JPH10195609A - Fcc metal in which crystal orientation is regulated and its production - Google Patents
Fcc metal in which crystal orientation is regulated and its productionInfo
- Publication number
- JPH10195609A JPH10195609A JP35817396A JP35817396A JPH10195609A JP H10195609 A JPH10195609 A JP H10195609A JP 35817396 A JP35817396 A JP 35817396A JP 35817396 A JP35817396 A JP 35817396A JP H10195609 A JPH10195609 A JP H10195609A
- Authority
- JP
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- Prior art keywords
- fcc
- fcc metal
- rolling
- metal
- ratio
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Physical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、各種ターゲット用
材料等として好適な結晶方位の制御されたＦＣＣ金属及
びその製造法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an FCC metal having a controlled crystal orientation suitable as a material for various targets and a method for producing the same.
【０００２】[0002]
【従来の技術】近時、エレクトロニクス産業の発達に伴
ない、各種スパッタリングターゲット材料用についても
その使用量が増大するとともに、特性面でもより高特性
が望まれている。例えば、基板ウエハー上でのスパッタ
配線用材料として使用されるＦＣＣ金属においても以下
のような特性が要求されている。 （１） 結晶方位において（１００）優先方位を有して
いること：スパッタリングを施されるＦＣＣ金属におい
てはスパッタレートを確保するために、（１００）優先
方位を有していることが望まれる場合がある。 （２） エレクトロマイグレーションに優れること：ス
パッタにより形成された基板ウエハー上での配線におい
ては配線幅の微細化により短絡現象の一種であるエレク
トロマイグレーションが問題となっている。ここでこの
現象は、膜の組成に大きく影響されることが確認されて
いるので膜の組成をほぼ一義的に決定するスパッタリン
グターゲット用材料についてもエレクトロマイグレーシ
ョン性に優れていることが望まれる。 （３） 不純物が少ないこと：スパッタリング膜の配線
信頼性は膜の微細構造の影響を強く受けるが、この膜の
微細構造はガス成分を含めた不純物の影響が大きいこと
がわかっている。そこで、スパッタリングターゲット用
材料としても所定の成分以外の不純物が少ないことが望
まれる。 （４） 平均結晶粒径が細かいこと：スパッタリング膜
の均一性を高めるため、さらにスパッタリングレートの
向上のため、スパッタリングターゲット用材料は平均結
晶粒径が微細であることが望まれている。スパッタリン
グターゲット用材料としては以上のような諸特性が要求
されている。2. Description of the Related Art In recent years, with the development of the electronics industry, the amount of various sputtering target materials used has increased, and higher characteristics have been desired in terms of characteristics. For example, the following characteristics are required for FCC metal used as a material for sputter wiring on a substrate wafer. (1) Having a (100) preferred orientation in the crystal orientation: When it is desired that the FCC metal to be sputtered has a (100) preferred orientation in order to secure a sputter rate. There is. (2) Excellent electromigration: In wiring on a substrate wafer formed by sputtering, electromigration, which is a kind of short-circuit phenomenon, has become a problem due to miniaturization of wiring width. Since this phenomenon has been confirmed to be greatly affected by the composition of the film, it is desired that the material for the sputtering target, which determines the composition of the film almost uniquely, also has excellent electromigration properties. (3) Fewer impurities: Although the wiring reliability of the sputtering film is strongly affected by the fine structure of the film, it is known that the fine structure of this film is greatly affected by impurities including gas components. Therefore, it is desired that the sputtering target material has a small amount of impurities other than the predetermined components. (4) Fine average crystal grain size: In order to increase the uniformity of the sputtering film and further improve the sputtering rate, it is desired that the sputtering target material has a fine average crystal grain size. Various properties as described above are required for a material for a sputtering target.
【０００３】[0003]
【発明が解決しようとする課題】基板ウエハー上のスパ
ッタ配線用材料としては従来、Ａｌ等が用いられてきた
が、要求される諸特性を十分に満たしているものではな
かった。したがって本発明の目的は、結晶方位が制御さ
れているほか、スパッタリングターゲット用材料に要求
される諸特性を兼備したＦＣＣ金属およびその製造方法
を提供することにある。Conventionally, Al or the like has been used as a material for sputter wiring on a substrate wafer, but does not sufficiently satisfy the required characteristics. Therefore, an object of the present invention is to provide an FCC metal having a crystal orientation controlled and having various characteristics required for a material for a sputtering target, and a method for producing the same.
【０００４】[0004]
【課題を解決するための手段】本発明は、スパッタリン
グターゲット用材料等に要求される上記のような諸特性
を兼備したＦＣＣＦ金属、特に各種スパッタリング特性
を向上させるためにその結晶方位の制御されたＦＣＣ金
属を開発すべく、鋭意研究の結果開発されたものであっ
て、下記のＦＣＣ金属及びその製造法を提供するもので
ある。すなわち、本発明は：第１にＸ線回折における
（１１１）面の積分強度Ｉ(111) にたいする（２００）
面の積分強度Ｉ(200) の比が、式： Ｉ(200) ／Ｉ(111) ≧４．６ の関係を満たす比の値を有していることを特徴とする
（１００）優先方位を持つＦＣＣ金属：第２に上記ＦＣ
Ｃ金属がＣｕマトリックスを有することを特徴とする前
記第１に記載のＦＣＣ金属：第３に上記Ｃｕの純度が６
Ｎ以上であることを特徴とする前記第２に記載のＦＣＣ
金属：第４に平均結晶粒径が２００μｍ以下であること
を特徴とする前記第２に記載のＦＣＣ金属：第５に純度
６Ｎ以上のＣｕマトリックスを有し、その平均結晶粒径
が２００μｍ以下であり、かつＸ線回折における（１１
１）面の積分強度Ｉ(111) に対する（２２０）面の積分
強度Ｉ(220) の比が、式： Ｉ(200) ／Ｉ(111) ≧４．６ の関係を満たす比の値を有していることを特徴とする
（１００）優先方位を持つＦＣＣ金属：第６に（１０
０）優先方位を持つＦＣＣ金属の製造方法であって、全
パスの圧延軸のずれを±１５°未満に制御しながら１方
向あるいは往復圧延を合計圧下率で２０％以上施した後
再結晶を伴なう、完全焼鈍を施すことによりＸ線回折で
測定される結晶の（１１１）面の積分強度Ｉ(111) に対
する（２００）面の積分強度Ｉ(200) の比が、式： Ｉ(200) ／Ｉ(111) ≧４．６ の関係を満たす比の値を有していることを特徴とする
（１００）優先方位を持つＦＣＣ金属の製造方法：第７
にＣｕマトリックスを有する（１００）優先方位を持つ
ＦＣＣ金属の製造方法であって、全パスの圧延軸のずれ
を±１５°未満に制御しながら１方向あるいは往復圧延
を合計圧下率で２０％以上施した後４９８〜８２３Ｋで
６０〜７２００ｓｅｃの熱処理を行うことを特徴とした
前記第６に記載のＦＣＣ金属の製造方法：第８にＣｕの
純度が６Ｎ以上ある（１００）優先方位を持つことを特
徴とする前記第７に記載のＦＣＣ金属の製造方法：第９
に平均結晶粒径が２００μｍ以下の（１００）優先方位
を持つＦＣＣ金属の製造方法であって、６２３〜８７３
Ｋで加工率２０％以上の熱間加工を施し、さらに加工率
１０％以上の冷間加工と４９３〜８２３Ｋで６０〜７２
００ｓｅｃの熱処理を少なくとも２回以上繰り返し行
い、かつ、全パスの圧延軸のずれを±１５°未満に制御
しながら１方向あるいは往復圧延を合計圧下率で２０％
以上施した後４９８〜８２３Ｋで６０〜７２００ｓｅｃ
の熱処理を行うことを特徴とした前記第６に記載のＦＣ
Ｃ金属の製造方法：第１０に前記第１〜５のいずれかに
記載の（１００）優先方位を持つＦＣＣ金属からなるタ
ーゲット用素材：第１１に前記第６〜第９のいずれかの
方法で製造された（１００）優先方位を持つＦＣＣ金属
からなるターゲット用素材を提供することである。SUMMARY OF THE INVENTION The present invention relates to an FCCF metal having the above-mentioned various characteristics required for a material for a sputtering target and the like, and in particular, to control the crystal orientation of the FCCF metal in order to improve various sputtering characteristics. It has been developed as a result of intensive research to develop an FCC metal, and provides the following FCC metal and a method for producing the same. That is, the present invention firstly relates to (200) the integrated intensity I (111) of the (111) plane in X-ray diffraction.
The (100) preferred orientation is characterized in that the ratio of the integrated intensity I (200) of the surface has a value satisfying the relationship of the following formula: I (200) / I (111) ≧ 4.6. FCC metal with: 2nd FC
The FCC metal according to the first aspect, wherein the C metal has a Cu matrix: Third, the purity of the Cu is 6
N. The FCC according to item 2, wherein
Metal: Fourth, the average grain size is 200 μm or less. FCC metal according to the second aspect: Fifth, having a Cu matrix having a purity of 6N or more, and having an average grain size of 200 μm or less. And (11) in X-ray diffraction.
1) The ratio of the integrated intensity I (220) of the (220 ) plane to the integrated intensity I (111) of the plane has a value satisfying the relationship of I: (200) / I (111) ≧ 4.6. FCC metal having a (100) preferred orientation characterized by:
0) A method for producing an FCC metal having a preferred orientation, in which a unidirectional or reciprocal rolling is performed at a total draft of 20% or more while controlling a rolling axis deviation of all passes to less than ± 15 °, and then recrystallization is performed. accompanied, the ratio of the fully annealed measured by X-ray diffraction by the applying is of the crystal with respect to (111) integrated intensity I (111) of the plane (200) plane of the integrated intensity I (200) has the formula: I ( 200) / I (111) ≧ 4.6. A method for producing an FCC metal having a (100) preferred orientation, characterized in that the ratio has a value satisfying the relationship: 4.6.
A method for producing an FCC metal having a (100) preferred orientation having a Cu matrix, wherein the total rolling reduction in one direction or reciprocating rolling is 20% or more while controlling the deviation of the rolling axis in all passes to less than ± 15 °. The method for producing an FCC metal according to the sixth aspect, wherein the heat treatment is performed at 498 to 823 K for 60 to 7200 seconds after the application. Eighthly, the method has a (100) preferred orientation in which the purity of Cu is 6N or more. The method for producing an FCC metal according to the item 7, wherein the method is ninth.
A method for producing an FCC metal having a (100) preferred orientation with an average crystal grain size of 200 μm or less, comprising 623 to 873
Hot working at a working ratio of 20% or more at K, and cold working at a working ratio of 10% or more and 60-72 at 493-823K.
The heat treatment of 00sec is repeated at least twice or more, and one-way or reciprocating rolling is performed at a total draft of 20% while controlling the deviation of the rolling axis in all passes to less than ± 15 °.
After applying the above, 60 ~ 7200sec at 498 ~ 823K
7. The FC according to the item 6, wherein the heat treatment is performed.
C metal production method: Tenth, a target material made of the FCC metal having the (100) preferred orientation according to any one of the first to fifth aspects: Eleventh, according to any one of the sixth to ninth methods. An object of the present invention is to provide a target material made of a manufactured FCC metal having a (100) preferred orientation.
【０００５】[0005]
【発明の実施の形態】本発明は、ＦＣＣ金属において適
切な加工熱処理を施し、その結晶方位を制御することに
よりスパッタリングターゲット用材料等として好適なＦ
ＣＣ金属を提供し得たことに基本的な特徴がある。次
に、本発明に係るＦＣＣ金属及びその製造方法を上記の
通りに限定した理由について説明する。BEST MODE FOR CARRYING OUT THE INVENTION The present invention provides an FCC metal which is suitable as a material for a sputtering target or the like by controlling the crystal orientation by performing an appropriate working heat treatment.
A fundamental feature is that CC metal can be provided. Next, the reason why the FCC metal and the method for producing the FCC metal according to the present invention are limited as described above will be described.
【０００６】結晶方位：結晶方位についてはスパッタリ
ングレートおよび膜の均一性を確保するために、スパッ
タリングターゲット用ＦＣＣ金属において（１００）優
先方位を有することが望まれる場合がある、その評価と
してはＸ線回折における（１１１）面と（２００）面の
積分強度の比が用いられる。すなわち（１１１）面の積
分強度Ｉ(111) に対する（２２０）面の積分強度Ｉ
(220) の比：Ｉ(220) ／Ｉ(111) の比の値が、４．６よ
り小さいと（１００）優先方位とは言い難く、スパッタ
リングレートも劣化する。そこで、Ｘ線回折における
（１１１）面と（２００）面の積分強度の比はＩ(200)
／Ｉ(111) ≧４．６となるようにすることを判定基準と
して熱処理の方法を工夫したところ、この基準を満たす
ものは良好な（１００）優先方位を有するＦＣＣ金属で
あることが認められた。これは、Ｘ線回折法で結晶面の
積分強度を測定するとき、（１１１）面、（２００）
面、（２２０）面の積分強度が最も強く現れるが、方位
制御しない場合、各方位の積分強度Ｉ(111) ：
Ｉ(200) ：Ｉ(220) の比は通常１００：４６：２０とな
ることに基づいている。すなわち、Ｉ(200) ／Ｉ(111)
の比が通常の場合の比の値０．４６の１０倍以上となる
ように方位制御するための熱処理時要件について研究し
たのである。Crystal Orientation: Regarding the crystal orientation, in order to ensure the sputtering rate and the uniformity of the film, it is sometimes desired that the FCC metal for the sputtering target has a (100) preferred orientation. The ratio of the integrated intensity of the (111) plane and the (200) plane in diffraction is used. That is, the integrated intensity I of the (220) plane with respect to the integrated intensity I (111) of the ( 111 ) plane
If the value of the ratio of (220) : I (220) / I (111) is smaller than 4.6, the (100) preferred orientation is hard to say, and the sputtering rate is also deteriorated. Therefore, the ratio of the integrated intensity of the (111) plane and the (200) plane in X-ray diffraction is I (200)
/ I (111) ≧ 4.6 When the heat treatment method was devised on the basis of a criterion, it was confirmed that the FCC metal having a good (100) preferred orientation was found to satisfy this criterion. Was. This is because the (111) plane and (200)
Plane, the integrated intensity of the (220) plane appears most strongly, but when azimuth control is not performed, the integrated intensity I (111) of each azimuth:
The ratio of I (200) : I (220) is usually based on 100: 46: 20. That is, I (200) / I (111)
The purpose of this study was to study the requirements at the time of heat treatment for controlling the orientation so that the ratio of the ratio becomes 10 times or more of the ratio value of 0.46 in a normal case.
【０００７】マトリックス：上記ＦＣＣの中では、特に
Ｃｕマトリックスを有するものがエレクトロマイグレー
ションに優れている。従って、上記ＦＣＣ金属はＣｕマ
トリックスを有するものであることが好ましい。Matrix: Among the above FCCs, those having a Cu matrix are particularly excellent in electromigration. Therefore, the FCC metal preferably has a Cu matrix.
【０００８】純度：上記Ｃｕの純度は膜の微細構造に大
きく影響を与えるが、その純度が６Ｎより劣化するとス
パッタリング膜の結晶性が劣化しエレクトロマイグレー
ション特性等にも悪影響を及ぼす。従って、上記Ｃｕマ
トリックス純度は６Ｎ以上であることが望ましい。Purity: The purity of the Cu greatly affects the fine structure of the film. However, if the purity is lower than 6N, the crystallinity of the sputtered film is deteriorated, and the electromigration characteristics and the like are adversely affected. Therefore, the Cu matrix purity is desirably 6N or more.
【０００９】平均結晶粒径：平均結晶粒径が粗大になる
と、スパッタリングレート、膜の均一性が劣化してく
る。この現象は特に平均結晶粒径が２００μｍより大き
くなると顕著である。従って、平均結晶粒径は２００μ
ｍ以下であることが好ましい。Average crystal grain size: When the average crystal grain size becomes coarse, the sputtering rate and the uniformity of the film deteriorate. This phenomenon is particularly remarkable when the average crystal grain size is larger than 200 μm. Therefore, the average crystal grain size is 200 μ
m or less.
【００１０】最終熱処理： （１００）優先方位を有するＦＣＣ金属を製造するため
には、再結晶を伴なういわゆる完全焼鈍を施す必要があ
る。特にマトリックスがＣｕからなる場合には熱処理温
度が４９３Ｋ未満あるいは熱処理時間が６０ｓｅｃ未満
では再結晶が十分進行せず、熱処理温度が８２３Ｋより
高くあるいは熱処理時間が７２００ｓｅｃを越えると経
済的に不利になるばかりでなく結晶粒の粗大化も生じて
しまう。従って、熱処理条件は４９３〜８２３Ｋで６０
〜７２００ｓｅｃとした。Final heat treatment: To produce an FCC metal having the (100) preferred orientation, it is necessary to perform a so-called complete annealing accompanied by recrystallization. In particular, when the matrix is made of Cu, recrystallization does not sufficiently proceed if the heat treatment temperature is less than 493 K or the heat treatment time is less than 60 sec. Instead, the crystal grains become coarse. Therefore, the heat treatment conditions are 493 to 823K and 60.
と し た 7200 sec.
【００１１】最終加工： （１００）優先方位を有するＦＣＣ金属を製造するため
には、１方向圧延を施す必要がある。ここで圧延軸のず
れを合計で１５°以上あるいは合計圧下率を２０％未満
とすると、（１００）面の集積度が弱くなる。従って最
終加工は、全パスの圧延軸のずれを±１５°未満に制御
しながら１方向あるいは往復圧延を合計圧下率で２０％
以上施すこととした。Final processing: In order to produce FCC metal having the (100) preferred orientation, it is necessary to perform unidirectional rolling. Here, if the total deviation of the rolling axis is 15 ° or more or the total draft is less than 20%, the degree of integration of the (100) plane is reduced. Therefore, in the final processing, one-way or reciprocating rolling is performed with a total rolling reduction of 20% while controlling the deviation of the rolling axis of all passes to less than ± 15 °.
It was decided to apply above.
【００１２】最終前加工熱処理：最終前加工熱処理とし
ては６２３〜８７３Ｋで加工率２０％以上の熱間加工を
施し、さらに加工率１０％以上の冷間加工と４９３〜８
２３Ｋで６０〜７２００ｓｅｃの熱処理を少なくとも２
回以上繰り返し行う必要がある。これらの条件を外れる
といずれも最終組織は混粒となり、かつ平均結晶粒径を
２００μｍ以下に制御することは、最終加工熱処理をい
かに行うとも困難である。以上のように結晶方位の制御
されたＦＣＣ金属は各種電気電子部品用材料として使用
されるのはもちろんのこと、各種スパッタリングターゲ
ット用素材として好適な材料である。次に本発明を実施
例により詳細に説明する以下に示す製造方法によりスパ
ッタリングターゲット用材料を製造し、特性調査を行っ
た。Final pre-processing heat treatment: The final pre-processing heat treatment includes hot working at a work rate of 20% or more at 623 to 873K, and cold working at a work rate of 10% or more and 493 to 8
Heat treatment at 23K for 60-7200 sec for at least 2
It needs to be repeated more than once. If these conditions are not satisfied, the final structure becomes mixed grains in any case, and it is difficult to control the average crystal grain size to 200 μm or less, no matter how the final working heat treatment is performed. As described above, the FCC metal whose crystal orientation is controlled is not only used as a material for various electric and electronic parts, but also a material suitable as a material for various sputtering targets. Next, a sputtering target material was manufactured by the following manufacturing method for describing the present invention in more detail with reference to examples, and the characteristics were investigated.
【００１３】[0013]
【実施例１】２６５×２６５×６０t ｍｍの７Ｎ高純度
銅を用い７２３Ｋ熱間クロス圧延にて３２０×３２０×
４２t ｍｍに加工した。この時の合計圧下率は約３０％
である。得られた熱延板の上下面を１ｍｍずつ切削加工
を施し、３２０×３２０×４０t ｍｍに加工した。得ら
れた切削板を用い冷間一方向圧延にて３８０×３２０×
３４t ｍｍに加工した。この時の合計圧下率は約１５％
である。得られた冷延板を用い６７３Ｋで３６００ｓｅ
ｃの熱処理を行った。得られた熱処理板を用い、一工程
前の冷間圧延と圧延軸を同じにして冷間一方向圧延を行
い４５０×３２０×２９t ｍｍに加工した。この時の合
計圧下率は約１５％である。得られた冷延板を用い６７
３Ｋで３６００ｓｅｃの熱処理を行った。得られた熱処
理板を用い、一工程前の冷間圧延とは圧延軸を９０°ず
らせて冷間一方向圧延を行い４５０×４５０×２０t ｍ
ｍに加工した。このとき合計圧下率は約３０％である。
得られた冷延板を用い６２３Ｋで１２００ｓｅｃの熱処
理を行った。得られた熱処理板より切削加工により、直
径４００φｍｍ×１５t ｍｍのスパッタリングターゲッ
ト用材料を得た。Embodiment 1 320 × 320 × by 723K hot cross rolling using 7N high-purity copper of 265 × 265 × 60 t mm.
It processed to 42 tmm . The total draft at this time is about 30%
It is. The upper and lower surfaces of the obtained hot rolled sheet were cut by 1 mm each, and processed into 320 × 320 × 40 tmm . 380 × 320 × by cold unidirectional rolling using the obtained cutting plate
It processed to 34 tmm . The total draft at this time is about 15%
It is. 3600 sec at 673K using the obtained cold rolled sheet
The heat treatment of c was performed. Using the obtained heat-treated plate, cold unidirectional rolling was performed by using the same rolling axis as that of the cold rolling one step before, and processed to 450 × 320 × 29 tmm . The total draft at this time is about 15%. Using the obtained cold rolled sheet, 67
Heat treatment was performed at 3K for 3600 seconds. Using the obtained heat-treated plate, cold rolling in one direction was performed by performing cold unidirectional rolling by shifting the rolling axis by 90 ° with 450 × 450 × 20 tm.
m. At this time, the total draft is about 30%.
The obtained cold-rolled sheet was subjected to a heat treatment at 623K for 1200 seconds. By cutting from the obtained heat-treated plate, to obtain a sputtering target material having a diameter of 400φmm × 15 t mm.
【００１４】[0014]
【実施例２】２６５×２６５×６０t ｍｍの６Ｎ高純度
銅を用い７２３Ｋ熱間クロス圧延にて３２０×３２０×
４２t ｍｍに加工した。この時の合計圧下率は約３０％
である。得られた熱延板の上下面を１ｍｍずつ切削加工
を施し、３２０×３２０×４０t ｍｍに加工した。得ら
れた切削板を用い冷間一方向圧延にて３８０×３２０×
３４t ｍｍに加工した。この時の合計圧下率は約１５％
である。得られた冷延板を用い６７３Ｋで３６００ｓｅ
ｃの熱処理を行った。得られた熱処理板を用い、一工程
前の冷間圧延とは圧延軸を同じにして冷間一方向圧延を
行い４５０×３２０×２９t ｍｍに加工した。この時の
合計圧下率は約１５％である。得られた冷延板を用い６
７３Ｋで３６００ｓｅｃの熱処理を行った。得られた熱
処理板を用い、一工程前の冷間圧延とは圧延軸を９０°
ずらせて冷間一方向圧延を行い、４５０×４５０×２０
t ｍｍに加工した。この時合計圧下率は約３０％であ
る。得られた冷延板を用い６２３Ｋで１２００ｓｅｃの
熱処理を行った。得られた熱処理板より切削加工によ
り、直径４００φｍｍ×１５t ｍｍのスパッタリングタ
ーゲット用材料を得た。Example 2 320 × 320 × by 723K hot cross rolling using 6N high-purity copper of 265 × 265 × 60 t mm.
It processed to 42 tmm . The total draft at this time is about 30%
It is. The upper and lower surfaces of the obtained hot rolled sheet were cut by 1 mm each, and processed into 320 × 320 × 40 tmm . 380 × 320 × by cold unidirectional rolling using the obtained cutting plate
It processed to 34 tmm . The total draft at this time is about 15%
It is. 3600 sec at 673K using the obtained cold rolled sheet
The heat treatment of c was performed. Using the obtained heat-treated plate, cold unidirectional rolling was performed by using the same rolling axis as that of the cold rolling one step before, and processed to 450 × 320 × 29 t mm. The total draft at this time is about 15%. 6 using the obtained cold rolled sheet
Heat treatment was performed at 73K for 3600 seconds. Using the obtained heat-treated plate, the rolling axis is 90 ° with the cold rolling one step before.
Perform cold unidirectional rolling with a shift of 450 × 450 × 20
It was processed to t mm. At this time, the total draft is about 30%. The obtained cold-rolled sheet was subjected to a heat treatment at 623K for 1200 seconds. By cutting from the obtained heat-treated plate, to obtain a sputtering target material having a diameter of 400φmm × 15 t mm.
【００１５】[0015]
【比較例１】２６５×２６５×６０t ｍｍの７Ｎ高純度
銅を用い冷間クロス圧延にて３２０×３２０×４２t ｍ
ｍに加工した。この時の合計圧下率は約３０％である。
得られた冷延板の上下面を１ｍｍずつ切削加工を施し、
３２０×３２０×４０t ｍｍに加工した。得られた切削
板を用い冷間一方向圧延にて３８０×３２０×３４t ｍ
ｍに加工した。この時の合計圧下率は約１５％である。
得られた冷延板を用い６７３Ｋで３６００ｓｅｃの熱処
理を行った。得られた熱処理板を用い、一工程前の冷間
圧延と圧延軸を同じにして冷間一方向圧延を行い４５０
×３２０×２９t ｍｍに加工した。この時の合計圧下率
は約１５％である。得られた冷延板を用い６７３Ｋで３
６００ｓｅｃの熱処理を行った。得られた熱処理板を用
い、一工程前の冷間圧延とは圧延軸を９０°ずらせて冷
間一方向圧延を行い４５０×４５０×２０t ｍｍに加工
した。この時の合計圧下率は約３０％である。得られた
冷延板を用い６２３Ｋで１２００ｓｅｃの熱処理を行っ
た。得られた熱処理板より切削加工により、直径４００
φｍｍ×１５t ｍｍのスパッタリングターゲット用材料
を得た。[Comparative Example 1] 265 × 265 × 60 t mm of 7N high purity copper 320 × 320 × at cold cross rolling with 42 t m
m. The total draft at this time is about 30%.
The upper and lower surfaces of the obtained cold rolled sheet are cut by 1 mm,
It processed to 320x320x40 tmm. 380 × 320 × 34 t m by cold unidirectional rolling using the obtained cutting plate
m. The total draft at this time is about 15%.
Using the obtained cold-rolled sheet, heat treatment was performed at 673K for 3600 seconds. Using the obtained heat-treated sheet, cold unidirectional rolling was performed by using the same rolling axis as that of the cold rolling one step before, and 450 ° C.
It processed to × 320 × 29 t mm. The total draft at this time is about 15%. 3 at 673K using the obtained cold rolled sheet
Heat treatment was performed for 600 seconds. Using the obtained heat-treated sheet, cold rolling in one direction was performed by performing cold unidirectional rolling with the rolling axis shifted by 90 ° from that of the cold rolling before one step, and processed to 450 × 450 × 20 tmm . The total draft at this time is about 30%. The obtained cold-rolled sheet was subjected to a heat treatment at 623K for 1200 seconds. 400 mm in diameter by cutting from the heat-treated plate obtained
It was obtained φmm × 15 t mm sputtering target material for.
【００１６】[0016]
【比較例２】２６５×２６５×６０t ｍｍの７Ｎ高純度
銅を用い７２３Ｋ熱間クロス圧延にて３２０×３２０×
４２t ｍｍに加工した。この時の合計圧下率は約３０％
である。得られた熱延板の上下面を１ｍｍずつ切削加工
を施し、３２０×３２０×４０t ｍｍに加工した。得ら
れた切削板を用い冷間一方向圧延にて３８０×３２０×
３４t ｍｍに加工した。この時の合計圧下率は約１５％
である。得られた冷延板を用い６７３Ｋで３６００ｓｅ
ｃの熱処理を行った。得られた熱処理板を用い、一工程
前の冷間圧延とは圧延軸を９０°ずらせて冷間一方向圧
延を行い３８０×３８０×２９t ｍｍに加工した。この
時の合計圧下率は約１５％である。得られた冷延板を用
い６７３Ｋで３６００ｓｅｃの熱処理を行った。得られ
た熱処理板を用い、冷間一方向圧延にて４５０×３８０
×２４t ｍｍに加工した。この時合計圧下率は約１７％
である。得られた冷延板を用い６２３Ｋで１２００ｓｅ
ｃの熱処理を行った。得られた熱処理板を用い、一工程
前の冷間圧延とは圧延軸を９０°ずらせて冷間一方向圧
延を行い４５０×４５０×２０t ｍｍに加工した。この
時の合計圧下率は約１５％である。得られた冷延板を用
い６２３Ｋで１２００ｓｅｃの熱処理を行った。得られ
た熱処理板より切削加工により、直径４００φｍｍ×１
５t ｍｍのスパッタリングターゲット用材料を得た。得
られたスパッタリングターゲット用材料について、純
度、結晶粒径、結晶方位について測定を行った。その結
果を表１に示す。COMPARATIVE EXAMPLE 2 320 × 320 × by 723K hot cross rolling using 7N high purity copper of 265 × 265 × 60 t mm.
It processed to 42 tmm . The total draft at this time is about 30%
It is. The upper and lower surfaces of the obtained hot rolled sheet were cut by 1 mm each, and processed into 320 × 320 × 40 tmm . 380 × 320 × by cold unidirectional rolling using the obtained cutting plate
It processed to 34 tmm . The total draft at this time is about 15%
It is. 3600 sec at 673K using the obtained cold rolled sheet
The heat treatment of c was performed. Using the obtained heat-treated plate, cold rolling in one direction was shifted by 90 ° from the cold rolling before one step, and cold rolling was performed in one direction to be processed to 380 × 380 × 29 tmm . The total draft at this time is about 15%. Using the obtained cold-rolled sheet, heat treatment was performed at 673K for 3600 seconds. Using the obtained heat-treated plate, 450 × 380 by cold unidirectional rolling
It processed to × 24 tmm . At this time, the total draft is about 17%
It is. 1200 sec at 623K using the obtained cold rolled sheet
The heat treatment of c was performed. Using the obtained heat-treated sheet, cold rolling in one direction was performed by performing cold unidirectional rolling with the rolling axis shifted by 90 ° from that of the cold rolling before one step, and processed to 450 × 450 × 20 tmm . The total draft at this time is about 15%. The obtained cold-rolled sheet was subjected to a heat treatment at 623K for 1200 seconds. 400mm in diameter x 1 by cutting from the obtained heat treated plate
A 5 tmm material for a sputtering target was obtained. The purity, crystal grain size, and crystal orientation of the obtained sputtering target material were measured. Table 1 shows the results.
【００１７】[0017]
【表１】 [Table 1]
【００１８】また実施例１にて製造したスパッタリング
ターゲット用高純度銅と現在基板ウエハー上のスパッタ
配線材料として使用されているＡｌターゲットにて製造
した膜についてＢＥＭ（breakdown energy of metals）
法によりエレクロトマイグレーション評価の平均故障エ
ネルギー（ＭＥＦ＝mdeian energy to fail ）を求めた
その結果を表２に示す。The BEM (breakdown energy of metals) of the film manufactured using the high-purity copper for the sputtering target manufactured in Example 1 and the Al target currently used as a sputter wiring material on the substrate wafer.
The average failure energy (MEF = mdeian energy to fail) of the electromigration evaluation obtained by the method is shown in Table 2.
【００１９】[0019]
【表２】 [Table 2]
【００２０】表２に示す結果より、本発明にて製造した
スパッタリングターゲット用高純度銅は現在基板ウエハ
ー上のスパッタ配線材料として使用されているＡｌター
ゲットに比べてエレクトロマイグレーション特性に優れ
ており、また、純度、結晶方位、結晶粒度も最適であ
り、スパッタリングターゲット用材料として極めて優れ
ていることは明らかである。From the results shown in Table 2, the high-purity copper for a sputtering target manufactured by the present invention is superior in electromigration characteristics as compared with an Al target currently used as a sputter wiring material on a substrate wafer. The purity, crystal orientation, and crystal grain size are also optimal, and it is clear that they are extremely excellent as a material for a sputtering target.
【００２１】[0021]
【発明の効果】以上の実施例から明らかなように、本発
明に係るＦＣＣ金属は適切な純度、結晶方位、結晶粒度
を有しており、各種用途に使用できることはもちろんで
あるが、特にスパッタリングターゲット用材料として使
用する時には、スパッタリングレート、膜の均一性に優
れ、製造した膜のエレクトロマイグレーション性にも優
れているものである。さらに、本発明では、その適切な
製造法も示したものである。As is clear from the above examples, the FCC metal according to the present invention has an appropriate purity, crystal orientation and crystal grain size, and can be used for various purposes. When used as a target material, it is excellent in sputtering rate and film uniformity, and the manufactured film is also excellent in electromigration property. Furthermore, the present invention also shows an appropriate manufacturing method thereof.
フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｃ２２Ｆ 1/00 ６８５ Ｃ２２Ｆ 1/00 ６８５Ｚ ６８６ ６８６Ｂ ６９１ ６９１Ｂ ６９１Ｃ ６９４ ６９４Ａ Ｃ２３Ｃ 14/34 Ｃ２３Ｃ 14/34 Ａ Continued on the front page (51) Int.Cl. 6 Identification code FI C22F 1/00 685 C22F 1/00 685Z 686 686B 691 691B 691C 694 694A C23C 14/34 C23C 14/34 A
Claims (11)
１）面の積分強度Ｉ(111) に対する（２００）面の積分
強度Ｉ(200) の比が、式： Ｉ(200) ／Ｉ(111) ≧４．６ の関係を満たす比の値を有していることを特徴とする
（１００）優先方位を持つＦＣＣ金属。The present invention relates to a method for measuring (11)
1) The ratio of the integrated intensity I (200) of the (200 ) surface to the integrated intensity I (111) of the surface has a value satisfying the relationship of the following formula: I (200) / I (111) ≧ 4.6. An FCC metal having a (100) preferred orientation.
することを特徴とする請求項１に記載のＦＣＣ金属。2. The FCC metal of claim 1, wherein said FCC metal has a Cu matrix.
特徴とする請求項２に記載のＦＣＣ金属。3. The FCC metal according to claim 2, wherein the purity of the Cu is 6N or more.
とを特徴とする請求項２に記載のＦＣＣ金属。4. The FCC metal according to claim 2, wherein the average crystal grain size is 200 μm or less.
し、その平均結晶粒径が２００μｍ以下であり、かつＸ
線回折における（１１１）面の積分強度Ｉ(111) に対す
る（２００）面の積分強度Ｉ(200) の比が、式： Ｉ(200) ／Ｉ(111) ≧４．６ の関係を満たす比の値を有していることを特徴とする
（１００）優先方位を持つＦＣＣ金属。5. It has a Cu matrix having a purity of 6 N or more, an average crystal grain size of 200 μm or less, and X
The ratio of the integrated intensity of the (111) plane in the line diffraction I (111) for (200) plane of the integrated intensity I (200) is of the formula: ratio satisfying I (200) / I (111) ≧ 4.6 Relationship An FCC metal having a (100) preferred orientation, characterized in that
製造方法であって、全パスの圧延軸のずれを±１５°未
満に制御しながら１方向あるいは往復圧延を合計圧下率
で２０％以上施した後再結晶を伴なう、完全焼鈍を施す
ことによりＸ線回折で測定される結晶の（１１１）面の
積分強度Ｉ(111) に対する（２００）面の積分強度Ｉ
(200) の比が、式： Ｉ(200) ／Ｉ(111) ≧４．６ の関係を満たす比の値を有していることを特徴とする
（１００）優先方位を持つＦＣＣ金属の製造方法。6. A method for producing an FCC metal having a (100) preferred orientation, wherein one-way or reciprocal rolling is performed in a total rolling reduction of 20% or more while controlling a deviation of a rolling axis in all passes to less than ± 15 °. The integrated intensity I of the (200) plane relative to the integrated intensity I (111) of the (111) plane of the crystal measured by X-ray diffraction by performing complete annealing accompanied by recrystallization after the application
(200) the ratio of the formula: I (200) / I (111), characterized in that it has a value of the ratio that satisfies the relation of ≧ 4.6 (100) the production of FCC metals with preferred orientation Method.
先方位を持つＦＣＣ金属の製造方法であって、全パスの
圧延軸のずれを±１５°未満に制御しながら１方向ある
いは往復圧延を合計圧下率で２０％以上施した後４９８
〜８２３Ｋで６０〜７２００ｓｅｃの熱処理を行うこと
を特徴とした請求項６に記載のＦＣＣ金属の製造方法。7. A method for producing an FCC metal having a (100) preferred orientation having a Cu matrix, wherein a rolling reduction in one direction or reciprocal rolling is controlled while controlling a deviation of a rolling axis in all passes to less than ± 15 °. 498 after applying 20% or more with
The method for producing an FCC metal according to claim 6, wherein the heat treatment is performed at 60 to 7200 sec at -823K.
優先方位を持つことを特徴とする請求項７に記載のＦＣ
Ｃ金属の製造方法。8. The purity of Cu is 6N or more (100).
The FC according to claim 7, wherein the FC has a preferred direction.
Method for producing C metal.
０）優先方位を持つＦＣＣ金属の製造方法であって、６
２３〜８７３Ｋで加工率２０％以上の熱間加工を施し、
さらに加工率１０％以上の冷間加工と４９３〜８２３Ｋ
で６０〜７２００ｓｅｃの熱処理を少なくとも２回以上
繰り返し行い、かつ、全パスの圧延軸のずれを±１５°
未満に制御しながら１方向あるいは往復圧延を合計圧下
率で２０％以上施した後４９８〜８２３Ｋで６０〜７２
００ｓｅｃの熱処理を行うことを特徴とした請求項６に
記載のＦＣＣ金属の製造方法。9. The method according to claim 1, wherein the average crystal grain size is 200 μm or less.
0) A method for producing an FCC metal having a preferred orientation,
Perform hot working at a working rate of 20% or more at 23 to 873K,
Furthermore, cold working with a working ratio of 10% or more and 493 to 823K
The heat treatment for 60 to 7200 sec is repeated at least twice or more, and the deviation of the rolling axis in all passes is ± 15 °.
After performing one-way or reciprocating rolling at a total reduction ratio of 20% or more while controlling to less than 60 to 72 at 498 to 823K.
The method for producing an FCC metal according to claim 6, wherein the heat treatment is performed for 00 seconds.
００）優先方位を持つＦＣＣ金属からなるターゲット用
素材。10. The method according to claim 1, wherein (1)
00) Target material made of FCC metal with preferred orientation.
された（１００）優先方位を持つＦＣＣ金属からなるタ
ーゲット用素材。11. A target material made of an FCC metal having a (100) preferred orientation manufactured by the method according to claim 6. Description:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35817396A JPH10195609A (en) | 1996-12-27 | 1996-12-27 | Fcc metal in which crystal orientation is regulated and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35817396A JPH10195609A (en) | 1996-12-27 | 1996-12-27 | Fcc metal in which crystal orientation is regulated and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH10195609A true JPH10195609A (en) | 1998-07-28 |
Family
ID=18457924
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35817396A Pending JPH10195609A (en) | 1996-12-27 | 1996-12-27 | Fcc metal in which crystal orientation is regulated and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH10195609A (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008041535A1 (en) | 2006-10-03 | 2008-04-10 | Nippon Mining & Metals Co., Ltd. | Cu-Mn ALLOY SPUTTERING TARGET AND SEMICONDUCTOR WIRING |
| JP2009108376A (en) * | 2007-10-31 | 2009-05-21 | Nikko Kinzoku Kk | Copper foil and flexible printed circuit board using the same |
| WO2011018895A1 (en) * | 2009-08-12 | 2011-02-17 | 株式会社アルバック | Sputtering target and method for manufacturing a sputtering target |
| WO2011024909A1 (en) * | 2009-08-28 | 2011-03-03 | 古河電気工業株式会社 | Copper material for use in a sputtering target, and manufacturing method therefor |
| WO2011034127A1 (en) * | 2009-09-18 | 2011-03-24 | 古河電気工業株式会社 | Copper material for use as sputtering target and process for producing same |
| JP2012172265A (en) * | 2011-02-22 | 2012-09-10 | Heraeus Materials Technology Gmbh & Co Kg | Tubular sputter target |
| US20130008692A1 (en) * | 2010-03-17 | 2013-01-10 | Keiichi Kimura | Metal tape material and interconnector for solar module current collection |
| JP2013019010A (en) * | 2011-07-08 | 2013-01-31 | Furukawa Electric Co Ltd:The | Copper material for sputtering target and method for production thereof |
-
1996
- 1996-12-27 JP JP35817396A patent/JPH10195609A/en active Pending
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