JP2001172795A - Aluminum composite and method for surface-treating aluminum composite - Google Patents
Aluminum composite and method for surface-treating aluminum compositeInfo
- Publication number
- JP2001172795A JP2001172795A JP35451899A JP35451899A JP2001172795A JP 2001172795 A JP2001172795 A JP 2001172795A JP 35451899 A JP35451899 A JP 35451899A JP 35451899 A JP35451899 A JP 35451899A JP 2001172795 A JP2001172795 A JP 2001172795A
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- JP
- Japan
- Prior art keywords
- aluminum
- film
- polysilazane
- aluminum composite
- composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Silicon Polymers (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、陽極酸化皮膜を有
するアルミニウム複合品及び陽極酸化皮膜を有するアル
ミニウム複合品の表面処理方法に関する。この表面処理
されたアルミニウム複合品は、宇宙産業、航空機産業、
一般産業機械部品、光学機械、食品機械、自動車産業、
船舶産業、家庭用品等の広い分野において利用可能であ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an aluminum composite article having an anodized film and a method for treating the surface of an aluminum composite article having an anodized film. This surface-treated aluminum composite is used in the space industry, aircraft industry,
General industrial machinery parts, optical machinery, food machinery, automotive industry,
It can be used in a wide range of fields such as the marine industry and household goods.
【０００２】[0002]
【従来の技術】従来、アルミニウム又はアルミニウム合
金からなる基体に陽極酸化皮膜を施し、この多孔性酸化
皮膜にフルオロカーボン樹脂を含浸及び被覆して、アル
ミニウム複合品を製造することが知られている。2. Description of the Related Art It is conventionally known to produce an aluminum composite article by applying an anodized film to a substrate made of aluminum or an aluminum alloy, impregnating and coating this porous oxide film with a fluorocarbon resin.
【０００３】[0003]
【発明が解決しようとする課題】上記従来技術の場合、
基体上に形成された陽極酸化皮膜に生じるクラック、微
細孔をフルオロカーボン樹脂で塞ぐことによって、陽極
酸化皮膜を形成しただけのアルミニウム複合品よりも耐
摩耗性、耐食性等の改良された複合品を提供しようとす
るものであるが、この複合品を使用する状況によって
は、耐摩耗性、耐食性等が十分であるとはいえない。フ
ルオロカーボン樹脂では、クラック、微細孔を完全に塞
ぐことができないので、この従来技術のアルミニウム複
合品においては、放出ガスやパーティクルが多く、耐絶
縁性や耐食性が十分ではないからである。また、このフ
ルオロカーボン樹脂は、該複合品を利用する技術分野、
例えば半導体製造装置、電子部品製造装置、真空中で使
用される各種装置、部品等の分野においては不純物とな
る可能性が高いという問題もある。In the case of the above prior art,
By providing cracks and micropores in the anodic oxide film formed on the substrate with fluorocarbon resin, we provide composite products with improved abrasion resistance and corrosion resistance compared to aluminum composite products with only an anodic oxide film formed. However, depending on the situation in which the composite article is used, it cannot be said that the abrasion resistance, corrosion resistance, and the like are sufficient. This is because the fluorocarbon resin cannot completely close the cracks and micropores, so that in this conventional aluminum composite product, a large amount of gas and particles are emitted, and the insulation resistance and corrosion resistance are not sufficient. In addition, this fluorocarbon resin is a technical field utilizing the composite product,
For example, in the fields of semiconductor manufacturing equipment, electronic component manufacturing equipment, various devices used in a vacuum, parts, and the like, there is also a problem that the possibility of becoming an impurity is high.
【０００４】本発明は、このような従来技術の問題点を
解消するものであり、陽極酸化皮膜の形成されたアルミ
ニウム複合品の表面を処理して、放出ガスやパーティク
ルが少なく、かつ耐絶縁性や耐食性が向上した複合品を
得るための表面処理方法及びこのように表面処理して得
たアルミニウム複合品を提供することを課題とする。The present invention has been made to solve the above-mentioned problems of the prior art. The surface of an aluminum composite article on which an anodic oxide film is formed is treated to reduce the amount of emitted gas and particles, and to improve the insulation resistance. It is an object to provide a surface treatment method for obtaining a composite product having improved corrosion resistance and corrosion resistance, and an aluminum composite product obtained by such surface treatment.
【０００５】[0005]
【課題を解決するための手段】本発明者らは、陽極酸化
皮膜の形成されたアルミニウム複合品の表面特性を改良
すべく、鋭意研究を重ねた結果、該複合品の表面特性を
向上せしめるための表面処理材を見出し、本発明を完成
するに至った。Means for Solving the Problems The present inventors have conducted intensive studies to improve the surface characteristics of an aluminum composite product having an anodized film formed thereon. The present inventors have found a surface treatment material, and have completed the present invention.
【０００６】本発明のアルミニウム複合品は、アルミニ
ウム又はアルミニウム合金からなる基体と、該基体上に
形成された陽極酸化皮膜と、該陽極酸化皮膜上に形成さ
れたポリシラザン由来のシリカ皮膜とを有するものであ
る。ポリシラザンを焼成して得たシリカ皮膜が陽極酸化
皮膜のクラック、微細孔を塞ぐように設けられているの
で、本発明のアルミニウム複合品は、放出ガスやパーテ
ィクルが少なく、かつ耐絶縁性や耐食性が向上した所望
の表面特性を有する。The aluminum composite article of the present invention comprises a substrate made of aluminum or an aluminum alloy, an anodic oxide film formed on the substrate, and a polysilazane-derived silica film formed on the anodic oxide film. It is. Since the silica film obtained by firing the polysilazane is provided so as to close the cracks and micropores of the anodic oxide film, the aluminum composite product of the present invention has a small amount of outgassing and particles, and has insulation resistance and corrosion resistance. Has improved desired surface properties.
【０００７】また、本発明のアルミニウム複合品の表面
処理方法は、アルミニウム又はアルミニウム合金からな
る基体の表面に陽極酸化皮膜の形成されたアルミニウム
複合品の表面をポリシラザン溶液で処理するものであ
る。該陽極酸化皮膜の表面にポリシラザン溶液を塗布
し、乾燥し、次いで焼成することによって、上記のよう
な所望の表面特性を有するアルミニウム複合品が得られ
る。乾燥後の焼成による硬化は、常圧、１５０〜４００
℃で行うことが好ましい。焼成温度が１５０℃未満であ
ると硬質かつ緻密なシリカ皮膜が形成され難い、また、
ポリシラザンと酸素とが反応し難いという問題がある。
焼成温度が４００℃を超えるとアルミの母材の熱特性が
悪くなるという問題がある。Further, in the method for treating the surface of an aluminum composite article of the present invention, the surface of an aluminum composite article having an anodized film formed on the surface of a substrate made of aluminum or an aluminum alloy is treated with a polysilazane solution. A polysilazane solution is applied to the surface of the anodic oxide film, dried and then fired to obtain an aluminum composite product having the desired surface characteristics as described above. Curing by baking after drying is normal pressure, 150 to 400
It is preferably carried out at a temperature of ° C. When the firing temperature is less than 150 ° C., a hard and dense silica film is hardly formed,
There is a problem that it is difficult for polysilazane to react with oxygen.
If the firing temperature exceeds 400 ° C., there is a problem that the thermal characteristics of the aluminum base material deteriorate.
【０００８】[0008]
【発明の実施の形態】以下、本発明をさらに詳細に説明
する。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail.
【０００９】アルミニウム又はアルミニウム合金からな
る基体の表面に陽極酸化皮膜（以下、アルマイト皮膜と
も称す。）を形成する方法は特に制限されるものではな
い。硫酸浴法、シュウ酸浴法、有機酸浴法等の公知の陽
極酸化方法に従って、例えば５〜１００μｍ厚さの陽極
酸化皮膜を形成することができる。例えば、「表面技術
総覧」（(株)広信社、昭和５８年６月１５日発行）に記
載された方法に従って基体表面に陽極酸化皮膜を形成す
ることができる。The method of forming an anodic oxide film (hereinafter also referred to as an alumite film) on the surface of a substrate made of aluminum or an aluminum alloy is not particularly limited. According to a known anodic oxidation method such as a sulfuric acid bath method, an oxalic acid bath method, and an organic acid bath method, for example, an anodic oxide film having a thickness of 5 to 100 μm can be formed. For example, an anodic oxide film can be formed on the surface of a substrate according to the method described in “Surface Technology Overview” (Koshinsha Co., Ltd., issued on June 15, 1983).
【００１０】本発明において用いるポリシラザンは、
（−Ｓｉ−Ｎ−）の単位を２以上有する鎖状、環状、架
橋構造等を有する重合体である。本発明の表面処理方法
では、実質的に有機基を含まないポリシラザンを用いる
ことが好ましいが、アルコキシ基等の加水分解基がケイ
素原子に結合したポリシラザン、アルキル基等の有機基
が窒素原子に結合したポリシラザン等を用いることもで
きる。このようなポリシラザンは焼成により分解し、例
えば窒素原子が酸素原子で置換されて、硬質の、緻密な
二酸化ケイ素皮膜（以下、シリカ皮膜とも称す。）を形
成する。本発明で加水分解基や有機基を有しているポリ
シラザンを使用する場合でも、焼成の際の加水分解反応
により実質的にこれらの基を含まないシリカ皮膜が形成
され得る。本発明におけるポリシラザンとしては、例え
ば、特開平１１−２４０１０３号公報及び特開平９−３
１３３３号公報やそこで引用されている文献に記載され
ているポリシラザンを用いることができる。また、ポリ
シラザン溶液としては、これらの従来技術に記載されて
いるように、ポリシラザンを、ペンタン、シクロヘキサ
ン、キシレン等の脂肪族、脂環族及び芳香族炭化水素溶
媒等の公知溶媒であって、後の焼成工程において蒸発し
得る溶媒に溶解した溶液として用いることができる。The polysilazane used in the present invention is
It is a polymer having a chain, cyclic, crosslinked structure or the like having two or more units of (-Si-N-). In the surface treatment method of the present invention, it is preferable to use a polysilazane substantially containing no organic group. Polysilazane or the like can also be used. Such polysilazane is decomposed by firing, for example, a nitrogen atom is replaced by an oxygen atom, and forms a hard and dense silicon dioxide film (hereinafter also referred to as a silica film). Even when a polysilazane having a hydrolyzable group or an organic group is used in the present invention, a silica film substantially free of these groups can be formed by a hydrolysis reaction at the time of firing. Examples of the polysilazane in the present invention include JP-A-11-240103 and JP-A-9-3.
For example, polysilazane described in Japanese Patent No. 1333 and the literature cited therein can be used. Further, as described in these prior arts, polysilazane is a known solvent such as aliphatic, alicyclic and aromatic hydrocarbon solvents such as pentane, cyclohexane and xylene. Can be used as a solution dissolved in a solvent that can be evaporated in the firing step.
【００１１】本発明においてポリシラザン溶液を塗布す
る方法は特に制限されるものではなく、ポリシラザンが
陽極酸化皮膜の表面に適切な量で付着すると共に、クラ
ック、微細孔を満たすことができるような方法であれば
いずれでもよい。例えば、ディッピング法、スプレー
法、ブレードコート法、スピンコート法、刷毛塗り法等
の各種の通常の塗布方法を採用することができる。例え
ば、スプレー法の場合、所定の濃度に調整したポリシラ
ザン溶液を、吹付け圧力、溶液噴出量、空気使用量、吹
付け距離等を適宜調整して、除湿雰囲気中で、焼成後の
皮膜厚さが通常０．５〜２μｍになるように塗布するこ
とが好ましい。In the present invention, the method of applying the polysilazane solution is not particularly limited, and the polysilazane can be attached to the surface of the anodic oxide film in an appropriate amount and can fill cracks and micropores. Any may be used. For example, various usual coating methods such as a dipping method, a spray method, a blade coating method, a spin coating method, and a brush coating method can be employed. For example, in the case of the spraying method, the polysilazane solution adjusted to a predetermined concentration is sprayed, and the film thickness after firing is adjusted in a dehumidified atmosphere by appropriately adjusting the spraying pressure, the solution ejection amount, the amount of air used, the spraying distance, and the like. Is preferably applied so as to be usually 0.5 to 2 μm.
【００１２】ポリシラザン溶液の塗布前に、陽極酸化処
理後の基体を清浄化処理することにより、ポリシラザン
の付着性能が向上する。例えば、陽極酸化処理された基
体を純水で洗浄して、陽極酸化処理後に残留した物質等
を除去し、次いで、９０〜１００℃で行う沸騰水法又は
３〜４ｋｇ／ｃｍ2Ｇで行う加圧蒸気法等で封孔処理を
し、その後、所望によりラップ加工等の機械加工により
陽極酸化皮膜の表面を均一化し、そして常圧乾燥炉中で
２００〜３００℃で脱気するか又は真空乾燥炉中で１５
０〜２００℃で真空脱気した後に、ポリシラザン溶液を
塗布すれば、ポリシラザンを効率的に付着することがで
きる。Before the application of the polysilazane solution, the substrate after the anodic oxidation treatment is subjected to a cleaning treatment, whereby the adhesion performance of the polysilazane is improved. For example, the anodized substrate is washed with pure water to remove substances and the like remaining after the anodization treatment, and then subjected to a boiling water method at 90 to 100 ° C. or a heat treatment at 3 to 4 kg / cm 2 G. The pores are sealed by a pressure steam method or the like, and then, if necessary, the surface of the anodic oxide film is made uniform by machining such as lapping, and then deaerated at 200 to 300 ° C. in a normal pressure drying oven or vacuum dried. 15 in the furnace
If a polysilazane solution is applied after vacuum degassing at 0 to 200 ° C., polysilazane can be efficiently attached.
【００１３】また、ポリシラザン溶液塗布後の乾燥は、
通常、常圧乾燥炉中で、８０〜１００℃で、１０〜３０
分間行うことが好ましく、また、焼成は、常圧、１５０
〜４００℃で２〜４時間行うことが好ましい。The drying after the application of the polysilazane solution is as follows:
Usually, in an atmospheric drying oven at 80-100 ° C, 10-30
Minutes, and baking is performed at normal pressure, 150
It is preferable to carry out at a temperature of 400 ° C. for 2 to 4 hours.
【００１４】上記のようにしてポリシラザン溶液により
表面処理されたアルミニウム複合品においては、ガス放
出やパーティクルが少なく、電気絶縁性（耐プラズマ
性）が向上し、また、陽極酸化皮膜中のクラック、微細
孔内がシリカ皮膜で埋められるので、耐食性も向上す
る。さらに、不純物の存在をできるだけ避けなければな
らない技術分野、例えば半導体製造装置、電子部品製造
装置、真空中で使用される各種装置、部品等の分野で本
発明のアルミニウム複合品を利用する場合、シリカ皮膜
は不純物となる可能性がないので、技術分野を問わず利
用できる。In the aluminum composite article surface-treated with the polysilazane solution as described above, gas emission and particles are small, electric insulation (plasma resistance) is improved, and cracks and fine particles in the anodic oxide film are reduced. Since the pores are filled with the silica film, the corrosion resistance is also improved. Furthermore, when the aluminum composite article of the present invention is used in a technical field in which the presence of impurities must be avoided as much as possible, for example, in the fields of semiconductor manufacturing equipment, electronic component manufacturing equipment, various devices used in a vacuum, and parts, silica is used. Since the coating has no possibility of becoming an impurity, it can be used regardless of technical fields.
【００１５】[0015]
【実施例】（実施例１）まず、市販のアルミニウム合金
（Ａ５０５２）を前処理した。すなわち、公知の方法に
従い、通常の条件下、脱脂処理し、いわゆるアルピカ処
理といわれる化学研磨により表面処理した。その後、公
知の硫酸浴法により、下記の条件でアルマイト処理（陽
極酸化処理）して、表面に硬質アルマイト皮膜を形成せ
しめた。(Example 1) First, a commercially available aluminum alloy (A5052) was pretreated. That is, according to a known method, a degreasing treatment was performed under ordinary conditions, and a surface treatment was performed by chemical polishing called so-called alpica treatment. Thereafter, alumite treatment (anodizing treatment) was performed by a known sulfuric acid bath method under the following conditions to form a hard alumite film on the surface.
【００１６】 硫酸 ２００〜３００ ｇ／Ｌ 添加剤 ４ ｇ／Ｌ 硫酸アルミ ２０ ｇ／Ｌ 膜厚 ５０〜１００ μｍ このようにして硬質アルマイト皮膜の形成されたアルミ
ニウム合金を常温で３０分間純水洗浄した後、純水を用
いる沸騰水法で封孔処理した（９５℃、６０分間）。次
いで、硬質アルマイト皮膜表面をラップ加工により均一
化した後、真空乾燥炉に入れ、真空脱気処理（１０-2Ｔ
ｏｒｒ、１５０℃）を行った。Sulfuric acid 200-300 g / L Additive 4 g / L Aluminum sulfate 20 g / L Film thickness 50-100 μm The aluminum alloy thus formed with a hard alumite film was washed with pure water at room temperature for 30 minutes. Thereafter, sealing was performed by a boiling water method using pure water (95 ° C., 60 minutes). Next, the surface of the hard alumite film is homogenized by lapping, and then placed in a vacuum drying furnace to perform vacuum degassing (10 -2 T).
orr, 150 ° C.).
【００１７】このようにして得られた硬質アルマイト皮
膜の形成されたアルミニウム合金に対し、ポリシラザン
溶液（東燃(株)製）を、以下の条件下、スプレー法によ
り塗布した。A polysilazane solution (manufactured by Tonen Co., Ltd.) was applied to the aluminum alloy thus formed with the hard alumite film by a spray method under the following conditions.
【００１８】 皮膜厚さ ０．５〜２．０ μｍ 吹き付け圧力 ３．０ ｋｇ／ｃｍ2 溶液噴出量 １５ ｍＬ／ｍｉｎ 空気使用量 ３５ Ｌ／ｍｉｎ 吹付け距離 ２００ ｍｍ その後、常圧乾燥炉中で、常圧、８０℃で、３０分間乾
燥処理し、引き続いて、４００℃で、２時間焼成して硬
化処理し、硬質アルマイト皮膜上に塗布したポリシラザ
ンをガラス皮膜化（ＳｉＯ2皮膜化）した。図１(Ａ)に
基体１上に硬質アルマイト皮膜２（この皮膜にはクラッ
ク、微細孔３が生じている）を形成した複合品の断面形
状を模式的に示し、また、図１(Ｂ)に図１(Ａ)の複合品
表面にポリシラザン溶液を塗布し、焼成して得た複合品
の断面形状を模式的に示す。図１(Ａ)及び(Ｂ)から明ら
かなようにポリシラザンを焼成して得られたシリカ皮膜
４がアルマイト皮膜のクラック、微細孔３内に入り込
み、これらを塞いでいることがわかる。Film thickness 0.5-2.0 μm Spraying pressure 3.0 kg / cm 2 Solution ejection amount 15 mL / min Air consumption 35 L / min Spraying distance 200 mm Then, in normal pressure drying oven After drying at 80 ° C. and normal pressure for 30 minutes, the film was baked at 400 ° C. for 2 hours for curing, and the polysilazane applied on the hard alumite film was formed into a glass film (SiO 2 film). FIG. 1A schematically shows a cross-sectional shape of a composite article having a hard alumite film 2 (cracks and micropores 3 formed in this film) formed on a substrate 1. FIG. FIG. 1A schematically shows a cross-sectional shape of a composite product obtained by applying a polysilazane solution to the surface of the composite product of FIG. As is clear from FIGS. 1A and 1B, it can be seen that the silica film 4 obtained by firing the polysilazane enters cracks and micropores 3 of the alumite film and blocks them.
【００１９】上記のようにしてポリシラザン溶液を用い
て表面処理した硬質アルマイト皮膜の施されたアルミニ
ウム合金複合品について、また、比較のために、ポリシ
ラザン処理していないアルミニウム合金複合品について
も、以下のような特性を調べた。 （１）表面観察によるクラックの状態 上記アルミニウム複合品の硬質アルマイト皮膜（ポリシ
ラザン未処理及び処理済）の表面を顕微鏡で観察した。
対照複合品であるポリシラザン未処理の硬質アルマイト
皮膜表面（以下、対照複合品と称す。）の顕微鏡写真を
図２(Ａ)に示し、また、本実施例の複合品であるポリシ
ラザン処理した硬質アルマイト皮膜表面（以下、本発明
複合品と称す。）の顕微鏡写真を図２(Ｂ)に示す。図２
(Ａ)からは、硬質アルマイト皮膜にクラックが発生して
いることが観察されるが、図２(Ｂ)からは、図２(Ａ)に
示したクラック発生硬質アルマイト皮膜に対するポリシ
ラザン処理により、硬質アルマイト皮膜表面が完全にガ
ラス化した皮膜（厚さ：約１〜２μｍ）で覆われて、ク
ラック、微細孔内部が埋められていることがわかる。従
って、パーティクルがなくなり、また、耐食性も向上す
る。 （２）ガス放出特性 上記対照複合品及び本発明複合品について、図３に概略
図を示すロードロック式の昇温脱離測定装置１号機を用
いてガス放出特性を調べた。The aluminum alloy composite article provided with the hard alumite film surface-treated with the polysilazane solution as described above, and for comparison, the aluminum alloy composite article not subjected to the polysilazane treatment, are as follows. Such characteristics were investigated. (1) State of Crack by Surface Observation The surface of the hard alumite film (untreated and treated with polysilazane) of the aluminum composite article was observed with a microscope.
FIG. 2 (A) shows a micrograph of the surface of a hard alumite film not treated with polysilazane as a control composite product (hereinafter referred to as a control composite product), and the hard alumite treated with polysilazane which is a composite product of this example. FIG. 2B shows a micrograph of the surface of the film (hereinafter, referred to as the composite product of the present invention). FIG.
From (A), it is observed that cracks are generated in the hard anodized film, but from FIG. 2 (B), the hard anodized film having cracks shown in FIG. It can be seen that the surface of the alumite film was completely covered with a vitrified film (thickness: about 1 to 2 μm), and cracks and the inside of the micropores were filled. Therefore, particles are eliminated and corrosion resistance is improved. (2) Gas release characteristics The control composite product and the composite product of the present invention were examined for gas release characteristics using a load-lock type thermal desorption measuring device No. 1 whose schematic diagram is shown in FIG.
【００２０】ロードロック室１１をターボ分子ポンプ１
２で３０分間排気後、試料１３をマニピュレータ１４で
測定室に移動し、測定室内で、１０分間排気したあと、
測定を開始した。ロードロック室１１のターボ分子ポン
プ１２で排気を開始したときを測定の０分にした。ガス
放出速度をオリフィス１５の上流及び下流側に設置した
Ｂ−Ａ真空計１６、１７及びオリフィスの上流側に設置
した四重極質量分析計（ＭＳＱ−４００）１８で測定し
た。この結果に基づき、単位面積当たりのガス放出速度
ｑ（Ｐａ・ｍ・Ｓ-1）を次式（１）により算出した。The load lock chamber 11 is connected to the turbo molecular pump 1
After evacuation for 30 minutes at 2, the sample 13 was moved to the measurement room by the manipulator 14 and evacuated for 10 minutes in the measurement room.
The measurement was started. The time when the evacuation was started by the turbo molecular pump 12 in the load lock chamber 11 was set to 0 minute of the measurement. The gas release rate was measured by BA vacuum gauges 16 and 17 installed upstream and downstream of the orifice 15 and a quadrupole mass spectrometer (MSQ-400) 18 installed upstream of the orifice. Based on the result, the gas release rate per unit area q (Pa · m · S −1 ) was calculated by the following equation (1).
【００２１】 ｑ ＝ Ｃ(Ｐ1−Ｐ2)／Ａ （１） 式（１）中、Ｐ1はＢ−Ａ真空計１６で測定したオリフ
ィス上流側圧力（Ｐａ）を表し、Ｐ2はＢ−Ａ真空計１
７で測定したオリフィス下流側圧力（Ｐａ）を表し、Ｃ
はオリフィスのコンダクタンス（９．６×１０-3ｍ3／
ｓ：Ｎ2）を表し、Ａは幾何学的表面積（ｍ2）を表す。Q = C (P 1 −P 2 ) / A (1) In the equation (1), P 1 represents an orifice upstream pressure (Pa) measured by the BA vacuum gauge 16, and P 2 represents B -A vacuum gauge 1
7 represents the pressure (Pa) on the downstream side of the orifice measured in
Is the conductance of the orifice (9.6 × 10 −3 m 3 /
s: N 2 ), and A represents the geometric surface area (m 2 ).
【００２２】上記対照複合品及び本発明複合品のガス放
出特性について、室温（２５〜２７℃）で大気圧から排
気したときのガス放出速度（Ｐａ・ｍ・Ｓ-1）と経過時
間（ｍｉｎ）との関係を図４に示す。図４から明らかな
ように、ポリシラザン処理によってガス放出特性が向上
しており、ポリシラザン処理しない場合と比べて、１０
-3Ｐａ・ｍ・Ｓ-1のオーダーから１０-5Ｐａ・ｍ・Ｓ-1
のオーダーまで２桁以上減少し、ガス放出特性が改良さ
れている。 （３）耐薬品性 上記対照複合品及び本発明複合品について、次のように
して耐薬品性を調べた。各試料を水酸化ナトリウム溶液
（１５０ｇ／Ｌ、５０℃）中に浸漬し、それぞれの試料
について、浸漬時間（ｍｉｎ）と膜厚変化との間の関係
を調べ、耐薬品性を検討した。得られた結果を図５に示
す。図５から明らかなように、硬質アルマイト処理のみ
の試料は、約３分の浸漬でほとんどの皮膜が溶解したの
に対し、硬質アルマイト処理とポリシラザン処理とを行
った試料は、２０分の浸漬でも皮膜はほとんど溶解せ
ず、膜厚はほとんど減少していなかった。本発明複合品
についてのこのような耐薬品性は、石英ガラスの場合と
同様であった。 （４）耐絶縁性 上記対照複合品及び本発明複合品について、ＡＳＴＭ
Ｄ−１４９記載の方法に従って、絶縁破壊電圧を測定し
た。得られた結果を以下に示す。With respect to the gas release characteristics of the control composite product and the composite product of the present invention, the gas release rate (Pa · m · S −1 ) and the elapsed time (min) when exhausted from atmospheric pressure at room temperature (25 to 27 ° C.) 4) are shown in FIG. As is clear from FIG. 4, the gas emission characteristics are improved by the polysilazane treatment, and the gas emission characteristics are improved by 10% compared to the case without the polysilazane treatment.
From the order of -3 Pa ・ m ・ S -1 to 10 -5 Pa ・ m ・ S -1
And the gas emission characteristics have been improved. (3) Chemical Resistance The chemical resistance of the control composite product and the composite product of the present invention was examined as follows. Each sample was immersed in a sodium hydroxide solution (150 g / L, 50 ° C.), and for each sample, the relationship between the immersion time (min) and the change in film thickness was examined, and the chemical resistance was examined. The results obtained are shown in FIG. As is clear from FIG. 5, the sample subjected to hard alumite treatment alone dissolved most of the film in about 3 minutes of immersion, whereas the sample subjected to hard alumite treatment and polysilazane treatment was subjected to immersion for 20 minutes. The film hardly dissolved and the film thickness hardly decreased. Such chemical resistance of the composite article of the present invention was similar to that of quartz glass. (4) Insulation resistance ASTM was used for the control composite product and the composite product of the present invention.
The dielectric breakdown voltage was measured according to the method described in D-149. The results obtained are shown below.
【００２３】 対照複合品 ２０ＫＶ／ｍｍ 本発明複合品 ２６０ＫＶ／ｍｍ 硬質アルマイト処理とポリシラザン処理とを行った本発
明複合品は、硬質アルマイト処理のみの対照複合品の１
０倍以上の耐絶縁性を有しており、耐プラズマ性を有す
ることがわかる。Control composite product 20 KV / mm The composite product of the present invention 260 KV / mm The composite product of the present invention which has been subjected to the hard alumite treatment and the polysilazane treatment is one of the control composite products having only the hard alumite treatment.
It can be seen that it has 0 times or more the insulation resistance and has the plasma resistance.
【００２４】[0024]
【発明の効果】本発明の表面処理方法によれば、陽極酸
化皮膜が形成されたアルミニウム複合品の表面をポリシ
ラザン溶液で処理し、焼成することにより、陽極酸化皮
膜に生じるクラックや微細孔内部がシリカ皮膜で埋めら
れ、表面がシリカ皮膜で覆われるので、かくして処理さ
れたアルミニウム複合品では、放出ガスやパーティクル
が少なく、また、耐絶縁性や耐食性が向上し得る。ま
た、シリカ皮膜は不純物となる可能性がないので、不純
物の存在をできるだけ避けなければならない技術分野で
本発明の表面処理されたアルミニウム複合品を利用する
場合でも、問題はない。According to the surface treatment method of the present invention, the surface of the aluminum composite article on which the anodic oxide film is formed is treated with a polysilazane solution and baked, so that cracks and fine pores generated in the anodic oxide film are reduced. Since the surface is covered with the silica coating and the surface is covered with the silica coating, the thus treated aluminum composite product has less outgassing and particles, and can have improved insulation resistance and corrosion resistance. Further, since the silica film has no possibility of becoming an impurity, there is no problem even when the surface-treated aluminum composite article of the present invention is used in a technical field in which the presence of the impurity must be avoided as much as possible.
【図１】（Ａ）対照複合品の断面形状を模式的に示す断
面図。 （Ｂ）本発明における複合品の断面形状を模式的に示す
断面図。FIG. 1A is a cross-sectional view schematically showing a cross-sectional shape of a control composite product. (B) Sectional drawing which shows typically the cross-sectional shape of the composite article in this invention.
【図２】（Ａ）対照複合品の硬質アルマイト皮膜表面の
状態を示す顕微鏡写真。 （Ｂ）本発明における複合品の硬質アルマイト皮膜表面
の状態を示す顕微鏡写真。FIG. 2 (A) is a micrograph showing the state of the surface of a hard alumite film of a control composite product. (B) A micrograph showing the state of the surface of the hard alumite film of the composite article in the present invention.
【図３】ガス放出特性を調べるためのロードロック式昇
温脱離測定装置１号機の構成を概略的に示す構成図。FIG. 3 is a configuration diagram schematically showing a configuration of a load-lock type thermal desorption measuring device No. 1 for examining gas release characteristics.
【図４】本発明における複合品について、対照複合品と
比べて、ガス放出速度（Ｐａ・ｍ・Ｓ-1）と経過時間
（ｍｉｎ）との関係を示すグラフ。FIG. 4 is a graph showing the relationship between the gas release rate (Pa · m · S −1 ) and the elapsed time (min) for the composite product of the present invention, as compared to the control composite product.
【図５】本発明における複合品について、対照複合品と
比べて、水酸化ナトリウム溶液中での浸漬時間（ｍｉ
ｎ）と膜厚変化との関係を示すグラフ。FIG. 5 shows the immersion time (mi) in the sodium hydroxide solution for the composite product of the present invention, as compared with the control composite product.
7 is a graph showing a relationship between n) and a change in film thickness.
１ 基体 ２ 硬質アルマ
イト皮膜 ３ クラック、微細孔 ４ シリカ皮膜 １１ ロードロック室 １２ ターボ分
子ポンプ １３ 試料 １４ マニピュ
レータ １５ オリフィス １６ Ｂ−Ａ真
空計 １７ Ｂ−Ａ真空計 １８ 四重極質
量分析計DESCRIPTION OF SYMBOLS 1 Substrate 2 Hard anodized film 3 Crack, micropore 4 Silica film 11 Load lock chamber 12 Turbo molecular pump 13 Sample 14 Manipulator 15 Orifice 16 BA vacuum gauge 17 BA vacuum gauge 18 Quadrupole mass spectrometer
Claims (3)
なる基体と、該基体上に形成された陽極酸化皮膜と、該
陽極酸化皮膜上に形成されたポリシラザン由来の二酸化
ケイ素皮膜とを有することを特徴とするアルミニウム複
合品。1. An aluminum having a substrate made of aluminum or an aluminum alloy, an anodic oxide film formed on the substrate, and a polysilazane-derived silicon dioxide film formed on the anodic oxide film. Composite products.
なる基体の表面に陽極酸化皮膜の形成されたアルミニウ
ム複合品の表面処理方法において、該陽極酸化皮膜の表
面にポリシラザン溶液を塗布し、乾燥し、次いで焼成す
ることを特徴とするアルミニウム複合品の表面処理方
法。2. A method for treating a surface of an aluminum composite article having an anodized film formed on the surface of a substrate made of aluminum or an aluminum alloy, wherein a polysilazane solution is applied to the surface of the anodized film, dried and then fired. A method for surface treating an aluminum composite article, comprising:
われることを特徴とする請求項２に記載のアルミニウム
複合品の表面処理方法。3. The surface treatment method for an aluminum composite article according to claim 2, wherein the sintering is performed at a normal pressure at 150 to 400 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35451899A JP2001172795A (en) | 1999-12-14 | 1999-12-14 | Aluminum composite and method for surface-treating aluminum composite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35451899A JP2001172795A (en) | 1999-12-14 | 1999-12-14 | Aluminum composite and method for surface-treating aluminum composite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001172795A true JP2001172795A (en) | 2001-06-26 |
Family
ID=18438107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35451899A Withdrawn JP2001172795A (en) | 1999-12-14 | 1999-12-14 | Aluminum composite and method for surface-treating aluminum composite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001172795A (en) |
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