JP3216703B2 - Method of anodizing aluminum or its alloy - Google Patents
Method of anodizing aluminum or its alloyInfo
- Publication number
- JP3216703B2 JP3216703B2 JP16232197A JP16232197A JP3216703B2 JP 3216703 B2 JP3216703 B2 JP 3216703B2 JP 16232197 A JP16232197 A JP 16232197A JP 16232197 A JP16232197 A JP 16232197A JP 3216703 B2 JP3216703 B2 JP 3216703B2
- Authority
- JP
- Japan
- Prior art keywords
- article
- treated
- time
- processed
- oxide film
- 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
Links
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、アルミニウム又は
その合金からなる被処理品を電解浴中で陽極酸化処理し
て表面に酸化皮膜を形成する陽極酸化処理方法に関する
ものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an anodic oxidation method for forming an oxide film on a surface of an article to be treated made of aluminum or an alloy thereof in an electrolytic bath.
【０００２】[0002]
【従来の技術】アルミニウム素材の表面硬度を向上させ
る方法として、陽極酸化処理（アルマイト処理）方法が
ある。この処理法はアルミニウム素材を酸浴中で陽極と
して電解するもので、この処理によってアルミニウム素
材の表面にアルミナ皮膜が形成され、機械的特性、耐食
性等を著しく向上させることができる。アルミナ皮膜の
厚さにより処理品の特性は大きく変化し、膜厚を制御す
ることは処理品の品質を管理するために非常に重要にな
る。2. Description of the Related Art Anodizing treatment (alumite treatment) is known as a method for improving the surface hardness of an aluminum material. In this treatment method, an aluminum material is electrolyzed as an anode in an acid bath. By this treatment, an alumina film is formed on the surface of the aluminum material, so that mechanical properties, corrosion resistance, and the like can be significantly improved. The characteristics of the processed product greatly change depending on the thickness of the alumina film, and controlling the film thickness is very important for controlling the quality of the processed product.
【０００３】一般に、アルミナ皮膜の膜厚は処理品の単
位面積当りに流れる電流量、即ち電流密度と通電時間に
比例するので、これら２つの要素を制御することができ
れば、膜厚は制御できる。電流密度を算出するためには
アルマイト処理される被処理品の表面積の値を求める必
要があるが、被処理品の形状及び大きさは多様である。
この点を解決する方法として、従来電解浴中の陽陰両極
間に通ずる電流を時間で積分したものに相当する通電量
を監視することにより皮膜の厚さを制御する方法が提案
されている（特開平４−１２０２９８号公報）。In general, the thickness of the alumina film is proportional to the amount of current flowing per unit area of the processed product, that is, the current density and the energizing time. Therefore, if these two factors can be controlled, the film thickness can be controlled. In order to calculate the current density, it is necessary to determine the surface area of the article to be alumite-treated, but the shape and size of the article vary.
As a method for solving this point, there has been proposed a method of controlling the thickness of a film by monitoring an amount of current corresponding to a value obtained by integrating a current passing between the positive and negative electrodes in an electrolytic bath with time ( JP-A-4-120298).
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、通電量
を監視する上記従来の方法では、電流密度を算出できな
いため、アルミナ皮膜の厚さを正確に制御することは困
難である。本発明の目的は、アルミニウム又はその合金
からなる複雑形状の被処理品の表面に電解浴中で陽極酸
化により形成される酸化皮膜の厚さを被処理品の表面積
を測定することなく、所望の厚さに正確に制御できるア
ルミニウム又はその合金の陽極酸化処理方法を提供する
ことにある。本発明の別の目的は、互いに異なる材質か
らなる複数種のアルミニウム又はその合金からなる被処
理品の表面に電解浴中で同時に陽極酸化により形成され
る酸化皮膜の厚さを被処理品の表面積を測定することな
く、所望の厚さに正確に制御できるアルミニウム又はそ
の合金の陽極酸化処理方法を提供することにある。However, in the above-mentioned conventional method of monitoring the amount of energization, the current density cannot be calculated, so that it is difficult to accurately control the thickness of the alumina film. An object of the present invention is to measure the thickness of an oxide film formed by anodic oxidation in an electrolytic bath on the surface of a workpiece having a complicated shape made of aluminum or its alloy without measuring the surface area of the workpiece. An object of the present invention is to provide a method of anodizing aluminum or an alloy thereof, which can be accurately controlled in thickness. Another object of the present invention is to determine the thickness of an oxide film formed by simultaneous anodic oxidation in an electrolytic bath on the surface of a workpiece made of a plurality of types of aluminum or alloys thereof made of different materials from each other. It is an object of the present invention to provide a method of anodizing aluminum or an alloy thereof, which can be accurately controlled to a desired thickness without measuring the anodization.
【０００５】[0005]
【課題を解決するための手段】請求項１に係る発明は、
図１に示すように、アルミニウム又はその合金を被処理
品１１としてこの被処理品１１を電解浴１２中で陽極酸
化処理して表面に酸化皮膜を形成する陽極酸化処理方法
において、面積が既知であって被処理品１１と同一材料
からなる標準試料片１３を同時に陽極酸化処理し、この
時に標準試料片１３を流れる電流値を測定して電流密度
を算出し、電流密度に基づいて被処理品１１の処理すべ
き時間を計算し、処理時間に基づいて被処理品１１の酸
化皮膜の厚さを制御することを特徴とするアルミニウム
又はその合金の陽極酸化処理方法である。複雑形状の被
処理品の表面に陽極酸化により形成される酸化皮膜の厚
さを被処理品の表面積を測定することなく正確に制御で
きる。The invention according to claim 1 is
As shown in FIG. 1, in an anodizing treatment method in which aluminum or its alloy is treated as an article to be treated 11 and the article to be treated 11 is anodized in an electrolytic bath 12 to form an oxide film on the surface, the area is known. At this time, the standard sample 13 made of the same material as the article 11 to be processed is anodized at the same time. At this time, the current flowing through the standard sample 13 is measured to calculate the current density. 11 is a method of anodizing aluminum or an alloy thereof, wherein a time to be processed is calculated and the thickness of an oxide film of the article to be processed 11 is controlled based on the processing time. The thickness of an oxide film formed by anodic oxidation on the surface of a workpiece having a complicated shape can be accurately controlled without measuring the surface area of the workpiece.
【０００６】請求項２に係る発明は、図２に示すよう
に、互いに異なる材質からなる複数種のアルミニウム又
はその合金を被処理品１１，２１としてこれらの被処理
品１１，２１を電解浴１２中で同時に陽極酸化処理して
表面に酸化皮膜を形成する陽極酸化処理方法において、
複数の被処理品１１，２１の材質の異なる毎に面積が既
知であってそれぞれの被処理品と同一材質からなる複数
種の標準試料片１３，２３を同時に陽極酸化処理し、こ
の時にそれぞれの標準試料片１３，２３を流れる電流値
を測定して電流密度を算出し、これらの電流密度に基づ
いて被処理品１１，２１の処理すべき時間を計算し、こ
の処理時間に基づいてそれぞれの被処理品１１，２１の
酸化皮膜の厚さを制御することを特徴とするアルミニウ
ム又はその合金の陽極酸化処理方法である。互いに異な
る材質からなる複数種の複雑形状の被処理品を同一電解
浴中で同一の電源を用いて同時に陽極酸化処理でき、被
処理品の表面に形成される酸化皮膜の厚さを被処理品の
表面積を測定することなく正確に制御できる。As shown in FIG. 2, the invention according to claim 2 uses a plurality of types of aluminum or alloys thereof made of different materials as workpieces 11 and 21, and converts these workpieces 11 and 21 to an electrolytic bath 12 as shown in FIG. In the anodizing treatment method of forming an oxide film on the surface by simultaneously anodizing in the
A plurality of types of standard sample pieces 13 and 23, each having a known area and having the same material as each of the processed objects, are simultaneously subjected to anodizing treatment. The current values flowing through the standard sample pieces 13 and 23 are measured to calculate the current density, the time to process the articles 11 and 21 is calculated based on the current densities, and the respective processing times are calculated based on the processing times. An anodic oxidation method for aluminum or an alloy thereof, characterized in that the thickness of an oxide film on the articles to be processed 11 and 21 is controlled. Anodizing can be performed simultaneously on multiple types of workpieces of different shapes made of different materials using the same power supply in the same electrolytic bath, and the thickness of the oxide film formed on the surface of the workpiece is controlled. Can be accurately controlled without measuring the surface area of the surface.
【０００７】[0007]
【発明の実施の形態】次に本発明の実施の形態を説明す
る。本発明の被処理品は純粋なアルミニウム材に限らず
その合金を含む。アルミニウム合金としては、Ａｌ−Ｃ
ｕ−Ｍｇ系、Ａｌ−Ｓｉ系、Ａｌ−Ｚｎ−Ｍｇ−Ｃｕ系
の加工用合金、Ａｌ−Ｃｕ−Ｓｉ系、Ａｌ−Ｓｉ系、Ａ
ｌ−Ｃｕ−Ｎｉ−Ｍｇ系、Ａｌ−Ｍｇ系、Ａｌ−Ｓｉ−
Ｃｕ−Ｎｉ−Ｍｇ系の鋳造用合金等が挙げられる。電解
浴の電解液としては、特に限定されないが、硫酸、シュ
ウ酸、クロム酸水溶液が使用される。電解浴の温度は通
常は−１０℃〜室温が採用される。Next, an embodiment of the present invention will be described. The workpiece of the present invention includes not only a pure aluminum material but also an alloy thereof. As an aluminum alloy, Al-C
u-Mg-based, Al-Si-based, Al-Zn-Mg-Cu-based processing alloys, Al-Cu-Si-based, Al-Si-based, A
l-Cu-Ni-Mg, Al-Mg, Al-Si-
Cu-Ni-Mg based casting alloys and the like can be mentioned. The electrolytic solution of the electrolytic bath is not particularly limited, but an aqueous solution of sulfuric acid, oxalic acid, or chromic acid is used. The temperature of the electrolytic bath is usually from −10 ° C. to room temperature.
【０００８】[0008]
【実施例】次に本発明の実施例を図面に基づいて説明す
る。 ＜実施例１＞図１に示すように、アルミニウム合金であ
るＡ５０５２材からなる３個の被処理品１１と、これら
の被処理品１１と同一材料からなる全表面積が１ｄｍ2
の正方形の標準試料片１３とを硫酸２００ｇ／ｌを含有
する０℃の電解浴１２に入れた。この例では被処理品１
１の目標とする酸化皮膜の厚さは３０μｍであった。こ
こで標準試料片１３は電流計１４及びスイッチ１６を介
して直流電源１７の陽極に接続され、直流電源１７の陰
極は電解浴１２を構成する導電性の電解槽１２ａに接続
した。また３個の被処理品１１はスイッチ１６を介して
直流電源１７の陽極に接続した。スイッチ１６を閉じて
回路に電流を流した。このとき電流計１４が３Ａの電流
値を示すように電源を調整した。電解処理は定電流電解
法で行った。このとき、被処理品１１にも３Ａ／ｄｍ2
の電流が流れることになる。予め電流密度から単位時間
に形成される酸化皮膜の厚さは既知であり、３Ａ／ｄｍ
2では６０μｍ／時の速度で皮膜が形成されることが分
っている。そこで、目標とする厚さ（３０μｍ）の酸化
皮膜を形成するために被処理品１１に対して３０分間電
解を行った。電解後の被処理品１１の酸化皮膜の厚さを
高周波うず電流式測定法により測定したところ、目標と
した３０μｍであった。Next, an embodiment of the present invention will be described with reference to the drawings. Embodiment 1 As shown in FIG. 1, three workpieces 11 made of aluminum alloy A5052 and a total surface area of 1 dm 2 made of the same material as those of the workpieces 11 were used.
Was placed in an electrolytic bath 12 at 200C containing 200 g / l sulfuric acid. In this example, the article to be processed 1
The target oxide film thickness of No. 1 was 30 μm. Here, the standard sample piece 13 was connected to the anode of a DC power supply 17 via an ammeter 14 and a switch 16, and the cathode of the DC power supply 17 was connected to a conductive electrolytic cell 12 a constituting the electrolytic bath 12. Further, the three articles to be processed 11 were connected to the anode of a DC power supply 17 via a switch 16. The switch 16 was closed to allow current to flow through the circuit. At this time, the power supply was adjusted so that the ammeter 14 indicates a current value of 3 A. The electrolytic treatment was performed by a constant current electrolytic method. At this time, 3 A / dm 2
Will flow. The thickness of the oxide film formed per unit time from the current density is known in advance, and is 3 A / dm.
2 , it was found that a film was formed at a speed of 60 μm / hour. Therefore, electrolysis was performed on the article to be processed 11 for 30 minutes in order to form an oxide film having a target thickness (30 μm). The thickness of the oxide film of the article to be treated 11 after the electrolysis was measured by a high-frequency eddy current measuring method, and was found to be 30 μm as a target.
【０００９】＜実施例２＞図２に示すように、アルミニ
ウム合金であるＡ５０５２材からなる３個の被処理品１
１と、これらの被処理品１１と同一材料からなる全表面
積が１ｄｍ2の正方形の標準試料片１３と、別のアルミ
ニウム合金であるＡＣ８Ａ材からなる３個の被処理品２
１と、これらの被処理品２１と同一材料からなる全表面
積が１ｄｍ 2の正方形の標準試料片２３とをそれぞれ実
施例１と同じ電解浴１２に入れた。この例では被処理品
１１及び２１の目標とする酸化皮膜の厚さはそれぞれ３
０μｍであった。ここで標準試料片１３及び３個の被処
理品１１は実施例１と同様に直流電源１７に接続した。
また標準試料片２３は電流計２４及びスイッチ２６を介
して、また３個の被処理品２１はスイッチ２６を介して
それぞれ直流電源１７の陽極に接続した。スイッチ１
６、２６を閉じて回路に電流を流した。このとき電流計
１４が３Ａの電流値を示すように電源を調整した。電解
処理は定電流電解法で行った。このとき、電流計２４の
電流値は１．５Ａを示した。これらの電流値からこの陽
極酸化処理時の標準試料片１３の電流密度は３Ａ／ｄｍ
2、標準試料片２３の電流密度は１．５Ａ／ｄｍ2と算出
された。このとき被処理品１１の電流密度は３Ａ／ｄｍ
2、被処理品２１の電流密度は１．５Ａ／ｄｍ2となる。
３Ａ／ｄｍ2では６０μｍ／時、１．５Ａ／ｄｍ2では３
０μｍ／時の速度で皮膜が形成されることが分っている
ので、スイッチ１６は３０分間だけ閉じ、スイッチ２６
は６０分間だけ閉じた。電解後の被処理品１１及び２１
の酸化皮膜の厚さを高周波うず電流式測定法により測定
したところ、それぞれに目標とした３０μｍであった。<Embodiment 2> As shown in FIG.
To-be-processed articles 1 made of A5052 material which is a
1 and the entire surface made of the same material as these workpieces 11
Product is 1dmTwoSquare standard specimen 13 and another aluminum
To-be-processed object 2 made of AC8A material which is a nickel alloy
1 and the entire surface made of the same material as those to be processed 21
Product is 1dm TwoOf the square standard specimen 23
It was placed in the same electrolytic bath 12 as in Example 1. In this example,
The target oxide film thickness of each of 11 and 21 is 3
It was 0 μm. Here, the standard specimen 13 and three
The article 11 was connected to a DC power supply 17 as in the first embodiment.
The standard sample piece 23 is connected via an ammeter 24 and a switch 26.
Then, the three articles to be processed 21 are connected via the switch 26 again.
Each was connected to the anode of the DC power supply 17. Switch 1
6, 26 were closed and current flowed through the circuit. At this time ammeter
The power supply was adjusted so that 14 indicated a current value of 3 A. electrolytic
The treatment was performed by a constant current electrolysis method. At this time, the ammeter 24
The current value was 1.5 A. From these current values,
The current density of the standard specimen 13 during the extreme oxidation treatment is 3 A / dm.
TwoThe current density of the standard specimen 23 is 1.5 A / dm.TwoAnd calculate
Was done. At this time, the current density of the article to be processed 11 is 3 A / dm.
TwoThe current density of the article to be processed 21 is 1.5 A / dm.TwoBecomes
3A / dmTwo60 μm / hour, 1.5 A / dmTwoThen 3
It is known that a film is formed at a speed of 0 μm / hour.
Therefore, the switch 16 is closed only for 30 minutes, and the switch 26 is closed.
Closed for only 60 minutes. Treated products 11 and 21 after electrolysis
Oxide thickness measured by high frequency eddy current method
As a result, the target was 30 μm.
【００１０】[0010]
【発明の効果】以上述べたように、本発明によれば、ア
ルミニウム又はその合金からなる被処理品を電解浴中で
陽極酸化処理して表面に酸化皮膜を形成するに際し、面
積が既知であって被処理品と同一材料からなる標準試料
片を同時に陽極酸化処理し、この時に標準試料片を流れ
る電流値を測定して電流密度を算出し、電流密度に基づ
いて被処理品の処理すべき時間を計算し、処理時間に基
づいて被処理品の酸化皮膜の厚さを制御するようにした
ので、形成される酸化皮膜の厚さを被処理品の表面積を
測定することなく正確に制御できる。また、互いに異な
る材質からなる複数種のアルミニウム又はその合金を被
処理品としてこれらの被処理品を電解浴中で陽極酸化処
理して表面に酸化皮膜を形成する場合、複数の被処理品
の材質の異なる毎に面積が既知であってそれぞれの被処
理品と同一材質からなる複数種の標準試料片を同時に陽
極酸化処理し、この時にそれぞれの標準試料片を流れる
電流値を測定して電流密度を算出し、これらの電流密度
に基づいて被処理品の処理すべき時間を計算し、この処
理時間に基づいてそれぞれの被処理品の酸化皮膜の厚さ
を制御するようにしたので、互いに異なる材質からなる
複数種の複雑形状の被処理品を同一電解浴中で同一の電
源を用いて同時に陽極酸化処理でき、酸化皮膜の厚さを
被処理品の表面積を測定することなく正確に制御でき
る。As described above, according to the present invention, when an article to be treated made of aluminum or an alloy thereof is anodized in an electrolytic bath to form an oxide film on the surface, the area is known. A standard specimen made of the same material as the workpiece is anodized at the same time.At this time, the current flowing through the standard specimen is measured to calculate the current density, and the workpiece should be treated based on the current density. Since the time is calculated and the thickness of the oxide film of the article to be processed is controlled based on the processing time, the thickness of the oxide film to be formed can be accurately controlled without measuring the surface area of the article to be processed. . Further, when a plurality of types of aluminum or alloys thereof made of different materials are to be processed, and these processed products are anodized in an electrolytic bath to form an oxide film on the surface, the materials of the plurality of processed products are required. Anodizing is performed simultaneously on a plurality of standard specimens of the same material as the object to be treated, the area of which is known for each of the different specimens, and the current value flowing through each standard specimen at this time is measured to determine the current density. Is calculated based on these current densities, and the time to process the article to be processed is calculated, and the thickness of the oxide film of each article to be processed is controlled based on the processing time. Anodizing can be performed simultaneously on multiple types of workpieces of complex shapes made of materials using the same power supply in the same electrolytic bath, and the thickness of the oxide film can be accurately controlled without measuring the surface area of the workpiece.
【図１】本発明の陽極酸化処理方法に使用される電解浴
を含む装置の構成図。FIG. 1 is a configuration diagram of an apparatus including an electrolytic bath used in the anodic oxidation treatment method of the present invention.
【図２】本発明の陽極酸化処理方法に使用される電解浴
を含む別の装置の構成図。FIG. 2 is a configuration diagram of another apparatus including an electrolytic bath used in the anodic oxidation treatment method of the present invention.
１１，２１ 被処理品 １２ 電解浴 １３，２３ 標準試料片 11, 21 Workpiece 12 Electrolytic bath 13, 23 Standard specimen
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) C25D 11/00 - 11/24 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int. Cl. 7 , DB name) C25D 11/00-11/24
Claims (2)
1)としてこの被処理品(11)を電解浴(12)中で陽極酸化処
理して表面に酸化皮膜を形成する陽極酸化処理方法にお
いて、 面積が既知であって前記被処理品(11)と同一材料からな
る標準試料片(13)を同時に陽極酸化処理し、この時に前
記標準試料片(13)を流れる電流値を測定して電流密度を
算出し、前記電流密度に基づいて前記被処理品(11)の処
理すべき時間を計算し、前記処理時間に基づいて前記被
処理品(11)の酸化皮膜の厚さを制御することを特徴とす
るアルミニウム又はその合金の陽極酸化処理方法。1. An article to be treated (1) made of aluminum or an alloy thereof.
In the anodic oxidation method for forming an oxide film on the surface by anodizing the article to be treated (11) in an electrolytic bath (12) as 1), the area is known and the article to be treated (11) is The standard sample pieces (13) made of the same material are simultaneously subjected to anodizing treatment.At this time, the current flowing through the standard sample pieces (13) is measured to calculate the current density, and the article to be processed is calculated based on the current density. A method for anodizing aluminum or an alloy thereof, comprising calculating a time to be treated in (11) and controlling a thickness of an oxide film of the article to be treated (11) based on the treatment time.
ミニウム又はその合金を被処理品(11,21)としてこれら
の被処理品(11,21)を電解浴(12)中で同時に陽極酸化処
理して表面に酸化皮膜を形成する陽極酸化処理方法にお
いて、 前記複数の被処理品(11,21)の材質の異なる毎に面積が
既知であってそれぞれの被処理品と同一材質からなる複
数種の標準試料片(13,23)を同時に陽極酸化処理し、こ
の時にそれぞれの標準試料片(13,23)を流れる電流値を
測定して電流密度を算出し、これらの電流密度に基づい
て前記被処理品(11,21)の処理すべき時間を計算し、前
記処理時間に基づいてそれぞれの被処理品(11,21)の酸
化皮膜の厚さを制御することを特徴とするアルミニウム
又はその合金の陽極酸化処理方法。2. A plurality of kinds of aluminum or alloys thereof made of different materials are treated as an article to be treated (11, 21), and these articles (11, 21) are simultaneously subjected to anodizing treatment in an electrolytic bath (12). In the anodic oxidation method of forming an oxide film on the surface by the method, the area of each of the plurality of workpieces (11, 21) is different for each different material is known, and a plurality of types of the same material as the respective workpieces The standard sample pieces (13, 23) are simultaneously subjected to anodizing treatment.At this time, the current flowing through each of the standard sample pieces (13, 23) is measured to calculate the current density, and the coating is performed based on these current densities. Aluminum or an alloy thereof, wherein the time to be processed of the processed product (11, 21) is calculated, and the thickness of the oxide film of each of the processed products (11, 21) is controlled based on the processing time. Anodizing treatment method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16232197A JP3216703B2 (en) | 1997-06-19 | 1997-06-19 | Method of anodizing aluminum or its alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16232197A JP3216703B2 (en) | 1997-06-19 | 1997-06-19 | Method of anodizing aluminum or its alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH1112794A JPH1112794A (en) | 1999-01-19 |
| JP3216703B2 true JP3216703B2 (en) | 2001-10-09 |
Family
ID=15752317
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16232197A Expired - Fee Related JP3216703B2 (en) | 1997-06-19 | 1997-06-19 | Method of anodizing aluminum or its alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3216703B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2359277A1 (en) | 2001-10-18 | 2003-04-18 | Ibm Canada Limited-Ibm Canada Limitee | Slow materialization of scrollable cursor result sets |
| KR101342413B1 (en) * | 2006-09-27 | 2013-12-17 | 신스케 모치즈키 | Ceramic coated metal material and production method thereof |
-
1997
- 1997-06-19 JP JP16232197A patent/JP3216703B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH1112794A (en) | 1999-01-19 |
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