CN1072282C - Film growth of silicon carbide monocrystal using silicon substrate beta-silicon carbide crystal - Google Patents
Film growth of silicon carbide monocrystal using silicon substrate beta-silicon carbide crystal Download PDFInfo
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- CN1072282C CN1072282C CN98112814A CN98112814A CN1072282C CN 1072282 C CN1072282 C CN 1072282C CN 98112814 A CN98112814 A CN 98112814A CN 98112814 A CN98112814 A CN 98112814A CN 1072282 C CN1072282 C CN 1072282C
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Abstract
The present invention relates to a method for growing silicon carbide monocrystal by a hetero epitaxy beta silicon carbide crystal on a silicon substrate, which belongs to the technical field of crystal preparation and is a special method for aiming at silicon carbide which is difficult to be dissolved and manufactured. The method uses a 3C-SiC hetero epitaxy monocrystal thin layer and a silicon substrate thereof as a liquid phase epitaxy substrate and a source which are integrated, a carbon saturation solution is formed by dissolving a graphite crucible wall after the silicon substrate is melted to realize the low temperature and low cost growth by using a beta-SiC epitaxy film as a seed crystal, and one side of a silicon carbide crystal is polished. Because the growth process only relates to high pure graphite and a silicon chip, the height impurity compensation of the silicon carbide grown by a sublimation method is avoided.
Description
The present invention relates to a kind of preparation method of carborundum crystals, particularly utilize the method for the beta-sic crystal film preparation carborundum crystals of growing on the silicon substrate.
Because silicon carbide can not exist with melt under normal pressure, the generation of the various carborundum crystals before the present invention finishes is all based on subliming method, the fritter carborundum crystals that promptly utilizes perfect structure is grown into larger-size crystal as seed crystal in the distillation atmosphere of silicon carbide.Its limitation is preparation temperature very high (～2400 ℃), and the temperature field is difficult to control, and earlier seed body will be arranged.Owing to the silicon carbide that can only grow α type (mainly being 6H type wherein) with these class methods at present, also and do not find to have the direct precedent report for preparing single-crystal silicon carbide with the beta-type silicon carbide seed crystal.
Detail knowledge to the above-mentioned background situation, can roll up " silicon carbide characteristic " (" Properties of Silicon Carbide " with reference to the electronic material data comment book series the 13rd that IEE (IEE) publishes, Cary L.Harris chief editor, EMIS Series No.13, IESPIE press nineteen ninety-five publishes) the 8th chapter the 1st joint " bulk single crystal silicon carbide growth (Bulk Growth of SiC) " (p.163) of a book.This book is to the most comprehensive comment of silicon carbide whisker preparation in the at present relevant new publication of silicon carbide, and provide and relate to the catalogue that carborundum crystals prepares the most important document of various work, very useful to overall understanding growing silicon carbice crystals research history and present Research.
The objective of the invention is to, a kind of method of utilizing the beta-sic crystal film preparation carborundum crystals of growing on the silicon substrate is provided.Adopt this method, can in the temperature range below 2000 ℃, do starting material with monocrystalline silicon piece cheap and easy to get, with fairly simple method and apparatus, the highly purified single-crystal silicon carbide body of growing.
The objective of the invention is to realize by the following method:
Its method is: the silicon substrate beta-sic crystal film that will utilize the ordinary method preparation, be placed on and make the silicon substrate fusing in the plumbago crucible, single crystal silicon carbide thin film does not melt yet and does not distil, formation makes the solid carborundum films become substrate conversely and is infiltrated on silicon carbide liquid phase epitaxy system in the saturated silicon solution of carbon, uses the growing silicon carbide single crystal body.When silicon solution exhausts, promptly obtain the silicon carbide that thickness is approximately 2 times of former silicon wafer thicknesses.If in crucible, be added with the silicon raw material in addition, the thicker carborundum crystals of also can growing.
Its step is as follows:
1, the β-SiC epitaxial film that on silicon substrate, prepares good uniformity with conventional gas phase heteroepitaxy;
2, the silicon substrate that will have β-SiC film places the pure plumbago crucible of electronics, and crucible places 10
-4In the Pa high vacuum chamber;
3, under the argon filling atmosphere protection after above-mentioned high vacuum or the high vacuum, with ratio-frequency heating or resistive heating mode silicon substrate is heated to its fusing point and makes its fusing for 1410 ℃;
4, continue the temperature of rising silicon solution, in 1600～1900 ℃ of scopes, determine growth temperature according to the needs of growth velocity, keep constant temperature, the silicon carbide liquid phase epitaxy is carried out under the quasistatic condition, growth velocity is regulated by growth temperature between 0.1-10 μ m/min.
Technical basis of the present invention and beneficial effect thereof are:
The rheotaxy that utilizes saturated solution growing semiconductor thin layer is a kind of effective growing method, employing (see before and state reference) is also arranged in the preparation of single crystal silicon carbide thin film, but all be to make the carborundum films that substrate epitaxial is counted micron thickness, comprise β-SiC film with the 6H-SiC wafer.This ordinary method need have certain thickness finished product silicon carbide wafer with one and make substrate, and as raw material, the fusing back generates carbon saturated solution with other silicon.The vapour phase epitaxy product that β-SiC crystal thin layer and silicon wafer are integrated in the present invention has solved the problem of shortage β-SiC substrate as incorporate rheotaxy substrate and source.
Because the temperature very high (above 2000 ℃) that β-SiC changes to alpha silicon carbide, more can not melt or distil (sublimation temperature is 2400 ℃), so after the silicon substrate fusing and forming carbon saturated solution, primary β-SiC film energy stable existence also serves as the seed crystal effect.
Because the fusing point of silicon hangs down 1000 ℃ than the sublimation temperature of silicon carbide, so in this way than much lower with the subliming method temperature; Because the raw material that subliming method is used is the silicon carbide (also do not have at present the silicon carbide of electronic-grade can be as the raw material of crystal growth) of Industrial products level, although can adopt porous graphite to filter some impurity, but effect is not fairly obvious, thereby the crystal impurity compensation of making is very serious.Present method only uses high-purity silicon chip of electronic-grade and high purity graphite to be raw material, and the source of pollution in the preparation facilities are also less, and how pure silicon chip have in principle, and how pure the silicon carbide plate that grows up to just have.And as long as temperature controls well, the good uniformity of β-SiC thin layer itself has the silicon substrate of much diameters just can grow the silicon carbide wafer of much diameters in principle.
Accompanying drawing is the structural representation with the device of the beta-sic crystal film growth single-crystal silicon carbide body on the silicon substrate.Wherein 1 is the stainless steel body of heater, and 2 is heat insulation quartz sleeve, and 3 is the high-frequency induction heating coil, and 4 is plumbago crucible, and 5 serve as reasons melts the carbon saturated solution that silicon forms, and 6 is the graphite lagging material, and 7 is quartzy cover plate, and 8 are the single-crystal silicon carbide thin slice in the growth.
Specific embodiments of the present invention is described below in conjunction with the accompanying drawings:
1, with the beta sic single crystal film of conventional heated filament CVD method thick 1 μ m of epitaxy on the n of thickness 0.4mm type (100) single-sided polishing silicon substrate, the resistivity of silicon substrate is 10 Ω cm, diameter 30mm;
2, said sample is placed in the plumbago crucible 4 (crucible outside diameter 50mm, interior diameter 30mm, long 50mm, the dark 10mm of pot) in silicon substrate mode down, cover quartzy cover plate 7, place in the stainless steel body of heater 1, vacuumize;
3, at furnace chamber pressure less than 10
-4Behind the handkerchief, be the high-frequency electric field of 2.5kHz by 3 pairs of plumbago crucible 4 coupling frequencies of high-frequency induction heating coil.High frequency electric source adopts the temperature closed loop control mode, the multiple step format heating.The first step is set at 1410 ℃ with temperature, makes the silicon substrate fusing, utilizes melt silicon that the solvency action of sidewall of crucible is formed carbon saturated solution.
4, temperature is set at 1800 ℃ again, keeps constant temperature, the interface of the saturated silicon solution of carborundum films and carbon is extended in melt gradually, film is thickening gradually, and when melt exhausted, the crystal growing process end generated light yellow silicon carbide wafer.About 20 hours consuming time of whole process.
1, uses n type single-sided polishing (111) silicon substrate instead, resistance substrate rate 10 Ω cm, diameter 30mm, thick 0.4mm; Beta sic single crystal film with the thick 1 μ m of conventional heated filament CVD method epitaxy thereon;
2, said sample is placed in the plumbago crucible 4 (crucible outside diameter 50mm, interior diameter 30mm, long 50mm, the dark 10mm of pot) in silicon substrate mode down, cover quartzy cover plate 7, place in the stainless steel body of heater 1, vacuumize;
3, at furnace chamber pressure less than 10
-4Behind the handkerchief, be the high-frequency electric field of 2.5kHz by 3 pairs of plumbago crucible 4 coupling frequencies of high-frequency induction heating coil.High frequency electric source adopts the temperature closed loop control mode, the multiple step format heating.The first step is set at 1410 ℃ with temperature, makes the silicon substrate fusing, utilizes melt silicon that the solvency action of sidewall of crucible is formed carbon saturated solution.
4, temperature is set at 1800 ℃ again, keeps constant temperature, the interface of the saturated silicon solution of carborundum films and carbon is extended in melt gradually, film is thickening gradually, and when melt exhausted, the crystal growing process end generated light yellow silicon carbide wafer.About 20 hours consuming time of whole process.
Claims (1)
- A kind of method of utilizing the beta-sic crystal film growth single-crystal silicon carbide body on the silicon substrate, realize by following method and step:Method provided by the invention is, utilization is with the silicon substrate beta-sic crystal film of ordinary method preparation, in plumbago crucible, its silicon substrate is melted, formation makes the solid carborundum films become substrate conversely and is infiltrated on silicon carbide liquid phase epitaxy system in the saturated silicon solution of carbon, uses the growing silicon carbide single crystal body;Its concrete steps are as follows:(1), the β-SiC epitaxial film that on silicon substrate, prepares good uniformity with conventional gas phase heteroepitaxy;(2), the silicon substrate that will have β-SiC film places the pure plumbago crucible of electronics, and crucible places 10 -4In the Pa high vacuum chamber;(3), under the argon filling atmosphere protection after above-mentioned high vacuum or the high vacuum, with ratio-frequency heating or resistive heating mode silicon substrate is heated to its fusing point and makes its fusing for 1410 ℃;(4), continue the temperature of rising silicon solution, in 1600～1900 ℃ of scopes, determine growth temperature, keep constant temperature according to the needs of growth velocity, the silicon carbide liquid phase epitaxy is carried out under the quasistatic condition, and growth velocity is regulated by growth temperature between 0.1-10 μ m/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98112814A CN1072282C (en) | 1998-01-23 | 1998-01-23 | Film growth of silicon carbide monocrystal using silicon substrate beta-silicon carbide crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98112814A CN1072282C (en) | 1998-01-23 | 1998-01-23 | Film growth of silicon carbide monocrystal using silicon substrate beta-silicon carbide crystal |
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| Publication Number | Publication Date |
|---|---|
| CN1224084A CN1224084A (en) | 1999-07-28 |
| CN1072282C true CN1072282C (en) | 2001-10-03 |
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| CN98112814A Expired - Fee Related CN1072282C (en) | 1998-01-23 | 1998-01-23 | Film growth of silicon carbide monocrystal using silicon substrate beta-silicon carbide crystal |
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| CN100497760C (en) * | 2007-07-24 | 2009-06-10 | 中国电子科技集团公司第五十五研究所 | High doping concentration silicon carbide epitaxial growth method |
| JP5556761B2 (en) | 2011-07-28 | 2014-07-23 | 株式会社デンソー | Silicon carbide single crystal manufacturing equipment |
| CN104593865A (en) * | 2014-12-25 | 2015-05-06 | 廖奇泊 | Manufacturing method of silicon carbide base crystal layer |
| CN111676516B (en) * | 2020-08-05 | 2024-01-19 | 常州臻晶半导体有限公司 | Carbon supply device for growing silicon carbide single crystal by melt method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19503976C1 (en) * | 1995-02-07 | 1996-05-09 | Max Planck Gesellschaft | Single crystal epitaxial silicon carbide layer prodn |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19503976C1 (en) * | 1995-02-07 | 1996-05-09 | Max Planck Gesellschaft | Single crystal epitaxial silicon carbide layer prodn |
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