JPH0143720B2 - - Google Patents
Info
- Publication number
- JPH0143720B2 JPH0143720B2 JP59138569A JP13856984A JPH0143720B2 JP H0143720 B2 JPH0143720 B2 JP H0143720B2 JP 59138569 A JP59138569 A JP 59138569A JP 13856984 A JP13856984 A JP 13856984A JP H0143720 B2 JPH0143720 B2 JP H0143720B2
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- film
- sapphire substrate
- silicon carbide
- crystal film
- 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.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
〔発明の技術分野〕
この発明は、絶縁性基板であるサフアイア基板
上への炭化硅素単結晶膜の製造方法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to a method for manufacturing a silicon carbide single crystal film on a sapphire substrate, which is an insulating substrate.
サフアイアなどの絶縁性基板上へのシリコン単
結晶膜の作製(SOS)は、素子集積化に際して素
子間の電気的分離が容易であるために、シリコン
集積回路作製技術上重要である。これと同様の理
由で絶縁性基板であるサフアイア基板上への炭化
硅素単結晶膜の作製技術は、炭化硅素を用いた電
子あるいは光電子素子作製上重要である。しか
し、サフアイア基板上への炭化硅素単結晶膜の作
製は殆ど行われていない。
The fabrication of single crystal silicon films (SOS) on insulating substrates such as sapphire is important in silicon integrated circuit fabrication technology because it facilitates electrical isolation between elements during element integration. For similar reasons, the technique for producing a silicon carbide single crystal film on a sapphire substrate, which is an insulating substrate, is important for producing electronic or optoelectronic devices using silicon carbide. However, a silicon carbide single crystal film has hardly been formed on a sapphire substrate.
例えば、化成蒸着法によりサフアイア基板上に
炭化硅素を成長させた場合、繊維構造膜は基板よ
り剥離しないが、単結晶膜は厚さ2000Å以上で、
膜成長後膜が基板から剥離してしまう。しかしサ
フアイア基板上に、化成蒸着法により窒化アルミ
ニウム単結晶膜を成長させ、この上に炭化硅素を
成長させることにより、剥離することなく炭化硅
素単結晶膜が成長できる。この炭化硅素単結晶膜
は双晶構造を含むため、電気的性質に劣り、電子
素子への応用上結晶の質の向上が必要である。 For example, when silicon carbide is grown on a sapphire substrate by chemical vapor deposition, the fiber structure film does not peel off from the substrate, but the single crystal film has a thickness of 2000 Å or more.
After film growth, the film peels off from the substrate. However, by growing an aluminum nitride single crystal film on a sapphire substrate by chemical vapor deposition and growing silicon carbide thereon, a silicon carbide single crystal film can be grown without peeling. Since this silicon carbide single crystal film contains a twin crystal structure, it has poor electrical properties, and it is necessary to improve the quality of the crystal for application to electronic devices.
この発明は、上記の点にかんがみなされたもの
で、絶縁基板であるサフアイア基板上に窒化アル
ミニウム単結晶膜を成長させた後、その上にアル
ミニウムの酸化層を成長させ、さらに、その上に
炭化硅素単結晶膜を成長させることにより、剥離
することなくサフアイア基板上に、結晶性の良好
な、電気的性質に優れた炭化硅素単結晶膜を成長
させる方法を提供することを目的とするものであ
る。
This invention was developed in view of the above points. After growing an aluminum nitride single crystal film on a sapphire substrate, which is an insulating substrate, an aluminum oxide layer is grown on it, and then a carbide layer is grown on it. The purpose is to provide a method for growing a silicon carbide single crystal film with good crystallinity and excellent electrical properties on a sapphire substrate without peeling by growing a silicon single crystal film. be.
本発明者等は、窒化アルミニウム単結晶膜上へ
のアルミニウムの酸化層がこの目的を達成するの
に極めて有効であることを見出し、この発明に至
つたものである。 The present inventors have discovered that an aluminum oxide layer on an aluminum nitride single crystal film is extremely effective in achieving this objective, leading to the present invention.
次に、この発明に至つた技術的経緯を説明す
る。 Next, the technical background that led to this invention will be explained.
サフアイア基板上に窒化アルミニウム単結晶を
成長させ、この上に炭化硅素単結晶を成長させる
場合、窒化アルミニウム単結晶膜成長後、室温に
おいて窒化アルミニウム単結晶表面を大気にさら
した後、この上に炭化硅素を成長させるほうが、
大気にさらさない窒化アルミニウム上に成長させ
るより、単結晶の成長が容易であつた。 When growing an aluminum nitride single crystal on a sapphire substrate and then growing a silicon carbide single crystal on it, after the aluminum nitride single crystal film is grown, the surface of the aluminum nitride single crystal is exposed to the atmosphere at room temperature, and then the aluminum nitride single crystal surface is exposed to the atmosphere at room temperature. It is better to grow silicon
It was easier to grow single crystals than on aluminum nitride, which is not exposed to the atmosphere.
窒化アルミニウム単結晶膜は、大気にさらされ
ることによりその表面には数10Å厚さの酸化層が
形成されることが、オージエ電子分光測定による
深さ方向の組成分析の結果よりわかつている。 It has been found from depth composition analysis using Auger electron spectroscopy that an oxide layer several tens of angstroms thick is formed on the surface of aluminum nitride single crystal films when exposed to the atmosphere.
また、サフアイア基板上へ直接炭化硅素単結晶
を成長させた場合には、膜は成長後数時間で基板
より剥離してしまうが、成長した炭化硅素単結晶
膜は双晶構造を含まない極めて良好な結晶性を示
す。 Furthermore, when a silicon carbide single crystal is grown directly on a sapphire substrate, the film peels off from the substrate within a few hours after growth, but the grown silicon carbide single crystal film is extremely good and does not contain a twin structure. It shows crystallinity.
窒化アルミニウムおよびその酸化層は1013Ω・
cm以上の高い抵抗率を持ち、また、熱的、化学的
に極めて安定であるために、窒化アルミニウムと
その酸化層が存在することは、炭化硅素単結晶膜
を絶縁基板上に成長させるという目的を妨げない
ばかりでなく、素子化のための炭化硅素膜に対す
る熱的、化学的プロセスに十分耐え得ると考えら
れる。 Aluminum nitride and its oxide layer have a resistance of 10 13 Ω.
The presence of aluminum nitride and its oxide layer is useful for growing silicon carbide single crystal films on insulating substrates, as they have a high resistivity of more than cm and are extremely stable both thermally and chemically. It is thought that not only does it not interfere with the process, but also it can sufficiently withstand the thermal and chemical processes applied to the silicon carbide film for device fabrication.
この発明は、以上の知見に基づいて完成したも
のである。以下、この発明につき実施例に基づき
化成蒸着法による方法を説明する。 This invention was completed based on the above findings. Hereinafter, a method using a chemical vapor deposition method of the present invention will be explained based on Examples.
図面は、この発明を実施するための装置を示す
構成図である。10-6Pa以下の超高真空に排気さ
れた真空槽1内には、基板の背面或いは側面に基
板加熱ヒータ2があり、基板加熱ヒータ2近くに
はサフアイア基板3が配置され、その前面はシヤ
ツタ4で遮断されるようになつている。また、サ
フアイア基板3の前方中央にはアンモニア
(NH3)と酸素(O2)およびアセチレンガス
(C2H2)を導入するパイプ5が、その開口部5a
をサフアイア基板3に向けて配置され、パイプ5
の両側にはアルミニウム(Al)蒸発源6および
シリコン(Si)蒸発源7が配置されている。ま
た、8は排気口、9,10,11は制御弁であ
る。なお、基板加熱ヒータ2の温度制御装置は省
略してある。
The drawing is a block diagram showing an apparatus for carrying out the present invention. Inside the vacuum chamber 1, which is evacuated to an ultra-high vacuum of 10 -6 Pa or less, there is a substrate heater 2 on the back or side of the substrate, a sapphire substrate 3 is placed near the substrate heater 2, and the front side is It is designed to be shut off by shutter 4. Further, in the front center of the sapphire substrate 3, a pipe 5 for introducing ammonia (NH 3 ), oxygen (O 2 ), and acetylene gas (C 2 H 2 ) is located at its opening 5a.
is placed facing the sapphire substrate 3, and the pipe 5
An aluminum (Al) evaporation source 6 and a silicon (Si) evaporation source 7 are arranged on both sides. Further, 8 is an exhaust port, and 9, 10, and 11 are control valves. Note that the temperature control device for the substrate heater 2 is omitted.
炭化硅素単結晶膜作製の工程としては、真空槽
1内を10-6Pa以下の超高真空に排気し、アルミ
ニウム蒸発源6よりアルミニウム分子線を、基板
方向に向いたガス導入パイプ5より10- 3Paのア
ンモニアを1000〜1200℃に加熱されたサフアイア
基板3を同時に入射させ、窒化アルミニウム単結
晶膜を成長させる。膜の成長速度は、アルミニウ
ム分子線強度およびアンモニア分圧に依存する
が、2×1015/cm2・sec、7×10-3Paの時、約2
Å/secである。 In the process of producing a silicon carbide single crystal film, the inside of the vacuum chamber 1 is evacuated to an ultra-high vacuum of 10 -6 Pa or less, and an aluminum molecular beam is introduced from the aluminum evaporation source 6 through the gas introduction pipe 5 facing toward the substrate. - 3 Pa of ammonia is simultaneously applied to the sapphire substrate 3 heated to 1000 to 1200°C to grow an aluminum nitride single crystal film. The growth rate of the film depends on the aluminum molecular beam intensity and the ammonia partial pressure, but at 2×10 15 /cm 2 ·sec, 7×10 -3 Pa, it is about 2
It is Å/sec.
次に、所定の膜厚の窒化アルミニウム単結晶膜
を成長させた後、アルミニウム分子線はそのまま
とし、アンモニアガスの供給を止めるとともに、
サフアイア基板3の温度を同一に保つたままガス
導入パイプ5より、10-4Paの酸素を窒化アルミ
ニウム単結晶膜でおおわれたサフアイア基板3に
向けて導入する。成長時間は5分間である。 Next, after growing an aluminum nitride single crystal film with a predetermined thickness, the aluminum molecular beam is left as is, and the supply of ammonia gas is stopped.
While keeping the temperature of the sapphire substrate 3 the same, 10 -4 Pa of oxygen is introduced from the gas introduction pipe 5 toward the sapphire substrate 3 covered with the aluminum nitride single crystal film. Growth time is 5 minutes.
さらに、アルミニウム分子線および酸素の供給
を止め、アンモニアガスおよび酸素などの残留ガ
スの影響を避けるため、サフアイア基板3を1000
℃で真空中に60分以上保持して後、約1200℃にサ
フアイア基板3の温度を保ち、シリコン蒸発源7
よりシリコン分子線を、ガス導入パイプ5より
10-3Paのアセチレンを窒化アルミニウム単結晶
膜とその酸化層でおおわれたサフアイア基板3に
同時に入射させ、炭化硅素単結晶膜を成長させ
る。 Furthermore, in order to stop the supply of aluminum molecular beams and oxygen, and to avoid the influence of residual gases such as ammonia gas and oxygen, the sapphire substrate 3 was
After keeping the temperature of the sapphire substrate 3 at about 1200°C for more than 60 minutes in a vacuum, the silicon evaporation source 7
A silicon molecular beam is introduced from the gas introduction pipe 5.
Acetylene of 10 -3 Pa is simultaneously applied to the sapphire substrate 3 covered with the aluminum nitride single crystal film and its oxide layer to grow a silicon carbide single crystal film.
膜の成長速度は、シリコン分子線強度およびア
セチレン分圧に依存するが、1.7×1015/cm2・sec、
1×10-3Paの時、約3Å/secである。 The growth rate of the film depends on the silicon molecular beam intensity and acetylene partial pressure, but is 1.7×10 15 /cm 2 ·sec,
At 1×10 -3 Pa, it is approximately 3 Å/sec.
この方法により作製したサフアイア基板3上の
窒化アルミニウム単結晶膜とその酸化層上の炭化
硅素膜は、数μmの膜厚であつても、作製後サフ
アイア基板3の温度を室温とし、大気中に取り出
しても剥離することはなく、また、膜をこすつて
も剥れることはなかつた。 Even though the aluminum nitride single crystal film on the sapphire substrate 3 and the silicon carbide film on its oxide layer produced by this method have a film thickness of several μm, the temperature of the sapphire substrate 3 is kept at room temperature after production, and the film is exposed to the atmosphere. Even when the film was taken out, it did not peel off, and even when the film was rubbed, it did not come off.
さらに、反射電子線回析により作成した膜は、
双晶構造を含まないβ(あるいは3C)−炭化硅素
単結晶膜であることが判明した。 Furthermore, the film created by backscattered electron beam diffraction is
It turned out to be a β (or 3C)-silicon carbide single crystal film that does not contain a twin structure.
また、作成した膜は従来の方法による絶縁基板
上の膜より電気的に優れている。すなわち、サフ
アイア基板3上に直接成長させた繊維状構造およ
びサフアイア基板3上へ窒化アルミニウムを成長
させその上に成長させた膜は電子移動度が5〜6
cm2/V・secであるのに対し、この方法による膜
は、電子移動度が24cm2/V・secと大きな値を示
した。 In addition, the films produced are electrically superior to films on insulating substrates produced by conventional methods. That is, the fibrous structure grown directly on the sapphire substrate 3 and the film grown on aluminum nitride on the sapphire substrate 3 have an electron mobility of 5 to 6.
cm 2 /V·sec, whereas the film produced by this method showed a large electron mobility of 24 cm 2 /V·sec.
なお、この発明は上記の実施例に示される化成
蒸着法による方法に限定されるものではなく、全
ての成長過程を反応性イオンプレーテイング法や
気相成長法などいずれに従つてもよい。 Note that the present invention is not limited to the chemical vapor deposition method shown in the above embodiments, and the entire growth process may be performed by any method such as reactive ion plating method or vapor phase growth method.
以上説明したように、この発明はサフアイア基
板上に窒化アルミニウム単結晶膜を成長させ、こ
の窒化アルミニウム単結晶膜上にアルミニウム酸
化層を成長させ、前記アルミニウムの酸化層上に
炭化硅素を成長させたもので、絶縁性基板である
サフアイア基板上に、結晶性に優れた炭化硅素単
結晶膜を剥離することなく成長させることがで
き、炭化硅素を用いた電子素子等の諸種の応用に
その活用が期待できる利点を有するものである。
As explained above, the present invention grows an aluminum nitride single crystal film on a sapphire substrate, grows an aluminum oxide layer on the aluminum nitride single crystal film, and grows silicon carbide on the aluminum oxide layer. It is possible to grow a silicon carbide single crystal film with excellent crystallinity on an insulating sapphire substrate without peeling it off, and it can be used in various applications such as electronic devices using silicon carbide. It has promising advantages.
図面はこの発明を実施するための装置を示す構
成図である。
図中、1は真空槽、2は基板加熱ヒータ、3は
サフアイア基板、4はシヤツタ、5はアンモニア
ガスと酸素およびアセチレンガスの導入パイプ、
6はアルミニウム蒸発源、7はシリコン蒸発源、
8は排気口、9〜11は制御弁である。
The drawing is a block diagram showing an apparatus for carrying out the present invention. In the figure, 1 is a vacuum chamber, 2 is a substrate heater, 3 is a sapphire substrate, 4 is a shutter, 5 is an introduction pipe for ammonia gas, oxygen, and acetylene gas,
6 is an aluminum evaporation source, 7 is a silicon evaporation source,
8 is an exhaust port, and 9 to 11 are control valves.
Claims (1)
膜を成長させ、この窒化アルミニウム単結晶膜上
にアルミニウム酸化層を成長させ、前記アルミニ
ウムの酸化層上に炭化硅素を成長させることを特
徴とする炭化硅素単結晶膜の製造方法。1. A silicon carbide single crystal characterized by growing an aluminum nitride single crystal film on a sapphire substrate, growing an aluminum oxide layer on the aluminum nitride single crystal film, and growing silicon carbide on the aluminum oxide layer. Membrane manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59138569A JPS6117497A (en) | 1984-07-04 | 1984-07-04 | Production of single crystal film of silicon carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59138569A JPS6117497A (en) | 1984-07-04 | 1984-07-04 | Production of single crystal film of silicon carbide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6117497A JPS6117497A (en) | 1986-01-25 |
| JPH0143720B2 true JPH0143720B2 (en) | 1989-09-22 |
Family
ID=15225197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59138569A Granted JPS6117497A (en) | 1984-07-04 | 1984-07-04 | Production of single crystal film of silicon carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6117497A (en) |
-
1984
- 1984-07-04 JP JP59138569A patent/JPS6117497A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6117497A (en) | 1986-01-25 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |