JP2003213407A - High purity nickel or nickel alloy sputtering target and production method therefor - Google Patents
High purity nickel or nickel alloy sputtering target and production method thereforInfo
- Publication number
- JP2003213407A JP2003213407A JP2002015347A JP2002015347A JP2003213407A JP 2003213407 A JP2003213407 A JP 2003213407A JP 2002015347 A JP2002015347 A JP 2002015347A JP 2002015347 A JP2002015347 A JP 2002015347A JP 2003213407 A JP2003213407 A JP 2003213407A
- Authority
- JP
- Japan
- Prior art keywords
- nickel
- sputtering target
- purity
- content
- nickel alloy
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Electrodes Of Semiconductors (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、スパッタリングタ
ーゲット、特にゲート電極材料用のサリサイドプロセス
によるシリサイド膜を形成するのに好適な高純度ニッケ
ル又はニッケル合金スパッタリングターゲット及びその
製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sputtering target, and more particularly to a high-purity nickel or nickel alloy sputtering target suitable for forming a silicide film for a gate electrode material by a salicide process and a method for manufacturing the same.
【０００２】[0002]
【従来の技術】従来、ゲート電極材料としてサリサイド
プロセスによるＷＳｉ２、ＴｉＳｉ２が用いられている
が、ＷＳｉ２は抵抗率が著しく高く、利用上の興味が失
われている。ＴｉＳｉ２は抵抗率がＷＳｉ２よりも低
く、特性上優れているが、高温でのアニールを必要とす
るため絶縁膜上へのシリサイドのオーバーグロースが起
こりやすく、細線抵抗が上昇するという欠点がある。ま
た、このＴｉＳｉ２は熱処理のやり方によっては凝集が
生じ、抵抗の上昇や接合リーク、ゲート耐圧の劣化の原
因となる問題がある。これらに替わるものとして、Ｃｏ
Ｓｉ２がある。このＣｏＳｉ２はシリサイド反応時の拡
散種がＣｏであるためにオーバーグロースが起こりにく
く、また細線抵抗の上昇も少ないという利点がある。し
かし、熱処理の条件によっては凝集が生じ易いと言う問
題があり、さらに材料が高価であり、コスト的に不利で
あるという欠点がある。 2. Description of the Related Art Conventionally, WSi 2 and TiSi 2 obtained by a salicide process have been used as a gate electrode material, but WSi 2 has a remarkably high resistivity and loses interest in use. TiSi 2 has a lower resistivity than WSi 2 and is superior in characteristics, but since it requires annealing at a high temperature, silicide overgrowth easily occurs on the insulating film, and there is a drawback that the fine wire resistance increases. . Further, this TiSi 2 causes agglomeration depending on the method of heat treatment, which causes problems such as increase in resistance, junction leakage, and deterioration of gate breakdown voltage. As an alternative to these, Co
There is Si 2 . Since CoSi 2 is Co as the diffusion species during the silicide reaction, overgrowth is less likely to occur, and the resistance of the thin wire is less likely to increase. However, there is a problem that aggregation is likely to occur depending on the condition of heat treatment, and there is a drawback that the material is expensive and it is disadvantageous in cost.
【０００３】以上から、ゲート電極材料としてサリサイ
ドプロセスによるニッケルシリサイド（ＮｉＳｉ）が注
目されている。このＮｉＳｉは、上記ＣｏＳｉ２と同様
に抵抗率が低く、シリサイド反応時の拡散種がＮｉであ
るためにオーバーグロースが起こりにくく、また細線抵
抗の上昇も少ないという利点がある。さらに、シリサイ
ド化反応におけるＳｉの消費量が少ないという特徴もあ
る。しかし、このニッケルシリサイドは、準安定相であ
るＮｉＳｉと安定相であるＮｉＳｉ２相があり、７００
°Ｃを超える熱処理温度ではこの安定相であるＮｉＳｉ
２相に相転移してしまう。このＮｉＳｉ２相は抵抗率が
高く、シリサイド化反応におけるＳｉの消費量も増大す
るので、従来のゲート電極材料に比べて何らメリットが
ないと言える。From the above, attention has been paid to nickel silicide (NiSi) by a salicide process as a gate electrode material. Similar to CoSi 2 , NiSi has a low resistivity, and since Ni is the diffusing species during the silicide reaction, overgrowth is unlikely to occur, and the resistance of the fine wire is small. Further, there is a feature that the amount of Si consumed in the silicidation reaction is small. However, this nickel silicide has NiSi which is a metastable phase and NiSi 2 phase which is a stable phase.
NiSi, which is in this stable phase at heat treatment temperatures above ° C
The phase transitions to two phases. Since this NiSi 2 phase has a high resistivity and increases the amount of Si consumed in the silicidation reaction, it can be said that it has no merit in comparison with the conventional gate electrode material.
【０００４】[0004]
【発明が解決しょうとする課題】以上から、本発明はゲ
ート電極材料としてサリサイドプロセスによるニッケル
シリサイド（ＮｉＳｉ）の利点を生かすと同時に、Ｎｉ
Ｓｉ２相に相転移させる原因を究明し、これを効果的に
抑制できる、特にゲート電極材料として有用な高純度ニ
ッケル又はニッケル合金スパッタリングターゲット及び
その製造方法を提供するものである。From the above, the present invention takes advantage of nickel silicide (NiSi) by a salicide process as a gate electrode material, and at the same time, Ni
It is intended to provide a high-purity nickel or nickel alloy sputtering target which is particularly useful as a gate electrode material, and a method for producing the same, which is capable of investigating the cause of phase transition to the Si 2 phase and effectively suppressing it.
【０００５】[0005]
【課題を解決するための手段】本発明は、
１．酸素、炭素の含有量がそれぞれ２０ｗｔｐｐｍ以下
であることを特徴とする高純度ニッケル又はニッケル合
金スパッタリングターゲット
２．酸素、炭素の含有量がそれぞれ１０ｗｔｐｐｍ以下
であることを特徴とする高純度ニッケル又はニッケル合
金スパッタリングターゲット
３．酸素、炭素の含有量がそれぞれ１ｗｔｐｐｍ以下で
あることを特徴とする高純度ニッケル又はニッケル合金
スパッタリングターゲット
４．水素の含有量が１０ｗｔｐｐｍ以下であることを特
徴とする上記１〜３のそれぞれに記載の高純度ニッケル
又はニッケル合金スパッタリングターゲット
５．水素の含有量が１ｗｔｐｐｍ以下であることを特徴
とする上記１〜３のそれぞれに記載の高純度ニッケル又
はニッケル合金スパッタリングターゲット
６．合金元素及び酸素、水素、窒素、炭素等のガス成分
を除く不純物元素の含有量が１０ｗｔｐｐｍ未満である
ことを特徴とする上記１〜５のそれぞれに記載の高純度
ニッケル又はニッケル合金スパッタリングターゲット
７．鉄の含有量が５ｐｐｍ以下であることを特徴とする
上記６に記載の高純度ニッケル又はニッケル合金スパッ
タリングターゲット
８．鉄の含有量が２ｐｐｍ以下であることを特徴とする
上記６に記載の高純度ニッケル又はニッケル合金スパッ
タリングターゲット
９．合金元素として、チタン、ジルコニウム、ハフニウ
ム、バナジウム、ニオブ、タンタル、クロム、マンガ
ン、ルテニウム、パラジウム、白金、モリブデン、レニ
ウム、タングステンから選択した少なくとも１種類以上
の元素を含有することを特徴とする上記１〜８のそれぞ
れに記載の高純度ニッケル合金スパッタリングターゲッ
ト
１０．合金元素として、鉄又はコバルトから選択した少
なくとも１種類以上の元素を含有することを特徴とする
上記１〜６及び９のそれぞれに記載の高純度ニッケル合
金スパッタリングターゲット
１１．合金元素の含有量が０．５〜１０ａｔ％であるこ
とを特徴とする上記１〜１０のそれぞれに記載の高純度
ニッケル合金スパッタリングターゲット
１２．合金元素の含有量が１〜５ａｔ％であることを特
徴とする上記１〜１０のそれぞれに記載の高純度ニッケ
ル合金スパッタリングターゲット
１３．ランタノイド系元素を０．２〜４０ｐｐｍ含有す
ることを特徴とする上記１〜１２のそれぞれに記載の高
純度ニッケル又は高純度ニッケル合金スパッタリングタ
ーゲット
１４．シリコンと反応させてシリサイド膜を形成させる
サリサイド工程で使用することを特徴とする上記１〜１
３のそれぞれに記載の高純度ニッケル又はニッケル合金
スパッタリングターゲット
を提供する。The present invention includes: 1. A high-purity nickel or nickel alloy sputtering target characterized in that oxygen and carbon contents are 20 wtppm or less, respectively. 2. A high-purity nickel or nickel alloy sputtering target characterized by containing oxygen and carbon in an amount of 10 wtppm or less, respectively. 3. High-purity nickel or nickel alloy sputtering target characterized by containing oxygen and carbon in an amount of 1 wtppm or less, respectively. 4. The high-purity nickel or nickel alloy sputtering target according to each of the above 1 to 3, wherein the hydrogen content is 10 wtppm or less. 5. The high-purity nickel or nickel alloy sputtering target according to each of the above 1 to 3, wherein the hydrogen content is 1 wtppm or less. 7. The high-purity nickel or nickel alloy sputtering target according to each of 1 to 5 above, wherein the content of the alloy element and the impurity element excluding gas components such as oxygen, hydrogen, nitrogen, and carbon is less than 10 wtppm. 7. The high-purity nickel or nickel alloy sputtering target according to the above 6, wherein the iron content is 5 ppm or less. 8. The high-purity nickel or nickel alloy sputtering target according to 6 above, wherein the iron content is 2 ppm or less. The alloy element contains at least one element selected from titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, manganese, ruthenium, palladium, platinum, molybdenum, rhenium, and tungsten as the alloy element 1 10. A high-purity nickel alloy sputtering target according to each of 8 to 10. 11. The high-purity nickel alloy sputtering target according to each of 1 to 6 and 9, which contains at least one element selected from iron or cobalt as an alloy element. 11. The high-purity nickel alloy sputtering target according to each of 1 to 10 above, wherein the content of the alloy element is 0.5 to 10 at%. 13. The high purity nickel alloy sputtering target according to each of 1 to 10 above, wherein the content of the alloy element is 1 to 5 at%. 13. The high-purity nickel or high-purity nickel alloy sputtering target according to each of the above 1 to 12, which contains 0.2 to 40 ppm of a lanthanoid element. 1 to 1 used in a salicide process of reacting with silicon to form a silicide film
3. A high-purity nickel or nickel alloy sputtering target according to each of item 3 is provided.
【０００６】また、本発明は
１５．粗ニッケルを電解精製法により金属不純物を除去
した後、電子ビーム溶解等の方法で溶解して高純度ニッ
ケルインゴットを作製し、これを鍛造、圧延等の塑性加
工により厚さを７〜１０ｍｍとした後水素雰囲気中で加
熱して脱酸素、脱炭素を行い、さらにこれを真空雰囲気
中で加熱して脱水素処理を行うことを特徴とする上記１
〜８、１３、１４のそれぞれに記載の高純度ニッケルス
パッタリングターゲットの製造方法
１６．粗ニッケルを電解精製法により金属不純物を除去
した後、高純度合金元素と共に電子ビーム溶解等の方法
で溶解して高純度ニッケル合金インゴットを作製し、こ
れを鍛造、圧延等の塑性加工により厚さを７〜１０ｍｍ
とした後、水素雰囲気中で加熱して脱酸素、脱炭素を行
い、さらにこれを真空雰囲気中で加熱して脱水素処理を
行うことを特徴とする上記１〜１２に記載の高純度ニッ
ケル合金スパッタリングターゲットの製造方法
１７．電子ビーム溶解等の方法で溶解して高純度ニッケ
ル合金インゴットを作製する際に、脱酸効果を高めるた
めに合金元素としてランタノイド系元素を０．２ｐｐｍ
〜４０ｐｐｍ添加することを特徴とする上記１３、１６
に記載の高純度ニッケル合金スパッタリングターゲット
の製造方法
を提供する。The present invention also relates to 15. After removing metallic impurities from the crude nickel by electrolytic refining method, it was melted by a method such as electron beam melting to prepare a high-purity nickel ingot, which was made to have a thickness of 7 to 10 mm by plastic working such as forging and rolling. After that, it is heated in a hydrogen atmosphere for deoxygenation and decarbonization, and further heated in a vacuum atmosphere for dehydrogenation treatment.
15. Manufacturing method of high-purity nickel sputtering target according to each of After removing metallic impurities by electrolytic refining from crude nickel, it is melted together with high-purity alloy elements by a method such as electron beam melting to produce a high-purity nickel alloy ingot, which is then forged and rolled by plastic working to obtain a thickness. 7 to 10 mm
And then heating in a hydrogen atmosphere for deoxygenation and decarbonization, and further for heating in a vacuum atmosphere for dehydrogenation treatment. Manufacturing method of sputtering target 17. When producing a high-purity nickel alloy ingot by melting it with a method such as electron beam melting, 0.2 ppm of lanthanoid-based element as an alloying element in order to enhance the deoxidizing effect.
The above 13, 16 characterized by adding ˜40 ppm
A method for manufacturing the high-purity nickel alloy sputtering target according to 1.
【０００７】[0007]
【発明の実施の形態】本発明は、酸素、炭素の含有量が
それぞれ２０ｗｔｐｐｍ以下である高純度ニッケル又は
ニッケル合金スパッタリングターゲット、好ましくは酸
素、炭素の含有量がそれぞれ１０ｗｔｐｐｍ以下、さら
に好ましくは酸素、炭素の含有量がそれぞれ１ｗｔｐｐ
ｍ以下である高純度ニッケル又はニッケル合金スパッタ
リングターゲットに関する。従来の高純度ニッケルター
ゲットは、ガス成分を除いて４Ｎ５（９９．９９５ｗｔ
％）程度のものであり、酸素あるいは炭素含有量がそれ
ぞれ５０〜８０ｗｔｐｐｍで、窒素含有量も５０ｗｔｐ
ｐｍと高いものであった。BEST MODE FOR CARRYING OUT THE INVENTION The present invention is a high-purity nickel or nickel alloy sputtering target having oxygen and carbon contents of 20 wtppm or less, preferably oxygen and carbon contents of 10 wtppm or less, and more preferably oxygen, respectively. Each carbon content is 1wtpp
It relates to a high-purity nickel or nickel alloy sputtering target of m or less. The conventional high-purity nickel target is 4N5 (99.995 wt.
%), The oxygen or carbon content is 50 to 80 wtppm, and the nitrogen content is 50 wtp.
It was as high as pm.
【０００８】このようなガス成分、特に酸素含有量が高
いターゲットを使用してゲート電極Ｎｉ膜をスパッタリ
ング成膜し、さらに熱処理（アニール）によりニッケル
シリサイド膜の形成を行う、すなわちサリサイドプロセ
スによりシリサイド処理した場合、ニッケルが酸素と反
応して酸化膜を形成し、この酸化膜がシリサイド反応を
阻害するばかりでなく、シリサイド膜とシリコン基板と
の界面領域に、これによる凹凸のある絶縁膜を形成し、
さらにはシリサイド膜の凝集の原因となるなど、界面の
ラフネスによって、Ｎ＋／Ｐの接合特性が劣化し、抵抗
が増加するという問題があった。特に、ニッケルシリサ
イドは他のシリサイド材料に比べても非常に酸化され易
く、一層その傾向が強い。炭素含有量に関しては、還元
剤として作用することも考えられるために、悪影響を及
ぼさないように思われるが、炭素含有量がバラツキつい
た場合は、界面ラフネスの変動要因になってしまうので
低く抑えることが必要である。A gate electrode Ni film is formed by sputtering using a target having such a high gas content, particularly a high oxygen content, and a nickel silicide film is formed by heat treatment (annealing), that is, a silicide treatment by a salicide process. In this case, nickel reacts with oxygen to form an oxide film, and this oxide film not only hinders the silicide reaction, but also forms an uneven insulating film in the interface region between the silicide film and the silicon substrate. ,
Further, there is a problem that the N + / P junction characteristics are deteriorated due to the roughness of the interface, which causes the aggregation of the silicide film, and the resistance increases. In particular, nickel silicide is much more easily oxidized than other silicide materials, and this tendency is even stronger. Regarding the carbon content, since it may also act as a reducing agent, it does not seem to have an adverse effect, but if the carbon content varies, it will be a factor for varying the interfacial roughness, so keep it low. It is necessary.
【０００９】従来は、このような接合特性の低下を成膜
プロセスで改善しようという試みがあったが、この界面
ラフネスを十分に制御できるものではなかった。本発明
は、スパッタリングターゲット中のガス成分である酸
素、炭素を著しく低減することにより、この問題を一挙
に解決することが可能となった。また、高純度ニッケル
又はニッケル合金スパッタリングターゲット中の水素が
１０ｗｔｐｐｍより好ましくは１ｗｔｐｐｍ以下である
ことが望ましい。このようなガス成分を除去した高純度
ニッケル又はニッケル合金スパッタリングターゲット
は、上記のようにシリサイド膜の特性を改善するだけで
なく、酸素、炭素、窒素、水素、フッ素、硫黄等のガス
成分に起因するスパッタリング中のスプラッシュ、異常
放電、パーティクル等の発生が減少するという特徴も有
する。また、合金元素及び酸素、水素、窒素、炭素等の
ガス成分を除く不純物元素の含有量が１０ｗｔｐｐｍ未
満、すなわち５Ｎの純度を持つ高純度ニッケル又はニッ
ケル合金スパッタリングターゲットとすることにより、
不純物により引き起こされる界面ラフネスの悪化を抑制
できるという優れた効果を有する。Conventionally, there has been an attempt to improve such deterioration of the bonding characteristics by a film forming process, but this interface roughness cannot be sufficiently controlled. The present invention has made it possible to solve this problem all at once by significantly reducing oxygen and carbon which are gas components in the sputtering target. Further, it is desirable that hydrogen in the high-purity nickel or nickel alloy sputtering target is 10 wtppm or more, preferably 1 wtppm or less. The high-purity nickel or nickel alloy sputtering target from which such a gas component is removed not only improves the characteristics of the silicide film as described above, but also is caused by a gas component such as oxygen, carbon, nitrogen, hydrogen, fluorine, and sulfur. It also has a feature that the generation of splash, abnormal discharge, particles, etc. during sputtering is reduced. Further, the content of the impurity element excluding the gas components such as oxygen, hydrogen, nitrogen, and carbon is less than 10 wtppm, that is, by using a high-purity nickel or nickel alloy sputtering target having a purity of 5N,
It has an excellent effect that the deterioration of the interfacial roughness caused by impurities can be suppressed.
【００１０】さらに本発明は、高純度ニッケル合金スパ
ッタリングターゲット中の合金元素として、チタン、ジ
ルコニウム、ハフニウム、バナジウム、ニオブ、タンタ
ル、クロム、モリブデン、レニウムから選択した少なく
とも１種類以上の元素を含有させる。合金元素の含有量
としては０．５〜１０ａｔ％である。上記の通り、ニッ
ケルシリサイドは、準安定相であるＮｉＳｉと安定相で
あるＮｉＳｉ２相があり、７００°Ｃを超える熱処理温
度ではこの安定相であるＮｉＳｉ２相に相転移してしま
うという問題を指摘したが、これらの合金元素を添加す
ることにより、安定相であるＮｉＳｉ２相への転移を遅
らせ、かつ抑制するのに極めて有効である。０．５ａｔ
％未満では効果がなく、また１０ａｔ％を超えると抵抗
率が高くなるので１０ａｔ％以下とする必要があり、好
ましくは１〜５ａｔ％である。これによって、抵抗率が
高いＮｉＳｉ２相の形成及びシリサイド化反応における
Ｓｉの消費量を抑制できる大きな効果が得られる。さら
に合金元素としては、ランタノイド系元素を０．２ｐｐ
ｍ〜４０ｐｐｍ添加することで、合金作製を溶解する工
程で脱酸効果を向上させることもできる。これらは少量
で効果的にＮｉＳｉ２相への相転移を抑制できる。下記
実施例及び比較例においては、上記合金元素のうち、チ
タンとニオブの添加の例を示すが、その他の元素を添加
した合金においても同様の結果が得られた。Further, according to the present invention, at least one element selected from titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum and rhenium is contained as an alloying element in the high purity nickel alloy sputtering target. The content of alloying elements is 0.5 to 10 at%. As described above, nickel silicide has a metastable phase of NiSi and a stable phase of NiSi 2 phase, and at a heat treatment temperature exceeding 700 ° C., a phase transition to the stable NiSi 2 phase occurs. As pointed out, the addition of these alloying elements is extremely effective in delaying and suppressing the transition to the stable phase NiSi 2 phase. 0.5 at
If it is less than 10% by weight, no effect is obtained, and if it exceeds 10 at%, the resistivity increases. Therefore, it is necessary to set it to 10 at% or less, preferably 1 to 5 at%. As a result, a large effect that the consumption of Si in the formation of the NiSi 2 phase having a high resistivity and the silicidation reaction can be suppressed can be obtained. Furthermore, as an alloying element, a lanthanoid element is 0.2 pp
By adding m to 40 ppm, the deoxidizing effect can be improved in the step of melting the alloy preparation. A small amount of these can effectively suppress the phase transition to the NiSi 2 phase. In the following examples and comparative examples, examples of addition of titanium and niobium among the above alloy elements are shown, but similar results were obtained for alloys to which other elements were added.
【００１１】本発明の高純度ニッケルスパッタリングタ
ーゲットを製造するに際しては、粗ニッケル（４Ｎレベ
ル）を電解精製法により金属不純物を除去した後、電子
ビーム溶解により精製して高純度ニッケルインゴットを
作製する。次に、このインゴットを鍛造、圧延等の塑性
加工により厚さを７〜１０ｍｍ程度に薄くした後、この
ニッケル板を水素雰囲気中で加熱し脱酸素、脱炭素を行
い、さらにこれを連続して真空雰囲気中で加熱し、脱水
素処理を行う。これによって得たニッケル板を、最終冷
間圧延及び再結晶焼鈍して高純度ニッケルスパッタリン
グターゲットを製造する。この最終冷間圧延、再結晶焼
鈍は、圧延率３０％以上の圧延と再結晶焼鈍を少なくと
も２回繰返し、結晶粒を調整することが望ましい。In producing the high-purity nickel sputtering target of the present invention, crude nickel (4N level) is electrolytically refined to remove metal impurities and then purified by electron beam melting to produce a high-purity nickel ingot. Next, this ingot is thinned to a thickness of about 7 to 10 mm by plastic working such as forging and rolling, and then this nickel plate is heated in a hydrogen atmosphere for deoxidation and decarbonization, and this is continuously performed. Dehydrogenation is performed by heating in a vacuum atmosphere. The nickel plate thus obtained is subjected to final cold rolling and recrystallization annealing to manufacture a high-purity nickel sputtering target. In this final cold rolling and recrystallization annealing, it is desirable to repeat rolling at a rolling rate of 30% or more and recrystallization annealing at least twice to adjust the crystal grains.
【００１２】高純度ニッケル合金スパッタリングターゲ
ットを製造する場合は、基本的には上記と同様である
が、電子ビーム溶解や、コールドウォールタイプの溶解
炉で溶解する際に高純度ニッケルと共に高純度の合金元
素を添加し、同時に溶解して高純度ニッケル合金インゴ
ットを作製する。その後同様の工程を経て、高純度ニッ
ケル合金スパッタリングターゲットを製造する。以上に
より、酸素等のガス成分及びその他の不純物元素を極め
て低減させた高純度ニッケルスパッタリングターゲット
及び高純度ニッケル合金スパッタリングターゲットを製
造することができる。When a high-purity nickel alloy sputtering target is manufactured, it is basically the same as the above, but when it is melted in an electron beam melting or a cold wall type melting furnace, it is a high-purity alloy together with high-purity nickel. An element is added and simultaneously melted to produce a high-purity nickel alloy ingot. After that, a high-purity nickel alloy sputtering target is manufactured through similar steps. As described above, a high-purity nickel sputtering target and a high-purity nickel alloy sputtering target in which gas components such as oxygen and other impurity elements are extremely reduced can be manufactured.
【００１３】[0013]
【実施例】次に、実施例に基づいて説明する。なお、こ
れらは本発明の理解を容易にするためのものであり、本
発明はこれらに制限されるものではない。EXAMPLES Next, examples will be described. These are for facilitating the understanding of the present invention, and the present invention is not limited to these.
【００１４】厚さ１０ｍｍのニッケル板を、モリブデン
製ヒーター炉にて１０００°Ｃ、１０５０°Ｃ、１１０
０°Ｃ、１１５０°Ｃ、１２００°Ｃ、１２５０°Ｃで
水素処理５時間後、急速アルゴンガス置換後連続して真
空処理３時間（到達真空度５×１０−５ｔｏｒｒ）行
い、水素、真空処理による脱酸素、脱炭素、脱水素効果
を調べた。その結果をグラフとして、図１に示す。図１
のグラフに示すように、熱処理温度の上昇と共に、ガス
成分の含有量は低下する。下記実施例においては、これ
らの条件を使用して適宜ガス成分を調節する。なお、厚
さ３ｍｍのニッケルターゲットを作製するには、脱酸素
後の厚さが７ｍｍ以上必要である。しかし、約１０ｍｍ
を超えると脱酸素時間が長くなり適当でない。A nickel plate having a thickness of 10 mm was heated at 1000 ° C., 1050 ° C., 110 at a heater furnace made of molybdenum.
After hydrogen treatment at 0 ° C, 1150 ° C, 1200 ° C, and 1250 ° C for 5 hours, rapid argon gas replacement was performed and vacuum treatment was continuously performed for 3 hours (attainment vacuum degree of 5 × 10 −5 torr), hydrogen, vacuum. The effects of deoxidation, decarbonization and dehydrogenation by the treatment were investigated. The result is shown as a graph in FIG. Figure 1
As shown in the graph, the content of the gas component decreases as the heat treatment temperature rises. In the examples below, these conditions are used to adjust the gas composition accordingly. In addition, in order to produce a nickel target having a thickness of 3 mm, the thickness after deoxidation needs to be 7 mm or more. However, about 10 mm
If it exceeds, deoxidation time becomes long and it is not suitable.
【００１５】（実施例１）粗ニッケル（純度４Ｎ（ガス
成分除く）、ナトリウム３０ｗｔｐｐｍ、鉄８ｗｔｐｐ
ｍ、コバルト５ｗｔｐｐｍ）を電解精製にて高純度化し
た。 これを電子ビーム溶解法にて５×１０−４〜５×
１０−５ｔｏｒｒ程度の真空雰囲気で溶解してインゴッ
ト（φ１５０×６０ｍｍ）を作製した。これを９００°
Ｃで熱間鍛造して溶解凝固組織を破壊して、さらに厚さ
を１０ｍｍ板にした。このニッケル板を塩酸で表面酸化
膜を除去したのち、３０％の圧延率で冷間圧延し、塩酸
で表面清浄してから３２５°Ｃで真空熱処理（到達真空
度５×１０− ５ｔｏｒｒ以下）した。その後さらに３０
％の圧延率で冷間圧延し、塩酸で表面清浄してから３２
５°Ｃで真空熱処理（真空度５×１０−５ｔｏｒｒ以
下）した。これから機械加工にて厚さ３ｍｍ、φ３００
ｍｍの高純度ニッケルターゲットを作製した。酸素、炭
素、水素及びガス成分と合金元素以外の不純物含有量を
表１に示す（ガス成分以外は、ＧＤＭＳ（グロー放電質
量分析法）による分析結果であり、以下同様である）。
表１に示すように、酸素含有量１８ｗｔｐｐｍ、炭素含
有量１６ｗｔｐｐｍ、水素含有量１２ｗｔｐｐｍ、ガス
成分及び合金成分以外の不純物含有量９ｗｔｐｐｍであ
った。(Example 1) Crude nickel (purity 4N (excluding gas components), sodium 30 wtppm, iron 8 wtpp
m, cobalt 5 wtppm) was highly purified by electrolytic refining. This is 5 × 10 −4 to 5 × by an electron beam melting method.
It was melted in a vacuum atmosphere of about 10 −5 torr to prepare an ingot (φ150 × 60 mm). This is 900 °
The molten solidified structure was destroyed by hot forging with C to obtain a plate having a thickness of 10 mm. Thereafter the nickel plate was to remove surface oxide film with hydrochloric acid, then cold-rolled at a rolling reduction of 30%, the vacuum heat treatment after surface cleaning with 325 ° C with hydrochloric acid (ultimate vacuum 5 × 10 - 5 torr or less) did. 30 more after that
32% after cold rolling at a rolling rate of% and cleaning the surface with hydrochloric acid
Vacuum heat treatment (vacuum degree 5 × 10 −5 torr or less) was performed at 5 ° C. It will be machined to a thickness of 3 mm and a diameter of 300 mm.
A mm high-purity nickel target was prepared. The content of impurities other than oxygen, carbon, hydrogen, and gas components and alloying elements is shown in Table 1 (other than gas components, analysis results by GDMS (glow discharge mass spectrometry), and the same applies hereinafter).
As shown in Table 1, the oxygen content was 18 wtppm, the carbon content was 16 wtppm, the hydrogen content was 12 wtppm, and the impurity content other than the gas component and the alloy component was 9 wtppm.
【００１６】（実施例２）粗ニッケル（純度４Ｎ（ガス
成分除く）、ナトリウム３０ｗｔｐｐｍ、鉄８ｗｔｐｐ
ｍ、コバルト５ｗｔｐｐｍ）を電解精製にて高純度化し
た。 これを電子ビーム溶解法にて５×１０−４〜５×
１０−５ｔｏｒｒ程度の真空雰囲気で溶解してインゴッ
ト（φ１５０×６０ｍｍ）を作製した。これを９００°
Ｃで熱間鍛造して溶解凝固組織を破壊して、さらに厚さ
を１０ｍｍ板にした。このニッケル板を塩酸で表面酸化
膜を除去したのち、モリブデン製ヒーターの熱処理炉に
て、水素雰囲気中１０５０°Ｃで５時間熱処理して、脱
酸素、脱炭素処理を行った。その後急速アルゴンガス置
換後、連続して１０５０°Ｃで３時間真空熱処理（到達
真空度５×１０−５ｔｏｒｒ）した。このニッケル板を
３０％の圧延率で冷間圧延し、塩酸で表面清浄してから
３２５°Ｃで真空熱処理（到達真空度５×１０−５ｔｏ
ｒｒ）した。その後さらに３０％の圧延率で冷間圧延
し、塩酸で表面清浄してから３２５°Ｃで真空熱処理
（到達真空度５×１０−５ｔｏｒｒ以下）した。これか
ら厚さ３ｍｍ、φ３００ｍｍの高純度ニッケルターゲッ
トを作製した。酸素、炭素、水素及びガス成分と合金元
素以外の不純物含有量を同様に表１に示す。表１に示す
ように、酸素含有量８ｗｔｐｐｍ、炭素含有量７ｗｔｐ
ｐｍ、水素含有量５ｗｔｐｐｍ、ガス成分及び合金成分
以外の不純物含有量７ｗｔｐｐｍであった。(Example 2) Crude nickel (purity 4N (excluding gas components), sodium 30 wtppm, iron 8 wtpp
m, cobalt 5 wtppm) was highly purified by electrolytic refining. This is 5 × 10 −4 to 5 × by an electron beam melting method.
It was melted in a vacuum atmosphere of about 10 −5 torr to prepare an ingot (φ150 × 60 mm). This is 900 °
The molten solidified structure was destroyed by hot forging with C to obtain a plate having a thickness of 10 mm. After removing the surface oxide film from this nickel plate with hydrochloric acid, it was heat-treated at 1050 ° C. for 5 hours in a hydrogen atmosphere in a heat treatment furnace made of a molybdenum heater for deoxidation and decarbonization. Then, after rapid argon gas replacement, vacuum heat treatment (ultimate vacuum degree 5 × 10 −5 torr) was continuously performed at 1050 ° C. for 3 hours. This nickel plate was cold-rolled at a rolling rate of 30%, surface-cleaned with hydrochloric acid, and then vacuum heat-treated at 325 ° C. (achieved vacuum degree 5 × 10 −5 to
rr). Then, it was further cold-rolled at a rolling ratio of 30%, the surface was cleaned with hydrochloric acid, and then vacuum heat treatment was performed at 325 ° C. (the ultimate vacuum degree was 5 × 10 −5 torr or less). From this, a high-purity nickel target having a thickness of 3 mm and a diameter of 300 mm was produced. The oxygen, carbon, hydrogen and gas components and the content of impurities other than alloying elements are also shown in Table 1. As shown in Table 1, oxygen content 8wtppm, carbon content 7wtp
pm, the hydrogen content was 5 wtppm, and the impurity content other than the gas component and the alloy component was 7 wtppm.
【００１７】（実施例３）粗ニッケル（純度４Ｎ（ガス
成分除く）、ナトリウム３０ｗｔｐｐｍ、鉄８ｗｔｐｐ
ｍ、コバルト５ｗｔｐｐｍ）を電解精製にて高純度化し
た。 これを電子ビーム溶解法にて５×１０−４〜５×
１０−５ｔｏｒｒ程度の真空雰囲気で溶解してインゴッ
ト（φ１５０×６０ｍｍ）を作製した。これを９００°
Ｃで熱間鍛造して溶解凝固組織を破壊して、さらに厚さ
を１０ｍｍ板にした。このニッケル板を塩酸で表面酸化
膜を除去したのち、モリブデン製ヒーターの熱処理炉に
て、水素雰囲気中１２５０°Ｃで５時間熱処理して、脱
酸素、脱炭素処理を行った。その後急速アルゴンガス置
換後、連続して１２５０°Ｃで３時間真空熱処理（到達
真空度５×１０−５ｔｏｒｒ以下）した。このニッケル
板を３０％の圧延率で冷間圧延し、塩酸で表面清浄して
から３２５°Ｃで真空熱処理（到達真空度５×１０−５
ｔｏｒｒ以下）した。その後、さらに３０％の圧延率で
冷間圧延し、塩酸で表面清浄してから３２５°Ｃで真空
熱処理（到達真空度５×１０−５ｔｏｒｒ以下）した。
これから厚さ３ｍｍ、φ３００ｍｍの高純度ニッケルタ
ーゲットを作製した。酸素、炭素、水素及びガス成分と
合金元素以外の不純物含有量を同様に表１に示す。表１
に示すように、酸素含有量１ｗｔｐｐｍ、炭素含有量１
ｗｔｐｐｍ、水素含有量１ｗｔｐｐｍ、ガス成分及び合
金成分以外の不純物含有量１ｗｔｐｐｍ未満であった。(Example 3) Crude nickel (purity 4N (excluding gas components), sodium 30 wtppm, iron 8 wtpp
m, cobalt 5 wtppm) was highly purified by electrolytic refining. This is 5 × 10 −4 to 5 × by an electron beam melting method.
It was melted in a vacuum atmosphere of about 10 −5 torr to prepare an ingot (φ150 × 60 mm). This is 900 °
The molten solidified structure was destroyed by hot forging with C to obtain a plate having a thickness of 10 mm. After removing the surface oxide film from this nickel plate with hydrochloric acid, it was heat-treated at 1250 ° C. for 5 hours in a hydrogen atmosphere in a heat treatment furnace of a molybdenum heater to perform deoxidation and decarbonization treatments. Then, after rapid argon gas replacement, vacuum heat treatment (ultimate vacuum degree of 5 × 10 −5 torr or less) was continuously performed at 1250 ° C. for 3 hours. This nickel plate was cold-rolled at a rolling rate of 30%, surface-cleaned with hydrochloric acid, and then vacuum heat-treated at 325 ° C. (achieved vacuum degree 5 × 10 −5
less than torr). Then, it was further cold-rolled at a rolling rate of 30%, the surface was cleaned with hydrochloric acid, and then vacuum heat treatment was performed at 325 ° C. (the ultimate vacuum degree was 5 × 10 −5 torr or less).
From this, a high-purity nickel target having a thickness of 3 mm and a diameter of 300 mm was produced. The oxygen, carbon, hydrogen and gas components and the content of impurities other than alloying elements are also shown in Table 1. Table 1
As shown in, oxygen content 1wtppm, carbon content 1
The content was less than 1 wtppm, and the content of impurities other than gas components and alloy components was less than 1 wtppm.
【００１８】[0018]
【表１】 [Table 1]
【００１９】上記実施例１〜３の高純度ニッケルターゲ
ットを用いて、シリコン膜上にニッケル膜をスパッタリ
ング成膜し、窒素雰囲気中５００°ＣでＲＴＡ（Ｒａｐ
ｉｄＴｈｅｒｍａｌ Ａｎｎｅａｌ）法にて熱処理し
て、ニッケルシリサイド膜を作製した。この膜の断面を
ＴＥＭ観察して界面ラフネスの様子を観察した。さらに
これらの膜を窒素雰囲気で加熱して、ＸＲＤ回折法にて
ニッケルシリサイド（ＮｉＳｉ）のＮｉＳｉ２への結晶
構造変化の温度を調べた。この結果を、上記表１に示
す。表１に示すように、実施例１〜３については、いず
れも界面ラフネスは良好である（なお、界面ラフネスは
３０〜４０ｎｍを良好とし、５０ｎｍ以上を不良とし
た。以下同様である。）。Using the high-purity nickel targets of Examples 1 to 3 above, a nickel film was formed by sputtering on a silicon film, and RTA (Rap) was performed at 500 ° C. in a nitrogen atmosphere.
A nickel silicide film was formed by heat treatment by the id Thermal Anneal method. The state of the interface roughness was observed by TEM observation of the cross section of this film. Further, these films were heated in a nitrogen atmosphere, and the temperature of the crystal structure change of nickel silicide (NiSi) into NiSi 2 was examined by XRD diffraction method. The results are shown in Table 1 above. As shown in Table 1, in each of Examples 1 to 3, the interface roughness was good (note that the interface roughness of 30 to 40 nm was good and 50 nm or more was bad. The same applies hereinafter).
【００２０】（比較例１）純度９９．９９５ｗｔ％の高
純度ニッケルターゲット板を３０％の圧延率で冷間圧延
し、塩酸で表面清浄してから３２５°Ｃで真空熱処理
（真空度５×１０− ５ｔｏｒｒ以下）した。その後さら
に３０％の圧延率で冷間圧延し、塩酸で表面清浄してか
ら３２５°Ｃで真空熱処理（真空度５×１０−５ｔｏｒ
ｒ以下）した。これから厚さ３ｍｍ、φ３００ｍｍの高
純度ニッケルターゲットを作製した。この場合のガス成
分は、酸素含有量５３ｗｔｐｐｍ、炭素含有量３６ｗｔ
ｐｐｍ、水素含有量２２ｗｔｐｐｍと高く、またガス成
分及び合金成分以外の不純物含有量４２ｗｔｐｐｍと高
かった。Comparative Example 1 A high-purity nickel target plate having a purity of 99.995 wt% was cold-rolled at a rolling rate of 30%, the surface was cleaned with hydrochloric acid, and then vacuum heat treatment was performed at 325 ° C. (vacuum degree 5 × 10 5). - 5 torr or less) was. After that, it is further cold rolled at a rolling rate of 30%, the surface is cleaned with hydrochloric acid, and then vacuum heat treatment is performed at 325 ° C. (vacuum degree 5 × 10 −5 torr).
r or less). From this, a high-purity nickel target having a thickness of 3 mm and a diameter of 300 mm was produced. In this case, the gas component is oxygen content 53 wtppm, carbon content 36 wt
ppm and hydrogen content were as high as 22 wtppm, and the content of impurities other than gas components and alloy components was as high as 42 wtppm.
【００２１】（比較例２）純度９９．９９５ｗｔ％の高
純度ニッケルターゲット板を３０％の圧延率で冷間圧延
し、塩酸で表面清浄してから３２５°Ｃで真空熱処理
（真空度５×１０− ５ｔｏｒｒ以下）した。その後さら
に３０％の圧延率で冷間圧延し、塩酸で表面清浄してか
ら３２５°Ｃで真空熱処理（真空度５×１０−５ｔｏｒ
ｒ以下）した。これから厚さ３ｍｍ、φ３００ｍｍの高
純度ニッケルターゲットを作製した。この場合のガス成
分は、酸素含有量４０ｗｔｐｐｍ、炭素含有量２８ｗｔ
ｐｐｍ、水素含有量３０ｗｔｐｐｍと高く、またガス成
分及び合金成分以外の不純物含有量２８ｗｔｐｐｍと高
かった。Comparative Example 2 A high-purity nickel target plate having a purity of 99.995 wt% was cold-rolled at a rolling rate of 30%, the surface was cleaned with hydrochloric acid, and then vacuum heat treatment was performed at 325 ° C. (vacuum degree 5 × 10 5). - 5 torr or less) was. After that, it is further cold rolled at a rolling rate of 30%, the surface is cleaned with hydrochloric acid, and then vacuum heat treatment is performed at 325 ° C. (vacuum degree 5 × 10 −5 torr).
r or less). From this, a high-purity nickel target having a thickness of 3 mm and a diameter of 300 mm was produced. The gas component in this case is 40 wtppm oxygen content, 28 wt% carbon content.
ppm and hydrogen content were as high as 30 wtppm, and impurities content other than gas components and alloy components were as high as 28 wtppm.
【００２２】（比較例３）純度９９．９９５ｗｔ％の高
純度ニッケルターゲット板を３０％の圧延率で冷間圧延
し、塩酸で表面清浄してから３２５°Ｃで真空熱処理
（真空度５×１０− ５ｔｏｒｒ以下）した。その後さら
に３０％の圧延率で冷間圧延し、塩酸で表面清浄してか
ら３２５°Ｃで真空熱処理（真空度５×１０−５ｔｏｒ
ｒ以下）した。これから厚さ３ｍｍ、φ３００ｍｍの高
純度ニッケルターゲットを作製した。この場合のガス成
分は、酸素含有量３５ｗｔｐｐｍ、炭素含有量２６ｗｔ
ｐｐｍ、水素含有量３５ｗｔｐｐｍと高く、またガス成
分及び合金成分以外の不純物含有量８ｗｔｐｐｍと高か
った。(Comparative Example 3) A high-purity nickel target plate having a purity of 99.995 wt% was cold-rolled at a rolling rate of 30%, the surface was cleaned with hydrochloric acid, and then vacuum heat treatment was performed at 325 ° C (vacuum degree 5 x 10). - 5 torr or less) was. After that, it is further cold rolled at a rolling rate of 30%, the surface is cleaned with hydrochloric acid, and then vacuum heat treatment is performed at 325 ° C. (vacuum degree 5 × 10 −5 torr).
r or less). From this, a high-purity nickel target having a thickness of 3 mm and a diameter of 300 mm was produced. In this case, the gas components are oxygen content 35 wtppm, carbon content 26 wt
ppm and hydrogen content were as high as 35 wtppm, and impurities content other than gas components and alloy components were as high as 8 wtppm.
【００２３】比較例１〜３のニッケルターゲットを用い
て、実施例と同様に、シリコン膜上にニッケル膜をスパ
ッタリング成膜し、さらに窒素雰囲気中５００°ＣでＲ
ＴＡ法にて熱処理してニッケルシリサイド膜を作製し
た。この膜の断面をＴＥＭ観察して界面ラフネスの様子
を観察した。さらに、この膜を窒素雰囲気中ＲＴＡ法で
加熱して、ＸＲＤ回折法にてニッケルシリサイドのＮｉ
Ｓｉ２への結晶構造変化を観察した。この結果を、同様
に上記表１に示す。表１に示すように、界面ラフネスは
いずれも不良であった。Using the nickel targets of Comparative Examples 1 to 3, a nickel film was formed on the silicon film by sputtering in the same manner as in the example, and further, R at 500 ° C. in a nitrogen atmosphere.
A nickel silicide film was produced by heat treatment by the TA method. The state of the interface roughness was observed by TEM observation of the cross section of this film. Further, this film is heated by a RTA method in a nitrogen atmosphere, and nickel of nickel silicide is measured by an XRD diffraction method.
The crystal structure change to Si 2 was observed. The results are also shown in Table 1 above. As shown in Table 1, the interface roughness was poor.
【００２４】（実施例４）Ｔｉ５ａｔ％をＥＢ溶解時に
添加したことを除き、実施例１の材料及び製造条件で、
高純度ニッケル合金ターゲットを作製した。酸素、炭
素、水素及びガス成分と合金元素以外の不純物含有量
を、同様に表１に示す。表１に示すように、酸素含有量
１２ｗｔｐｐｍ、炭素含有量１１ｗｔｐｐｍ、水素含有
量１３ｗｔｐｐｍ、ガス成分及び合金成分以外の不純物
含有量８ｗｔｐｐｍであった。(Example 4) The material and manufacturing conditions of Example 1 were changed except that 5 at% of Ti was added during EB dissolution.
A high-purity nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, the oxygen content was 12 wtppm, the carbon content was 11 wtppm, the hydrogen content was 13 wtppm, and the impurity content other than the gas component and the alloy component was 8 wtppm.
【００２５】（実施例５）Ｔｉ５ａｔ％をＥＢ溶解時に
添加したことを除き、実施例２の材料及び製造条件で、
高純度ニッケル合金ターゲットを作製した。酸素、炭
素、水素及びガス成分と合金元素以外の不純物含有量
を、同様に表１に示す。表１に示すように、酸素含有量
６ｗｔｐｐｍ、炭素含有量９ｗｔｐｐｍ、水素含有量６
ｗｔｐｐｍ、ガス成分及び合金成分以外の不純物含有量
９ｗｔｐｐｍであった。(Example 5) Using the materials and manufacturing conditions of Example 2, except that 5 at% of Ti was added during EB dissolution.
A high-purity nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, oxygen content 6 wtppm, carbon content 9 wtppm, hydrogen content 6
The content of impurities other than wtppm and gas components and alloy components was 9 wtppm.
【００２６】（実施例６）Ｔｉ５ａｔ％をＥＢ溶解時に
添加したことを除き、実施例３の材料及び製造条件で、
高純度ニッケル合金ターゲットを作製した。酸素、炭
素、水素及びガス成分と合金元素以外の不純物含有量
を、同様に表１に示す。表１に示すように、酸素含有量
１ｗｔｐｐｍ、炭素含有量１ｗｔｐｐｍ、水素含有量１
ｗｔｐｐｍ、ガス成分及び合金成分以外の不純物含有量
１ｗｔｐｐｍ未満であった。(Example 6) Using the materials and manufacturing conditions of Example 3, except that 5 at% of Ti was added during EB dissolution.
A high-purity nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, oxygen content 1 wtppm, carbon content 1 wtppm, hydrogen content 1
The content of impurities other than wtppm, gas components and alloy components was less than 1 wtppm.
【００２７】上記実施例４〜６の高純度ニッケルターゲ
ットを用いて、シリコン膜上にニッケル膜をスパッタリ
ング成膜し、窒素雰囲気中５００°ＣでＲＴＡ（Ｒａｐ
ｉｄＴｈｅｒｍａｌ Ａｎｎｅａｌ）法にて熱処理し
て、ニッケルシリサイド膜を作製した。この膜の断面を
ＴＥＭ観察して界面ラフネスの様子を観察した。さらに
これらの膜を窒素雰囲気中ＲＴＡ法で加熱して、ＸＲＤ
回折法にてニッケルシリサイド（ＮｉＳｉ）のＮｉＳｉ
２への結晶構造変化の温度を調べた。この結果を、同様
に上記表１に示す。表１に示すように、実施例４〜６に
ついては、いずれも界面ラフネスは良好である。また、
ニッケルシリサイド相変化温度は７５０°Ｃ以上とな
り、高温での熱処理でも相変化が抑制できるという効果
が得られた。この温度は、ニッケル合金としたことによ
り、より高温側にシフトしたものであり、純ニッケルに
比べてさらに良好な特性を有する。Using the high-purity nickel targets of Examples 4 to 6, a nickel film was formed by sputtering on a silicon film, and RTA (Rap) was performed at 500 ° C. in a nitrogen atmosphere.
A nickel silicide film was formed by heat treatment by the id Thermal Anneal method. The state of the interface roughness was observed by TEM observation of the cross section of this film. Further, these films are heated by the RTA method in a nitrogen atmosphere to perform XRD.
NiSi of nickel silicide (NiSi) by diffraction method
The temperature at which the crystal structure changed to 2 was investigated. The results are also shown in Table 1 above. As shown in Table 1, in each of Examples 4 to 6, the interface roughness is good. Also,
The nickel silicide phase change temperature was 750 ° C. or higher, and the effect that the phase change could be suppressed even by heat treatment at high temperature was obtained. This temperature is shifted to a higher temperature side by using the nickel alloy, and has better characteristics than pure nickel.
【００２８】（比較例４）Ｔｉ５ａｔ％をＥＢ溶解時に
添加したことを除き、比較例１の材料及び製造条件で、
ニッケル合金ターゲットを作製した。酸素、炭素、水素
及びガス成分と合金元素以外の不純物含有量を、同様に
表１に示す。表１に示すように、酸素含有量６０ｗｔｐ
ｐｍ、炭素含有量４５ｗｔｐｐｍ、水素含有量１５ｗｔ
ｐｐｍ、ガス成分及び合金成分以外の不純物含有量４３
ｗｔｐｐｍであった。(Comparative Example 4) Except that 5 at% of Ti was added during EB dissolution, the material and manufacturing conditions of Comparative Example 1 were changed to
A nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, the oxygen content is 60 wtp
pm, carbon content 45wtppm, hydrogen content 15wt
Impurity content other than ppm, gas components and alloy components 43
It was wtppm.
【００２９】（比較例５）Ｔｉ５ａｔ％をＥＢ溶解時に
添加したことを除き、比較例２の材料及び製造条件で、
ニッケル合金ターゲットを作製した。酸素、炭素、水素
及びガス成分と合金元素以外の不純物含有量を、同様に
表１に示す。表１に示すように、酸素含有量３５ｗｔｐ
ｐｍ、炭素含有量３２ｗｔｐｐｍ、水素含有量２５ｗｔ
ｐｐｍ、ガス成分及び合金成分以外の不純物含有量２５
ｗｔｐｐｍであった。(Comparative Example 5) With the material and manufacturing conditions of Comparative Example 2, except that 5 at% of Ti was added during EB dissolution.
A nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, the oxygen content is 35 wtp
pm, carbon content 32wtppm, hydrogen content 25wt
Impurity content other than ppm, gas components and alloy components 25
It was wtppm.
【００３０】（比較例６）Ｔｉ５ａｔ％をＥＢ溶解時に
添加したことを除き、比較例３の材料及び製造条件で、
ニッケル合金ターゲットを作製した。酸素、炭素、水素
及びガス成分と合金元素以外の不純物含有量を、同様に
表１に示す。表１に示すように、酸素含有量３２ｗｔｐ
ｐｍ、炭素含有量２３ｗｔｐｐｍ、水素含有量２５ｗｔ
ｐｐｍ、ガス成分及び合金成分以外の不純物含有量９ｗ
ｔｐｐｍ未満であった。(Comparative Example 6) With the material and manufacturing conditions of Comparative Example 3, except that 5 at% of Ti was added during EB dissolution.
A nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, the oxygen content is 32 wtp
pm, carbon content 23wtppm, hydrogen content 25wt
Impurity content other than ppm, gas components and alloy components 9w
It was less than tppm.
【００３１】上記比較例４〜６の高純度ニッケルターゲ
ットを用いて、シリコン膜上にニッケル膜をスパッタリ
ング成膜し、窒素雰囲気中５００°ＣでＲＴＡ（Ｒａｐ
ｉｄＴｈｅｒｍａｌ Ａｎｎｅａｌ）法にて熱処理し
て、ニッケルシリサイド膜を作製した。この膜の断面を
ＴＥＭ観察して界面ラフネスの様子を観察した。さらに
これらの膜を窒素雰囲気中、ＲＴＡ法で加熱して、ＸＲ
Ｄ回折法にてニッケルシリサイド（ＮｉＳｉ）のＮｉＳ
ｉ２への結晶構造変化の温度を調べた。この結果を、同
様に上記表１に示す。表１に示すように、比較例４〜６
については、いずれも界面ラフネスは不良であった。Using the high-purity nickel targets of Comparative Examples 4 to 6, a nickel film was formed by sputtering on a silicon film, and RTA (Rap) was performed at 500 ° C. in a nitrogen atmosphere.
A nickel silicide film was formed by heat treatment by the id Thermal Anneal method. The state of the interface roughness was observed by TEM observation of the cross section of this film. Further, these films are heated by the RTA method in a nitrogen atmosphere to perform XR
NiS of nickel silicide (NiSi) by D diffraction method
The temperature of the crystal structure change to i 2 was investigated. The results are also shown in Table 1 above. As shown in Table 1, Comparative Examples 4-6
For all of the above, the interface roughness was poor.
【００３２】（実施例７）Ｎｂ３ａｔ％をＥＢ溶解時に
添加したことを除き、実施例１の材料及び製造条件で、
高純度ニッケル合金ターゲットを作製した。酸素、炭
素、水素及びガス成分と合金元素以外の不純物含有量
を、同様に表１に示す。表１に示すように、酸素含有量
１５ｗｔｐｐｍ、炭素含有量１２ｗｔｐｐｍ、水素含有
量８ｗｔｐｐｍ、ガス成分及び合金成分以外の不純物含
有量７ｗｔｐｐｍであった。(Example 7) With the material and manufacturing conditions of Example 1, except that Nb3at% was added during EB dissolution.
A high-purity nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, the oxygen content was 15 wtppm, the carbon content was 12 wtppm, the hydrogen content was 8 wtppm, and the impurity content other than the gas component and the alloy component was 7 wtppm.
【００３３】（実施例８）Ｎｂ３ａｔ％をＥＢ溶解時に
添加したことを除き、実施例２の材料及び製造条件で、
高純度ニッケル合金ターゲットを作製した。酸素、炭
素、水素及びガス成分と合金元素以外の不純物含有量
を、同様に表１に示す。表１に示すように、酸素含有量
７ｗｔｐｐｍ、炭素含有量６ｗｔｐｐｍ、水素含有量４
ｗｔｐｐｍ、ガス成分及び合金成分以外の不純物含有量
５ｗｔｐｐｍであった。(Example 8) With the materials and manufacturing conditions of Example 2, except that Nb3at% was added during EB dissolution.
A high-purity nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, oxygen content 7 wtppm, carbon content 6 wtppm, hydrogen content 4
The content of impurities other than wtppm and gas components and alloy components was 5 wtppm.
【００３４】（実施例９）Ｎｂ３ａｔ％をＥＢ溶解時に
添加したことを除き、実施例３の材料及び製造条件で、
高純度ニッケル合金ターゲットを作製した。酸素、炭
素、水素及びガス成分と合金元素以外の不純物含有量
を、同様に表１に示す。表１に示すように、酸素含有量
１ｗｔｐｐｍ、炭素含有量１ｗｔｐｐｍ、水素含有量１
ｗｔｐｐｍ、ガス成分及び合金成分以外の不純物含有量
１ｗｔｐｐｍ未満であった。(Example 9) With the materials and manufacturing conditions of Example 3, except that Nb3at% was added during EB dissolution.
A high-purity nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, oxygen content 1 wtppm, carbon content 1 wtppm, hydrogen content 1
The content of impurities other than wtppm, gas components and alloy components was less than 1 wtppm.
【００３５】上記実施例７〜９の高純度ニッケルターゲ
ットを用いて、シリコン膜上にニッケル膜をスパッタリ
ング成膜し、窒素雰囲気中５００°ＣでＲＴＡ（Ｒａｐ
ｉｄＴｈｅｒｍａｌ Ａｎｎｅａｌ）法にて熱処理し
て、ニッケルシリサイド膜を作製した。この膜の断面を
ＴＥＭ観察して界面ラフネスの様子を観察した。さらに
これらの膜を窒素雰囲気中ＲＴＡ法で加熱して、ＸＲＤ
回折法にてニッケルシリサイド（ＮｉＳｉ）のＮｉＳｉ
２への結晶構造変化の温度を調べた。この結果を、同様
に上記表１に示す。表１に示すように、実施例７〜９に
ついては、いずれも界面ラフネスは良好であった。ま
た、ニッケルシリサイド相変化温度は７４０°Ｃ以上と
なり、高温での熱処理でも相変化が抑制できるという効
果が得られた。この温度は、ニッケル合金としたことに
より、より高温側にシフトしたものであり、純ニッケル
に比べてさらに良好な特性を有する。Using the high-purity nickel targets of Examples 7 to 9 above, a nickel film was formed by sputtering on a silicon film, and RTA (Rap) was performed at 500 ° C. in a nitrogen atmosphere.
A nickel silicide film was formed by heat treatment by the id Thermal Anneal method. The state of the interface roughness was observed by TEM observation of the cross section of this film. Further, these films are heated by the RTA method in a nitrogen atmosphere to perform XRD.
NiSi of nickel silicide (NiSi) by diffraction method
The temperature at which the crystal structure changed to 2 was investigated. The results are also shown in Table 1 above. As shown in Table 1, in each of Examples 7 to 9, the interface roughness was good. Further, the nickel silicide phase change temperature was 740 ° C. or higher, and the effect that the phase change could be suppressed even by heat treatment at high temperature was obtained. This temperature is shifted to a higher temperature side by using the nickel alloy, and has better characteristics than pure nickel.
【００３６】（比較例７）Ｎｂ３ａｔ％をＥＢ溶解時に
添加したことを除き、比較例１の材料及び製造条件で、
ニッケル合金ターゲットを作製した。酸素、炭素、水素
及びガス成分と合金元素以外の不純物含有量を、同様に
表１に示す。表１に示すように、酸素含有量７５ｗｔｐ
ｐｍ、炭素含有量６２ｗｔｐｐｍ、水素含有量１２ｗｔ
ｐｐｍ、ガス成分及び合金成分以外の不純物含有量３８
ｗｔｐｐｍであった。(Comparative Example 7) With the material and manufacturing conditions of Comparative Example 1 except that Nb3at% was added during EB dissolution.
A nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, the oxygen content is 75 wtp
pm, carbon content 62wtppm, hydrogen content 12wt
Impurity content other than ppm, gas components and alloy components 38
It was wtppm.
【００３７】（比較例８）Ｎｂ３ａｔ％をＥＢ溶解時に
添加したことを除き、比較例２の材料及び製造条件で、
ニッケル合金ターゲットを作製した。酸素、炭素、水素
及びガス成分と合金元素以外の不純物含有量を、同様に
表１に示す。表１に示すように、酸素含有量４５ｗｔｐ
ｐｍ、炭素含有量３６ｗｔｐｐｍ、水素含有量２１ｗｔ
ｐｐｍ、ガス成分及び合金成分以外の不純物含有量３１
ｗｔｐｐｍであった。(Comparative Example 8) With the material and manufacturing conditions of Comparative Example 2 except that 3 at% of Nb was added during EB dissolution.
A nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, the oxygen content is 45 wtp
pm, carbon content 36wtppm, hydrogen content 21wt
Impurity content other than ppm, gas components and alloy components 31
It was wtppm.
【００３８】（比較例９）Ｎｂ３ａｔ％をＥＢ溶解時に
添加したことを除き、比較例３の材料及び製造条件で、
ニッケル合金ターゲットを作製した。酸素、炭素、水素
及びガス成分と合金元素以外の不純物含有量を、同様に
表１に示す。表１に示すように、酸素含有量３３ｗｔｐ
ｐｍ、炭素含有量２６ｗｔｐｐｍ、水素含有量１８ｗｔ
ｐｐｍ、ガス成分及び合金成分以外の不純物含有量１０
ｗｔｐｐｍ未満であった。(Comparative Example 9) With the material and manufacturing conditions of Comparative Example 3, except that Nb3at% was added during EB dissolution.
A nickel alloy target was produced. The contents of impurities other than oxygen, carbon, hydrogen and gas components and alloying elements are also shown in Table 1. As shown in Table 1, the oxygen content is 33 wtp
pm, carbon content 26wtppm, hydrogen content 18wt
Impurity content other than ppm, gas components and alloy components 10
It was less than wtppm.
【００３９】上記比較例７〜９の高純度ニッケルターゲ
ットを用いて、シリコン膜上にニッケル膜をスパッタリ
ング成膜し、窒素雰囲気中５００°ＣでＲＴＡ（Ｒａｐ
ｉｄＴｈｅｒｍａｌ Ａｎｎｅａｌ）法にて熱処理し
て、ニッケルシリサイド膜を作製した。この膜の断面を
ＴＥＭ観察して界面ラフネスの様子を観察した。さらに
これらの膜を窒素雰囲気中ＲＴＡ法で加熱して、ＸＲＤ
回折法にてニッケルシリサイド（ＮｉＳｉ）のＮｉＳｉ
２への結晶構造変化の温度を調べた。この結果を、同様
に上記表１に示す。表１に示すように、比較例７〜９に
ついては、いずれも界面ラフネスは不良であった。Using the high-purity nickel targets of Comparative Examples 7 to 9 above, a nickel film was formed by sputtering on a silicon film, and RTA (Rap) was performed at 500 ° C. in a nitrogen atmosphere.
A nickel silicide film was formed by heat treatment by the id Thermal Anneal method. The state of the interface roughness was observed by TEM observation of the cross section of this film. Further, these films are heated by the RTA method in a nitrogen atmosphere to perform XRD.
NiSi of nickel silicide (NiSi) by diffraction method
The temperature at which the crystal structure changed to 2 was investigated. The results are also shown in Table 1 above. As shown in Table 1, in Comparative Examples 7 to 9, the interface roughness was poor.
【００４０】[0040]
【発明の効果】高純度ニッケル又はニッケル合金スパッ
タリングターゲット中の酸素、炭素等のガス成分及びそ
の他の不純物元素を極力低減させることにより、サリサ
イドプロセスによりニッケルシリサイドのゲート電極膜
の形成に際して、ニッケルが酸素と反応して酸化膜を形
成すること、この酸化膜がシリサイド反応を阻害するこ
と、シリサイド膜とシリコン基板との界面領域に凹凸の
ある絶縁膜を形成すること、さらにはこの酸化物がシリ
サイド膜の凝集の原因となること等、界面のラフネスに
よって、Ｎ＋／Ｐの接合特性が劣化し抵抗が増加すると
いうニッケルシリサイド固有の問題点を解決することが
できる著しい効果を有する。また、高純度ニッケルに合
金元素を添加することにより、準安定相であるＮｉＳｉ
から、抵抗率が高くシリサイド化反応におけるＳｉの消
費量も増大させる原因となっていた安定相であるＮｉＳ
ｉ２相への転移を遅らせかつ抑制することができるとい
う優れた効果を有する。EFFECTS OF THE INVENTION By reducing the gas components such as oxygen and carbon and other impurity elements in the high-purity nickel or nickel alloy sputtering target as much as possible, nickel is not oxygen when forming the gate electrode film of nickel silicide by the salicide process. To form an oxide film, to inhibit the silicide reaction, to form an uneven insulating film in the interface region between the silicide film and the silicon substrate, and further, this oxide forms a silicide film. It has a remarkable effect of solving the problem peculiar to nickel silicide that the N + / P junction characteristic is deteriorated and the resistance is increased due to the roughness of the interface, such as the cause of the agglomeration of nickel. In addition, by adding an alloying element to high-purity nickel, the metastable phase NiSi
Therefore, NiS, which is a stable phase, has a high resistivity and causes an increase in Si consumption in the silicidation reaction.
It has an excellent effect that the transition to the i 2 phase can be delayed and suppressed.
【図１】水素及び真空処理温度と脱酸素、炭素、水素と
の関係を示すグラフ（図）である。FIG. 1 is a graph (diagram) showing the relationship between hydrogen and vacuum processing temperatures and deoxidization, carbon, and hydrogen.
フロントページの続き (72)発明者 宮下 博仁 茨城県北茨城市華川町臼場187番地４ 株 式会社日鉱マテリアルズ磯原工場内 Ｆターム(参考） 4K029 BA52 BD02 DC03 DC04 DC07 DC08 4M104 AA01 BB05 BB21 BB38 BB39 CC05 DD40 DD84 Continued front page (72) Inventor Hirohito Miyashita 4 shares, 187 Usba, Hwagawa-cho, Kitaibaraki, Ibaraki Ceremony Company Nikko Materials Isohara Factory F-term (reference) 4K029 BA52 BD02 DC03 DC04 DC07 DC08 4M104 AA01 BB05 BB21 BB38 BB39 CC05 DD40 DD84
Claims (17)
ｐｐｍ以下であることを特徴とする高純度ニッケル又は
ニッケル合金スパッタリングターゲット。1. The contents of oxygen and carbon are each 20 wt.
A high-purity nickel or nickel alloy sputtering target characterized by having a content of ppm or less.
ｐｐｍ以下であることを特徴とする高純度ニッケル又は
ニッケル合金スパッタリングターゲット。2. The contents of oxygen and carbon are each 10 wt.
A high-purity nickel or nickel alloy sputtering target characterized by having a content of ppm or less.
ｐｍ以下であることを特徴とする高純度ニッケル又はニ
ッケル合金スパッタリングターゲット。3. The oxygen and carbon contents are 1 wtp each.
A high-purity nickel or nickel alloy sputtering target having a pm or less.
ることを特徴とする請求項１〜３のそれぞれに記載の高
純度ニッケル又はニッケル合金スパッタリングターゲッ
ト。4. The high-purity nickel or nickel alloy sputtering target according to each of claims 1 to 3, wherein the hydrogen content is 10 wtppm or less.
とを特徴とする請求項１〜３のそれぞれに記載の高純度
ニッケル又はニッケル合金スパッタリングターゲット。5. The high-purity nickel or nickel alloy sputtering target according to each of claims 1 to 3, wherein the hydrogen content is 1 wtppm or less.
のガス成分を除く不純物元素の含有量が１０ｗｔｐｐｍ
未満であることを特徴とする請求項１〜５のそれぞれに
記載の高純度ニッケル又はニッケル合金スパッタリング
ターゲット。6. The content of alloy elements and impurity elements excluding gas components such as oxygen, hydrogen, nitrogen and carbon is 10 wtppm.
The high-purity nickel or nickel alloy sputtering target according to each of claims 1 to 5, wherein
それぞれ５ｐｐｍ以下であることを特徴とする請求項６
に記載の高純度ニッケル又はニッケル合金スパッタリン
グターゲット。7. The content of each of iron and cobalt as impurities is 5 ppm or less.
The high-purity nickel or nickel alloy sputtering target according to 1.
れぞれ２ｐｐｍ以下であることを特徴とする請求項６に
記載の高純度ニッケル又はニッケル合金スパッタリング
ターゲット。8. The high-purity nickel or nickel alloy sputtering target according to claim 6, wherein the contents of impurities iron and cobalt are each 2 ppm or less.
ム、ハフニウム、バナジウム、ニオブ、タンタル、クロ
ム、マンガン、ルテニウム、パラジウム、白金、モリブ
デン、レニウム、タングステンから選択した少なくとも
１種類以上の元素を含有することを特徴とする請求項１
〜８のそれぞれに記載の高純度ニッケル合金スパッタリ
ングターゲット。9. An alloying element containing at least one element selected from titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, manganese, ruthenium, palladium, platinum, molybdenum, rhenium, and tungsten. Claim 1 characterized by
~ The high-purity nickel alloy sputtering target according to each of 8).
選択した少なくとも１種類以上の元素を含有することを
特徴とする請求項１〜６及び９のそれぞれに記載の高純
度ニッケル合金スパッタリングターゲット。10. The high-purity nickel alloy sputtering target according to each of claims 1 to 6 and 9, wherein the alloy element contains at least one element selected from iron and cobalt.
％であることを特徴とする請求項１〜１０のそれぞれに
記載の高純度ニッケル合金スパッタリングターゲット。11. The alloying element content is from 0.5 to 10 at.
%, The high-purity nickel alloy sputtering target according to each of claims 1 to 10, wherein
ることを特徴とする請求項１〜１０のそれぞれに記載の
高純度ニッケル合金スパッタリングターゲット。12. The high-purity nickel alloy sputtering target according to each of claims 1 to 10, wherein the content of the alloy element is 1 to 5 at%.
ｐｍ含有することを特徴とする請求項１〜１２のそれぞ
れに記載の高純度ニッケル又は高純度ニッケル合金スパ
ッタリングターゲット。13. A lanthanoid element is used in an amount of 0.2 to 40 p.
The high-purity nickel or high-purity nickel alloy sputtering target according to each of claims 1 to 12, characterized by containing pm.
形成させるサリサイド工程で使用することを特徴とする
請求項１〜１３のそれぞれに記載の高純度ニッケル又は
ニッケル合金スパッタリングターゲット。14. The high-purity nickel or nickel alloy sputtering target according to each of claims 1 to 13, which is used in a salicide process of reacting with silicon to form a silicide film.
純物を除去した後、電子ビーム溶解等の方法で溶解して
高純度ニッケルインゴットを作製し、これを鍛造、圧延
等の塑性加工により厚さを７〜１０ｍｍとした後水素雰
囲気中で加熱して脱酸素、脱炭素を行い、さらにこれを
真空雰囲気中で加熱して脱水素処理を行うことを特徴と
する請求項１〜８、１３、１４のそれぞれに記載の高純
度ニッケルスパッタリングターゲットの製造方法。15. After removing metallic impurities from the crude nickel by electrolytic refining, the crude nickel is melted by a method such as electron beam melting to prepare a high-purity nickel ingot, which is subjected to plastic working such as forging and rolling to reduce its thickness. The dehydrogenating treatment is performed by heating in a hydrogen atmosphere after the thickness is adjusted to 7 to 10 mm, and the dehydrogenation treatment is performed by further heating this in a vacuum atmosphere. 1. A method for producing a high-purity nickel sputtering target according to each of 1.
純物を除去した後、高純度合金元素と共に電子ビーム溶
解等の方法で溶解して高純度ニッケル合金インゴットを
作製し、これを鍛造、圧延等の塑性加工により厚さを７
〜１０ｍｍとした後、水素雰囲気中で加熱して脱酸素、
脱炭素を行い、さらにこれを真空雰囲気中で加熱して脱
水素処理を行うことを特徴とする請求項１〜１２に記載
の高純度ニッケル合金スパッタリングターゲットの製造
方法。16. A method for producing a high-purity nickel alloy ingot by removing metal impurities from crude nickel by an electrolytic refining method and then melting the nickel with a high-purity alloy element by a method such as electron beam melting, which is subjected to forging, rolling, etc. Thickness is increased to 7 by plastic working
After setting to 10 mm, deoxidize by heating in a hydrogen atmosphere,
The method for producing a high-purity nickel alloy sputtering target according to any one of claims 1 to 12, wherein decarbonization is performed, and the dehydrogenation treatment is performed by heating the carbon in a vacuum atmosphere.
純度ニッケル合金インゴットを作製する際に、脱酸効果
を高めるために合金元素としてランタノイド系元素を
０．２ｐｐｍ〜４０ｐｐｍ添加することを特徴とする請
求項１３、１６に記載の高純度ニッケル合金スパッタリ
ングターゲットの製造方法。17. When producing a high-purity nickel alloy ingot by melting by a method such as electron beam melting, 0.2 ppm to 40 ppm of a lanthanoid element is added as an alloying element to enhance the deoxidizing effect. The method for producing a high-purity nickel alloy sputtering target according to claim 13 or 16.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002015347A JP2003213407A (en) | 2002-01-24 | 2002-01-24 | High purity nickel or nickel alloy sputtering target and production method therefor |
| PCT/JP2002/012698 WO2003062488A1 (en) | 2002-01-24 | 2002-12-04 | High-purity nickel or nickel alloy sputtering target, and its manufacturing method |
| TW91135521A TW200302288A (en) | 2002-01-24 | 2002-12-09 | High-purity nickel or nickel alloy sputtering target, and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002015347A JP2003213407A (en) | 2002-01-24 | 2002-01-24 | High purity nickel or nickel alloy sputtering target and production method therefor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2003213407A true JP2003213407A (en) | 2003-07-30 |
Family
ID=27606109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2002015347A Withdrawn JP2003213407A (en) | 2002-01-24 | 2002-01-24 | High purity nickel or nickel alloy sputtering target and production method therefor |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP2003213407A (en) |
| TW (1) | TW200302288A (en) |
| WO (1) | WO2003062488A1 (en) |
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| JP2005057233A (en) * | 2003-08-02 | 2005-03-03 | Samsung Electronics Co Ltd | Method of manufacturing semiconductor device and semiconductor device manufactured using same |
| WO2005083138A1 (en) * | 2004-03-01 | 2005-09-09 | Nippon Mining & Metals Co., Ltd. | Ni-Pt ALLOY AND TARGET COMPRISING THE ALLOY |
| WO2005086567A2 (en) * | 2004-03-15 | 2005-09-22 | Agency For Science, Technology And Research | Silicide formed from ternary metal alloy films |
| JP2010132974A (en) * | 2008-12-04 | 2010-06-17 | Nippon Steel Materials Co Ltd | Ni-Mo BASED ALLOY SPUTTERING TARGET PLATE |
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| JP3455721B2 (en) * | 1993-07-27 | 2003-10-14 | 株式会社半導体エネルギー研究所 | Method for manufacturing semiconductor device |
| JP3532063B2 (en) * | 1997-03-17 | 2004-05-31 | 株式会社日鉱マテリアルズ | Sputtering target and film forming method |
| JPH11152592A (en) * | 1997-11-18 | 1999-06-08 | Japan Energy Corp | Production of high purity nickel and high purity nickel material for forming thin film |
-
2002
- 2002-01-24 JP JP2002015347A patent/JP2003213407A/en not_active Withdrawn
- 2002-12-04 WO PCT/JP2002/012698 patent/WO2003062488A1/en active Application Filing
- 2002-12-09 TW TW91135521A patent/TW200302288A/en unknown
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Also Published As
| Publication number | Publication date |
|---|---|
| TW200302288A (en) | 2003-08-01 |
| WO2003062488A1 (en) | 2003-07-31 |
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