JP4522117B2 - Method for manufacturing processing container member used in semiconductor or liquid crystal manufacturing apparatus - Google Patents

Method for manufacturing processing container member used in semiconductor or liquid crystal manufacturing apparatus Download PDF

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JP4522117B2
JP4522117B2 JP2004084273A JP2004084273A JP4522117B2 JP 4522117 B2 JP4522117 B2 JP 4522117B2 JP 2004084273 A JP2004084273 A JP 2004084273A JP 2004084273 A JP2004084273 A JP 2004084273A JP 4522117 B2 JP4522117 B2 JP 4522117B2
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molded body
ceramic molded
firing
abrasive grains
ceramic
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JP2005272161A (en
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秀則 山之口
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Kyocera Corp
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本発明は、ＣＶＤやＰＶＤのような成膜装置やエッチング装置等において、腐食性ガスやプラズマに曝される部位に使用される半導体もしくは液晶製造装置に用いられる処理容器用部材の製造方法に関する。   The present invention relates to a method of manufacturing a member for a processing vessel used in a semiconductor or liquid crystal manufacturing apparatus used in a part exposed to corrosive gas or plasma in a film forming apparatus or an etching apparatus such as CVD or PVD.

半導体デバイスの製造プロセスにおけるＰＶＤやＣＶＤのような成膜工程やエッチング工程では、一般的にフッ素系や塩素系等種々の腐食性ガスをプラズマ化させて半導体ウェハ上に成膜や微細加工が施される。このような製造プロセスにおける半導体製造装置に用いられる処理容器用部材は、プラズマ化したガスによる腐食が少ないように、石英や耐食性の強いアルミナ，ＹＡＧ（イットリウム・アルミニウム・ガーネット），イットリア，窒化アルミニウム，炭化珪素および窒化珪素などのセラミックスからなる部材が使用されている。   In film formation processes and etching processes such as PVD and CVD in the manufacturing process of semiconductor devices, various corrosive gases such as fluorine and chlorine are generally turned into plasma to perform film formation and fine processing on semiconductor wafers. Is done. The processing vessel member used in the semiconductor manufacturing apparatus in such a manufacturing process is made of quartz, strong corrosion-resistant alumina, YAG (yttrium, aluminum, garnet), yttria, aluminum nitride, so as to reduce corrosion caused by plasma gas. Members made of ceramics such as silicon carbide and silicon nitride are used.

図４は、上記の処理容器用部材が適用された誘導結合型プラズマエッチング装置を示す断面図である。処理容器用部材５はドーム状をなし、その下に金属製の下部チャンバー６１が処理容器用部材５に密着するように設けられており、これらによりチャンバーが構成されている。下部チャンバー６１内の上部にはＲＦ電極が接続された支持テーブル６２が配置され、その上に静電チャック６３が設けられており、静電チャック６３の電極に直流電圧を印加することにより静電チャック６３上に半導体ウェハ６４を静電吸着することができる。また、下部チャンバー６１の底部には真空ポンプ６７が接続されており、チャンバー６１内を真空排気することができる。また、下部チャンバー６１の上部には、半導体ウェハ６４の上方にエッチングガス例えばＣＦ４ガスを供給するガス供給ノズル６５が設けられている。処理容器用部材５の周囲には誘導コイル６６が設けられており、この誘導コイル６６にはＲＦ電源から例えば４００ｋＨｚの高周波が印加される。
この誘導結合型プラズマエッチング装置においては、真空ポンプ６７によりチャンバー６１内を所定の真空度まで排気し、静電チャック６３により半導体ウェハ６４を静電吸着した後、ノズル６５からエッチングガスとして例えばＣＦ４ガスを供給しつつ、ＲＦ電源から誘導コイル６６に給電することにより、半導体ウェハ６４の上方部分にエッチングガスのプラズマが形成され、所定のパターンに半導体ウェハ６４がエッチングされることとなる。
このようなエッチング処理の際、プラズマからの衝撃を受ける処理容器用部材５の表面は、フッ化物膜等が付着したり堆積したりするので、このフッ化物膜等が半導体ウェハ６４上に剥がれ落ちてパーティクルとなるのを防止するため、処理容器用部材５の表面に粗面部５１が形成されている。 FIG. 4 is a cross-sectional view showing an inductively coupled plasma etching apparatus to which the processing container member is applied. The processing container member 5 is formed in a dome shape, and a metal lower chamber 61 is provided below the processing container member 5 so as to be in close contact with the processing container member 5, thereby forming a chamber. A support table 62 to which an RF electrode is connected is disposed in the upper part of the lower chamber 61, and an electrostatic chuck 63 is provided on the support table 62, and a electrostatic voltage is applied by applying a DC voltage to the electrode of the electrostatic chuck 63. The semiconductor wafer 64 can be electrostatically adsorbed on the chuck 63. A vacuum pump 67 is connected to the bottom of the lower chamber 61 so that the inside of the chamber 61 can be evacuated. In addition, a gas supply nozzle 65 for supplying an etching gas such as CF 4 gas is provided above the semiconductor wafer 64 above the lower chamber 61. An induction coil 66 is provided around the processing container member 5, and a high frequency of 400 kHz, for example, is applied to the induction coil 66 from an RF power source.
In this inductively coupled plasma etching apparatus, the inside of the chamber 61 is evacuated to a predetermined degree of vacuum by the vacuum pump 67, the semiconductor wafer 64 is electrostatically adsorbed by the electrostatic chuck 63, and then, for example, CF 4 is used as an etching gas from the nozzle 65. By supplying power to the induction coil 66 from the RF power supply while supplying the gas, etching gas plasma is formed in the upper portion of the semiconductor wafer 64, and the semiconductor wafer 64 is etched into a predetermined pattern.
During such an etching process, a fluoride film or the like adheres or accumulates on the surface of the processing container member 5 that receives an impact from the plasma, and the fluoride film or the like peels off on the semiconductor wafer 64. In order to prevent the particles from becoming particles, a rough surface portion 51 is formed on the surface of the processing container member 5.

従来、処理容器用部材５の表面に粗面部５１を形成する方法としては、ブラスト処理を施す方法が知られており、図５に示すようにブラスト処理装置を用いて、ノズル７よりエアー圧力により噴射した砥粒８を焼結後のセラミック部材（処理容器用部材５）に衝突させることによって粗面部５１を形成することができる（特許文献１参照）。また、ラバープレス成形法において、使用する金型の表面を同様にブラスト処理し、転写する方法が知られている（特許文献１参照）。
特開２００１−１０２３６５号公報 Conventionally, as a method for forming the rough surface portion 51 on the surface of the processing container member 5, a method of performing a blasting process is known. As shown in FIG. The rough surface portion 51 can be formed by causing the sprayed abrasive grains 8 to collide with the sintered ceramic member (processing container member 5) (see Patent Document 1). Moreover, in the rubber press molding method, a method is also known in which the surface of a mold to be used is similarly blasted and transferred (see Patent Document 1).
JP 2001-102365 A

しかしながら、焼結後のセラミック部材（処理容器用部材５）の表面にブラスト処理装置を用いて粗面部５１を形成する場合、電融アルミナや炭化珪素質からなるグリーンカーボン（以下「ＧＣ」という）等の砥粒８を衝突させて物理的に破砕するため、図６に示すように、長さ１〜５μｍの微細クラック５２が無数に発生してしまう。そして、これらの砥粒８がその微細クラック５２に咬み込み、半導体デバイスの製造プロセス中に処理容器用部材５が高温により熱膨張し微細クラック５２が進展した場合には、砥粒８や処理容器用部材５のセラミックスの微小片がウェハ上に落ちて、パーティクルとなるという問題があった。特にプラズマに対する耐食性に優れるＹＡＧ（イットリウム・アルミニウム・ガーネット）やイットリアは、一般的にアルミナよりも強度、破壊靭性値が低く、微細クラック５２が生じやすかった。
また、ラバープレスにおける金型の面粗さを大きくし、転写する方法では、実際には成形時に１００ＭＰａ程の圧力により成形される為、金型と成形体とはかなり密着された状態となり、成形体を金型から引き離すときに密着面を粗くすると離れにくくなり、金型表面に成形体の一部が付着してしまい、所望の形状を得られなかった。
本発明は、上記事情に鑑みてなされたものであって、半導体もしくは液晶デバイス製造プロセス中に砥粒やセラミックスの微小片が半導体ウェハもしくは液晶のガラス基板上に落ちてパーティクルとなるのを防止する半導体もしくは液晶製造装置に用いられる処理容器用部材の製造方法を提供することを目的とする。 However, when the rough surface portion 51 is formed on the surface of the sintered ceramic member (processing vessel member 5) using a blast processing apparatus, green carbon (hereinafter referred to as "GC") made of fused alumina or silicon carbide. Since the abrasive grains 8 such as the above collide with each other and are physically crushed, an infinite number of fine cracks 52 having a length of 1 to 5 μm are generated as shown in FIG. And when these abrasive grains 8 bite into the fine cracks 52 and the process vessel member 5 is thermally expanded due to high temperature and the fine cracks 52 are developed during the manufacturing process of the semiconductor device, the abrasive grains 8 and the process containers There was a problem that the ceramic fine pieces of the member 5 fell on the wafer and became particles. In particular, YAG (yttrium, aluminum, garnet) and yttria, which are excellent in corrosion resistance to plasma, generally have lower strength and fracture toughness than alumina, and fine cracks 52 are likely to occur.
In addition, in the method of increasing and transferring the surface roughness of the mold in the rubber press, the mold and the molded body are in a state of being in close contact with each other because the mold is actually formed with a pressure of about 100 MPa at the time of molding. If the adhesion surface is roughened when the body is pulled away from the mold, it becomes difficult to separate, and a part of the molded body adheres to the mold surface, and a desired shape cannot be obtained.
The present invention has been made in view of the above circumstances, and prevents particles of abrasive grains or ceramics from falling on a semiconductor wafer or liquid crystal glass substrate into particles during the semiconductor or liquid crystal device manufacturing process. It aims at providing the manufacturing method of the member for processing containers used for a semiconductor or a liquid crystal manufacturing apparatus.

本発明は、ドーム状に形成され、開口部内に粗面部を有するセラミックス製の半導体もしくは液晶製造装置に用いられる処理容器用部材の製造方法であって、焼成前のセラミック成形体の外壁形状が転写された凹みであって、曲面状の底面を支えるとともに、側面の外径部まで嵌め込むことのできる凹みを有する焼成治具を用い、該焼成治具に前記セラミック成形体の前記開口部を上方に向けて載置し、前記セラミック成形体と同材質で平均粒径が５０〜２００μｍの砥粒もしくは有機物からなる平均粒径が２００〜６００μｍの砥粒を用いて、０．３〜０．５ＭＰａの噴射圧力で前記セラミック成形体の前記開口部内にブラスト処理を施した後、前記焼成治具に前記セラミック成形体を載置したまま焼成することを特徴とする。
なお、本発明における半導体もしくは液晶製造装置に用いられる処理容器用部材とは、半導体製造装置にも液晶製造装置にも利用可能であることを意味する。
The present invention relates to a method of manufacturing a member for a processing container used in a ceramic semiconductor or liquid crystal manufacturing apparatus formed in a dome shape and having a rough surface in an opening, wherein the outer wall shape of the ceramic molded body before firing is transferred a a recess is, with supporting a curved bottom surface, with a firing jig having a recess can be fitted to the outer diameter portion of the side surface, the upper and the opening of the ceramic molded body該焼Seiji tool Using an abrasive having the same material as that of the ceramic molded body and having an average particle diameter of 50 to 200 μm or an abrasive having an average particle diameter of 200 to 600 μm made of an organic substance, 0.3 to 0.5 MPa A blasting process is performed in the opening of the ceramic molded body at an injection pressure of, and then the ceramic molded body is fired while being placed on the firing jig.
In addition, the member for processing containers used for the semiconductor or liquid crystal manufacturing apparatus in the present invention means that it can be used for both the semiconductor manufacturing apparatus and the liquid crystal manufacturing apparatus.

本発明の半導体もしくは液晶製造装置に用いられる処理容器用部材の製造方法によれば、粗面部における微細クラックを防止し、腐食性ガス雰囲気に曝されても、砥粒やセラミックスの微小片が脱落することがないので、半導体ウェハもしくは液晶のガラス基板上へのパーティクルを減少させることができる。
また、平均粒径が５０〜２００μｍのセラミック成形体と同材質の砥粒、または、平均粒径が２００〜６００μｍの有機物からなる砥粒を用いることにより、よりパーティクルの発生を低減させることができる。
また、上記粒径の砥流において、ブラスト処理を施すときの噴射圧力が０．３〜０．５ＭＰａであることにより、良好な粗面部を得ることが可能である。
また、焼成前のセラミック成形体の外壁形状が転写されて、曲面状の底面を支えるとともに、側面の外径部まで嵌め込むことのできる凹みを有する焼成治具を用い、該焼成治具に前記セラミック成形体の前記開口部を上方に向けて載置し、上記粒径の砥粒を用いるとともに上記噴射圧力で前記セラミック成形体の前記開口部内にブラスト処理を施した後、前記焼成治具に前記セラミック成形体を載置したまま焼成することにより、ブラスト処理を施して粗面部とする際に発生するセラミック成形体の反りや変形を防止することができ、さらに焼成時の収縮による変形を防止することができる。
According to the method for manufacturing a processing container member used in a semiconductor or liquid crystal manufacturing apparatus of the present invention, fine cracks in a rough surface portion are prevented, and even when exposed to a corrosive gas atmosphere, abrasive grains and ceramic fine pieces fall off. Therefore, particles on the semiconductor wafer or liquid crystal glass substrate can be reduced.
Moreover, generation | occurrence | production of a particle can be reduced more by using the abrasive grain of the same material as a ceramic molded object with an average particle diameter of 50-200 micrometers, or the abrasive grain which consists of an organic substance with an average particle diameter of 200-600 micrometers. .
In addition, in the abrasive flow having the above particle diameter , a good rough surface portion can be obtained when the injection pressure when performing the blasting treatment is 0.3 to 0.5 MPa.
Further, the outer wall shape of the ceramic molded body before firing is transferred, and a firing jig having a recess that can be fitted to the outer diameter part of the side surface while supporting the curved bottom surface is used for the firing jig. The ceramic molded body is placed with the opening facing upward, abrasive grains having the above-mentioned particle diameter are used , and blasting is performed in the opening of the ceramic molded body with the spraying pressure. By firing with the ceramic molded body placed, it is possible to prevent warping and deformation of the ceramic molded body that occurs when the blast treatment is performed to form a rough surface portion, and also prevents deformation due to shrinkage during firing. can do.

以下、本発明の実施形態を図面に基づいて説明する。
本発明は、ドーム状に形成され、開口部内に粗面部を有するセラミックス製の半導体もしくは液晶製造装置に用いられる処理容器用部材の製造方法であって、焼成前のセラミック成形体の外壁形状が転写された凹みであって、曲面状の底面を支えるとともに、側面の外径部まで嵌め込むことのできる凹みを有する焼成治具を用い、該焼成治具に前記セラミック成形体の前記開口部を上方に向けて載置し、前記セラミック成形体と同材質の砥粒もしくは有機物からなる平均粒径が２００〜６００μｍの砥粒を用いて、０．３〜０．５ＭＰａの噴射圧力で前記セラミック成形体の前記開口部内にブラスト処理を施した後、前記焼成治具に前記セラミック成形体を載置したまま焼成することを特徴とするものである。
Hereinafter, embodiments of the present invention will be described with reference to the drawings.
The present invention relates to a method of manufacturing a member for a processing container used in a ceramic semiconductor or liquid crystal manufacturing apparatus formed in a dome shape and having a rough surface in an opening, wherein the outer wall shape of the ceramic molded body before firing is transferred a a recess is, with supporting a curved bottom surface, with a firing jig having a recess can be fitted to the outer diameter portion of the side surface, the upper and the opening of the ceramic molded body該焼Seiji tool placed toward, said average particle size of a ceramic formed body of the same material abrasive or organic matter is by using abrasive grains of 200 to 600 [mu] m, the ceramic molded body in injection pressure 0.3~0.5MPa After the blast treatment is performed in the opening, the ceramic molded body is fired while being placed on the firing jig.

図１に示すように、セラミック成形体１は、セラミックスからなるドーム状の部材である。このセラミック成形体１は、セラミック原料をこのセラミック成形体１の内面を模した芯金が挿入されたゴム型内に充填し、これをゴム蓋やシール用テープを使用して密封し、湿式静水圧水槽内へ浸漬して、約１００ＭＰａの圧力で成形することで得られる。なお、セラミック原料は、アルミナ，ＹＡＧ（イットリウム・アルミニウム・ガーネット），イットリア，窒化アルミニウム，炭化珪素および窒化珪素などの主成分に、ＰＥＧ，ＰＶＡの成形助剤および焼結助剤が含まれたスラリーを、ボールミルで混合・粉砕し、スプレードライ乾燥により得られた顆粒状のものである。そして、このセラミック成形体１をゴム型より取り出し、旋盤やフライス盤を使用して外面を加工し、さらにマシニングセンターなどを使用して目的の形状に切削加工する。このとき、後述のブラスト処理により粗面部１１となるセラミック成形体１の開口部内の表面は、ある程度目的とする形状に近似した形状に成形されてはいるが、微妙な収縮率の違いなどを補正するために、若干の切削加工を施しても良い。   As shown in FIG. 1, the ceramic molded body 1 is a dome-shaped member made of ceramics. In the ceramic molded body 1, a ceramic raw material is filled in a rubber mold in which a core bar imitating the inner surface of the ceramic molded body 1 is inserted, and this is sealed using a rubber lid or a sealing tape, and wet-static. It is obtained by being immersed in a hydraulic water tank and molded at a pressure of about 100 MPa. The ceramic raw material is a slurry in which main components such as alumina, YAG (yttrium, aluminum, garnet), yttria, aluminum nitride, silicon carbide, and silicon nitride are included and a molding aid and a sintering aid of PEG and PVA. Are granulated by mixing and grinding with a ball mill and spray drying. Then, the ceramic molded body 1 is taken out from the rubber mold, the outer surface is processed using a lathe or a milling machine, and further cut into a target shape using a machining center or the like. At this time, the surface in the opening of the ceramic molded body 1 that becomes the rough surface portion 11 by blasting described later is shaped to a shape that approximates the target shape to some extent, but corrects for a slight difference in shrinkage rate. In order to do so, you may give some cutting.

次に、この切削加工済みのセラミック成形体１の開口部内の表面を粗面部１１とするために、図２に示すように、図１に示すセラミック成形体１の開口部１２を上方に向けて、ブラスト処理装置のノズル３よりエアー圧力により噴射した砥粒２を上方からセラミック成形体１の開口部１２内の表面に衝突させて、ブラスト処理を施す。このブラスト処理装置は乾式のブラスト処理装置で、本来は焼結したガラスの表面に絵柄などを施すための装置であり、一般にセラミックスの焼成後にその表面の面粗さを大きくするためにも使用されている。
焼成前のセラミック成形体１にブラスト処理を施すのは、焼成前のセラミック成形体１が成形助剤などの有機バインダーを含んでおり、焼成後の焼結体に比べて硬度が低いので
、焼成前のセラミック成形体１にブラスト処理を施したときの方が微細クラックを生じにくく、微細クラックが生じたとしてもその後の焼成段階において、表面にガラス成分が析出することにより略修復されるからである。
そして、このブラスト処理のとき、図２に示すように、セラミック成形体１の開口部１２を上方に向けて載置可能に、上部にセラミック成形体１の外壁形状が転写された凹みであって、曲面状の底面を支えるとともに、側面の外径部まで嵌め込むことのできる凹み４１を有する焼成治具４を用いることが重要である。このような形状の焼成治具４を用いて、セラミック成形体１の開口部１２を上方に向け、外径部１３までの部分をこの焼成治具４の凹み４１に嵌め込んだ状態でセラミック成形体１の開口部内にブラスト処理を施すのは、セラミック成形体１を固定できるのみならず、セラミック成形体１の表面の変化によってセラミック成形体１に反りや変形が発生しようとする問題を抑える効果があるからである。 Next, in order to make the surface in the opening of the ceramic molded body 1 that has been processed into a rough surface portion 11, as shown in FIG. 2, the opening 12 of the ceramic molded body 1 shown in FIG. The abrasive grains 2 sprayed by the air pressure from the nozzle 3 of the blasting apparatus are collided with the surface in the opening 12 of the ceramic molded body 1 from above to perform blasting. This blasting device is a dry blasting device, originally intended to apply a pattern to the surface of sintered glass, and is generally used to increase the surface roughness of ceramics after firing. ing.
The ceramic molded body 1 before firing is blasted because the ceramic molded body 1 before firing contains an organic binder such as a molding aid and has a lower hardness than the sintered body after firing. When the previous ceramic molded body 1 is subjected to the blasting treatment, it is less likely to cause fine cracks, and even if the fine cracks are generated, they are substantially restored by precipitation of glass components on the surface in the subsequent firing stage. is there.
At the time of this blasting process, as shown in FIG. 2, it is a recess in which the shape of the outer wall of the ceramic molded body 1 is transferred to the upper part so that the opening 12 of the ceramic molded body 1 can be placed upward. It is important to use the firing jig 4 that has a recess 41 that supports the curved bottom surface and can be fitted to the outer diameter portion of the side surface . Such shapes using firing jig 4, toward the opening 12 of the ceramic molded body 1 upwardly, ceramic molding in a state of fitting the portion up to the outer diameter 13 into the recesses 41 of the firing jig 4 The blasting process in the opening of the body 1 not only can fix the ceramic molded body 1, but also has an effect of suppressing the problem that the ceramic molded body 1 is warped or deformed due to a change in the surface of the ceramic molded body 1. Because there is.

ここで、ブラスト処理に使用される砥粒２としては、セラミック成形体１と同材質の砥粒もしくは有機物からなる砥粒を用いる。   Here, as the abrasive grains 2 used for the blast treatment, abrasive grains made of the same material as the ceramic molded body 1 or abrasive grains made of an organic substance are used.

セラミック成形体１と同材質の砥粒は、セラミックスの一次原料に圧力を加えることなく、１０００〜１７００℃で焼成または仮焼したものである。この砥粒の平均粒径は５０〜２００μｍであることが重要であり、特に７０〜１００μｍであるのが好ましい。５０μｍ未満であると衝撃が小さ過ぎるためブラスト処理の噴射圧力を高くしても粗面部１１とすることが困難となり、また２００μｍを超えると粗面部１１の面粗さが大きくなり過ぎてしまう傾向があるからである。
焼成前のセラミック成形体１にセラミック成形体１と同材質の砥粒を噴射すると、そのセラミック成形体１の硬度が低いために、セラミック成形体１の表面に砥粒が埋め込まれてしまったり、微細クラック中に砥粒が食い込んでしまったりする可能性があるが、砥粒がセラミックス成形体１と同材質であることにより、焼成工程の段階で両者は同化し、砥粒がパーティクルとなることが低減されるという効果を有する。
さらに、このセラミックス成形体１と同材質の砥粒は、その純度が９９％以上であり不純物が１％未満であるのが好ましい。ここで、不純物としてはＮａ，Ｆｅ２Ｏ３，ＳｉＯ２，ＣａＯ等が挙げられるが、不純物が１％未満であるのが好ましいのは、不純物が１％以上であると、セラミック成形体１の表面に砥粒が埋め込まれてしまったり、微細クラック中に砥粒が食い込んでしまったりした場合に、結晶の結合力が弱く半導体ウェハもしくは液晶のガラス基板上に脱落してパーティクルとなる可能性が高くなるからである。 Abrasive grains made of the same material as the ceramic molded body 1 are fired or calcined at 1000 to 1700 ° C. without applying pressure to the primary material of the ceramic. It is important that the average particle size of the abrasive grains is 50 to 200 μm, and particularly preferably 70 to 100 μm. If it is less than 50 μm, the impact is too small, so that it becomes difficult to make the rough surface portion 11 even if the spray pressure of blasting is increased, and if it exceeds 200 μm, the surface roughness of the rough surface portion 11 tends to be too large. Because there is.
When abrasive grains made of the same material as the ceramic molded body 1 are sprayed onto the ceramic molded body 1 before firing, the ceramic molded body 1 has a low hardness, so that the abrasive grains are embedded in the surface of the ceramic molded body 1. There is a possibility that the abrasive grains may bite into the microcracks, but since the abrasive grains are the same material as the ceramic molded body 1, both are assimilated at the stage of the firing process, and the abrasive grains become particles. Has the effect of being reduced.
Furthermore, it is preferable that the abrasive grains made of the same material as the ceramic molded body 1 have a purity of 99% or more and impurities of less than 1%. Here, Na, Fe 2 O 3 , SiO 2 , CaO and the like can be mentioned as impurities, but it is preferable that the impurities are less than 1%. If the impurities are 1% or more, the ceramic molded body 1 When abrasive grains are embedded in the surface or abrasive grains bite into fine cracks, the bonding force of the crystals is weak, and there is a possibility that they will fall on the semiconductor wafer or liquid crystal glass substrate and become particles. Because it becomes high.

また、有機物からなる砥粒の材質としては、天然樹脂および合成樹脂ともに使用でき、合成樹脂としては、ポリエチレン，ポリビニルアルコール，アクリル樹脂およびフェノール樹脂等が挙げられる。また、この砥粒の平均粒径は２００〜６００μｍであることが重要であり、粒径が２００μｍ未満であると、衝撃が小さ過ぎるためブラスト処理の噴射圧力を高くしても粗面部１１とすることが困難となり、６００μｍを超えると衝突する面積が大きくなるため粗面部１１とすることが困難となる傾向があるからである。
有機物からなる砥粒は、セラミック成形体１と同材質の砥粒に比べて硬度が低いので、ブラスト処理装置内の金属部品を磨耗させることなく、これにより不純物が混入されることが少ないという効果を有する。さらに、有機物からなる砥粒はセラミック成形体１にぶつかる衝撃で、変形して破砕されるため、部材に大きな衝撃を与えることがなく、その表面が必要以上に大きな粗面部１１になりにくいという効果を有する。さらに、セラミックスの焼成温度は、アルミナで１４００〜１７００℃，窒化アルミ・炭化珪素が約２０００℃，窒化珪素で約１８００℃であり、焼成前の脱脂工程あるいは焼成中に有機バインダーと同様に有機物からなる砥粒は５００℃付近で揮発して飛んでしまうため、焼成前のセラミック成形体１の表面に残っていたとしても、焼成後に完全に無くなることとなる。
さらに、有機物からなる砥粒は、その純度が９９％以上であり不純物が１％未満であるのが好ましい。ここで、不純物としてはＮａおよびＣｌ等が挙げられるが、不純物が１％未満であるのが好ましいのは、不純物が１％以上であると、有機物からなる砥粒がセラミック成形体１の表面に残っていた場合に、脱脂工程や焼成工程において反応物としてその表面に異物（コンタミネーション）として付着したり、変色したりすることがあるからである。 Moreover, as a material of the abrasive grains made of organic matter, both natural resin and synthetic resin can be used. Examples of the synthetic resin include polyethylene, polyvinyl alcohol, acrylic resin, and phenol resin. Moreover, it is important that the average particle size of the abrasive grains is 200 to 600 μm. If the particle size is less than 200 μm, the impact is too small, so that the rough surface portion 11 is formed even if the spray pressure of the blast treatment is increased. This is because, when the thickness exceeds 600 μm, the area of collision increases, and the rough surface portion 11 tends to be difficult.
Since the abrasive grains made of organic matter have a lower hardness than the abrasive grains of the same material as the ceramic molded body 1, the effect that impurities are not mixed by this without wearing metal parts in the blasting apparatus. Have Furthermore, since the abrasive grains made of organic matter are deformed and crushed by the impact of hitting the ceramic molded body 1, the surface does not give a large impact to the member, and the surface does not easily become a rough surface portion 11 larger than necessary. Have Furthermore, the firing temperature of ceramics is 1400 to 1700 ° C. for alumina, about 2000 ° C. for aluminum nitride / silicon carbide, and about 1800 ° C. for silicon nitride. From the organic material during the degreasing process or firing before firing, Since the resulting abrasive grains volatilize and fly around 500 ° C., even if they remain on the surface of the ceramic molded body 1 before firing, they are completely lost after firing.
Furthermore, it is preferable that the abrasive grains made of an organic substance have a purity of 99% or more and impurities of less than 1%. Here, examples of impurities include Na and Cl. The impurities are preferably less than 1%. When the impurities are 1% or more, abrasive grains made of organic matter are formed on the surface of the ceramic molded body 1. This is because if it remains, it may adhere to the surface as a foreign substance (contamination) or change its color as a reaction product in the degreasing step or the firing step.

そして、ブラスト処理におけるセラミック成形体１と同材質の砥粒もしくは有機物からなる砥粒の噴射圧力としては、０．３〜０．５ＭＰａであることが重要である。０．３ＭＰａ未満であると噴射圧力が弱過ぎて粗面部１１とすることが困難であり、０．５ＭＰａを超えると噴射圧力が強過ぎて粗面部１１の面粗さが大きくなり過ぎてしまったり、粗面部１１に砥粒が食い込んでしまったりする可能性がある。この食い込みはセラミック成形体１と同材質の砥粒もしくは有機物からなる砥粒を用いることによりそれほど問題とはならないが、食い込みがないほうが好ましい。したがって、その砥粒の平均粒径を考慮しながら、その噴射圧力を０．３〜０．５ＭＰａとすることで、その粗面部１１の面粗さが焼結後の処理容器用部材として好ましい１．５〜５．５μｍの範囲となり、使用中のフッ化物膜等が付着・堆積しても、これが半導体ウェハもしくは液晶のガラス基板上に剥がれ落ちてパーティクルとなるのを防止できる。   And it is important that it is 0.3-0.5 Mpa as injection pressure of the abrasive grain which consists of the abrasive grain or organic substance of the same material as the ceramic molded object 1 in a blasting process. If it is less than 0.3 MPa, the injection pressure is too weak to make the rough surface portion 11 difficult, and if it exceeds 0.5 MPa, the injection pressure is too strong and the surface roughness of the rough surface portion 11 becomes too large. The abrasive grains may bite into the rough surface portion 11. Although this biting does not cause much problem by using abrasive grains made of the same material as the ceramic molded body 1 or abrasive grains made of organic matter, it is preferable that no biting occurs. Therefore, considering the average particle size of the abrasive grains, the surface pressure of the rough surface portion 11 is preferable as a processing vessel member after sintering by setting the injection pressure to 0.3 to 0.5 MPa. In the range of 0.5 to 5.5 μm, even if a fluoride film or the like in use adheres and accumulates, it can be prevented from peeling off onto a semiconductor wafer or a liquid crystal glass substrate to form particles.

また、砥粒２をセラミック成形体１に噴射するときの距離は、粗面部１１より５０〜１００ｍｍ程度とすることが好ましい。この距離が５０ｍｍ未満であると粗面部１１に砥粒２が集中して噴射されて、その粗面部１１が必要以上に凹んでしまうことがあり、また距離が１００ｍｍを超えると噴射した砥粒２の勢いが弱くなり過ぎて、粗面部１１を均一にブラスト処理を施す際に多くの時間を費やすことになる。
さらに、砥粒２をセラミック成形体１に噴射するときの角度は、ブラスト処理を施す粗面部１１に対して、砥粒２が垂直に当たるように噴射することが好ましい。このとき、その粗面部１１に対してノズル３の角度を３０°以上に倒して噴射すると、粗面部１１に噴射された砥粒２が斜めに衝突するため、その分粗面となりにくく、また、噴射された砥粒２と粗面部１１との距離が、近い部分と遠い部分とが発生するため、その粗面部１１の面粗さのばらつきが大きくなる。 Further, the distance when the abrasive grains 2 are sprayed onto the ceramic molded body 1 is preferably about 50 to 100 mm from the rough surface portion 11. When this distance is less than 50 mm, the abrasive grains 2 are concentrated and sprayed on the rough surface portion 11, and the rough surface portion 11 may be recessed more than necessary, and when the distance exceeds 100 mm, the sprayed abrasive particles 2 This momentum becomes too weak, and a lot of time is spent when the rough surface portion 11 is uniformly blasted.
Furthermore, it is preferable that the angle at which the abrasive grains 2 are sprayed onto the ceramic molded body 1 is sprayed so that the abrasive grains 2 are perpendicularly applied to the rough surface portion 11 to be blasted. At this time, if the angle of the nozzle 3 is inclined to 30 ° or more with respect to the rough surface portion 11 and sprayed, the abrasive grains 2 sprayed onto the rough surface portion 11 collide obliquely, so that it is less likely to become a rough surface, Since the distance between the sprayed abrasive grain 2 and the rough surface portion 11 is near and far, a variation in the surface roughness of the rough surface portion 11 increases.

なお、砥粒２を噴射する際は、一部分だけ長い間砥粒２を噴射し続けると、その部分だけが大きく凹んでしまうため、その部材を回転させながら砥粒２を噴射するか、もしくは噴射するノズル３が一定の速度で移動できるように工夫することで、粗面部１１とした際の面粗さのばらつきを少なくすることができる。また、粗面部１１を必要としない部分は、その部分をテープなどで覆うことで、粗面部１１となることを防ぐことができる。   In addition, when injecting the abrasive grains 2, if the abrasive grains 2 are continuously ejected for a long time, only that part will be greatly dented. Therefore, the abrasive grains 2 are ejected while rotating the member, or the injecting is performed. By devising the nozzle 3 to be moved at a constant speed, it is possible to reduce variations in surface roughness when the rough surface portion 11 is formed. Moreover, the part which does not require the rough surface part 11 can prevent becoming the rough surface part 11 by covering the part with a tape.

このように粗面部１１の形成されたセラミック成形体１は、その後、電気炉やガス炉内で、３００〜５００℃の比較的低温で有機バインダーを揮発させる脱脂工程、１４００〜２０００℃の温度での焼成工程からなる焼成段階を経て、焼結体としての処理容器用部材となる。
この焼成段階における脱脂工程で急激に昇温すると、有機バインダーが一気に揮発して、セラミック成形体１にクラックが発生することがある。また、焼成段階における焼成工程で、１０００℃を超える部分より収縮が始まり結晶化が進んで緻密化していくが、この工程でもその昇温が速いとセラミック成形体１において、収縮の遅い部分が収縮の早い部分に追いつけずにクラックが発生したり、また大きく変形したりする可能性がある。したがって、これらの温度域での昇温速度を５０℃／ｈ以下にすることが好ましい。 The ceramic molded body 1 having the rough surface portion 11 thus formed is then degreased in the electric furnace or gas furnace at a relatively low temperature of 300 to 500 ° C. and a temperature of 1400 to 2000 ° C. Through the firing step consisting of the above-described firing step, a processing container member as a sintered body is obtained.
When the temperature is rapidly raised in the degreasing process in this firing stage, the organic binder may volatilize at once and cracks may occur in the ceramic molded body 1. Further, in the firing process in the firing stage, shrinkage starts from a portion exceeding 1000 ° C., and crystallization progresses and becomes denser. Even in this process, if the temperature rises fast, the slow shrinking portion of the ceramic molded body 1 shrinks. There is a possibility that cracks may occur without catching up with the early part of the film, or that the part may be greatly deformed. Therefore, it is preferable to set the rate of temperature rise in these temperature ranges to 50 ° C./h or less.

ここで、この焼成段階においても、図２に示すブラスト処理で用いた焼成治具４をそのまま用いることが重要である。このような形状の焼成治具４を用いて、セラミック成形体１の開口部１２を上方に向け、外径部１３までの部分をこの焼成治具４の凹み４１に嵌め込んだ状態で、脱脂、焼成することにより、焼成治具４が焼成の際の変形防止や矯正の役割を果たし、寸法精度が良好な焼結体としての処理容器用部材を得ることができる。このように曲面状の底面を支えるだけではなく、側面の外径部１３まで嵌め込むことでその形状を良好に保つことができ、寸法精度が確保できるため、焼成前のブラスト処理でその内面を粗面部１１とすることができ、焼成後にその内面を粗面部１１とする必要がない。   Here, also in this firing step, it is important to use the firing jig 4 used in the blasting process shown in FIG. 2 as it is. Using the firing jig 4 having such a shape, degreasing is performed with the opening 12 of the ceramic molded body 1 facing upward and the portion up to the outer diameter portion 13 being fitted in the recess 41 of the firing jig 4. By firing, the firing jig 4 plays a role of preventing deformation and correcting during firing, and a member for a processing container as a sintered body with good dimensional accuracy can be obtained. In addition to supporting the curved bottom surface in this way, it is possible to keep the shape good by fitting up to the outer diameter portion 13 on the side surface, and to ensure dimensional accuracy, so that the inner surface is blasted before firing It can be set as the rough surface part 11, and it is not necessary to make the inner surface into the rough surface part 11 after baking.

焼成前に微細クラックが生じていたとしても、この焼成段階において、表面にガラス成分が析出することにより略修復される。また、砥粒とセラミックス成形体１とが同材質の場合、セラミック成形体１の表面に砥粒が埋め込まれてしまったり、微細クラック中に砥粒が食い込んでしまったりしていたとしても、焼成工程の段階で両者は同化する。さらに、有機物からなる砥粒の場合、焼成前の脱脂工程あるいは焼成中に有機バインダーと同様に５００℃付近で揮発して飛んでしまうため、焼成後に完全に無くなってしまう。したがって、半導体もしくは液晶デバイス製造プロセス中に砥粒やセラミックスの微小片が半導体ウェハもしくは液晶のガラス基板上に落ちてパーティクルとなることはない。   Even if fine cracks are generated before firing, the glass component is substantially repaired by precipitation of glass components on the surface in this firing stage. In addition, when the abrasive grains and the ceramic molded body 1 are made of the same material, even if the abrasive grains are embedded in the surface of the ceramic molded body 1 or the abrasive grains have bite into the fine cracks, firing is performed. Both are assimilated at the process stage. Furthermore, in the case of abrasive grains made of organic matter, they volatilize around 500 ° C. during the degreasing step before firing or during firing, and are completely lost after firing. Therefore, during the semiconductor or liquid crystal device manufacturing process, abrasive grains and fine ceramic pieces do not fall on the semiconductor wafer or liquid crystal glass substrate to form particles.

（実施例１）
純度９９％のアルミナセラミックス材料を用いて、ラバープレス法で成形した成形体を切削し、外径１００ｍｍで厚み１０ｍｍの大きさの円盤形状の試料を製作し、焼成後の状態を評価した。 Example 1
Using a 99% purity alumina ceramic material, a molded body molded by a rubber press method was cut to produce a disk-shaped sample having an outer diameter of 100 mm and a thickness of 10 mm, and the state after firing was evaluated.

比較例として、焼成後に平均粒径が６００μｍのＧＣ砥粒を使用してブラスト処理したものを試料１とした。   As a comparative example, Sample 1 was obtained by blasting using GC abrasive grains having an average particle diameter of 600 μm after firing.

また、比較例として、焼成後に平均粒径が４００μｍのＧＣ砥粒を使用してブラスト処理したものを試料２とした。   Further, as a comparative example, Sample 2 was obtained by blasting using GC abrasive grains having an average particle diameter of 400 μm after firing.

以下、本発明の実施例として、焼成前の成形体にこの成形体と同材質の純度９５％アルミナセラミックスの原料を１０００℃で約２時間仮焼した粉体からなる砥粒を使用してブラスト処理したものを試料３とした。   As an example of the present invention, blasting is performed by using abrasive grains made of powder obtained by calcining a raw material of 95% purity alumina ceramic of the same material as that of the molded body at 1000 ° C. for about 2 hours. Sample 3 was treated.

また、同様に純度９８％の砥粒を使用してブラスト処理したものを試料４、また、同様に純度９９．５％の砥粒を使用してブラスト処理したものを試料５とした。   Similarly, Sample 4 was blasted using abrasive grains having a purity of 98%, and Sample 5 was similarly blasted using abrasive grains having a purity of 99.5%.

また、焼成前の成形体にポリエチレン樹脂からなる平均粒径が１００μｍの有機物の砥粒を使用してブラスト処理したものを試料６とした。   Sample 6 was obtained by blasting the molded body before firing using organic abrasive grains having an average particle diameter of 100 μm made of polyethylene resin.

また、焼成前の成形体にポリエチレン樹脂からなる平均粒径が２００μｍの有機物の砥粒を使用してブラスト処理したものを試料７とした。   Sample 7 was obtained by blasting the molded body before firing using organic abrasive grains having an average particle diameter of 200 μm made of polyethylene resin.

また、焼成前の成形体にポリエチレン樹脂からなる平均粒径が４００μｍの有機物の砥粒を使用してブラスト処理したものを試料８とした。   Sample 8 was obtained by blasting the molded body before firing using organic abrasive grains having an average particle diameter of 400 μm made of polyethylene resin.

その他の条件として、ブラスト処理装置は乾式ブラスト機を使用し、その噴射圧力を０．４ＭＰａとし、ノズルから試料までの距離を３０ｍｍに設定した。また、ノズルは一定の速さで移動し、試料の全面を５分間でブラスト処理した。   As other conditions, a dry blasting machine was used as the blasting apparatus, the injection pressure was set to 0.4 MPa, and the distance from the nozzle to the sample was set to 30 mm. The nozzle moved at a constant speed, and the entire surface of the sample was blasted in 5 minutes.

このときのノズルの口径は、１０ｍｍのものを使用した。   The nozzle diameter at this time was 10 mm.

評価方法として、ブラスト処理後の面粗さを測定し、続いて試料を２分割に研削加工して、処理面の断面を倍率１万倍の光学レンズにて観察し、微細クラック（マイクロクラック）の長さを測定した。また、これに超音波洗浄を行なった後、粘着テープをその表面に貼り付け、これを剥離した際に、粘着テープの表面についた脱粒の有無を確認し、さらに走査型電子分光分析により粗面部の表面分析を実施し、アルミナ以外の不純物量を測定して比較した。   As an evaluation method, the surface roughness after blasting is measured, the sample is then ground in two parts, the cross section of the treated surface is observed with an optical lens with a magnification of 10,000 times, and microcracks are observed. The length of was measured. In addition, after performing ultrasonic cleaning on this, the adhesive tape was applied to the surface, and when it was peeled off, the presence of degranulation on the surface of the adhesive tape was confirmed, and the rough surface portion was further determined by scanning electron spectroscopy analysis. The surface analysis was conducted, and the amount of impurities other than alumina was measured and compared.

結果を表１に示す。

Figure 0004522117
The results are shown in Table 1.
Figure 0004522117

表１の結果より、比較例の試料１は、砥粒が大きいことから面粗さは試料中最も粗面となっていた。また、焼成後にブラスト処理をして粗面化したものである粗面部の表面を観察した結果、微細クラックが確認され、粘着テープを剥離した際に脱粒が確認された。また、その表面の不純物量も１％以上と多かった。   From the results shown in Table 1, the surface roughness of Sample 1 of the comparative example was the most rough in the sample because of the large abrasive grains. Moreover, as a result of observing the surface of the rough surface part which was roughened by blasting after firing, fine cracks were confirmed, and degreasing was confirmed when the adhesive tape was peeled off. Further, the amount of impurities on the surface was as large as 1% or more.

また、比較例の試料２は、試料１よりも粒径の小さい砥粒を使用してブラスト処理したものであるが、試料１と同様に微細クラック・脱粒ともに確認された。   Sample 2 of the comparative example was blasted using abrasive grains having a particle diameter smaller than that of sample 1, and both microcracks and degranulation were confirmed as in sample 1.

これらに対し、焼成前の成形体にこの成形体と同材質の砥粒を使用してブラスト処理して粗面化した本発明の実施例の試料３〜５は、面粗さも規格内で、微細クラックの長さが１μｍ未満であり、脱粒もなく、良好な粗面であった。なお、砥粒の純度が低い試料３，４は、焼成後の面に異物の発生が見られたが、砥粒の純度が高い試料５は、不純物も少なく良好であった。   On the other hand, the samples 3 to 5 of the examples of the present invention, which were roughened by blasting using the same abrasive material as the molded body on the molded body before firing, the surface roughness was also within the standard, The length of the fine cracks was less than 1 μm, and there was no grain loss and the surface was good. In Samples 3 and 4 having low abrasive grain purity, foreign matters were observed on the surface after firing, but Sample 5 having high abrasive grain purity was good with few impurities.

また、焼成前の成形体に有機物からなる砥粒を使用してブラスト処理して粗面化した本発明の実施例の試料６〜８は、成形体と同材質の砥粒を使用してブラスト処理した試料３〜５より微細クラックや脱粒が無く、異物の発生も確認できなかった。また、不純物も少ないため、耐食性の向上が図れることがわかった。   Samples 6 to 8 of the examples of the present invention, which were roughened by blasting using an organic abrasive grain on the green body before firing, were blasted using abrasives of the same material as the molded body. There were no fine cracks or degranulation from the treated samples 3 to 5, and the occurrence of foreign matter could not be confirmed. Further, it was found that the corrosion resistance can be improved because there are few impurities.

以上のように、焼成前の成形体に有機物からなる砥粒を使用してブラスト処理を施して粗面部を形成したことにより、微細クラックや脱粒の発生を防ぐことができることがわかった。   As described above, it was found that the occurrence of fine cracks and degranulation can be prevented by forming a rough surface portion by subjecting the formed body before firing to blasting using an organic abrasive.

本発明の製造方法により得られたセラミック成形体の断面図である。It is sectional drawing of the ceramic molded body obtained by the manufacturing method of this invention. 本発明の製造方法におけるブラスト処理の説明図である。It is explanatory drawing of the blast process in the manufacturing method of this invention. 本発明の製造方法により得られたセラミック成形体の粗面部表面の拡大断面図である。It is an expanded sectional view of the rough surface part surface of the ceramic molded body obtained by the manufacturing method of this invention. 半導体製造装置内の各部材の概略図である。It is the schematic of each member in a semiconductor manufacturing apparatus. 従来の製造方法におけるブラスト処理の説明図である。It is explanatory drawing of the blast process in the conventional manufacturing method. 従来の製造方法における処理容器用部材の粗面部表面の拡大断面図である。It is an expanded sectional view of the rough surface part surface of the member for processing containers in the conventional manufacturing method.

１ ：セラミック成形体1: Ceramic molded body
１１：粗面部11: Rough surface
１２：開口部12: Opening
１３：外径部13: Outer diameter part
２ ：砥粒2: Abrasive grains
３ ：ノズル3: Nozzle
４ ：焼成治具4: Firing jig
４１：凹み41: dent

Claims (1)

ドーム状に形成され、開口部内に粗面部を有するセラミックス製の半導体もしくは液晶製造装置に用いられる処理容器用部材の製造方法であって、焼成前のセラミック成形体の外壁形状が転写された凹みであって、曲面状の底面を支えるとともに、側面の外径部まで嵌め込むことのできる凹みを有する焼成治具を用い、該焼成治具に前記セラミック成形体の前記開口部を上方に向けて載置し、前記セラミック成形体と同材質で平均粒径が５０〜２００μｍの砥粒もしくは有機物からなる平均粒径が２００〜６００μｍの砥粒を用いて、０．３〜０．５ＭＰａの噴射圧力で前記セラミック成形体の前記開口部内にブラスト処理を施した後、前記焼成治具に前記セラミック成形体を載置したまま焼成することを特徴とする半導体もしくは液晶製造装置に用いられる処理容器用部材の製造方法。 It is formed in a dome shape, a manufacturing method of the processing container member for use in a semiconductor or liquid crystal manufacturing apparatus of a ceramic having a rough surface in the opening, with recessed outer walls the shape of the ceramic molded body before firing is transferred And using a firing jig that supports the curved bottom surface and has a recess that can be fitted to the outer diameter part of the side surface, and mounts the ceramic molded body with the opening facing upward on the firing jig. And using an abrasive having the same material as the ceramic molded body and having an average particle size of 50 to 200 μm or an abrasive having an average particle size of 200 to 600 μm and an injection pressure of 0.3 to 0.5 MPa. A blasting process is performed in the opening of the ceramic molded body, and then firing is performed with the ceramic molded body placed on the firing jig. Manufacturing method of the member for processing containers used for installation.
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