JP5024886B2 - Planarization processing method and crystal growth method - Google Patents
Planarization processing method and crystal growth method Download PDFInfo
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- 238000002109 crystal growth method Methods 0.000 title claims description 8
- 238000003672 processing method Methods 0.000 title claims description 3
- 239000000758 substrate Substances 0.000 claims description 97
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 38
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 229930195733 hydrocarbon Natural products 0.000 claims description 24
- 150000002430 hydrocarbons Chemical class 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- 229910002804 graphite Inorganic materials 0.000 claims description 19
- 239000010439 graphite Substances 0.000 claims description 19
- 239000004215 Carbon black (E152) Substances 0.000 claims description 18
- 239000010409 thin film Substances 0.000 claims description 15
- 239000011810 insulating material Substances 0.000 claims description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 134
- 229910010271 silicon carbide Inorganic materials 0.000 description 134
- 238000010438 heat treatment Methods 0.000 description 21
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 18
- 239000010408 film Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 229910003465 moissanite Inorganic materials 0.000 description 10
- 238000005530 etching Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 230000003746 surface roughness Effects 0.000 description 5
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000002123 temporal effect Effects 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- -1 For example Chemical compound 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
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Description
この発明は、ＳｉＣ基板（ＳｉＣウェハーということもある）表面の平坦化処理方法およびＳｉＣエピタキシャル結晶成長法に関し、さらに詳しくはカーボンの供給を抑えた反応室内条件下に、特定の条件で前処理した後、水素ガス雰囲気下にＳｉＣ基板表面をエッチングすることによってＳｉドロップレットが抑制されて平滑な表面が得られるＳｉＣ基板表面の平坦化処理方法およびＳｉＣエピタキシャル結晶成長法に関する。 The present invention relates to a method for planarizing a surface of a SiC substrate (sometimes referred to as a SiC wafer) and a SiC epitaxial crystal growth method , and more particularly, pre-treatment is performed under specific conditions under reaction chamber conditions in which carbon supply is suppressed. Then, the present invention relates to a method for planarizing a SiC substrate surface and a SiC epitaxial crystal growth method in which a Si droplet is suppressed by etching the SiC substrate surface in a hydrogen gas atmosphere to obtain a smooth surface.
近年、エレクトロニクス分野における低損失化や小型化の実現に向けて、従来のＳｉ半導体に比べて高い電気変換効率および高い熱伝導率などによって大幅な性能向上が期待できるＳｉＣ単結晶半導体がパワー半導体デバイス材料として有望視されている。このＳｉＣ単結晶半導体はＣＶＤ（Chemical Vapor Deposition）装置などの製膜装置を用いて半導体基板上へのエピタキシャル薄膜の形成によって得られる。
このＣＶＤ装置によれば、サセプタおよび断熱材を備えた反応室に原料ガスをキャリアガスとともに供給してＳｉＣ基板にＳｉＣ単結晶薄膜をエピタキシャル結晶成長させることができる。
In recent years, SiC single crystal semiconductors that can be expected to significantly improve performance due to high electrical conversion efficiency and high thermal conductivity compared to conventional Si semiconductors are becoming power semiconductor devices in order to achieve low loss and miniaturization in the electronics field. Promising as a material. This SiC single crystal semiconductor is obtained by forming an epitaxial thin film on a semiconductor substrate using a film forming apparatus such as a CVD (Chemical Vapor Deposition) apparatus.
According to this CVD apparatus, an SiC single crystal thin film can be epitaxially grown on an SiC substrate by supplying a source gas together with a carrier gas to a reaction chamber equipped with a susceptor and a heat insulating material.
しかし、一般的なグラファイトサセプタやグラファイト断熱材などを備えた製膜装置を使用してエピタキシャル結晶成長させると、この製膜装置を起源とするハイドロカーボン・不純物の発生があり、その発生量や種類の制御が難しく、ＳｉＣ単結晶の成長条件の精密な制御が困難である。
このため、サセプタとしてＳｉＣを用いるかサセプタ表面をＳｉＣでコートしたＳｉＣコートグラファイトを用いるなどのカーボンの供給を抑えた反応室内条件下にＳｉＣ基板上にＳｉＣ単結晶をエピタキシャル成長させる技術が検討されている。
However, when epitaxial film growth is performed using a film-forming device equipped with a general graphite susceptor or graphite heat insulating material, hydrocarbons and impurities are generated from this film-forming device. Is difficult to control, and it is difficult to precisely control the growth conditions of the SiC single crystal.
For this reason, a technique for epitaxially growing a SiC single crystal on a SiC substrate under reaction chamber conditions in which the supply of carbon is suppressed, such as using SiC as a susceptor or using SiC-coated graphite whose susceptor surface is coated with SiC, has been studied. .
一方、ＳｉＣ基板のスライス技術や研磨技術がシリコン基板（シリコンウェハー）の技術に比べて未だ十分でないため、ＳｉＣ基板には研磨によるダメージ層やスクラッチと呼ばれる傷が全面に発生する。最終的なデバイス性能の多くはＳｉＣ基板上に成長させたエピタキシャル薄膜の膜質に左右され、エピタキシャル薄膜は下地層の影響を受けるから、高品質のエピタキシャル薄膜を得るためには、エピタキシャル薄膜の成膜前にＳｉＣ基板表面のダメージ層を除去して平坦かつ清浄な表面を得ることが必要となる。
このため、エピタキシャル成長の前処理として、ＳｉＣ基板の水素雰囲気によるエッチング処理が提案された（特許文献１〜３）。
On the other hand, since the SiC substrate slicing technique and polishing technique are not yet sufficient as compared with the silicon substrate (silicon wafer) technique, a damage layer or scratches called scratches are generated on the entire surface of the SiC substrate. Much of the final device performance depends on the quality of the epitaxial thin film grown on the SiC substrate, and the epitaxial thin film is affected by the underlying layer. To obtain a high-quality epitaxial thin film, the epitaxial thin film must be formed. It is necessary to obtain a flat and clean surface by removing the damaged layer on the surface of the SiC substrate before.
For this reason, the etching process by the hydrogen atmosphere of a SiC substrate was proposed as a pretreatment of epitaxial growth (patent documents 1-3).
上記の特許文献１には、炭化珪素単結晶ウェハーを１５５０℃以上の温度で水素ガス又は塩化水素ガス流通雰囲気中で前処理を行った後に、該ウェハー上に炭化珪素薄膜をエピタキシャル成長する炭化珪素エピタキシャル基板の製造方法が記載されている。そして、具体例として、グラファイトサセプタを用いて前記温度および雰囲気で前処理を行った例が示されている。 In the above-mentioned Patent Document 1, a silicon carbide single crystal wafer is pretreated in a hydrogen gas or hydrogen chloride gas circulation atmosphere at a temperature of 1550 ° C. or higher, and then a silicon carbide epitaxial film is epitaxially grown on the wafer. A method for manufacturing a substrate is described. As a specific example, an example in which pretreatment is performed at the temperature and atmosphere using a graphite susceptor is shown.
上記の特許文献２には、炭化珪素基板の平滑化における水素エッチング時に原料ガスを添加する炭化珪素平滑化基板の作製方法が記載されている。そして、原料ガスとしてシランが記載され、サセプタの種類については記載がない。 Patent Document 2 described above describes a method for manufacturing a silicon carbide smoothed substrate in which a source gas is added during hydrogen etching in smoothing a silicon carbide substrate. And silane is described as source gas and there is no description about the kind of susceptor.
上記の特許文献３には、炭化珪素基板の表面を水素エッチングで処理した後に、この処理面から炭化珪素をエピタキシャル成長させてエピタキシャル層を形成するバイポーラ型半導体装置の製造方法が記載されているが、サセプタの種類については記載がない。 Patent Document 3 described above describes a method for manufacturing a bipolar semiconductor device in which after the surface of a silicon carbide substrate is treated by hydrogen etching, silicon carbide is epitaxially grown from the treated surface to form an epitaxial layer. There is no description of the type of susceptor.
このように、公知文献に記載の方法は、グラファイトサセプタを用いるなどカーボンの供給を前提とする反応室内条件下あるいはカーボンの供給を抑えることが不明な反応室内条件下での水素エッチングによるエピタキシャル成長の前処理であり、カーボンの供給を抑えた反応室内条件下で平滑な表面を有するＳｉＣ基板表面の平坦化処理法は知られていない。
従って、この発明の目的は、カーボンの供給を抑えた反応室内条件下で平滑な表面を形成することが出来るＳｉＣ基板表面の平坦化処理方法を提供することである。
As described above, the method described in the publicly known literature is based on the pre-epitaxial growth by hydrogen etching under the reaction chamber conditions that require the supply of carbon, such as using a graphite susceptor, or under the reaction chamber conditions where it is unknown to suppress the supply of carbon. There is no known method for flattening the surface of a SiC substrate having a smooth surface under reaction chamber conditions in which carbon supply is suppressed.
Accordingly, an object of the present invention is to provide a method for planarizing a SiC substrate surface, which can form a smooth surface under conditions in a reaction chamber in which the supply of carbon is suppressed.
この発明者らは、前記の目的を達成することを目的として鋭意検討した結果、カーボンの供給を抑えた反応室内条件下に水素ガスを供給してＳｉＣ基板を高温熱処理すると基板表面がＳｉ過剰となりＳｉドロップレットが生じることを見出し、さらに検討を行った結果、この発明を完成した。
この発明は、水素ガスによるＳｉＣ基板表面の平坦化処理において、サセプタをＳｉＣ、ＳｉＣコートグラファイト又はＴａＣコートグラファイトによって構成するカーボンの供給を抑えた反応室内条件下にＳｉＣ基板の昇温中にハイドロカーボンを供給し、エピタキシャル成長温度に到達後にハイドロカーボンの供給を停止又は減らして、引き続き水素ガスを供給してＳｉＣ基板表面をエッチングすることを特徴とするＳｉＣ基板表面の平坦化処理方法に関する。
また、この出願の発明は、前記の平坦化処理方法によって得られた平滑な表面を有するＳｉＣ基板表面に、エピタキシャル結晶成長法によってＳｉＣ薄膜を形成するＳｉＣエピタキシャル結晶成長法に関する。
As a result of intensive studies aimed at achieving the above object, the present inventors have found that when the SiC substrate is heated at a high temperature by supplying hydrogen gas under the reaction chamber conditions in which the supply of carbon is suppressed, the substrate surface becomes Si-excessive. As a result of finding out that Si droplets are generated and conducting further studies, the present invention has been completed.
In the planarization treatment of the SiC substrate surface with hydrogen gas, the present invention provides a hydrocarbon during the temperature rise of the SiC substrate under a reaction chamber condition in which the supply of carbon in which the susceptor is composed of SiC, SiC-coated graphite or TaC-coated graphite is suppressed. And then, after reaching the epitaxial growth temperature, the supply of hydrocarbons is stopped or reduced, and hydrogen gas is subsequently supplied to etch the SiC substrate surface.
The invention of this application also relates to a SiC epitaxial crystal growth method in which a SiC thin film is formed by an epitaxial crystal growth method on a SiC substrate surface having a smooth surface obtained by the planarization method.
この発明によれば、カーボンの供給を抑えた反応室内条件下でＳｉＣ基板表面を平坦化処理して、基板表面のＳｉドロップレットが抑制されて平滑な表面を形成することができる。 According to the present invention, the SiC substrate surface can be planarized under the reaction chamber conditions in which the supply of carbon is suppressed, and the Si droplets on the substrate surface can be suppressed to form a smooth surface.
この発明における好適な態様を次に示す。
１）カーボンの供給を抑えた反応室内条件が、サセプタをＳｉＣ、ＳｉＣコートグラファイト又はＴａＣコートグラファイトによって構成することである前記の平坦化処理方法。
２）カーボンの供給を抑えた反応室内条件が、さらに断熱材をＳｉＣ、ＳｉＣコートグラファイト又はＴａＣコートグラファイトによって構成することである前記の平坦化処理方法。
３）水素ガスを５〜３０分間供給してＳｉＣ基板表面をエッチングする前記の平坦化処理方法。
A preferred embodiment of the present invention will be described below.
1) The planarization method as described above, wherein the reaction chamber condition in which the supply of carbon is suppressed is that the susceptor is composed of SiC, SiC-coated graphite, or TaC-coated graphite.
2) The planarization method as described above, wherein the reaction chamber condition in which the supply of carbon is suppressed is that the heat insulating material is further composed of SiC, SiC-coated graphite, or TaC-coated graphite.
3) The said planarization method of supplying a hydrogen gas for 5 to 30 minutes and etching the SiC substrate surface.
以下、この発明を図面を参照して説明する。図１は、この発明の平坦化処理方法に用いる製膜装置の１実施態様の概略図であり、図２はこの発明の１実施態様における加熱温度の時間変化およびハイドロカーボン供給の時間変化を示すグラフである。
図１において、製膜装置は、反応室１内にサセプタ２および断熱材３を備え、サセプタ２上のＳｉＣ基板４に薄膜を形成するためのチャンバー、例えば、石英製チャンバーからなり、反応室１外に装置内加熱装置５、例えば、高周波電源と装置内加熱温度測定用の熱電対温度計６と、ガス、例えば水素キャリアガス、原料ガスの供給配管（図示せず）、排気管（図示せず）および形成された薄膜を取り出す薄膜取り出し装置（図示せず）を備えている。
The present invention will be described below with reference to the drawings. FIG. 1 is a schematic view of one embodiment of a film forming apparatus used in the planarization processing method of the present invention, and FIG. 2 shows the time variation of heating temperature and the time variation of hydrocarbon supply in one embodiment of the present invention. It is a graph.
In FIG. 1, a film forming apparatus includes a susceptor 2 and a heat insulating material 3 in a reaction chamber 1, and includes a chamber for forming a thin film on a SiC substrate 4 on the susceptor 2, for example, a quartz chamber. In addition, an in-apparatus heating device 5, for example, a high-frequency power source and a thermocouple thermometer 6 for measuring the in-apparatus heating temperature, a supply pipe (not shown) for a gas, for example, a hydrogen carrier gas and a source gas, and an exhaust pipe (not shown) And a thin film take-out device (not shown) for taking out the formed thin film.
この発明は、例えば図１に一例を示す製膜装置を用いたＳｉＣ基板表面の平坦化処理方法に関するものであり、先ずカーボンの供給を抑えた反応室内条件下に水素ガス供給下にＳｉＣ基板の昇温中にハイドロカーボンを供給することが必要である。
前記のカーボンの供給を抑えた反応室内条件としては、好適にはサセプタをＳｉＣ、ＳｉＣコートグラファイト又はＴａＣコートグラファイトで構成することが挙げられ、さらに断熱材もＳｉＣ、ＳｉＣコートグラファイト又はＴａＣコートグラファイトで構成することが挙げられる。
The present invention relates to a method for flattening the surface of an SiC substrate using, for example, a film forming apparatus shown in FIG. 1, for example. First, an SiC substrate under a reaction chamber condition in which carbon supply is suppressed under supply of hydrogen gas. It is necessary to supply hydrocarbon during the temperature rise.
As the reaction chamber conditions in which the supply of carbon is suppressed, preferably, the susceptor is composed of SiC, SiC-coated graphite or TaC-coated graphite, and the heat insulating material is also SiC, SiC-coated graphite or TaC-coated graphite. It may be configured.
そして、前記のカーボンの供給を抑えた反応室内条件下とＳｉＣ基板の水素ガス供給下の昇温中にハイドロカーボンを供給する方法としては、図２に示すように、昇温の最初は水素ガスを供給し、次いで水素ガスとともにハイドロカーボンを昇温の途中、好適には５００℃以上の温度、特に７５０℃以上の温度、その中でも１０００℃以上の温度に達した段階で供給することが好ましい。この温度は、図１に示すように熱伝対温度計で測定される加熱温度を意味する。また、前記の昇温中とは、エピタキシャル成長温度に到達するまでの温度範囲内で熱電対温度計が示す温度が上昇している状態を示す。昇温の条件については特に制限はなく、図２に示すように一定の昇温速度で温度上昇させてもよく又は、温度上昇−温度保持−温度上昇等の段階的な昇温を繰り返しても良い。 And, as shown in FIG. 2, as a method of supplying hydrocarbons during the temperature increase in the reaction chamber with the carbon supply suppressed and during the temperature increase under the hydrogen gas supply of the SiC substrate, as shown in FIG. Then, it is preferable to supply the hydrocarbon together with hydrogen gas in the course of raising the temperature, preferably at a temperature of 500 ° C. or higher, particularly 750 ° C. or higher, particularly 1000 ° C. or higher. This temperature means the heating temperature measured with a thermocouple thermometer as shown in FIG. The term “during temperature rise” means that the temperature indicated by the thermocouple thermometer is rising within the temperature range until the epitaxial growth temperature is reached. There are no particular restrictions on the temperature raising conditions, and the temperature may be raised at a constant rate of temperature rise as shown in FIG. good.
この発明の方法において、水素ガス単独で供給した後に水素ガスとともにハイドロカーボンを供給する条件については特に制限はないが、圧力は、１ｔｏｒｒ〜１ａｔｍ、特に２ｔｏｒｒ〜１ａｔｍであることが好ましい。また、水素ガスは、好適には１０〜５０００ｓｃｃｍ（ｓｔａｎｄａｒｄ ｃｃ／ｍｉｎの略号、０℃で規格化したｓｃｃｍを表示する。）、特に５０〜２５００ｓｃｃｍ程度の供給量で供給することが好ましい。
また、水素ガスとともに供給するハイドロカーボンとしては、特に制限はなく、例えばメタン、プロパン、アセチレンなどを使用することができる。
前記のハイドロカーボンは、水素ガスの供給量中の割合が０．１〜５０容積％、特に１〜１０容積％、その中でも２〜１０容積％で供給することが好ましい。
In the method of the present invention, there is no particular limitation on the conditions for supplying hydrocarbons together with hydrogen gas after supplying hydrogen gas alone, but the pressure is preferably 1 torr to 1 atm, particularly 2 torr to 1 atm. The hydrogen gas is preferably supplied at a supply amount of about 10 to 5000 sccm (abbreviation of standard cc / min, sccm normalized at 0 ° C.), particularly about 50 to 2500 sccm.
Moreover, there is no restriction | limiting in particular as hydrocarbon supplied with hydrogen gas, For example, methane, a propane, acetylene etc. can be used.
The above-mentioned hydrocarbon is preferably supplied at a ratio of 0.1 to 50% by volume, particularly 1 to 10% by volume, particularly 2 to 10% by volume in the supply amount of hydrogen gas.
この発明においては、前記のカーボンの供給を抑えた反応室内条件下で昇温中に水素ガスとともにハイドロカーボンを供給することが必要であり、ハイドロカーボンを供給せず水素ガスを単独で供給したのではＳｉＣ基板表面にシリコンドロップレットが生じる。
この従来の昇温中での水素ガスの単独供給によるＳｉドロップレット生成の要因として、水素雰囲気下でＳｉＣ基板を加熱することによって下記の反応がおきることによると考えられる。
In the present invention, it is necessary to supply hydrocarbon together with hydrogen gas during the temperature rise under the above-described reaction chamber conditions in which supply of carbon is suppressed, and hydrogen gas is supplied alone without supplying hydrocarbon. Then, silicon droplets are generated on the surface of the SiC substrate.
It is considered that the following reaction occurs by heating the SiC substrate in a hydrogen atmosphere as a factor for the generation of Si droplets by the single supply of hydrogen gas during the conventional temperature increase.
ＳｉＣ＋２Ｈ２→Ｓｉ（ｓ）＋ＣＨ４（ｇ）＋０．７２ｅＶ
このＳｉＣ基板表面に発生したＳｉ（ｓ）がドロップレットとして表面に残ると考えられる。
このＳｉ（ｓ）は加熱により次式に従って蒸発すると考えられる。
Ｓｉ（ｓ）→Ｓｉ（ｇ）＋４．４ｅＶ
この反応によるＳｉの蒸発は、活性化エネルギーの関係から低温域では遅く、高温域では早い。また、飽和蒸気圧の関係から、蒸発速度は圧力の平方根分の１に比例するため温度や圧力によってＳｉＣ基板表面に残るＳｉ量が異なり、結局水素ガス雰囲気ではＳｉＣ基板表面にＳｉがドロップレットとして残ることは避けられない。
SiC + 2H 2 → Si (s) + CH 4 (g) +0.72 eV
It is considered that Si (s) generated on the surface of the SiC substrate remains on the surface as droplets.
This Si (s) is considered to evaporate by heating according to the following formula.
Si (s) → Si (g) +4.4 eV
The evaporation of Si due to this reaction is slow in the low temperature range and fast in the high temperature range due to the activation energy. In addition, because of the saturation vapor pressure, the evaporation rate is proportional to 1 / square root of the pressure, so the amount of Si remaining on the SiC substrate surface varies depending on the temperature and pressure. As a result, in the hydrogen gas atmosphere, Si becomes droplets on the SiC substrate surface. It is inevitable to remain.
これに対して、この発明においてＳｉドロップレットが抑制される要因としては、ＳｉＣ基板の昇温中に水素ガスとともにハイドロカーボンを供給するため、下記の反応がおきることによると考えられる。
Ｓｉ＋ＣＨ４→ＳｉＣ＋Ｈ２−０．７２ｅＶ
３Ｓｉ＋Ｃ３Ｈ８→３ＳｉＣ＋４Ｈ２−０．８８ｅＶ
２Ｓｉ＋Ｃ２Ｈ２→２ＳｉＣ＋Ｈ２＋０．９１ｅＶ
この反応式に示すように、ハイドロカーボンの種類によって反応式は異なるが、いずれによってもＳｉＣ基板でＳｉＣの再生成が起き、Ｓｉのドロップレットが解消されると考えられる。
On the other hand, it is considered that the reason why the Si droplets are suppressed in the present invention is that the following reaction occurs because the hydrocarbon is supplied together with the hydrogen gas during the temperature rise of the SiC substrate.
Si + CH 4 → SiC + H 2 −0.72 eV
3Si + C 3 H 8 → 3SiC + 4H 2 −0.88 eV
2Si + C 2 H 2 → 2SiC + H 2 +0.91 eV
As shown in this reaction equation, although the reaction equation varies depending on the type of hydrocarbon, it is considered that in any case, SiC is regenerated on the SiC substrate, and Si droplets are eliminated.
この発明においては、ＳｉＣ基板の昇温中に水素ガスとともにハイドロカーボンを供給し、エピタキシャル成長温度に到達後にハイドロカーボンの供給を停止又は減らして、引き続き水素ガスを供給してＳｉＣ基板表面をエッチングすることが必要である。後者の場合はハイドロカーボン（特にアセチレン）の供給を昇温中の３分の１以下、特に５分の１以下に減らすことが好ましい。エピタキシャル成長温度に到達後にハイドロカーボンの供給を停止又は減らさないで、そのまま水素ガスとともにハイドロカーボンを供給すると、ＳｉＣ基板表面が曇り等の現象が現れ平坦面が得られないので好ましくない。 In the present invention, hydrocarbon is supplied together with hydrogen gas during the temperature rise of the SiC substrate, the supply of hydrocarbon is stopped or reduced after reaching the epitaxial growth temperature, and the surface of the SiC substrate is etched by subsequently supplying hydrogen gas. is required. In the latter case, it is preferable to reduce the supply of hydrocarbon (particularly acetylene) to 1/3 or less, particularly 1/5 or less of the temperature rising. If the hydrocarbon is supplied together with hydrogen gas without stopping or reducing the supply of the hydrocarbon after reaching the epitaxial growth temperature, a phenomenon such as cloudiness appears on the surface of the SiC substrate and a flat surface cannot be obtained.
前記のエピタキシャル成長温度に到達後は、図２に示すように一定温度で水素ガスを供給してＳｉＣ基板表面をエッチングすることが好ましいが、エピタキシャル成長温度以上の温度であれば加熱温度について特に制限はなく、前記の範囲で温度を上昇又は降温させてＳｉＣ基板表面を水素ガスエッチングしてもよい。
前記のエピタキシャル成長温度としては、１３００℃以上〜２０００℃未満、特に１５００℃以上〜１８００℃、その中でも特に１５００〜１５５０℃の温度が好適である。
また、前記のハイドロカーボンの供給を停止した後に引き続き水素ガスを供給してＳｉＣ基板表面をエッチングする条件としては、１０〜５０００ｓｃｃｍ、特に５０〜２５００ｓｃｃｍ程度の水素ガス供給量、１５００℃以上〜２０００℃未満、特に１５００〜１８００℃程度、その中でも特に１５００〜１５５０℃の温度、５分間〜２時間、特に５〜３０分間の時間が好ましい。
After reaching the epitaxial growth temperature, it is preferable to etch the SiC substrate surface by supplying hydrogen gas at a constant temperature as shown in FIG. 2, but there is no particular limitation on the heating temperature as long as the temperature is equal to or higher than the epitaxial growth temperature. The SiC substrate surface may be subjected to hydrogen gas etching by raising or lowering the temperature within the above range.
As said epitaxial growth temperature, 1300 degreeC or more-less than 2000 degreeC, Especially 1500 degreeC or more-1800 degreeC, Among these, the temperature of 1500-1550 degreeC is especially suitable.
The conditions for etching the SiC substrate surface by continuously supplying hydrogen gas after stopping the supply of the hydrocarbon are 10 to 5000 sccm, particularly about 50 to 2500 sccm, and about 1500 to 2000 ° C. Less than, especially about 1500-1800 degreeC, Among these, the temperature of 1500-1550 degreeC is especially preferable for the time for 5 minutes-2 hours, especially 5-30 minutes.
前記の一連の工程によるこの発明の方法によりＳｉＣ基板表面をエッチングすることによって、ＳｉＣドロップレットの発生が抑制され、表面の研磨ひずみ層が除去されてＳＲｑ（粗さ曲面の自乗平均平方根粗さを示す）が好適には１ｎｍ以下、特に０．５ｎｍ以下、その中でも０．４ｎｍ以下の平坦面を有するＳｉＣ基板を得ることができる。
前記のエッチング処理されたＳｉＣ基板に、引き続いてキャリアガス（前記の水素ガスを使用しても良い。）および原料ガスを供給してＳｉＣ単結晶をエピタキシャル成長させることができる。
By etching the surface of the SiC substrate by the method of the present invention through the above-described series of steps, the generation of SiC droplets is suppressed, the polishing strain layer on the surface is removed, and SRq (root mean square roughness of the roughness curved surface is reduced. It is preferable to obtain a SiC substrate having a flat surface of 1 nm or less, particularly 0.5 nm or less, and more preferably 0.4 nm or less.
The SiC single crystal can be epitaxially grown by supplying a carrier gas (the hydrogen gas may be used) and a raw material gas to the etched SiC substrate.
前記のＳｉＣ単結晶をエピタキシャル成長させる方法としては特に制限はなく、任意の方法を採用することが出来る。
例えば、エピタキシャル成長によって形成される薄膜は単一層であってもよく２種以上の多層であってもよい。また、ＳｉＣのみからなる薄膜の場合、ｐ型およびｎ型の単結晶が相互に接合されて構成されてもよく、異種の結晶からなる薄膜が相互に接合されて構成されてもよい。
前記のＳｉＣをエピタキシャル結晶成長させるために原料ガスとしては、シリコン源としてＳｉＨ４やジクロルシランなどを挙げることができ、カーボン源としてメタン、プロパン、アセチレンなどを使用することができる。
The method for epitaxially growing the SiC single crystal is not particularly limited, and any method can be adopted.
For example, the thin film formed by epitaxial growth may be a single layer or two or more types of multilayers. Further, in the case of a thin film made of only SiC, p-type and n-type single crystals may be joined to each other, or thin films made of different types of crystals may be joined to each other.
Examples of the source gas for epitaxial crystal growth of SiC include SiH 4 and dichlorosilane as the silicon source, and methane, propane, acetylene, and the like as the carbon source.
さらに、反応室内の温度（サセプタの熱電対温度）は１０００℃以上２０００℃未満、特に１５００〜１８００℃の範囲内の温度であることが好ましく、１ｔｏｒｒ〜２ａｔｍの圧力、厚みによって異なるが５〜１０μｍの場合には通常１〜２時間の反応時間（素子１枚ごとの成長時間）でエピタキシャル成長を行うことが好ましい。
前記の各サセプタおよび断熱材のうちどれを組み合わせて使用するかによって、原料のシリコン源およびカーボン源の割合を変えることが好ましく、例えば、ＳｉＣサセプタおよびＳｉＣ断熱材の場合、ＳｉＣエピタキシャル結晶成長時の適切な原料供給比：Ｃ／Ｓｉは６である。
Furthermore, the temperature in the reaction chamber (thermocouple temperature of the susceptor) is preferably 1000 ° C. or more and less than 2000 ° C., particularly 1500 to 1800 ° C., preferably 5 to 10 μm, depending on the pressure and thickness of 1 torr to 2 atm. In this case, it is preferable to perform epitaxial growth usually with a reaction time of 1 to 2 hours (growth time for each element).
It is preferable to change the ratio of the raw silicon source and carbon source depending on which of the above susceptors and heat insulating materials is used in combination. For example, in the case of SiC susceptor and SiC heat insulating material, during the epitaxial growth of SiC Appropriate raw material supply ratio: C / Si is 6.
この発明のＳｉＣ基板表面の平坦化処理方法によって得られるＳｉドロップレットがなく平滑な表面を有するＳｉＣ基板表面に、前記のＳｉＣエピタキシャル結晶成長法によってＳｉＣ薄膜を得ることができる。 A SiC thin film can be obtained by the above-described SiC epitaxial crystal growth method on the surface of a SiC substrate having no smooth surface and having a smooth surface obtained by the method for planarizing a surface of a SiC substrate of the present invention.
以下にこの発明の実施例を示すが、この発明は以下の実施例に限定されるものではない。
以下の各例において、ＳｉＣ基板の表面粗さをＡＦＭ（Ａｔｏｍｉｃ Ｆｏｒｃｅ Ｍｉｃｒｏｓｃｏｐｏ、原子間力顕微鏡）によって測定し、ＳＲｑで表示する。
Examples of the present invention are shown below, but the present invention is not limited to the following examples.
In each of the following examples, the surface roughness of the SiC substrate is measured by an AFM (Atomic Force Microscope) and displayed as SRq.
実施例１
図１に示す製膜装置を用いて、下記の工程でＳｉＣ基板の表面平坦化処理を行った。
１）洗浄したＳｉＣ基板を、ＳｉＣサセプタおよびＳｉＣ断熱材を備えた製膜装置の反応室に設置した。
２）水素ガス５００ｓｃｃｍを流しながら２ｔｏｒｒの圧力下で加熱を始め、４０℃／分の一定の昇温速度で昇温し、温度が１０００℃になったところで水素ガス希釈５％メタンの供給を開始した。この際の水素ガス希釈５％メタンの供給量を０．５ｓｃｃｍ、１ｓｃｃｍ、１．４ｓｃｃｍおよび２ｓｃｃｍで行った。
３）引き続き一定速度で昇温し、エピタキシャル成長温度の１５００℃になったところでメタンの供給を停止し、そのまま３０分間水素ガスを供給しながら温度を保持して、ＳｉＣ基板を表面平坦化処理した。
Example 1
Using the film forming apparatus shown in FIG. 1, the surface flattening process of the SiC substrate was performed in the following steps.
1) The cleaned SiC substrate was placed in a reaction chamber of a film forming apparatus equipped with a SiC susceptor and a SiC heat insulating material.
2) Heating is started at a pressure of 2 torr while flowing 500 sccm of hydrogen gas, the temperature is raised at a constant rate of 40 ° C./min, and supply of hydrogen gas diluted 5% methane is started when the temperature reaches 1000 ° C. did. At this time, hydrogen gas diluted 5% methane was supplied at 0.5 sccm, 1 sccm, 1.4 sccm, and 2 sccm.
3) Subsequently, the temperature was raised at a constant rate, and when the epitaxial growth temperature reached 1500 ° C., the supply of methane was stopped, and the temperature was maintained as it was for 30 minutes while supplying the hydrogen gas.
ＳｉＣ基板の表面平坦化処理が終了後、降温してＳｉＣ基板を取り出し、ＳｉＣ基板の表面形状をＡＦＭを用いて評価した。
この加熱温度の時間変化およびハイドロカーボン供給の時間変化の概略を示すグラフを図２に示す。
また、表面平坦化処理によって得られたＳｉＣ基板の表面粗さを測定した結果を比較例の結果とともにまとめて図５に、ＡＦＭによるＳｉＣ基板の表面形状を図６に示す。
After finishing the surface flattening process of the SiC substrate, the temperature was lowered, the SiC substrate was taken out, and the surface shape of the SiC substrate was evaluated using AFM.
FIG. 2 shows a graph showing an outline of the time change of the heating temperature and the time change of the hydrocarbon supply.
Moreover, the result of having measured the surface roughness of the SiC substrate obtained by the surface flattening process is shown together with the result of the comparative example in FIG. 5, and the surface shape of the SiC substrate by AFM is shown in FIG.
比較例１
下記の工程に変えた他は、実施例１と同様にしてＳｉＣ基板の表面平坦化処理を行った。
１）洗浄したＳｉＣ基板を、ＳｉＣサセプタおよびＳｉＣ断熱材を備えた製膜装置の反応室に設置した。
２）水素ガス５００ｓｃｃｍを流しながら２ｔｏｒｒの圧力下で加熱を始め、４０℃／分の一定の昇温速度で昇温した。
３）引き続き一定速度で昇温し、エピタキシャル成長温度の１５００℃になるまで加熱を続けて、ＳｉＣ基板を表面平坦化処理した。
Comparative Example 1
The surface flattening treatment of the SiC substrate was performed in the same manner as in Example 1 except that the following steps were changed.
1) The cleaned SiC substrate was placed in a reaction chamber of a film forming apparatus equipped with a SiC susceptor and a SiC heat insulating material.
2) Heating was started under a pressure of 2 torr while flowing 500 sccm of hydrogen gas, and the temperature was increased at a constant temperature increase rate of 40 ° C./min.
3) Subsequently, the temperature was raised at a constant rate, and heating was continued until the epitaxial growth temperature reached 1500 ° C., thereby surface-treating the SiC substrate.
ＳｉＣ基板の表面平坦化処理が終了後、降温してＳｉＣ基板を取り出し、ＳｉＣ基板の表面形状をＡＦＭを用いて評価した。
この加熱温度の時間変化を示すグラフを図３に示す。
また、ＡＦＭによるＳｉＣ基板の表面形状を図７に示す。
After finishing the surface flattening process of the SiC substrate, the temperature was lowered, the SiC substrate was taken out, and the surface shape of the SiC substrate was evaluated using AFM.
A graph showing the time change of the heating temperature is shown in FIG.
Moreover, the surface shape of the SiC substrate by AFM is shown in FIG.
比較例２
下記の工程に変えた他は、実施例１と同様にしてＳｉＣ基板の表面平坦化処理を行った。
１）洗浄したＳｉＣ基板を、ＳｉＣサセプタおよびＳｉＣ断熱材を備えた製膜装置の反応室に設置した。
２）水素ガス５００ｓｃｃｍを流しながら２ｔｏｒｒの圧力下で加熱を始め、４０℃／分の一定の昇温速度で昇温し、温度が１０００℃になったところで水素ガス希釈５％メタンの供給を開始した。この際のメタンの供給量を０．５ｓｃｃｍ、１．４ｓｃｃｍ、２．８ｓｃｃｍ、１０ｓｃｃｍおよび１００ｓｃｃｍで行った。
３）引き続き一定速度で昇温し、エピタキシャル成長温度の１５００℃になったところで昇温を停止し、そのまま３０分間水素ガスおよびメタンを供給しながら温度を保持して、ＳｉＣ基板を表面平坦化処理した。
Comparative Example 2
The surface flattening treatment of the SiC substrate was performed in the same manner as in Example 1 except that the following steps were changed.
1) The cleaned SiC substrate was placed in a reaction chamber of a film forming apparatus equipped with a SiC susceptor and a SiC heat insulating material.
2) Heating is started at a pressure of 2 torr while flowing 500 sccm of hydrogen gas, the temperature is raised at a constant rate of 40 ° C./min, and supply of hydrogen gas diluted 5% methane is started when the temperature reaches 1000 ° C. did. At this time, the supply amount of methane was 0.5 sccm, 1.4 sccm, 2.8 sccm, 10 sccm, and 100 sccm.
3) Subsequently, the temperature was raised at a constant rate, and when the epitaxial growth temperature reached 1500 ° C., the temperature raising was stopped, and the temperature was maintained as it was for 30 minutes while supplying the hydrogen gas and methane, and the SiC substrate was surface planarized. .
ＳｉＣ基板の表面平坦化処理が終了後、降温してＳｉＣ基板を取り出し、ＳｉＣ基板の表面形状をＡＦＭを用いて評価した。
この加熱温度の時間変化を示すグラフを図４に示す。
また、表面平坦化処理によって得られたＳｉＣ基板の表面は曇り、表面粗さを測定したところ、ＳＲｑが数十〜２００ｎｍで、且つ晶癖を有した形状であった。メタンの供給量が０．５ｓｃｃｍ、１．４ｓｃｃｍおよび２．８ｓｃｃｍの場合のＳｉＣ基板のＡＦＭによる表面形状を図８に示す。
After finishing the surface flattening process of the SiC substrate, the temperature was lowered, the SiC substrate was taken out, and the surface shape of the SiC substrate was evaluated using AFM.
The graph which shows the time change of this heating temperature is shown in FIG.
Further, the surface of the SiC substrate obtained by the surface flattening treatment was cloudy, and the surface roughness was measured. As a result, the SRq was several tens to 200 nm and had a crystal habit. FIG. 8 shows the surface shape of the SiC substrate by AFM when the supply amount of methane is 0.5 sccm, 1.4 sccm, and 2.8 sccm.
比較例３
下記の工程に変えた他は、実施例１と同様にしてＳｉＣ基板の表面平坦化処理を行った。
１）洗浄したＳｉＣ基板を、ＳｉＣサセプタおよびＳｉＣ断熱材を備えた製膜装置の反応室に設置した。
２）水素ガス５００ｓｃｃｍを流しながら２ｔｏｒｒの圧力下で加熱を始め、４０℃／分の一定の昇温速度で昇温した。
３）引き続き一定速度で昇温し、エピタキシャル成長温度の１５００℃になったところで昇温を停止し、そのまま水素ガスを供給しながら３０分間保持して、ＳｉＣ基板を表面平坦化処理した。
Comparative Example 3
The surface flattening treatment of the SiC substrate was performed in the same manner as in Example 1 except that the following steps were changed.
1) The cleaned SiC substrate was placed in a reaction chamber of a film forming apparatus equipped with a SiC susceptor and a SiC heat insulating material.
2) Heating was started under a pressure of 2 torr while flowing 500 sccm of hydrogen gas, and the temperature was increased at a constant temperature increase rate of 40 ° C./min.
3) Subsequently, the temperature was raised at a constant rate, and when the epitaxial growth temperature reached 1500 ° C., the temperature raising was stopped, and the SiC substrate was flattened by maintaining the hydrogen gas as it was for 30 minutes.
ＳｉＣ基板の表面平坦化処理が終了後、降温してＳｉＣ基板を取り出し、ＳｉＣ基板の表面形状をＡＦＭを用いて評価した。
この加熱温度の時間変化を示すグラフは図４と同じである。
また、表面平坦化処理によって得られたＳｉＣ基板の表面形状をＡＦＭにより評価した。
ＳｉＣ基板の表面形状をＡＦＭにより評価した結果について、実施例１と比較例１〜３の結果をまとめて表１に示す。
After finishing the surface flattening process of the SiC substrate, the temperature was lowered, the SiC substrate was taken out, and the surface shape of the SiC substrate was evaluated using AFM.
The graph showing the change over time in the heating temperature is the same as in FIG.
Moreover, the surface shape of the SiC substrate obtained by the surface flattening treatment was evaluated by AFM.
About the result of having evaluated the surface shape of a SiC substrate by AFM, the result of Example 1 and Comparative Examples 1-3 is put together in Table 1, and is shown.
実施例２
図１に示す製膜装置を用いて、下記の工程でＳｉＣ基板の表面平坦化処理を行った。
１）洗浄したＳｉＣ基板を、ＳｉＣサセプタおよびＳｉＣ断熱材を備えた製膜装置の反応室に設置した。
２）水素ガス５００ｓｃｃｍを流しながら２ｔｏｒｒの圧力下で加熱を始め、４０℃／分の一定の昇温速度で昇温し、温度が１０００℃になったところで水素ガス希釈１％アセチレンの供給を開始した。この際のアセチレンの供給量を７ｓｃｃｍで行った。
３）引き続き一定速度で昇温し、エピタキシャル成長温度の１５００℃になったところでアセチレンの供給量を１ｓｃｃｍに減らし、そのまま３０分間温度を維持して、ＳｉＣ基板を表面平坦化処理した。
Example 2
Using the film forming apparatus shown in FIG. 1, the surface flattening process of the SiC substrate was performed in the following steps.
1) The cleaned SiC substrate was placed in a reaction chamber of a film forming apparatus equipped with a SiC susceptor and a SiC heat insulating material.
2) Start heating at a pressure of 2 torr while flowing 500 sccm of hydrogen gas, raise the temperature at a constant rate of 40 ° C / min, and start supplying hydrogen gas diluted 1% acetylene when the temperature reaches 1000 ° C did. At this time, the supply amount of acetylene was 7 sccm.
3) Subsequently, the temperature was raised at a constant rate, and when the epitaxial growth temperature reached 1500 ° C., the amount of acetylene supplied was reduced to 1 sccm, and the temperature was maintained for 30 minutes to planarize the SiC substrate.
ＳｉＣ基板の表面平坦化処理が終了後、降温してＳｉＣ基板を取り出し、ＳｉＣ基板の表面形状をＡＦＭを用いて評価した。
表面粗さＳＲｑは０．３ｎｍと平坦になった。
Ｒａｍａｎ散乱測定から、表面にＳｉドロップレットが発生していないことを確認した。
After finishing the surface flattening process of the SiC substrate, the temperature was lowered, the SiC substrate was taken out, and the surface shape of the SiC substrate was evaluated using AFM.
The surface roughness SRq became flat at 0.3 nm.
From Raman scattering measurement, it was confirmed that Si droplets were not generated on the surface.
１ 反応室
２ サセプタ
３ 断熱材
４ 基板
５ 装置内加熱装置
６ 熱電対温度計
１０ 製膜装置
DESCRIPTION OF SYMBOLS 1 Reaction chamber 2 Susceptor 3 Heat insulation material 4 Board | substrate 5 In-apparatus heating apparatus 6 Thermocouple thermometer 10 Film-forming apparatus
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