JPH0463840B2 - - Google Patents
Info
- Publication number
- JPH0463840B2 JPH0463840B2 JP13538287A JP13538287A JPH0463840B2 JP H0463840 B2 JPH0463840 B2 JP H0463840B2 JP 13538287 A JP13538287 A JP 13538287A JP 13538287 A JP13538287 A JP 13538287A JP H0463840 B2 JPH0463840 B2 JP H0463840B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- sic
- substrate
- single crystal
- tic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 52
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 51
- 239000013078 crystal Substances 0.000 claims description 44
- 239000000758 substrate Substances 0.000 claims description 24
- 238000004519 manufacturing process Methods 0.000 claims description 8
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 239000010408 film Substances 0.000 description 37
- 239000010936 titanium Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000005229 chemical vapour deposition Methods 0.000 description 8
- 230000007547 defect Effects 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000001294 propane Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001835 Lely method Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- -1 methaneethylene Natural products 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- VEDJZFSRVVQBIL-UHFFFAOYSA-N trisilane Chemical compound [SiH3][SiH2][SiH3] VEDJZFSRVVQBIL-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
産業上の利用分野
本発明は半導体素子の原料として用いられる炭
化珪素（SiC）単結晶膜の製造方法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for producing a silicon carbide (SiC) single crystal film used as a raw material for semiconductor devices.
従来技術
炭化珪素半導体は、広い禁制帯幅をもち（2.2
〜3.3eV）、また熱的、化学的および機械的に極
めて安定で、放射線損傷にも強いという特徴を有
している。したがつて炭化珪素（以下、SiCと記
す）を用いた半導体素子は、従来の珪素（以下、
Siと記す）等を用いた他の半導体では使用が困難
な高温・高出力、放射線損傷等の苛酷な条件下で
も使用することができる素子材料として広範な分
野での応用が期待されている。Conventional technology Silicon carbide semiconductors have a wide forbidden band width (2.2
~3.3eV), and is extremely stable thermally, chemically, and mechanically, and is resistant to radiation damage. Therefore, semiconductor devices using silicon carbide (hereinafter referred to as SiC) are different from conventional silicon (hereinafter referred to as SiC).
It is expected to be applied in a wide range of fields as an element material that can be used under harsh conditions such as high temperatures, high output, and radiation damage, which are difficult to use with other semiconductors using materials such as Si (hereinafter referred to as Si).
このようにSiC半導体は、多くの利点、可能性
を有する材料であるにも拘わらず、その実用化が
阻まれているのは、生産性を考慮した工業的規模
での量産に必要な寸法・形状を制御した大面積か
つ高品質の単結晶を安定に供給し得る結晶成長技
術が確立されていなかつたところに原因がある。
従来、研究室規模で昇華再結晶法（レーリ法とも
称される）等でSiC単結晶を成長させたり、この
レーリ法による単結晶上に気相成長や液相成長に
よりエビタキシヤル成長させることでSiC単結晶
を得ている。しかしながら、これらの単結晶は小
面積であり、寸法・形状を制御することは困難で
ある。また、SiCに存在する結晶多形の制御およ
び不純物濃度の制御も容易ではない。 Although SiC semiconductors are a material with many advantages and possibilities, their practical application is hindered by the size and size required for mass production on an industrial scale with productivity in mind. The reason for this is that crystal growth technology that could stably supply large-area, high-quality single crystals with controlled shapes had not been established.
Conventionally, SiC has been grown by growing SiC single crystals on a laboratory scale using the sublimation recrystallization method (also known as the Lely method), or by ebitaxial growth using vapor phase growth or liquid phase growth on single crystals using the Ley method. Obtaining a single crystal. However, these single crystals have a small area, and it is difficult to control their size and shape. Furthermore, it is not easy to control the crystal polymorphism and impurity concentration present in SiC.
最近になつて、Si単結晶基板上に化学的気相成
長法（CVD法）で良質かつ大面積の3C型のSiC
単結晶を成長させる方法が開発された（特願昭58
−76842号）「炭化珪素単結晶基板の製造方法」）。
また、Si基板表面を炭化水素ガス雰囲気下で加熱
して炭化することでSiCの薄膜を表面に形成し、
この薄膜上のCVD法によりSiC単結晶を成長させ
る方法も開発され、すでに公知の技術となつてい
る。 Recently, high-quality, large-area 3C-type SiC has been developed using chemical vapor deposition (CVD) on a single-crystal Si substrate.
A method for growing single crystals was developed (patent application 1983).
-76842) "Method for manufacturing silicon carbide single crystal substrate").
In addition, a thin film of SiC is formed on the surface of the Si substrate by heating and carbonizing it in a hydrocarbon gas atmosphere.
A method for growing SiC single crystals using the CVD method on this thin film has also been developed and is already a well-known technique.
発明が解決しようとする問題点
上記の技術ではSi単結晶基板上にSiCを直接成
長させる方法であるため、SiとSiCとの20％もの
格子定数のちがい、あるいはSiとSiCの熱膨張係
数のちがいに起因する結晶欠陥が多数含まれてお
り、またSiC成長層に反りやクラツクが発生しや
すいという問題がある。SiC半導体素子を実用化
するためには反り、クラツクがなく欠陥の少ない
高品質なSiC単結晶を作製することが必要であ
り、このための製造技術の開発が強く要望されて
いる。Problems to be Solved by the Invention Since the above technology is a method of growing SiC directly on a Si single crystal substrate, there may be a 20% difference in lattice constant between Si and SiC, or a difference in thermal expansion coefficient between Si and SiC. It contains many crystal defects caused by differences, and there is also the problem that warping and cracks are likely to occur in the SiC growth layer. In order to put SiC semiconductor devices into practical use, it is necessary to produce high-quality SiC single crystals that are free from warpage and cracks and have few defects, and there is a strong demand for the development of manufacturing technology for this purpose.
本発明の目的は、上述の問題点を解決し、結晶
欠陥が低減された高品質の炭化珪素単結晶膜の製
造方法を提供することである。 An object of the present invention is to solve the above-mentioned problems and provide a method for manufacturing a high-quality silicon carbide single crystal film with reduced crystal defects.
問題点を解決するための手段
本発明は、珪素基板上に炭化チタン膜層を形成
した後、該炭化チタン膜上に炭化珪素単結晶を成
長させることを特徴とする炭化珪素単結晶膜の製
造方法である。Means for Solving the Problems The present invention provides production of a silicon carbide single crystal film, which is characterized in that a titanium carbide film layer is formed on a silicon substrate, and then a silicon carbide single crystal is grown on the titanium carbide film. It's a method.
作 用
本発明は上記の問題に鑑み、Si基板上に単結晶
炭化チタン（以下TiCと記す）膜を中間層として
導入し、その上にSiC単結晶を成長させることに
より反り、クラツクがなく結晶欠陥の少ないSiC
単結晶を得ることができる。Effects In view of the above problems, the present invention introduces a single crystal titanium carbide (hereinafter referred to as TiC) film as an intermediate layer on a Si substrate, and grows a SiC single crystal on top of the film to prevent warping and cracks. SiC with fewer defects
Single crystals can be obtained.
実施例
第１図は本発明の基本原理を説明する模式図で
ある。従来技術（第１図１）では珪素基板１上に
直接SiC２を成長させていたため、Si（格子定数
ａ）と、SiC（格子定数ｂ）の格子定数あるは熱
膨張係数のちがいが、SiC成長層２の反り、クラ
ツクあるいは結晶欠陥の原因となつていた。本発
明はSi基板１上のチタン（以下、Tiと記す）膜
６全部あるいはその表面のみを、SiCと格子定数
や熱膨張係数の値の近い炭化チタン（以下、TiC
と記す）膜４（格子定数ｂ１）とし（第１図２ま
たは同図３）、そのTiC膜４上にSiC単結晶２を成
長させるものである。Embodiment FIG. 1 is a schematic diagram illustrating the basic principle of the present invention. In the conventional technology (Fig. 1 1), SiC2 was grown directly on the silicon substrate 1, so the difference in lattice constant or thermal expansion coefficient between Si (lattice constant a) and SiC (lattice constant b) caused the growth of SiC. This caused warpage, cracks, or crystal defects in layer 2. In the present invention, the entire titanium (hereinafter referred to as Ti) film 6 on the Si substrate 1 or only its surface is coated with titanium carbide (hereinafter referred to as TiC), which has a lattice constant and thermal expansion coefficient similar to that of SiC.
A SiC single crystal 2 is grown on the TiC film 4 (see FIG. 1 or 3).
TiCはSiCと同様の結晶構造を持ち、格子定数
や熱膨張係数の値がSiCの値と近いものであり、
とくにTi膜４を炭化することによつて得られる
TiC薄膜は、Si基板１の結晶方位を引き継いだ単
結晶膜となつていると推定される。このような
TiC層はSiとSiCとの間の格子定数や熱膨張係数
のちがいを緩和する層として働き、良質のSiC単
結晶をエピタキシヤル成長させることができる。 TiC has a crystal structure similar to SiC, and its lattice constant and coefficient of thermal expansion are close to those of SiC.
In particular, it can be obtained by carbonizing the Ti film 4.
It is estimated that the TiC thin film is a single crystal film that has inherited the crystal orientation of the Si substrate 1. like this
The TiC layer acts as a layer that alleviates the difference in lattice constant and thermal expansion coefficient between Si and SiC, and enables epitaxial growth of high-quality SiC single crystals.
以下に本発明方法の具体的な実施について第１
図を参照して記載する。Si基板１上に形成される
TiC膜層４は、Si基板１上にTiC膜４が形成され
ている形であつてもよいし、Ti層６の表面のみ
が、TiC膜となつていてもよい。すなわちSi基板
１上にTi膜６を蒸着等の方法により形成したの
ち、炭化水素雰囲気中で高温で加熱することによ
り、該Ti膜の全部または表面のみをTiC化しても
よい。またSi基板上にたとえばスパツタ法などに
より、TiCを直接形成させてもよい。 The following is the first part about the specific implementation of the method of the present invention.
Describe with reference to figures. formed on Si substrate 1
The TiC film layer 4 may be formed on the Si substrate 1, or only the surface of the Ti layer 6 may be a TiC film. That is, after the Ti film 6 is formed on the Si substrate 1 by a method such as vapor deposition, the whole or only the surface of the Ti film may be converted into TiC by heating at a high temperature in a hydrocarbon atmosphere. Alternatively, TiC may be directly formed on the Si substrate by, for example, a sputtering method.
TiC膜の厚さは５Å以上、好ましくは５Å〜
1000Å、より好ましくは約200Åである。形成さ
れたTiC膜４表面上にSiC単結晶膜２を形成する。
SiC単結晶膜２を形成させる方法としては、熱分
解CVD法が好ましい。すなわち、適当な炭素源
（たとえばプロパン、メタンエチレン、アセチレ
ン）と珪素源（たとえば、モノシラン、ジシラ
ン、トリシラン）等を用いて、約800〜1400℃、
好ましくは1300〜1350℃に加熱することにより、
TiC４上にSiC単結晶膜２が形成される。この場
合、Si基板１上にTiC４をエピタキシヤル成長さ
せると、形成されるSiC単結晶膜２もSi基板１の
面方位を受け継いでエピタキシヤル成長する。 The thickness of the TiC film is 5 Å or more, preferably 5 Å or more
1000 Å, more preferably about 200 Å. A SiC single crystal film 2 is formed on the surface of the formed TiC film 4.
As a method for forming the SiC single crystal film 2, a thermal decomposition CVD method is preferable. That is, using a suitable carbon source (e.g. propane, methaneethylene, acetylene) and silicon source (e.g. monosilane, disilane, trisilane), etc., at a temperature of about 800 to 1400°C,
Preferably by heating to 1300-1350°C,
SiC single crystal film 2 is formed on TiC 4. In this case, when TiC 4 is epitaxially grown on the Si substrate 1, the formed SiC single crystal film 2 also inherits the plane orientation of the Si substrate 1 and grows epitaxially.
したがつてたとえばSi（111）基板１上にエピタ
キシヤル成長させてTiC層４を形成し、この上に
SiCを熱分解CVD法により形成すると得られた
SiC単結晶膜６の面方位も（111）である。なお、
CVD装置においてTi膜６を堆積させたSi基板１
を用いて、炭化水素ガスによりTiC層４を形成し
た場合は、同装置内で引き続いて、該TiC膜４上
にSiC単結晶膜２を成長させることができるた
め、製造工程が単純で有利である。 Therefore, for example, a TiC layer 4 is formed by epitaxial growth on a Si (111) substrate 1, and a TiC layer 4 is formed on this.
Obtained by forming SiC by pyrolysis CVD method
The plane orientation of the SiC single crystal film 6 is also (111). In addition,
Si substrate 1 with Ti film 6 deposited in CVD equipment
When the TiC layer 4 is formed with hydrocarbon gas using the same device, the SiC single crystal film 2 can be subsequently grown on the TiC film 4 in the same device, so the manufacturing process is simple and advantageous. be.
次に具体例により本発明の実施態様を示す。 Next, embodiments of the present invention will be illustrated by specific examples.
Si基板１上に形成したTi膜６の炭化にはプロ
パン（C3H8）を用い、炭化後のCVD成長の原料
ガスとしてはモノシラン（SiH4）とプロパン
（C3H8）とを用いて行なつた。 Propane (C 3 H 8 ) is used to carbonize the Ti film 6 formed on the Si substrate 1 , and monosilane (SiH 4 ) and propane (C 3 H 8 ) are used as source gases for CVD growth after carbonization. I did it.
第２図は実施例に用いられた成長装置の概略図
である。黒鉛試料台９上にTi膜を５〜1000Å、
一般的にはほぼ200Åに真空蒸着したSi（111）単
結晶基板１０を載置する。キヤリアガスとして水
素ガスを毎分３、原料ガスとしてプロパンガス
を毎分１c.c.程度流し、ワークコイル１１に高周波
電流を流して黒鉛試料台９を加熱して、該基板を
約1350℃まで加熱し、１〜５分程度保持すること
によりTi膜を炭化して、TiC膜を形成する。 FIG. 2 is a schematic diagram of a growth apparatus used in Examples. A Ti film with a thickness of 5 to 1000 Å is placed on the graphite sample stage 9.
Generally, a Si (111) single crystal substrate 10 vacuum-deposited to a thickness of approximately 200 Å is mounted. Hydrogen gas is flowed as a carrier gas at a rate of 3 c.c./min, propane gas is flowed as a raw material gas at a rate of 1 c.c./min, and a high frequency current is passed through the work coil 11 to heat the graphite sample stage 9 and heat the substrate to approximately 1350°C. The Ti film is then carbonized by holding it for about 1 to 5 minutes to form a TiC film.
次いでモオシランとプロパンガスをそれぞれ毎
分0.1〜0.9c.c.、キヤリアガスの水素（毎分３）
とともに流してSiC単結晶膜を1300〜1350℃の温
度で成長させる、１時間で約3μｍの成長膜が得
られた。得られたSiC成長膜は反り、クラツクが
なくＸ線回析および電子線回析により（111）方
向にエピタキシヤル成長した単結晶膜であること
がわかつた。また電子顕微鏡観察の結果結晶欠陥
の少ない良質のSiC単結晶膜であることがわかつ
た。 Next, moosilane and propane gas each at 0.1 to 0.9 cc/min, and carrier gas hydrogen (3/min)
A SiC single crystal film was grown at a temperature of 1,300 to 1,350°C, and a grown film of about 3 μm was obtained in one hour. The SiC grown film obtained was free of warpage and cracks, and was found to be a single crystal film epitaxially grown in the (111) direction by X-ray diffraction and electron beam diffraction. Furthermore, electron microscopy revealed that it was a high quality SiC single crystal film with few crystal defects.
効 果
本発明によれば、Si基板上に反り、クラツクが
なく結晶欠陥の少ない高品質のSiC単結晶を得る
ことができるため、SiCを用いた半導体素子の実
用化を急速に促進する。Effects According to the present invention, it is possible to obtain a high-quality SiC single crystal without warping or cracking and with few crystal defects on a Si substrate, thereby rapidly promoting the practical application of semiconductor devices using SiC.
第１図は本発明によるSiC成長を説明するため
の結晶格子を示す図である。第２図は本発明の実
施例に用いたCVD装置の概略図である。
１……Si基板、２……SiC成長膜、３，５……
界面、４……TiC膜、６……TiまたはTiとTiCの
混合した膜、９……試料台、１０……Ti薄膜付
Si単結晶基板、１１……ワークコイル、ａ……Si
の格子定数、ｂ……SiCの格子定数、ｂ１……
TiCの格子定数。
FIG. 1 is a diagram showing a crystal lattice for explaining SiC growth according to the present invention. FIG. 2 is a schematic diagram of a CVD apparatus used in an embodiment of the present invention. 1...Si substrate, 2...SiC growth film, 3, 5...
Interface, 4...TiC film, 6...Ti or mixed film of Ti and TiC, 9...sample stand, 10...with Ti thin film
Si single crystal substrate, 11...work coil, a...Si
Lattice constant of, b... Lattice constant of SiC, b1...
Lattice constant of TiC.
Claims (1)
該炭化チタン膜上に炭化珪素単結晶を成長させる
ことを特徴とする炭化珪素単結晶膜の製造方法。1 After forming a titanium carbide film layer on a silicon substrate,
A method for producing a silicon carbide single crystal film, comprising growing a silicon carbide single crystal on the titanium carbide film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13538287A JPS63303896A (en) | 1987-05-30 | 1987-05-30 | Production of silicon carbide single crystal film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13538287A JPS63303896A (en) | 1987-05-30 | 1987-05-30 | Production of silicon carbide single crystal film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63303896A JPS63303896A (en) | 1988-12-12 |
| JPH0463840B2 true JPH0463840B2 (en) | 1992-10-13 |
Family
ID=15150400
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13538287A Granted JPS63303896A (en) | 1987-05-30 | 1987-05-30 | Production of silicon carbide single crystal film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63303896A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5010035A (en) * | 1985-05-23 | 1991-04-23 | The Regents Of The University Of California | Wafer base for silicon carbide semiconductor device |
| WO2016104291A1 (en) * | 2014-12-22 | 2016-06-30 | 信越化学工業株式会社 | Composite substrate, method for forming nanocarbon film, and nanocarbon film |
-
1987
- 1987-05-30 JP JP13538287A patent/JPS63303896A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63303896A (en) | 1988-12-12 |
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