JPH06346271A - Nickel laminate and its production - Google Patents
Nickel laminate and its productionInfo
- Publication number
- JPH06346271A JPH06346271A JP16007993A JP16007993A JPH06346271A JP H06346271 A JPH06346271 A JP H06346271A JP 16007993 A JP16007993 A JP 16007993A JP 16007993 A JP16007993 A JP 16007993A JP H06346271 A JPH06346271 A JP H06346271A
- Authority
- JP
- Japan
- Prior art keywords
- nickel
- nickel layer
- layer
- electroforming
- laminate
- 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
Landscapes
- Particle Formation And Scattering Control In Inkjet Printers (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、例えばインクジェット
用ノズル振動板のように耐振動性が要求される部品や電
子部品用チップ挿入用治具などに好適に用いられる、密
着良好なニッケル積層体並びにその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a nickel laminate having good adhesion, which is suitable for use in components requiring vibration resistance such as ink jet nozzle diaphragms and chip insertion jigs for electronic components. And the manufacturing method thereof.
【０００２】[0002]
【従来の技術】従来、例えばインクジェット用ノズル振
動板は、エッチングで作られるのが一般的である。その
エッチングに際しては、図４の（Ａ）に示すようにＳＵ
Ｓ材１０（１５〜２０μ厚）の裏面側にポリイミド１１
をコートし、ついで同図の（Ｂ）に示すようにＳＵＳ材
１０の表面にレジスト膜１２をパターンニング形成し、
ついで同図の（Ｃ）に示すようにエッチング処理する。
最後に、同図の（Ｄ）に示すようにレジスト膜１２を除
去してインクジェット用ノズル振動板１３を得る（文献
不詳）。2. Description of the Related Art Conventionally, for example, an ink jet nozzle diaphragm is generally made by etching. At the time of etching, as shown in FIG.
Polyimide 11 on the back side of S material 10 (15 to 20 μm thick)
And then patterning a resist film 12 on the surface of the SUS material 10 as shown in FIG.
Then, an etching process is performed as shown in FIG.
Finally, the resist film 12 is removed to obtain an inkjet nozzle vibrating plate 13 as shown in FIG.
【０００３】[0003]
【発明が解決しようとする課題】しかるに、ポリイミド
１１をベース材として使用すると、金属に比べて耐久性
に劣り、ＳＵＳ材１０との密着もあまり良くない。ま
た、エッチング時にダレが発生し易く、高精度な形状の
ものが得難い。そこで、本発明者達は、耐久性に優れ、
また高精度なインクジェット用ノズル振動板を得ること
を期してニッケル電鋳でそれを作ることを試みた。ベー
ス材として第１ニッケル層を通常の光沢ニッケル浴で１
次電鋳で形成し、ついで、その第１ニッケル層の表面に
フォトレジスト膜をパターンニング形成した後、第１ニ
ッケル層のフォトレジスト膜で覆われていない表面に第
２ニッケル層を２次電鋳する試みである。However, when the polyimide 11 is used as the base material, the durability is inferior to that of metal and the adhesion with the SUS material 10 is not so good. In addition, sagging easily occurs during etching, and it is difficult to obtain a highly precise shape. Therefore, the present inventors have excellent durability,
In addition, in order to obtain a highly accurate nozzle diaphragm for inkjet, we tried to make it by nickel electroforming. 1st nickel layer as a base material in a normal bright nickel bath
Then, a photoresist film is patterned on the surface of the first nickel layer, and then a second nickel layer is formed on the surface of the first nickel layer which is not covered by the photoresist film. It is an attempt to cast.
【０００４】しかし、第１ニッケル層と第２ニッケル層
は密着しにくく、剥がれ易かった。これはベース材とし
て第１ニッケル層を光沢ニッケル浴で電鋳することに原
因があることを確認した。この理由については定かでな
いが、そのひとつとして考えられるのは、ブチンジオー
ル、あるいはサッカリンやＮＴＳなどの光沢剤を添加し
たスルファミン酸ニッケル浴でベース材の第１ニッケル
層を１次電鋳した場合は、その第１ニッケル層にイオウ
やカーボンの含有量が多くなるため、１次電鋳後２次電
鋳するまでの間に、その表面に酸化皮膜ができたり、ア
ルカリ現像液などの薬品付着などで第１ニッケル層の表
面状態が変化する。そのため、その第１ニッケル層の表
面に対し第２ニッケル層が組成的に密着しにくくなるも
のと考えられる。そのほかに、第１ニッケル層の光沢表
面の結晶がち密になるため、第２ニッケル層が物理的に
も密着しにくいかと考えられる。However, the first nickel layer and the second nickel layer were difficult to adhere to each other and were easily peeled off. It was confirmed that this was due to electroforming the first nickel layer as a base material in a bright nickel bath. The reason for this is not clear, but one of the possible reasons is that when the primary nickel layer of the base material is subjected to primary electroforming in a nickel sulfamate bath containing butynediol or a brightener such as saccharin or NTS. Since the first nickel layer contains a large amount of sulfur and carbon, an oxide film may be formed on the surface of the first nickel layer between the first electroforming and the second electroforming, and chemicals such as alkaline developer may be attached. The surface condition of the first nickel layer changes. Therefore, it is considered that the second nickel layer is compositionally difficult to adhere to the surface of the first nickel layer. In addition, since the crystals on the glossy surface of the first nickel layer are densely packed, it is considered that the second nickel layer is hard to physically adhere.
【０００５】本発明は、こうした点に鑑みてなされたも
ので、ニッケル層相互間の密着性に優れるニッケル積層
体並びにその製造方法を提供せんとするものである。The present invention has been made in view of these points, and an object thereof is to provide a nickel laminate having excellent adhesion between nickel layers and a method for producing the same.
【０００６】[0006]
【課題を解決するための手段】本発明のニッケル積層体
は、１次電鋳された第１ニッケル層１の表面に、所定パ
ターンを持つ第２ニッケル層２を２次電鋳してなり、第
１ニッケル層１は光沢剤を添加しない無光沢ニッケルで
形成してなるものである。A nickel laminate of the present invention is obtained by secondary electroforming a second nickel layer 2 having a predetermined pattern on the surface of a primary electroformed first nickel layer 1. The first nickel layer 1 is made of matte nickel to which no brightener is added.
【０００７】本発明のニッケル積層体を製造するに際し
ては、電鋳母型３の表面に無光沢ニッケル浴で第１ニッ
ケル層１を１次電鋳する工程と、第１ニッケル層１の表
面にフォトレジスト膜６をパターンニング形成する工程
と、第１ニッケル層１のフォトレジスト膜６で覆われて
いない表面に第２ニッケル層２を２次電鋳する工程と、
電鋳母型３から第１ニッケル層１を第２ニッケル層２ご
と剥離する工程とからなる。In the production of the nickel laminate of the present invention, a step of primary electroforming the first nickel layer 1 on the surface of the electroforming mold 3 with a matte nickel bath, and a step of forming the first nickel layer 1 on the surface A step of patterning the photoresist film 6, and a step of secondarily electroforming the second nickel layer 2 on the surface of the first nickel layer 1 which is not covered with the photoresist film 6.
And a step of peeling the first nickel layer 1 together with the second nickel layer 2 from the electroforming mold 3.
【０００８】ここで、肝要なことは、第１ニッケル層１
を無光沢ニッケル電鋳で形成することで、第２ニッケル
層２は光沢ニッケルあるいは無光沢ニッケルのいずれの
電鋳で形成するかは任意である。ここに、光沢剤を添加
しない無光沢ニッケルとは、建浴後に意図的に光沢剤を
添加しないことを意味し、浴に不純物としてカーボンが
入っている場合その許容範囲は0.０１２％以下とする。
それ以上含まれると、光沢ニッケルで第１ニッケル層を
形成する場合と同様に良好な密着性が得られないからで
ある。Here, it is important that the first nickel layer 1
It is arbitrary whether the second nickel layer 2 is formed by electroforming of bright nickel or dull nickel by electroforming of dull nickel. Here, matte nickel with no brightener added means that no brightener is intentionally added after the construction bath, and when carbon is contained as an impurity in the bath, the allowable range is 0.012% or less. To do.
This is because if it is contained more than that, good adhesion cannot be obtained as in the case of forming the first nickel layer with bright nickel.
【０００９】[0009]
【作用】無光沢ニッケルで電鋳される第１ニッケル層１
は光沢ニッケルで形成されるものよりも表面の結晶が粗
く、梨地状になり、第２ニッケル層２が物理的に強固に
密着し易くなる。また、第１ニッケル層１を無光沢ニッ
ケルで電鋳すると、カーボンやイオウの含有量が僅少で
あるか、全く含まないため、第１ニッケル層１の表面状
態の変化が少なく、組成的にも第２ニッケル層２との密
着力を高めることができる。Function: First nickel layer 1 electroformed with matte nickel
Has a crystal on the surface that is rougher than that formed by bright nickel, and has a satin-like texture, and the second nickel layer 2 is likely to be physically and firmly adhered. Further, when the first nickel layer 1 is electroformed with matte nickel, the content of carbon or sulfur is very small or not contained at all, so that the surface condition of the first nickel layer 1 is not significantly changed, and the composition is also improved. The adhesion with the second nickel layer 2 can be enhanced.
【００１０】[0010]
【実施例】図１は本発明の対象とするニッケル積層体を
示しており、ベース材となる第１ニッケル層１の表面に
所定パターンを持つ第２ニッケル層２を積層してなる。
このようなニッケル積層体の電鋳法の一例を図２の
（Ａ）ないし（Ｇ）に基づき説明する。まず、電鋳母型
３を無光沢ニッケル浴の電解液に浸漬して該母型３の表
面に１次電鋳を行う。この無光沢ニッケル浴の組成とメ
ッキ条件を次に示す。 スルファミン酸ニッケル ４５０ｇ／ｌ ホウ酸 ３０ｇ／ｌ ｐＨ ４〜4.５ 浴温 ５０℃ 電流密度 ２Ａ／ｄｍ2 〜７Ａ／ｄｍ2 以上の浴にて電鋳を行うことにより、図２の（Ａ）に示
すように、電鋳母型３の表面に第１ニッケル層１を形成
する。この第１ニッケル層１の厚みは、例えば１５μ程
度にする。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows a nickel laminated body to which the present invention is applied, in which a second nickel layer 2 having a predetermined pattern is laminated on the surface of a first nickel layer 1 serving as a base material.
An example of the electroforming method of such a nickel laminated body will be described with reference to FIGS. First, the electroforming mother die 3 is immersed in an electrolytic solution of a matte nickel bath to perform primary electroforming on the surface of the mother die 3. The composition and plating conditions of this matte nickel bath are shown below. Nickel sulfamate 450 g / l Boric acid 30 g / l pH 4 to 4.5 Bath temperature 50 ° C. Current density 2 A / dm 2 to 7 A / dm By performing electroforming in a bath of 2 or more, (A) of FIG. As shown in FIG. 1, the first nickel layer 1 is formed on the surface of the electroforming mold 3. The thickness of this first nickel layer 1 is, eg, about 15 μm.
【００１１】ついで、この第１ニッケル層１を付けた電
鋳母型３を上記浴より引き上げ、同図の（Ｂ）に示すご
とく第１ニッケル層１の表面にネガタイプのフォトレジ
スト４を均一に塗布して乾燥させるか、またはラミネー
トする。ついで、そのレジスト４の上に同図の（Ｃ）に
示すごとく所望のパターンに対応するネガタイプフイル
ム５を密着させ、焼き付け、現像の各処理を行って、同
図の（Ｄ）に示すごとく所望パターンのフォトレジスト
膜６を形成する。勿論、上記フォトレジスト４として
は、ネガタイプのものに代えて、ポジタイプのものであ
ってもよい。Then, the electroforming mold 3 having the first nickel layer 1 attached thereto is lifted from the bath, and a negative type photoresist 4 is uniformly formed on the surface of the first nickel layer 1 as shown in FIG. Apply and dry or laminate. Then, a negative type film 5 corresponding to a desired pattern is brought into close contact with the resist 4 as shown in (C) of the figure, and each process of baking and developing is performed to obtain the desired pattern as shown in (D) of the figure. A patterned photoresist film 6 is formed. Of course, the photoresist 4 may be a positive type instead of the negative type.
【００１２】ついで、このフォトレジスト膜６が形成さ
れた電鋳母型３を、光沢ニッケル浴に移して２次電鋳を
行う。この光沢ニッケル浴の組成とメッキ条件を次に示
す。 スルファミン酸ニッケル ４５０ｇ／ｌ ブチンジオール 0.００５〜0.０１ｇ／ｌ ＮＴＳ 0.０１〜0.０５ｇ／ｌ ホウ酸 ３０ｇ／ｌ ｐＨ ４〜4.５ 浴温 ５０℃ 以上の浴にて電流密度２Ａ／ｄｍ2 〜７Ａ／ｄｍ2 で電
鋳を行うことにより、同図の（Ｅ）に示すごとく第１ニ
ッケル層１のフォトレジスト膜６で覆われていない表面
に、第２ニッケル層２を形成する。この第２ニッケル層
２の厚みは３０μ程度とする。Then, the electroforming mold 3 having the photoresist film 6 formed thereon is transferred to a bright nickel bath for secondary electroforming. The composition and plating conditions of this bright nickel bath are shown below. Nickel sulfamate 450 g / l Butynediol 0.005 to 0.01 g / l NTS 0.01 to 0.05 g / l Boric acid 30 g / l pH 4 to 4.5 Bath temperature 50A or above Current density 2A / Dm 2 to 7 A / dm 2 , electroforming is performed to form the second nickel layer 2 on the surface of the first nickel layer 1 not covered with the photoresist film 6 as shown in FIG. To do. The thickness of the second nickel layer 2 is about 30 μm.
【００１３】この第２ニッケル層２の電鋳後、フォトレ
ジスト膜６を除去し、同図の（Ｆ）に示すごとく電鋳母
型３から第１ニッケル層１を第２ニッケル層２ごと剥離
する。かくして、同図の（Ｇ）および図２に示すごとき
ニッケル積層体電鋳製品が得られる。After the electroforming of the second nickel layer 2, the photoresist film 6 is removed, and the first nickel layer 1 is peeled off together with the second nickel layer 2 from the electroforming mold 3 as shown in FIG. To do. Thus, a nickel laminate electroformed product as shown in FIG. 2G and FIG. 2 is obtained.
【００１４】このようにして得られたニッケル積層体の
第１・第２ニッケル層１・２相互間の密着強さをテスト
してみた。すなわち、このニッケル積層体に振動を加え
てみたが、光沢ニッケルで形成する第１ニッケル層と第
２ニッケル層の積層体のごとき第２ニッケル層２が第１
ニッケル層１から剥がれるようなことがなく、完全に密
着していた。また、ニッケル積層体を第１ニッケル層１
側に折り曲げて第１・第２ニッケル層１・２相互間の一
端に剥離応力を加えてみたが、電子顕微鏡で拡大して見
た図３に示すようにその接合部の剥がれが無く、むしろ
第１ニッケル層１の第２ニッケル層２との接合部Ｃとは
異なり、その近傍の第１ニッケル層１の第２ニッケル層
２で覆われていない露出表面部の箇所Ｄが引きちぎれる
様な破壊状態が認められ、ニッケル層１・２相互間がい
かに強く密着しているかがよく判った。The adhesion strength between the first and second nickel layers 1 and 2 of the nickel laminated body thus obtained was tested. That is, although vibration was applied to this nickel laminated body, the second nickel layer 2 such as a laminated body of the first nickel layer and the second nickel layer formed of bright nickel is
It did not peel off from the nickel layer 1, and it was in perfect contact. In addition, the nickel laminate is used as the first nickel layer 1
It was bent to the side and a peeling stress was applied to one end between the first and second nickel layers 1 and 2, but there was no peeling of the joint as shown in FIG. Unlike the joint portion C of the first nickel layer 1 with the second nickel layer 2, the portion D of the exposed surface portion of the first nickel layer 1 which is not covered with the second nickel layer 2 in the vicinity thereof is torn off. A fractured state was recognized, and it was clearly understood how strongly the nickel layers 1 and 2 were closely attached.
【００１５】第２ニッケル層２は光沢ニッケルあるいは
無光沢ニッケルのいずれの電鋳で形成しても、第１ニッ
ケル層１との密着性に優れるが、上記実施例のように第
２ニッケル層２をブチンジオールを添加する光沢ニッケ
ル浴で電鋳した場合は、腐食環境においてイオウを含む
第２ニッケル層２がイオウを含まない第１ニッケル層１
に対してアノードとして作用し、腐食は第２ニッケル層
２で止まるため耐蝕性を向上させることができる。Although the second nickel layer 2 is formed by electroforming either bright nickel or dull nickel, it has excellent adhesion to the first nickel layer 1, but as in the above-mentioned embodiment, the second nickel layer 2 is formed. When electroforming is carried out in a bright nickel bath containing butynediol, the second nickel layer 2 containing sulfur is the first nickel layer 1 containing no sulfur in a corrosive environment.
On the other hand, it acts as an anode, and the corrosion stops at the second nickel layer 2, so that the corrosion resistance can be improved.
【００１６】なお、第２ニッケル層２は通常、上記のご
とく２〜７Ａ／ｄｍ2 程度の電流密度で形成することが
多いが、好ましくは0.５〜１Ａ／ｄｍ2 の低電流密度で
第２ニッケル層２を形成すれば、電着時間は長くかかる
が、第１ニッケル層１との親和力が向上し、より一層良
好な密着性が得られる。The second nickel layer 2 is usually formed at a current density of about 2 to 7 A / dm 2 as described above, but preferably at a low current density of 0.5 to 1 A / dm 2 . If the two-nickel layer 2 is formed, the electrodeposition time will be long, but the affinity with the first nickel layer 1 will be improved, and even better adhesion can be obtained.
【００１７】[0017]
【発明の効果】本発明によれば、１次電鋳された第１ニ
ッケル層１の表面に所定パターンを持つ第２ニッケル層
２を形成してなる積層体において、その第１ニッケル層
１を光沢剤を添加しない無光沢ニッケルで形成するの
で、密着性に優れるニッケル積層体を得ることができ、
例えば、耐振動性の要求されるインクジェット用ノズル
振動板などの部品に好適に使用することができる。According to the present invention, the first nickel layer 1 is formed in the laminated body in which the second nickel layer 2 having a predetermined pattern is formed on the surface of the first electroformed first nickel layer 1. Since it is made of matte nickel without the addition of a brightener, a nickel laminate with excellent adhesion can be obtained,
For example, it can be suitably used for parts such as ink jet nozzle diaphragms that require vibration resistance.
【図１】ニッケル積層体の一部を切欠して示す斜視図で
ある。FIG. 1 is a perspective view showing a nickel laminate with a part cut away.
【図２】ニッケル積層体の電鋳工程図である。FIG. 2 is an electroforming process diagram of a nickel laminate.
【図３】ニッケル積層体の密着強さをテストしてみた状
態を示すその一部斜視図である。FIG. 3 is a partial perspective view showing a state in which the adhesion strength of the nickel laminate is tested.
【図４】従来のエッチング法によるインクジェット用ノ
ズル振動板のエッチング工程図である。FIG. 4 is an etching process diagram of an inkjet nozzle diaphragm according to a conventional etching method.
１ 第１ニッケル層 ２ 第２ニッケル層 ３ 電鋳母型 ６ フォトレジスト膜 1 First Nickel Layer 2 Second Nickel Layer 3 Electroforming Master 6 Photoresist Film
Claims (2)
に、所定パターンを持つ第２ニッケル層２を２次電鋳し
てなり、第１ニッケル層１は光沢剤を添加しない無光沢
ニッケルで形成されていることを特徴とするニッケル積
層体。1. A second nickel layer 2 having a predetermined pattern is secondarily electroformed on a surface of the first electroformed first nickel layer 1, and the first nickel layer 1 does not include a brightening agent. A nickel laminate characterized by being formed of bright nickel.
第１ニッケル層１を１次電鋳する工程と、 第１ニッケル層１の表面にフォトレジスト膜６をパター
ンニング形成する工程と、 第１ニッケル層１のフォトレジスト膜６で覆われていな
い表面に第２ニッケル層２を２次電鋳する工程と、 電鋳母型３から第１ニッケル層１を第２ニッケル層２ご
と剥離する工程とからなるニッケル積層体の製造方法。2. A step of primary electroforming the first nickel layer 1 on the surface of the electroforming mold 3 in a matte nickel bath, and a step of patterning a photoresist film 6 on the surface of the first nickel layer 1. And a step of secondary electroforming the second nickel layer 2 on the surface of the first nickel layer 1 which is not covered with the photoresist film 6, and from the electroforming mold 3 to the first nickel layer 1 to the second nickel layer 2 A method for manufacturing a nickel laminate, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16007993A JP3270948B2 (en) | 1993-06-03 | 1993-06-03 | Nickel laminate and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16007993A JP3270948B2 (en) | 1993-06-03 | 1993-06-03 | Nickel laminate and method for producing the same |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000161038A Division JP3295810B2 (en) | 1993-06-03 | 2000-05-30 | Nickel laminate and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06346271A true JPH06346271A (en) | 1994-12-20 |
| JP3270948B2 JP3270948B2 (en) | 2002-04-02 |
Family
ID=15707421
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16007993A Expired - Fee Related JP3270948B2 (en) | 1993-06-03 | 1993-06-03 | Nickel laminate and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3270948B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10172529A (en) * | 1996-12-09 | 1998-06-26 | Oputonikusu Seimitsu:Kk | Manufacture of battery explosion-proof safety piece |
| JPH1194196A (en) * | 1997-09-18 | 1999-04-09 | Oputonikusu Seimitsu:Kk | Explosion-proof safety valve for battery and manufacture therefor |
| JP2002180282A (en) * | 2000-12-20 | 2002-06-26 | Kyushu Hitachi Maxell Ltd | Electroformed metal and its manufacturing method |
| JP2002356793A (en) * | 2001-05-30 | 2002-12-13 | Kyushu Hitachi Maxell Ltd | Electrocasting metal and method of manufacturing for the same |
| JP2022551136A (en) * | 2019-10-24 | 2022-12-07 | イルジン マテリアルズ カンパニー リミテッド | Nickel foil for manufacturing thin-film capacitors and method for manufacturing same |
-
1993
- 1993-06-03 JP JP16007993A patent/JP3270948B2/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10172529A (en) * | 1996-12-09 | 1998-06-26 | Oputonikusu Seimitsu:Kk | Manufacture of battery explosion-proof safety piece |
| US6180279B1 (en) | 1996-12-09 | 2001-01-30 | Optnics Precision Co., Ltd. | Method of manufacturing battery explosion prevention safety device |
| JPH1194196A (en) * | 1997-09-18 | 1999-04-09 | Oputonikusu Seimitsu:Kk | Explosion-proof safety valve for battery and manufacture therefor |
| JP2002180282A (en) * | 2000-12-20 | 2002-06-26 | Kyushu Hitachi Maxell Ltd | Electroformed metal and its manufacturing method |
| JP4674735B2 (en) * | 2000-12-20 | 2011-04-20 | 九州日立マクセル株式会社 | Method for producing electroformed metal |
| JP2002356793A (en) * | 2001-05-30 | 2002-12-13 | Kyushu Hitachi Maxell Ltd | Electrocasting metal and method of manufacturing for the same |
| JP2022551136A (en) * | 2019-10-24 | 2022-12-07 | イルジン マテリアルズ カンパニー リミテッド | Nickel foil for manufacturing thin-film capacitors and method for manufacturing same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3270948B2 (en) | 2002-04-02 |
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