JP2006206974A - Surface treatment method for member for thin film manufacturing apparatus and member for thin film manufacturing apparatus - Google Patents

Surface treatment method for member for thin film manufacturing apparatus and member for thin film manufacturing apparatus Download PDF

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JP2006206974A
JP2006206974A JP2005021995A JP2005021995A JP2006206974A JP 2006206974 A JP2006206974 A JP 2006206974A JP 2005021995 A JP2005021995 A JP 2005021995A JP 2005021995 A JP2005021995 A JP 2005021995A JP 2006206974 A JP2006206974 A JP 2006206974A
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manufacturing apparatus
thin film
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JP4732765B2 (en
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Norihiro Kurauchi
宣博 倉内
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Neos Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a surface treatment method for members for the thin film manufacturing apparatus which solves the degradation in the vacuum characteristics of the thin film manufacturing apparatus and effectively reduces the generation of particles by solving the problems that the thin film manufacturing apparatus, more particularly, the semiconductor manufacturing apparatus like vacuum-deposited film manufacturing apparatus, and flat panel display manufacturing apparatus, are subjected to formation of thermally sprayed films and sealing treatment of the thermally sprayed films, in order to effectively prevent the contamination by particles etc., but the generation of the particles cannot heretofore be sufficiently reduced due to the influence of plasma and the like generated at film deposition. <P>SOLUTION: The surface treatment method for the members for the thin film manufacturing apparatus comprises performing sealing treatment of the thermally sprayed film by forming the thermally sprayed film on the surface of a substrate and impregnating aluminum phosphate into the pores of the obtained thermally sprayed film. The members for the thin film manufacturing apparatus are obtained by the method. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

本発明は、薄膜製造装置、特に、真空蒸着膜形成装置等の半導体製造装置やフラットパネルディスプレイ製造装置等の装置内部のパーティクル等による汚染を有効に防止するための装置の部材の表面処理方法及び表面処理された部材に関する。   The present invention relates to a surface treatment method for a member of an apparatus for effectively preventing contamination caused by particles or the like inside a thin film manufacturing apparatus, particularly a semiconductor manufacturing apparatus such as a vacuum deposition film forming apparatus or a flat panel display manufacturing apparatus, and the like. The present invention relates to a surface-treated member.

半導体製造装置やフラットパネルディスプレイ製造装置等の内部でのパーティクルの発生は、半導体等の被製造物を汚染し、歩留まりを低下させる為、内部の汚染を防止する方法が幾つか提案されている。一般的には、装置内面の部材に溶射膜を施す表面処理が行われている。また、該溶射の後処理として窒化物、シリカおよびアルミナ等による封孔処理を行うことが提案されている（特許文献１、２）。   Since generation of particles inside a semiconductor manufacturing apparatus, a flat panel display manufacturing apparatus or the like contaminates a manufactured object such as a semiconductor and lowers the yield, several methods for preventing the internal contamination have been proposed. In general, a surface treatment for applying a sprayed film to a member on the inner surface of the apparatus is performed. In addition, it has been proposed to perform a sealing treatment with nitride, silica, alumina or the like as a post-treatment of the thermal spraying (Patent Documents 1 and 2).

しかし、該特許文献に記載の封孔処理剤では、半導体等の製造時のプラズマなどの影響を受けた場合、パーティクルの発生を十分に抑える効果には問題があった。   However, the sealing agent described in the patent document has a problem in the effect of sufficiently suppressing the generation of particles when affected by plasma during the production of a semiconductor or the like.

特開２００２−８３８６１号公報JP 2002-83861 A 特開２００２−１３４４８１号公報Japanese Patent Laid-Open No. 2002-134481

本発明は、上記に示した従来の技術の問題点を解決するためになされたものである。つまり、溶射膜がもつ真空特性の低下を解決するとともに、薄膜製造時におけるスッパタリング、プラズマエッチング、化学蒸着時のプラズマの影響を受けにくい薄膜製造装置部材の表面処理方法及び薄膜製造装置部材を提供することである。   The present invention has been made to solve the above-described problems of the prior art. In other words, the surface treatment method of a thin film manufacturing apparatus member and a thin film manufacturing apparatus member that are not easily affected by plasma sputtering during thin film production, plasma sputtering, and chemical vapor deposition while solving the deterioration of the vacuum characteristics of the sprayed film are provided. It is to be.

上記課題を解決するために、リン酸アルミニウムを含有した封孔処理剤を溶射皮膜の気孔に含浸させ焼成することにより、気孔が少なく、プラズマ等によるパーティクルの発生を効果的に抑えることができることを見出した。   In order to solve the above problems, the pores of the thermal spray coating are impregnated with a sealing agent containing aluminum phosphate and baked to reduce the number of pores and to effectively suppress the generation of particles due to plasma or the like. I found it.

即ち、本発明は、基材表面に溶射皮膜を形成し、得られた溶射皮膜の気孔にリン酸アルミニウムを含有する封孔処理剤を含浸させて、溶射皮膜の封孔処理を行うことを特徴とする薄膜製造装置部材の表面処理方法及び該方法により得られる薄膜製造装置部材を提供する。   That is, the present invention is characterized in that a thermal spray coating is formed on the surface of the base material, and pores of the obtained thermal spray coating are impregnated with a sealing agent containing aluminum phosphate to perform the sealing treatment of the thermal spray coating. A thin film manufacturing apparatus member surface treatment method and a thin film manufacturing apparatus member obtained by the method are provided.

本発明の封孔処理された溶射皮膜により、従来の溶射皮膜と比較して、真空特性が上昇、すなわち、装置の立ち上げ時間が短縮され、さらに、パーティクルの発生を低減できる。   Compared with the conventional thermal spray coating, the thermal spray coating subjected to the sealing treatment of the present invention increases the vacuum characteristics, that is, shortens the apparatus start-up time, and further reduces the generation of particles.

本発明に用いる溶射膜の材料は、アルミおよびアルミを含む合金、銅および銅を含む合金、ニッケルおよびニッケルを含む合金、チタンおよびチタンを含む合金等の金属材料である。作成方法においても従来から行われているアーク法、プラズマ法やフレーム法、コールドスプレー法が例示される。また、溶射前にブラスト等により表面処理を行うとよい。   The material of the thermal spray film used in the present invention is a metal material such as aluminum and an alloy containing aluminum, an alloy containing copper and copper, an alloy containing nickel and nickel, an alloy containing titanium and titanium. Examples of the production method include conventionally used arc method, plasma method, flame method, and cold spray method. In addition, surface treatment may be performed by blasting or the like before spraying.

次いで、リン酸アルミニウム含有する封孔処理剤で封孔処理を行うが、封孔処理剤は、溶液状態でもコロイド、またスラリー状態のものであってもよく、リン酸アルミニウムを含有するものであればよい。   Next, the sealing treatment is performed with a sealing agent containing aluminum phosphate. The sealing agent may be in a solution state, a colloidal state, or a slurry state, and may contain an aluminum phosphate. That's fine.

封孔処理剤の使用方法は、特に問うものではない。スプレーによる塗布、刷毛塗り、浸漬などを行い溶射皮膜に含浸させた後、オーブン、真空オーブンなどを用いて焼結すればよい。焼結温度は、１５０〜５００℃で、好ましくは２００〜３５０℃である。１５０℃以上でリン酸アルミニウムがガラス状化して十分に含侵され真空特性が得られ、５００℃以下ではアルミ基材等に対しての変色が抑えられる。
The method for using the sealing agent is not particularly limited. What is necessary is just to sinter using an oven, a vacuum oven, etc., after applying by spraying, brushing, dipping, etc. and impregnating the sprayed coating. The sintering temperature is 150 to 500 ° C, preferably 200 to 350 ° C. At 150 ° C. or higher, the aluminum phosphate is vitrified and sufficiently impregnated to obtain a vacuum characteristic.

以下に実施例及び比較例を示し、本発明をより具体的に説明する。但し、本発明は実施例に限定されない。結果を表１及び２に纏めた。   Hereinafter, the present invention will be described in more detail with reference to examples and comparative examples. However, the present invention is not limited to the examples. The results are summarized in Tables 1 and 2.

実施例１
基材としてＳＵＳ３０４（１３０ｍｍ×１３０ｍｍ×３ｍｍ）を用い、基材の１３０ｍｍ×１３０ｍｍの面をアルミナを用いてブラスト処理を行った。基材のブラスト表面にアーク溶射法でアルミニウム（純度９９．９％以上）を２００μｍ堆積させた。このアルミニウム溶射皮膜上にリン酸アルミニウムを含む封孔処理剤を含浸させ、封孔処理剤を自然乾燥させた後に２００℃のオーブン内で乾燥、焼結させた。この封孔処理を施したアルミニウム溶射皮膜を２００μｍ堆積させたＳＵＳ３０４をテストピースとして使用した。このテストピースを超純水中で超音波洗浄を行った。洗浄後にテストピースを１０５℃で乾燥させた。洗浄後に乾燥させたテストピースの封孔処理した溶射皮膜上を気中パーティクルカウンター（リオン株式会社製 ＫＭ−２０）を用いて測定した。表１のようにφ０．２μｍ以上のパーティクルの数は８個／ｃｍ２であった。 Example 1
SUS304 (130 mm × 130 mm × 3 mm) was used as the base material, and the 130 mm × 130 mm surface of the base material was blasted with alumina. 200 μm of aluminum (purity 99.9% or more) was deposited on the blast surface of the substrate by arc spraying. The aluminum spray coating was impregnated with a sealing agent containing aluminum phosphate, and the sealing agent was naturally dried and then dried and sintered in an oven at 200 ° C. SUS304 on which 200 μm of the aluminum sprayed coating subjected to the sealing treatment was deposited was used as a test piece. This test piece was subjected to ultrasonic cleaning in ultrapure water. The test piece was dried at 105 ° C. after washing. The surface of the sprayed coating of the test piece dried after washing was measured using an air particle counter (KM-20, manufactured by Rion Co., Ltd.). As shown in Table 1, the number of particles having a diameter of 0.2 μm or more was 8 / cm 2 .

実施例２
洗浄した実施例１のテストピースにスパッタリング装置を用いて０．５μｍの窒化チタンのスパッタ膜を作製した。スパッタリングでのプラズマに影響を受ける場合、テストピースからのパーティクルの増加が激しくなるが、この窒化チタンスパッタ膜上を気中パーティクルカウンターを用いて測定したところ、表１のようにφ０．２μｍ以上のパーティクルの数は２０個／ｃｍ２であった。 Example 2
A sputtering film of 0.5 μm titanium nitride was prepared on the cleaned test piece of Example 1 using a sputtering apparatus. When the plasma is affected by sputtering, the increase in particles from the test piece becomes severe. When measured on the sputtered titanium nitride film using an air particle counter, as shown in Table 1, φ0.2 μm or more The number of particles was 20 / cm 2 .

実施例３
基材としてＳＵＳ３０４（６００ｍｍ×６００ｍｍ×３ｍｍ）を用い、基材の６００ｍｍ×６００ｍｍの両面をアルミナを用いてブラスト処理を行った。基材のブラスト表面にアーク溶射法でアルミニウム（純度９９．９％以上）を２００μｍ堆積させた。このアルミニウム溶射皮膜上にリン酸アルミニウムを含む封孔処理剤を含浸させ、封孔処理剤を自然乾燥させた後に２００℃のオーブン内で乾燥、焼結させた。この封孔処理を施したアルミニウム溶射皮膜を２００μｍ堆積させたＳＵＳ３０４をテストピースとして使用した。このテストピースをスパッタリング装置のチャンバー内に入れ、ポンプを用いて排気した。１×１０−４Ｐａに到達するまでの時間を測定したところ、表２のように７時間要した。 Example 3
SUS304 (600 mm × 600 mm × 3 mm) was used as a base material, and both surfaces of the base material 600 mm × 600 mm were blasted using alumina. 200 μm of aluminum (purity 99.9% or more) was deposited on the blast surface of the substrate by arc spraying. The aluminum spray coating was impregnated with a sealing agent containing aluminum phosphate, and the sealing agent was naturally dried and then dried and sintered in an oven at 200 ° C. SUS304 on which 200 μm of the aluminum sprayed coating subjected to the sealing treatment was deposited was used as a test piece. The test piece was placed in a sputtering apparatus chamber and evacuated using a pump. When the time required to reach 1 × 10 −4 Pa was measured, it took 7 hours as shown in Table 2.

比較例１
基材としてＳＵＳ３０４（１３０ｍｍ×１３０ｍｍ×３ｍｍ）を用い、基材の１３０ｍｍ×１３０ｍｍの面をアルミナを用いてブラスト処理を行った。基材のブラスト表面にアーク溶射法でアルミニウム（純度９９．９％以上）を２００μｍ堆積させた。このアルミニウム溶射皮膜を２００μｍ堆積させたＳＵＳ３０４をテストピースとして使用した。このテストピースを超純水中で超音波洗浄を行った。洗浄後にテストピースを１０５℃で乾燥させた。洗浄後に乾燥させたテストピースの溶射皮膜上を気中パーティクルカウンター（リオン株式会社製 ＫＭ−２０）を用いて測定した。表１のようにφ０．２μｍ以上のパーティクルの数は２２７個／ｃｍ２であり、実施例１と比較して２８倍以上であった。 Comparative Example 1
SUS304 (130 mm × 130 mm × 3 mm) was used as the base material, and the 130 mm × 130 mm surface of the base material was blasted with alumina. 200 μm of aluminum (purity 99.9% or more) was deposited on the blast surface of the substrate by arc spraying. SUS304 on which 200 μm of this aluminum spray coating was deposited was used as a test piece. This test piece was subjected to ultrasonic cleaning in ultrapure water. The test piece was dried at 105 ° C. after washing. It measured on the sprayed coating of the test piece dried after washing | cleaning using the air particle counter (Rion Co., Ltd. KM-20). As shown in Table 1, the number of particles having a diameter of 0.2 μm or more was 227 / cm 2 , which was 28 times or more compared with Example 1.

比較例２
基材としてＳＵＳ３０４（１３０ｍｍ×１３０ｍｍ×３ｍｍ）を用い、基材の１３０ｍｍ×１３０ｍｍの面をアルミナを用いてブラスト処理を行った。基材のブラスト表面にアーク溶射法でアルミニウム（純度９９．９％以上）を２００μｍ堆積させた。このアルミニウム溶射皮膜上にアルミナを含む封孔処理剤を含浸させ、封孔処理剤を自然乾燥させた後に２００℃のオーブン内で乾燥、焼結させた。この封孔処理を施したアルミニウム溶射皮膜を２００μｍ堆積させたＳＵＳ３０４をテストピースとして使用した。このテストピースを超純水中で超音波洗浄を行った。洗浄後にテストピースを１０５℃で乾燥させた。洗浄後に乾燥させたテストピースの封孔処理した溶射皮膜上を気中パーティクルカウンター（実施例と同じ）を用いて測定した。表１のようにφ０．２μｍ以上のパーティクルの数は２３個／ｃｍ２であった。 Comparative Example 2
SUS304 (130 mm × 130 mm × 3 mm) was used as the base material, and the 130 mm × 130 mm surface of the base material was blasted with alumina. 200 μm of aluminum (purity 99.9% or more) was deposited on the blast surface of the substrate by arc spraying. The aluminum sprayed coating was impregnated with a sealing agent containing alumina, and the sealing agent was naturally dried and then dried and sintered in an oven at 200 ° C. SUS304 on which 200 μm of the aluminum sprayed coating subjected to the sealing treatment was deposited was used as a test piece. This test piece was subjected to ultrasonic cleaning in ultrapure water. The test piece was dried at 105 ° C. after washing. The measurement was performed on the sprayed coating on the test piece that had been dried after washing using an air particle counter (same as in the example). As shown in Table 1, the number of particles having a diameter of 0.2 μm or more was 23 / cm 2 .

比較例３
洗浄した比較例１のテストピースにスパッタリング装置を用いて０．５μｍの窒化チタンのスパッタ膜を作製した。スパッタリングでのプラズマに影響を受ける場合、テストピースからのパーティクルの増加が激しくなるが、この窒化チタンスパッタ膜上を気中パーティクルカウンターを用いて測定したところ、表１のようにφ０．２μｍ以上のパーティクルの数は３５個／ｃｍ２であり、実施例２と比較して１．７倍以上であった。 Comparative Example 3
A sputtering film of 0.5 μm titanium nitride was prepared on the cleaned test piece of Comparative Example 1 using a sputtering apparatus. When the plasma is affected by sputtering, the increase in particles from the test piece becomes severe. When measured on the sputtered titanium nitride film using an air particle counter, as shown in Table 1, φ0.2 μm or more The number of particles was 35 / cm 2 , which was 1.7 times or more compared with Example 2.

比較例４
洗浄した比較例２のテストピースにスパッタリング装置を用いて０．５μｍの窒化チタンのスパッタ膜を作製した。この窒化チタンスパッタ膜上を気中パーティクルカウンターを用いて測定したところ、表１のようにφ０．２μｍ以上のパーティクルの数は４５個／ｃｍ２であった。 Comparative Example 4
A sputtering film of 0.5 μm titanium nitride was prepared on the cleaned test piece of Comparative Example 2 using a sputtering apparatus. When this titanium nitride sputtered film was measured using an air particle counter, the number of particles having a diameter of 0.2 μm or more was 45 / cm 2 as shown in Table 1.

比較例５
基材としてＳＵＳ３０４（６００ｍｍ×６００ｍｍ×３ｍｍ）を用い、基材の６００ｍｍ×６００ｍｍの両面をアルミナを用いてブラスト処理を行った。基材のブラスト表面にアーク溶射法でアルミニウム（純度９９．９％以上）を２００μｍ堆積させた。このテストピースを超純水中で超音波洗浄を行った。洗浄後にテストピースを１０５℃で乾燥させた。このテストピースをスパッタリング装置のチャンバー内に入れ、ポンプを用いて排気した。１×１０−４Ｐａに到達するまでの時間を測定したところ、表１のように１１時間要した。 Comparative Example 5
SUS304 (600 mm × 600 mm × 3 mm) was used as a base material, and both surfaces of the base material 600 mm × 600 mm were blasted using alumina. 200 μm of aluminum (purity 99.9% or more) was deposited on the blast surface of the substrate by arc spraying. This test piece was subjected to ultrasonic cleaning in ultrapure water. The test piece was dried at 105 ° C. after washing. The test piece was placed in a sputtering apparatus chamber and evacuated using a pump. When the time to reach 1 × 10 −4 Pa was measured, it took 11 hours as shown in Table 1.

比較例６
基材としてＳＵＳ３０４（６００ｍｍ×６００ｍｍ×３ｍｍ）を用い、基材の６００ｍｍ×６００ｍｍの両面をアルミナを用いてブラスト処理を行った。基材のブラスト表面にアーク溶射法でアルミニウム（純度９９．９％以上）を２００μｍ堆積させた。このアルミニウム溶射皮膜上にアルミナを含む封孔処理剤を含浸させ、封孔処理剤を自然乾燥させた後に２００℃のオーブン内で乾燥、焼結させた。この封孔処理を施したアルミニウム溶射皮膜を２００μｍ堆積させたＳＵＳ３０４をテストピースとして使用した。このテストピースを超純水中で超音波洗浄を行った。洗浄後にテストピースを１０５℃で乾燥させた。このテストピースをスパッタリング装置のチャンバー内に入れ、ポンプを用いて排気した。１×１０−４Ｐａに到達するまでの時間を測定したところ、表１のように９時間要した。 Comparative Example 6
SUS304 (600 mm × 600 mm × 3 mm) was used as a base material, and both sides of 600 mm × 600 mm of the base material were blasted using alumina. 200 μm of aluminum (purity 99.9% or more) was deposited on the blast surface of the substrate by arc spraying. The aluminum sprayed coating was impregnated with a sealing agent containing alumina, and the sealing agent was naturally dried and then dried and sintered in an oven at 200 ° C. SUS304 on which 200 μm of the aluminum sprayed coating subjected to the sealing treatment was deposited was used as a test piece. This test piece was subjected to ultrasonic cleaning in ultrapure water. The test piece was dried at 105 ° C. after washing. The test piece was placed in a sputtering apparatus chamber and evacuated using a pump. When the time to reach 1 × 10 −4 Pa was measured, it took 9 hours as shown in Table 1.

Figure 2006206974
Figure 2006206974

Figure 2006206974
Figure 2006206974

本発明の封孔処理を施工した溶射皮膜は、半導体製造装置およびフラットパネルディスプレイ製造装置の防着板等に利用できる。   The thermal spray coating to which the sealing treatment of the present invention has been applied can be used for a deposition plate of a semiconductor manufacturing apparatus and a flat panel display manufacturing apparatus.

Claims (2)

基材表面に溶射皮膜を形成し、得られた溶射皮膜の気孔にリン酸アルミニウムを含浸させて、溶射皮膜の封孔処理を行うことを特徴とする薄膜製造装置部材の表面処理方法。 A method for treating a surface of a thin film manufacturing apparatus member, comprising: forming a thermal spray coating on a surface of a substrate; impregnating aluminum phosphate into pores of the obtained thermal spray coating; 請求項１に記載の方法により得られた薄膜製造装置部材。 A thin film manufacturing apparatus member obtained by the method according to claim 1.
JP2005021995A 2005-01-28 2005-01-28 Surface treatment method for thin film manufacturing apparatus member and thin film manufacturing apparatus member Expired - Fee Related JP4732765B2 (en)

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JPS56127449A (en) * 1980-03-11 1981-10-06 Matsushita Electric Ind Co Ltd Article with layer coated with fluorine resin
JPS63100169A (en) * 1986-10-16 1988-05-02 Nittetsu Hard Kk Heat treatment furnace hearth roll having excellent build-up resistance
JPH06306571A (en) * 1993-04-20 1994-11-01 Ishikawajima Harima Heavy Ind Co Ltd Formation of reinforced layer on base material
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JPH09125221A (en) * 1995-10-31 1997-05-13 Dainippon Toryo Co Ltd Sealing method of sprayed coating and sealing material
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