JPH0525694A - Production of aluminum or aluminum alloy for vacuum equipment - Google Patents
Production of aluminum or aluminum alloy for vacuum equipmentInfo
- Publication number
- JPH0525694A JPH0525694A JP17384391A JP17384391A JPH0525694A JP H0525694 A JPH0525694 A JP H0525694A JP 17384391 A JP17384391 A JP 17384391A JP 17384391 A JP17384391 A JP 17384391A JP H0525694 A JPH0525694 A JP H0525694A
- Authority
- JP
- Japan
- Prior art keywords
- voltage
- aluminum
- constant
- alloy material
- aluminum alloy
- 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.)
- Granted
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、例えばＭＢＥ装置、ド
ライエッチング装置、ＣＶＤ装置、イオンプレーティン
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のような真空
機器における真空チャンバーの表面材として利用される
真空機器用アルミニウム又はアルミニウム合金材の製造
法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vacuum in semiconductor manufacturing equipment such as MBE equipment, dry etching equipment, CVD equipment, ion plating equipment, plasma CVD equipment and sputtering equipment, or vacuum equipment such as thin film forming equipment. The present invention relates to a method for producing an aluminum or aluminum alloy material for vacuum equipment used as a surface material of a chamber.
【０００２】[0002]
【発明の背景】真空機器における真空チャンバーの表面
材としてステンレス鋼製のものが広く用いられて来たも
のの、ステンレス鋼材は重量があること、熱伝導性が悪
いこと、表面からのガス放出度が高いこと等から、アル
ミニウム又はアルミニウム合金（以下、アルミニウム合
金）材を使用することが試みられている。BACKGROUND OF THE INVENTION Although stainless steel materials have been widely used as the surface material of vacuum chambers in vacuum equipment, the stainless steel material is heavy, has poor thermal conductivity, and has a high degree of gas release from the surface. Since it is expensive, it has been attempted to use an aluminum or aluminum alloy (hereinafter, aluminum alloy) material.
【０００３】ところで、アルミニウム合金材は、ＭＢＥ
装置でＧａＡｓなどの半導体膜を形成する場合、あるい
は塩素などのエッチングガスが用いられる場合、腐食す
る問題が有り、この問題点を解決する為に、硫酸電解液
中で陽極酸化処理を施して陽極酸化皮膜を形成しておく
ことが提案されている。しかしながら、この技術は、真
空機器用アルミニウム合金材に加熱脱ガス処理をする場
合に、陽極酸化皮膜にクラックを引き起こし、耐食性が
低下する問題が有り、又、陽極酸化皮膜に吸着している
水分が多いことから、真空室内でのガス放出が多いこと
になり、高真空度達成の目的が充分に発揮できにくい問
題がある。By the way, the aluminum alloy material is MBE.
When a semiconductor film such as GaAs is formed in the apparatus, or when an etching gas such as chlorine is used, there is a problem of corrosion, and in order to solve this problem, anodization is performed in a sulfuric acid electrolyte solution and the anode is It has been proposed to form an oxide film. However, this technique has a problem that when an aluminum alloy material for vacuum equipment is heated and degassed, it causes cracks in the anodic oxide film, reducing corrosion resistance, and that the water content adsorbed on the anodic oxide film is reduced. Since the amount of gas is large, a large amount of gas is released in the vacuum chamber, and there is a problem that it is difficult to sufficiently achieve the purpose of achieving a high degree of vacuum.
【０００４】そこで、このような問題点を解決する為の
手段として、０．０５〜４重量％の銅を含有するアルミ
ニウム合金材を所定形状のものに成形加工し、これをシ
ュウ酸電解液中で陽極酸化処理して表面に陽極酸化皮膜
を形成した後、引き続き同一シュウ酸電解液中で電圧を
前の電圧値から急激に降下させて５〜５０Ｖで定電圧電
解処理することを特徴とする真空用アルミニウム合金材
の製造方法が提案（特開平３−７２０９８号公報）され
ている。Therefore, as a means for solving such a problem, an aluminum alloy material containing 0.05 to 4% by weight of copper is formed into a predetermined shape and then processed in an oxalic acid electrolytic solution. After forming an anodic oxide film on the surface by anodizing with, the voltage is rapidly dropped from the previous voltage value in the same oxalic acid electrolytic solution, and constant voltage electrolysis is performed at 5 to 50V. A method for manufacturing a vacuum aluminum alloy material has been proposed (Japanese Patent Laid-Open No. 3-72098).
【０００５】しかしながら、この提案のものでも充分な
ものではなく、さらなる改善が求められている。However, this proposal is not sufficient and further improvement is required.
【０００６】[0006]
【発明の開示】本発明の目的は、真空環境下でのガス放
出量が極めて少なく、かつ、耐食性に優れた真空機器用
アルミニウム合金材を提供することである。この本発明
の目的は、アルミニウム又はアルミニウム合金材を皮膜
溶解性の低い電解質溶液中で定電流電解処理を行い、そ
の後前記定電流電解処理時の電圧より高い電圧での定電
圧電解処理を行うことを特徴とする真空機器用アルミニ
ウム又はアルミニウム合金材の製造法によって達成され
る。DISCLOSURE OF THE INVENTION An object of the present invention is to provide an aluminum alloy material for vacuum equipment, which has an extremely small amount of gas released in a vacuum environment and is excellent in corrosion resistance. An object of the present invention is to perform constant current electrolysis treatment of an aluminum or aluminum alloy material in an electrolyte solution having a low film solubility, and then perform constant voltage electrolysis treatment at a voltage higher than the voltage during the constant current electrolysis treatment. And a method for manufacturing an aluminum or aluminum alloy material for vacuum equipment.
【０００７】又、アルミニウム又はアルミニウム合金材
を皮膜溶解性の低い電解質溶液中で定電流電解処理を行
い、その後前記定電流電解処理時の電圧より高い電圧で
の定電圧電解処理を所定時間行い、中断後、再度定電圧
電解処理を所定時間行うことを特徴とする真空機器用ア
ルミニウム又はアルミニウム合金材の製造法によって達
成される。Further, aluminum or aluminum alloy material is subjected to constant current electrolysis treatment in an electrolyte solution having low film solubility, and then constant voltage electrolysis treatment at a voltage higher than the voltage during the constant current electrolysis treatment is performed for a predetermined time, After the interruption, the constant voltage electrolysis treatment is again performed for a predetermined time, which is achieved by a method for manufacturing an aluminum or aluminum alloy material for vacuum equipment.
【０００８】又、アルミニウム又はアルミニウム合金材
を皮膜溶解性の低い電解質溶液中で定電流電解処理を行
い、その後前記定電流電解処理時の電圧より高い電圧で
の定電圧電解処理を行い、その後熱処理することを特徴
とする真空機器用アルミニウム又はアルミニウム合金材
の製造法によって達成される。又、アルミニウム又はア
ルミニウム合金材をベーマイト処理した後、皮膜溶解性
の低い電解質溶液中で定電流電解処理を行い、その後前
記定電流電解処理時の電圧より高い電圧での定電圧電解
処理を行うことを特徴とする真空機器用アルミニウム又
はアルミニウム合金材の製造法によって達成される。Further, aluminum or aluminum alloy material is subjected to constant current electrolysis treatment in an electrolyte solution having low film-solubility, followed by constant voltage electrolysis treatment at a voltage higher than the voltage at the constant current electrolysis treatment, and then heat treatment. It is achieved by a method for producing an aluminum or aluminum alloy material for vacuum equipment. Also, after boehmite treatment of aluminum or aluminum alloy material, perform constant current electrolysis treatment in an electrolyte solution having low film solubility, and then perform constant voltage electrolysis treatment at a voltage higher than the voltage during the constant current electrolysis treatment. And a method for manufacturing an aluminum or aluminum alloy material for vacuum equipment.
【０００９】尚、皮膜溶解性の低い電解質溶液として
は、アジピン酸塩、ホウ酸、ホウ酸塩、リン酸塩、フタ
ル酸塩、マレイン酸塩、安息香酸塩、酒石酸塩、クエン
酸塩の群の中から選ばれる少なくとも一つを含むもので
あることが好ましい。耐食性の観点から選ぶと、フタル
酸塩やアジピン酸塩は好ましいものである。電流効率の
観点から選ぶと、ホウ酸やホウ酸塩は好ましいものであ
る。As the electrolyte solution having low film solubility, a group of adipate, boric acid, borate, phosphate, phthalate, maleate, benzoate, tartrate and citrate is available. It is preferable that at least one selected from the above is included. From the viewpoint of corrosion resistance, phthalates and adipates are preferable. From the viewpoint of current efficiency, boric acid and borate are preferable.
【００１０】以下、本発明をさらに詳しく説明する。本
発明において用いられるアルミニウム合金材としては、
格別なる制限はないが、例えば２０１４，２０２４，２
０１７，５０５２，５０８３，６０６１，６０６３，７
Ｎ０１，７０７５等が好ましく用いられる。そして、こ
のようなアルミニウム合金材を、先ず、表面の油成分及
び酸化皮膜を除去する為に界面活性剤あるいは弱エッチ
ング性脱脂剤で脱脂といった前処理を行う。The present invention will be described in more detail below. As the aluminum alloy material used in the present invention,
There is no particular limitation, for example, 2014, 2024, 2
017, 5052, 5083, 6061, 6063, 7
N01, 7075 and the like are preferably used. Then, such an aluminum alloy material is first subjected to a pretreatment such as degreasing with a surfactant or a weak etching degreasing agent in order to remove the oil component and the oxide film on the surface.
【００１１】この後、アルミニウム合金材を皮膜溶解性
の低い電解質溶液中で電解を行い、陽極酸化皮膜を形成
する。この電解操作は二段階で行うことが極めて大事で
ある。すなわち、先ず定電流電解処理を行い、その後定
電流電解処理時の電圧より高い電圧での定電圧電解処理
を行う。この定電流電解処理時の条件は、電解質濃度が
好ましくは１．０〜２００ｇ／ｌであることが、電解液
の温度が好ましくは１０〜１００℃、より好ましくは２
０〜５０℃であることが、そして定電流電解の電流密度
が好ましくは０．５〜３Ａ／ｄｍ2 、より好ましくは１
〜２Ａ／ｄｍ2 であることが、そしてこの定電流電解で
電圧が所定の値（１５０〜２０００Ｖ）まで上昇した
後、この電圧に保持して定電圧電解処理を行う。定電圧
電解処理時の条件は、電解質溶液や温度については定電
流電解処理時のままで良く、そして定電圧電解の電圧が
好ましくは１５０〜２０００Ｖ、より好ましくは５００
〜１５００Ｖであることが、時間が好ましくは５〜３０
分、より好ましくは１０〜２０分である。例えば、電解
質濃度が１．０ｇ／ｌ未満の薄すぎる場合には、形成し
た皮膜にミクロ的な欠陥が生じ、耐食性や絶縁性が劣る
傾向が有り、逆に、２００ｇ／ｌを越えて濃すぎる場合
には、皮膜の絶縁破壊により５００Ｖを越える電圧での
電解処理が困難になる傾向が有り、電解質濃度は１．０
〜２００ｇ／ｌであることが好ましい。電解液の温度が
１０℃未満の低すぎる場合には、皮膜の絶縁性が低下す
る傾向が有り、逆に、１００℃を越えて高すぎる場合に
は、皮膜が多孔質化し、ガス放出量が増加する傾向が有
り、又、圧力容器も必要になることから、電解温度は１
０〜１００℃であることが好ましい。定電流電解の電流
密度が０．５Ａ／ｄｍ2 未満の小さすぎる場合には、電
解時間が長く要り、皮膜が多孔質化し、ガス放出量が増
加する傾向が有り、逆に、３Ａ／ｄｍ2 を越えて大きす
ぎる場合には、皮膜焼けが発生し、耐食性が低下する傾
向が有り、定電流電解の電流密度は０．５〜３Ａ／ｄｍ
2 であることが好ましい。定電圧電解の電圧が１５０Ｖ
未満の小さすぎる場合には、ガス放出性の改善度が乏し
く、逆に、２０００Ｖを越えて大きすぎる場合には、皮
膜が絶縁破壊される傾向が有り、電解電圧は１５０〜２
０００Ｖであることが好ましい。定電圧電解の時間が５
分未満の短すぎる場合には、皮膜に欠陥が多く残り、耐
食性や絶縁性が劣る傾向が有り、逆に、３０分を越えて
長すぎる場合には、耐食性や絶縁性は充分であるもの
の、ガス放出量が増加する傾向が有り、定電圧電解の時
間は５〜３０分であることが好ましい。Thereafter, the aluminum alloy material is electrolyzed in an electrolyte solution having a low film solubility to form an anodic oxide film. It is extremely important to carry out this electrolysis operation in two stages. That is, the constant current electrolysis treatment is first performed, and then the constant voltage electrolysis treatment is performed at a voltage higher than the voltage during the constant current electrolysis treatment. The conditions for the constant current electrolysis treatment are that the electrolyte concentration is preferably 1.0 to 200 g / l, the temperature of the electrolytic solution is preferably 10 to 100 ° C., and more preferably 2
0 to 50 ° C., and the current density of the constant current electrolysis is preferably 0.5 to 3 A / dm 2 , more preferably 1
˜2 A / dm 2 , and after the voltage has risen to a predetermined value (150 to 2000 V) in this constant current electrolysis, the voltage is maintained at this voltage for constant voltage electrolysis. Regarding the conditions during the constant voltage electrolysis treatment, the electrolyte solution and the temperature may be the same as those during the constant current electrolysis treatment, and the voltage of the constant voltage electrolysis is preferably 150 to 2000 V, more preferably 500.
~ 1500V, preferably 5-30 hours
Minutes, more preferably 10 to 20 minutes. For example, when the electrolyte concentration is less than 1.0 g / l, which is too thin, microscopic defects occur in the formed film, and corrosion resistance and insulating properties tend to be poor. Conversely, when the electrolyte concentration exceeds 200 g / l, the concentration is too high. In this case, the electrolytic treatment at a voltage exceeding 500 V tends to be difficult due to the dielectric breakdown of the film, and the electrolyte concentration is 1.0
It is preferably ˜200 g / l. If the temperature of the electrolytic solution is too low, less than 10 ° C, the insulating property of the coating tends to decrease, and conversely, if it exceeds 100 ° C and is too high, the coating becomes porous and the gas release amount is high. Since the temperature tends to increase and a pressure vessel is also required, the electrolysis temperature is 1
It is preferably 0 to 100 ° C. When the current density of constant current electrolysis is too small, less than 0.5 A / dm 2 , electrolysis time is long, the film tends to be porous, and the amount of gas released tends to increase. On the contrary, 3 A / dm 2 If it is too large, the film burns and the corrosion resistance tends to decrease, and the current density of constant current electrolysis is 0.5 to 3 A / dm.
It is preferably 2 . Constant voltage electrolysis voltage is 150V
If the amount is too small, the degree of improvement in the gas releasing property is poor, and conversely, if it exceeds 2000 V and is too large, the coating tends to cause dielectric breakdown, and the electrolytic voltage is 150 to 2
It is preferably 000V. Constant voltage electrolysis time is 5
If the time is too short, the coating will have many defects and the corrosion resistance and insulation will tend to be inferior. On the other hand, if it is longer than 30 minutes, the corrosion resistance and insulation will be sufficient, but The amount of gas released tends to increase, and the time for constant voltage electrolysis is preferably 5 to 30 minutes.
【００１２】そして、上記のような条件の下で電解処理
を行うことにより、真空機器内面に要求される耐食性、
耐摩耗性や絶縁性に優れ、さらにはガス放出量が極めて
少ないバリヤー型陽極酸化皮膜が約０．１〜２．１μｍ
厚形成され、真空機器用アルミニウム合金材として好適
なものが得られる。上記のような電解処理によるバリヤ
ー型陽極酸化皮膜の形成のみでもガス放出量が極めて少
なく、かつ、耐食性に優れたものとなるが、より一層の
耐食性の向上を図るには、定電流電解処理の後に行う高
電圧での定電圧電解処理を何回かに分けて行ったり、す
なわち定電圧電解処理−中断−定電圧電解処理のように
して高電圧での定電圧電解処理を繰り返して行ったり、
高電圧での定電圧電解処理の後に熱処理（１５０〜４０
０℃、０．５〜８時間）したり、アルミニウム合金材を
ベーマイト処理（例えば、１００℃の純水中に浸漬）し
た後、定電流電解処理及び高電圧での定電圧電解処理を
行うといった技術を実施することが好ましい。By performing the electrolytic treatment under the above conditions, the corrosion resistance required for the inner surface of the vacuum equipment,
Barrier type anodic oxide film with excellent wear resistance and insulation, and very little gas emission is about 0.1-2.1 μm
A thick aluminum alloy material suitable for vacuum equipment can be obtained. Even if only the barrier type anodic oxide film is formed by the electrolytic treatment as described above, the amount of released gas is extremely small, and the corrosion resistance is excellent, but in order to further improve the corrosion resistance, the constant current electrolytic treatment The constant-voltage electrolysis treatment at a high voltage to be performed later may be divided into several times, that is, the constant-voltage electrolysis treatment-interruption-a constant-voltage electrolysis treatment at a high voltage such as a constant-voltage electrolysis treatment may be repeatedly performed, or
After constant voltage electrolysis at high voltage, heat treatment (150-40
0 ° C., 0.5 to 8 hours), or boehmite treatment of the aluminum alloy material (for example, immersion in pure water at 100 ° C.), followed by constant current electrolysis and high voltage constant voltage electrolysis. It is preferable to implement the technique.
【００１３】[0013]
〔実施例１〕厚さ０．２ｍｍのアルミニウム合金材（１
２００合金）を界面活性剤あるいは弱エッチング性脱脂
剤で脱脂した後、ホウ酸（１６ｇ／ｌ）水溶液中で、２
０℃、２Ａ／ｄｍ2 の条件で定電流電解処理を２分間行
い、その後引き続き１０００Ｖの条件で定電圧電解処理
を１５分間行った。[Example 1] An aluminum alloy material (1
200 alloy) is degreased with a surfactant or a weakly etching degreasing agent, and then 2 in an aqueous solution of boric acid (16 g / l).
A constant current electrolysis treatment was performed for 2 minutes at 0 ° C. and 2 A / dm 2 , and then a constant voltage electrolysis treatment was performed for 15 minutes under a condition of 1000V.
【００１４】〔実施例２〕厚さ０．２ｍｍのアルミニウ
ム合金材（１２００合金）を界面活性剤あるいは弱エッ
チング性脱脂剤で脱脂した後、リン酸アンモニウム
（１．４ｇ／ｌ）水溶液中で、５０℃、２Ａ／ｄｍ2 の
条件で定電流電解処理を１分間行い、その後引き続き２
３０Ｖの条件で定電圧電解処理を１５分間行った。Example 2 An aluminum alloy material (1200 alloy) having a thickness of 0.2 mm was degreased with a surfactant or a weak etching degreasing agent, and then, in an ammonium phosphate (1.4 g / l) aqueous solution, Constant-current electrolysis treatment was performed for 1 minute at 50 ° C. and 2 A / dm 2 , and then 2
A constant voltage electrolysis treatment was performed for 15 minutes under the condition of 30V.
【００１５】〔実施例３〕厚さ０．２ｍｍのアルミニウ
ム合金材（１２００合金）を界面活性剤あるいは弱エッ
チング性脱脂剤で脱脂した後、フタル酸カリウム（２０
ｇ／ｌ）水溶液中で、５０℃、２Ａ／ｄｍ2 の条件で定
電流電解処理を１分間行い、その後引き続き２３０Ｖの
条件で定電圧電解処理を１５分間行った。Example 3 An aluminum alloy material (1200 alloy) having a thickness of 0.2 mm was degreased with a surfactant or a weakly etching degreasing agent, and then potassium phthalate (20
g / l) An aqueous solution was subjected to constant current electrolysis for 1 minute under the conditions of 50 ° C. and 2 A / dm 2 , and then underwent constant voltage electrolysis for 15 minutes under the condition of 230V.
【００１６】〔実施例４〕厚さ０．２ｍｍのアルミニウ
ム合金材（１２００合金）を界面活性剤あるいは弱エッ
チング性脱脂剤で脱脂した後、ホウ酸アンモニウム（１
００ｇ／ｌ）水溶液中で、５０℃、２Ａ／ｄｍ2 の条件
で定電流電解処理を２．５分間行い、その後引き続き３
００Ｖの条件で定電圧電解処理を１５分間行った。Example 4 An aluminum alloy material (1200 alloy) having a thickness of 0.2 mm was degreased with a surfactant or a weak etching degreasing agent, and then ammonium borate (1
Constant current electrolysis treatment for 2.5 minutes under the conditions of 50 ° C. and 2 A / dm 2 in an aqueous solution of 00 g / l) and then 3 times.
A constant voltage electrolysis treatment was performed for 15 minutes under the condition of 00V.
【００１７】〔実施例５〕厚さ０．２ｍｍのアルミニウ
ム合金材（１２００合金）を界面活性剤あるいは弱エッ
チング性脱脂剤で脱脂した後、アジピン酸アンモニウム
（１５０ｇ／ｌ）水溶液中で、５０℃、２Ａ／ｄｍ2 の
条件で定電流電解処理を２分間行い、その後引き続き２
００Ｖの条件で定電圧電解処理を１０分間行った。Example 5 An aluminum alloy material (1200 alloy) having a thickness of 0.2 mm was degreased with a surfactant or a weak etching degreasing agent, and then 50 ° C. in an ammonium adipate (150 g / l) aqueous solution. Constant current electrolysis for 2 minutes under the condition of 2 A / dm 2 and then 2
Constant voltage electrolysis was performed for 10 minutes under the condition of 00V.
【００１８】〔実施例６〕厚さ０．２ｍｍのアルミニウ
ム合金材（１２００合金）を界面活性剤あるいは弱エッ
チング性脱脂剤で脱脂した後、シュウ酸塩（１５ｇ／
ｌ）水溶液中で、３０℃、１．５Ａ／ｄｍ2 の条件で定
電流電解処理を３分間行い、その後引き続き１５０Ｖの
条件で定電圧電解処理を１５分間行った。[Example 6] An aluminum alloy material (1200 alloy) having a thickness of 0.2 mm was degreased with a surfactant or a weakly etching degreasing agent, and then oxalate (15 g /
l) In the aqueous solution, a constant current electrolysis treatment was performed for 3 minutes under the conditions of 30 ° C. and 1.5 A / dm 2 , and then a constant voltage electrolysis treatment was performed for 15 minutes under the condition of 150V.
【００１９】〔実施例７〕厚さ０．２ｍｍのアルミニウ
ム合金材（１２００合金）を界面活性剤あるいは弱エッ
チング性脱脂剤で脱脂した後、１００℃の純水中に１０
分間浸漬してベーマイト処理した後、アジピン酸アンモ
ニウム（１５０ｇ／ｌ）水溶液中で、５０℃、２Ａ／ｄ
ｍ2 の条件で定電流電解処理を１分間行い、その後引き
続き２００Ｖの条件で定電圧電解処理を１５分間行っ
た。Example 7 An aluminum alloy material (1200 alloy) having a thickness of 0.2 mm was degreased with a surfactant or a weak etching degreasing agent, and then degreased in pure water at 100 ° C.
After immersion for a minute and boehmite treatment, in an ammonium adipate (150 g / l) aqueous solution at 50 ° C., 2 A / d
A constant current electrolysis treatment was carried out for 1 minute under the condition of m 2 and then a constant voltage electrolysis treatment was carried out for 15 minutes under the condition of 200V.
【００２０】〔実施例８〕厚さ０．２ｍｍのアルミニウ
ム合金材（１２００合金）を界面活性剤あるいは弱エッ
チング性脱脂剤で脱脂した後、ホウ酸（１６ｇ／ｌ）水
溶液中で、２０℃、２Ａ／ｄｍ2 の条件で定電流電解処
理を２分間行い、その後引き続き１０００Ｖの条件で定
電圧電解処理を５分間行い、そして６分間中断した後、
１０００Ｖの条件で定電圧電解処理を５分間行い、又、
６分間中断した後に１０００Ｖの条件で定電圧電解処理
を５分間行った。Example 8 An aluminum alloy material (1200 alloy) having a thickness of 0.2 mm was degreased with a surfactant or a weakly etching degreasing agent, and then in a boric acid (16 g / l) aqueous solution at 20 ° C. After constant current electrolysis for 2 minutes under the condition of 2 A / dm 2 , then constant voltage electrolysis for 5 minutes under the condition of 1000 V, and after interrupting for 6 minutes,
Perform constant voltage electrolysis for 5 minutes under the condition of 1000V.
After interruption for 6 minutes, constant voltage electrolysis was performed for 5 minutes under the condition of 1000V.
【００２１】〔比較例１〕厚さ０．２ｍｍのアルミニウ
ム合金材（１２００合金）を界面活性剤あるいは弱エッ
チング性脱脂剤で脱脂した後、シュウ酸（１５ｇ／ｌ）
水溶液中で、３０℃、１．５Ａ／ｄｍ2 の条件で定電流
電解処理を３分間行い、その後前記定電流電解処理時の
電圧より低い３６Ｖの条件で定電圧電解処理を１５分間
行った。[Comparative Example 1] An aluminum alloy material (1200 alloy) having a thickness of 0.2 mm was degreased with a surfactant or a weakly etching degreasing agent, and then oxalic acid (15 g / l).
In an aqueous solution, a constant current electrolysis treatment was performed for 3 minutes under the conditions of 30 ° C. and 1.5 A / dm 2 , and then a constant voltage electrolysis treatment was performed for 15 minutes under a condition of 36 V lower than the voltage during the constant current electrolysis treatment.
【００２２】[0022]
【特性】上記各例で得られたアルミニウム合金材の皮膜
ガス放出量（加熱減量）及び耐食性（ＣＡＳＳ試験８時
間後の孔食深さ、変色の程度）について調べたので、そ
の結果を下記の表１に示す。
この表１によれば、アルミニウム合金材を皮膜溶解性の
低い電解質溶液中で定電流電解処理を行い、その後前記
定電流電解処理時の電圧より高い電圧での定電圧電解処
理を行うと、ガス放出量が少なく、耐食性に優れたアル
ミニウム合金材が得られているのに対して、二段階の電
解処理が行われても、後段の定電圧電解処理時の電解電
圧が低いと、本発明のような特長を奏するアルミニウム
合金材が得られていないことが判る。[Characteristics] The amount of coating gas released (heat loss) and corrosion resistance (pitting depth after 8 hours of CASS test, degree of discoloration) of the aluminum alloy material obtained in each of the above examples were examined. The results are shown below. It shows in Table 1. According to this Table 1, when an aluminum alloy material is subjected to constant current electrolysis treatment in an electrolyte solution having low film solubility, and then subjected to constant voltage electrolysis treatment at a voltage higher than the voltage at the time of constant current electrolysis treatment, A small amount of release, while an aluminum alloy material excellent in corrosion resistance is obtained, even if two-stage electrolytic treatment is performed, if the electrolytic voltage during the constant-voltage electrolytic treatment of the latter stage is low, It can be seen that an aluminum alloy material having such characteristics has not been obtained.
Claims (5)
皮膜溶解性の低い電解質溶液中で定電流電解処理を行
い、その後前記定電流電解処理時の電圧より高い電圧で
の定電圧電解処理を行うことを特徴とする真空機器用ア
ルミニウム又はアルミニウム合金材の製造法。1. An aluminum or aluminum alloy material is subjected to a constant current electrolysis treatment in an electrolyte solution having a low film solubility, and then subjected to a constant voltage electrolysis treatment at a voltage higher than the voltage during the constant current electrolysis treatment. And a method for manufacturing aluminum or aluminum alloy material for vacuum equipment.
皮膜溶解性の低い電解質溶液中で定電流電解処理を行
い、その後前記定電流電解処理時の電圧より高い電圧で
の定電圧電解処理を所定時間行い、中断後、再度定電圧
電解処理を所定時間行うことを特徴とする真空機器用ア
ルミニウム又はアルミニウム合金材の製造法。2. An aluminum or aluminum alloy material is subjected to a constant current electrolysis treatment in an electrolyte solution having a low film solubility, and then a constant voltage electrolysis treatment at a voltage higher than the voltage during the constant current electrolysis treatment is performed for a predetermined time, After the interruption, a constant voltage electrolysis treatment is again performed for a predetermined time, and a method for producing an aluminum or aluminum alloy material for vacuum equipment.
皮膜溶解性の低い電解質溶液中で定電流電解処理を行
い、その後前記定電流電解処理時の電圧より高い電圧で
の定電圧電解処理を行い、その後熱処理することを特徴
とする真空機器用アルミニウム又はアルミニウム合金材
の製造法。3. An aluminum or aluminum alloy material is subjected to a constant current electrolysis treatment in an electrolyte solution having a low film solubility, followed by a constant voltage electrolysis treatment at a voltage higher than the voltage during the constant current electrolysis treatment, and then a heat treatment. A method for producing an aluminum or aluminum alloy material for vacuum equipment, comprising:
ベーマイト処理した後、皮膜溶解性の低い電解質溶液中
で定電流電解処理を行い、その後前記定電流電解処理時
の電圧より高い電圧での定電圧電解処理を行うことを特
徴とする真空機器用アルミニウム又はアルミニウム合金
材の製造法。4. A boehmite treatment of aluminum or an aluminum alloy material, a constant current electrolysis treatment in an electrolyte solution having a low film solubility, and a constant voltage electrolysis treatment at a voltage higher than the voltage during the constant current electrolysis treatment. A method for producing an aluminum or aluminum alloy material for vacuum equipment, the method comprising:
酸、ホウ酸、ホウ酸塩、リン酸塩、フタル酸塩、マレイ
ン酸塩、安息香酸塩、酒石酸塩、クエン酸塩の群の中か
ら選ばれる少なくとも一つを含むものであることを特徴
とする請求項１〜請求項４の真空機器用アルミニウム又
はアルミニウム合金材の製造法。5. An electrolyte solution having low film solubility is selected from the group consisting of adipic acid, boric acid, borate, phosphate, phthalate, maleate, benzoate, tartrate and citrate. The method for producing an aluminum or aluminum alloy material for vacuum equipment according to any one of claims 1 to 4, which comprises at least one selected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17384391A JP3152960B2 (en) | 1991-07-15 | 1991-07-15 | Manufacturing method of aluminum or aluminum alloy material for vacuum equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17384391A JP3152960B2 (en) | 1991-07-15 | 1991-07-15 | Manufacturing method of aluminum or aluminum alloy material for vacuum equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0525694A true JPH0525694A (en) | 1993-02-02 |
| JP3152960B2 JP3152960B2 (en) | 2001-04-03 |
Family
ID=15968193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17384391A Expired - Fee Related JP3152960B2 (en) | 1991-07-15 | 1991-07-15 | Manufacturing method of aluminum or aluminum alloy material for vacuum equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3152960B2 (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05114582A (en) * | 1991-10-22 | 1993-05-07 | Tokyo Electron Yamanashi Kk | Vacuum processor |
| WO1996015295A1 (en) * | 1994-11-16 | 1996-05-23 | Kabushiki Kaisha Kobe Seiko Sho | Vacuum chamber made of aluminum or its alloy, and surface treatment and material for the vacuum chamber |
| KR100583283B1 (en) * | 2005-07-13 | 2006-05-26 | 주식회사 브이엠티 | Method for manufacturing extremely high vacuum ion pump |
| JP2006184822A (en) * | 2004-12-28 | 2006-07-13 | Shin Etsu Chem Co Ltd | Pellicle for photolithography and pellicle frame |
| WO2006123736A1 (en) * | 2005-05-18 | 2006-11-23 | Ulvac, Inc. | Corrosion resistance treatment method for aluminum or aluminum alloy |
| JP2008153273A (en) * | 2006-12-14 | 2008-07-03 | Ulvac Japan Ltd | Vacuum cooling member and vacuum apparatus |
| JP2008163432A (en) * | 2006-12-28 | 2008-07-17 | Mitsubishi Alum Co Ltd | Method for producing surface-treated aluminum material, and production device for surface-treated aluminum material |
| JP2008240024A (en) * | 2007-03-26 | 2008-10-09 | Ulvac Japan Ltd | Compound object and manufacturing method of the same |
| JP2010095774A (en) * | 2008-10-20 | 2010-04-30 | Mitsubishi Alum Co Ltd | Method for producing surface-treated aluminum material for vacuum apparatus |
| JP2012057256A (en) * | 2005-06-17 | 2012-03-22 | Tohoku Univ | Metal oxide film, laminate, metal member and process for producing the same |
| KR20180007237A (en) * | 2016-07-12 | 2018-01-22 | 에이비엠 주식회사 | Metal component and manufacturing method thereof and process chamber having the metal component |
-
1991
- 1991-07-15 JP JP17384391A patent/JP3152960B2/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05114582A (en) * | 1991-10-22 | 1993-05-07 | Tokyo Electron Yamanashi Kk | Vacuum processor |
| WO1996015295A1 (en) * | 1994-11-16 | 1996-05-23 | Kabushiki Kaisha Kobe Seiko Sho | Vacuum chamber made of aluminum or its alloy, and surface treatment and material for the vacuum chamber |
| JP2006184822A (en) * | 2004-12-28 | 2006-07-13 | Shin Etsu Chem Co Ltd | Pellicle for photolithography and pellicle frame |
| KR100935964B1 (en) * | 2005-05-18 | 2010-01-08 | 가부시키가이샤 알박 | Corrosion resistance treatment method for aluminum or aluminum alloy |
| WO2006123736A1 (en) * | 2005-05-18 | 2006-11-23 | Ulvac, Inc. | Corrosion resistance treatment method for aluminum or aluminum alloy |
| JP2006322040A (en) * | 2005-05-18 | 2006-11-30 | Ulvac Japan Ltd | Method for anticorrosion-treating aluminum or aluminum alloy |
| US9476137B2 (en) | 2005-06-17 | 2016-10-25 | Tohoku University | Metal oxide film, laminate, metal member and process for producing the same |
| JP2012057256A (en) * | 2005-06-17 | 2012-03-22 | Tohoku Univ | Metal oxide film, laminate, metal member and process for producing the same |
| KR100583283B1 (en) * | 2005-07-13 | 2006-05-26 | 주식회사 브이엠티 | Method for manufacturing extremely high vacuum ion pump |
| JP2008153273A (en) * | 2006-12-14 | 2008-07-03 | Ulvac Japan Ltd | Vacuum cooling member and vacuum apparatus |
| JP2008163432A (en) * | 2006-12-28 | 2008-07-17 | Mitsubishi Alum Co Ltd | Method for producing surface-treated aluminum material, and production device for surface-treated aluminum material |
| JP2008240024A (en) * | 2007-03-26 | 2008-10-09 | Ulvac Japan Ltd | Compound object and manufacturing method of the same |
| JP2010095774A (en) * | 2008-10-20 | 2010-04-30 | Mitsubishi Alum Co Ltd | Method for producing surface-treated aluminum material for vacuum apparatus |
| KR20180007237A (en) * | 2016-07-12 | 2018-01-22 | 에이비엠 주식회사 | Metal component and manufacturing method thereof and process chamber having the metal component |
| JP2018021255A (en) * | 2016-07-12 | 2018-02-08 | エイビーエム カンパニー リミテッドＡｂｍ Ｃｏ．，Ｌｔｄ． | Metal component and manufacturing method thereof, and process chamber having the metal component |
| US11417503B2 (en) | 2016-07-12 | 2022-08-16 | Abm Co., Ltd. | Metal component and manufacturing method thereof and process chamber having the metal component |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3152960B2 (en) | 2001-04-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP3647461B2 (en) | Cleaning of processed aluminum products | |
| TWI421380B (en) | Corrosion resistance of aluminum or aluminum alloys | |
| TWI352749B (en) | ||
| JP3152960B2 (en) | Manufacturing method of aluminum or aluminum alloy material for vacuum equipment | |
| Peng et al. | Preparation of anodic films on 2024 aluminum alloy in boric acid-containing mixed electrolyte | |
| CN110863227B (en) | Titanium alloy pulse-direct current anodic oxidation surface treatment method | |
| JPH08144088A (en) | Surface treatment of vacuum chamber member made of aluminium or aluminum alloy | |
| US3351442A (en) | Treatment of aluminum foil and product produced thereby | |
| US6242111B1 (en) | Anodized aluminum susceptor for forming integrated circuit structures and method of making anodized aluminum susceptor | |
| KR101819918B1 (en) | Method of Plasma electrolytic oxidation | |
| JP2005105300A (en) | Surface treatment method of aluminum or aluminum alloy used for vacuum device and its components, and vacuum device and its components | |
| JPH09184094A (en) | Surface treated aluminum material and its production | |
| JPH0372098A (en) | Production of aluminum material for vacuum | |
| JP5534951B2 (en) | Heat exchanger processing method and heat exchanger | |
| JP5352204B2 (en) | Surface-treated aluminum material for vacuum equipment | |
| JP5371477B2 (en) | Formation method of oxide film | |
| US3578570A (en) | Aluminum capacitor foil | |
| KR101765005B1 (en) | Preparing method of aluminium alloy hybrid oxide coating layers | |
| US4381231A (en) | DC Etching of aluminum electrolytic capacitor foil | |
| JP5452034B2 (en) | Surface treatment member for semiconductor manufacturing apparatus and method for manufacturing the same | |
| KR20220058691A (en) | Post-treatment method of aluminum alloys in oxalic acid anodizing and Aluminum alloys manufactured by this method | |
| JPH09302499A (en) | Aluminum material | |
| KR102599930B1 (en) | Sealing agent for aluminum series matter anodized and Sealing method using the same | |
| JP5334125B2 (en) | Method for producing surface-treated aluminum material for vacuum equipment | |
| KR20180131280A (en) | Method of desmut treatment of aluminum alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 8 Free format text: PAYMENT UNTIL: 20090126 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 9 Free format text: PAYMENT UNTIL: 20100126 |
|
| FPAY | Renewal fee payment (prs date is renewal date of database) |
Year of fee payment: 10 Free format text: PAYMENT UNTIL: 20110126 |
|
| LAPS | Cancellation because of no payment of annual fees |