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JPH0777203B2 - Method for manufacturing sapphire substrate having silicon single crystal film - Google Patents
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JPH0777203B2 - Method for manufacturing sapphire substrate having silicon single crystal film - Google Patents

Method for manufacturing sapphire substrate having silicon single crystal film

Info

Publication number
JPH0777203B2
JPH0777203B2 JP62071362A JP7136287A JPH0777203B2 JP H0777203 B2 JPH0777203 B2 JP H0777203B2 JP 62071362 A JP62071362 A JP 62071362A JP 7136287 A JP7136287 A JP 7136287A JP H0777203 B2 JPH0777203 B2 JP H0777203B2
Authority
JP
Japan
Prior art keywords
single crystal
silicon single
crystal film
sapphire substrate
silicon
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 - Lifetime
Application number
JP62071362A
Other languages
Japanese (ja)
Other versions
JPS63239812A (en
Inventor
誠 石田
哲郎 中村
勝可 原田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toagosei Co Ltd
Original Assignee
Toagosei Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Toagosei Co Ltd filed Critical Toagosei Co Ltd
Priority to JP62071362A priority Critical patent/JPH0777203B2/en
Publication of JPS63239812A publication Critical patent/JPS63239812A/en
Publication of JPH0777203B2 publication Critical patent/JPH0777203B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Description

【発明の詳細な説明】 イ)発明の目的 〔産業上の利用分野〕 本発明はIC、VLSI等のデバイス等に有用な、シリコン単
結晶膜を有するサファイア基板の製造方法に関するもの
である。
DETAILED DESCRIPTION OF THE INVENTION (a) Purpose of the invention [Industrial field of application] The present invention relates to a method for producing a sapphire substrate having a silicon single crystal film, which is useful for devices such as IC and VLSI.

〔従来の技術〕 従来、結晶格子定数がシリコンに近いサファイア基板上
に、シリコンを気相成長させることにより、シリコン単
結晶膜を形成させる方法はよく知られている。
[Prior Art] Conventionally, a method of forming a silicon single crystal film by vapor-phase growing silicon on a sapphire substrate having a crystal lattice constant close to that of silicon is well known.

しかしながら、この従来法で得られたシリコン単結晶膜
は、 単結晶が完全でない 結晶欠陥が多い 例えばサファイア基板等から浮遊するアルミニウム等
の混入がある 等の問題があり、良質のシリコン単結晶膜を得ることは
困難であった。
However, the silicon single crystal film obtained by this conventional method has a problem that the single crystal is not perfect and has many crystal defects, for example, aluminum floating from a sapphire substrate or the like is mixed. It was difficult to get.

このような問題を解決する為に、シリコンを、速い膜成
長速度、例えば2μm/分以上で気相成長させる方法、ま
た初め速く次いで遅い成長速度で気相成長させる方法、
さらに初期の気相成長素度を比較的遅くして下地膜を成
長させ、引き続き比較的速い成長速度で気相成長させる
方法、あるいは多結晶または非晶質のシリコン膜を基板
の上に所定の厚さだけ付着した後、単結晶膜を気相成長
させる方法等が試みられているが、前記の問題点を解決
するまでには至っていなかった。
In order to solve such a problem, a method of vapor-depositing silicon at a high film growth rate, for example, 2 μm / min or more, and a method of first vapor-depositing silicon at a fast and then a slow growth rate,
Further, a method of growing the underlying film while making the initial vapor phase growth rate relatively slow, and then performing vapor phase growth at a relatively high growth rate, or by depositing a polycrystalline or amorphous silicon film on the substrate in a predetermined manner. Although a method of vapor-depositing a single crystal film after depositing it by a thickness has been attempted, it has not been possible to solve the above problems.

またサファイア基板上へ気相成長させるシリコンの原料
としては、以前は四塩化珪素が用いられていたが、最近
は主にモノシランが使用されている。この理由として
は、四塩化珪素よりモノシランの法が、より低い温度で
シリコンを気相成長させることが可能であり、たとえば
サファイア基板中のアルミニウムがシリコン成長層中へ
オートドーピングやオートデイヒュージョンせず、より
良質なシリコン単結晶膜が得られるためと言われてい
る。
Further, silicon tetrachloride has been used as a raw material of silicon for vapor phase growth on a sapphire substrate, but recently, monosilane has been mainly used. The reason for this is that the method of monosilane rather than silicon tetrachloride allows vapor phase growth of silicon at a lower temperature, for example, aluminum in a sapphire substrate does not undergo autodoping or autodiffusion in the silicon growth layer. It is said that a higher quality silicon single crystal film can be obtained.

しかしながらモノシランを用いる方法によっても、上記
したような問題を完全に解決したシリコン単結晶膜を得
ることは出来ず、実用上さらに改良することが望まれて
いる。
However, even with the method using monosilane, it is not possible to obtain a silicon single crystal film that completely solves the above-mentioned problems, and further improvement in practical use is desired.

〔発明が解決しようとする問題〕[Problems to be solved by the invention]

本発明者らは、シリコン単結晶膜の結晶が完全で、結晶
欠陥がなく、生産効率に優れ、かつ各種のIC、VLSI等の
デバイスに適用しうるシリコン単結晶膜を有するサファ
イアの製造方法につき鋭意研究した結果、本発明を完成
した。
The inventors of the present invention are concerned with a method for producing sapphire having a silicon single crystal film having a perfect crystal, no crystal defects, excellent production efficiency, and applicable to various ICs, VLSIs, and other devices. As a result of intensive research, the present invention has been completed.

ロ)発明の構成 〔問題点を解決する手段〕 本発明は、熱CVD法による気相成長法でシリコン単結晶
膜を有するサファイア基板を製造するにあたり、ジシラ
ンを0.001vol%〜10vol%含有する希釈ガスを原料とし
て用い、気相成長温度を500℃〜1,300℃とし、かつシリ
コン単結晶膜の成長速度を0.001μm/min〜10μm/minと
することを特徴とするシリコン単結晶膜を有するサファ
イア基板の製造方法である。
(B) Configuration of the invention [Means for solving the problem] The present invention is a dilution containing 0.001 vol% to 10 vol% of disilane in producing a sapphire substrate having a silicon single crystal film by a vapor phase growth method by a thermal CVD method. A sapphire substrate having a silicon single crystal film characterized by using a gas as a raw material, a vapor growth temperature of 500 ° C to 1,300 ° C, and a growth rate of the silicon single crystal film of 0.001 μm / min to 10 μm / min Is a manufacturing method.

本発明においてシリコン単結晶膜を形成すべきサファイ
ア基板としては、特に限定されるものではないが、たと
えば(012)面、(114)面、(0001)面等の面方
位のものが好ましい。
In the present invention, the sapphire substrate on which the silicon single crystal film is to be formed is not particularly limited, but for example, those having a plane orientation such as (012) plane, (114) plane and (0001) plane are preferable.

本発明におけるジシラン(Si2H6)は高純度のものが望
ましい。ジシランを反応系へ供給する場合は、希釈ガス
と共に供給する。希釈ガスとしては、通常、水素、不活
性ガスが上げられ、好ましくは水素、ヘリウムである。
希釈ガスはいずれも精製したものを用いるのがよく、例
えば水素はパラジウム膜透過精製、モレキュラーシーブ
による吸着精製したものを用いればよい。
The disilane (Si 2 H 6 ) in the present invention is preferably highly pure. When disilane is supplied to the reaction system, it is supplied together with the diluent gas. As the diluting gas, hydrogen or an inert gas is usually used, and hydrogen or helium is preferable.
It is preferable to use purified gas as the diluent gas. For example, hydrogen gas may be used after being purified by permeation through a palladium membrane or adsorbed and purified by a molecular sieve.

ジシランと希釈ガスを反応系に供給する場合、別々に供
給してもよいが、両者が充分に混合されているのがより
望ましく、例えば混合器を用いて供給する方法が挙げら
れる。
When the disilane and the diluent gas are supplied to the reaction system, they may be supplied separately, but it is more preferable that both are sufficiently mixed. For example, a method using a mixer may be used.

ジシランと希釈ガスの反応系への供給割合は、ジシラン
と希釈ガスの合計量基準で、ジシランが0.001Vol%〜10
Vol%である。0.001Vol%未満ではジシランの成長速度
が遅くなり過ぎ実用的でなくなる恐れがあり、10Vol%
を越えると、反応器壁への堆積、あるいは気相中での核
成長によるジシランのロスが大きくなるのみならず、精
製した微粉がシリコン膜に入り結晶欠陥の原因となる恐
れがある。
The supply ratio of disilane and diluent gas to the reaction system is 0.001 Vol% to 10% of disilane based on the total amount of disilane and diluent gas.
Vol%. If it is less than 0.001 Vol%, the growth rate of disilane may be too slow and may be impractical.
If it exceeds, not only the loss of disilane due to the deposition on the reactor wall or the nucleus growth in the vapor phase becomes large, but also the refined fine powder may enter the silicon film and cause a crystal defect.

ジシランを分解してシリコン単結晶を気相成長させる手
段としては、熱CVDを適用する。
Thermal CVD is applied as a means for decomposing disilane to vapor-deposit a silicon single crystal.

熱CVDを行うための加熱手段としては、高周波加熱、赤
外線ランプによる加熱等を用いればよいが、低温成長を
行えるという利点を生かして、抵抗加熱を用いてもよ
い。
As a heating means for performing thermal CVD, high frequency heating, heating by an infrared lamp, or the like may be used, but resistance heating may be used by taking advantage of low temperature growth.

気相成長温度は1300℃〜500℃であり、更に好ましくは9
00℃〜600℃である。500℃未満ではシリコン単結晶膜の
成長速度が非常に小さくなり、成長に要する時間が長く
なるため実用的であるとは言えず、また結晶欠陥が増大
したり多結晶になる恐れがあり電気的特性の悪化につな
がる可能性がある。1300℃を越えるとシリコン単結晶膜
へのアルミニウムの混入が促進され、電気的特性が悪く
なる可能性の他、基板上へのシリコン単結晶膜の堆積
後、室温に戻すとシリコン単結晶膜と基板との界面に応
力が生じ、電気特性への劣化につながる可能性がある。
The vapor growth temperature is 1300 ° C to 500 ° C, more preferably 9
The temperature is 00 ° C to 600 ° C. If the temperature is lower than 500 ° C, the growth rate of the silicon single crystal film becomes very small, and the time required for the growth becomes long, so it cannot be said to be practical, and there is a possibility that crystal defects may increase or polycrystal may occur. It may lead to deterioration of characteristics. If the temperature exceeds 1300 ° C, aluminum may be mixed into the silicon single crystal film, and the electrical characteristics may deteriorate.In addition, after the silicon single crystal film is deposited on the substrate, if it is returned to room temperature, it becomes a silicon single crystal film. Stress is generated at the interface with the substrate, which may lead to deterioration in electrical characteristics.

シリコン単結晶膜の成長速度は0.001μm/min〜10μm/mi
nである。0.001μm/min未満では成長が遅すぎて実用的
であるとは言えず、10μm/minを越えると完全な単結晶
を得がたくなる。
Growth rate of silicon single crystal film is 0.001μm / min ~ 10μm / mi
n. If it is less than 0.001 μm / min, the growth is too slow to be considered practical, and if it exceeds 10 μm / min, it becomes difficult to obtain a complete single crystal.

反応器は縦型、横型、バレル型等が挙げられるが、特に
その形状を問うものではない。
The reactor may be a vertical type, a horizontal type, a barrel type, or the like, but the shape thereof is not particularly limited.

圧力は常圧でも、減圧、加圧下でも行えるが、好ましく
は5Torr〜900Torrである。5Torr未満ではシリコン単結
晶膜の成長速度が遅くなり過ぎ、900Torrを越えると反
応器の選択範囲が限定される恐れがあるため好ましいと
は言えない。
The pressure may be normal pressure, reduced pressure or increased pressure, but is preferably 5 Torr to 900 Torr. If it is less than 5 Torr, the growth rate of the silicon single crystal film becomes too slow, and if it exceeds 900 Torr, the selection range of the reactor may be limited, which is not preferable.

本発明においてサファイア基板上に形成させるべきシリ
コン単結晶膜の厚さは、使用目的に応じて適宜定めれば
よい。
In the present invention, the thickness of the silicon single crystal film to be formed on the sapphire substrate may be appropriately determined according to the purpose of use.

また本発明方法におけるその他の操作方法及び操作条件
などは、気相成長の技術分野において知られているとこ
ろに従えば足りる。
Further, other operating methods and operating conditions in the method of the present invention may be in accordance with those known in the technical field of vapor phase growth.

〔実施例および比較例〕[Examples and Comparative Examples]

以下に実施例および比較例を示して本発明をさらに具体
的に説明する。
Hereinafter, the present invention will be described more specifically with reference to Examples and Comparative Examples.

実施例1 第1図に示した如き装置を用いてサファイア基板上にシ
リコン単結晶膜を形成させた。すなわち高周波加熱タイ
プの縦型石英製反応管8内のSiCコートしたグラファイ
ト製サセプター(回転数5rpm)7上に、苛性カリ水溶液
で超音波洗浄し、脱イオン水で充分洗浄、乾燥した、厚
さが0.4mm、大きさが2インチの鏡面研磨したサファイ
ア基板(012)6を載置した。
Example 1 A silicon single crystal film was formed on a sapphire substrate using the apparatus as shown in FIG. That is, on a SiC-coated graphite susceptor (rotation speed 5 rpm) 7 in a vertical quartz reaction tube 8 of high-frequency heating type, ultrasonic cleaning was performed with a caustic potash solution, thoroughly washed with deionized water, and dried. A mirror-polished sapphire substrate (012) 6 having a size of 0.4 mm and a size of 2 inches was placed.

水素精製装置2により精製した水素1を反応管8に1
/分で流しながら、高周波加熱用コイル5により、サフ
ァイア基板6の温度を室温から900℃まで5分間で上昇
させ、同温度で10分間保った。
1 of hydrogen 1 purified by the hydrogen purifier 2 is fed to the reaction tube 8.
The temperature of the sapphire substrate 6 was raised from room temperature to 900 ° C. in 5 minutes by the high-frequency heating coil 5 while flowing at a flow rate of 10 minutes / minute, and kept at the same temperature for 10 minutes.

その後同温度を保ち、マスフロメーター4により流量を
調節しながら、5Vol%のジシランを含有する水素3を5c
c/分の流量で、また水素1を1/分の流量で、導入管
10より反応管8に流し、3分間シリコン単結晶を気相成
長させた。
Then, while maintaining the same temperature, while adjusting the flow rate with the mass flow meter 4, 5 c of hydrogen 3 containing 5 vol% of disilane was added.
Introducing tube at a flow rate of c / min and hydrogen 1 / min
It was made to flow into the reaction tube 8 from 10, and the silicon single crystal was vapor-phase grown for 3 minutes.

反応管8の下部にはターボ分子ポンプ11、回転式真空ポ
ンプ12が接続され、これにより未反応ガス、希釈ガスを
排気した。
A turbo molecular pump 11 and a rotary vacuum pump 12 are connected to the lower part of the reaction tube 8 to exhaust unreacted gas and diluted gas.

堆積したシリコン単結晶膜9の膜厚は0.3μmであり、
成長速度は0.10μm/分であった。
The thickness of the deposited silicon single crystal film 9 is 0.3 μm,
The growth rate was 0.10 μm / min.

このシリコン単結晶膜を電子線回折法により調べた結
果、菊池線がみられ、完全な単結晶である判った。また
エッチングにより結晶欠陥を調べたところ、エッチピッ
ト、スタッフキングフォールト等は殆ど見られず良質な
結晶であった。また膜の比抵抗は280Ω−cmであった。
As a result of examining this silicon single crystal film by an electron diffraction method, the Kikuchi line was observed, and it was found that the film was a perfect single crystal. Further, when crystal defects were examined by etching, it was found that etch pits, stuffing faults, etc. were hardly seen and the crystals were of good quality. The specific resistance of the film was 280 Ω-cm.

次いで、このサファイア基板上のシリコン単結晶膜を用
いてMOS型FETを試作し、電子易動度を測定したところ60
0cm2/V−secであった。
Next, using a silicon single crystal film on this sapphire substrate, we prototyped a MOS-type FET and measured its electron mobility.
It was 0 cm 2 / V-sec.

実施例2 サファイア基板の温度を850℃にした以外は実施例1と
同情の方法でシリコン単結晶膜を製造した。得られた膜
は菊池線がみられ完全な単結晶であることが判った。
Example 2 A silicon single crystal film was produced in the same manner as in Example 1 except that the temperature of the sapphire substrate was set to 850 ° C. The Kikuchi line was observed in the obtained film, which revealed that it was a perfect single crystal.

比較例1 モノシランを原料とした以外は実施例2と同様の方法で
シリコン単結晶膜を製造したが、多結晶となった。
Comparative Example 1 A silicon single crystal film was produced in the same manner as in Example 2 except that monosilane was used as a raw material, but it became polycrystalline.

ハ)発明の効果 本発明によれば、低温でサファイア基板上にシリコン単
結晶膜を製造することが出来、従来では実現出来なかっ
た、完全で殆ど結晶欠陥がない、電気的特性にすぐれ
た、各種のIC、VSLI等のデバイス等に有用されるシリコ
ン単結晶膜を有するサファイア基板を、優れた生産効率
で製造することが可能である。
C) Effect of the Invention According to the present invention, it is possible to manufacture a silicon single crystal film on a sapphire substrate at a low temperature, which has not been realized in the past, is complete and has almost no crystal defects, and has excellent electrical characteristics. It is possible to manufacture a sapphire substrate having a silicon single crystal film useful for various ICs, devices such as VSLI, etc., with excellent production efficiency.

【図面の簡単な説明】[Brief description of drawings]

第1図は本発明方法を行う適した気相成長装置の一例を
示す概略図である。 1……水素 3……ジシランを含有する水素 5……高周波加熱用コイル 6……サファイア基板 7……サセプター 8……反応管 9……シリコン単結晶膜 10……導入管
FIG. 1 is a schematic view showing an example of a suitable vapor phase growth apparatus for carrying out the method of the present invention. 1 ... Hydrogen 3 ... Hydrogen containing disilane 5 ... High frequency heating coil 6 ... Sapphire substrate 7 ... Susceptor 8 ... Reaction tube 9 ... Silicon single crystal film 10 ... Introduction tube

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】熱CVD法による気相成長法でシリコン単結
晶膜を有するサファイア基板を製造するにあたり、ジシ
ランを0.001vol%〜10vol%含有する希釈ガスを原料と
して用い、気相成長温度を500℃〜1,300℃とし、かつシ
リコン単結晶膜の成長速度を0.001μm/min〜10μm/min
とすることを特徴とするシリコン単結晶膜を有するサフ
ァイア基板の製造方法。
1. When manufacturing a sapphire substrate having a silicon single crystal film by a vapor phase growth method by a thermal CVD method, a diluting gas containing 0.001 vol% to 10 vol% of disilane is used as a raw material, and a vapor phase growth temperature is 500. ℃ ~ 1,300 ℃, and the growth rate of the silicon single crystal film 0.001μm / min ~ 10μm / min
And a method for manufacturing a sapphire substrate having a silicon single crystal film.
JP62071362A 1987-03-27 1987-03-27 Method for manufacturing sapphire substrate having silicon single crystal film Expired - Lifetime JPH0777203B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62071362A JPH0777203B2 (en) 1987-03-27 1987-03-27 Method for manufacturing sapphire substrate having silicon single crystal film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62071362A JPH0777203B2 (en) 1987-03-27 1987-03-27 Method for manufacturing sapphire substrate having silicon single crystal film

Publications (2)

Publication Number Publication Date
JPS63239812A JPS63239812A (en) 1988-10-05
JPH0777203B2 true JPH0777203B2 (en) 1995-08-16

Family

ID=13458311

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62071362A Expired - Lifetime JPH0777203B2 (en) 1987-03-27 1987-03-27 Method for manufacturing sapphire substrate having silicon single crystal film

Country Status (1)

Country Link
JP (1) JPH0777203B2 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0816040B2 (en) * 1988-03-07 1996-02-21 日本電気株式会社 Molecular beam growth method for silicon
US5221412A (en) * 1989-09-26 1993-06-22 Toagosei Chemical Industry Co., Ltd. Vapor-phase epitaxial growth process by a hydrogen pretreatment step followed by decomposition of disilane to form monocrystalline Si film

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6193617A (en) * 1984-10-15 1986-05-12 Matsushita Electric Ind Co Ltd Manufacture of silicon film
JP2609844B2 (en) * 1985-06-10 1997-05-14 三洋電機株式会社 Epitaxy growth method
JPH0758692B2 (en) * 1986-01-07 1995-06-21 富士通株式会社 Method for manufacturing semiconductor device

Also Published As

Publication number Publication date
JPS63239812A (en) 1988-10-05

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