JP2573350B2 - Permanent mold for cast products made of aluminum alloy or magnesium alloy - Google Patents
Permanent mold for cast products made of aluminum alloy or magnesium alloyInfo
- Publication number
- JP2573350B2 JP2573350B2 JP1088114A JP8811489A JP2573350B2 JP 2573350 B2 JP2573350 B2 JP 2573350B2 JP 1088114 A JP1088114 A JP 1088114A JP 8811489 A JP8811489 A JP 8811489A JP 2573350 B2 JP2573350 B2 JP 2573350B2
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- mold
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- weight
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- casting
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Description
【発明の詳細な説明】 ［発明の技術分野］ 本発明は、金型の内面に合金およびセラミックを溶射
することによって金型の耐摩耗性および耐久性を改善し
たアルミニウム合金−またはマグネシウム合金製鋳造製
品用金型、特に熱伝導性のよい銅合金製金型に関する。Description: TECHNICAL FIELD OF THE INVENTION The present invention relates to a casting made of an aluminum alloy or a magnesium alloy in which the wear resistance and durability of a mold are improved by spraying an alloy and ceramic on the inner surface of the mold. The present invention relates to a product mold, particularly a copper alloy mold having good heat conductivity.
［従来技術および発明が解決しようとする課題］ 特公昭61-5819号公報から、鋳型内面にNiメッキ層を
形成しそしてその上にCo:45〜65重量％、Mo:20〜40％お
よび残部Crから成るCo-Mo-Cr合金層を溶射した連続鋳造
鋳型が公知である。この連続鋳造用鋳型を通例の不連続
鋳造、例えば低圧鋳造、重力鋳造等の為の鋳型として用
いた場合には、鋳造時にガスを排除することが充分には
できない為に、“ふかれ”（凹凸）が生じ成形体の表面
状態がわるいという欠点がある。[Prior Art and Problems to be Solved by the Invention] From JP-B-61-5819, a Ni plating layer is formed on the inner surface of a mold and Co: 45 to 65% by weight, Mo: 20 to 40% and the balance are formed. A continuous casting mold in which a Co-Mo-Cr alloy layer made of Cr is sprayed is known. When this continuous casting mold is used as a mold for ordinary discontinuous casting, for example, low-pressure casting, gravity casting, etc., gas cannot be sufficiently removed at the time of casting. However, there is a disadvantage that the surface condition of the molded article is bad.
更にこの従来技術の金型の欠点として、セラミック粉
末を含む水ガラス等でできた軟塗型剤でたびたび塗型を
する必要があることが挙げられる。その為に、その作業
上の時間的および経済的費用が甚大であり、この点にも
問題がある。A further disadvantage of this prior art mold is that it is often necessary to mold with a soft coat agent made of water glass or the like containing ceramic powder. As a result, the time and economic costs for the operation are enormous, which is also problematic.
本発明者は、これらの欠点を解決する為に、特願平1-
46621号にて、銅合金製鋳型の内面にNiメッキ層が形成
され、次いで中間層としてCo/Mo/Cr−合金被覆がそして
外側層としてAl2O3/ZrO2−多孔質セラミック被覆が設け
られ、中間層の合金の組成が45〜60重量％のCo、20〜40
重量％のMoおよび残量のCrでありそしてセラミック層の
組成が40〜60重量％、殊に55〜60重量％のAl2O3と60〜4
0重量％、殊に45〜40重量％のZrO2であることを特徴と
する、不連続鋳造用銅合金製パーマネント金型を提案し
た。The present inventor has proposed in Japanese Patent Application No.
In 46621, a Ni plating layer was formed on the inner surface of the copper alloy mold, and then a Co / Mo / Cr-alloy coating was provided as an intermediate layer and an Al 2 O 3 / ZrO 2 -porous ceramic coating was provided as an outer layer. The composition of the alloy of the intermediate layer is 45-60% by weight of Co, 20-40% by weight.
Wt% of Mo and the balance is of Cr and composition of the ceramic layer is 40 to 60 wt%, preferably 55-60% Al 2 O 3 and 60-4
0 wt%, in particular, characterized in that 45 to 40 by weight% of ZrO 2, has proposed a copper alloy permanent mold for discontinuous casting.
本発明者は更に鋭意研究した結果、上述の従来技術の
欠点を有さず且つ、上記特願平1-46621号に記載の場合
よりも更に合金被覆層およびセラミック層との金型本体
との密着性が良いアルミニウム合金−またはマグネシウ
ム合金製鋳造製品用パーマネント金型を開発することに
成功した。As a result of further intensive studies, the present inventor did not have the above-mentioned disadvantages of the prior art and furthermore, compared with the case described in the above-mentioned Japanese Patent Application No. 1-46621, with an alloy coating layer and a ceramic layer and a mold body. We have succeeded in developing a permanent mold for cast products made of aluminum alloy or magnesium alloy with good adhesion.
［発明の構成］ 本発明は、NiメッキされたまたはNiメッキされていな
い鋳型の内壁にNiをベースとする合金被覆が形成されそ
してそして更にその上にジルコニヤをベースとするセラ
ミック被覆が設けられ、上記合金被覆層の組成が40〜60
重量％のNi、20〜40重量％のCo、15〜25重量％のCrおよ
び0.1〜１重量％のＹでありそして上記セラミック層の
組成が約２〜10％のイットリア（Y2O3）と残量のジルコ
ニア（ZrO2）であることを特徴とする、アルミニウム合
金−またはマグネシウム合金製鋳造製品用パーネント金
型に関する。SUMMARY OF THE INVENTION The present invention provides a Ni-plated or non-Ni-plated mold having an inner wall formed with a Ni-based alloy coating and further provided with a zirconia-based ceramic coating thereon. The composition of the alloy coating layer is 40-60
Wt% of Ni, 20 to 40 wt% of Co, 15-25% Cr and 0.1-1% by weight of Y a and then the composition of the ceramic layer is about 2-10% of yttria (Y 2 O 3) and characterized in that it is a balance zirconia (ZrO 2), aluminum alloy - about or a magnesium alloy casting product for Panento mold.
本発明で使用する金型は、鋳鉄（FC）および鋼材鉄
（FCD）製でも銅合金製でもよく、特に適度の強度を有
し且つ４以上の熱伝導率を有する良熱伝導性銅合金を用
いるのが有利である。銅合金は、例えば、“金属データ
ブック”、日本金属学会編、丸善株式会社発行、昭和49
年７月20日に記載されている如き、銅に種々の非鉄金属
を希少量混入することによって強度を増し且つ適当な熱
伝導率を保持したものである。例えば、0.05〜１％の僅
かな量のSn、Zr、Zn、Si、Be、CrおよびTiの群の内の少
なくとも一種類を含有する銅合金がこれに当たる。本発
明では、0.15重量％のZr、0.85重量％のCr、0.2重量％
のTiまたは0.15重量％のZrと0.85重量％のCrとを含有す
る銅合金が特に有利である。The mold used in the present invention may be made of cast iron (FC) and steel iron (FCD) or a copper alloy. Particularly, a good heat conductive copper alloy having a moderate strength and a heat conductivity of 4 or more is used. It is advantageous to use it. Copper alloys are described in, for example, “Metal Data Book”, edited by The Japan Institute of Metals, published by Maruzen Co., Ltd., Showa 49
As described on July 20, 2005, copper is mixed with a small amount of various non-ferrous metals to increase strength and maintain appropriate thermal conductivity. For example, a copper alloy containing a small amount of 0.05 to 1% of at least one of the group of Sn, Zr, Zn, Si, Be, Cr and Ti is applicable. In the present invention, 0.15% by weight of Zr, 0.85% by weight of Cr, 0.2% by weight
Particularly preferred are copper alloys containing 0.15% by weight of Zr and 0.85% by weight of Cr.
銅合金金型の場合には、銅合金は一般に軟化点が低い
ので、Niメッキを前もって施し、Niベースの合金を溶射
する際に掛かる熱により銅合金の軟化を防止する必要が
ある。鋼鉄製の金型の場合には、鋼鉄自体の軟化点が高
い為に、このNiメッキ層を設ける必要がない。In the case of a copper alloy mold, since the copper alloy generally has a low softening point, it is necessary to apply Ni plating in advance to prevent the copper alloy from softening due to heat applied when spraying the Ni-based alloy. In the case of a steel mold, there is no need to provide this Ni plating layer because the softening point of the steel itself is high.
更に銅合金金型の場合にはこのNiメッキ層が、次に被
覆形成されるNiベース被覆層の溶射による密着をより強
固にするのに役立つ。このNiメッキ層は、Niベース合金
の溶射の際にその合金が銅合金にまで達しない程の厚さ
が必要である。一般には、50〜300μｍの厚さであるの
が好ましい。Further, in the case of a copper alloy mold, this Ni plating layer serves to further strengthen the adhesion by thermal spraying of the Ni base coating layer formed next. The Ni plating layer needs to have such a thickness that the alloy does not reach the copper alloy when the Ni base alloy is sprayed. Generally, a thickness of 50 to 300 μm is preferred.
Niベース合金は40〜60重量％のNi、20〜40重量％のC
o、15〜25重量％のCrおよび0.1〜１重量％のＹで組成さ
れており、これらの成分をかゝる割合で混合溶融しそし
て微細粉砕することによって得ることによって粉末状で
溶射する。このNiベース合金層は、鋼鉄製金型および銅
合金金型の場合のNiメッキ層並びに後続のセラミック層
との密着性を持ちそして金型内面に強度を与え、結果的
に鋳型の耐久性および耐摩耗性を高める働きをする。こ
の層は一般に50〜600μｍの厚さであるのが好ましい。Ni-based alloy is 40-60 wt% Ni, 20-40 wt% C
o, composed of 15 to 25% by weight of Cr and 0.1 to 1% by weight of Y, and sprayed in powder form by mixing and melting these components in such proportions and obtaining them by fine grinding. This Ni-based alloy layer has adhesion to the Ni plating layer and subsequent ceramic layers in the case of steel molds and copper alloy molds and provides strength to the mold inner surface, resulting in mold durability and durability. Works to increase wear resistance. This layer is generally preferably between 50 and 600 μm thick.
セラミック層は、約２〜10重量％のイットリアと残量
のジルコニヤで組成されており、多孔質であることに起
因して鋳造時にガスを排除する働きをする他に、鋳型の
耐熱性および耐久性を著しく向上させる働きもする。イ
ットリアの量が上記の範囲より少なくとも多くともセラ
ミック層の強度並びに合金層との密着性が悪くなる。こ
の層の厚さは一般に50〜500μｍであるのが好ましい。The ceramic layer is composed of about 2 to 10% by weight of yttria and the remaining amount of zirconia. In addition to the function of eliminating gas during casting due to being porous, the heat resistance and durability of the mold are also increased. Also works to significantly improve the properties. If the amount of yttria is at least larger than the above range, the strength of the ceramic layer and the adhesion to the alloy layer are deteriorated. The thickness of this layer is generally preferably between 50 and 500 μm.
本発明に従う鋳造用銅合金製金型の有利な製造例を以
下に説明する。最初に下記表に記載の銅合金（表中の各
合金の残量成分は全て銅である）より成る銅合金製金型
の内面にNiメッキ層を50〜300μｍ、殊に100〜200μｍ
の厚さで通例の方法で形成し、必要に応じて型内部水冷
装置により水で冷却しながらNiメッキ層の上に上述の合
金組成のNi/Co/Cr/Y合金を約10,000〜約5,000℃でプラ
ズマ溶射または約2,700℃でジェットコートによって50
〜600μｍ、殊に200〜300μｍの厚さで被覆する。次い
で上述の組成のセラミック被覆層を同様な条件の溶射法
によって50〜500μｍ、殊に200〜300μｍの厚さに溶射
する。セラミック層には沢山の連続孔が生じ、これがセ
ラミック層を多孔質にしている。この多孔質の孔は成形
体の表面に凹凸を生じさせる程の大きさではなく、顕微
鏡にて見ることができる程のものである。An advantageous production example of the copper alloy mold for casting according to the present invention will be described below. First, a Ni plating layer is formed on the inner surface of a copper alloy mold made of a copper alloy described in the following table (all of the remaining components of the alloy are copper) by 50 to 300 μm, particularly 100 to 200 μm.
It is formed in a conventional manner with a thickness of about 10,000 to about 5,000 with a Ni / Co / Cr / Y alloy having the above-mentioned alloy composition on the Ni plating layer while being cooled with water by a mold internal water cooling device as necessary. 50 ° C by plasma spraying or jet coating at about 2,700 ° C
It is coated with a thickness of .about.600 .mu.m, in particular 200-300 .mu.m. Next, the ceramic coating layer having the above composition is sprayed to a thickness of 50 to 500 μm, particularly 200 to 300 μm by the spraying method under the same conditions. The ceramic layer has a number of continuous pores which make the ceramic layer porous. The porous pores are not large enough to cause irregularities on the surface of the molded body, but are small enough to be seen with a microscope.
本発明の合金製金型は、連続孔よりなる多孔質セラミ
ック層を有しており、この連続孔が鋳造の際に発生する
ガスを収容し且つ外部に導き出す働きをするので、成形
体の表面にガスによる害を及ぼすことがない。即ち、ふ
かれ（凹凸）の発生がない。 The alloy mold of the present invention has a porous ceramic layer composed of continuous holes, and the continuous holes serve to receive gas generated at the time of casting and to guide the gas to the outside. The gas is not harmed. That is, there is no occurrence of wiping (unevenness).
セラミック層を有する本発明の鋳型は、高い耐久性お
よび耐摩耗性を有しており、軟塗型剤を鋳型内面に塗布
する必要なしに、従来の型に比較して非常に多いショッ
ト数、例えば30,000ショット以上の鋳造にも耐え得る。The mold of the present invention having a ceramic layer has high durability and abrasion resistance, and requires a very large number of shots as compared with the conventional mold without the need to apply a soft coating mold to the inner surface of the mold. For example, it can withstand casting of 30,000 shots or more.
本発明のアルミニウム合金−またはマグネシウム合金
鋳造製品用パーマネント金型は、アルミニウム合金やマ
グネシウム合金の鋳造だけでなく、合成樹脂や他の金属
の鋳造にも使用できる。The permanent mold for an aluminum alloy or magnesium alloy casting product of the present invention can be used not only for casting an aluminum alloy or a magnesium alloy, but also for casting a synthetic resin or other metal.
本発明を実施例および比較例によって以下に更に詳細
に説明する。The present invention will be described in more detail below with reference to examples and comparative examples.
実施例１ 0.15重量％のジルコニウムを含有し、熱伝導率７の銅
合金で製造した金型の内面に、電気メッキ法によって20
0μｍの厚さのNiメッキ層を設ける。次いでプラズマ溶
射法によって44.55重量％のNi、35重量％のCo、20重量
％のCrおよび0.45重量％のＹより成る溶融粉砕粉末合金
を8000℃で溶射して150μｍの被覆膜を形成する。Example 1 An inner surface of a mold made of a copper alloy containing 0.15% by weight of zirconium and having a thermal conductivity of 7 was coated by electroplating with a metal plating method.
A Ni plating layer having a thickness of 0 μm is provided. Next, a melt-pulverized powder alloy composed of 44.55% by weight of Ni, 35% by weight of Co, 20% by weight of Cr and 0.45% by weight of Y is sprayed at 8000 ° C. by plasma spraying to form a 150 μm coating film.
このようにして形成されたNi/Co/Cr/Y合金被覆層の上
に、同様な溶射法によって92重量％のジルコニヤと８重
量％のイットリアとより成るセラミック粉末を250μｍ
の厚さで被覆する。その際の溶射温度は8000℃である。
セラミック層には非常に小さい沢山の孔が存在し、多孔
質と成っている。On the Ni / Co / Cr / Y alloy coating layer thus formed, a ceramic powder composed of 92% by weight of zirconia and 8% by weight of yttria was coated by a similar thermal spraying method to a thickness of 250 μm.
To a thickness of The spraying temperature at that time is 8000 ° C.
The ceramic layer has many very small holes and is porous.
この様にして製造された銅合金製パーマネント金型
を、350〜400℃に冷却しながら自動車エンジンのマグネ
シウム合金ケーシングの鋳造に用いたところ、30,000シ
ョット行っても、未だ表面に変化がなく、成形体の表面
状態も良好であった。When the copper alloy permanent mold manufactured in this way was used for casting a magnesium alloy casing of an automobile engine while cooling to 350 to 400 ° C., even after 30,000 shots, there was no change in the surface, and the molding was still performed. The surface condition of the body was also good.
実施例２ 0.2重量％Tiを含有し且つ熱伝導率が６の銅合金より
成る金型を使用し、溶射される合金層が50重量％のNi、
31重量％のCo、18.55重量％のCrおよび0.45重量％のＹ
より成りそしてセラミック層が96重量％のジルコニヤ粉
末と４重量％のイットリアとより成ることを除いて、実
施例１と同様いパーマネット金型を製造した。この金型
で自動車エンジン用のアルミニウム合金ケーシングを鋳
造する鋳造実験を実施例１と同様に行ったところ、30,0
00ショット行っても、未だ表面に変化がなく、成形体の
表面状態も良好であった。Example 2 A mold made of a copper alloy containing 0.2 wt% Ti and having a thermal conductivity of 6 was used, and the sprayed alloy layer was 50 wt% Ni,
31% by weight Co, 18.55% by weight Cr and 0.45% by weight Y
A permanet mold similar to that of Example 1 was made except that the ceramic layer consisted of 96% by weight zirconia powder and 4% by weight yttria. A casting experiment of casting an aluminum alloy casing for an automobile engine with this mold was performed in the same manner as in Example 1.
Even after the 00 shot, the surface did not change, and the surface condition of the molded body was good.
実施例３ 0.15重量％のZrと0.85重量％のCrとを含有する熱伝導
率５の銅合金より成る金型を使用しそして溶射される合
金層が57.55重量％のNi、25重量％のCo、17重量％のCr
および0.45重量％のＹより成ることを除いて、実施例１
と同様にパーマネット金型を製造しそして同様な鋳造実
験を行った。Example 3 A mold made of a copper alloy with a thermal conductivity of 5 containing 0.15% by weight of Zr and 0.85% by weight of Cr was used and the sprayed alloy layer was 57.55% by weight of Ni, 25% by weight of Co , 17 wt% Cr
Example 1 with the exception that it consists of
A permanet mold was manufactured as in Example 1 and a similar casting experiment was performed.
実施例１におけるのと同等の結果が得られた。 The same results as in Example 1 were obtained.
実施例４ 鋼鉄製金型を使用し、これに直接的にプラズマ溶射法
によって44.55重量％のNi、35 重量％のCo、20重量％
のCrおよび0.45重量％のＹより成る溶融粉砕粉末合金を
8000℃で溶射して150μｍの被覆膜を形成する。Example 4 Using a steel mold, directly by plasma spraying, 44.55% by weight of Ni, 35% by weight of Co, 20% by weight
Powdered alloy consisting of Cr and 0.45 wt% Y
Thermal spraying at 8000 ° C. to form a 150 μm coating film.
このようにして形成されたNi/Co/Cr/Y合金被覆層の上
に、同様な溶射法によって92重量％のジルコニヤと８重
量％のイットリアとより成るセラミック粉末を250μｍ
の厚さで被覆する。On the Ni / Co / Cr / Y alloy coating layer thus formed, a ceramic powder composed of 92% by weight of zirconia and 8% by weight of yttria was coated by a similar thermal spraying method to a thickness of 250 μm.
To a thickness of
この様にして製造された鋼鉄製パーマネント金型を、
エンジンのシリンダーヘッドの鋳造に用いたところ、10
0,000ショット行っても、未だ表面に変化がなく、成形
体の表面状態も良好であった。The steel permanent mold manufactured in this way is
When used to cast engine cylinder heads, 10
Even after performing 000 shots, there was no change in the surface, and the surface condition of the molded body was good.
比較例 セラミック層を設けない点を除いて、実施例１と同様
にして金型を製造し、実施例１と同様に試験した。Comparative Example A mold was manufactured in the same manner as in Example 1 except that the ceramic layer was not provided, and was tested in the same manner as in Example 1.
この金型の場合には、200ショット毎に市販の塗型剤
（セラミックを水ガラスに練込んだもの）にて塗型をし
ながら8,000ショットを行ったところ、金型表面に歪み
や亀裂が生じ、使用できない状態となった。また3,000
ショット頃から成形体の表面状態が悪くなった。In the case of this mold, when performing 8,000 shots while performing coating with a commercially available coating agent (ceramic kneaded in water glass) every 200 shots, distortion and cracks were observed on the mold surface. And became unusable. Also 3,000
From the time of the shot, the surface condition of the molded body deteriorated.
［発明の効果］ 本発明の金型は、鋼鉄製金型の場合に優れた耐摩耗性
および耐久性が達成されることは言うまでもないが、銅
合金製金型の場合にも従来の銅合金製金型と比べて、銅
合金の良好な熱伝導性およびそれ故の容易な温度制御性
を有しながら、塗型を行う煩雑さが省略でき、極端に長
い寿命を示すと言う優れた効果を示し、産業への貢献は
顕著なものである。[Effect of the Invention] It goes without saying that the mold of the present invention achieves excellent wear resistance and durability in the case of a steel mold, but also in the case of a copper alloy mold, Compared to mold making, it has the excellent thermal conductivity of copper alloy and hence the easy temperature controllability. The contribution to the industry is remarkable.
Claims (1)
い鋳型の内壁にNiをベースとする合金被覆が形成されて
おりそして更にその上にジルコニアをベースとするセラ
ミック被覆層が設けられており、上記合金被覆層の組成
が40〜60重量％のNi、20〜40重量％のCo、15〜25重量％
のCrおよび0.1〜１重量％のＹでありそして上記セラミ
ック層の組成が約２〜10重量％のイットリア（Y2O3）と
残量のジルコニア（ZrO2）であることを特徴とする、ア
ルミニウム合金−またはマグネシウム合金製鋳造製品用
パーマネント金型。1. A Ni-based or non-Ni-plated mold having an inner wall formed with an Ni-based alloy coating and further provided thereon with a zirconia-based ceramic coating layer. The composition of the alloy coating layer is 40-60 wt% Ni, 20-40 wt% Co, 15-25 wt%
Wherein the composition of a Cr and 0.1-1% by weight of Y and the ceramic layer is from about 2 to 10 wt% of yttria (Y 2 O 3) and the balance zirconia (ZrO 2), Permanent mold for cast products made of aluminum alloy or magnesium alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1088114A JP2573350B2 (en) | 1989-04-10 | 1989-04-10 | Permanent mold for cast products made of aluminum alloy or magnesium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1088114A JP2573350B2 (en) | 1989-04-10 | 1989-04-10 | Permanent mold for cast products made of aluminum alloy or magnesium alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02270953A JPH02270953A (en) | 1990-11-06 |
| JP2573350B2 true JP2573350B2 (en) | 1997-01-22 |
Family
ID=13933863
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1088114A Expired - Fee Related JP2573350B2 (en) | 1989-04-10 | 1989-04-10 | Permanent mold for cast products made of aluminum alloy or magnesium alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2573350B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05132752A (en) * | 1991-06-13 | 1993-05-28 | T-P Kogyo Kk | Method for thermally spraying ceramic on casting mold |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6213236A (en) * | 1985-07-11 | 1987-01-22 | Honda Motor Co Ltd | Metallic mold for casting and its production |
| JPS62103314A (en) * | 1985-10-28 | 1987-05-13 | Yoshikawa Kogyo Co Ltd | Manufacture of transfer roll for heat treating furnace |
| JPS62210330A (en) * | 1986-03-10 | 1987-09-16 | Matsushita Electric Ind Co Ltd | Gas range |
| JPS62210329A (en) * | 1986-03-12 | 1987-09-16 | Hitachi Ltd | Ceramic coated heat-resistant material and manufacture thereof |
| JPH02267253A (en) * | 1989-04-06 | 1990-11-01 | Sugitani Kinzoku Kogyo Kk | Permanent metal mold for casting |
-
1989
- 1989-04-10 JP JP1088114A patent/JP2573350B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02270953A (en) | 1990-11-06 |
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