JPH05311424A - Sputtering target for forming thin metal film and its production - Google Patents
Sputtering target for forming thin metal film and its productionInfo
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- JPH05311424A JPH05311424A JP11895392A JP11895392A JPH05311424A JP H05311424 A JPH05311424 A JP H05311424A JP 11895392 A JP11895392 A JP 11895392A JP 11895392 A JP11895392 A JP 11895392A JP H05311424 A JPH05311424 A JP H05311424A
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- purity
- thin film
- weight
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、例えば電機配線として
使用する金属薄膜をスパッタリング法によって形成する
場合等に適した金属薄膜形成用スパッタリング・ターゲ
ット並びにその製造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 a sputtering target for forming a metal thin film suitable for forming a metal thin film used for electrical wiring by a sputtering method and a method for manufacturing the same.
【０００２】[0002]
【従来の技術】これまで、ＬＳＩ等の半導体素子では、
配線材料として、Ａｌ（アルミニウム）合金が広く使用
されてきた。また、衛生放送や自動車通信等の普及によ
り需要が高まった高周波用ハイブリッドＩＣの分野で
は、高速信号処理や配線の高密度化といった要求のため
に、配線長の短縮化や薄膜技術の利用による配線の微細
化，高精度化が必要とされており、この高周波用ハイブ
リッドＩＣの内部配線等には、低抵抗配線材料であるＣ
ｕ（銅）の薄膜が広く使用されている。2. Description of the Related Art Up to now, in semiconductor elements such as LSI,
Al (aluminum) alloy has been widely used as a wiring material. Further, in the field of high-frequency hybrid ICs, which have been in high demand due to the spread of satellite broadcasting and automobile communication, due to the demands for high-speed signal processing and high-density wiring, the wiring length is shortened and wiring by using thin film technology is used. It is necessary to miniaturize and improve the precision of the high-frequency hybrid IC.
A thin film of u (copper) is widely used.
【０００３】なお、Ｃｕの薄膜は、通常、純度９９．９
９％の純銅を用いて形成するが、ＳｉＯ2 等の素子基板
に対する付着強度が弱いことから、従来では、予め基板
上にＣｒ（クロム）の薄膜を形成しておいて、そのＣｒ
膜の上にＣｕの薄膜を成膜することとしている。また、
電気配線として使用する金属薄膜の形成には、旧来から
の印刷技術だけでなく、配線材料による成形体をターゲ
ットとして使うスパッタリング法なども応用されるよう
になってきた。The Cu thin film usually has a purity of 99.9.
It is formed by using pure copper of 9%, but since the adhesion strength of the element substrate such as SiO 2 is weak, conventionally, a thin film of Cr (chrome) is previously formed on the substrate and the Cr
A Cu thin film is formed on the film. Also,
In order to form a metal thin film used as an electric wiring, not only the conventional printing technique but also a sputtering method using a molded body made of a wiring material as a target have come to be applied.
【０００４】[0004]
【発明が解決しようとする課題】しかし、近年のＬＳＩ
製作技術の進歩はめざましく、配線幅の微細化の実現に
よってＬＳＩから超ＬＳＩへ、さらに超々ＬＳＩへと急
速に発展し、高集積化のために配線幅の微細化が進むに
つれて、従来の配線材料では、抵抗増加による信号遅延
などの問題が懸念されるようになってきた。However, recent LSIs
The progress of manufacturing technology has been remarkable, and the progress of miniaturization of wiring width has led to rapid development from LSI to ultra-LSI and ultra super LSI. Now, there is a growing concern about problems such as signal delay due to increased resistance.
【０００５】特に、チップ面積に対して配線面積の大き
なロジック系の半導体素子では、抵抗増加による信号遅
延が深刻な問題になりつつある。従って、次世代ＶＬＳ
Ｉを実現するには、さらに低抵抗でしかも信頼性の高い
配線材料が必要になる。In particular, in a logic semiconductor device having a wiring area larger than a chip area, signal delay due to increased resistance is becoming a serious problem. Therefore, next-generation VLS
In order to realize I, a wiring material having lower resistance and higher reliability is required.
【０００６】前述したように、現在では、Ａｌ合金やＣ
ｕの薄膜が配線材料として広く利用されているが、Ａｌ
合金による配線は、純金属Ａｌと比較して比抵抗が高
く、更に、エレクロトマイグレーションやストレスマイ
グレーションによる断線、コンタクト部でのＳｉ（ケイ
素）の析出、熱処理によるヒロックの発生といった不安
材料もあり、今後の高集積化、高速化を進めていく上で
は、問題が多い。As mentioned above, Al alloys and C are currently used.
Although a thin film of u is widely used as a wiring material,
The wiring made of an alloy has a higher specific resistance than pure metal Al, and there are also uneasy materials such as disconnection due to electromigration or stress migration, precipitation of Si (silicon) at the contact portion, and generation of hillocks due to heat treatment. There are many problems in promoting high integration and high speed in the future.
【０００７】このようなＡｌ合金に変る配線材料とし
て、高融点金属やＣｕが再検討されているが、高融点金
属は一般的に比抵抗が高いという問題がある。一方、Ｃ
ｕは素子基板となるＳｉＯ2 に対する付着強度が弱く、
前述したように、従来では素子基板上にＣｒ薄膜を介し
て成膜するようにしているが、このような構造では、Ｃ
ｕの薄膜が高抵抗のＣｒの影響を受け、周波数特性の改
善が困難になるという問題も指摘されていた。また、Ｃ
ｕ薄膜は、耐食性が劣るという問題も指摘されていた。Refractory metals and Cu have been reexamined as wiring materials that can be replaced with Al alloys, but refractory metals generally have a problem of high specific resistance. On the other hand, C
u has a weak adhesion strength to SiO 2 which is the element substrate,
As described above, conventionally, the Cr film is formed on the element substrate via the Cr thin film.
It has also been pointed out that the thin film of u is affected by Cr having high resistance, making it difficult to improve frequency characteristics. Also, C
It has been pointed out that the u thin film has a poor corrosion resistance.
【０００８】しかし、Ｃｕは、バルク抵抗が低く、しか
もＡｌに較べてエレクロトマイグレーション等にも強い
など、配線材料として優れた特性も備えており、容易に
は捨てがたい。そこで、Ｃｕの耐食性や素子基板への付
着強度を改善することから、合金化等も検討されてきた
が、合金を鋳造した場合の鋳塊における添加元素の偏析
や、鋳造時の引け巣、鋳塊の結晶粒の粗大化等の多くの
課題が残されていたため、実用化には至らなかった。However, Cu has excellent characteristics as a wiring material, such as low bulk resistance and higher resistance to electromigration than Al, and is not easily discarded. Therefore, alloying and the like have been studied in order to improve the corrosion resistance of Cu and the adhesion strength to the element substrate. However, when alloys are cast, segregation of additive elements in the ingot, shrinkage cavities during casting, and casting Since many problems such as coarsening of the crystal grains of the lump remained, they were not put to practical use.
【０００９】本発明は、前記事情に鑑みてなされたもの
で、スパッタリング法によって電気配線として使用する
金属薄膜を形成する場合に、耐食性が高く、しかも素子
基板等への付着強度も強く、エレクロトマイグレーショ
ン等にも強い銅合金薄膜を形成することができ、今後の
半導体素子等の配線の微細化等を担う配線材料として好
適な金属薄膜形成用スパッタリング・ターゲット並びに
その製造方法を提供することを目的とする。The present invention has been made in view of the above circumstances, and when forming a metal thin film used as an electric wiring by a sputtering method, the corrosion resistance is high, and the adhesion strength to an element substrate or the like is high. An object of the present invention is to provide a sputtering target for forming a metal thin film, which is capable of forming a copper alloy thin film that is resistant to migration and the like, and which is suitable as a wiring material that bears future miniaturization of wiring of semiconductor elements and the like, and a manufacturing method thereof. And
【００１０】[0010]
【課題を解決するための手段】請求項１に記載の金属薄
膜形成用スパッタリング・ターゲットは、純度が９９．
９９９９重量％以上の高純度銅を基体金属とし、この基
体金属に純度が９９．９重量％以上のチタンを０．０４
〜０．１５重量％添加することによって高純度銅合金製
のターゲット材としたことを特徴とする。The sputtering target for forming a metal thin film according to claim 1 has a purity of 99.
High purity copper of 9999% by weight or more is used as a base metal, and titanium having a purity of 99.9% by weight or more is added to the base metal 0.04%.
The target material is made of a high-purity copper alloy by adding 0.15 wt%.
【００１１】請求項２に記載の金属薄膜形成用スパッタ
リング・ターゲットは、純度が９９．９９９９重量％以
上の高純度銅を基体金属とし、この基体金属に純度が９
９．９９９９重量％以上の亜鉛を０．０１４〜０．０２
１重量％添加することによって高純度銅合金製のターゲ
ット材としたことを特徴とする。A sputtering target for forming a metal thin film according to a second aspect uses a high purity copper having a purity of 99.9999% by weight or more as a base metal, and the purity of the base metal is 9
9.9999% by weight or more of zinc 0.014 to 0.02
The target material is made of a high-purity copper alloy by adding 1% by weight.
【００１２】請求項３に記載の金属薄膜形成用スパッタ
リング・ターゲットの製造方法は、請求項１または２に
記載の高純度銅合金の組成比に合わせて基体金属と添加
元素とを混合して溶解槽に投入し、真空中または不活性
ガス雰囲気下で溶湯を連続鋳造することによって、所定
の断面形状をしたターゲット母材を形成し、このターゲ
ット母材から金属薄膜形成用スパッタリング・ターゲッ
トに加工することを特徴とする。According to a third aspect of the present invention, there is provided a method of manufacturing a sputtering target for forming a metal thin film, wherein a base metal and an additive element are mixed and melted in accordance with the composition ratio of the high purity copper alloy according to the first or second aspect. A target base material having a predetermined cross-sectional shape is formed by continuously casting a molten metal in a tank and in a vacuum or in an inert gas atmosphere, and the target base material is processed into a sputtering target for forming a metal thin film. It is characterized by
【００１３】[0013]
【作用】請求項１および請求項２に記載の金属薄膜形成
用スパッタリング・ターゲットは、スパッタリング法に
よって電気配線として使用する金属薄膜を形成に使用し
た場合に、耐食性が高く、しかも素子基板等への付着強
度も強く、エレクロトマイグレーション等にも強い銅合
金薄膜を提供することができ、今後の半導体素子等の配
線の微細化等を担うに好適な配線材料となる。The sputtering target for forming a metal thin film according to claims 1 and 2 has high corrosion resistance when used for forming a metal thin film to be used as an electric wiring by a sputtering method, and furthermore, it can be applied to an element substrate or the like. It is possible to provide a copper alloy thin film having high adhesion strength and high resistance to electromigration and the like, and it is a wiring material suitable for future miniaturization of wiring of semiconductor elements and the like.
【００１４】また、請求項３に記載の金属薄膜形成用ス
パッタリング・ターゲットの製造方法によれば、添加元
素の偏析や引け巣等の鋳造欠陥を防止して、請求項１あ
るいは請求項２に係る高品位な金属薄膜形成用スパッタ
リング・ターゲットを製造することが可能になる。According to the method of manufacturing a sputtering target for forming a metal thin film according to claim 3, casting defects such as segregation of additional elements and shrinkage cavities are prevented, and the sputtering target according to claim 1 or 2 is provided. It becomes possible to manufacture a high-quality sputtering target for forming a metal thin film.
【００１５】[0015]
［第１実施例］図１は、本発明に係る金属薄膜形成用ス
パッタリング・ターゲットの製造方法の第１実施例の処
理手順を示し、図２は、この第１実施例に使用した装置
の概略を示したものである。[First Embodiment] FIG. 1 shows a processing procedure of a first embodiment of a method of manufacturing a sputtering target for forming a metal thin film according to the present invention, and FIG. 2 is a schematic view of an apparatus used in this first embodiment. Is shown.
【００１６】この第１実施例は、純度が９９．９９９９
重量％以上の高純度銅を基体金属とし、この基体金属に
純度が９９．９重量％以上のＴｉ（チタン）を０．０４
〜０．１５重量％添加した高純度銅合金製の金属薄膜形
成用スパッタリング・ターゲットを得るものである。The first embodiment has a purity of 99.9999.
High-purity copper of at least wt% is used as a base metal, and Ti (titanium) having a purity of at least 99.9 wt% is added to the base metal at 0.04%.
It is intended to obtain a sputtering target for forming a metal thin film made of a high-purity copper alloy containing 0.15 wt% or so.
【００１７】まず、図２に基づいて、使用する装置につ
いて説明する。この装置は、連続鋳造用の鋳造装置で、
図２において、符号１は銅合金の溶湯を得るための溶解
槽であるカーボンるつぼ、２はカーボンるつぼ１内に投
入された合金材料を溶解させるためのヒーター、３は連
続鋳造するために前記カーボンるつぼ１の低部に設置さ
れたカーボン鋳型、４は鋳込みを開始時にカーボンるつ
ぼ１内の溶湯をカーボン鋳型３に導くためのスターター
バー（ダミーバー）、５は鋳込んだ溶湯の冷却を促進す
るための水冷ジャケット、６はカーボン鋳型３で鋳造し
た鋳造品（連続した板状の鋳塊）を徐々に引出してゆく
引出しロール、８は連続鋳造を所定の雰囲気下で行うた
めに周囲を気密に囲った装置本体である。装置本体８
は、鋳造品の引出し口として真空シール９が装備され、
さらに、囲った空間内を真空雰囲気とするための真空系
接続部１０や、不活性ガス雰囲気とするための不活性ガ
ス供給部１１がバルブ１２を介して接続されている。First, the apparatus used will be described with reference to FIG. This equipment is a casting equipment for continuous casting,
In FIG. 2, reference numeral 1 is a carbon crucible which is a melting tank for obtaining a molten copper alloy, 2 is a heater for melting the alloy material charged in the carbon crucible 1, and 3 is the carbon for continuous casting. A carbon mold 4 installed at the lower part of the crucible 1 is a starter bar (dummy bar) for guiding the molten metal in the carbon crucible 1 to the carbon mold 3 at the start of casting, and 5 is for promoting cooling of the cast molten metal. Water cooling jacket, 6 is a drawing roll that gradually draws out a cast product (continuous plate-shaped ingot) cast by the carbon mold 3, and 8 is an airtight surrounding that surrounds the continuous casting under a predetermined atmosphere. It is the main body of the device. Device body 8
Is equipped with a vacuum seal 9 as a casting outlet,
Further, a vacuum system connecting portion 10 for creating a vacuum atmosphere in the enclosed space and an inert gas supply portion 11 for creating an inert gas atmosphere are connected via a valve 12.
【００１８】次に、第１実施例の製造方法を、図１に基
づいて説明する。まず、純度が９９．９９９９重量％以
上の高純度銅と純度が９９．９％以上のＴｉとを前述し
た高純度銅合金の組成比に合わせて混合する（ステップ
１０１）。そして、混合した材料をカーボン鋳型３に投
入し、Ａｒガスによる不活性ガス雰囲気下（真空度：１
×１０-4Ｔｏｒｒ）で溶湯を連続鋳造することによって
所定の断面形状をしたターゲット母材を形成する（ステ
ップ１０２）。Next, the manufacturing method of the first embodiment will be described with reference to FIG. First, high-purity copper having a purity of 99.9999% by weight or more and Ti having a purity of 99.9% or more are mixed according to the composition ratio of the high-purity copper alloy described above (step 101). Then, the mixed materials are put into the carbon mold 3 and are placed in an inert gas atmosphere of Ar gas (degree of vacuum: 1
A target base material having a predetermined cross-sectional shape is formed by continuously casting a molten metal at (10 −4 Torr) (step 102).
【００１９】一般的に、添加元素を均一に分散させたタ
ーゲット材としての銅合金を鋳造法によって得ること
は、非常に困難とされてきた。しかし、前記水冷ジャケ
ット５等の冷却効果によって溶湯を急冷凝固させること
によって添加元素の偏析を防止することができ、また、
連続鋳造することによって、引け巣や結晶粒の粗大化等
といった鋳造欠陥の発生を防止することが可能になる。
実際、前述の製造工程によって得たターゲット母材（鋳
塊）は、引け巣がなく、また、添加元素の偏析も防止さ
れた健全なものであった。In general, it has been very difficult to obtain a copper alloy as a target material in which additional elements are uniformly dispersed by a casting method. However, it is possible to prevent the segregation of the additional element by quenching and solidifying the molten metal by the cooling effect of the water cooling jacket 5 and the like.
By continuous casting, it becomes possible to prevent the occurrence of casting defects such as shrinkage cavities and coarsening of crystal grains.
In fact, the target base material (ingot) obtained by the above-described manufacturing process was sound with no shrinkage cavities and in which segregation of the additional element was prevented.
【００２０】次いで、必要に応じて圧延または研削加工
等の機械加工を実施して（ステップ１０３）、前記ター
ゲット母材から金属薄膜形成用スパッタリング・ターゲ
ットを切り出す（ステップ１０４）。Next, if necessary, mechanical processing such as rolling or grinding is carried out (step 103), and a sputtering target for forming a metal thin film is cut out from the target base material (step 104).
【００２１】この第１実施例では、以上のような製造工
程によって、直径が５インチ、厚さが５ミリの金属薄膜
形成用スパッタリング・ターゲットを得た。そして、こ
のターゲットをスパッタリング装置に装着し、Ａｒガス
圧が３×１０-3Ｔｏｒｒ、入力電力が１５００Ｗの条件
下におけるスパッタリングで、ＳｉＯ2 等の素子基板上
に高純度Ｃｕ−Ｔｉ合金膜（以下、単に、Ｃｕ−Ｔｉ膜
と記述する）を成膜した。膜厚は、３０００オングスト
ロームとした。In the first embodiment, a sputtering target for forming a metal thin film having a diameter of 5 inches and a thickness of 5 mm was obtained by the above manufacturing process. Then, wearing the target in a sputtering apparatus, Ar gas pressure 3 × 10 -3 Torr, a sputtering input power under the condition of 1500 W, a high-purity Cu-Ti alloy film on the device substrate, such as SiO 2 (hereinafter , Simply described as a Cu-Ti film). The film thickness was 3000 angstrom.
【００２２】このように形成したＣｕ−Ｔｉ膜につい
て、抵抗率（単位：μΩｃｍ）の測定を行った。また、
本願発明者等は、Ｔｉの添加による抵抗率への影響を調
べるために、Ｔｉの添加率のみを０．０２〜０．２重量
％の範囲で種々に変化させて、前記第１実施例と同様の
製造方法で金属薄膜形成用スパッタリング・ターゲット
を製造し、それらのスパッタリング・ターゲットに対し
ても、同様にＣｕ−Ｔｉ膜の形成を行って、抵抗率の測
定を行った。抵抗率の測定は、２０℃で４ｍＡの電流を
印加することによって行った。次の表１は、その測定結
果を示したものである。なお、この抵抗率測定におい
て、アニール条件は、Ａｒガス雰囲気下で、２５０℃、
１時間とした。また、表１では、スパッタリング・ター
ゲットの金属組成として、Ｔｉの添加率が０．０２９重
量％のもの、０．０４０重量％のもの、０．１１０重量
％ものにおける測定結果を示した。さらに、参考とし
て、純度が９９．９９重量％の純銅（表１では、４Ｎと
記述している）、純度が９９．９９９９重量％の純銅
（表１では、６Ｎと記述している）、純金属Ａｌについ
ても、同じ条件による測定結果を示した。The resistivity (unit: μΩcm) of the Cu-Ti film thus formed was measured. Also,
In order to investigate the effect of the addition of Ti on the resistivity, the inventors of the present application changed variously only the addition rate of Ti within the range of 0.02 to 0.2% by weight, and compared with the first embodiment. Sputtering targets for forming a metal thin film were manufactured by the same manufacturing method, and Cu-Ti films were similarly formed on these sputtering targets, and the resistivity was measured. The resistivity was measured by applying a current of 4 mA at 20 ° C. The following Table 1 shows the measurement results. In this resistivity measurement, the annealing conditions were 250 ° C. under an Ar gas atmosphere.
It was one hour. In addition, Table 1 shows the measurement results of the metal composition of the sputtering target with the Ti addition ratio of 0.029% by weight, 0.040% by weight, and 0.110% by weight. Further, as a reference, pure copper having a purity of 99.99% by weight (described as 4N in Table 1), pure copper having a purity of 99.9999% by weight (described as 6N in Table 1), pure For metal Al, the measurement results under the same conditions are also shown.
【００２３】[0023]
【表１】 この表１に示されているように、高純度銅にＴｉを添加
したスパッタリング・ターゲットによって形成したＣｕ
−Ｔｉ膜では、アニール条件では、Ｔｉの添加率の増大
に応じて抵抗率が増加するという傾向がみられるもの
の、いずれの添加率においても、Ａｌの場合よりも、よ
い抵抗率が得られることが確認された。[Table 1] As shown in Table 1, Cu formed by a sputtering target in which Ti is added to high-purity copper
In the -Ti film, under the annealing condition, the resistivity tends to increase in accordance with the increase in the Ti addition rate, but at any addition rate, a better resistivity can be obtained than in the case of Al. Was confirmed.
【００２４】さらに、前述の各Ｃｕ−Ｔｉ膜について、
Ａｒガス雰囲気中において２５０℃で１時間の熱処理を
施した後、液温３５℃の１Ｎの食塩水中に一定時間浸漬
して、そのときの反射率の経時変化を測定することによ
って、Ｔｉ添加率の異なる各Ｃｕ−Ｔｉ膜について耐食
性を評価した。図３は、その耐食性の評価結果を示した
ものである。Further, regarding each of the Cu-Ti films mentioned above,
After heat treatment at 250 ° C. for 1 hour in an Ar gas atmosphere, it is immersed in 1N saline solution at a liquid temperature of 35 ° C. for a certain period of time, and the change in reflectance with time at that time is measured. The corrosion resistance was evaluated for each of the Cu-Ti films having different values. FIG. 3 shows the evaluation result of the corrosion resistance.
【００２５】図３において、縦軸は反射率の変化（食塩
水中に浸漬させた後の反射率Ｒｃと評価試験前の反射率
Ｒｉとの比率）を示し、横軸は時間の経過を示してい
る。また、図中において、曲線２０は純金属Ａｌによる
金属薄膜に対するもの、曲線２１はＴｉの添加率が０．
１１重量％のターゲットで形成したＣｕ−Ｔｉ膜に対す
るもの、曲線２２はＴｉの添加率が０．０４０重量％の
ターゲットで形成したＣｕ−Ｔｉ膜に対するもの、曲線
２３は純度が９９．９９重量％の純銅による金属薄膜に
対するもの、曲線２４はＴｉの添加率が０．０２９重量
％のターゲットで形成したＣｕ−Ｔｉ膜に対するもの、
曲線２５は純度が９９．９９９９重量％の高純度の純銅
による金属薄膜に対するもの、曲線２６はＴｉの添加率
が０．２６重量％のターゲットで形成したＣｕ−Ｔｉ膜
に対するものである。In FIG. 3, the vertical axis represents the change in reflectance (the ratio of the reflectance Rc after immersion in saline solution to the reflectance Ri before the evaluation test), and the horizontal axis represents the passage of time. There is. In the figure, a curve 20 is for a metal thin film made of pure metal Al, and a curve 21 is for a Ti addition ratio of 0.
For a Cu-Ti film formed with an 11 wt% target, curve 22 is for a Cu-Ti film formed with a target with a Ti addition rate of 0.040 wt%, and curve 23 is a purity of 99.99 wt%. Curve 24 for a Cu-Ti film formed with a target having a Ti addition rate of 0.029% by weight,
A curve 25 is for a thin metal film of high-purity pure copper with a purity of 99.9999% by weight, and a curve 26 is for a Cu-Ti film formed with a target having a Ti addition rate of 0.26% by weight.
【００２６】図３にも示しているように、Ｔｉの添加率
が０．０４０重量％および０．１１重量％のターゲット
で形成したＣｕ−Ｔｉ膜は、いずれも、純度が９９．９
９重量％の純銅によって形成した金属薄膜よりも高い耐
食性を示し、Ｔｉの添加率の０．１１重量％の場合で
は、純金属Ａｌによる金属薄膜の場合にかなり接近して
いる。しかし、Ｔｉの添加率が更に増大した０．２６重
量％の場合には、逆に耐食性が低下してしまった。As shown in FIG. 3, the Cu-Ti films formed with the targets having the Ti addition rates of 0.040% by weight and 0.11% by weight have a purity of 99.9.
It exhibits higher corrosion resistance than the metal thin film formed by 9 wt% pure copper, and when the Ti addition rate is 0.11 wt%, it is quite close to the metal thin film made of pure metal Al. However, when the Ti addition rate was further increased to 0.26% by weight, conversely the corrosion resistance deteriorated.
【００２７】本願発明者等は、Ｔｉの添加率と耐食性と
の関係をさらに究明するため、より細かくＴｉの添加率
を変化させて、同様の耐食性の評価を行った。その結
果、純度が９９．９９９９重量％以上の高純度銅を基体
金属とし、この基体金属に純度が９９．９重量％以上の
Ｔｉを０．０４〜０．１５重量％添加した高純度銅合金
製の金属薄膜形成用スパッタリング・ターゲットの場合
には、何れも、純度９９．９９重量％の純銅による金属
薄膜よりも耐食性が優れ、純金属Ａｌによる金属薄膜に
近い耐食性を持った金属薄膜が得られることを確認し
た。In order to further investigate the relationship between the Ti addition ratio and the corrosion resistance, the inventors of the present application performed the same corrosion resistance evaluation by changing the Ti addition ratio more finely. As a result, a high-purity copper alloy having a purity of 99.9999% by weight or more as a base metal and 0.04 to 0.15% by weight of Ti having a purity of 99.9% by weight or more added to the base metal. In the case of a sputtering target for forming a metal thin film, the metal thin film is superior in corrosion resistance to a metal thin film made of pure copper having a purity of 99.99% by weight, and has a corrosion resistance close to that of a metal thin film made of pure metal Al. I was confirmed.
【００２８】また、純度が９９．９９９９重量％以上の
高純度銅を基体金属とし、この基体金属に純度が９９．
９重量％以上のＴｉを０．０４〜０．１５重量％添加し
た高純度銅合金製の金属薄膜形成用スパッタリング・タ
ーゲットについては、スパッタリング法によってガラス
基板上にＣｕ−Ｔｉ膜を成膜させ、そのＣｕ−Ｔｉ膜に
ついて、引っ張り法によって付着強度の評価を行った。
純度９９．９９重量％の純銅による金属薄膜の付着強度
は約８９ｋｇ／ｃｍ2 、純度９９．９９９９重量％の純
銅による金属薄膜の付着強度は約１０２ｋｇ／ｃｍ2 で
あったのに対し、Ｃｕ−Ｔｉ膜の場合は、何れの添加率
の場合においても、１５０ｋｇ／ｃｍ2以上の付着強度
が得られ、付着強度も大幅に改善されていることが確認
できた。以下の表２は、以上の評価結果をまとめたもの
である。表２において、「４Ｎ」とは純度９９．９９重
量％の純銅による金属薄膜を示し、「６Ｎ」とは純度９
９．９９９９重量％の純銅による金属薄膜を示し、「Ｃ
ｕ−Ｔｉ」とはＴｉの添加率が０．０４〜０．１５重量
％のターゲットで形成したＣｕ−Ｔｉ膜を示し、「Ｃｕ
−Ｚｎ」とは後述の第２実施例で説明するＺｎを添加元
素としたターゲットで形成した金属薄膜を示している。Further, high purity copper having a purity of 99.9999% by weight or more is used as a base metal, and the base metal has a purity of 99.
Regarding a sputtering target for forming a metal thin film made of a high-purity copper alloy in which 0.04 to 0.15 wt% of Ti is added by 9 wt% or more, a Cu-Ti film is formed on a glass substrate by a sputtering method, The adhesion strength of the Cu-Ti film was evaluated by the tensile method.
The adhesion strength of the metal thin film made of pure copper having a purity of 99.99 wt% was about 89 kg / cm 2 , and the adhesion strength of the metal thin film made of pure copper having a purity of 99.9999 wt% was about 102 kg / cm 2 , whereas Cu- In the case of the Ti film, it was confirmed that the adhesion strength of 150 kg / cm 2 or more was obtained and the adhesion strength was significantly improved at any addition rate. Table 2 below summarizes the above evaluation results. In Table 2, “4N” indicates a metal thin film made of pure copper having a purity of 99.99% by weight, and “6N” indicates a purity of 9
A metal thin film made of 9.9999% by weight of pure copper is shown.
“U-Ti” refers to a Cu—Ti film formed with a target having a Ti addition rate of 0.04 to 0.15% by weight.
"-Zn" refers to a metal thin film formed of a target containing Zn as an additive element, which will be described in the second embodiment below.
【００２９】[0029]
【表２】 以上に説明したように、この第１実施例で製造した金属
薄膜形成用スパッタリング・ターゲットは、スパッタリ
ング法によって電気配線として使用する金属薄膜を形成
に使用した場合に、耐食性が高く、しかも素子基板等へ
の付着強度も強く、エレクロトマイグレーション等にも
強い銅合金薄膜を提供することができ、今後の半導体素
子等の配線の微細化等を担うに好適な配線材料となる。[Table 2] As described above, the sputtering target for forming a metal thin film manufactured in the first embodiment has high corrosion resistance when used for forming a metal thin film used as an electric wiring by a sputtering method, and further, an element substrate or the like. It is possible to provide a copper alloy thin film that has a strong adhesion strength to, and is resistant to electromigration and the like, and is a wiring material suitable for future miniaturization of wiring of semiconductor elements and the like.
【００３０】［第２実施例］本願発明者等は、本発明に
係る金属薄膜形成用スパッタリング・ターゲットの製造
方法の第２実施例として、添加元素としてＺｎ（亜鉛）
を用いた高純度銅合金製の金属薄膜形成用スパッタリン
グ・ターゲットを製造した。[Second Embodiment] As a second embodiment of the method for manufacturing a sputtering target for forming a metal thin film according to the present invention, the inventors of the present invention used Zn (zinc) as an additive element.
Was used to produce a sputtering target for forming a metal thin film made of a high-purity copper alloy.
【００３１】この第２実施例の場合、製造する金属薄膜
形成用スパッタリング・ターゲットは、純度が９９．９
９９９重量％以上の高純度銅を基体金属とし、この基体
金属に純度が９９．９９９９重量％以上のＺｎを０．０
１４〜０．０２１重量％添加したものである。In the case of the second embodiment, the sputtering target for forming a metal thin film produced has a purity of 99.9.
High purity copper of 999% by weight or more is used as a base metal, and Zn having a purity of 99.9999% by weight or more is 0.0
14 to 0.021% by weight is added.
【００３２】添加元素が純度が９９．９９９９重量％以
上のＺｎで、添加率が０．０１４〜０．０２１重量％に
変更されたことを除けば、製造上のそれ以外の条件は、
すべて第１実施例の場合に準じて製造した。Except for the fact that the additive element is Zn with a purity of 99.9999% by weight or more and the addition rate is changed to 0.014 to 0.021% by weight, the other manufacturing conditions are as follows:
All were manufactured according to the case of the first embodiment.
【００３３】即ち、まず、純度が９９．９９９９重量％
以上の高純度銅と純度が９９．９９９９％以上のＺｎと
を前述した高純度銅合金の組成比に合わせて混合する。
次いで、混合した材料をカーボン鋳型３に投入し、Ａｒ
ガスによる不活性ガス雰囲気下で溶湯を連続鋳造するこ
とによって所定の断面形状をしたターゲット母材を形成
する。That is, first, the purity is 99.9999% by weight.
The above high-purity copper and Zn having a purity of 99.9999% or more are mixed according to the composition ratio of the above-mentioned high-purity copper alloy.
Then, the mixed material is put into the carbon mold 3 and Ar
A target base material having a predetermined cross-sectional shape is formed by continuously casting a molten metal in an inert gas atmosphere of gas.
【００３４】次いで、必要に応じて圧延または研削加工
等の機械加工を実施して、前記ターゲット母材から金属
薄膜形成用スパッタリング・ターゲットを切り出す。Then, if necessary, mechanical processing such as rolling or grinding is carried out to cut out a sputtering target for forming a metal thin film from the target base material.
【００３５】この第２実施例では、以上のような製造工
程によって、直径が５インチ、厚さが５ミリの金属薄膜
形成用スパッタリング・ターゲットを得た。そして、こ
のターゲットをスパッタリング装置に装着し、Ａｒガス
圧が３×１０-3Ｔｏｒｒ、入力電力が１５００Ｗの条件
下におけるスパッタリングで、ＳｉＯ2 等の素子基板上
に高純度Ｃｕ−Ｚｎ合金膜（以下、単に、Ｃｕ−Ｚｎ膜
と記述する）を成膜した。膜厚は、３０００オングスト
ロームとした。In the second embodiment, a sputtering target for forming a metal thin film having a diameter of 5 inches and a thickness of 5 mm was obtained by the above manufacturing process. Then, wearing the target in a sputtering apparatus, Ar gas pressure 3 × 10 -3 Torr, a sputtering input power under the condition of 1500 W, a high-purity Cu-Zn alloy layer on the element substrate of SiO 2 or the like (hereinafter , Simply described as a Cu—Zn film). The film thickness was 3000 angstrom.
【００３６】このように形成したＣｕ−Ｚｎ膜につい
て、第１実施例と同様に、抵抗率（単位：μΩｃｍ）の
測定を行った。Ｚｎの添加による抵抗率への影響を調べ
るために、Ｚｎの添加率のみを０．００５〜０．０５０
重量％の範囲で種々に変化させて、前記第２実施例と同
様の製造方法で金属薄膜形成用スパッタリング・ターゲ
ットを製造し、それらのスパッタリング・ターゲットに
対しても、同様にＣｕ−Ｚｎ膜の形成を行って、抵抗率
の測定を行った。抵抗率の測定は、２０℃で４ｍＡの電
流を印加することによって行った。次の表３は、その測
定結果を示したものである。なお、この抵抗率測定にお
いて、アニール条件は、Ａｒガス雰囲気下で、２５０
℃、１時間とした。また、表３では、スパッタリング・
ターゲットの金属組成として、Ｚｎの添加率が０．０１
４重量％のもの、０．０２１重量％のもの、０．０．０
４０重量％ものにおける測定結果を示した。さらに、参
考として、純度が９９．９９重量％の純銅（表３では、
４Ｎと記述している）、純度が９９．９９９９重量％の
純銅（表３では、６Ｎと記述している）、純金属Ａｌに
ついても、同じ条件による測定結果を示した。The resistivity (unit: μΩcm) of the Cu--Zn film thus formed was measured in the same manner as in the first embodiment. In order to investigate the influence of the addition of Zn on the resistivity, only the addition rate of Zn is 0.005 to 0.050.
The sputtering target for forming a metal thin film is manufactured by the same manufacturing method as that of the second embodiment, with various changes within the range of wt%, and the Cu--Zn film of the sputtering target is similarly formed for these sputtering targets. After formation, the resistivity was measured. The resistivity was measured by applying a current of 4 mA at 20 ° C. Table 3 below shows the measurement results. In this resistivity measurement, the annealing condition is 250 in Ar gas atmosphere.
C. and 1 hour. In addition, in Table 3,
As the metal composition of the target, the Zn addition rate is 0.01
4% by weight, 0.021% by weight, 0.0.
The measurement results at 40% by weight are shown. Further, as a reference, pure copper having a purity of 99.99% by weight (in Table 3,
4N), pure copper having a purity of 99.9999% by weight (described as 6N in Table 3), and pure metal Al also show the measurement results under the same conditions.
【００３７】[0037]
【表３】 この表３に示されているように、高純度銅にＺｎを添加
したスパッタリング・ターゲットによって形成したＣｕ
−Ｚｎ膜では、いずれの添加率においても、純銅の場合
よりは高いがＡｌの場合よりも、よい抵抗率が得られる
ことが確認された。[Table 3] As shown in Table 3, Cu formed by a sputtering target in which Zn is added to high-purity copper
It was confirmed that in the -Zn film, at any addition rate, a higher resistivity than that of pure copper but a better resistivity than that of Al was obtained.
【００３８】さらに、前述の各Ｃｕ−Ｚｎ膜について、
Ａｒガス雰囲気中において２５０℃で１時間の熱処理を
施した後、液温３５℃の１Ｎの食塩水中に一定時間浸漬
して、そのときの反射率の経時変化を測定することによ
って、Ｚｎ添加率の異なる各Ｃｕ−Ｚｎ膜について耐食
性を評価した。図４は、その耐食性の評価結果を示した
ものである。Further, regarding each of the Cu-Zn films described above,
After performing a heat treatment at 250 ° C. for 1 hour in an Ar gas atmosphere, immersing it in 1N saline solution at a liquid temperature of 35 ° C. for a certain period of time, and measuring the change with time of the reflectance at that time, the Zn addition rate The corrosion resistance was evaluated for each of the Cu-Zn films having different values. FIG. 4 shows the evaluation result of the corrosion resistance.
【００３９】図４において、縦軸は反射率の変化（食塩
水中に浸漬させた後の反射率Ｒｃと評価試験前の反射率
Ｒｉとの比率）を示し、横軸は時間の経過を示してい
る。また、図中において、曲線３０は純金属Ａｌによる
金属薄膜に対するもの、曲線３１はＺｎの添加率が０．
０１４重量％のターゲットで形成したＣｕ−Ｚｎ膜に対
するもの、曲線３２はＺｎの添加率が０．０２１重量％
のターゲットで形成したＣｕ−Ｚｎ膜に対するもの、曲
線３３はＺｎの添加率が０．０４０重量％のターゲット
で形成したＣｕ−Ｚｎ膜に対するもの、曲線３４はＺｎ
の添加率が０．００９重量％のターゲットで形成したＣ
ｕ−Ｚｎ膜に対するもの、曲線３５は純度が９９．９９
重量％の純銅による金属薄膜に対するもの、曲線３６は
純度が９９．９９９９重量％の高純度の純銅による金属
薄膜に対するものである。In FIG. 4, the vertical axis represents the change in reflectance (the ratio of the reflectance Rc after being immersed in saline to the reflectance Ri before the evaluation test), and the horizontal axis represents the passage of time. There is. In the figure, a curve 30 is for a metal thin film made of pure metal Al, and a curve 31 is for a Zn addition ratio of 0.
For a Cu-Zn film formed with a target of 014 wt%, curve 32 shows a Zn addition rate of 0.021 wt%
Curve 33 is for the Cu-Zn film formed with the target of FIG.
C formed with a target having an addition rate of 0.009% by weight
For the u-Zn film, curve 35 has a purity of 99.99.
Curve 36 is for a thin metal film of pure copper at wt.%, Curve 36 is for a thin metal film of pure copper at 99.9999 wt.% Purity.
【００４０】図４にも示しているように、Ｚｎの添加率
が０．００９重量％および０．０４０重量％のターゲッ
トで形成したＣｕ−Ｚｎ膜は、純度が９９．９９重量％
の純銅によって形成した金属薄膜よりも経過時間の一部
においては高い耐食性を示す。これに対して、Ｚｎの添
加率が０．０１４重量％および０．０２１重量％のター
ゲットで形成したＣｕ−Ｚｎ膜は、純度が９９．９９重
量％の純銅によって形成した金属薄膜よりも経過時間の
全域で高い耐食性を示し、純金属Ａｌによる金属薄膜の
場合に接近した様相が確認された。As shown in FIG. 4, the Cu—Zn film formed with the targets having Zn addition rates of 0.009% by weight and 0.040% by weight has a purity of 99.99% by weight.
Shows higher corrosion resistance than the metal thin film formed by pure copper for a part of the elapsed time. On the other hand, the Cu-Zn film formed with the targets having Zn addition rates of 0.014% by weight and 0.021% by weight has a longer elapsed time than the metal thin film formed of pure copper having a purity of 99.99% by weight. A high corrosion resistance was exhibited in the entire area of, and a close appearance was confirmed in the case of a metal thin film made of pure metal Al.
【００４１】本願発明者等は、Ｚｎの添加率と耐食性と
の関係をさらに究明するため、より細かくＳｉの添加率
を変化させて、同様の耐食性の評価を行った。その結
果、純度が９９．９９９９重量％以上の高純度銅を基体
金属とし、この基体金属に純度が９９．９９９９重量％
以上のＺｎを０．０１４〜０．０２１重量％添加した高
純度銅合金製の金属薄膜形成用スパッタリング・ターゲ
ットの場合には、何れも、純度９９．９９重量％の純銅
による金属薄膜よりも耐食性が優れ、純金属Ａｌによる
金属薄膜に近い耐食性を持った金属薄膜が得られること
を確認した。In order to further investigate the relationship between the Zn addition rate and the corrosion resistance, the inventors of the present application performed a similar evaluation of the corrosion resistance by changing the Si addition rate more finely. As a result, high purity copper having a purity of 99.9999% by weight or more is used as the base metal, and the purity of the base metal is 99.9999% by weight.
In the case of a sputtering target for forming a metal thin film made of a high-purity copper alloy containing 0.014 to 0.021% by weight of Zn, corrosion resistance is higher than that of a metal thin film made of pure copper having a purity of 99.99% by weight. It was confirmed that a metal thin film having excellent corrosion resistance and corrosion resistance similar to that of a metal thin film made of pure metal Al was obtained.
【００４２】また、純度が９９．９９９９重量％以上の
高純度銅を基体金属とし、この基体金属に純度が９９．
９９９９重量％以上のＺｎを０．０１４〜０．０２１重
量％添加した高純度銅合金製の金属薄膜形成用スパッタ
リング・ターゲットについては、スパッタリング法によ
ってガラス基板上にＣｕ−Ｚｎ膜を成膜させ、そのＣｕ
−Ｚｎ膜について、引っ張り法によって付着強度の評価
を行った。Ｃｕ−Ｚｎ膜の場合は、何れの添加率の場合
においても、１５０ｋｇ／ｃｍ2 以上の付着強度が得ら
れ（前述の表２参照００）、付着強度も大幅に改善され
ていることが確認できた。High-purity copper having a purity of 99.9999% by weight or more is used as a base metal, and the base metal has a purity of 99.
Regarding a sputtering target for forming a metal thin film made of a high-purity copper alloy in which 0.014 to 0.021% by weight of Zn of 9999% by weight or more is added, a Cu-Zn film is formed on a glass substrate by a sputtering method, The Cu
With respect to the Zn film, the adhesion strength was evaluated by the tensile method. In the case of the Cu-Zn film, it was confirmed that the adhesion strength of 150 kg / cm 2 or more was obtained (see Table 2 above, 00) and the adhesion strength was significantly improved at any addition rate. It was
【００４３】以上に説明したように、この第２実施例で
製造した金属薄膜形成用スパッタリング・ターゲット
は、スパッタリング法によって電気配線として使用する
金属薄膜を形成に使用した場合に、耐食性が高く、しか
も素子基板等への付着強度も強く、エレクロトマイグレ
ーション等にも強い銅合金薄膜を提供することができ、
今後の半導体素子等の配線の微細化等を担うに好適な配
線材料となる。As described above, the metal thin film forming sputtering target manufactured in the second embodiment has high corrosion resistance when used for forming a metal thin film used as an electric wiring by the sputtering method, and It is possible to provide a copper alloy thin film that has a strong adhesion strength to the element substrate, etc. and is strong against electromigration, etc.
It is a suitable wiring material for future miniaturization of wiring of semiconductor elements and the like.
【００４４】[0044]
【発明の効果】請求項１および請求項２に記載の金属薄
膜形成用スパッタリング・ターゲットは、スパッタリン
グ法によって電気配線として使用する金属薄膜を形成に
使用した場合に、耐食性が高く、しかも素子基板等への
付着強度も強く、エレクロトマイグレーション等にも強
い銅合金薄膜を提供することができ、今後の半導体素子
等の配線の微細化等を担うに好適な配線材料となる。[Effects of the Invention] The sputtering target for forming a metal thin film according to claims 1 and 2 has high corrosion resistance when used for forming a metal thin film used as an electric wiring by a sputtering method, and further, it is an element substrate or the like. It is possible to provide a copper alloy thin film that has a strong adhesion strength to, and is resistant to electromigration and the like, and is a wiring material suitable for future miniaturization of wiring of semiconductor elements and the like.
【００４５】また、請求項３に記載の金属薄膜形成用ス
パッタリング・ターゲットの製造方法によれば、添加元
素の偏析や引け巣等の鋳造欠陥を防止して、請求項１あ
るいは請求項２に係る高品位な金属薄膜形成用スパッタ
リング・ターゲットを製造することが可能になる。According to the method of manufacturing a sputtering target for forming a metal thin film according to claim 3, casting defects such as segregation of additional elements and shrinkage cavities are prevented, and the sputtering target according to claim 1 or 2 is provided. It becomes possible to manufacture a high-quality sputtering target for forming a metal thin film.
【図１】本発明に係る金属薄膜形成用スパッタリング・
ターゲットの製造方法の工程説明図である。FIG. 1 is a diagram illustrating a sputtering method for forming a metal thin film according to the present invention.
It is process explanatory drawing of the manufacturing method of a target.
【図２】本発明に係る金属薄膜形成用スパッタリング・
ターゲットの製造方法で使用する鋳造装置の構成図であ
る。[FIG. 2] Sputtering for forming a metal thin film according to the present invention
It is a block diagram of the casting apparatus used by the manufacturing method of a target.
【図３】本発明の第１実施例で製造した高純度銅合金の
耐食特性図である。FIG. 3 is a corrosion resistance characteristic diagram of the high-purity copper alloy produced in the first embodiment of the present invention.
【図４】本発明の第２実施例で製造した高純度銅合金の
耐食特性図である。FIG. 4 is a corrosion resistance characteristic diagram of the high-purity copper alloy manufactured in the second embodiment of the present invention.
１ カーボンるつぼ ２ ヒーター ３ カーボン鋳型 ４ スターターバー ５ 水冷ジャケット ６ 引き出しロール ８ 装置本体 1 Carbon crucible 2 Heater 3 Carbon mold 4 Starter bar 5 Water cooling jacket 6 Drawer roll 8 Machine body
───────────────────────────────────────────────────── フロントページの続き (72)発明者 永田 長寿 東京都千代田区丸の内一丁目８番２号 同 和鉱業 株式会社内 ─────────────────────────────────────────────────── ─── Continued Front Page (72) Inventor Nagatoshi Nagata 1-2-8 Marunouchi, Chiyoda-ku, Tokyo Dowa Mining Co., Ltd.
Claims (3)
度銅を基体金属とし、この基体金属に純度が９９．９重
量％以上のチタンを０．０４〜０．１５重量％添加する
ことによって高純度銅合金製のターゲット材としたこと
を特徴とする金属薄膜形成用スパッタリング・ターゲッ
ト。1. A high purity copper having a purity of 99.9999% by weight or more is used as a base metal, and 0.04 to 0.15% by weight of titanium having a purity of 99.9% by weight or more is added to the base metal. A sputtering target for forming a metal thin film, which is a target material made of a high-purity copper alloy.
度銅を基体金属とし、この基体金属に純度が９９．９９
９９重量％以上の亜鉛を０．０１４〜０．０２１重量％
添加することによって高純度銅合金製のターゲット材と
したことを特徴とする金属薄膜形成用スパッタリング・
ターゲット。2. A base metal is high-purity copper having a purity of 99.9999% by weight or more, and the base metal has a purity of 99.99.
0.014 to 0.021% by weight of 99% by weight or more of zinc
Sputtering for metal thin film formation characterized by making it a target material made of high-purity copper alloy by adding
target.
の組成比に合わせて基体金属と添加元素とを混合して溶
解槽に投入し、真空中または不活性ガス雰囲気下で溶湯
を連続鋳造することによって、所定の断面形状をしたタ
ーゲット母材を形成し、このターゲット母材から金属薄
膜形成用スパッタリング・ターゲットに加工することを
特徴とする金属薄膜形成用スパッタリング・ターゲット
の製造方法。3. A base metal and an additive element are mixed according to the composition ratio of the high-purity copper alloy according to claim 1 and charged into a melting tank, and the molten metal is added in a vacuum or in an inert gas atmosphere. A method for producing a sputtering target for forming a metal thin film, comprising forming a target base material having a predetermined cross-sectional shape by continuous casting, and processing the target base material into a sputtering target for forming a metal thin film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11895392A JP2862727B2 (en) | 1992-05-12 | 1992-05-12 | Sputtering target for forming metal thin film and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11895392A JP2862727B2 (en) | 1992-05-12 | 1992-05-12 | Sputtering target for forming metal thin film and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05311424A true JPH05311424A (en) | 1993-11-22 |
| JP2862727B2 JP2862727B2 (en) | 1999-03-03 |
Family
ID=14749352
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11895392A Expired - Fee Related JP2862727B2 (en) | 1992-05-12 | 1992-05-12 | Sputtering target for forming metal thin film and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2862727B2 (en) |
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