization technique temperature-fall period that the distillation of Siliciumatom is the key issue that realizes that the preparation of low number of plies graphene film need to solve in the SiC substrate.
Summary of the invention
What the present invention proposed is a kind of method of making low number of plies graphene film in silicon carbide substrates, and its purpose is intended to control effective carbonization time that the SiC thermal decomposition method prepares graphene film, realizes the preparation of low number of plies graphene film.The present invention reduces reaction chamber temperature after the SiC substrate is finished the hydrogen etching, pass into hydrogen remaining in the argon replaces reaction chamber to reaction chamber, and improves chamber pressure, suppresses the distillation of Siliciumatom in the SiC substrate in the temperature-rise period.Finish carbonization technique, in the temperature-fall period, passing into equally argon gas and improve chamber pressure, suppressing the distillation of Siliciumatom in the SiC substrate in the temperature-fall period.
Technical solution of the present invention, the method comprise following processing step:
One, chooses silicon face silicon carbide substrates (1), substrate is placed on the graphite base of tantalum carbide coating;
Two, system is warming up to 1570 ℃, it is 100mbar that chamber pressure is set, and online substrate surface is processed under hydrogen flowing quantity 80L/min, argon flow amount 3L/min atmosphere, removes the damage on surface, and forming little step at substrate surface, the treatment time needs 30 minutes approximately;
Three, reduce reaction chamber temperature to 1200 ℃, and hydrogen flowing quantity is reduced to 0L/min by gradual mode from 80L/min, argon flow amount keeps 3L/min constant, and it is 100mbar that chamber pressure is set, and the treatment time needs 20 minutes approximately;
Four, argon flow amount is increased to 15L/min by gradual mode from 3L/min, the treatment time needs 5 minutes approximately, and chamber pressure is climbed gradually to more than the 200mbar;
Five, system is warming up to 1580 ~ 1650 ℃ of carbonization temperatures, and it is 200mbar that chamber pressure is set, argon flow amount 15L/min;
Six, reduce argon flow amount to 0L/min by gradual method, chamber pressure is reduced to 0 ~ 1mbar, and the treatment time needs 10 minutes approximately;
Seven, continue to adopt mechanical pump control reaction chamber vacuum tightness, the treatment time needs 15 minutes approximately;
Eight, close mechanical pump, adopt molecular pump control reaction chamber vacuum tightness, reaction chamber vacuum tightness 10
-4~ 10
-1Mbar, the beginning carbonization technique, the treatment time needs 15 ~ 60 minutes approximately;
Seven, close heating, pass into argon gas to reaction chamber, argon flow amount is gradual to 10L/min by 0L/min, and chamber pressure is gradual to 200mbar by 0mbar, and the treatment time needs 5 minutes approximately;
Eight, reaction chamber temperature is reduced to after 1000 ℃, closes the argon gas input;
Nine, reaction chamber temperature is reduced to after the room temperature, passes into argon gas to normal atmosphere to reaction chamber, begins to speak to get sheet.
Advantage of the present invention: finish after the hydrogen etching technics, pass into the hydrogen in the argon replaces reaction chamber, can effectively reduce the amount of remaining hydrogen in the reaction chamber, the hydrogen that adsorbs when avoiding high temperature discharges the carbon atom that causes producing after the Siliciumatom distillation and forms gaseous hydrocarbon but not Graphene.In addition heat up and temperature-fall period in, by argon atmospher in conjunction with the method that improves chamber pressure, can establishment heat up and temperature-fall period in the distillation of Siliciumatom, thereby the effective carbonization time of realization SiC substrate is stablized controlled.
Description of drawings
Reaction chamber vacuum tightness synoptic diagram over time in accompanying drawing 1 carbonization process has preferably repeatability.
The Raman collection of illustrative plates of single-layer graphene on the SiC substrate of accompanying drawing 2 employing present method preparations, the 2D peak of Graphene can be by the peak match of single Lorentz, halfwidth 36cm
-1
The Raman collection of illustrative plates of double-layer graphite alkene on the SiC substrate of accompanying drawing 3 employing present method preparations, the 2D peak of Graphene can be by 4 Lorentz peak matches.
Embodiment
Embodiment
The method at the low number of plies graphene film of positive crystal orientation (0001) silicon face high-purity semi-insulating silicon carbide substrate growth that provides may further comprise the steps:
1) chooses positive crystal orientation (0001) silicon face high-purity semi-insulating silicon carbide substrate, substrate is placed on the graphite base of tantalum carbide coating;
2) system is warming up to 1570 ℃, it is 100mbar that chamber pressure is set, and online substrate surface is processed under hydrogen flowing quantity 80L/min, argon flow amount 3L/min atmosphere, removes the damage on surface, and forming little step at substrate surface, the treatment time is 30 minutes;
3) reduce reaction chamber temperature to 1200 ℃, and hydrogen flowing quantity is reduced to 0L/min gradually from 80L/min, argon flow amount keeps 3L/min constant, and it is 100mbar that chamber pressure is set, and the treatment time is 20 minutes;
4) argon flow amount is increased to 15L/min gradually from 3L/min, chamber pressure is increased to 200mbar gradually by 100mbar, and the treatment time is 5 minutes;
5) system is warming up to 1600 ℃, and chamber pressure is set 200mbar, argon flow amount 15L/min, and the heating-up time is 30 minutes;
6) argon flow amount is reduced to 0L/min gradually by 15 L/min, chamber pressure is reduced to 0 ~ 1mbar, and the treatment time is 10 minutes;
7) continue to adopt mechanical pump control reaction chamber vacuum tightness, 15 minutes treatment times;
8) close mechanical pump, open molecular pump control reaction chamber vacuum tightness, beginning carbonization technique, reaction chamber vacuum tightness 10
-4~ 10
-1Mbar, 30 minutes treatment times;
9) close heating, pass into argon gas to reaction chamber, argon flow amount is enlarged to 10L/min gradually by 0L/min, and chamber pressure is increased to 200mbar gradually by 0mbar, and the treatment time is 5 minutes;
10) reaction chamber temperature is reduced to after 1000 ℃, closes the argon gas input;
11) reaction chamber temperature is reduced to after the room temperature, passes into argon gas to normal atmosphere to reaction chamber, begins to speak to get sheet.
Adopt Raman spectrometer that the graphene film of preparation is characterized.By can judge the number of plies of Graphene to the match at Graphene 2D peak.Can judge simultaneously the crystal mass of Graphene in conjunction with the contrast of Graphene D peak intensity and G peak intensity.
Present method can effectively prepare high quality low layer graphene film.Pass into the hydrogen in the argon replaces reaction chamber, can effectively reduce the amount of remaining hydrogen in the reaction chamber, by argon atmospher in conjunction with the method that improves chamber pressure, can establishment heat up and temperature-fall period in the distillation of Siliciumatom, thereby realize that effective carbonization time stablizes controlled.Process repeatability and high conformity are fit to scale production.
Claims (3)
1. method of making low number of plies graphene film in silicon carbide substrates is characterized in that the method comprises following processing step:
One, chooses silicon face silicon carbide substrates (1), the silicon face silicon carbide substrates is placed on the graphite base of tantalum carbide coating;
Two, system is warming up to 1570 ℃, it is 100mbar that chamber pressure is set, under hydrogen flowing quantity 80L/min, argon flow amount 3L/min atmosphere, online silicon face silicon carbide substrates surface is processed, remove the damage on surface, and form little step on silicon face silicon carbide substrates surface;
Three, reduce below the reaction chamber temperature to 1200 ℃, and hydrogen flowing quantity is reduced to 0L/min by gradual mode from 80L/min, argon flow amount keeps 3L/min constant, and it is 100mbar that chamber pressure is set;
Four, argon flow amount is increased to 15L/min by gradual mode from 3L/min, adopts mechanical pump control reaction chamber vacuum tightness, chamber pressure is climbed gradually to more than the 200mbar;
Five, system is warming up to 1580 ~ 1650 ℃ of carbonization temperatures, and argon flow amount 15L/min is set more than the chamber pressure 200mbar;
Six, reduce argon flow amount to 0L/min by gradual method;
Seven, continue to adopt mechanical pump control reaction chamber 0 ~ 1mbar;
Eight, close mechanical pump, adopt molecular pump control reaction chamber vacuum tightness, chamber pressure 10
-4~ 10
-1Mbar, beginning carbonization technique, 15 ~ 60 minutes time;
Seven, close heating, pass into argon gas to reaction chamber, argon flow amount is gradual to 10L/min by 0L/min, and chamber pressure is gradual to more than the 200mbar by 0mbar;
Eight, reaction chamber temperature is reduced to after 1000 ℃, closes the argon gas input;
Nine, reaction chamber temperature is reduced to after the room temperature, passes into argon gas to normal atmosphere to reaction chamber, begins to speak to get sheet.
2. a kind of method of making low number of plies graphene film in silicon carbide substrates as claimed in claim 1 is characterized in that described silicon face silicon carbide substrates (1) is selected from the many types of silicon carbide of 4H, 6H.
3. a kind of method of making low number of plies graphene film in silicon carbide substrates as claimed in claim 1 is characterized in that under greater than the 200mbar argon atmospher growth temperature by being promoted to carbonization temperature below 1200 ℃.
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| CN104409594A (en) * | 2014-11-20 | 2015-03-11 | 北京中科天顺信息技术有限公司 | SiC substrate-based nitride LED (Light Emitting Diode) film flip chip and preparation method thereof |
| CN104477903A (en) * | 2014-12-22 | 2015-04-01 | 上海集成电路研发中心有限公司 | Preparation method of graphene film |
| CN104947184A (en) * | 2015-06-04 | 2015-09-30 | 山东大学 | Method for growing grapheme on epitaxy of large-diameter 4H/6H-SiC silicon surface substrate based on in-situ Si atmosphere action |
| CN105951179A (en) * | 2016-04-28 | 2016-09-21 | 山东大学 | Method for selectable single-side growth of graphene on SiC substrate |
| CN106521618A (en) * | 2016-11-07 | 2017-03-22 | 山东大学 | Method for located growing of big single crystal graphene on SiC substrate through point-seed way |
| CN106835268A (en) * | 2017-01-17 | 2017-06-13 | 苏州瑞而美光电科技有限公司 | A kind of preparation method of group III-nitride substrate |
| CN106856164A (en) * | 2016-12-29 | 2017-06-16 | 苏州纳维科技有限公司 | Adopt patterned substrate and preparation method thereof outward |
| CN107344868A (en) * | 2016-05-06 | 2017-11-14 | 山东大学 | A kind of method for the single-layer graphene for preparing no cushion on sic substrates |
| CN107954418A (en) * | 2017-12-29 | 2018-04-24 | 北京华进创威电子有限公司 | A kind of multi-disc carborundum pyrolytic graphite alkene preparation method |
| CN108046246A (en) * | 2017-12-22 | 2018-05-18 | 中国电子科技集团公司第五十五研究所 | A kind of graphene film growing method of process gas auxiliary |
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| CN104409594A (en) * | 2014-11-20 | 2015-03-11 | 北京中科天顺信息技术有限公司 | SiC substrate-based nitride LED (Light Emitting Diode) film flip chip and preparation method thereof |
| CN104477903A (en) * | 2014-12-22 | 2015-04-01 | 上海集成电路研发中心有限公司 | Preparation method of graphene film |
| CN104947184A (en) * | 2015-06-04 | 2015-09-30 | 山东大学 | Method for growing grapheme on epitaxy of large-diameter 4H/6H-SiC silicon surface substrate based on in-situ Si atmosphere action |
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| CN106521618B (en) * | 2016-11-07 | 2018-10-26 | 山东大学 | A method of passing through a seed crystal located growth large-size monocrystal graphene on sic substrates |
| CN106856164A (en) * | 2016-12-29 | 2017-06-16 | 苏州纳维科技有限公司 | Adopt patterned substrate and preparation method thereof outward |
| CN106835268A (en) * | 2017-01-17 | 2017-06-13 | 苏州瑞而美光电科技有限公司 | A kind of preparation method of group III-nitride substrate |
| CN108046246A (en) * | 2017-12-22 | 2018-05-18 | 中国电子科技集团公司第五十五研究所 | A kind of graphene film growing method of process gas auxiliary |
| CN108046247A (en) * | 2017-12-25 | 2018-05-18 | 中国电子科技集团公司第五十五研究所 | The method for improving carborundum pyrolytic graphite alkene thin layer number uniformity |
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| CN109411552A (en) * | 2018-10-11 | 2019-03-01 | 苏州大学 | A kind of miniature flexible ultraviolet detector and preparation method thereof based on gallium nitride film |
| CN111410191A (en) * | 2020-05-07 | 2020-07-14 | 山东华达新材料有限公司 | Graphene semiconductor preparation device and method |
| CN113735627A (en) * | 2021-09-06 | 2021-12-03 | 杭州幄肯新材料科技有限公司 | Graphite thermal field material with tantalum carbide coating coated on surface and preparation method thereof |
| CN114314569A (en) * | 2022-01-10 | 2022-04-12 | 厦门大学 | Method for forming graphene on substrate |
| CN114314569B (en) * | 2022-01-10 | 2024-01-09 | 厦门大学 | Method for forming graphene on substrate |
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