JPH0754138A - Sputtering rolling target material having high strength - Google Patents
Sputtering rolling target material having high strengthInfo
- Publication number
- JPH0754138A JPH0754138A JP22286193A JP22286193A JPH0754138A JP H0754138 A JPH0754138 A JP H0754138A JP 22286193 A JP22286193 A JP 22286193A JP 22286193 A JP22286193 A JP 22286193A JP H0754138 A JPH0754138 A JP H0754138A
- Authority
- JP
- Japan
- Prior art keywords
- sputtering
- target material
- rolling
- high strength
- rolling target
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、圧延加工が可能で、
したがって圧延加工後の熱処理で微細な再結晶組織とす
ることができ、これによって高強度を具備せしめたスパ
ッタリングターゲット材に関するものである。This invention is capable of rolling,
Therefore, the present invention relates to a sputtering target material having a high strength, which can be made into a fine recrystallized structure by heat treatment after rolling.
【０００２】[0002]
【従来の技術】従来、例えば半導体装置の集積回路の電
極や配線などを構成する薄膜が、例えば特開平４−３２
３８７１号公報に記載されるように、原子％で（以下、
％は原子％を示す）、Ｔａ：０．１〜５％、を含有し、
残りがＡｌと不可避不純物からなる組成を有するＡｌ合
金で構成された鋳造ターゲット材を用い、スパッタリン
グにて形成されることは良く知られている。2. Description of the Related Art Conventionally, for example, a thin film forming an electrode or wiring of an integrated circuit of a semiconductor device has been disclosed in, for example, Japanese Patent Laid-Open No. 4-32
As described in Japanese Patent No. 3871, in atomic% (hereinafter,
% Represents atomic%), Ta: 0.1 to 5%,
It is well known that the rest is formed by sputtering using a cast target material composed of an Al alloy having a composition of Al and unavoidable impurities.
【０００３】[0003]
【発明が解決しようとする課題】一方、近年のスパッタ
リング装置の大型化および高性能化はめざましく、これ
に伴ない、省力化とも相まってターゲット材は大型化の
傾向にあるが、上記従来鋳造ターゲット材においては、
鋳物であるために、相対的に結晶粒が平均粒径で５００
μｍ以上と大きく、かつ第２相であるＡｌ−Ｔａ金属間
化合物の大きさも平均粒径で１００μｍ以上となってお
り、十分な強度を具備するものでないことから、これを
大型化すると、取扱上および操業上割れや欠けが発生し
易く、実用に供することができないのが現状である。ま
た、上記従来鋳造ターゲット材は圧延加工がきわめて困
難であるという事情もある。On the other hand, in recent years, the size and performance of the sputtering apparatus have been remarkably increased, and along with this, the target material tends to increase in size due to the labor saving. In
Since it is a casting, the average crystal grain size is 500
The size of the Al-Ta intermetallic compound, which is the second phase, is as large as 100 μm or more in terms of average particle size, and it does not have sufficient strength. In addition, cracks and chips are liable to occur during operation, and it cannot be put to practical use at present. There is also a circumstance that the conventional casting target material is extremely difficult to roll.
【０００４】[0004]
【課題を解決するための手段】そこで、本発明者等は、
上述のような観点から、上記の従来鋳造ターゲット材に
着目し、これの強度向上をはかるべく研究を行なった結
果、上記従来鋳造ターゲット材を構成するＡｌ合金に、
合金成分としてＢ，Ｓｉ，Ｃａ、およびＭｇのうちの１
種または２種以上を５〜１００ppm の割合で含有させる
と、これへの圧延が可能となり、したがって圧延加工後
に再結晶化熱処理を施すことにより、組織が微細化し、
結晶粒およびＡｌ−Ｔａ金属間化合物の粒径が、いずれ
も平均粒径で３０μｍ以下になり、さらに酸素含有量も
相対的に低減して、上記従来鋳造ターゲット材では、通
常４０〜１００ppm であった酸素含有量が３５ppm 以下
になり、この結果高強度を具備するようになるという研
究結果を得たのである。Therefore, the present inventors have
From the above viewpoints, focusing on the above conventional casting target material, as a result of research to improve the strength of the conventional casting target material, the Al alloy constituting the above conventional casting target material,
One of B, Si, Ca, and Mg as an alloy component
If one or two or more kinds are contained in a proportion of 5 to 100 ppm, rolling to this is possible, and therefore, by performing recrystallization heat treatment after rolling, the structure becomes finer,
The average grain size of the crystal grains and the grain size of the Al-Ta intermetallic compound are both 30 μm or less, and the oxygen content is also relatively reduced. In the conventional casting target material, it is usually 40 to 100 ppm. Moreover, the research results that the oxygen content becomes 35 ppm or less, and as a result, high strength is obtained, were obtained.
【０００５】この発明は、上記の研究結果にもとづいて
なされたものであって、Ｔａ：０．１〜５％、Ｂ，Ｓ
ｉ，Ｃａ、およびＭｇのうちの１種または２種以上：５
〜１００ppm 、を含有し、残りがＡｌと不可避不純物か
らなる組成、並びに再結晶組織を有するＡｌ合金で構成
してなる高強度を有するスパッタリング圧延ターゲット
材に特徴を有するものである。The present invention was made based on the above research results, Ta: 0.1 to 5%, B, S
One or more of i, Ca, and Mg: 5
It is characterized by a high-strength sputtering rolled target material composed of an Al alloy having a recrystallization structure and a composition containing Al and unavoidable impurities, the remaining content being ˜100 ppm.
【０００６】つぎに、この発明の圧延ターゲット材を構
成するＡｌ合金の成分組成を上記の通りに限定した理由
を説明する。 （ａ） Ｔａ Ｔａ成分には、スパッタで形成される薄膜の耐ストレス
マイグレーション性（耐熱性）および耐食性を向上させ
る作用があるが、その含有量が０．１％未満では前記作
用に所望の向上効果が得られず、一方その含有量が５％
を越えると、薄膜の電気抵抗が急激に増大するようにな
ることから、その含有量を０．１〜５％と定めた。Next, the reason why the component composition of the Al alloy constituting the rolling target material of the present invention is limited as described above will be explained. (A) The Ta-Ta component has an effect of improving the stress migration resistance (heat resistance) and the corrosion resistance of a thin film formed by sputtering, but if the content thereof is less than 0.1%, the above-mentioned effect is improved as desired. No effect, while its content is 5%
If it exceeds, the electric resistance of the thin film will rapidly increase, so the content was set to 0.1 to 5%.
【０００７】（ｂ） Ｂ，Ｓｉ，Ｃａ、およびＭｇ これらの成分は、強力な脱酸作用を発揮し、酸素含有量
を３５ppm 以下に低減すると共に、割れの発生のない圧
延を可能ならしめ、もって圧延後の熱処理で微細な再結
晶組織を形成して、結晶粒およびＡｌ−Ｔａ金属間化合
物の粒径をいずれも平均粒径で３０μｍ以下にし、強度
を著しく向上させる作用があるが、その含有量が５ppm
未満では前記作用に所望の効果が得られず、一方その含
有量がｌ００ppm を越えると薄膜の電気的特性が低下す
るようになることから、その含有量を５〜１００ppm と
定めた。(B) B, Si, Ca, and Mg These components exert a strong deoxidizing action, reduce the oxygen content to 35 ppm or less, and enable rolling without cracking, Therefore, a fine recrystallized structure is formed by the heat treatment after rolling, and the grain size of the crystal grains and the Al-Ta intermetallic compound are both 30 μm or less in average grain size, which has the effect of significantly improving the strength. Content is 5ppm
If it is less than the above range, the desired effect cannot be obtained, while if the content exceeds 100 ppm, the electrical characteristics of the thin film will be deteriorated. Therefore, the content is defined as 5 to 100 ppm.
【０００８】[0008]
【実施例】つぎに、この発明の圧延ターゲット材を実施
例により具体的に説明する。真空度を１×１０-4torr以
下とした真空溶解炉で表１，２に示される組成のＡｌ合
金溶湯を溶製し、鉄製鋳型に鋳造して平面寸法：２００
mm×２００mm、厚さ：４０mmのインゴットとし、このイ
ンゴットに、大気中、６００℃に加熱後、５パスの圧延
を１サイクルとし、これを３回繰り返す熱間圧延を施し
て、厚さ：８mmの熱延板とし、引続いてこの熱延板に、
大気中、温度：６００℃に１時間保持の再結晶熱処理を
施すことにより、いずれも割れの発生の全くない本発明
圧延ターゲット材１〜１５をそれぞれ製造した。EXAMPLES Next, the rolling target material of the present invention will be specifically described by way of examples. In a vacuum melting furnace with a vacuum degree of 1 × 10 −4 torr or less, molten Al alloys having the compositions shown in Tables 1 and 2 were melted and cast into an iron mold to obtain a plane dimension: 200.
mm × 200 mm, thickness: 40 mm, and the ingot was heated to 600 ° C. in the atmosphere and then subjected to 5 passes of rolling for 1 cycle, and hot rolling was repeated 3 times to obtain a thickness of 8 mm. As a hot rolled sheet of
By subjecting to recrystallization heat treatment in the air at a temperature of 600 ° C. for 1 hour, rolling target materials 1 to 15 of the present invention were produced, each of which was free from cracks.
【０００９】また、比較の目的で、同じく真空度を１×
１０-4torr以下とした真空溶解炉にて表２に示される組
成のＡｌ合金溶湯を溶製し、鉄製鋳型に鋳造して幅：３
１５mm×厚さ：８mm×長さ：６２０mmの寸法をもったイ
ンゴットとすることにより従来鋳造ターゲット材１〜３
をそれぞれ製造した。For comparison purposes, the degree of vacuum is also set to 1 ×.
A molten Al alloy having the composition shown in Table 2 was melted in a vacuum melting furnace with a pressure of 10 -4 torr or less, cast into an iron mold, and width: 3
By using an ingot having the dimensions of 15 mm × thickness: 8 mm × length: 620 mm, the conventional casting target materials 1 to 3
Were manufactured respectively.
【００１０】ついで、この結果得られた本発明圧延ター
ゲット材１〜１５および従来鋳造ターゲット材１〜３に
ついて、酸素含有量を測定すると共に、その組織を観察
して平均結晶粒径およびＡｌ−Ｔａ金属間化合物の平均
粒径を測定し、さらに強度を評価する目的で、上記の各
種のターゲット材を、幅：３００mm×厚さ：５mm×長
さ：６００mmの大型寸法に切削加工した状態で、純Ｉｎ
はんだを用い、大気中、温度：１８０℃、保持時間：２
０分の条件で無酸素銅製バッキングプレートにはんだ付
けし、直流マグネトロンスパッタリング装置にて、真空
度：２×１０-4torrを保持しながら、５ml／min のＡｒ
気流中、１０ｋｗの出力でガラス基板上に薄膜を形成す
るスパッタリングを３００時間行ない、ターゲット材に
割れが発生するまでのスパッタ時間を測定した。これら
の測定時間を表１，２にそれぞれ示した。Then, the oxygen content of each of the rolling target materials 1 to 15 of the present invention and the conventional casting target materials 1 to 3 obtained as a result was measured, and the microstructure was observed to observe the average crystal grain size and Al-Ta. For the purpose of measuring the average particle size of the intermetallic compound and further evaluating the strength, the above various target materials were cut into a large size of width: 300 mm × thickness: 5 mm × length: 600 mm, Pure In
Using solder, in air, temperature: 180 ° C, holding time: 2
Soldered to an oxygen-free copper backing plate under the condition of 0 minutes and kept a vacuum degree of 2 × 10 −4 torr with a DC magnetron sputtering device while maintaining 5 ml / min of Ar.
Sputtering for forming a thin film on a glass substrate was performed for 300 hours in an air stream at an output of 10 kw, and the sputtering time until cracks were generated in the target material was measured. These measurement times are shown in Tables 1 and 2, respectively.
【００１１】[0011]
【表１】 [Table 1]
【００１２】[0012]
【表２】 [Table 2]
【００１３】[0013]
【発明の効果】表１，２に示される結果から、本発明圧
延ターゲット材１〜１５は、従来鋳造ターゲット材１〜
３に比して、酸素含有量が相対的に低く、かつ結晶粒径
およびＡｌ−Ｔａ金属間化合物の粒径も小さく、組成が
相対的に微細であり、この結果高強度をもつようになる
ことから、実用に際してもスパッタ中に割れが発生する
ことがなく、使用寿命に至るまですぐれた性能を発揮す
ることが明らかである。上述のように、この発明の圧延
ターゲット材は、圧延加工後の熱処理による微細組織で
高強度をもつようになり、この結果大型の実用化が可能
となり、スパッタリング装置の大型化、高性能化、およ
び省力化などに大いに寄与するものである。From the results shown in Tables 1 and 2, the rolled target materials 1 to 15 of the present invention are the conventional cast target materials 1 to 1.
3, the oxygen content is relatively low, the crystal grain size and the Al-Ta intermetallic compound grain size are also small, and the composition is relatively fine, resulting in high strength. Therefore, it is clear that even in practical use, cracking does not occur during sputtering, and excellent performance is exhibited up to the service life. As described above, the rolling target material of the present invention has a high microstructure due to the heat treatment after the rolling process, and as a result, it is possible to put the large-sized practical application into the sputtering apparatus. It also greatly contributes to labor saving.
Claims (1)
上：５〜１００ppm 、 を含有し、残りがＡｌと不可避不純物からなる組成、並
びに再結晶組織を有するＡｌ合金で構成したことを特徴
とする高強度を有するスパッタリング圧延ターゲット
材。1. A composition containing Ta: 0.1 to 5 atomic%, one or more of B, Si, Ca, and Mg: 5 to 100 ppm, and the balance Al and unavoidable impurities. And a sputtering-rolled target material having high strength, which is composed of an Al alloy having a recrystallized structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22286193A JP3416999B2 (en) | 1993-08-16 | 1993-08-16 | Sputtering roll target material with high strength |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22286193A JP3416999B2 (en) | 1993-08-16 | 1993-08-16 | Sputtering roll target material with high strength |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0754138A true JPH0754138A (en) | 1995-02-28 |
| JP3416999B2 JP3416999B2 (en) | 2003-06-16 |
Family
ID=16789047
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22286193A Expired - Fee Related JP3416999B2 (en) | 1993-08-16 | 1993-08-16 | Sputtering roll target material with high strength |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3416999B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010280992A (en) * | 2010-09-29 | 2010-12-16 | Toshiba Corp | Method for producing sputtering target |
| US20130092534A1 (en) * | 2010-08-09 | 2013-04-18 | Jx Nippon Mining & Metals Corporation | Tantalum Sputtering Target |
-
1993
- 1993-08-16 JP JP22286193A patent/JP3416999B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130092534A1 (en) * | 2010-08-09 | 2013-04-18 | Jx Nippon Mining & Metals Corporation | Tantalum Sputtering Target |
| US9085819B2 (en) * | 2010-08-09 | 2015-07-21 | Jx Nippon Mining & Metals Corporation | Tantalum sputtering target |
| JP2010280992A (en) * | 2010-09-29 | 2010-12-16 | Toshiba Corp | Method for producing sputtering target |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3416999B2 (en) | 2003-06-16 |
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