JP4372988B2 - CVD-SiC excellent in NH3 resistance, CVD-SiC coating material excellent in NH3 resistance, and jig for CVD or MBE apparatus - Google Patents
CVD-SiC excellent in NH3 resistance, CVD-SiC coating material excellent in NH3 resistance, and jig for CVD or MBE apparatus Download PDFInfo
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【0001】
【発明の属する技術分野】
本発明は、耐NH3 に優れたCVD−SiC及び基材表面が耐NH3 に優れたCVD−SiCで被覆されたCVD−SiC被覆材及びそれらを用いたCVDまたはMBE装置用治具に関する。
【0002】
【従来の技術】
従来より、半導体製造工程における各種装置の構成部品や、治具等には、SiC単独のものや、黒鉛等の炭素質材料やセラミックス等からなる基材表面をCVD−SiCで被覆したCVD−SiC被覆材が広く利用されている。
【0003】
しかしながら、この種のSiCは、例えば、GaN、InN、AlN、Si3 N4 、BN等の窒化物の結晶を成長させる、例えば、MOCVD、HVPE等のCVD装置またはMBE装置等のようにNH3 雰囲気の装置の治具として使用すると、NH3 と反応、分解することで、部分的または全体的にNH3 によって腐食されていく。これによって、例えば、基材の黒鉛が露出してしまい、製品となるGaN、InN、AlN、Si3 N4 、BN等の窒化物の結晶の成長過程に悪影響を与え、GaN、InN、AlN、Si3 N4 、BN等の製造の歩留りの低下の原因となる。
【0004】
【発明が解決しようとする課題】
そこで、本発明では、NH3 に対して耐食性に優れたCVD−SiC、それにより基材表面を被覆されたCVD−SiC被覆材及びこれらを用いたCVDまたはMBE装置用治具を提供する事を目的とする。
【0005】
【課題を解決するための手段】
本発明者らは、CVD法によって表面に形成されているβ−SiCの(111)面が、形成される主な結晶面中に占める比率が0.5未満であるときに、NH3 に対して耐食性が優れていることを見いだし、本発明を完成させた。
【0006】
すなわち、本発明の請求項1の発明は、CVD法により形成されたβ‐SiCを構成する結晶のうち、X線回折図形において、SiC(200)面の占める比率が、SiC(220)面の占める比率及びSiC(311)面の占める比率のそれぞれより大きく、且つ、SiC(111)面のピーク強度の占める比率であるSiC(111)/{SiC(111)+SiC(200)+SiC(220)+SiC(311)}が、0.5未満である耐NH3性に優れるCVD−SiCである。また、本発明の請求項2の発明は、前記SiC(111)面のピーク強度の占める比率が0.3〜0.4である請求項1に記載の耐NH 3 性に優れるCVD−SiCである。
【0007】
請求項3の発明は、CVD法により形成されたβ‐SiCを構成する結晶のうち、X線回折図形において、SiC(200)面の占める比率が、SiC(220)面の占める比率及びSiC(311)面の占める比率のそれぞれより大きく、且つ、SiC(111)面のピーク強度の占める比率であるSiC(111)/{SiC(111)+SiC(200)+SiC(220)+SiC(311)}が、0.5未満であるCVD−SiCが、SiCまたは炭素質材からなる基材上に被覆されてなる耐NH3に優れるCVD−SiC被覆材である。また、請求項4の発明は、前記SiC(111)面のピーク強度の占める比率が0.3〜0.4である請求項3に記載の耐NH 3 性に優れるCVD−SiCである。
【0008】
請求項5の発明は、請求項1又は2に記載のCVD−SiCを用いたCVDまたはMBE装置用治具である。また、請求項6の発明は、請求項3又は4に記載のCVD−SiC被覆材を用いたCVDまたはMBE装置用治具である。
【0009】
本発明におけるSiCは、黒鉛基材にCVD法によりSiCを被覆し、その後、黒鉛を機械的あるいは化学的に除去させ緻密質なCVD−SiCのみとしたもの、また、黒鉛材、黒鉛材から転化したSiC、焼結質SiC、前記CVD−SiCのうち何れかからなる基材表面にCVD法で被覆形成されたものの何れであってもよい。ここで、黒鉛材から転化したSiCとは、黒鉛材とSiOガスを反応させて黒鉛材の一部または全部をSiCに転化させた、いわゆるCVR−SiCのことであり、焼結質SiCとはSiC粉末に焼結助剤を添加し、1600℃以上の高温で焼結させたもののことである。
【0010】
また、CVD法により形成されるSiCとは、CVD処理時に原料ガスより生成されるSiCが、基材表面に析出し、成長していくことにより形成される非常に緻密な膜である。また、SiCには六方晶及び菱面体晶であるα型、立方晶であるβ型の2種類があるが、本発明にかかるCVD法ではβ型のSiCが生成される。
【0011】
このCVD法によるβ−SiCの表面を構成する結晶のうち(111)面方向の結晶方位を示す結晶の占める比率を全体の0.5未満、好ましくは0.45以下、更に好ましくは0.4以下とする。0.5より大きい場合は、同一面の配向性が大きくなることによって、結晶間若しくは結晶層間が浸食されやすくなると考えられ、NH3 に対して、耐食性が発現しない。ここで、この比率の対象となる結晶面は、(111)面と方位の異なる(200)面、(220)面、(311)面である。この比率は、X線回折結果より、前記(111)面と(111)面と方位の異なる結晶面を表すピークのピーク強度(ピーク高さ)の和で、(111)面のピーク強度を割った値を採用している。
【0012】
β−SiCの表面は、CVD処理条件を調整することで、構成する結晶子の(111)面方向の結晶の比率が0.5未満とすることができ、表面を被覆したSiCを構成する各結晶の方位が乱雑となる。そして、(111)面方向にのみ成長した結晶子で形成されたβ−SiCに比較すると、NH3 に対して耐食性に優れるようになる。
【0013】
この(111)面の方位と異なる結晶面である(200)面、(220)面、(311)面はCVD処理時の基材、基材温度、原料ガス、炉内圧力、原料ガス濃度等の各制御因子のなかでも特に温度に影響を受け、CVD処理時の基材温度が高くなるほど、顕著に現れる。したがって、(111)面の占める比率を0.5未満、好ましくは0.45以下、更に好ましくは0.4以下とするためには、CVD処理時の基材温度を少なくとも1300℃、好ましくは1400℃以上とする。
【0014】
以上のように、CVD−SiCや、或いは黒鉛等の炭素質材やSiC等のセラミックスの基材表面にSiCをCVD法で被覆したCVD−SiC被覆材の表面に形成されたβ−SiCを構成する結晶のうち、(111)面の占める比率を0.5未満とすることで、NH3 に対して耐食性を有することとなる。これによりGaN、InN、AlN、Si3 N4 、BN等の窒化物の結晶を成長させるMOCVD、HVPE等のCVD装置、または、MBE装置等のCVDまたはMBE装置用治具として使用することができ、治具表面に本発明に係るCVD−SiCを形成させることで、ピンホールや剥離等の発生を抑制することができ、耐用寿命の延命化が行える。
【0015】
以上のように、本発明におけるCVD−SiC若しくはCVD−SiC被覆材はCVDまたはMBE装置用の治具として適用することができる。また、CVDまたはMBE装置用治具に限らず、例えば、耐NH3 に優れた特性を生かし、GaN、InN、AlN、Si3 N4 、BN等の窒化物の結晶の成長用の基板としても使用することができる。
【0016】
以下に実施例を挙げ、本発明を具体的に説明する。
【0017】
【実施例】
(実施例1)
基材として嵩密度1.85g/cm3 の等方性黒鉛材(東洋炭素(株)製)を使用し、20×20×5mmに加工した。次にこれらをCVD装置内に設置し、原料ガスにSiCl4 +C3 H8 を使用し、炉内圧力250Torr、基材温度1400℃でCVD処理を行い、表面全面にSiCを被覆した。
【0018】
CVD−SiCを被覆後、その表面をCuの管球を使用しX線回折分析を行った。図1にその分析結果を示す。図中に記載しているβ−SiC(111)等は各結晶面を表している。次に、表面を構成する結晶のうち、この(111)面の占める比率は、(111)面と結晶方位を異にする各結晶面の強度比(各結晶面を表すピークの高さ)を用いて、次式により算出した。すなわち、
比率 = (111)/((111)+(200)+(220)+(311))
である。表面を被覆したSiCの構成結晶子のうち(111)面の占める比率は0.3であった。
【0019】
(実施例2)
実施例1と同質の基材を同形状に加工後、実施例1と同じCVD装置を用いて、原料ガスにSiCl4 +C3 H8 を使用し、炉内圧力250Torr、基材温度1350℃でCVD処理を行い、表面全面にSiCを被覆した。その後、実施例1と同様にして、SiC被覆された表面のX線回折分析を行った。図2にそのX線回折結果を示す。この結果より、実施例1と同様にして、表面を被覆したSiCの構成結晶子のうち(111)面の占める比率を求めたところ、0.4であった。
【0020】
(比較例1)
実施例1と同質の基材を同形状に加工後、実施例1と同じCVD装置を用いて、原料ガスにSiCl4 +C3 H8 を使用し、炉内圧力250Torr、基材温度1300℃でCVD処理を行い、表面全面にSiCを被覆した。その後、実施例1と同様にして、SiC被覆された表面のX線回折分析を行った。図3にそのX線回折結果を示す。この結果より、実施例1と同様にして、表面を被覆したSiCの構成結晶子のうち(111)面の占める比率を求めたところ、0.5であった。
【0021】
(比較例2)
実施例1と同質の基材を同形状に加工後、実施例1と同じCVD装置を用いて、原料ガスにSiCl4 +C3 H8 を使用し、炉内圧力250Torr、基材温度1280℃でCVD処理を行い、表面全面にSiCを被覆した。その後、実施例1と同様にして、SiC被覆された表面のX線回折分析を行った。図4にそのX線回折結果を示す。この結果より、実施例1と同様にして、表面を被覆したSiCの構成結晶子のうち(111)面の占める比率を求めたところ、0.6であった。
【0022】
実施例1及び2と比較例1及び2は、CVD処理時の基材温度が違うのみで、それ以外の処理条件は全て同じであるが、CVD処理時の基材温度が高くなることによって、表面を構成する結晶のうち(111)面の占める割合が小さくなる。換言すると、基材温度が高くなることによって、SiCの析出成長する方向が多方向になり、表面を構成する結晶が乱雑になるといえる。
【0023】
実施例1及び2と比較例1の試料のNH3 に対する耐食性を調べるために、各試料を1200℃、13.3kPaのNH3 に180分暴露し、その時のエッチング速度を求めた。
【0024】
表1に各試料のNH3 に対する耐食性を示す。
【0025】
【表1】
【0026】
表1より、CVD法により形成されたβーSiCを構成する結晶のうち(111)面の占める比率が0.5で、NH3 に対する耐食性が異なる、すなわち、エッチング速度が0.5を境にして0.5未満では遅く、0.5を越えると速くなっていることがわかる。したがって、CVD法により形成されたβーSiCを構成する結晶のうち(111)面の占める比率を0.5未満とすることで、NH3 に対する耐食性が向上することがわかる。
【0027】
【発明の効果】
本発明にかかる、少なくとも表面がβ−SiCで形成され、その表面を構成する結晶のうち(111)面の占める比率を0.5未満とすることによって、NH3 に対する耐食性が向上し、NH3 雰囲気下で使用されるCVDまたはMBE装置用の治具として使用することが可能となる。これにより、GaN、InN、AlN、Si3 N4 、BN等の窒化物の結晶の製造における生産効率、歩留りの向上に貢献できる。
【図面の簡単な説明】
【図1】1400℃でCVD処理を行ったSiCのX線回折結果である。
【図2】1350℃でCVD処理を行ったSiCのX線回折結果である。
【図3】1300℃でCVD処理を行ったSiCのX線回折結果である。
【図4】1280℃でCVD処理を行ったSiCのX線回折結果である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to superior CVD-SiC and the substrate surface is CVD-SiC coated material coated with excellent CVD-SiC to withstand NH 3 and CVD or MBE apparatus jig using them resistant to NH 3.
[0002]
[Prior art]
Conventionally, the component parts and jigs of various devices in the semiconductor manufacturing process are made of SiC alone, or CVD-SiC in which a substrate surface made of carbonaceous material such as graphite or ceramics is coated with CVD-SiC. Coating materials are widely used.
[0003]
However, this type of SiC grows a nitride crystal such as GaN, InN, AlN, Si 3 N 4 , or BN, for example, NH 3 as in a CVD apparatus such as MOCVD or HVPE or an MBE apparatus. When used as a jig for an atmospheric device, it reacts and decomposes with NH 3, and is partially or totally corroded by NH 3 . As a result, for example, the graphite of the base material is exposed, adversely affecting the growth process of nitride crystals such as GaN, InN, AlN, Si 3 N 4 , and BN, which are products, and GaN, InN, AlN, This causes a decrease in the production yield of Si 3 N 4 , BN and the like.
[0004]
[Problems to be solved by the invention]
Therefore, the present invention provides a CVD-SiC excellent in corrosion resistance to NH 3 , a CVD-SiC coating material coated on the surface of the substrate thereby, and a jig for a CVD or MBE apparatus using them. Objective.
[0005]
[Means for Solving the Problems]
The present inventors have found that when (111) plane of the beta-SiC formed on the surface by CVD method, a ratio occupied in the main crystal plane formed is less than 0.5, with respect to NH 3 And found that the corrosion resistance is excellent, and completed the present invention.
[0006]
That is, according to the first aspect of the present invention, the ratio of the SiC (200) plane in the X-ray diffraction pattern of the β-SiC crystal formed by the CVD method is that of the SiC (220) plane. SiC (111) / {SiC (111) + SiC (200) + SiC (220) + SiC, which is larger than each of the ratio occupied by the SiC (311) plane and the ratio occupied by the peak intensity of the SiC (111) plane. (311)} is CVD-SiC excellent in NH 3 resistance, which is less than 0.5. The invention according to
[0007]
In the invention of
[0008]
The invention of claim 5 is a jig for a CVD or MBE apparatus using the CVD-SiC according to
[0009]
The SiC in the present invention is obtained by coating a graphite substrate with SiC by a CVD method, and then removing the graphite mechanically or chemically to make only dense CVD-SiC. Any of the above-described SiC, sintered SiC, and the base material surface made of any one of the above-mentioned CVD-SiCs may be coated by the CVD method. Here, SiC converted from graphite material is so-called CVR-SiC in which graphite material and SiO gas are reacted to convert part or all of graphite material into SiC. Sintered SiC is This is one obtained by adding a sintering aid to SiC powder and sintering it at a high temperature of 1600 ° C. or higher.
[0010]
Further, SiC formed by the CVD method is a very dense film formed by the SiC generated from the source gas during the CVD process being deposited on the substrate surface and growing. There are two types of SiC, α-type that is hexagonal and rhombohedral, and β-type that is cubic, but β-type SiC is generated by the CVD method according to the present invention.
[0011]
The ratio of the crystal showing the crystal orientation in the (111) plane direction among the crystals constituting the surface of β-SiC by this CVD method is less than 0.5, preferably 0.45 or less, more preferably 0.4. The following. When the ratio is larger than 0.5, it is considered that the crystal orientation between the crystals or the crystal layer is easily eroded by increasing the orientation of the same plane, and the corrosion resistance is not exhibited against NH 3 . Here, the crystal planes that are the targets of this ratio are the (200) plane, (220) plane, and (311) plane that have different orientations from the (111) plane. This ratio is obtained by dividing the peak intensity of the (111) plane by the sum of the peak intensities (peak heights) representing crystal planes having different orientations from the (111) plane and the (111) plane from the X-ray diffraction results. Value is adopted.
[0012]
The surface of β-SiC can be adjusted such that the ratio of crystals in the (111) plane direction of the constituent crystallites is less than 0.5 by adjusting the CVD processing conditions. The crystal orientation is messy. And, compared with β-SiC formed of crystallites grown only in the (111) plane direction, it has better corrosion resistance than NH 3 .
[0013]
The (200), (220), and (311) planes, which are crystal planes different from the orientation of the (111) plane, are the base material, base material temperature, source gas, furnace pressure, source gas concentration, etc. during the CVD process. Among these control factors, it is particularly affected by the temperature, and becomes more noticeable as the substrate temperature during the CVD process increases. Therefore, in order to set the ratio of the (111) plane to less than 0.5, preferably 0.45 or less, more preferably 0.4 or less, the substrate temperature during the CVD process is at least 1300 ° C., preferably 1400. ℃ or more.
[0014]
As described above, β-SiC formed on the surface of a CVD-SiC coating material in which SiC is coated on the surface of a CVD-SiC, or a carbonaceous material such as graphite, or a ceramic substrate such as SiC is formed. When the ratio of the (111) plane in the crystal to be made is less than 0.5, the crystal has corrosion resistance to NH 3 . As a result, it can be used as a CVD apparatus for MOCVD, HVPE or the like for growing nitride crystals such as GaN, InN, AlN, Si 3 N 4 , BN, or a jig for CVD or MBE apparatus such as MBE apparatus. By forming the CVD-SiC according to the present invention on the jig surface, it is possible to suppress the occurrence of pinholes and peeling, and to extend the service life.
[0015]
As described above, the CVD-SiC or CVD-SiC coating material in the present invention can be applied as a jig for a CVD or MBE apparatus. In addition to a CVD or MBE apparatus jig, for example, a substrate for growing a nitride crystal such as GaN, InN, AlN, Si 3 N 4 , or BN by taking advantage of its excellent NH 3 resistance. Can be used.
[0016]
The present invention will be specifically described with reference to examples.
[0017]
【Example】
Example 1
An isotropic graphite material (manufactured by Toyo Tanso Co., Ltd.) having a bulk density of 1.85 g / cm 3 was used as a base material and processed into 20 × 20 × 5 mm. Next, these were installed in a CVD apparatus, SiCl 4 + C 3 H 8 was used as a source gas, a CVD process was performed at a furnace pressure of 250 Torr and a substrate temperature of 1400 ° C., and the entire surface was coated with SiC.
[0018]
After coating with CVD-SiC, the surface was subjected to X-ray diffraction analysis using a Cu tube. FIG. 1 shows the analysis result. In the figure, β-SiC (111) and the like represent each crystal plane. Next, in the crystal constituting the surface, the ratio of the (111) plane is the intensity ratio of each crystal plane having a crystal orientation different from that of the (111) plane (the peak height representing each crystal plane). And calculated by the following formula. That is,
Ratio = (111) / ((111) + (200) + (220) + (311))
It is. Of the constituent crystallites of SiC covering the surface, the ratio of the (111) plane was 0.3.
[0019]
(Example 2)
After processing a base material of the same quality as in Example 1 into the same shape, using the same CVD apparatus as in Example 1, using SiCl 4 + C 3 H 8 as the source gas, with a furnace pressure of 250 Torr and a base material temperature of 1350 ° C. A CVD process was performed to coat the entire surface with SiC. Thereafter, in the same manner as in Example 1, X-ray diffraction analysis of the surface coated with SiC was performed. FIG. 2 shows the result of X-ray diffraction. From this result, in the same manner as in Example 1, the ratio of the (111) plane to the constituent crystallites of SiC covering the surface was found to be 0.4.
[0020]
(Comparative Example 1)
After processing a substrate of the same quality as in Example 1 into the same shape, using the same CVD apparatus as in Example 1, using SiCl 4 + C 3 H 8 as the source gas, with a furnace pressure of 250 Torr and a substrate temperature of 1300 ° C. A CVD process was performed to coat the entire surface with SiC. Thereafter, in the same manner as in Example 1, X-ray diffraction analysis of the surface coated with SiC was performed. FIG. 3 shows the result of X-ray diffraction. From this result, in the same manner as in Example 1, the ratio of the (111) plane in the constituent crystallites of SiC covering the surface was determined to be 0.5.
[0021]
(Comparative Example 2)
After processing a base material of the same quality as in Example 1 into the same shape, using the same CVD apparatus as in Example 1, using SiCl 4 + C 3 H 8 as the source gas, with a furnace pressure of 250 Torr and a base material temperature of 1280 ° C. A CVD process was performed to coat the entire surface with SiC. Thereafter, in the same manner as in Example 1, X-ray diffraction analysis of the surface coated with SiC was performed. FIG. 4 shows the result of X-ray diffraction. From this result, in the same manner as in Example 1, the ratio of the (111) plane in the constituent crystallites of SiC covering the surface was determined to be 0.6.
[0022]
Examples 1 and 2 and Comparative Examples 1 and 2 differ only in the substrate temperature during the CVD process, and all other processing conditions are the same, but the substrate temperature during the CVD process increases, The proportion of the (111) plane in the crystal constituting the surface is reduced. In other words, it can be said that as the substrate temperature increases, the direction of SiC precipitation and growth becomes multi-directional, and the crystals constituting the surface become messy.
[0023]
In order to examine the corrosion resistance of the samples of Examples 1 and 2 and Comparative Example 1 against NH 3 , each sample was exposed to 1200 ° C. and 13.3 kPa NH 3 for 180 minutes, and the etching rate at that time was determined.
[0024]
Table 1 shows the corrosion resistance of each sample to NH 3 .
[0025]
[Table 1]
[0026]
From Table 1, the proportion of the (111) plane in the crystals constituting β-SiC formed by the CVD method is 0.5, and the corrosion resistance to NH 3 is different, that is, the etching rate is 0.5. It can be seen that it is slow when it is less than 0.5, and it is fast when it exceeds 0.5. Therefore, it can be seen that the corrosion resistance to NH 3 is improved by setting the ratio of the (111) plane to less than 0.5 in the crystals constituting β-SiC formed by the CVD method.
[0027]
【The invention's effect】
According to the present invention, at least the surface is formed of β-SiC, and the proportion of the (111) plane in the crystal constituting the surface is less than 0.5, whereby the corrosion resistance to NH 3 is improved, and NH 3 It can be used as a jig for a CVD or MBE apparatus used in an atmosphere. Thus, can contribute GaN, InN, AlN, Si 3 N 4, production in the manufacture of crystals of a nitride such as BN efficiency, the improvement in yield.
[Brief description of the drawings]
FIG. 1 is an X-ray diffraction result of SiC subjected to CVD treatment at 1400 ° C. FIG.
FIG. 2 is an X-ray diffraction result of SiC subjected to CVD treatment at 1350 ° C.
FIG. 3 is an X-ray diffraction result of SiC subjected to CVD treatment at 1300 ° C.
FIG. 4 is an X-ray diffraction result of SiC subjected to CVD treatment at 1280 ° C.
Claims (6)
X線回折図形において、SiC(200)面の占める比率が、SiC(220)面の占める比率及びSiC(311)面の占める比率のそれぞれより大きく、且つ、SiC(111)面のピーク強度の占める比率であるSiC(111)/{SiC(111)+SiC(200)+SiC(220)+SiC(311)}が、0.5未満である耐NH3性に優れるCVD−SiC。Of the crystals constituting β-SiC formed by the CVD method ,
In the X-ray diffraction pattern, the proportion of the SiC (200) plane is greater than the proportion of the SiC (220) plane and the proportion of the SiC (311) plane, and the peak intensity of the SiC (111) plane is occupied. CVD-SiC excellent in NH 3 resistance , in which the ratio of SiC (111) / {SiC (111) + SiC (200) + SiC (220) + SiC (311)} is less than 0.5.
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