JP4283478B2 - Method for growing SiC single crystal on electronic device substrate - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は、電子素子の基板上にＳｉＣ単結晶を成長させる方法に関するものである。
【０００２】
【従来の技術】
ＳｉＣは、広いバンドギャップ、高い電子移動度、高い耐熱性を持っており、構成元素の資源量が豊富でかつ環境汚染への懸念が小さい等の特徴を持つ化合物半導体として、ＳｉＣは、次世代電子素子、高速高温動作可能電子素子、太陽光発電素子等としての応用が期待される材料である。特にシリコン基板上に形成されたＳｉＣ薄膜は、現在のシリコンテクノロジーを継承できることから、産業技術の開発コストにおける優位性からも、実用化が求められる材料である。
【０００３】
ＳｉＣ薄膜の形成法としては、各種ＣＶＤ法、スパッタリング法、各種ＭＢＥ法等が知られている。
【０００４】
結晶性の良いＳｉＣ膜を得るためには、ＣＶＤ法では１２００℃以上の高温が必要であるといわれている。
【０００５】
スパッタリングやＭＢＥ法においては高真空雰囲気下での成長が必要である。
これはＳｉ−Ｃ間の結合が共有結合であるため、化学結合形成エネルギーおよびエピタキシャル結晶成長のための拡散エネルギーが、ともに大きなものになるためである。
【０００６】
【発明が解決しようとする課題】
１２００℃以下でのＣＶＤ法では、アモルファスＳｉＣとなる場合が多く、良好な結晶性を得るのが難しい。
【０００７】
ＳｉとＳｉＣの格子定数には約２０％の大きな格子不整合があるため、高品質の連続した膜を成長させることが極めて難しい。
【０００８】
本発明の目的は、１２００℃以下の温度で良好な結晶性を得ることができる、電子素子基板上へのＳｉＣ単結晶の成長方法を提供することである。
【０００９】
【課題を解決するための手段】
本発明の解決手段を例示すると、次のとおりである。
【００１０】
（１）電子素子の基板にＳｉＣ単結晶をＣＶＤ法を用いて成長させる方法において、ＳｉＣ単結晶を１２００℃以下の温度領域で複数の成長温度に分けて成長させ、かつ、中間層としてＳｉＣ単結晶を成長温度７８０〜９５０℃で厚みが５０〜７５０ｎｍになるまで成長させることを特徴とする電子素子基板上へのＳｉＣ単結晶の成長方法。
【００１１】
（２）ＳｉＣ単結晶がβ−ＳｉＣであることを特徴とする前述の電子素子基板上へのＳｉＣ単結晶の成長方法。
【００１３】
（３）所望の膜厚を確保するために中間層の成形後に成長温度１０００〜１２００℃でＳｉＣ単結晶を成長させることを特徴とする前述の電子素子基板上へのＳｉＣ単結晶の成長方法。
【００１４】
【発明の実施の形態】
本発明においては、１２００℃以下の温度で２種類以上の温度域に分けて、電子素子の基板にＳｉＣ単結晶をＣＶＤ法を用いて成長させる。とくに、ＳｉＣのエピタキシャル成長を行う際に、低温でバッファ層を形成し、そのあと、高温（ただし１２００℃以下）でＳｉＣ単結晶を形成する。そのことにより、ＭＯＣＶＤ（有機金属気相成長）で高品質のＳｉＣの単結晶を形成することができる。
【００１５】
まず、ＳｉＣ単結晶の成長法について説明する。
【００１６】
Ｓｉ基板上にＭＯＣＶＤ法を用いてβ−ＳｉＣ半導体結晶を成長させるときに、Ｓｉ基板上に第１のβ−ＳｉＣ結晶を比較的低温（たとえば７８０℃以上でかつ９５０℃以下）の成長温度で５０ｎｍから７５０ｎｍの膜厚になるまで形成する。その後、比較的高温（たとえば１０００〜１２００℃）で、第１のβ−ＳｉＣ結晶層（中間バッファ層）の上に第２のβ−ＳｉＣ結晶を成長させて、連続した膜を形成する。
【００１７】
Ｓｉ基板上に、すぐに高温で成長させようとしても、連続膜を得ることは極めて困難である。
【００１８】
本発明では、図１（ａ）〜（ｂ）に順に示すように、第１のＳｉＣ単結晶を比較的低温（７８０〜９５０℃）で成長させて、まず単結晶の連続膜をＳｉ基板上に形成し、次に、そのまま、その単結晶の連続膜（これが中間バッファ層として機能する）上に、成長温度を高めて、高温（１０００〜１２００℃）にして、第２のＳｉＣの単結晶を成長させて、連続膜を形成する。
【００１９】
このような本発明の中間バッファ層の低温成長方法は、従来のアモルファス状ＳｉＣのバッファ層の低温形成法とは相違している。
【００２０】
従来の方法では、アモルファス状ＳｉＣのバッファ層をＳｉ基板上に形成し、その上にＳｉＣ結晶を成長させるが、この低温成長バッファ層の構成と作用は、次の通りである。すなわち、Ｓｉ基板上に６００℃の低温で成長するＳｉＣ層は、アモルファス状であり、このアモルファス状の層が、ＳｉＣを成長させるために１２５０℃の温度まで昇温する際に、部分的に単結晶化する。この単結晶化した部分が、１２５０℃でＳｉＣを成長させる際に核となり、そこからＳｉＣ結晶が成長し、均一なＳｉＣ単結晶の層が成長する。中間バッファ層が無いときは、Ｓｉ基板においてこの核になる部分が極めて少なく、均一なＳｉＣ層を成長させることができない。
【００２１】
この結果従来の方法と、本発明のようにＳｉを基板としてＭＯＣＶＤ法で１２００℃以下の温度で少くとも２種類の成長温度に分けて単結晶のＳｉＣ膜を成長させる場合とを比較すると、以下の点で異なる。
【００２２】
従来方法では、最初に成長する膜がアモルファスＳｉＣ膜であるのに対し、本発明では、ＭＯＣＶＤ法により単結晶のＳｉＣ膜を基板上に成長させる。この点で両者は大きく異なる。本発明では、第２のＳｉＣ単結晶の層を完全に二次元成長化させることができるために、より表面性にすぐれて、しかも結晶性に優れた膜を成長させることができる。
【００２３】
【実施例】
本発明を明らかにするために、実施例を説明する。
【００２４】
実施例１
ＭＭＳ（モノメチルシランＳｉＨ3ＣＨ3）を原料とするＭＯＣＶＤ法を使用した。
【００２５】
図３（ａ）に示すように、まず、Ｓｉ基板の表面をケミカルエッチングして、Ｓｉ基板を基板ホルダーにのせ、反応管内の成長領域にセットした。ガス導入管からキャリアガスとして水素（Ｈ2）を供給しながら、Ｓｉ基板を１１００℃に 昇温して基板の表面のクリーニングをおこなった。その後、８３０℃まで基板表面の温度を下げ、安定したところで、ＭＭＳ：Ｈ2のガス流量比１：１００００ にてＳｉ基板表面のＳｉＣ成長領域にＭＭＳとキャリアガスを供給した。３０分間で約６７０ｎｍの膜厚の第１のＳｉＣ層が形成できた。つぎに、ＭＭＳの供給を止め、キャリアガスだけを供給しながら基板を１０５０℃まで昇温した。温度が１０５０℃に安定したところで、再びＭＭＳ：Ｈ2のガス流量比１：１０００ ０にてＭＭＳとＨ2ガスを供給して、第２のＳｉＣ層が形成された。このとき、 第２のＳｉＣ層は３０分間の成長で１１μｍの膜厚が得られた。成長した第２のＳｉＣ層の表面は、非常に平坦であった。
【００２６】
このようにして得られたＳｉ（１００）基板上の第１及び第２のＳｉＣ層について、Ｘ線回折によりその結晶性を調べた結果、β−ＳｉＣ（２００）面の単結晶からなる連続した膜が得られた。また、Ｘ線回折の結果によれば、この実施例１による方法で形成した第２のＳｉＣ膜は、非常にシャープなピークが検出され、結晶性が大幅に向上したことが確認できた。
【００２７】
比較例
実際にＤＣＳ（ジクロロシランＳｉＨ2Ｃｌ2）、プロパンＣ3Ｈ8を原料とするハイドライド法を用いて１０５０℃でＳｉ（１００）基板上にＳｉＣの成長をおこなったところ、図２に示すように、表面の凹凸が顕著となり、平坦な表面を有するＳｉＣ膜を得ることができなかった。また、得られた結晶のＸ線回折の結果、多結晶ＳｉＣが成長していた。
【００２８】
【発明の効果】
以上のように、本発明によれば、ＭＯＣＶＤ法を用いて基板上に結晶性にすぐれた高品質の半導体結晶を得ることができる。これは、１２００℃以下の温度において、複数の成長温度に分けたことによる効果である。たとえば、９５０℃以下の低温成長で、まず平坦性に優れた単結晶を成長させ、その後、昇温して比較的高温（ただし１２００℃以下の温度）で単結晶の成長速度を上げることにより、高品質の単結晶を基板上に得ることができる。
【図面の簡単な説明】
【図１】 本発明方法を示す概念図。
【図２】 従来方法を示す概念図。
【図３】 本発明の１つの実施例による単結晶成長方法の一例を概念的に示す。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for growing a SiC single crystal on a substrate of an electronic device.
[0002]
[Prior art]
SiC is a compound semiconductor with features such as a wide band gap, high electron mobility, high heat resistance, abundant amounts of constituent elements, and low concern about environmental pollution. It is a material expected to be applied as an electronic element, an electronic element capable of high-speed and high-temperature operation, a solar power generation element, and the like. In particular, an SiC thin film formed on a silicon substrate is a material that is required to be put into practical use because of its superiority in industrial technology development costs because it can inherit the current silicon technology.
[0003]
As a method for forming a SiC thin film, various CVD methods, sputtering methods, various MBE methods and the like are known.
[0004]
In order to obtain a SiC film having good crystallinity, it is said that a high temperature of 1200 ° C. or higher is necessary in the CVD method.
[0005]
In sputtering and MBE, growth in a high vacuum atmosphere is necessary.
This is because the bond between Si—C is a covalent bond, so that the chemical bond formation energy and the diffusion energy for epitaxial crystal growth are both large.
[0006]
[Problems to be solved by the invention]
In the CVD method at 1200 ° C. or lower, amorphous SiC is often obtained, and it is difficult to obtain good crystallinity.
[0007]
Since the lattice constants of Si and SiC have a large lattice mismatch of about 20%, it is extremely difficult to grow a high quality continuous film.
[0008]
An object of the present invention is to provide a method for growing a SiC single crystal on an electronic device substrate, which can obtain good crystallinity at a temperature of 1200 ° C. or lower.
[0009]
[Means for Solving the Problems]
Examples of the solving means of the present invention are as follows.
[0010]
(1) In a method of growing a SiC single crystal on a substrate of an electronic device using a CVD method, the SiC single crystal is grown at a plurality of growth temperatures in a temperature range of 1200 ° C. or lower, and an SiC single crystal is used as an intermediate layer. A method for growing a SiC single crystal on an electronic device substrate, wherein the crystal is grown at a growth temperature of 780 to 950 ° C. until the thickness reaches 50 to 750 nm .
[0011]
(2) The method for growing a SiC single crystal on the electronic device substrate described above, wherein the SiC single crystal is β-SiC.
[0013]
( 3 ) The SiC single crystal growth method on the electronic element substrate described above, wherein the SiC single crystal is grown at a growth temperature of 1000 to 1200 ° C. after forming the intermediate layer in order to ensure a desired film thickness.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
In the present invention, a SiC single crystal is grown on a substrate of an electronic device by using a CVD method at a temperature of 1200 ° C. or lower and divided into two or more temperature ranges. In particular, when performing epitaxial growth of SiC, a buffer layer is formed at a low temperature, and thereafter, a SiC single crystal is formed at a high temperature (but 1200 ° C. or less). Thereby, a high-quality SiC single crystal can be formed by MOCVD (metal organic chemical vapor deposition).
[0015]
First, a method for growing a SiC single crystal will be described.
[0016]
When the β-SiC semiconductor crystal is grown on the Si substrate by using the MOCVD method, the first β-SiC crystal is grown on the Si substrate at a relatively low growth temperature (for example, 780 ° C. or more and 950 ° C. or less). The film is formed until the film thickness is 50 nm to 750 nm. Thereafter, a second β-SiC crystal is grown on the first β-SiC crystal layer (intermediate buffer layer) at a relatively high temperature (for example, 1000 to 1200 ° C.) to form a continuous film.
[0017]
It is extremely difficult to obtain a continuous film on a Si substrate even if it is immediately grown at a high temperature.
[0018]
In the present invention, as shown in FIGS. 1A to 1B in order, the first SiC single crystal is grown at a relatively low temperature (780 to 950 ° C.), and a single-crystal continuous film is first formed on the Si substrate. Next, the second SiC single crystal is formed on the continuous single crystal film (which functions as an intermediate buffer layer) by raising the growth temperature to a high temperature (1000 to 1200 ° C.). To form a continuous film.
[0019]
Such a low temperature growth method of the intermediate buffer layer of the present invention is different from the conventional low temperature formation method of the buffer layer of amorphous SiC.
[0020]
In the conventional method, an amorphous SiC buffer layer is formed on a Si substrate and a SiC crystal is grown thereon. The configuration and action of this low-temperature growth buffer layer are as follows. That is, the SiC layer grown on the Si substrate at a low temperature of 600 ° C. is amorphous, and when this amorphous layer is heated up to a temperature of 1250 ° C. in order to grow SiC, it is partially isolated. Crystallize. This single crystal portion becomes a nucleus when SiC is grown at 1250 ° C., from which a SiC crystal grows and a uniform SiC single crystal layer grows. When there is no intermediate buffer layer, there are very few core parts on the Si substrate, and a uniform SiC layer cannot be grown.
[0021]
As a result, a comparison between the conventional method and the case where a single crystal SiC film is grown at a temperature of 1200 ° C. or less at a temperature of 1200 ° C. or less and at least two types of growth temperatures using Si as a substrate as in the present invention is as follows. Is different.
[0022]
In the conventional method, the first grown film is an amorphous SiC film, whereas in the present invention, a single crystal SiC film is grown on the substrate by MOCVD. The two are very different in this respect. In the present invention, since the second SiC single crystal layer can be completely two-dimensionally grown, a film having better surface properties and excellent crystallinity can be grown.
[0023]
【Example】
In order to clarify the present invention, examples will be described.
[0024]
Example 1
The MOCVD method using MMS (monomethylsilane SiH 3 CH 3 ) as a raw material was used.
[0025]
As shown in FIG. 3A, first, the surface of the Si substrate was chemically etched, and the Si substrate was placed on a substrate holder and set in a growth region in the reaction tube. While supplying hydrogen (H 2 ) as a carrier gas from the gas introduction pipe, the temperature of the Si substrate was raised to 1100 ° C. to clean the surface of the substrate. Thereafter, the temperature of the substrate surface was lowered to 830 ° C., and when stabilized, MMS and carrier gas were supplied to the SiC growth region on the Si substrate surface at a gas flow ratio of 1: 10000 of MMS: H 2 . A first SiC layer having a thickness of about 670 nm was formed in 30 minutes. Next, the supply of MMS was stopped, and the substrate was heated to 1050 ° C. while supplying only the carrier gas. When the temperature was stabilized at 1050 ° C., MMS and H 2 gas were supplied again at an MMS: H 2 gas flow ratio of 1: 1000 to form a second SiC layer. At this time, the second SiC layer had a thickness of 11 μm after 30 minutes of growth. The surface of the grown second SiC layer was very flat.
[0026]
As a result of examining the crystallinity of the first and second SiC layers on the Si (100) substrate thus obtained by X-ray diffraction, a continuous crystal composed of a single crystal of β-SiC (200) plane was obtained. A membrane was obtained. Further, according to the result of X-ray diffraction, it was confirmed that the second SiC film formed by the method according to Example 1 had a very sharp peak and the crystallinity was greatly improved.
[0027]
Comparative Example When SiC was actually grown on a Si (100) substrate at 1050 ° C. using a hydride method using DCS (dichlorosilane SiH 2 Cl 2 ) and propane C 3 H 8 as raw materials, it is shown in FIG. As described above, the unevenness of the surface became remarkable, and an SiC film having a flat surface could not be obtained. Further, as a result of X-ray diffraction of the obtained crystal, polycrystalline SiC was grown.
[0028]
【The invention's effect】
As described above, according to the present invention, a high-quality semiconductor crystal having excellent crystallinity can be obtained on a substrate using the MOCVD method. This is an effect obtained by dividing the growth temperature into a plurality of growth temperatures at a temperature of 1200 ° C. or lower. For example, by growing a single crystal excellent in flatness at a low temperature growth of 950 ° C. or lower, and then raising the temperature to increase the growth rate of the single crystal at a relatively high temperature (temperature of 1200 ° C. or lower), A high quality single crystal can be obtained on a substrate.
[Brief description of the drawings]
FIG. 1 is a conceptual diagram showing a method of the present invention.
FIG. 2 is a conceptual diagram showing a conventional method.
FIG. 3 conceptually illustrates an example of a single crystal growth method according to one embodiment of the present invention.
Claims (3)
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| JP2002018257A JP4283478B2 (en) | 2002-01-28 | 2002-01-28 | Method for growing SiC single crystal on electronic device substrate |
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| JP2002018257A JP4283478B2 (en) | 2002-01-28 | 2002-01-28 | Method for growing SiC single crystal on electronic device substrate |
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| JP4283478B2 true JP4283478B2 (en) | 2009-06-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006253617A (en) * | 2005-02-14 | 2006-09-21 | Toshiba Ceramics Co Ltd | SiC SEMICONDUCTOR AND ITS MANUFACTURING METHOD |
| JP2009007205A (en) * | 2007-06-28 | 2009-01-15 | Sumitomo Electric Ind Ltd | Method for manufacturing substrate product |
| JP5693946B2 (en) | 2010-03-29 | 2015-04-01 | エア・ウォーター株式会社 | Method for producing single crystal 3C-SiC substrate |
| JP4850960B2 (en) | 2010-04-07 | 2012-01-11 | 新日本製鐵株式会社 | Epitaxial silicon carbide single crystal substrate manufacturing method |
| JP5353800B2 (en) * | 2010-04-07 | 2013-11-27 | 新日鐵住金株式会社 | Method for manufacturing silicon carbide epitaxial film |
| JP2018101721A (en) * | 2016-12-21 | 2018-06-28 | 株式会社ニューフレアテクノロジー | Vapor growth method |
| JP7259906B2 (en) * | 2021-09-21 | 2023-04-18 | 信越半導体株式会社 | Manufacturing method of heteroepitaxial wafer |
| WO2023079880A1 (en) * | 2021-11-08 | 2023-05-11 | 信越半導体株式会社 | Method for producing heteroepitaxial wafer |
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