JP3416999B2 - Sputtering roll target material with high strength - Google Patents

Sputtering roll target material with high strength

Info

Publication number
JP3416999B2
JP3416999B2 JP22286193A JP22286193A JP3416999B2 JP 3416999 B2 JP3416999 B2 JP 3416999B2 JP 22286193 A JP22286193 A JP 22286193A JP 22286193 A JP22286193 A JP 22286193A JP 3416999 B2 JP3416999 B2 JP 3416999B2
Authority
JP
Japan
Prior art keywords
target material
high strength
sputtering
rolling
ppm
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.)
Expired - Fee Related
Application number
JP22286193A
Other languages
Japanese (ja)
Other versions
JPH0754138A (en
Inventor
真 木下
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Materials Corp
Original Assignee
Mitsubishi Materials Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsubishi Materials Corp filed Critical Mitsubishi Materials Corp
Priority to JP22286193A priority Critical patent/JP3416999B2/en
Publication of JPH0754138A publication Critical patent/JPH0754138A/en
Application granted granted Critical
Publication of JP3416999B2 publication Critical patent/JP3416999B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Physical Vapour Deposition (AREA)

Description

【発明の詳細な説明】 【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。 【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。 【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。 【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Caおよび/またはMgを5〜100pp
m 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。 【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%、 Caおよび/またはMg:5〜100ppm 、 を含有し、残りがAlと不可避不純物からなる組成、並
びに圧延加工後の熱処理で形成された再結晶組織を有す
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。 【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。 【0007】(b) 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。 【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:200mm×
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1〜3をそれぞれ製造した。 【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同じく表1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:315mm×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。 【0010】ついで、この結果得られた本発明圧延ター
ゲット材1〜3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:20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/m in のA
r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にそれぞれ示した。 【0011】 【表1】【0012】 【発明の効果】表1に示される結果から、本発明圧延タ
ーゲット材1〜3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。
Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention
Therefore, the present invention relates to a sputtering target material having a high strength because a fine recrystallized structure can be obtained by heat treatment after rolling. 2. Description of the Related Art Conventionally, for example, a thin film constituting an electrode or a wiring of an integrated circuit of a semiconductor device has been disclosed in, for example, JP-A-4-32.
No. 3871, the atomic% (hereinafter, referred to as
% Represents atomic%), Ta: 0.1 to 5%,
It is well known that the remainder is formed by sputtering using a casting target material composed of an Al alloy having a composition of Al and inevitable impurities. [0003] On the other hand, in recent years, the size and performance of the sputtering apparatus have been remarkably increased, and accompanying this, the target material has tended to be larger due to labor savings. For casting target materials,
Since it is a casting, the average crystal grain size is relatively 500
μm or more, and the size of the Al-Ta intermetallic compound, which is the second phase, is also 100 μm or more in average particle diameter, and does not have sufficient strength. In addition, cracking and chipping are likely to occur during operation, and it is currently impossible to use the material for practical use. In addition, there is a situation that the above-mentioned conventional cast target material is extremely difficult to be rolled. [0004] Therefore, the present inventors have proposed:
From the viewpoint as described above, focusing on the above-mentioned conventional casting target material, as a result of researching to improve the strength thereof, Al alloy constituting the above-mentioned conventional casting target material,
5-100 pp of Ca and / or Mg as alloy components
If it is contained in the proportion of m, rolling to this becomes possible,
Therefore, by performing a recrystallization heat treatment after the rolling process, the structure is refined, and the grain size of the crystal grains and the Al-Ta intermetallic compound are each reduced to an average grain size of 30 μm or less, and the oxygen content is relatively reduced. In the conventional casting target material, the oxygen content, which was usually 40 to 100 ppm, was reduced to 35 ppm or less, and as a result, a research result was obtained that high strength was obtained. The present invention has been made on the basis of the above research results, and contains 0.1 to 5% of Ta, 5 to 100 ppm of Ca and / or Mg, and the balance of Al and inevitable impurities. And a high-strength sputtering roll target material composed of an Al alloy having a recrystallized structure formed by heat treatment after rolling. 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 described. (A) Ta The Ta component has an effect of improving the stress migration resistance (heat resistance) and corrosion resistance of a thin film formed by sputtering, but if the content is less than 0.1%, the effect is desired to be improved. No effect is obtained, while its content is 5%
, The electric resistance of the thin film suddenly increases, so the content was determined to be 0.1 to 5%. (B) Ca and Mg These components exert a strong deoxidizing effect, reduce the oxygen content to 35 ppm or less, and enable rolling free of cracks. A fine recrystallized structure is formed by heat treatment, and the grain size of the crystal grains and the Al-Ta intermetallic compound are both reduced to an average grain size of 30 μm or less, and the strength is significantly improved.
If the content is less than 100 ppm, the desired effect cannot be obtained. On the other hand, if the content exceeds 100 ppm, the electrical characteristics of the thin film deteriorates. Therefore, the content is set to 5 to 100 ppm. [0008] Next, the rolling target material of the present invention will be specifically described with reference to examples. In a vacuum melting furnace having a degree of vacuum of 1 × 10 −4 torr or less, an aluminum alloy melt having the composition shown in Table 1 was melted and cast into an iron mold, and the plane size was 200 mm ×
The ingot is 200 mm in thickness and 40 mm in thickness.
Hot rolling, which is repeated three times,
A hot-rolled sheet having a thickness of 8 mm and subsequently subjected to a recrystallization heat treatment at 600 ° C. for 1 hour in the atmosphere to thereby obtain a hot-rolled sheet without any cracks. Target materials 1 to 3 were manufactured respectively. Also, for the purpose of comparison, the degree of vacuum was similarly set to 1 ×
In a vacuum melting furnace of 10 −4 torr or less, an Al alloy melt having the composition shown in Table 1 is also melted and cast into an iron mold, and the dimensions of width: 315 mm × thickness: 8 mm × length: 620 mm Conventional casting target materials 1 to 3 were manufactured by using the ingots. Next, the oxygen content of each of the rolled target materials 1 to 3 of the present invention and the conventional cast target materials 1 to 3 obtained as a result is measured, and their structures are observed to determine the average crystal grain size and Al-Ta. For the purpose of measuring the average particle diameter of the intermetallic compound and further evaluating the strength, the above-mentioned various target materials were subjected to width: 300 mm × thickness: 5 mm × length:
After cutting to a large size of 600 mm, using pure In solder, it was soldered to an oxygen-free copper backing plate in the atmosphere at a temperature of 180 ° C. and a holding time of 20 minutes. Vacuum degree: 5 ml / min A while maintaining 2 × 10 -4 torr
Sputtering for forming a thin film on a glass substrate was performed for 300 hours in an r stream at an output of 10 kW, and the sputtering time until cracks occurred in the target material was measured. Table 1 shows the measurement times. [Table 1] From the results shown in Table 1, the rolled target materials 1 to 3 of the present invention have a relatively lower oxygen content and a smaller crystal grain than the conventionally cast target materials 1 to 3. The diameter and the particle size of the Al-Ta intermetallic compound are small, and the composition is relatively fine. As a result, the composition has a high strength. It is clear that it performs well over its lifetime. As described above, the rolling target material of the present invention has high strength in a microstructure by heat treatment after rolling, and as a result, large-scale practical use becomes possible. It greatly contributes to labor saving.

Claims (1)

(57)【特許請求の範囲】 【請求項1】 Ta:0.1〜5原子%、 Caおよび/またはMg:5〜100ppm 、を含有し、
残りがAlと不可避不純物からなる組成、並びに圧延加
工後の熱処理で形成された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。
(57) [Claim 1] Ta: 0.1 to 5 atomic%, Ca and / or Mg: 5 to 100 ppm,
Composition balance being Al and inevitable impurities, and the rolling pressure
A high-strength sputtering rolled target material comprising an Al alloy having a recrystallized structure formed by post-processing heat treatment .
JP22286193A 1993-08-16 1993-08-16 Sputtering roll target material with high strength Expired - Fee Related JP3416999B2 (en)

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 JPH0754138A (en) 1995-02-28
JP3416999B2 true 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)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103052733B (en) * 2010-08-09 2015-08-12 吉坤日矿日石金属株式会社 Tantalum sputtering target
JP5462120B2 (en) * 2010-09-29 2014-04-02 株式会社東芝 Manufacturing method of sputtering target

Also Published As

Publication number Publication date
JPH0754138A (en) 1995-02-28

Similar Documents

Publication Publication Date Title
KR100568392B1 (en) Silver alloy sputtering target and process for producing the same
JP2003073810A5 (en)
JP2002294437A (en) Copper alloy sputtering target
WO2021177461A1 (en) Pure copper plate, copper/ceramic joined body, and insulated circuit substrate
JP3634208B2 (en) Electrode / wiring material for liquid crystal display and sputtering target
JP2004027257A (en) Copper alloy with excellent bendability, and its manufacturing method
TWI740611B (en) Titanium-copper alloy plate for uniform temperature plate and uniform temperature plate
JP2002266041A (en) Rolled copper alloy foil and production method therefor
JP3416999B2 (en) Sputtering roll target material with high strength
JPH08100255A (en) Sputtering target material for forming thin film of thin film transistor
JP2002294438A (en) Copper alloy sputtering target
JPS5823452B2 (en) Softening resistant copper alloy
JPH0864554A (en) Sputtering target material for forming thin film of thin film transistor
JP2004084065A (en) Silver alloy sputtering target and its producing method
JP2001279351A (en) Rolled copper alloy foil and its production method
JP2000303131A (en) High strength aluminum alloy
JP3306585B2 (en) Cu alloy rolled sheet with fine crystals and precipitates and low distribution ratio
JP4405008B2 (en) Electrode / wiring material for liquid crystal display and manufacturing method thereof
TW202130827A (en) Copper alloy, copper alloy plastic working material, electronic/electrical device component, terminal, busbar, heat-dissipating board
JP4110563B2 (en) Copper alloy sputtering target
JPS6142772B2 (en)
JP3410278B2 (en) Al-based target material for liquid crystal display and method for producing the same
JPH0379734A (en) Copper alloy for backing plate
JP2552920B2 (en) Copper alloy for backing plate
JP3235149B2 (en) Rolled copper alloy foil for film carrier

Legal Events

Date Code Title Description
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20030311

LAPS Cancellation because of no payment of annual fees