JP3506827B2 - Surface-treated aluminum material and method for producing the same - Google Patents
Surface-treated aluminum material and method for producing the sameInfo
- Publication number
- JP3506827B2 JP3506827B2 JP34419195A JP34419195A JP3506827B2 JP 3506827 B2 JP3506827 B2 JP 3506827B2 JP 34419195 A JP34419195 A JP 34419195A JP 34419195 A JP34419195 A JP 34419195A JP 3506827 B2 JP3506827 B2 JP 3506827B2
- Authority
- JP
- Japan
- Prior art keywords
- aluminum
- anodic oxide
- oxide film
- porous anodic
- aluminum material
- 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.)
- Expired - Fee Related
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- Other Surface Treatments For Metallic Materials (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、化学気相蒸着（Ｃ
ＶＤ）装置、イオンプレーティング装置、ドライエッチ
ング装置、プラズマＣＶＤ装置、スパッタリング装置の
ような半導体製造装置あるいは薄膜形成装置等の真空機
器における真空チャンバーやその部品の表面材として用
いられる表面処理アルミニウム材とその製造方法に関
し、真空環境下でのガス放出量が少なく、真空特性及び
耐食性を高めたものである。TECHNICAL FIELD The present invention relates to chemical vapor deposition (C).
VD) equipment, ion plating equipment, dry etching equipment, plasma CVD equipment, surface treatment aluminum material used as the surface material of vacuum chambers in vacuum equipment such as thin film forming equipment, such as semiconductor manufacturing equipment such as sputtering equipment Regarding the manufacturing method, the amount of gas released in a vacuum environment is small, and the vacuum characteristics and corrosion resistance are improved.
【０００２】[0002]
【従来の技術】従来、半導体製造装置あるいは薄膜形成
装置等の真空機器における真空チャンバーやその部品の
表面材としては、ステンレス鋼が用いられているが、ス
テンレス鋼の使用は、重量が重いことや、クロム、ニッ
ケルなどの重金属が系内に混入することに起因して半導
体等の薄膜の性能が低下してしまう場合があるため、ア
ルミニウムまたはアルミニウム合金材の使用が試みられ
ている。ところがアルミニウムまたはアルミニミウム合
金を用いた場合においては、エッチングに用いる塩素ガ
スやフッ素プラズマ等により腐食を受ける問題がある。2. Description of the Related Art Conventionally, stainless steel has been used as a surface material of a vacuum chamber and its parts in a vacuum equipment such as a semiconductor manufacturing apparatus or a thin film forming apparatus. The use of aluminum or aluminum alloy materials has been attempted because the performance of thin films such as semiconductors may deteriorate due to the incorporation of heavy metals such as chromium and nickel into the system. However, when aluminum or aluminum alloy is used, there is a problem that it is corroded by chlorine gas or fluorine plasma used for etching.
【０００３】そこでこのような問題を解決するために、
アルミニウムまたはアルミニミウム合金の表面に硫酸電
解液により多孔質陽極酸化処理を施して多孔質陽極酸化
皮膜を形成したアルミニウム材が考えられている。この
多孔質陽極酸化皮膜は、膜厚を薄くすると耐食性が悪く
なるため、通常厚さ１０μｍ以上に形成されている。し
かしながらこのような多孔質陽極酸化皮膜を有するアル
ミニウム材を前述の真空機器等に用いる場合に加熱脱ガ
ス処理を施すと、皮膜にクラックが生じ耐食性が低下し
てしまうという問題がある。また、硫酸浴、シュウ酸浴
で得られた多孔質陽極酸化皮膜は、含水量が封孔処理後
で１５重量％程度と極めて多く、また、アニオン含有量
も１２〜１５重量％程度と極めて多く、真空環境下での
放出ガス量が多いことから、真空機器内を高真空にする
という目的を十分に達成できないという問題があった。
また、この陽極酸化皮膜にあっては、表面に微小穴の形
成が避けられないことから、空孔率が５〜６０％と非常
に高く（表面が多孔質で）、従って表面積が大きくな
り、吸着される水分やガス等も多くなってしまう。Therefore, in order to solve such a problem,
An aluminum material in which a porous anodic oxide film is formed by subjecting the surface of aluminum or an aluminum alloy to a porous anodic oxidation treatment with a sulfuric acid electrolytic solution is considered. This porous anodic oxide film is generally formed to have a thickness of 10 μm or more because the corrosion resistance deteriorates when the film thickness is reduced. However, when an aluminum material having such a porous anodic oxide film is used in the above-mentioned vacuum equipment or the like, if a heating degassing process is carried out, there is a problem that the film is cracked and the corrosion resistance is lowered. In addition, the porous anodic oxide film obtained in the sulfuric acid bath and the oxalic acid bath has an extremely large water content of about 15% by weight after the sealing treatment, and an anion content of about 12 to 15% by weight. However, since the amount of released gas is large in a vacuum environment, there has been a problem that the purpose of making the inside of the vacuum equipment a high vacuum cannot be sufficiently achieved.
Further, in this anodized film, since the formation of minute holes is inevitable on the surface, the porosity is very high at 5-60% (the surface is porous), and therefore the surface area becomes large, A large amount of water and gas will be adsorbed.
【０００４】また、前記真空機器では前述したように塩
素ガス等の反応性ガスやプラズマ等を用いて半導体基板
のエッチングが行われているが、このとき、前記多孔質
陽極酸化皮膜表面から放出される水分やアニオンがこれ
らの反応性ガスやプラズマと反応すると、エッチングが
均一に為されず、半導体の特性が不安定になる問題もあ
った。In the vacuum equipment, the semiconductor substrate is etched by using a reactive gas such as chlorine gas or plasma as described above. At this time, the semiconductor substrate is released from the surface of the porous anodic oxide film. When water or anions contained therein react with these reactive gases or plasma, there is a problem that the characteristics of the semiconductor become unstable due to uneven etching.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、上記事情に
鑑みてなされたもので、真空環境下でのガス放出量が少
なく、真空特性及び耐食性が優れた表面処理アルミニウ
ム材と、その製造方法を提供することにある。SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and is a surface-treated aluminum material which has a small amount of gas released in a vacuum environment and is excellent in vacuum characteristics and corrosion resistance, and a method for producing the same. To provide.
【０００６】[0006]
【課題を解決するための手段】本願発明者は、真空環境
下で前述のような問題を生じるアルミニウム材からのガ
スの放出量を低減すべく、種々の検討及び実験を重ねた
結果、以下に述べる無孔質陽極酸化皮膜を形成すること
が極めて有効であることを究明し、本願発明に至ったの
である。すなわち、請求項１記載の表面処理アルミニウ
ム材にあっては、アルミニウムまたはアルミニウム合金
の表面に、ベーキング処理が施された無孔質陽極酸化皮
膜が形成され、該無孔質陽極酸化皮膜は厚さが３００〜
７０００Å、含水量が３％以下、アルミニウムに対する
アニオンの含有量が重量比で０．０５以下であることを
特徴とする。また、請求項２記載の表面処理アルミニウ
ム材にあっては、請求項１記載の表面処理アルミニウム
材において、アニオン含有量が無孔質陽極酸化皮膜中の
硼素／アルミニウム重量比またはリン／アルミニウム重
量比で０．０５以下であることを特徴とする。また、請
求項３記載の表面処理アルミニウム材にあっては、請求
項１又は２記載の表面処理アルミニウム材において、無
孔質陽極酸化皮膜の空孔率が５％以下であることを特徴
とする。The inventor of the present application has conducted various studies and experiments in order to reduce the amount of gas released from an aluminum material that causes the above-mentioned problems in a vacuum environment. The inventors have found out that it is extremely effective to form the non-porous anodic oxide film described below, and have arrived at the present invention. That is, in the surface-treated aluminum material according to claim 1, a non-porous anodized film that has been subjected to a baking treatment is formed on the surface of aluminum or an aluminum alloy, and the non-porous anodized film has a thickness. Is 300-
7,000Å, the water content is 3% or less, and the anion content relative to aluminum is 0.05 or less in weight ratio. Further, in the surface-treated aluminum material according to claim 2, in the surface-treated aluminum material according to claim 1, the anion content is boron / aluminum weight ratio or phosphorus / aluminum weight ratio in the nonporous anodized film. And is 0.05 or less. The surface-treated aluminum material according to claim 3 is characterized in that, in the surface-treated aluminum material according to claim 1 or 2, the non-porous anodic oxide film has a porosity of 5% or less. .
【０００７】請求項４記載の表面処理アルミニウム材の
製造方法にあっては、アルミニウムまたはアルミニウム
合金を、硼酸、硼酸塩、リン酸塩、アジピン酸塩の群か
ら選ばれる１種または２種以上からなる電解質水溶液に
より電解し、アルミニウムまたはアルミニウム合金の表
面に無孔質陽極酸化皮膜を形成する工程と、該無孔質陽
極酸化皮膜の表面に１５０〜３５０℃のベーキング処理
を施して該無孔質陽極酸化皮膜の含水量を３重量％以
下、アルミニウムに対するアニオンの含有量を重量比で
０．０５以下にする工程を備えることを特徴とする。ま
た、請求項５記載の表面処理アルミニウム材の製造方法
にあっては、請求項４記載の表面処理アルミニウム材の
製造方法において、ベーキング処理を真空環境下で行う
ことを特徴とする。In the method for producing a surface-treated aluminum material according to claim 4, aluminum or aluminum alloy is selected from one or more selected from the group consisting of boric acid, borate, phosphate and adipate. To form a non-porous anodic oxide film on the surface of aluminum or an aluminum alloy, and subjecting the surface of the non-porous anodic oxide film to a baking treatment at 150 to 350 ° C. The method is characterized by comprising a step of setting the water content of the anodized film to 3% by weight or less and the anion content to aluminum of 0.05 or less in weight ratio. Further, in the method for producing a surface-treated aluminum material according to claim 5, the method for producing a surface-treated aluminum material according to claim 4 is characterized in that the baking treatment is performed in a vacuum environment.
【０００８】[0008]
【発明の実施の形態】以下、本発明の表面処理アルミニ
ウム材について、その製造方法により詳しく説明する。
本発明の表面処理アルミニウム材の素材となるアルミニ
ウムまたはアルミニウム合金としては、特に限定され
ず、純アルミ系の１０００系合金、Ａｌ−Ｃｕ系、Ａｌ
−Ｃｕ−Ｍｇ系の２０００系合金、Ａｌ−Ｍｎ系の３０
００系合金、Ａｌ−Ｓｉ系の４０００系合金、Ａｌ−Ｍ
ｇ系の５０００系合金、Ａｌ−Ｍｇ−Ｓｉ系の６０００
系合金、Ａｌ−Ｚｎ−Ｍｇ−Ｃｕ系、Ａｌ−Ｚｎ−Ｍｇ
系の７０００系合金、７Ｎ０１合金、Ａｌ−Ｆｅ−Ｍｎ
系の８０００系合金などが用いられ、成形用合金、構造
用合金、電気用合金、ＡＣ１Ａ、ＡＣ２Ａ、ＡＣ３Ａ、
ＡＣ４Ｂなどの鋳造用合金が用いられる。BEST MODE FOR CARRYING OUT THE INVENTION The surface-treated aluminum material of the present invention will be described in detail below by its manufacturing method.
The aluminum or aluminum alloy used as the material of the surface-treated aluminum material of the present invention is not particularly limited, and is a pure aluminum 1000 series alloy, Al-Cu series, Al.
-Cu-Mg-based 2000 series alloy, Al-Mn-based 30
00 series alloy, Al-Si series 4000 series alloy, Al-M
g series 5000 series alloy, Al-Mg-Si series 6000
System alloy, Al-Zn-Mg-Cu system, Al-Zn-Mg
7000 series alloy, 7N01 alloy, Al-Fe-Mn
8000 series alloys and the like are used, forming alloys, structural alloys, electrical alloys, AC1A, AC2A, AC3A,
Casting alloys such as AC4B are used.
【０００９】また、これらの合金に溶体化処理、時効処
理などの種々の調質処理を施したものも用いられる。さ
らに、これらのアルミニウム合金の表面にクラディング
したクラッド材も使用できる。本発明にあっては、これ
らの合金のなかでも、１０００系、５０００系、６００
０系が好ましい。Further, those alloys that have undergone various heat treatments such as solution treatment and aging treatment are also used. Further, a clad material obtained by cladding the surface of these aluminum alloys can also be used. In the present invention, among these alloys, 1000 series, 5000 series, 600 series
0 series is preferable.
【００１０】このような素材に対して前処理が施され
る。この前処理としては特に限定されず、要は素材の表
面に付着した油脂分を除去し、素材表面の不均質な酸化
物皮膜が除去できるものであればよい。例えば、弱アル
カリ性の脱脂液による脱脂処理を施したのち、水酸化ナ
トリウム水溶液でアルカリエッチングをしたのち、硝酸
水溶液中でデスマット処理を行う方法や、脱脂処理後に
酸洗浄を行う方法などが適宜選択して用いられる。Pretreatment is applied to such a material. The pretreatment is not particularly limited as long as it can remove the oil and fat adhering to the surface of the material and remove the heterogeneous oxide film on the material surface. For example, after performing degreasing treatment with a weak alkaline degreasing solution, alkali etching with an aqueous sodium hydroxide solution, then performing desmutting treatment in a nitric acid aqueous solution, a method of performing acid cleaning after the degreasing treatment, etc. are appropriately selected. Used.
【００１１】ついで、この前処理が施された素材を電解
質溶液中で電解する陽極酸化処理を施すことにより、素
材の表面に無孔質陽極酸化皮膜を形成する。電解液とし
ては、生成する無孔質陽極酸化皮膜を溶解しにくく、か
つ無孔質の陽極酸化皮膜を生成する電解質である硼酸、
硼酸塩、リン酸塩、アジピン酸塩などの群から選ばれる
１種または２種以上を溶解した皮膜溶解性の低い電解質
水溶液が用いられる。これらの電解質のなかでも硼酸、
硼酸塩、リン酸塩、アジピン酸塩が好ましい。Then, the pretreated material is subjected to anodizing treatment in which the material is electrolyzed in an electrolyte solution to form a nonporous anodized film on the surface of the material. As the electrolytic solution, it is difficult to dissolve the non-porous anodic oxide film to be produced, and boric acid which is an electrolyte to form a non-porous anodic oxide film,
An electrolyte aqueous solution having low film solubility in which one or more selected from the group consisting of borate, phosphate and adipate is dissolved is used. Among these electrolytes, boric acid,
Borate, phosphate and adipate are preferred.
【００１２】電解質水溶液中の電解質濃度は、１〜２０
０ｇ／ｌが好ましい。電解質濃度が１ｇ／ｌより低濃度
では皮膜むらが生じ易く、一方、２００ｇ／ｌを超える
と溶解し難く沈澱を生じることがあるからである。電解
浴の浴温は、５０℃以上、好ましくは５０℃〜９５℃、
より好ましくは５０〜８０℃の範囲である。浴温が５０
℃未満では、電解質の溶解性が低く、液抵抗による電圧
ロスが大きくなるからである。一方、浴温が９５℃を超
えると、沸騰を伴うことや加熱にコストを要するからで
ある。また、浴温が５０〜８０℃であると、質陽極酸化
皮膜の含水量を少なくするのに効果的である。The electrolyte concentration in the aqueous electrolyte solution is 1 to 20.
0 g / l is preferred. This is because if the electrolyte concentration is lower than 1 g / l, uneven coating is likely to occur, while if it exceeds 200 g / l, it may be difficult to dissolve and precipitate may occur. The bath temperature of the electrolytic bath is 50 ° C. or higher, preferably 50 ° C. to 95 ° C.,
More preferably, it is in the range of 50 to 80 ° C. Bath temperature is 50
This is because if the temperature is lower than 0 ° C, the solubility of the electrolyte is low and the voltage loss due to the liquid resistance is large. On the other hand, if the bath temperature exceeds 95 ° C., it will be accompanied by boiling and heating will be costly. Further, when the bath temperature is 50 to 80 ° C., it is effective to reduce the water content of the anodic oxide film.
【００１３】この電解浴中で、アルミニウムまたはアル
ミニウム合金素材は、連続あるいは断続であっても陽極
となるように電源に接続されて電解される。陰極には不
溶性の導電材料が用いられる。電解電流は、直流電流が
用いられ直流電解では直流密度０．２〜５Ａ／ｄｍ2程
度である。電流密度が０．２Ａ／ｄｍ2 未満では皮膜形
成に長時間を要してしまう。一方、５Ａ／ｄｍ2 を超え
ると、皮膜やけ等の表面欠損が生じ易くなるからであ
る。電解時間は、数秒〜３０分程度で目的とする皮膜厚
さと電解条件により選択して電解が行われる。In this electrolytic bath, the aluminum or aluminum alloy material is electrolyzed by being connected to a power source so as to be an anode even if it is continuous or intermittent. An insoluble conductive material is used for the cathode. A direct current is used as an electrolysis current, and a direct current electrolysis has a direct current density of about 0.2 to 5 A / dm 2 . If the current density is less than 0.2 A / dm 2, it takes a long time to form the film. On the other hand, if it exceeds 5 A / dm 2 , surface defects such as film and scaly are likely to occur. The electrolysis time is about several seconds to 30 minutes, and the electrolysis is performed by selecting the desired film thickness and electrolysis conditions.
【００１４】印加電圧は、直流電流では、電圧１Ｖに対
して形成される酸化皮膜厚さが約１４Åとなる関係があ
ることから約２０〜５００Ｖ、好ましくは約３０〜５０
０Ｖの範囲とされる。電源装置などの点からは５０Ｖ以
下とすることが好ましく、このような低電圧での電解で
も優れた真空特性及び耐食性が得られる。このような陽
極酸化処理によって素材の表面に厚さの均一な無孔質陽
極酸化皮膜が形成される。無孔質陽極酸化皮膜の膜厚
は、３００〜７０００Å、好ましくは５００〜７０００
Å程度である。膜厚が３００Å未満であると、厚さが薄
すぎて十分な耐食性が得られ難いからである。一方、膜
厚の上限としては、７０００Åまで可能である。The applied voltage is about 20 to 500 V, and preferably about 30 to 50 V, since there is a relation that the thickness of the oxide film formed is about 14 Å with a voltage of 1 V under direct current.
The range is 0V. From the viewpoint of a power supply device or the like, it is preferably 50 V or less, and excellent vacuum characteristics and corrosion resistance can be obtained even in electrolysis at such a low voltage. By such anodizing treatment, a non-porous anodized film having a uniform thickness is formed on the surface of the material. The thickness of the non-porous anodic oxide film is 300 to 7,000Å, preferably 500 to 7,000.
It is about Å. If the film thickness is less than 300Å, the thickness is too thin to obtain sufficient corrosion resistance. On the other hand, the upper limit of the film thickness can be up to 7,000 Å.
【００１５】このようにして得られた陽極酸化皮膜は無
孔質であり、その空孔率は最大でも５％程度以下が好ま
しい。空孔率が５％を超えると、陽極酸化皮膜の表面積
が大きくなり、吸着される水分やガス等も多くなってし
まい、含水量が増えたのと同様の悪影響を及ぼす恐れが
ある。また、空孔率が５％を超えると無孔質皮膜とは言
えなくなるからである。空孔率は、前述の電解条件によ
って決定される。The anodic oxide film thus obtained is non-porous, and its porosity is preferably about 5% or less at the maximum. If the porosity exceeds 5%, the surface area of the anodic oxide film increases, and the amount of adsorbed water, gas, etc. increases, which may have the same adverse effect as increasing the water content. Also, if the porosity exceeds 5%, it cannot be said to be a non-porous coating. The porosity is determined by the above-mentioned electrolysis conditions.
【００１６】後述するベーキング処理が施される前の無
孔質陽極酸化皮膜の含水量は、３〜１０重量％程度であ
る。後述するベーキング処理が施される前の無孔質陽極
酸化皮膜中のアルミニウムに対するアニオンの含有量が
重量比で０．０５〜０．１０程度である。The water content of the non-porous anodic oxide film before the baking process to be described later is performed is about 3 to 10 by weight%. The content of anions to aluminum in the non-porous anodic oxide coating before being subjected to the baking treatment described later is about 0.05 to 0.10.
【００１７】前述の陽極酸化処理は、コイル状などの未
加工の状態のアルミニウムまたはアルミニウム合金に対
して行うこともできるが、プレス加工などの加工を施し
たものに対して行うことが好ましい。The above-mentioned anodizing treatment can be performed on unprocessed aluminum or aluminum alloy such as a coil, but it is preferably performed on a product that has been processed such as pressing.
【００１８】ついで、電解が終了後、無孔質陽極酸化皮
膜の表面に１５０〜３５０℃のベーキング処理を施すこ
とにより、無孔質陽極酸化皮膜の含水量を３重量％以
下、好ましくは０．１〜２重量％、アルミニウムに対す
るアニオン含有量を重量比で０．０５以下、好ましくは
０．０１〜０．０３にする。無孔質陽極酸化皮膜中のア
ニオン種としては、硼酸、硼酸塩、リン酸塩、アジピン
酸塩のアニオンの１種または２種以上が含まれる。無孔
質陽極酸化皮膜中のアニオン種として、硼素、硼酸塩の
アニオンが含まれている場合のアルミニウム重量に対す
る硼素重量の割合は重量比で０．０５以下、好ましくは
０．０１〜０．０４であり、あるいはリン酸塩のアニオ
ンが含まれている場合のアルミニウム重量に対するリン
重量の割合は重量比で０．０５以下、好ましくは０．０
１〜０．０４である。Then, after the electrolysis is completed, the surface of the non-porous anodic oxide film is subjected to a baking treatment at 150 to 350 ° C., so that the water content of the non-porous anodic oxide film is 3% by weight or less, preferably 0. 1 to 2% by weight, and the anion content relative to aluminum is 0.05 or less, preferably 0.01 to 0.03 by weight ratio. The anionic species in the non-porous anodic oxide film include one or more anions of boric acid, borate, phosphate and adipate. When the anion species in the non-porous anodic oxide coating contains boron and borate anions, the weight ratio of boron to aluminum is 0.05 or less, preferably 0.01 to 0.04. Or the ratio of the weight of phosphorus to the weight of aluminum when the anion of the phosphate is contained is 0.05 or less, preferably 0.0 or less by weight ratio.
It is 1 to 0.04.
【００１９】ベーキング処理温度が１５０℃未満である
と、無孔質陽極酸化皮膜中の水分や、成膜成分であるア
ニオンや、表面に吸着した水分やガス等を除去する効果
が低く、含水量が３重量％以下、アニオン含有量が０．
０５以下の無孔質陽極酸化皮膜が得られにくく、真空機
器等に用いた場合に、無孔質陽極酸化皮膜からのガスの
放出量を低減する効果が低い。一方、ベーキング処理温
度が３５０℃を超えると、無孔質陽極酸化皮膜にクラッ
クが入り易くなり、また、アルミニウムまたはアルミニ
ウム合金素材がなまって強度等が大きく低下してしまう
場合があるからである。If the baking temperature is lower than 150 ° C., the effect of removing water in the non-porous anodic oxide film, anions as film forming components, water and gas adsorbed on the surface is low, and the water content is low. Is 3% by weight or less, and the anion content is 0.
It is difficult to obtain a non-porous anodic oxide film of 05 or less, and when used in a vacuum device or the like, the effect of reducing the amount of gas released from the non-porous anodic oxide film is low. On the other hand, if the baking temperature exceeds 350 ° C., the non-porous anodic oxide film may be easily cracked, and the aluminum or aluminum alloy material may become dull, resulting in a large decrease in strength and the like.
【００２０】また、本発明のベーキング処理は、常圧下
あるいは真空環境下のいずれでも行うことができるが、
真空環境下で行う方がベーキング処理時間の短縮の点で
好ましい。その理由は、ベーキング処理を真空環境下で
行うと、無孔質陽極酸化皮膜中の水分やアニオン等の除
去効率が良いからである。本発明のベーキング処理は、
常圧下で行う場合、１時間以上、好ましくは１〜３時間
であり、真空環境下で行う場合、０．３時間以上、好ま
しくは０．５〜１．０時間である。The baking treatment of the present invention can be carried out under either normal pressure or vacuum environment.
Performing in a vacuum environment is preferable from the viewpoint of shortening the baking processing time. The reason is that when the baking treatment is performed in a vacuum environment, the removal efficiency of water, anions and the like in the non-porous anodic oxide film is good. The baking process of the present invention is
When it is carried out under normal pressure, it is 1 hour or longer, preferably 1 to 3 hours, and when it is carried out in a vacuum environment, it is 0.3 hours or longer, preferably 0.5 to 1.0 hour.
【００２１】ベーキング処理後の無孔質陽極酸化皮膜の
含水量が３重量％を超えると、皮膜から揮散する水分
（皮膜から放出されるガス）の量が増加し、真空機器内
を高真空にするという目的を十分に達成できないため真
空特性が悪く、また、塩素ガスやプラズマ等と反応し、
エッチング不良が生じ、半導体基板の特性に悪影響を与
えるという問題がある。When the water content of the non-porous anodic oxide coating after baking exceeds 3% by weight, the amount of water vaporized from the coating (gas released from the coating) increases, and the inside of the vacuum equipment is evacuated to a high vacuum. The vacuum characteristics are poor because it is not possible to sufficiently achieve the purpose of, and it also reacts with chlorine gas, plasma, etc.
There is a problem that etching defects occur and the characteristics of the semiconductor substrate are adversely affected.
【００２２】ベーキング処理後の無孔質陽極酸化皮膜の
アニオン含有量が０．０５を超えると、皮膜から揮散す
るアニオン（皮膜から放出されるガス）の量が増加し、
真空機器内を高真空にするという目的を十分に達成でき
ないため真空特性が悪く、また、皮膜から揮散したアニ
オンが不純物として真空機器の系内に放出され、塩素ガ
ス等の反応性ガスやプラズマ等と反応し、エッチング不
良が生じたり、半導体基板を汚染し、半導体基板の特性
に悪影響を及ぼすという問題がある。一方、０．０１未
満の無孔質陽極酸化皮膜は、電解浴では製造し難いから
である。以上のようにすると、目的とする表面処理アル
ミニウム材が得られる。If the anion content of the non-porous anodic oxide coating after baking exceeds 0.05, the amount of anions volatilized from the coating (gas released from the coating) increases,
The vacuum characteristics are poor because the purpose of making the vacuum equipment a high vacuum cannot be achieved sufficiently, and the anions volatilized from the film are released into the vacuum equipment system as impurities, and reactive gases such as chlorine gas and plasma, etc. However, there is a problem in that the semiconductor substrate reacts with the semiconductor substrate to cause etching defects or contaminate the semiconductor substrate, which adversely affects the characteristics of the semiconductor substrate. On the other hand, a non-porous anodic oxide coating with a content of less than 0.01 is difficult to produce in an electrolytic bath. By doing the above, the target surface-treated aluminum material can be obtained.
【００２３】本発明の表面処理アルミニウム材にあって
は、アルミニウムまたはアルミニウム合金の表面に、ベ
ーキング処理が施された無孔質陽極酸化皮膜が形成さ
れ、該無孔質陽極酸化皮膜は厚さが３００〜７０００
Å、含水量が３％以下、アルミニウムに対するアニオン
の含有量が重量比で０．０５以下のものであるので、多
孔質陽極酸化皮膜が形成された従来のアルミニウム材と
比べて、皮膜の含水量ならびにアニオン含有量が少な
い。従って、本発明の表面処理アルミニウム材を、半導
体製造装置あるいは薄膜形成装置等の真空機器やその部
品の表面材として用い、真空環境下においても、前記水
分やアニオンに起因する皮膜からのガスの放出量が少く
なるので、真空特性が優れ、また、前記皮膜から放出さ
れたガスが、塩素ガス等の反応性ガスやプラズマ等と反
応することも殆どなくなるので、エッチング不良が生じ
たり、薄膜が汚染されることが改善され、特性の安定し
た薄膜が得られ易いという利点がある。また、本発明で
形成される陽極酸化皮膜は無孔質のものであるので、耐
食性が優れ、また、表面に水分やガスが吸着されにくい
ので、真空環境下での皮膜からのガスの放出量が少くな
るので、真空特性が優れるうえ、特性の安定した薄膜が
得られる易い。また、無孔質陽極酸化皮膜の空孔率を５
％以下したものにあっては、特に、表面に吸着される水
分やガスを低減する効果ならびに耐食性が格段に優れ
る。In the surface-treated aluminum material of the present invention, a non-porous anodized film which has been subjected to a baking treatment is formed on the surface of aluminum or an aluminum alloy, and the non-porous anodized film has a thickness of 300-7000
Å The water content is 3% or less, and the anion content relative to aluminum is 0.05 or less in weight ratio, so the water content of the film is more than that of the conventional aluminum material on which a porous anodized film is formed. In addition, the anion content is low. Therefore, the surface-treated aluminum material of the present invention is used as a surface material of a vacuum device such as a semiconductor manufacturing apparatus or a thin film forming apparatus or a part thereof, and the gas is released from the film due to the moisture or anion even in a vacuum environment. Since the amount is small, the vacuum characteristics are excellent, and the gas released from the film hardly reacts with a reactive gas such as chlorine gas or plasma, so that etching defects occur or the thin film is contaminated. There is an advantage that a thin film having stable characteristics is easily obtained. Further, since the anodic oxide film formed by the present invention is a non-porous one, it has excellent corrosion resistance, and since moisture and gas are difficult to be adsorbed on the surface, the amount of gas released from the film in a vacuum environment Is less, so that the vacuum characteristics are excellent and it is easy to obtain a thin film with stable characteristics. In addition, the porosity of the non-porous anodic oxide film is 5
%, The effect of reducing moisture and gas adsorbed on the surface and the corrosion resistance are particularly excellent.
【００２４】[0024]
【実施例】以下、本発明を、実施例および比較例によ
り、具体的に説明するが、本発明はこれらの実施例のみ
に限定されるものではない。
（実施例１）アルミニウム合金としてＪＩＳ５０５２合
金を用い、弱エッチング性の脱脂剤で脱脂処理した後、
５０ｇ／ｌのアジピン酸アンモニウムと２ｇ／ｌのリン
酸２水素アンモニウムを溶解した電解質水溶液で、２０
Ｖ、電流密度１Ａ／ｄｍ2、７０℃、３０分の電解を施
し、アルミニウム合金の表面に無孔質陽極酸化皮膜を形
成した。電解終了後、合金を水洗し、１５０℃、１時間
のベーキング処理を施し、表面処理アルミニウム材を得
た。
（実施例２）実施例１と同様にしてアルミニウム合金を
脱脂処理した後、５０ｇ／ｌの硼酸と２ｇ／ｌのリン酸
２水素アンモニウムを溶解した電解質水溶液で、１０５
Ｖ、電流密度１Ａ／ｄｍ2、７０℃、３０分の電解を施
し、アルミニウム合金の表面に無孔質陽極酸化皮膜を形
成した。電解終了後、合金を水洗し、２００℃、１時間
のベーキング処理を施し、表面処理アルミニウム材を得
た。EXAMPLES The present invention will be specifically described below with reference to Examples and Comparative Examples, but the present invention is not limited to these Examples. (Example 1) After using JIS5052 alloy as an aluminum alloy and degreasing with a weak etching degreasing agent,
20 g of an aqueous electrolyte solution in which 50 g / l ammonium adipate and 2 g / l ammonium dihydrogen phosphate were dissolved
V, current density 1 A / dm 2 , 70 ° C., electrolysis was performed for 30 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy. After completion of electrolysis, the alloy was washed with water and baked at 150 ° C. for 1 hour to obtain a surface-treated aluminum material. Example 2 After degreasing an aluminum alloy in the same manner as in Example 1, 105 g / l of boric acid and 2 g / l of ammonium dihydrogen phosphate were dissolved in an electrolyte aqueous solution to obtain 105
V, current density 1 A / dm 2 , 70 ° C., electrolysis was performed for 30 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy. After completion of electrolysis, the alloy was washed with water and baked at 200 ° C. for 1 hour to obtain a surface-treated aluminum material.
【００２５】（実施例３）実施例１と同様にしてアルミ
ニウム合金を脱脂処理した後、１０ｇ／ｌの硼酸と５０
ｇ／ｌのアジピン酸アンモニウムを溶解した電解質水溶
液で、２００Ｖ、電流密度１Ａ／ｄｍ2、７０℃、３０
分の電解を施し、アルミニウム合金の表面に無孔質陽極
酸化皮膜を形成した。電解終了後、合金を水洗し、２０
０℃、１時間のベーキング処理を施し、表面処理アルミ
ニウム材を得た。
（実施例４）実施例１と同様にしてアルミニウム合金を
脱脂処理した後、５０ｇ／ｌの硼酸と２ｇ／ｌの硼酸ア
ンモニウムを溶解した電解質水溶液で、５００Ｖ、電流
密度１Ａ／ｄｍ2、７０℃、３０分の電解を施し、アル
ミニウム合金の表面に無孔質陽極酸化皮膜を形成した。
電解終了後、合金を水洗し、３５０℃、１時間のベーキ
ング処理を施し、表面処理アルミニウム材を得た。Example 3 An aluminum alloy was degreased in the same manner as in Example 1, and then 10 g / l of boric acid and 50 were added.
An electrolyte aqueous solution in which g / l ammonium adipate was dissolved was used, 200 V, current density 1 A / dm 2 , 70 ° C., 30
Electrolysis was performed for a minute to form a non-porous anodic oxide film on the surface of the aluminum alloy. After electrolysis, wash the alloy with water and
A baking treatment was performed at 0 ° C. for 1 hour to obtain a surface-treated aluminum material. Example 4 After degreasing an aluminum alloy in the same manner as in Example 1, 500 V, current density 1 A / dm 2 , 70 ° C. with an electrolyte aqueous solution in which 50 g / l boric acid and 2 g / l ammonium borate were dissolved. Electrolysis was performed for 30 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy.
After completion of electrolysis, the alloy was washed with water and baked at 350 ° C. for 1 hour to obtain a surface-treated aluminum material.
【００２６】（比較例１）実施例１と同様にしてアルミ
ニウム合金を脱脂処理した後、５０ｇ／ｌのアジピン酸
アンモニウムと２ｇ／ｌのリン酸２水素アンモニウムを
溶解した電解質水溶液で、２０Ｖ、電流密度１Ａ／ｄｍ
2、７０℃、３０分の電解を施し、アルミニウム合金の
表面に無孔質陽極酸化皮膜を形成し、表面処理アルミニ
ウム材を得た。
（比較例２）実施例１と同様にしてアルミニウム合金を
脱脂処理した後、１０ｇ／ｌの硼酸と５０ｇ／ｌのアジ
ピン酸アンモニウムを溶解した電解質水溶液で、２００
Ｖ、電流密度１Ａ／ｄｍ2、７０℃、３０分の電解を施
し、アルミニウム合金の表面に無孔質陽極酸化皮膜を形
成し、表面処理アルミニウム材を得た。Comparative Example 1 After degreasing an aluminum alloy in the same manner as in Example 1, 20 V at a current of 20 V was applied with an electrolyte aqueous solution in which 50 g / l ammonium adipate and 2 g / l ammonium dihydrogen phosphate were dissolved. Density 1A / dm
2 , electrolysis was performed at 70 ° C. for 30 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy to obtain a surface-treated aluminum material. (Comparative Example 2) After degreasing an aluminum alloy in the same manner as in Example 1, 200 g of an electrolyte aqueous solution in which 10 g / l of boric acid and 50 g / l of ammonium adipate were dissolved was used.
V, current density 1 A / dm 2 , 70 ° C., electrolysis was performed for 30 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy to obtain a surface-treated aluminum material.
【００２７】（比較例３）実施例１と同様にしてアルミ
ニウム合金を脱脂処理した後、５０ｇ／ｌの硼酸と２ｇ
／ｌの硼酸アンモニウムを溶解した電解質水溶液で、５
００Ｖ、電流密度１Ａ／ｄｍ2、７０℃、３０分の電解
を施し、アルミニウム合金の表面に無孔質陽極酸化皮膜
を形成し、表面処理アルミニウム材を得た。
（比較例４）実施例１と同様にしてアルミニウム合金を
脱脂処理した後、５０ｇ／ｌの硼酸と２ｇ／ｌの硼酸ア
ンモニウムを溶解した電解質水溶液で、２０Ｖ、電流密
度１Ａ／ｄｍ2、９８℃、２０分の電解を施し、アルミ
ニウム合金の表面に無孔質陽極酸化皮膜を形成し、表面
処理アルミニウム材を得た。Comparative Example 3 After degreasing an aluminum alloy in the same manner as in Example 1, 50 g / l boric acid and 2 g were added.
1 / l ammonium borate in an aqueous electrolyte solution
Electrolysis was carried out at 00 V, current density 1 A / dm 2 , 70 ° C. for 30 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy to obtain a surface-treated aluminum material. (Comparative Example 4) After degreasing an aluminum alloy in the same manner as in Example 1, 20 V, current density 1 A / dm 2 , 98 ° C. with an electrolyte aqueous solution in which 50 g / l boric acid and 2 g / l ammonium borate were dissolved. After 20 minutes of electrolysis, a non-porous anodic oxide film was formed on the surface of the aluminum alloy to obtain a surface-treated aluminum material.
【００２８】（比較例５）実施例１と同様にしてアルミ
ニウム合金を脱脂処理した後、５０ｇ／ｌの硼酸と２ｇ
／ｌの硼酸アンモニウムを溶解した電解質水溶液で、５
００Ｖ、電流密度１Ａ／ｄｍ2、９８℃、２０分の電解
を施し、アルミニウム合金の表面に無孔質陽極酸化皮膜
を形成し、表面処理アルミニウム材を得た。
（比較例６）実施例１と同様にしてアルミニウム合金を
脱脂処理した後、５０ｇ／ｌの硼酸と２ｇ／ｌの硼酸ア
ンモニウムを溶解した電解質水溶液で、５００Ｖ、電流
密度５Ａ／ｄｍ2、９８℃、２０分の電解を施し、アル
ミニウム合金の表面に無孔質陽極酸化皮膜を形成し、表
面処理アルミニウム材を得た。(Comparative Example 5) The aluminum alloy was degreased in the same manner as in Example 1, and then 50 g / l boric acid and 2 g were added.
1 / l ammonium borate in an aqueous electrolyte solution
Electrolysis was carried out at 00 V, current density 1 A / dm 2 , 98 ° C. for 20 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy to obtain a surface-treated aluminum material. Comparative Example 6 After degreasing an aluminum alloy in the same manner as in Example 1, 500 V, current density 5 A / dm 2 , 98 ° C. with an electrolyte aqueous solution in which 50 g / l boric acid and 2 g / l ammonium borate were dissolved. After 20 minutes of electrolysis, a non-porous anodic oxide film was formed on the surface of the aluminum alloy to obtain a surface-treated aluminum material.
【００２９】（比較例７）実施例１と同様にしてアルミ
ニウム合金を脱脂処理した後、５０ｇ／ｌの硼酸と２ｇ
／ｌの硼酸アンモニウムを溶解した電解質水溶液で、１
５Ｖ、電流密度１Ａ／ｄｍ2、９８℃、２０分の電解を
施し、アルミニウム合金の表面に無孔質陽極酸化皮膜を
形成した。電解終了後、合金を水洗し、１５０℃、１時
間のベーキング処理を施し、表面処理アルミニウム材を
得た。
（比較例８）実施例１と同様にしてアルミニウム合金を
脱脂処理した後、５０ｇ／ｌの硼酸と２ｇ／ｌのリン酸
２水素アンモニウムを溶解した電解質水溶液で、１０７
Ｖ、電流密度５Ａ／ｄｍ2、９８℃、２０分の電解を施
し、アルミニウム合金の表面に無孔質陽極酸化皮膜を形
成した。電解終了後、合金を水洗し、１５０℃、１時間
のベーキング処理を施し、表面処理アルミニウム材を得
た。Comparative Example 7 After degreasing an aluminum alloy in the same manner as in Example 1, 50 g / l boric acid and 2 g were added.
1 / l of an aqueous solution of an ammonium borate solution
Electrolysis was carried out at 5 V, current density 1 A / dm 2 , 98 ° C. for 20 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy. After completion of electrolysis, the alloy was washed with water and baked at 150 ° C. for 1 hour to obtain a surface-treated aluminum material. (Comparative Example 8) After degreasing an aluminum alloy in the same manner as in Example 1, 107 g of an aqueous electrolyte solution was prepared by dissolving 50 g / l boric acid and 2 g / l ammonium dihydrogen phosphate.
V, current density 5 A / dm 2 , 98 ° C., electrolysis was performed for 20 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy. After completion of electrolysis, the alloy was washed with water and baked at 150 ° C. for 1 hour to obtain a surface-treated aluminum material.
【００３０】（比較例９）実施例１と同様にしてアルミ
ニウム合金を脱脂処理した後、２０ｇ／ｌのフタル酸水
素アンモニウムを溶解した電解質水溶液で、１０７Ｖ、
電流密度５Ａ／ｄｍ2、９８℃、２０分の電解を施し、
アルミニウム合金の表面に無孔質陽極酸化皮膜を形成し
た。電解終了後、合金を水洗し、１５０℃、１時間のベ
ーキング処理を施し、表面処理アルミニウム材を得た。
（比較例１０）実施例１と同様にしてアルミニウム合金
を脱脂処理した後、１０ｇ／ｌのクエン酸アンモニウム
を溶解した電解質水溶液で、１０７Ｖ、電流密度５Ａ／
ｄｍ2、９８℃、２０分の電解を施し、アルミニウム合
金の表面に無孔質陽極酸化皮膜を形成した。電解終了
後、合金を水洗し、１５０℃、１時間のベーキング処理
を施し、表面処理アルミニウム材を得た。(Comparative Example 9) After degreasing an aluminum alloy in the same manner as in Example 1, 107 V was applied with an electrolyte aqueous solution in which 20 g / l ammonium hydrogen phthalate was dissolved.
Electrolyzed at a current density of 5 A / dm 2 , 98 ° C. for 20 minutes,
A non-porous anodic oxide film was formed on the surface of the aluminum alloy. After completion of electrolysis, the alloy was washed with water and baked at 150 ° C. for 1 hour to obtain a surface-treated aluminum material. (Comparative Example 10) After degreasing an aluminum alloy in the same manner as in Example 1, 107 V at a current density of 5 A / with an electrolyte aqueous solution in which 10 g / l of ammonium citrate was dissolved.
Electrolysis was carried out at dm 2 , 98 ° C. for 20 minutes to form a non-porous anodic oxide film on the surface of the aluminum alloy. After completion of electrolysis, the alloy was washed with water and baked at 150 ° C. for 1 hour to obtain a surface-treated aluminum material.
【００３１】（比較例１１）実施例１と同様にしてアル
ミニウム合金を脱脂処理した後、５０℃、１０％の水酸
化ナトリウム水溶液で、２分間エッチング処理し水洗し
た。ついで、室温、１０％の硝酸に１分間浸漬しデスマ
ットした後、１５％硫酸で、１．３Ａ／ｄｍ2で、２０
℃、２０分の電解を施し、アルミニウム合金の表面に多
孔質陽極酸化皮膜を形成した。さらに、この多孔質陽極
酸化皮膜が形成されたアルミニウム合金を１００℃の純
水に３０分間浸漬し封孔処理し乾燥し、表面処理アルミ
ニウム材を得た。
（比較例１２）実施例１と同様にしてアルミニウム合金
を脱脂処理した後、５０℃、１０％の水酸化ナトリウム
水溶液で、２分間エッチング処理し水洗した。ついで、
室温、１０％の硝酸に１分間浸漬しデスマットした後、
１５％硫酸で、１．３Ａ／ｄｍ2で、２０℃、２０分の
電解を施し、アルミニウム合金の表面に多孔質陽極酸化
皮膜を形成した。さらに、この多孔質陽極酸化皮膜が形
成されたアルミニウム合金を１００℃の純水に３０分間
浸漬し封孔処理し乾燥した。この後、さらに、この合金
に、１５０℃、１時間のベーキング処理を施し、表面処
理アルミニウム材を得た。(Comparative Example 11) The aluminum alloy was degreased in the same manner as in Example 1, then, etched at 50 ° C for 10 minutes in a 10% aqueous sodium hydroxide solution and washed with water. Then, after immersing in 10% nitric acid at room temperature for 1 minute to desmut, it was added with 15% sulfuric acid at 1.3 A / dm 2 for 20 minutes.
Electrolysis was performed at 20 ° C. for 20 minutes to form a porous anodic oxide film on the surface of the aluminum alloy. Further, the aluminum alloy on which the porous anodic oxide film was formed was immersed in pure water at 100 ° C. for 30 minutes, sealed and dried to obtain a surface-treated aluminum material. (Comparative Example 12) After degreasing an aluminum alloy in the same manner as in Example 1, the aluminum alloy was etched with a 10% aqueous sodium hydroxide solution at 50 ° C for 2 minutes and washed with water. Then,
After immersing in room temperature, 10% nitric acid for 1 minute and desmutting,
Electrolysis was performed with 15% sulfuric acid at 1.3 A / dm 2 at 20 ° C. for 20 minutes to form a porous anodic oxide film on the surface of the aluminum alloy. Further, the aluminum alloy having the porous anodic oxide film formed thereon was immersed in pure water at 100 ° C. for 30 minutes for sealing treatment and dried. Then, this alloy was further baked at 150 ° C. for 1 hour to obtain a surface-treated aluminum material.
【００３２】（実験例）実施例１〜４、比較例１〜１２
得られた表面処理アルミニウム材の陽極酸化皮膜の含水
量を熱重量分析によって測定し、アニオン含有量をＸＰ
Ｓによって測定した。また、得られた表面処理アルミニ
ウム材を１０-6トール以下の真空に吸引した雰囲気下
で、３００℃まで加熱したときの放出されたガスの量を
測定し、ガス放出性（アウトガス性）を評価した。その
結果を下記表１に示す。評価基準は、ガスが殆ど放出さ
れないものを秀（◎）、やや放出されたものを良
（○）、多量に放出されたものを（×）、極めて多量に
放出されたものを（××）とした。さらに、得られた表
面処理アルミニウム材に４０ｅＶのＣＦ4プラズマを３
０分照射し、膜厚の変化を測定することにより耐食性
（プラズマ耐久性）評価した。その結果を下記表１に示
す。評価基準は、膜厚減少が１０％以内のものを
（○）、膜厚減少が１０％以上のものを（×）とした。(Experimental Examples) Examples 1 to 4 and Comparative Examples 1 to 12
The water content of the anodized film of the obtained surface-treated aluminum material was measured by thermogravimetric analysis, and the anion content was measured by XP.
Measured by S. Also, the amount of gas released when the surface-treated aluminum material obtained was heated to 300 ° C. in an atmosphere in which it was sucked in a vacuum of 10 −6 Torr or less, and the gas releasing property (outgassing property) was evaluated. did. The results are shown in Table 1 below. The criteria for evaluation are excellent (∘) when gas is hardly released, good (○) when slightly released, × (x) when released in large amounts, and (xx) when released in extremely large amounts. And Furthermore, 40 eV of CF 4 plasma was applied to the obtained surface-treated aluminum material for 3 times.
Corrosion resistance (plasma durability) was evaluated by irradiating for 0 minutes and measuring the change in film thickness. The results are shown in Table 1 below. As an evaluation criterion, a film thickness reduction of 10% or less was (O), and a film thickness reduction of 10% or more was (X).
【００３３】[0033]
【表１】 [Table 1]
【００３４】表１中のＢ／Ａｌ比、Ｐ／Ａｌ比は重量比
である。B / Al ratio and P / Al ratio in Table 1 are weight ratios.
【００３５】[0035]
【発明の効果】以上説明したように本発明の表面処理ア
ルミニウム材にあっては、前述の構成としたことによ
り、真空環境下でのガス放出量が少なく、真空特性及び
耐食性が優れる。従って、本発明の表面処理アルミニウ
ム材を、半導体製造装置あるいは薄膜形成装置等の真空
機器やその部品の表面材として用いると、エッチング不
良が生じたり、薄膜が汚染されることが殆どなくなり、
特性の安定した薄膜が得られ易いという利点がある。As described above, the surface-treated aluminum material of the present invention has the above-mentioned constitution, so that the amount of gas released in a vacuum environment is small and the vacuum characteristics and the corrosion resistance are excellent. Therefore, when the surface-treated aluminum material of the present invention is used as a surface material of a vacuum device such as a semiconductor manufacturing apparatus or a thin film forming apparatus or a component thereof, an etching defect or a thin film is hardly contaminated.
There is an advantage that a thin film having stable characteristics can be easily obtained.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) C25D 11/04 302 C25D 11/16 302 C25D 11/18 313 ─────────────────────────────────────────────────── ─── Continuation of the front page (58) Fields surveyed (Int.Cl. 7 , DB name) C25D 11/04 302 C25D 11/16 302 C25D 11/18 313
Claims (5)
表面に、ベーキング処理が施された無孔質陽極酸化皮膜
が形成され、該無孔質陽極酸化皮膜は厚さが３００〜７
０００Å、含水量が３％以下、アルミニウムに対するア
ニオンの含有量が重量比で０．０５以下であることを特
徴とする表面処理アルミニウム材。1. A non-porous anodic oxide coating that has been subjected to a baking treatment is formed on the surface of aluminum or an aluminum alloy, and the non-porous anodic oxide coating has a thickness of 300 to 7
A surface-treated aluminum material having a water content of 3% or less and an anion content of 0.05 or less relative to aluminum.
中の硼素／アルミニウム重量比またはリン／アルミニウ
ム重量比で０．０５以下であることを特徴とする請求項
１記載の表面処理アルミニウム材。2. The surface-treated aluminum material according to claim 1, wherein the anion content is 0.05 or less in terms of boron / aluminum weight ratio or phosphorus / aluminum weight ratio in the non-porous anodic oxide film. .
であることを特徴とする請求項１又は２記載の表面処理
アルミニウム材。3. The surface-treated aluminum material according to claim 1, wherein the non-porous anodic oxide coating has a porosity of 5% or less.
を、硼酸、硼酸塩、リン酸塩、アジピン酸塩の群から選
ばれる１種または２種以上からなる電解質水溶液により
電解し、アルミニウムまたはアルミニウム合金の表面に
無孔質陽極酸化皮膜を形成する工程と、該無孔質陽極酸
化皮膜の表面に１５０〜３５０℃のベーキング処理を施
して該無孔質陽極酸化皮膜の含水量を３重量％以下、ア
ルミニウムに対するアニオン含有量を重量比で０．０５
以下にする工程を備えることを特徴とする表面処理アル
ミニウム材の製造方法。4. Aluminum or an aluminum alloy is electrolyzed with an aqueous electrolyte solution consisting of one or more selected from the group consisting of boric acid, borate, phosphate and adipate, so that the surface of aluminum or aluminum alloy is free from A step of forming a porous anodic oxide film, and a baking treatment at 150 to 350 ° C. on the surface of the nonporous anodic oxide film so that the water content of the nonporous anodic oxide film is 3% by weight or less, and anion relative to aluminum. Content is 0.05 by weight
A method for manufacturing a surface-treated aluminum material, comprising the following steps.
を特徴とする請求項４記載の表面処理アルミニウム材の
製造方法。5. The method for producing a surface-treated aluminum material according to claim 4, wherein the baking treatment is performed in a vacuum environment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34419195A JP3506827B2 (en) | 1995-12-28 | 1995-12-28 | Surface-treated aluminum material and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34419195A JP3506827B2 (en) | 1995-12-28 | 1995-12-28 | Surface-treated aluminum material and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09184094A JPH09184094A (en) | 1997-07-15 |
| JP3506827B2 true JP3506827B2 (en) | 2004-03-15 |
Family
ID=18367339
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34419195A Expired - Fee Related JP3506827B2 (en) | 1995-12-28 | 1995-12-28 | Surface-treated aluminum material and method for producing the same |
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| Country | Link |
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| JP (1) | JP3506827B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101031674B (en) * | 2005-05-18 | 2010-05-19 | 株式会社爱发科 | Method for anticorrosion-treating aluminum or aluminum alloy |
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| JP2005350775A (en) * | 2000-05-31 | 2005-12-22 | Mitsubishi Alum Co Ltd | Surface-treated aluminum material and production method therefor |
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| JP2006128370A (en) * | 2004-10-28 | 2006-05-18 | Tokyo Electron Ltd | Film forming apparatus and metod, program, and recording medium |
| JP2006173413A (en) * | 2004-12-16 | 2006-06-29 | Ulvac Japan Ltd | Thin film formation device |
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| WO2006134737A1 (en) * | 2005-06-17 | 2006-12-21 | Tohoku University | Metal oxide film, laminate, metal member and process for producing the same |
| JP4842618B2 (en) * | 2005-11-09 | 2011-12-21 | 株式会社アルバック | Surface treatment method of aluminum and aluminum alloy |
| JP4814073B2 (en) * | 2006-12-14 | 2011-11-09 | 株式会社神戸製鋼所 | Aluminum alloy for semiconductor or liquid crystal manufacturing apparatus and method for manufacturing the same |
| JP5162148B2 (en) * | 2007-03-26 | 2013-03-13 | 株式会社アルバック | Composite and production method thereof |
| CN114808075A (en) * | 2022-05-27 | 2022-07-29 | 重庆臻宝实业有限公司 | Method for preparing anode film layer with plasma corrosion resistance and low gas overflow amount |
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1995
- 1995-12-28 JP JP34419195A patent/JP3506827B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101031674B (en) * | 2005-05-18 | 2010-05-19 | 株式会社爱发科 | Method for anticorrosion-treating aluminum or aluminum alloy |
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| Publication number | Publication date |
|---|---|
| JPH09184094A (en) | 1997-07-15 |
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