CN105140102A - Improved method for epitaxial growth of [Beta]-silicon carbide film on silicon substrate - Google Patents
Improved method for epitaxial growth of [Beta]-silicon carbide film on silicon substrate Download PDFInfo
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- CN105140102A CN105140102A CN201510398440.1A CN201510398440A CN105140102A CN 105140102 A CN105140102 A CN 105140102A CN 201510398440 A CN201510398440 A CN 201510398440A CN 105140102 A CN105140102 A CN 105140102A
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- H—ELECTRICITY
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Abstract
The invention relates to an improved method for epitaxial growth of a [Beta]-silicon carbide film on a silicon substrate. According to the invention, a very low carbonization pressure is applied to large-flow propane so as to form a high-quality silicon carbide buffer layer in a carbonization manner; then a large-flow hydrogen atmosphere is maintained, and a layer of thin [Beta]-silicon carbide film is grown at a relatively low speed; then an etching process is added so as to reduce defects and improve the crystal quality; and finally a high-quality [Beta]-silicon carbide film is obtained by growth at a relatively high speed. In the epitaxial process, pure silane and pure propane serve as growth sources, and hydrogen serves as carrying gas. The flows of the epitaxial silicon carbide growth sources and the epitaxial growth time are set according to the structure of an epitaxial layer, and when the epitaxial layer is relatively thick, a short etching process is added into the high-speed growth process. By adopting the method, the high-quality [Beta]-silicon carbide film is obtained; in addition, the method is simple and easy, the cost is low, and the application value is high.
Description
Technical field
What the present invention relates to is a kind of method of the high-quality of epitaxial growth on a silicon substrate beta-silicon carbide thin film of optimization, belongs to technical field of semiconductor.
Background technology
Carborundum (SiC) is as third generation semi-conducting material, there is unique physical property and electric property compared with silicon, there is the strong and good chemical stability of large, the high electronics saturation drift velocity of breakdown field strength, high electron mobility, high heat conductance, high-melting-point, capability of resistance to radiation, thus have very wide application prospect making to be operated on high temperature, high pressure, electronic device at a high speed, under the extreme condition such as high frequency and intense radiation.Relative to other SiC crystal formation of homoepitaxy, silicon B-carbide (3C-SiC) has relatively high electron mobility, high saturated electron drift velocity, because it can at silicon (Si) Epitaxial growth, thus possesses the advantage making broad area device, and low cost compatible with ripe Si device technology.In addition, the SiC of heteroepitaxy also can be used as the resilient coating of growing gallium nitride, Graphene other relevant new material relevant with other on a si substrate.So the heteroepitaxy of 3C-SiC causes the extensive concern of people on Si substrate.But owing to there is the problem because of thermal coefficient of expansion between substrate and epitaxial loayer and lattice constant mismatch in heteroepitaxy process, cause in epitaxial film and there is huge misfit dislocation and stress, the crystal mass of the 3C-SiC film of heteroepitaxy is on a si substrate declined.Therefore, preparing high-quality 3C-SiC film is on a si substrate the key realizing the practical application of Si base SiC device.
At present, in order to obtain making the high-quality 3C-SiC epitaxial film needed for silicon carbide device, conventional process is that carbonization forms silicon carbide buffer layer then epitaxial growth again.Namely usual by passing into carbon source by Si substrate silicon carbide before epitaxial growth 3C-SiC film, generate the SiC resilient coating that one deck is very thin, then at this resilient coating basis Epitaxial growth 3C-SiC film.However, make extension subsequently not be perfect homoepitaxy owing to being obtained resilient coating quality problems by carbonization, the 3C-SiC film crystal quality obtained still can not meet the requirement of the practical application of Si base SiC device.In addition, the method for existing document and patent report mainly for aspects such as scrap build, complicated pre-treatment and Conventional process parameters optimizations, the problem such as mostly there is complex process, not good or cost is higher compared with thick epitaxial layer crystal mass.First this method adopts low-down carbonization pressure to pass into propane (C
3h
8) carbonization forms high-quality silicon carbide buffer layer.Hydrogen (the H that one large is kept when growing
2) flow atmosphere, first thin with the silicon B-carbide growing one deck thin compared with low rate on above-mentioned high-quality resilient coating, add an etching process afterwards to reduce defect and to improve crystal mass, obtain high-quality beta-silicon carbide thin film with two-forty growth subsequently.This preparation method is simple for process, with low cost, has major application and is worth.
Summary of the invention
The present invention is directed to the problem being difficult to heteroepitaxy high-quality beta-silicon carbide thin film on a silicon substrate because larger lattice mismatch and thermal mismatching cause, propose a kind of simple epitaxy method of the technique preparing beta-silicon carbide thin film on a silicon substrate based on chemical vapor deposition (CVD) equipment, its object is intended to the crystal mass effectively being improved epitaxial film by process optimization.The present invention by passing into large discharge propane (C under low-down carbonization pressure
3h
8) carbonization formed high-quality silicon carbide buffer layer and grow time keep a large discharge hydrogen (H
2) atmosphere, obtain high-quality silicon carbide buffer layer in conjunction with original position etching, and to make in epitaxial process subsequently without secondary nucleation, be entirely step flow mode and grow, effectively improve the crystal mass of epitaxial film.In addition, by bradyauxesis resilient coating, etching and high-speed rapid growth epitaxial loayer
Processing step, further increase film crystal quality.
Technical solution of the present invention, comprises following processing step:
(1) substrate prepares: choose Si substrate, and it is stand-by to carry out standard cleaning to it;
(2) pre-treatment is grown: use hydrogen (H
2) original position etching the preliminary treatment of growth front surface is carried out to substrate, H
2flow be 60 ~ 90L/min, chamber pressure is 80 ~ 200mbar, and temperature is 900 ~ 1100 DEG C, and the processing time is 5 ~ 15min;
(3) carbonisation: start when temperature rises to 1100 ~ 1250 DEG C to pass into 40 ~ 80ml/min propane (C
3h
8), chamber pressure is 50 ~ 80mbar, and start carbonization, carbonization time is 2 ~ 10min;
(4) first time growth: start growing silicon carbide film when temperature rises to 1250 ~ 1350 DEG C, growth source is silane (SiH
4) and C
3h
8, flow is respectively 5 ~ 10ml/min and 5 ~ 10ml/min, carrier gas H
2flow be 90 ~ 150L/min, growth pressure is 80 ~ 200mbar, and growth time is 5 ~ 30min;
(5) original position etching: use H
2to first time, the epitaxial wafer of growth carries out surface in situ etching, H
2flow be 90 ~ 150L/min, chamber pressure is 80 ~ 200mbar, and etching temperature is growth temperature, and etch period is 5 ~ 20min;
(6) second time growth: keep growth temperature and pressure constant, improve growth source SiH
4and C
3h
8flow respectively to 15 ~ 50ml/min and 15 ~ 50ml/min, start high speed epi-taxial silicon carbide silicon thin film, growth time is determined by epitaxy layer thickness.
Advantage of the present invention: be a kind of new method preparing beta-silicon carbide thin film on cheap and widely used Si substrate, by passing into propane (C under low-down carbonization pressure
3h
8) carbonization forms high-quality silicon carbide buffer layer, improves crystal mass by large flow hydrogen atmosphere during growth simultaneously.In addition, improve crystal mass further by the technical process of bradyauxesis resilient coating, etching and high-speed rapid growth epitaxial loayer, finally successfully prepare high-quality 3C-SiC film on a si substrate.Method is with low cost and simple, and epitaxy technique is repeated and consistency is good, and epitaxial film quality is high.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction spectrogram of 5 μm of thick beta-silicon carbide thin films prepared by the present invention.
Fig. 2 is the X ray swing curve spectrogram of 5 μm of thick beta-silicon carbide thin films prepared by the present invention.
Embodiment
Embodiment 1, embodiment 2, embodiment 3;
A method for the high-quality of the epitaxial growth on a silicon substrate beta-silicon carbide thin film of optimization, comprises following processing step:
(1) substrate prepares: choose Si substrate, and it is stand-by to carry out standard cleaning to it;
(2) pre-treatment is grown: use hydrogen H
2original position etching carries out the preliminary treatment of growth front surface to substrate, H
2flow be respectively 60/min, 75L/min, 90L/min; Chamber pressure is respectively 80mbar, 100mbar, 200mbar; Temperature for being respectively 900 DEG C, 1000 DEG C, 1100 DEG C; Processing time is respectively 5min, 10min, 15min;
(3) carbonisation: when temperature rises to 1100 DEG C, when 1200 DEG C, starts when 1250 DEG C to pass into 40ml/min propane C
3h
8, 70ml/min propane C
3h
8, 100ml/min propane C
3h
8; Chamber pressure is 50mbar, 65mbar, 80mbar; Start carbonization, carbonization time is 2min, 6min, 10min;
(4) first time growth: start growing silicon carbide film when temperature rises to 1250 DEG C, start growing silicon carbide film when 1300 DEG C, start growing silicon carbide film when 1350 DEG C, growth source is silane SiH
4and C
3h
8, wherein silane SiH
4flow is 5ml/min, 7ml/min, 10ml/min; C
3h
8flow is 5ml/min, 7ml/min, 10ml/min; Carrier gas H
2flow be 90L/min, 120L/min, 150L/min; Growth pressure is 80mbar, 140mbar, 200mbar; Growth time is 5min, 18min, 30min;
(5) original position etching: use H
2to first time, the epitaxial wafer of growth carries out surface in situ etching, H
2flow be 90L/min, 120L/min, 150L/min; Chamber pressure is 80mbar, 140mbar, 200mbar; Etching temperature is growth temperature, and etch period is 5min, 14min, 20min;
(6) second time growth: keep growth temperature and pressure constant, improve growth source SiH
4and C
3h
8flow, wherein SiH
4flow is to 15ml/min, 34ml/min, 50ml/min; C
3h
8flow is to 15ml/min, 34ml/min, 50ml/min; Start epi-taxial silicon carbide silicon thin film, growth time is determined by epitaxy layer thickness.
Described Si substrate including but not limited to Si (100) and Si (111) crystal orientation substrate, and comprises the P type of 2 ~ 8 inch dimension, N-type and high resistant Si substrate.
Described growth pre-treatment is to remove substrate surface oxide layer and contamination, and its hydrogen flowing quantity should guarantee to remove oxide layer can not cross process again.
Described carbonisation by passing into the large discharge C of 40 ~ 100ml/min under low carbonization pressure
3h
8obtain high-quality silicon carbide buffer layer.
Realize improving crystal mass further by passing into large discharge hydrogen in described first time growth and second time growth course.
Described first time epitaxial growth is by being respectively the low discharge SiH of 5 ~ 10ml/min
4and C
3h
8flow and high-carbon silicon ratio, realize low speed high quality epitaxial growth, forms the high-quality silicon B-carbide resilient coating that one deck 0.1 ~ 0.6 μm is thick.
Original position etching after described first time epitaxial growth, can reduce blemish, improves subsequent epitaxial layer crystal weight.
Described second time growth is by improving SiH
4and C
3h
8flow and the comparatively low carbon silicon ratio of first time extension, aforementioned resilient coating realizes the high-speed high-quality amount epitaxial growth of 5 ~ 25 μm/h, growth temperature and pressure with first time growth phase with, controllable precise within the scope of thickness 1 ~ 50 μm can be realized according to extension needs.
The carbon silicon ratio used in described first time growth and for the second time growth course is respectively 3:1 ~ 6:1 and 2:1 ~ 4:1.
With the beta-silicon carbide thin film that the method obtains, optical microphotograph Microscopic observation is known, this epitaxial film surfacing light.Test analysis is carried out to the sample that the embodiment of the present invention obtains.Fig. 1 is the x ray diffraction spectrogram of 5 μm of thick beta-silicon carbide thin films prepared by the present invention, XRD test shows now epitaxial film and only there is 3C-SiC (111) peak, there is not other SiC peak, illustrate that the beta-silicon carbide thin film obtained is preferred orientation polycrystal film or monocrystal thin films.Fig. 2 is the X ray swing curve spectrogram of 5 μm of thick beta-silicon carbide thin films prepared by the present invention, and its XRD half-peak breadth is 0.44 °, and the beta-silicon carbide thin film crystal mass that explanation the method obtains is very high.The above results shows that the present invention can prepare high-quality beta-silicon carbide thin film in CVD equipment.And the present invention is simple, the epitaxy technique related to is repeated and consistency is good, is applicable to large-scale production.
Above example of making is general embodiment of the present invention, and in manufacture method, actual adoptable production program is a lot, and all equalizations done according to claim of the present invention change and decoration, all belong to covering scope of the present invention.
Claims (8)
1. a method for the beta-silicon carbide thin film of epitaxial growth on a silicon substrate optimized, is characterized in that the method comprises following processing step:
(1) substrate prepares: choose Si substrate, and it is stand-by to carry out standard cleaning to it;
(2) pre-treatment is grown: use hydrogen H
2original position etching carries out the preliminary treatment of growth front surface to substrate, H
2flow be 60 ~ 90L/min, chamber pressure is 80 ~ 200mbar, and temperature is 900 ~ 1100 DEG C, and the processing time is 5 ~ 15min;
(3) carbonisation: start when temperature rises to 1100 ~ 1250 DEG C to pass into 40 ~ 100ml/min propane C
3h
8, chamber pressure is 50 ~ 80mbar, and start carbonization, carbonization time is 2 ~ 10min;
(4) first time growth: start growing silicon carbide film when temperature rises to 1250 ~ 1350 DEG C, growth source is silane SiH
4and C
3h
8, wherein silane SiH
4flow is 5 ~ 10ml/min, C
3h
8flow is 5 ~ 10ml/min, carrier gas H
2flow be 90 ~ 150L/min, growth pressure is 80 ~ 200mbar, and growth time is 5 ~ 30min;
(5) original position etching: use H
2to first time, the epitaxial wafer of growth carries out surface in situ etching, H
2flow be 90 ~ 150L/min, chamber pressure is 80 ~ 200mbar, and etching temperature is growth temperature, and etch period is 5 ~ 20min;
(6) second time growth: keep growth temperature and pressure constant, improve growth source SiH
4and C
3h
8flow, wherein SiH
4flow to 15 ~ 50ml/min, C
3h
8flow to 15 ~ 50ml/min, start epi-taxial silicon carbide silicon thin film, growth time is determined by epitaxy layer thickness.
2. the method for the beta-silicon carbide thin film of epitaxial growth on a silicon substrate of a kind of optimization according to claim 1, it is characterized in that described Si substrate is including but not limited to Si (100) and Si (111) crystal orientation substrate, and comprise P type, N-type and the high resistant Si substrate of 2 ~ 8 inches.
3. the method for the beta-silicon carbide thin film of epitaxial growth on a silicon substrate of a kind of optimization according to claim 1, it is characterized in that described growth pre-treatment is to remove substrate surface oxide layer and contamination, its hydrogen flowing quantity should guarantee to remove oxide layer can not cross process again.
4. the method for the beta-silicon carbide thin film of epitaxial growth on a silicon substrate of a kind of optimization according to claim 1, is characterized in that described carbonisation by passing into the large discharge C of 40 ~ 100ml/min under low carbonization pressure
3h
8obtain high-quality silicon carbide buffer layer.
5. the method for the beta-silicon carbide thin film of epitaxial growth on a silicon substrate of a kind of optimization according to claim 1, is characterized in that the carbon silicon ratio used in the growth of described first time and second time growth course is respectively 3:1 ~ 6:1 and 2:1 ~ 4:1.
6. the method for the beta-silicon carbide thin film of epitaxial growth on a silicon substrate of a kind of optimization according to claim 1, is characterized in that described first time epitaxial growth is by being respectively the low discharge SiH of 5 ~ 10ml/min
4and C
3h
8and be greater than the high-carbon silicon ratio of 3, realize low speed high quality epitaxial growth, form the high-quality silicon B-carbide resilient coating that one deck 0.1 ~ 0.6 μm is thick.
7. the method for the beta-silicon carbide thin film of epitaxial growth on a silicon substrate of a kind of optimization according to claim 1, is characterized in that the original position etching after described first time epitaxial growth, can reduce blemish, improve subsequent epitaxial layer crystal weight.
8. the method for the beta-silicon carbide thin film of epitaxial growth on a silicon substrate of a kind of optimization according to claim 1, is characterized in that the growth of described second time is by improving SiH
4and C
3h
8flow and the comparatively low carbon silicon ratio of first time extension, aforementioned resilient coating realizes the epitaxial growth of 5 ~ 25 μm/h, growth temperature and pressure with first time growth phase with, controllable precise within the scope of thickness 1 ~ 50 μm can be realized according to extension needs.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107578988A (en) * | 2017-09-13 | 2018-01-12 | 中国电子科技集团公司第十三研究所 | Silicon carbide epitaxial layers passivating method |
| CN110117814A (en) * | 2018-02-05 | 2019-08-13 | 西安电子科技大学 | The preparation method of silicon carbide epitaxy with low-density C vacancy defect |
| CN112410762A (en) * | 2020-12-07 | 2021-02-26 | 湖南德智新材料有限公司 | Silicon-based tray for MOCVD equipment and preparation method |
| CN113113290A (en) * | 2021-04-02 | 2021-07-13 | 眉山博雅新材料有限公司 | Preparation method of silicon carbide crystals |
| CN113957535A (en) * | 2021-10-19 | 2022-01-21 | 林健峯 | Method for forming single crystal silicon carbide film on silicon substrate |
| CN114068308A (en) * | 2022-01-17 | 2022-02-18 | 季华实验室 | Substrate for silicon-based MOSFET device and preparation method thereof |
| CN115074825A (en) * | 2022-06-10 | 2022-09-20 | 厦门紫硅半导体科技有限公司 | Silicon carbide epitaxial structure, pulse type growth method and application thereof |
| CN117293015A (en) * | 2023-11-23 | 2023-12-26 | 希科半导体科技(苏州)有限公司 | Growth method of silicon carbide epitaxial layer of silicon substrate and silicon-based silicon carbide epitaxial wafer |
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| CN112410762A (en) * | 2020-12-07 | 2021-02-26 | 湖南德智新材料有限公司 | Silicon-based tray for MOCVD equipment and preparation method |
| CN113113290B (en) * | 2021-04-02 | 2021-12-24 | 眉山博雅新材料股份有限公司 | Preparation method of silicon carbide crystals |
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| CN113957535A (en) * | 2021-10-19 | 2022-01-21 | 林健峯 | Method for forming single crystal silicon carbide film on silicon substrate |
| CN113957535B (en) * | 2021-10-19 | 2022-12-27 | 林健峯 | Method for forming single crystal silicon carbide film on silicon substrate |
| CN114068308A (en) * | 2022-01-17 | 2022-02-18 | 季华实验室 | Substrate for silicon-based MOSFET device and preparation method thereof |
| CN115074825A (en) * | 2022-06-10 | 2022-09-20 | 厦门紫硅半导体科技有限公司 | Silicon carbide epitaxial structure, pulse type growth method and application thereof |
| CN117293015A (en) * | 2023-11-23 | 2023-12-26 | 希科半导体科技(苏州)有限公司 | Growth method of silicon carbide epitaxial layer of silicon substrate and silicon-based silicon carbide epitaxial wafer |
| CN117293015B (en) * | 2023-11-23 | 2024-02-20 | 希科半导体科技(苏州)有限公司 | Growth method of silicon carbide epitaxial layer of silicon substrate and silicon-based silicon carbide epitaxial wafer |
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