JP3871544B2 - Aluminum alloy for film formation treatment, aluminum alloy material excellent in corrosion resistance and method for producing the same - Google Patents
Aluminum alloy for film formation treatment, aluminum alloy material excellent in corrosion resistance and method for producing the same Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Description
【０００１】
【発明の属する技術分野】
この発明は、例えば半導体、ＬＣＤ（液晶ディスプレイ）等の製造装置材料として好適に使用され、皮膜形成処理によって優れた耐食性が得られるアルミニウム合金、ならびに耐食性に優れたアルミニウム合金材およびその製造方法に関する。
【０００２】
【従来の技術】
半導体やＬＣＤ等の製造装置を構成するチャンバー、サセプター、バッキングプレート等の部材材料として、アルミニウム合金、特にＡｌ−Ｓｉ系のＪＩＳ ５０５２アルミニウム合金やＡｌ−Ｓｉ−Ｍｇ系のＪＩＳ ６０６１アルミニウム合金からなる展伸材や鋳物材が使用されることが多い。また、これらの製造装置は高温で使用される上にシラン（ＳｉＨ4）やフッ素系または塩素系のハロゲンガス等の腐食性ガス雰囲気で使用されるため、各部材に陽極酸化処理を施して表面に硬質の陽極酸化皮膜を形成し、耐食性を向上させている。
【０００３】
しかし、このような表面処理をしても使用環境や使用頻度によっては早期に表面劣化が起こり、表面処理の更新が必要であった。特に、ＣＶＤ、ＰＶＤ処理装置では、使用温度が室温から約４００℃までの広範囲にわたり、しかも繰り返し熱応力が加わるため、母材と陽極酸化皮膜との熱変形能の違いにより割れが生じることがある。また長期使用の間には、顕著な損傷はなくてもワークを処理する際に装置表面に接触して陽極酸化皮膜が摩耗することもある。
【０００４】
そこで、半導体等の製造装置材料として、例えば特開平１１−４３７３４号公報においてＭｎ、Ｃｕ、Ｆｅを添加したアルミニウム合金が提案されている。このアルミニウム合金は、重金属を添加することで熱的に安定な金属間化合物を生成させるとともに、熱サイクルが加わったときに緩衝効果を果たす二重構造の陽極酸化皮膜を生成させることによって、熱サイクルおよび腐食環境下における耐食性向上を図ったものである。
【０００５】
また、特開平８−９２６８４号公報においてフッ化処理用Ａｌ−Ｍｇ系合金が提案されている。このアルミニウム合金は、フッ化処理により形成されるフッ化不働態膜によって耐食性向上を図ったものである。
【０００６】
【発明が解決しようとする課題】
しかしながら、上述の特開平１１−４３７３４号公報記載のアルミニウム合金は、陽極酸化皮膜の欠陥から、母材中のＡｌ−Ｆｅ系等の金属間化合物が腐食性ガスと反応して放出されたり、あるいは陽極酸化皮膜中の金属間化合物が僅かずつ蒸発または析出により放出されるという問題があった。このようなアルミニウム合金を、例えば半導体等の絶縁膜の成膜装置に使用すると、処理チャンバー内が放出された金属間化合物で汚染され、ひいては生成される絶縁膜が金属間化合物で汚染されて膜質が低下するという問題があった。
【０００７】
また、特開平８−９２６８４号公報記載のアルミニウム合金についても、形成されたフッ化不働態膜による耐食性が不十分であり、さらなる耐食性の向上が求められている。
【０００８】
この発明は、上述の技術背景に鑑み、高温熱サイクル、腐食雰囲気下において強度および耐食性に優れた皮膜形成処理用アルミニウム合金、ならびに耐食性に優れたアルミニウム合金材およびその製造方法の提供を目的とする。
【０００９】
【課題を解決するための手段】
前記目的を達成するために、この発明の皮膜形成処理用アルミニウム合金は、フッ化処理による単独皮膜、Ｎｉ−Ｐメッキ処理とフッ化処理による複合皮膜、陽極酸化処理とフッ化処理による複合皮膜のいずれかの耐食性皮膜を形成する処理を施すアルミニウム合金であって、Ｓｉ：０．２〜１．０wt％およびＭｇ：０．３〜２．０wt％を含有し、不純物としてのＦｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉの各含有量がそれぞれ０．１wt％以下に規制され、残部がＡｌおよび他の不純物からなることを基本要旨とする。
【００１０】
前記皮膜形成処理用アルミニウム合金において、Ｓｉ含有量は０．４〜０．７wt％、Ｍｇ含有量は０．５〜１．５wt％、Ｆｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉの各含有量はそれぞれ０．０５wt％以下に規制されていることが好ましい。
【００１１】
また、前記皮膜形成処理用アルミニウム合金は、ＣＶＤ装置、ＰＶＤ装置、液晶ディスプレイ（ＬＣＤ）製造装置、半導体製造装置のいずれかにおけるチャンバー、サセプター、バッキングプレートのいずれかの材料として用いられるアルミニウム合金として好適に使用される。
【００１２】
この発明の耐食性に優れたアルミニウム合金材は、Ｓｉ：０．２〜１．０wt％およびＭｇ：０．３〜２．０wt％を含有し、不純物としてのＦｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉの各含有量がそれぞれ０．１wt％以下に規制され、残部がＡｌおよび他の不純物からなるアルミニウム合金母材の表面に、フッ化処理による単独皮膜、Ｎｉ−Ｐメッキ処理とフッ化処理による複合皮膜、陽極酸化処理とフッ化処理による複合皮膜のいずれかの耐食性皮膜が形成されてなることを基本要旨とする。
【００１３】
また、前記アルミニウム合金母材におけるＳｉ含有量は０．４〜０．７wt％、Ｍｇ含有量は０．５〜１．５wt％、Ｆｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉの各含有量はそれぞれ０．０５wt％以下に規制されていることが好ましい。
【００１４】
また、耐食性に優れたアルミニウム合金材は、ＣＶＤ装置、ＰＶＤ装置、液晶ディスプレイ（ＬＣＤ）製造装置、半導体製造装置のいずれかにおけるチャンバー、サセプター、バッキングプレートのいずれかの材料として用いられるアルミニウム合金材として好適に使用される。
【００１５】
この発明の耐食性に優れたアルミニウム合金材の製造方法は、Ｓｉ：０．２〜１．０wt％およびＭｇ：０．３〜２．０wt％を含有し、不純物としてのＦｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉの各含有量がそれぞれ０．１wt％以下に規制され、残部がＡｌおよび他の不純物からなるアルミニウム合金母材の表面に、フッ化処理による単独皮膜、Ｎｉ−Ｐメッキ処理とフッ化処理による複合皮膜、陽極酸化処理とフッ化処理による複合皮膜のいずれかの耐食性皮膜形成処理を施すことを基本要旨とする。
【００１６】
前記耐食性に優れたアルミニウム合金材は、ＣＶＤ装置、ＰＶＤ装置、液晶ディスプレイ（ＬＣＤ）製造装置、半導体製造装置のいずれかにおけるチャンバー、サセプター、バッキングプレートのいずれかの材料として用いられるアルミニウム合金材として好適に使用される。
【００１７】
この発明の皮膜形成処理用アルミニウム合金、および耐食性に優れたアルミニウム合金材のアルミニウム合金母材の化学組成において、各元素の添加意義および規制意義は次のとおりである。
【００１８】
ＳｉおよびＭｇはいずれも強度を向上させる元素である。Ｓｉが０．２wt％未満、Ｍｇが０．３wt％未満では強度向上効果に乏しく、Ｓｉが１．０wt％を超えると靱性が低下し、Ｍｇが２．０wt％を超えると加工性が低下するという不都合がある。従って、Ｓｉ含有量は０．２〜１．０wt％、Ｍｇ含有量は０．３〜２．０wt％とする。さらに、Ｍｇには、フッ化処理を施した場合にフッ素とともにフッ化不働態膜を形成させ、また機械加工性を向上させる効果がある。好ましいＳｉ含有量は０．４〜０．７wt％である。また、好ましいＭｇ含有量０．５〜１．５wt％である。
【００１９】
また、不純物としての重金属Ｆｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉが多量に含有されていると、母材および皮膜中のＡｌ−Ｆｅ系金属間化合物の生成量が増し、皮膜欠陥から、金属間化合物が蒸発または析出により放出され、あるいはハロゲンガス等の腐食性ガスと反応して金属組織から脱落して放出される。重金属単体でも放出される。また、重金属含有量および金属間化合物量が増えると皮膜の欠陥が増大し、重金属および金属間化合物が放出され易くなる。そして、このアルミニウム合金またはアルミニウム合金材がＣＶＤ装置、ＰＶＤ装置、液晶ディスプレイ（ＬＣＤ）製造装置、半導体製造装置のいずれかにおけるチャンバー、サセプター、バッキングプレートのいずれかの材料として用いられる場合には、放出された重金属および金属間化合物が処理または製造されるＬＣＤ、半導体等を汚染して製品品質を劣化させる。さらに、強度向上のために上記範囲のＳｉ、Ｍｇの添加するためには、金属間化合物を生成させる不純物としての重金属を規制する必要がある。このため、前記各重金属元素はそれぞれ０．１wt％以下に規制して、金属間化合物の生成量を抑制するとともに皮膜欠陥を減少させる必要がある。これらの重金属元素の好ましい含有量はそれぞれ０．０５wt％以下である。
【００２０】
この発明の耐食性に優れたアルミニウム合金材は、上述した組成のアルミニウム合金母材の表面に、耐食性皮膜が形成されている。前記皮膜は、上述したように母材合金の組成制御によって欠陥の少ない皮膜に形成されているため、高温熱サイクル、腐食環境下においても重金属および金属間化合物が放出されにくく、優れた耐食性、特にガス耐食性を有し、ひいては合金材としての耐食性が優れている。また、長時間の使用劣化によって皮膜が割れたり摩耗して母材が露出した場合でも、母材中の重金属含有量そのものが規制されているために放出量も少なく、半導体等への汚染による悪影響も少ない。
【００２１】
前記耐食性皮膜としては、フッ化処理皮膜の単独皮膜、あるいはＮｉ−Ｐメッキ処理とフッ化処理による複合皮膜、または陽極酸化処理とフッ化処理による複合皮膜を例示でき、いずれも上述した優れた耐食性が得られる。これらのうち、単独皮膜は皮膜形成処理が容易である点で推奨でき、複合皮膜は異種皮膜の複合化により耐食性を相乗的に向上しうる点で推奨できる。
【００２２】
なお、このような皮膜によって優れたガス耐食性を有する合金材は、水に対しても優れた耐食性を示す。
【００２３】
前記耐食性に優れたアルミニウム合金材の製造方法において、各耐食性皮膜形成処理は常法に従って行えば良く、条件は限定されない。
【００２４】
陽極酸化処理は、硫酸浴、蓚酸浴等により処理する。例えばアルミニウム合金材を半導体等製造装置材料として使用する場合であれば、液組成：１０％Ｈ2ＳＯ4、液温０+/-２℃、電流密度：ＤＣ２〜４．５Ａ／ｄｍ2、電圧：２３〜１２０Ｖ、処理時間：６０分の条件で処理すると、約５０μｍの硬質陽極酸化皮膜を形成することができる。
【００２５】
フッ化処理は、加熱下でフッ素ガスまたはフッ化物ガスをアルミニウム合金母材の表面に接触させるか、あるいは液体フッ化物を接触させる方法等を例示でき、フッ化不働態皮膜を形成することができる。
【００２６】
Ｎｉ−Ｐメッキ処理とフッ化処理による複合皮膜を形成する場合は、例えば次亜りん酸塩を還元剤とした硫酸ニッケル浴を用いてＮｉ−Ｐメッキ処理を施してメッキ皮膜を形成した後、上述したフッ化処理を施す。これにより、Ｎｉ−Ｐメッキ皮膜とフッ化不働態皮膜との複合皮膜が形成される。
【００２７】
また、陽極酸化処理とフッ化処理による複合皮膜を形成する場合は、上述した陽極酸化処理を施して陽極酸化皮膜を形成した後、上述したフッ化処理を施す。これにより、陽極酸化皮膜とフッ化不働態皮膜との複合皮膜が形成される。
【００２８】
また、いずれの場合も、皮膜形成処理の前処理として脱脂洗浄、エッチング、表面研磨等、後処理としての洗浄、乾燥、加熱等は適宜行う。
【００２９】
所要形状への加工も常法に従えば良く限定されないが、半導体等製造装置材料として高温熱サイクル、腐食環境下で使用する場合は、切削、研削時および接合時の残留応力を除去するために、それぞれの加工後に３５０〜３８０℃で熱処理することが好ましい。
【００３０】
また、この発明のアルミニウム合金および合金材は、高温、腐食ガス雰囲気に曝されるあらゆる部材に適した合金および合金材であり、特にＣＶＤ装置、ＰＶＤ装置、液晶ディスプレイ（ＬＣＤ）製造装置、半導体製造装置のいずれかのチャンバー、サセプター、バッキングプレートのいずれかの材料として用いられるアルミニウム合金材料として好適に使用される。
【００３１】
【実施例】
後掲の表１に示す各組成のアルミニウム合金について、常法に従ってＤＣ鋳造した鋳塊を４５０〜６００℃で均質化処理し、その後熱間圧延および冷間圧延を施して厚さ４mmのアルミニウム合金板を製作した。
【００３２】
５０mm×５０mmに切断した各アルミニウム合金板に対し、下記条件で皮膜を形成した。ただし、比較例１４は皮膜形成処理を施さなかった。
（硫酸陽極酸化皮膜の形成）
浴組成：１５％Ｈ2ＳＯ4、浴温：２５℃、電圧：２０Ｖ、処理時間：２０分で陽極酸化処理を行い、膜厚：２０μｍの皮膜を形成した。
（蓚酸陽極酸化皮膜の形成）
浴組成：４％（ＣＯＯＨ）2・２Ｈ2Ｏ、浴温：２５℃、電圧：３０Ｖ、処理時間：３０分で陽極酸化処理を行い、膜厚：１５μｍの皮膜を形成した。
（フッ化処理皮膜の形成）
前処理として化学研磨を行った後、２０％フッ素ガス（Ｆ2）＋８０％Ｎ2を導入したチャンバー内で、２６０℃×２４時間保持し、膜厚５μｍのフッ化不働態皮膜を形成した。
（Ｎｉ−Ｐメッキ処理とフッ化処理の複合皮膜の形成）
次亜りん酸塩を還元剤とした硫酸ニッケル浴中で、無電解Ｎｉ−Ｐメッキを行い５μｍのメッキ皮膜を形成した後、２０％フッ素ガス（Ｆ2）＋８０％Ｎ2を導入したチャンバー内で２６０℃×２４時間保持し、Ｎｉ−Ｐメッキ皮膜とフッ化不働態皮膜との複合皮膜を形成した。この複合皮膜の膜厚は３０μｍであった。
（陽極酸化処理とフッ化処理の複合皮膜の形成）
上述の方法で２０μｍの硫酸陽極酸化皮膜を形成した後、２０％フッ素ガス（Ｆ2）＋８０％Ｎ2を導入したチャンバー内で２６０℃×２４時間保持し、硫酸陽極酸化皮膜とフッ化不働態皮膜との複合皮膜を形成した。この複合皮膜の膜厚は１５μｍであった。
【００３３】
そして、各皮膜を形成したアルミニウム合金板に対し、下記の方法によりガス耐食性試験および強度試験を行った。
〔ガス耐食性試験〕
前記アルミニウム合金板を、半導体製造工程における絶縁膜の成膜装置の処理チャンバー内に投入し、半導体絶縁膜の絶縁不良が発生するまでの時間を計測した。試験に使用したシリコンウエーハは直径２００mm、厚さ７００μｍ、チャンバー寸法は幅４００mm×奥行き４００mm×高さ２００mmであり、絶縁膜の成膜はプラズマＣＶＤ（４００℃、腐食性ガス：ＳｉＨ4−Ｎ2Ｏ、プラズマ励起雰囲気）により行った。
【００３４】
前記絶縁膜の成膜試験において、絶縁不良は、アルミニウム合金中に不純物として含有される重金属またはこの重金属によって形成された金属間化合物が絶縁膜を汚染し、ＳｉまたはＳｉＯ2への拡散係数が大となったためであると推測される。従って、絶縁不良までの時間、換言すれば成膜可能時間が長いほどアルミニウム合金母材または各皮膜からの重金属および金属間化合物の放出量が少ないと評価することができる。評価結果を表１に示す。
【００３５】
なお、参考例９，１０の同一組成のアルミニウム合金において、硫酸陽極酸化皮膜よりも蓚酸陽極酸化皮膜の成膜可能時間が長いのは、蓚酸陽極酸化皮膜の耐熱性によるものと推測される。
【００３６】
また、複合皮膜を形成した２種類のアルミニウム合金板（実施例１２，１３））が、陽極酸化処理皮膜またはフッ化処理皮膜の単独皮膜（参考例１〜１０、実施例１１）よりも成膜可能時間が長いのは異種皮膜の複合化によりガス耐食性が相乗的に向上したことによると考えられる。
〔強度試験〕
ガス耐食性試験と同サンプルを用い、ＪＩＳ Ｚ２２０１に基づいて引張試験を行い、強度を比較した。評価結果を表１に示す。
【００３７】
【表１】
表１の結果より、重金属の含有量を規制したアルミニウム合金、および各耐食性皮膜を形成したアルミニウム合金板は、高温、腐食雰囲気下における絶縁膜の成膜可能時間が長く、母材または各皮膜からの重金属および金属間化合物の放出量が少ないことを裏付けている。また、重金属含有量の規制により、金属化合物の生成量が少ないことに加え、欠陥の少ない皮膜が形成されて、重金属や金属間化合物が放出されにくいことも成膜可能時間延長に寄与していると推測される。さらに所定量のＳｉおよびＭｇを含有することで優れた強度が得られた。
【００３９】
これらの結果より、各実施例の皮膜形成処理用アルミニウム合金および皮膜を形成したアルミニウム合金板は、強度、耐食性が優れており、ＣＶＤ装置用材料、ＰＶＤ装置用材料、ＬＣＤ製造装置用材料、半導体製造装置用材料として好適である。
【００４０】
【発明の効果】
以上説明したように、この発明の皮膜形成処理用アルミニウム合金は、フッ化処理による単独皮膜、Ｎｉ−Ｐメッキ処理とフッ化処理による複合皮膜、陽極酸化処理とフッ化処理による複合皮膜のいずれかの耐食性皮膜を形成する処理を施すアルミニウム合金であって、Ｓｉ：０．２〜１．０wt％およびＭｇ：０．３〜２．０wt％を含有し、不純物としてのＦｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉの各含有量がそれぞれ０．１wt％以下に規制され、残部がＡｌおよび他の不純物からなるから、母材および形成される皮膜中の重金属含有量、およびこれらの重金属によって形成される金属間化合物量が少ない。また、これらの量が少ないことによって、欠陥の少ない皮膜を生成させることができて耐食性が優れ、高温熱サイクル、腐食環境下においても、皮膜欠陥からの重金属および金属間化合物の放出量が少ない。さらに、Ｓｉ、Ｍｇの含有により優れた強度が得ることができる。
【００４１】
前記皮膜形成処理用アルミニウム合金において、Ｓｉ含有量が０．４〜０．７wt％である場合、あるいはＭｇ含有量がは０．５〜１．５wt％であるには、特に優れた強度が得られる。
【００４２】
また、Ｆｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉの各含有量がそれぞれ０．０５wt％以下に規制されている場合には、特にこれらの重金属含有量および金属間化合物の少ない皮膜を形成することができる。
【００４３】
また、この発明の耐食性に優れたアルミニウム合金材は、母材が上述の化学組成であり、重金属含有量およびこれらの重金属によって形成される金属間化合物量が少ない。このため、表面に形成されている耐食性皮膜は欠陥の少ない耐食性に優れたものとなり、高温熱サイクル、腐食環境下においても、皮膜欠陥からの重金属および金属間化合物の放出量が少ない。また、Ｓｉ、Ｍｇの含有によって母材強度が優れている。
【００４４】
従って、高温熱サイクル、腐食環境下で使用されるＣＶＤ装置、ＰＶＤ装置、液晶ディスプレイ（ＬＣＤ）製造装置、半導体製造装置のいずれかにおけるチャンバー、サセプター、バッキングプレートのいずれかの材料として、この発明の皮膜形成処理用アルミニウム合金または耐食性に優れたアルミニウム合金材を使用することにより、これらの装置で処理または製造される製品への重金属および金属間化合物の汚染を抑制し、製品品質を向上させることができる。さらに、長時間の使用劣化によって耐食性皮膜が割れたり摩耗して母材が露出した場合でも、重金属含有量そのものが規制されているから放出量も少なく、製品への汚染による悪影響も少ない。
【００４５】
特に、前記耐食性皮膜が、フッ化処理皮膜の単独皮膜である場合は皮膜形成処理が容易である。また、前記耐食性皮膜が、Ｎｉ−Ｐメッキ処理とフッ化処理による複合皮膜、または陽極酸化処理とフッ化処理による複合皮膜である場合には、異種皮膜の複合化によって特に優れた耐食性が得られる。
【００４６】
また、この発明の耐食性に優れたアルミニウム合金材の製造方法は、上述の組成の合金母材に対して各皮膜形成処理を施すものであり、この発明の耐食性に優れたアルミニウム合金材を製造することができる。
【００４７】
また、この発明のアルミニウム合金および合金材は耐食性に優れているから、高温、腐食ガス雰囲気に曝されるあらゆる部材材料に適している。特にこのような環境で使用されるＣＶＤ装置、ＰＶＤ装置、液晶ディスプレイ（ＬＣＤ）製造装置、半導体製造装置のいずれかにおけるチャンバー、サセプター、バッキングプレートのいずれかの材料として用いられるアルミニウム合金材料として適し、優れた耐食性を有するこれらの装置を構成することができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an aluminum alloy that is suitably used as a manufacturing apparatus material such as a semiconductor or an LCD (liquid crystal display), for example, and has excellent corrosion resistance by a film forming process, an aluminum alloy material having excellent corrosion resistance, and a method for manufacturing the same.
[0002]
[Prior art]
As a material for chambers, susceptors, backing plates, etc. constituting manufacturing devices such as semiconductors and LCDs, an aluminum alloy, particularly an Al-Si JIS 5052 aluminum alloy or an Al-Si-Mg JIS 6061 aluminum alloy is used. Stretched and cast materials are often used. In addition, these manufacturing devices are used at high temperatures and in corrosive gas atmospheres such as silane (SiH 4 ) and fluorine-based or chlorine-based halogen gases. A hard anodized film is formed on the surface to improve corrosion resistance.
[0003]
However, even with such a surface treatment, depending on the use environment and the frequency of use, the surface deterioration occurred early, and the surface treatment had to be updated. In particular, in CVD and PVD processing apparatuses, cracks may occur due to the difference in thermal deformability between the base material and the anodic oxide film because the operating temperature is in a wide range from room temperature to about 400 ° C. and repeated thermal stress is applied. . During long-term use, the anodic oxide film may be worn by contact with the surface of the apparatus when the workpiece is processed even if there is no significant damage.
[0004]
Accordingly, as a manufacturing apparatus material such as a semiconductor, for example, JP-A-11-43734 proposes an aluminum alloy to which Mn, Cu, and Fe are added. This aluminum alloy generates thermally stable intermetallic compounds by adding heavy metals, and also creates a double-structured anodic oxide film that acts as a buffer when heated. In addition, the corrosion resistance is improved in a corrosive environment.
[0005]
JP-A-8-92684 proposes an Al—Mg alloy for fluorination treatment. This aluminum alloy is intended to improve corrosion resistance by a fluorinated passive film formed by fluorination treatment.
[0006]
[Problems to be solved by the invention]
However, in the aluminum alloy described in JP-A-11-43734 described above, an intermetallic compound such as an Al—Fe system in the base material is released by reacting with a corrosive gas due to a defect in the anodized film, or There is a problem that the intermetallic compound in the anodized film is released little by little by evaporation or deposition. When such an aluminum alloy is used in an apparatus for forming an insulating film such as a semiconductor, for example, the inside of the processing chamber is contaminated with the released intermetallic compound, and as a result, the generated insulating film is contaminated with the intermetallic compound. There was a problem that decreased.
[0007]
Further, the aluminum alloy described in JP-A-8-92684 also has insufficient corrosion resistance due to the formed fluorinated passive film, and further improvement in corrosion resistance is required.
[0008]
In view of the above technical background, an object of the present invention is to provide an aluminum alloy for film formation treatment excellent in strength and corrosion resistance under a high temperature thermal cycle and a corrosive atmosphere, an aluminum alloy material excellent in corrosion resistance, and a method for producing the same. .
[0009]
[Means for Solving the Problems]
In order to achieve the above object, the aluminum alloy for film formation treatment of the present invention comprises a single film by fluorination treatment, a composite film by Ni-P plating treatment and fluorination treatment, and a composite film by anodic oxidation treatment and fluorination treatment. a aluminum alloy subjected to the treatment to form either a corrosion-resistant coating, Si: 0.2~1.0wt% and Mg: containing 0.3~2.0wt%, Fe as impurities, Cu, Mn The basic gist is that the contents of Cr, Zn and Ni are each regulated to 0.1 wt% or less, and the balance is made of Al and other impurities.
[0010]
In the film forming treatment aluminum alloy, the Si content is 0.4 to 0.7 wt%, the Mg content is 0.5 to 1.5 wt%, and each content of Fe, Cu, Mn, Cr, Zn, and Ni Is preferably regulated to 0.05 wt% or less.
[0011]
The film forming treatment aluminum alloy is suitable as an aluminum alloy used as a material for a chamber, a susceptor, or a backing plate in any of a CVD apparatus , a PVD apparatus, a liquid crystal display (LCD) manufacturing apparatus, and a semiconductor manufacturing apparatus. Used for.
[0012]
The aluminum alloy material having excellent corrosion resistance according to the present invention contains Si: 0.2 to 1.0 wt% and Mg: 0.3 to 2.0 wt%, and includes Fe, Cu, Mn, Cr, Zn as impurities. Each content of Ni is regulated to 0.1 wt% or less, and the surface of the aluminum alloy base material consisting of Al and other impurities is applied to the surface of the single film by fluorination treatment, Ni-P plating treatment and fluorination treatment The basic point is that a corrosion-resistant film of any one of the composite film, the composite film by anodizing treatment and fluorination treatment is formed.
[0013]
In the aluminum alloy base material, the Si content is 0.4 to 0.7 wt%, the Mg content is 0.5 to 1.5 wt%, and each content of Fe, Cu, Mn, Cr, Zn, and Ni is Each is preferably regulated to 0.05 wt% or less.
[0014]
In addition, an aluminum alloy material excellent in corrosion resistance is an aluminum alloy material used as a material for a chamber, a susceptor, or a backing plate in any of a CVD apparatus , a PVD apparatus, a liquid crystal display (LCD) manufacturing apparatus, and a semiconductor manufacturing apparatus. Preferably used.
[0015]
The method for producing an aluminum alloy material having excellent corrosion resistance according to the present invention contains Si: 0.2 to 1.0 wt% and Mg: 0.3 to 2.0 wt%, and contains Fe, Cu, Mn, and Cr as impurities. , Zn and Ni contents are regulated to 0.1 wt% or less, and the surface of an aluminum alloy base material composed of Al and other impurities as the balance is applied to a single film by fluorination treatment, Ni-P plating treatment and fluoride. The basic gist is to perform a corrosion-resistant film forming treatment of any one of the composite film by the oxidization treatment and the composite film by the anodic oxidation treatment and the fluorination treatment .
[0016]
The aluminum alloy material having excellent corrosion resistance is suitable as an aluminum alloy material used as a material for a chamber, a susceptor, or a backing plate in any of a CVD apparatus , a PVD apparatus, a liquid crystal display (LCD) manufacturing apparatus, and a semiconductor manufacturing apparatus. Used for.
[0017]
In the chemical composition of the aluminum alloy for film formation treatment of the present invention and the aluminum alloy base material of the aluminum alloy material excellent in corrosion resistance, the significance of addition of each element and the significance of regulation are as follows.
[0018]
Si and Mg are both elements that improve the strength. When Si is less than 0.2 wt% and Mg is less than 0.3 wt%, the strength improvement effect is poor. When Si exceeds 1.0 wt%, the toughness decreases, and when Mg exceeds 2.0 wt%, the workability decreases. There is an inconvenience. Accordingly, the Si content is 0.2 to 1.0 wt%, and the Mg content is 0.3 to 2.0 wt%. Further, Mg has an effect of forming a fluoride passivation film together with fluorine when fluorination treatment is performed, and improving machinability. A preferable Si content is 0.4 to 0.7 wt%. Moreover, preferable Mg content is 0.5 to 1.5 wt%.
[0019]
In addition, if a large amount of heavy metals Fe, Cu, Mn, Cr, Zn and Ni as impurities are contained, the amount of Al-Fe-based intermetallic compound in the base material and the film increases, and from the film defects, metal The intermetallic compound is released by evaporation or precipitation, or reacts with a corrosive gas such as a halogen gas to drop out of the metal structure and be released. Even heavy metals alone are released. Further, when the heavy metal content and the intermetallic compound amount are increased, the defects of the film are increased, and the heavy metal and the intermetallic compound are easily released. When this aluminum alloy or aluminum alloy material is used as a material for a chamber, susceptor, or backing plate in any of a CVD apparatus , PVD apparatus, liquid crystal display (LCD) manufacturing apparatus, and semiconductor manufacturing apparatus , release The processed heavy metals and intermetallic compounds contaminate LCDs, semiconductors and the like to be processed or manufactured, thereby deteriorating product quality. Furthermore, in order to add Si and Mg within the above range to improve the strength, it is necessary to regulate heavy metals as impurities that generate intermetallic compounds. For this reason, it is necessary to regulate each heavy metal element to 0.1 wt% or less to suppress the amount of intermetallic compound produced and reduce film defects. The preferred contents of these heavy metal elements are each 0.05 wt% or less.
[0020]
In the aluminum alloy material having excellent corrosion resistance according to the present invention, a corrosion-resistant film is formed on the surface of the aluminum alloy base material having the above-described composition. As described above, since the coating is formed into a coating with few defects by controlling the composition of the base alloy, heavy metals and intermetallic compounds are hardly released even under high-temperature thermal cycles and corrosive environments, and excellent corrosion resistance, particularly It has gas corrosion resistance, and therefore has excellent corrosion resistance as an alloy material. Even if the coating is cracked or worn out due to long-term use deterioration and the base metal is exposed, the release amount is small because the heavy metal content itself in the base material is regulated, and adverse effects due to contamination of semiconductors, etc. There are few.
[0021]
Examples of the corrosion-resistant coating, can be exemplified a full Tsu of single coating treatment film or Ni-P plating and the composite coating by fluorination treatment or composite coating film by anodic oxidation treatment and fluorination treatment, were all excellent above Corrosion resistance is obtained. Among these, a single film can be recommended in terms of easy film formation treatment, and a composite film can be recommended in that the corrosion resistance can be synergistically improved by combining different types of films.
[0022]
Note that an alloy material having excellent gas corrosion resistance due to such a film exhibits excellent corrosion resistance against water.
[0023]
In the method for producing an aluminum alloy material having excellent corrosion resistance, each corrosion-resistant film forming treatment may be performed according to a conventional method, and the conditions are not limited.
[0024]
The anodizing treatment is performed using a sulfuric acid bath, an oxalic acid bath, or the like. For example, if the case of using an aluminum alloy material as a semiconductor like manufacturing device material, the liquid composition: 10% H 2 SO 4, the liquid temperature 0 +/- 2 ° C., a current density: DC2~4.5A / dm 2, the voltage When processed under the conditions of: 23 to 120 V, processing time: 60 minutes, a hard anodized film of about 50 μm can be formed.
[0025]
Examples of the fluorination treatment include a method in which fluorine gas or fluoride gas is brought into contact with the surface of the aluminum alloy base material under heating, or a method in which liquid fluoride is brought into contact, and a fluoride passivation film can be formed. .
[0026]
In the case of forming a composite film by Ni-P plating treatment and fluorination treatment, for example, after forming a plating film by performing Ni-P plating treatment using a nickel sulfate bath using hypophosphite as a reducing agent, The above-described fluorination treatment is performed. Thereby, the composite film of a Ni-P plating film and a fluoride passivation film is formed.
[0027]
Moreover, when forming the composite film by an anodizing process and a fluorination process, after performing the above-mentioned anodizing process and forming an anodized film, the above-mentioned fluorination process is performed. As a result, a composite film of the anodized film and the fluorinated passive film is formed.
[0028]
In either case, degreasing cleaning, etching, surface polishing, etc. as pretreatment of the film forming treatment, post-treatment washing, drying, heating, etc. are appropriately performed.
[0029]
Processing to the required shape is not limited as long as the conventional method is followed, but when used under high temperature thermal cycle and corrosive environment as a manufacturing equipment material such as semiconductor, in order to remove residual stress during cutting, grinding and joining It is preferable to perform heat treatment at 350 to 380 ° C. after each processing.
[0030]
In addition, the aluminum alloy and alloy material of the present invention are alloys and alloy materials suitable for all members exposed to high temperature and corrosive gas atmosphere, and in particular, CVD apparatus , PVD apparatus, liquid crystal display (LCD) manufacturing apparatus, semiconductor manufacturing It is suitably used as an aluminum alloy material used as a material for any chamber, susceptor, or backing plate of the apparatus .
[0031]
【Example】
The aluminum alloy having the composition shown in Table 1 is homogenized at 450 to 600 ° C., and then hot-rolled and cold-rolled to obtain an aluminum alloy having a thickness of 4 mm. I made a board.
[0032]
A film was formed on each aluminum alloy plate cut to 50 mm × 50 mm under the following conditions. However, Comparative Example 14 was not subjected to film formation treatment.
(Formation of sulfuric acid anodized film)
Bath composition: 15% H 2 SO 4 , bath temperature: 25 ° C., voltage: 20 V, treatment time: 20 minutes, anodizing treatment was performed to form a film with a thickness of 20 μm.
(Formation of oxalic acid anodized film)
Bath composition: 4% (COOH) 2 · 2H 2 O, bath temperature: 25 ° C., voltage: 30 V, treatment time: 30 minutes, anodization was performed to form a film with a film thickness of 15 μm.
(Formation of fluoride treatment film)
After chemical polishing as pretreatment, the film was kept at 260 ° C. for 24 hours in a chamber into which 20% fluorine gas (F 2 ) + 80% N 2 was introduced to form a fluorinated passive film having a thickness of 5 μm.
(Formation of Ni-P plating treatment and fluoride treatment composite film)
In a nickel sulfate bath using hypophosphite as a reducing agent, after electroless Ni-P plating was performed to form a 5 μm plating film, the inside of the chamber into which 20% fluorine gas (F 2 ) + 80% N 2 was introduced At 260 ° C. for 24 hours to form a composite film of a Ni—P plating film and a fluoride passivation film. The film thickness of this composite film was 30 μm.
(Formation of composite film of anodizing treatment and fluorination treatment)
After forming a 20 μm sulfuric acid anodic oxide film by the above-mentioned method, it is kept at 260 ° C. for 24 hours in a chamber into which 20% fluorine gas (F 2 ) + 80% N 2 is introduced. A composite film with the film was formed. The film thickness of this composite film was 15 μm.
[0033]
And the gas corrosion resistance test and the strength test were done with the following method with respect to the aluminum alloy plate in which each film was formed.
[Gas corrosion resistance test]
The aluminum alloy plate was put into a processing chamber of an insulating film forming apparatus in a semiconductor manufacturing process, and the time until an insulation failure of the semiconductor insulating film occurred was measured. The silicon wafer used for the test had a diameter of 200 mm, a thickness of 700 μm, a chamber size of 400 mm wide × 400 mm deep × 200 mm high, and an insulating film was formed by plasma CVD (400 ° C., corrosive gas: SiH 4 -N 2 O, plasma excitation atmosphere).
[0034]
In the insulation film formation test, insulation failure is caused by heavy metal contained as an impurity in an aluminum alloy or an intermetallic compound formed by this heavy metal contaminates the insulation film and has a large diffusion coefficient into Si or SiO 2 . This is presumed to be due to this. Therefore, it can be evaluated that the amount of release of heavy metals and intermetallic compounds from the aluminum alloy base material or each film decreases as the time until insulation failure, in other words, the longer the film formation time is. The evaluation results are shown in Table 1.
[0035]
Incidentally, in the aluminum alloy of the same composition of Example 9 and 10, the long film formation time of the oxalic acid anodized film than sulfuric anodized film it is presumed to be due to the heat resistance of the oxalate anodized film.
[0036]
In addition, two types of aluminum alloy plates (Examples 12 and 13) on which a composite film is formed are formed more than single films ( Reference Examples 1 to 10 and Example 11 ) of an anodized film or a fluorinated film. The long possible time is thought to be due to the synergistic improvement in gas corrosion resistance due to the composite of different types of coatings.
〔Strength test〕
Using the same sample as the gas corrosion resistance test, a tensile test was performed based on JIS Z2201, and the strength was compared. The evaluation results are shown in Table 1.
[0037]
[Table 1]
From the results of Table 1, the aluminum alloy plate in which the content of heavy metals is regulated and the aluminum alloy plate on which each corrosion-resistant film is formed are long in the time at which an insulating film can be formed at a high temperature and in a corrosive atmosphere. This confirms that the release amount of heavy metals and intermetallic compounds is small. Moreover, due to the regulation of heavy metal content, in addition to the small amount of metal compound produced, the formation of a film with few defects and the difficulty of releasing heavy metals and intermetallic compounds contributes to the extension of the film formation time. It is guessed. Furthermore, the outstanding intensity | strength was obtained by containing predetermined amount Si and Mg.
[0039]
From these results, the aluminum alloy plate for film formation treatment and the aluminum alloy plate on which the film is formed of each example have excellent strength and corrosion resistance, and materials for CVD devices, materials for PVD devices, materials for LCD manufacturing devices, semiconductors It is suitable as a material for manufacturing equipment.
[0040]
【The invention's effect】
As described above, the aluminum alloy for film formation treatment of the present invention is either a single film by fluorination treatment, a composite film by Ni-P plating treatment and fluorination treatment, or a composite film by anodic oxidation treatment and fluorination treatment. An aluminum alloy that is subjected to a treatment for forming a corrosion-resistant film of Si: 0.2 to 1.0 wt% Si: 0.3 to 2.0 wt%, Fe, Cu, Mn, Cr as impurities , Zn and Ni content is regulated to 0.1 wt% or less, and the balance is made of Al and other impurities, so the heavy metal content in the base material and the film to be formed, and these heavy metals are formed. The amount of intermetallic compound is small. Further, since these amounts are small, a film with few defects can be formed and the corrosion resistance is excellent, and the amount of heavy metal and intermetallic compounds released from the film defects is small even under a high temperature thermal cycle and a corrosive environment. Furthermore, excellent strength can be obtained by containing Si and Mg.
[0041]
In the aluminum alloy for film formation treatment, particularly excellent strength is obtained when the Si content is 0.4 to 0.7 wt%, or when the Mg content is 0.5 to 1.5 wt%. It is done.
[0042]
In addition, when each content of Fe, Cu, Mn, Cr, Zn and Ni is regulated to 0.05 wt% or less, a film with a small content of these heavy metals and intermetallic compounds should be formed. Can do.
[0043]
In the aluminum alloy material excellent in corrosion resistance of the present invention, the base material has the above-described chemical composition, and the heavy metal content and the amount of intermetallic compounds formed by these heavy metals are small. For this reason, the corrosion-resistant film formed on the surface is excellent in corrosion resistance with few defects, and the release amount of heavy metals and intermetallic compounds from the film defects is small even under high temperature thermal cycle and corrosive environment. Moreover, the base material strength is excellent by containing Si and Mg.
[0044]
Therefore, as a material for a chamber, a susceptor, or a backing plate in any one of a CVD apparatus , a PVD apparatus, a liquid crystal display (LCD) manufacturing apparatus, and a semiconductor manufacturing apparatus used in a high-temperature thermal cycle, a corrosive environment, By using an aluminum alloy for film formation treatment or an aluminum alloy material with excellent corrosion resistance, it is possible to suppress contamination of heavy metals and intermetallic compounds in products treated or manufactured by these devices and improve product quality. it can. Furthermore, even when the corrosion-resistant film is cracked or worn due to long-term use deterioration and the base material is exposed, the release amount is small because the heavy metal content itself is regulated, and the adverse effects due to contamination of the product are also small.
[0045]
In particular, the corrosion-resistant coating, when a single film of full Tsu treatment film is easy film-forming process. Further, when the corrosion-resistant film is a composite film by Ni-P plating treatment and fluorination treatment, or a composite film by anodization treatment and fluorination treatment, particularly excellent corrosion resistance can be obtained by combining different kinds of films. .
[0046]
Moreover, the manufacturing method of the aluminum alloy material excellent in corrosion resistance of the present invention is to perform each film forming treatment on the alloy base material having the above composition, and manufactures the aluminum alloy material excellent in corrosion resistance of the present invention. be able to.
[0047]
Moreover, since the aluminum alloy and alloy material of the present invention are excellent in corrosion resistance, they are suitable for all member materials exposed to high temperature and corrosive gas atmosphere. Particularly suitable as an aluminum alloy material used as a material of chamber, susceptor, backing plate in any of CVD apparatus , PVD apparatus, liquid crystal display (LCD) manufacturing apparatus, semiconductor manufacturing apparatus used in such an environment, These devices can be constructed with excellent corrosion resistance.
Claims (21)
Ｓｉ：０．２〜１．０wt％およびＭｇ：０．３〜２．０wt％を含有し、不純物としてのＦｅ、Ｃｕ、Ｍｎ、Ｃｒ、ＺｎおよびＮｉの各含有量がそれぞれ０．１wt％以下に規制され、残部がＡｌおよび他の不純物からなることを特徴とする皮膜形成処理用アルミニウム合金。 An aluminum alloy that is subjected to a treatment to form a corrosion-resistant coating of any one of a single coating by fluorination treatment, a composite coating by Ni-P plating treatment and fluorination treatment, and a composite coating by anodic oxidation treatment and fluorination treatment,
Si: 0.2 to 1.0 wt% and Mg: 0.3 to 2.0 wt%, and the contents of Fe, Cu, Mn, Cr, Zn and Ni as impurities are each 0.1 wt% or less An aluminum alloy for film formation treatment, characterized in that the balance is made of Al and other impurities.
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| JP2001315973A JP3871544B2 (en) | 2001-10-12 | 2001-10-12 | Aluminum alloy for film formation treatment, aluminum alloy material excellent in corrosion resistance and method for producing the same |
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| JP4168066B2 (en) | 2006-08-11 | 2008-10-22 | 株式会社神戸製鋼所 | Aluminum alloy for anodizing treatment used in plasma processing apparatus and manufacturing method thereof, aluminum alloy member having anodized film, and plasma processing apparatus |
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| WO2020008704A1 (en) * | 2018-07-04 | 2020-01-09 | 昭和電工株式会社 | Aluminum alloy member for forming fluoride film and aluminum alloy member having fluoride film |
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| JP7190491B2 (en) | 2018-07-04 | 2022-12-15 | 昭和電工株式会社 | Aluminum alloy member for forming fluoride film and aluminum alloy member having fluoride film |
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