JP4126461B2 - Components for plasma process equipment - Google Patents
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本発明は、ハロゲン系腐食性ガスのプラズマに対して高い耐食性を有する、プラズマ処理装置や半導体・液晶製造用プラズマ装置内の内壁材や治具等として使用されるプラズマプロセス装置用部材に関するものである。 The present invention relates to a member for a plasma processing apparatus used as an inner wall material or jig in a plasma processing apparatus or a plasma apparatus for manufacturing semiconductors and liquid crystals, which has high corrosion resistance against plasma of a halogen-based corrosive gas. is there.
半導体製造におけるドライプロセスやプラズマコーティングなど、プラズマの利用は近年急速に進んでいる。半導体の製造時におけるプラズマプロセスでは、特にデポジション、エッチング、クリーニング用として、反応性の高いフッ素系、塩素系等のハロゲン系腐食ガスが多用されている。 In recent years, the use of plasma, such as dry processes and plasma coating in semiconductor manufacturing, has been progressing rapidly. In the plasma process during the manufacture of semiconductors, halogen-based corrosive gases such as fluorine and chlorine having high reactivity are frequently used particularly for deposition, etching and cleaning.
これら腐食性ガス及びプラズマに接触する部材には、高い耐食性が要求される。従来より、被処理物以外でこれらの腐食性ガス及びプラズマに接触する部材は、一般にガラスや石英などのＳｉＯ２を主成分とする材料やステンレス、モネル等の耐食性金属が利用されている。 High corrosion resistance is required for members that come into contact with these corrosive gases and plasmas. Conventionally, members that are in contact with these corrosive gases and plasma other than the object to be processed generally use a material mainly composed of SiO 2 such as glass and quartz, and a corrosion-resistant metal such as stainless steel and monel.
また、半導体製造時において、半導体を支持固定するサセプタ材としてアルミナ焼結体、サファイア、ＡｌＮ焼結体又は、これらをＣＶＤ法等により表面被覆したものが耐食性に優れるとして使用されている。また、グラファイトや窒化硼素を被覆したヒータ等も使用されている。 Further, during semiconductor manufacturing, alumina sintered bodies, sapphire, AlN sintered bodies, or those obtained by surface coating these by CVD or the like are used as susceptor materials for supporting and fixing semiconductors because they have excellent corrosion resistance. In addition, a heater coated with graphite or boron nitride is also used.
しかしながら、従来から用いられているガラスや石英ではプラズマ中の耐食性が不充分で消耗が激しく、特にフッ素や塩素プラズマに接すると接触面がエッチングされ、表面性状が変化したり、光透過性が必要とされる部材では、表面が次第に白く曇って透光性が低下する等の問題が生じていた。 However, conventionally used glass and quartz have insufficient corrosion resistance in the plasma and are very exhausted, especially when they come into contact with fluorine or chlorine plasma, the contact surface is etched, the surface properties change, and light transmittance is required. In the member, the surface gradually becomes white and cloudy, resulting in a problem that the translucency is lowered.
また、ステンレスなどの金属を使用した部材でも耐食性が不充分なため、腐食によってパーティクルが発生し、特に半導体製造においては不良品発生の原因となる。さらに、窒化硼素はハロゲン系ガスと反応してガス化し、コンタミネーションの原因となっていた。 Further, even a member using a metal such as stainless steel has insufficient corrosion resistance, so that particles are generated due to corrosion, and in particular, in semiconductor manufacturing, it may cause defective products. Further, boron nitride reacts with the halogen-based gas and gasifies, causing contamination.
特に、アルミナ、ＡｌＮの焼結体は、あらゆる形状品に適用できることからその有用性が高い。アルミナ、ＡｌＮ自体は、ＳｉＯ２系材料や金属に比較してハロゲン系ガスに対して耐食性に優れるものの、高温でプラズマと接すると腐食が徐々に進行して、しまいには焼結体の表面からアルミナやＡｌＮの結晶粒子の脱粒が生じ、パーティクル発生の原因になるという問題が生じている。 In particular, the sintered body of alumina and AlN is highly useful because it can be applied to any shape product. Alumina and AlN itself are superior in corrosion resistance to halogen-based gases compared to SiO 2 -based materials and metals, but corrosion gradually proceeds when in contact with plasma at high temperatures, and eventually from the surface of the sintered body There is a problem in that the crystal grains of alumina and AlN are shattered, which causes generation of particles.
また、ＭｇＯやＹ３Ａｌ５Ｏ１２等の周期律表第２ａ、３ａ族含有酸化物を主結晶相とする焼結体は、単味では優れた耐食性を有するが、焼結体においては、プラズマによってその粒界が選択的にエッチングされてしまい、焼結体表面が荒れやすくなるという問題があった。 In addition, a sintered body having a main crystal phase of the 2a, 3a group-containing oxides of the periodic table such as MgO and Y 3 Al 5 O 12 has excellent corrosion resistance by itself, but in the sintered body, The grain boundary is selectively etched by the plasma, and there is a problem that the surface of the sintered body is easily roughened.
本発明者らは、ハロゲン系腐食ガスのプラズマに対する耐食性を具備するセラミック焼結体の具体的な構成について検討を重ねた結果、特に焼結体材料の場合には、主結晶粒子に比較して粒界相が腐食され易いことから、主結晶粒子自体の耐食性が良好であっても、粒界相腐食の進行によって焼結体表面の主結晶粒子の脱粒が生じ、パーティクルの発生、さらには材料自体の耐食性低下を引き起こすことがわかった。 As a result of repeated studies on the specific structure of the ceramic sintered body having corrosion resistance to the plasma of the halogen-based corrosive gas, the present inventors have compared with the main crystal particles, particularly in the case of the sintered body material. Since the grain boundary phase is easily corroded, even if the main crystal particles themselves have good corrosion resistance, the main crystal particles on the surface of the sintered body are shattered due to the progress of the grain boundary phase corrosion, and the generation of particles and further the material It has been found that it causes a decrease in its corrosion resistance.
そこで、本発明者らは、粒界相の耐食性を高めるための方法について検討を重ねた結果、主結晶相をＡｌ ２ Ｏ ３ またはＮｉＡｌ ２ Ｏ ４ により形成するとともに、粒界相を前記主結晶相と同等以上の耐食性を有し、前記主結晶と異なる酸化物により構成することによって、粒界相の腐食の進行を抑制し、粒界相の腐食による結晶子の脱粒、それに起因するパーティクルの発生の防止、および材料自体の耐食性を高めることが可能となることを知見し、本発明に至った。 Accordingly, the present inventors have made extensive investigations on how to improve the corrosion resistance of the grain boundary phase, the main crystalline phase and forming the Al 2 O 3 or NiAl 2 O 4, the grain boundary phase before Symbol main Corrosion resistance equal to or higher than that of the crystal phase, and composed of an oxide different from that of the main crystal, suppresses the progress of corrosion of the grain boundary phase, and crystal grain detachment due to corrosion of the grain boundary phase. prevention of the occurrence, and the corrosion resistance of the material itself was found that it is possible to Rukoto increased, leading to the present invention.
即ち、本発明のプラズマプロセス装置用部材は、ハロゲン系腐食ガスのプラズマに曝される部位を、Ａｌ ２ Ｏ ３ からなる主結晶相と、ＮｉＡｌ ２ Ｏ ４ からなる粒界相とを具備するセラミック焼結体により構成するか、またはＮｉＡｌ ２ Ｏ ４ からなる主結晶相と、ＭｇＯからなる粒界相とを具備するセラミック焼結体により構成したことを特徴とする。 That is, the plasma processing apparatus member of the present invention, a portion exposed to plasma of the halogen-based corrosive gas, comprising a main crystal phase of Al 2 O 3, and Ru NiAl 2 O 4 Tona particle Sakaisho or constituted by a ceramic sintered body, or a main crystal phase consisting of NiAl 2 O 4, characterized in that it is constituted by a ceramic sintered body and a grain boundary phase composed of MgO.
本発明のプラズマプロセス装置用部材は、上記の知見に基づき完成されたものであり、ハロゲン系腐食ガスのプラズマに曝される部位を、Ａｌ ２ Ｏ ３ 又はＮｉＡｌ ２ Ｏ ４ を主結晶とするセラミック焼結体により構成するとともに、該セラミック焼結体の粒界相を、前記主結晶相と同等以上の耐食性を有し、前記主結晶と異なるＮｉＡｌ ２ Ｏ ４ 又はＭｇＯにより形成したことにより、セラミック焼結体の粒界腐食の進行、パーティクルの発生を抑制し、焼結体材料自体の耐食性向上を図る事が出来る。 The member for a plasma processing apparatus of the present invention has been completed based on the above-mentioned knowledge, and the part exposed to the plasma of the halogen-based corrosive gas is a ceramic having Al 2 O 3 or NiAl 2 O 4 as a main crystal. together constituting a sintered body, the grain boundary phase of the sintered ceramic body, prior to Symbol main has a crystal phase equal to or higher than corrosion resistance, by forming a different NiAl 2 O 4 or MgO and the main crystal, The progress of intergranular corrosion and generation of particles in the ceramic sintered body can be suppressed, and the corrosion resistance of the sintered body material itself can be improved.
以上詳述したとおり、本発明のプラズマプロセス装置用部材は、ハロゲン系の腐食性ガスのプラズマに曝される部位を構成するセラミック焼結体が高い耐食性を有し、且つ粒界相が主結晶相と同等以上の耐食性を有し、主結晶相と異なる高耐食性酸化物からなるため、粒界の腐食を抑制し、脱粒やそれに起因するパーティクルの発生を防止することが可能となる。具体的には、プラズマ処理装置や液晶製造用部材、ウェハ固定用クランプリングやエッチング装置の上部電極周りのシールドリング等の半導体製造装置用部材に使用することによって部材の長寿命化、特に半導体製造用部材として使用する場合には、半導体の歩留り向上を図ることが出来る。 As described above in detail, the plasma processing apparatus member of the present invention has a high corrosion resistance in the ceramic sintered body constituting the portion exposed to the plasma of the halogen-based corrosive gas, and the grain boundary phase is the main crystal. has a phase equal to or higher than corrosion resistance, to become a main crystal phase different high corrosion resistance oxide, and inhibit corrosion of grain boundaries, it is possible to prevent the generation of particles caused by the shattering or it. Specifically, it can be used for semiconductor manufacturing equipment members such as plasma processing equipment, liquid crystal manufacturing equipment, wafer fixing clamp rings and shield rings around the upper electrode of etching equipment, especially for semiconductor manufacturing. When used as a member, the yield of semiconductors can be improved.
本発明のプラズマプロセス装置用部材は、ハロゲン系の腐食ガスのプラズマに曝される部材であり、ハロゲン系腐食ガスとしては、ＳＦ６、ＣＦ４、ＣＨＦ３、ＣｌＦ３、ＮＦ３、ＨＦ等のフッ素系ガス、Ｃｌ２、ＨＣｌ、ＢＣｌ３等の塩素系ガス、Ｂｒ２、ＨＢｒ、ＢＢｒ３等の臭素系ガス、ＨＩ等のヨウ素系ガス等であり、これらのガスが導入された雰囲気にマイクロ波や高周波を導入したり、あるいはガスの解離電圧以上の電位差を加えることによりこれらのガスがプラズマ化される。 The member for a plasma processing apparatus of the present invention is a member that is exposed to plasma of a halogen-based corrosive gas, and examples of the halogen-based corrosive gas include SF 6 , CF 4 , CHF 3 , ClF 3 , NF 3 , and HF. Fluorine gas, chlorine gas such as Cl 2 , HCl, BCl 3 , bromine gas such as Br 2 , HBr, BBr 3 , iodine gas such as HI, etc. These gases are turned into plasma by introducing waves or high frequencies, or by applying a potential difference equal to or greater than the gas dissociation voltage.
本発明によれば、この様なハロゲン系腐食ガスのプラズマに曝されるプラズマプロセス装置用部材として、Ａｌ ２ Ｏ ３ 又はＮｉＡｌ ２ Ｏ ４ を主結晶相とするセラミック焼結体により構成する。 According to the present invention, the member for a plasma processing apparatus that is exposed to the plasma of such a halogen-based corrosive gas is composed of a ceramic sintered body having Al 2 O 3 or NiAl 2 O 4 as a main crystal phase.
本発明によれば、上記のセラミック焼結体において、上記主結晶粒子がＡｌ ２ Ｏ ３ であるときには、上記主結晶粒子の粒界相を、ＮｉＡｌ ２ Ｏ ４ により形成し、上記主結晶粒子がＮｉＡｌ ２ Ｏ ４ であるときには、上記主結晶粒子の粒界相を、ＭｇＯにより形成する。セラミック焼結体の粒界は、一般に粒子と比較して高蒸気圧、易腐食性であり、この性質により粒界の化学的エッチングやサーマルエッチングが可能となる。その為、腐食雰囲気等に曝された場合、主結晶粒子よりも粒界の腐食進行が早く、脱粒やパーティクル発生の原因となる。そこで、粒界相を耐食性が主結晶粒子と同等、好ましくは主結晶粒子よりも優れた物質で形成して強化することにより、粒界相の腐食の進行を抑制し、粒界相の腐食による結晶子の脱粒・パーティクルの発生を防止する事が可能となる。 According to the present invention, in the ceramic sintered body, when the main crystal particle is Al 2 O 3 , a grain boundary phase of the main crystal particle is formed of NiAl 2 O 4 , and the main crystal particle is When NiAl 2 O 4 is used, the grain boundary phase of the main crystal grains is formed of MgO . Grain boundaries of the ceramic sintered body is generally compared to particles high vapor pressure, easily corrosive, it is possible to chemically etch or service over Mar etching of the grain boundaries by this property. For this reason, when exposed to a corrosive atmosphere or the like, the progress of corrosion at the grain boundary is faster than that of the main crystal particles, which causes degranulation and generation of particles. Therefore, by forming and strengthening the grain boundary phase with a material having corrosion resistance equivalent to that of the main crystal particles, preferably better than that of the main crystal particles, the progress of the corrosion of the grain boundary phase is suppressed, and the corrosion of the grain boundary phase is caused. It is possible to prevent crystal grain detachment and particle generation.
このセラミック焼結体の粒界を構成するＮｉＡｌ ２ Ｏ ４ 又はＭｇＯは、結晶質、ガラス質のいずれでもよいが、耐食性の点からは結晶相を含むことが望ましい。 NiAl 2 O 4 or MgO constituting the grain boundary of this ceramic sintered body may be either crystalline or glassy, but it is desirable to include a crystalline phase from the viewpoint of corrosion resistance.
この様な耐食性のセラミック焼結体を作製するには、主結晶粒子がＮｉＡｌ ２ Ｏ ４ である場合、添加物としてＭｇＯを添加し、また主結晶粒子がＡｌ ２ Ｏ ３ である場合、添加物としてＡｌ ２ Ｏ ３ と反応して粒界にＮｉＡｌ ２ Ｏ ４ が生成されるようにＮｉＯを添加する。 When To produce a ceramic sintered body such corrosion resistance, when the main crystal grains is NiAl 2 O 4, MgO is added as an additive, or the main crystal grains, Al 2 O 3, is added reacts with for Al 2 O 3 things Ru added pressure to the NiO as NiAl 2 O 4 is produced at the grain boundaries.
焼結体は、上記各種の組み合わせにより組成物からなる粉末を成形し、焼成した焼結体、反応焼結体、或いは周知のゾルゲル法で液相を塗布し焼成した膜であっても良い。 The sintered body may be a sintered body obtained by molding a powder composed of the composition by the above-described various combinations, fired, a reaction sintered body, or a film obtained by applying a liquid phase by a known sol-gel method and firing.
また、必要に応じて上記以外に焼結を促進するための助剤を添加することもできる。 Also, it is possible to add auxiliaries for promoting the sintering in addition to the above if necessary.
なお、粒界を構成する酸化物は、酸化物換算で１〜３０重量％の割合で添加するのが適当である。 In addition, it is appropriate to add the oxide which comprises a grain boundary in the ratio of 1 to 30 weight% in conversion of an oxide.
この様な原料組成物を、所望の形状に成形、或いは所定基体に塗布して焼成する。成形方法としては、通常の乾式プレス、静水圧プレス、鋳込み成形、押し出し成形、シート状成形等、目的形状を得るのに適した成形方法を利用出来る。 Such a raw material composition is molded into a desired shape, or applied to a predetermined substrate and fired. As a molding method, a molding method suitable for obtaining a target shape, such as a normal dry press, hydrostatic press, cast molding, extrusion molding, or sheet molding, can be used.
成形体は、材料に応じて緻密化に適した雰囲気、圧力、温度で焼成すればよい。必要であれば１０００〜２０００気圧の不活性ガス中で熱処理する熱間静水圧法によって焼結すると、焼結体中の気孔を１体積％以下にまで消失することができ、これにより耐食性を高めることができる。 The formed body may be fired in an atmosphere, pressure, and temperature suitable for densification depending on the material. If necessary, when sintered by a hot isostatic pressure method in which heat treatment is performed in an inert gas at 1000 to 2000 atmospheres, pores in the sintered body can be lost to 1% by volume or less, thereby improving corrosion resistance. be able to.
また、焼成後の焼結体表面に荒れ等が発生する場合には、焼結体の少なくともプラズマに接触する表面を周知の研磨処理によって表面粗さ１μｍ以下まで鏡面研磨処理することで耐食性を高めることができる。 Further, in the case where roughness or the like occurs on the surface of the sintered body after firing, the corrosion resistance is improved by mirror-polishing the surface roughness of the sintered body to a surface roughness of 1 μm or less by a known polishing process. be able to.
実施例１
表１に示すような種々の酸化物からなる焼結体試料を作製した。これらの試料は、母相となるＡｌ ２ Ｏ ３ の高純度粉末（９９．９％以上）又はＮｉＡｌ ２ Ｏ ４ にＭｇＯ、ＮｉＯを加えて混合し、プレス成形した後、１３００〜１８００℃で焼成した相対密度９８％以上の焼結体である。また、比較例として、ＳｉＯ ２ を加えた試料を準備した。また、試料のプラズマ照射面はあらかじめ鏡面処理を施し表面粗さ１μｍ以下とした。これらの試料をＲＩＥプラズマエッチング装置内に設置して、この装置内にＨＣｌガスを導入し、高周波にてプラズマを発生させ、室温（２５℃）で塩素プラズマ照射テストを行なった。装置内圧力は１０Ｐａに保持し、１３．５６ＭＨｚ、１ｋＷの高周波を利用した。上記の条件下で、３時間エッチング処理を行った後の表面状態を目視および光学顕微鏡で観察し、その結果を表１に示した。なお粒界相の成分についてはＸ線マイクロアナライザーによって同定した。テスト結果を表１に示す。
The sintered compact sample which consists of various oxides as shown in Table 1 was produced. These samples are made of Al 2 O 3 high-purity powder (99.9% or more) or NiAl 2 O 4 as a parent phase, mixed with MgO and NiO, press-molded, and then fired at 1300 to 1800 ° C. The sintered body has a relative density of 98% or more. As a comparative example, were prepared samples plus SiO 2. Further, the plasma irradiation surface of the sample was mirror-treated in advance so that the surface roughness was 1 μm or less. By installing these samples in the RIE plasma etching apparatus, by introducing HCl gas into the apparatus, plasma is generated at a high frequency, becomes the row chlorine plasma irradiation test at room temperature (25 ° C.). The pressure inside the apparatus was maintained at 10 Pa, and a high frequency of 13.56 MHz and 1 kW was used. The surface condition after performing the etching treatment for 3 hours under the above conditions was observed visually and with an optical microscope, and the results are shown in Table 1. The grain boundary phase components were identified by an X-ray microanalyzer. The test results are shown in Table 1 .
塩素プラズマを照射すると、試料Ｎｏ．１、３の粒界相がＳｉＯ ２ やＳｉＯ ２ とＡｌ ２ Ｏ ３ からなるものは、脱粒・パーティクル発生が起きていた。これに対し、試料Ｎｏ．２、４はその傾向が抑制され、脱粒は見られなかった。 When irradiated with chlorine plasma, sample no. When the grain boundary phases 1 and 3 were composed of SiO 2 , SiO 2, and Al 2 O 3 , degranulation and particle generation occurred. In contrast, sample no. In 2 and 4, the tendency was suppressed, and degranulation was not observed.
実施例２
実施例１と同様にして作製した表２の各試料に対して、ＲＩＥプラズマエッチング装置内にＨＢｒガスを導入し、高周波にてプラズマを発生させ、室温で臭素プラズマ照射テストを行なった。装置内圧力は１０Ｐａに保持し、１３．５６ＭＨｚ、１ｋＷの高周波を利用した。評価法は実施例１と同様である。テスト結果を表２に示す。
For each sample in Table 2 was prepared in the same manner as in Example 1, by introducing HBr gas into the RIE plasma etching apparatus, plasma is generated at a high frequency, it becomes the row bromine plasma irradiation test at room temperature. The pressure inside the apparatus was maintained at 10 Pa, and a high frequency of 13.56 MHz and 1 kW was used. The evaluation method is the same as in Example 1. The test results are shown in Table 2 .
臭素プラズマを照射すると、塩素の場合と同様に粒界相がＳｉＯ ２ からなる試料Ｎｏ．５は、粒界の腐食が局所的に進行し、脱粒・パーティクル発生が起きていた。これに対し、試料Ｎｏ．６は上記の粒界の腐食が抑制され、若干の曇りは生じても脱粒は見られなかった。 Upon irradiation with bromine plasma sample grain boundary phase as in the case of chlorine consists SiO 2 No. In No. 5, grain boundary corrosion locally progressed and degranulation and particle generation occurred. In contrast, sample no. In No. 6, the above grain boundary corrosion was suppressed, and even though some clouding occurred, no degranulation was observed.
実施例３
実施例１と同様にして作製した表３の各試料に対して、ＲＩＥプラズマエッチング装置内にＨＩガスを導入し、高周波にてプラズマを発生させ、室温でヨウ素プラズマ照射テストを行なった。装置内圧力は１０Ｐａに保持し、１３．５６ＭＨｚ、１ｋＷの高周波を利用した。評価法は実施例１と同様である。テスト結果を表３に示す。
For each sample in Table 3 were prepared in the same manner as in Example 1, introducing HI gas into the RIE plasma etching apparatus, plasma is generated at a high frequency, it becomes the row iodine plasma irradiation test at room temperature. The pressure inside the apparatus was maintained at 10 Pa, and a high frequency of 13.56 MHz and 1 kW was used. The evaluation method is the same as in Example 1. Table 3 shows the test results.
ヨウ素プラズマを照射すると、他のハロゲンプラズマの場合と同様に粒界相がＳｉＯ ２ からなる試料Ｎｏ．７は、局所的に粒界の腐食が進行し、脱粒・パーティクル発生が起きていた。これに対し、試料Ｎｏ．８は、その傾向が抑制され、若干の曇りは生じても脱粒は見られなかった。 Upon irradiation with iodine plasma, samples for other halogen plasma as well as the grain boundary phase consists SiO 2 No. In No. 7 , grain boundary corrosion locally progressed, and degranulation and particle generation occurred. In contrast, sample no. In No. 8, the tendency was suppressed, and even though some clouding occurred, no degranulation was observed .
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