JPH08269698A - Ti target for sputtering - Google Patents
Ti target for sputteringInfo
- Publication number
- JPH08269698A JPH08269698A JP9458295A JP9458295A JPH08269698A JP H08269698 A JPH08269698 A JP H08269698A JP 9458295 A JP9458295 A JP 9458295A JP 9458295 A JP9458295 A JP 9458295A JP H08269698 A JPH08269698 A JP H08269698A
- Authority
- JP
- Japan
- Prior art keywords
- target
- sputtering
- crystal grains
- particles
- purity
- 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.)
- Withdrawn
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、スパッタリングによ
りＴｉ金属膜を形成したり、反応性スパッタリングによ
り窒化Ｔｉ膜を形成するために使用するＴｉターゲット
に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a Ti target used for forming a Ti metal film by sputtering and for forming a Ti nitride film by reactive sputtering.
【０００２】[0002]
【従来の技術】一般に、スパッタリングによりＴｉ金属
膜または窒化Ｔｉ膜を形成する際に、Ｔｉターゲットを
使用することは知られており、スパッタリングにより形
成したＴｉ金属膜または窒化Ｔｉ膜にパーティクルが付
着し、このパーティクルが多量に付着したＴｉ金属膜ま
たは窒化Ｔｉ膜は不良品となることも知られている。2. Description of the Related Art Generally, it is known to use a Ti target when forming a Ti metal film or a Ti nitride film by sputtering, and particles adhere to the Ti metal film or Ti nitride film formed by sputtering. It is also known that a Ti metal film or a Ti nitride film having a large amount of these particles attached becomes a defective product.
【０００３】したがって、スパッタリングに際しパーテ
ィクル発生の少ないＴｉターゲットが求められており、
その１つとして結晶粒を微細化したＴｉターゲットが提
案されている。例えば、Ｓｉ，Ｇｅ，Ｂ等の結晶粒成長
抑制元素を微量（１００〜２０００ppm ）添加して結晶
粒を微細化したＴｉターゲット（特開平５−２５５８４
３号公報参照）または熱間鍛造後、４００℃以下で冷間
加工し、さらに５００〜６５０℃で熱処理することによ
り結晶粒を微細化（１０〜３５μｍ）したＴｉターゲッ
ト（特開平６−１０１０７号公報参照）などが提案され
ている。Therefore, there is a demand for a Ti target which produces few particles during sputtering.
As one of them, a Ti target in which crystal grains are made fine has been proposed. For example, a Ti target in which crystal grains are made fine by adding a trace amount (100 to 2000 ppm) of a crystal grain growth suppressing element such as Si, Ge, B (Japanese Patent Laid-Open No. 25584/1993).
3) or hot forging, followed by cold working at 400 ° C. or lower and further heat treatment at 500 to 650 ° C. to refine the crystal grains (10 to 35 μm) Ti target (JP-A-6-10107). For example, refer to the official gazette).
【０００４】[0004]
【発明が解決しようとする課題】しかし、上記Ｓｉ，Ｇ
ｅ，Ｂ等の結晶粒成長抑制元素を微量添加して得られた
微細結晶粒を有するＴｉターゲットは、スパッタして得
られたＴｉ金属膜中に添加元素が混入し、バリア性が劣
化するという問題があり、さらに冷間加工および熱処理
条件を制御して得られた微細結晶粒を有するＴｉターゲ
ットは、Ｔｉ金属膜中に添加元素が混入しバリア性が劣
化するという問題点は解決されたが、パーティクルの発
生を十分に抑制することができなかった。However, the above Si, G
A Ti target having fine crystal grains obtained by adding a small amount of crystal grain growth suppressing elements such as e and B is said to have a barrier property deteriorated because the additive element is mixed in the Ti metal film obtained by sputtering. The Ti target having fine crystal grains obtained by controlling the cold working and heat treatment conditions has a problem that the additive element is mixed in the Ti metal film to deteriorate the barrier property. However, the generation of particles could not be sufficiently suppressed.
【０００５】[0005]
【課題を解決するための手段】そこで、本発明者等は、
上述のように結晶粒の微細化したＴｉターゲットを用い
ても十分にパーティクル発生を抑制することができない
という原因を究明していたところ、微細結晶粒に含まれ
る双晶がパーティクル発生に影響を及ぼし、双晶を含む
結晶粒の面積率が少ないＴｉターゲットほどパーティク
ル発生数は少なくなり、従来の製造条件を制御して得ら
れたＴｉターゲットは双晶を含む結晶粒の面積率が５０
％を越えていることによりパーティクルの発生数が増大
するという研究結果が得られたのである。この発明はか
かる研究結果に基づいてなされたものであって、双晶を
含む結晶粒が５０面積％以下である多結晶組織からなる
スパッタリング用Ｔｉターゲットに特徴を有するもので
ある。Therefore, the present inventors have
As a result of investigating the cause that the generation of particles cannot be sufficiently suppressed even by using a Ti target with fine crystal grains as described above, twin crystals contained in the fine crystal grains influence the generation of particles. The smaller the area ratio of twin-containing crystal grains, the smaller the number of particles generated, and the Ti target obtained by controlling the conventional manufacturing conditions has the area ratio of twin-containing crystal grains of 50.
The result of the study was that the number of particles increased when the ratio exceeded%. The present invention has been made on the basis of such research results, and is characterized by a Ti target for sputtering having a polycrystalline structure in which crystal grains containing twins are 50 area% or less.
【０００６】この発明の双晶を含む結晶粒の面積率が５
０％以下である多結晶組織からなるスパッタリング用Ｔ
ｉターゲットを製造するには、先ず高純度のＴｉ原料を
電子ビーム法またはアーク溶解法により溶解し、純度：
９９．９９％以上の高純度Ｔｉインゴットを作製する。
この高純度Ｔｉインゴットを熱間鍛造したのち、加工
率：６０〜９０％の冷間加工を行ない、ついで４５０〜
４９５℃で熱処理すると、双晶を含む結晶粒が５０面積
％以下のＴｉターゲットが得られる。双晶を含む結晶粒
は存在しないことが最も好ましく、この双晶を含まない
結晶粒は、加工率：８０％の冷間加工を行ない、ついで
４８５℃で熱処理することにより得られる。The area ratio of the crystal grains containing twins according to the present invention is 5
T for sputtering having a polycrystalline structure of 0% or less
In order to manufacture an i target, first, a high-purity Ti raw material is melted by an electron beam method or an arc melting method, and the purity:
A high purity Ti ingot of 99.99% or more is produced.
After hot forging this high-purity Ti ingot, cold working is performed at a working rate of 60 to 90%, and then 450 to
When heat-treated at 495 ° C., a Ti target having crystal grains containing twins of 50 area% or less can be obtained. It is most preferable that there are no twin-containing crystal grains, and these twin-free crystal grains can be obtained by cold working at a working ratio of 80% and then heat-treating at 485 ° C.
【０００７】[0007]
【実施例】電子ビーム法により、直径：３００mm、長
さ：６００mmのインゴットを８００℃に３時間加熱保持
後、熱間鍛造して直径：１３０mmの鍛造棒とした。この
鍛造棒を長さ：７０mmに切断したのち、表１に示される
圧下率で冷間圧延して圧延板を作製した。Example An ingot having a diameter of 300 mm and a length of 600 mm was heated and held at 800 ° C. for 3 hours by an electron beam method, and then hot forged to obtain a forged rod having a diameter of 130 mm. This forged rod was cut into a length of 70 mm and then cold-rolled at a rolling reduction shown in Table 1 to produce a rolled plate.
【０００８】次に、この圧延板を表１に示される温度お
よび保持時間の熱処理を施すことにより表１に示される
多結晶組織を有する本発明Ｔｉターゲット１〜１４およ
び従来Ｔｉターゲットを作製した。Next, the rolled plate was heat-treated at the temperature and the holding time shown in Table 1 to produce Ti targets 1 to 14 of the present invention having the polycrystalline structure shown in Table 1 and conventional Ti targets.
【０００９】上記本発明Ｔｉターゲット１〜１４および
従来Ｔｉターゲットの表面を研摩し、その研摩面を４０
０倍の金属顕微鏡で写真撮影し、得られた金属組織写真
から双晶を含む結晶粒（以下、双晶結晶という）の面積
率およびその最大結晶粒径を測定し、その測定結果を表
１に示した。The surfaces of the Ti targets 1 to 14 of the present invention and the conventional Ti target are polished, and the polished surface is 40
The area ratio of the crystal grains containing twins (hereinafter referred to as twin crystals) and the maximum crystal grain size were measured from the obtained metallographic photograph, and the measurement results are shown in Table 1. It was shown to.
【００１０】さらに、上記本発明Ｔｉターゲット１〜１
４および従来Ｔｉターゲットを冷却用銅板にＰｂ−Ｓｎ
ハンダにて接合し、洗浄した後、スパッタリングに供し
た。その時のスパッタリング条件は下記の如くである。Further, the Ti targets 1 to 1 according to the present invention described above.
4 and conventional Ti target on a copper plate for cooling with Pb-Sn
After joining with solder and cleaning, the product was subjected to sputtering. The sputtering conditions at that time are as follows.
【００１１】スパッタリング条件 初期排気の到達真空度：１．７×１０-7Torr、 スパッタガスの全圧：０．０１０Torr、 Ｎ2 ガス圧：０．００６Torr、 スパッタ出力：６ＫＷ、 スパッタ処理時間：３０秒、 膜厚：２０００オングストローム、 ウエハサイズ：８インチ。Sputtering conditions Initial vacuum exhaust ultimate vacuum: 1.7 × 10 −7 Torr, total sputtering gas pressure: 0.010 Torr, N 2 gas pressure: 0.006 Torr, sputtering output: 6 KW, sputtering processing time: 30 Second, film thickness: 2000 angstrom, wafer size: 8 inches.
【００１２】上記条件でスパッタリングを行った後、ウ
エハ上に付着した直径：０．３μｍ以上のパーティクル
数をパーティクルカウンターにて計測し、その結果を表
１に示した。After performing the sputtering under the above conditions, the number of particles having a diameter of 0.3 μm or more attached on the wafer was measured by a particle counter, and the results are shown in Table 1.
【００１３】[0013]
【表１】 [Table 1]
【００１４】[0014]
【発明の効果】表１に示される結果から、双晶結晶の面
積率が５０％以下の本発明Ｔｉターゲット１〜１４は、
双晶結晶の面積率が５０％を越える従来Ｔｉターゲット
に比べてスパッタリングにより発生する直径：０．３μ
ｍ以上のパーティクル数が格段に少ないことがわかる。From the results shown in Table 1, the Ti targets 1 to 14 of the present invention having an area ratio of twin crystals of 50% or less are
Compared with the conventional Ti target in which the area ratio of twin crystals exceeds 50%, the diameter generated by sputtering is 0.3μ.
It can be seen that the number of particles of m or more is remarkably small.
【００１５】したがって、この発明のスパッタリング用
Ｔｉターゲットを用いてウエハ表面にＴｉ金属膜または
窒化Ｔｉ膜を形成すると、直径：０．５μｍ以上のパー
ティクル付着が極めて少ないところから不良品発生率が
極めて少なく、特に半導体産業上すぐれた効果をもたら
すものである。Therefore, when a Ti metal film or a Ti nitride film is formed on the surface of a wafer by using the sputtering Ti target of the present invention, the deposition rate of particles having a diameter of 0.5 μm or more is extremely small, and hence the defective product generation rate is extremely low. In particular, it has an excellent effect on the semiconductor industry.
Claims (1)
いて、 上記多結晶組織を構成する結晶粒のうち、双晶を含む結
晶粒の面積率が５０％以下（０％も含む）であることを
特徴とするスパッタリング用Ｔｉターゲット。1. A Ti target having a polycrystal structure, wherein the area ratio of crystal grains containing twins is 50% or less (including 0%) among the crystal grains constituting the polycrystal structure. And a Ti target for sputtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9458295A JPH08269698A (en) | 1995-03-28 | 1995-03-28 | Ti target for sputtering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9458295A JPH08269698A (en) | 1995-03-28 | 1995-03-28 | Ti target for sputtering |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08269698A true JPH08269698A (en) | 1996-10-15 |
Family
ID=14114279
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9458295A Withdrawn JPH08269698A (en) | 1995-03-28 | 1995-03-28 | Ti target for sputtering |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08269698A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5993621A (en) * | 1997-07-11 | 1999-11-30 | Johnson Matthey Electronics, Inc. | Titanium sputtering target |
| US6024847A (en) * | 1997-04-30 | 2000-02-15 | The Alta Group, Inc. | Apparatus for producing titanium crystal and titanium |
| US6063254A (en) * | 1997-04-30 | 2000-05-16 | The Alta Group, Inc. | Method for producing titanium crystal and titanium |
| US6210502B1 (en) | 1997-12-24 | 2001-04-03 | Toho Titanium Co., Ltd. | Processing method for high-pure titanium |
| US6309595B1 (en) | 1997-04-30 | 2001-10-30 | The Altalgroup, Inc | Titanium crystal and titanium |
| US6984272B2 (en) * | 2002-01-15 | 2006-01-10 | Toho Titanium Co., Ltd. | Process for producing titanium material for target, titanium material for target, and sputtering target using the same |
| CN104114303A (en) * | 2012-02-14 | 2014-10-22 | 吉坤日矿日石金属株式会社 | High-purity titanium ingots, manufacturing method therefor, and titanium sputtering target |
-
1995
- 1995-03-28 JP JP9458295A patent/JPH08269698A/en not_active Withdrawn
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6024847A (en) * | 1997-04-30 | 2000-02-15 | The Alta Group, Inc. | Apparatus for producing titanium crystal and titanium |
| US6063254A (en) * | 1997-04-30 | 2000-05-16 | The Alta Group, Inc. | Method for producing titanium crystal and titanium |
| US6309595B1 (en) | 1997-04-30 | 2001-10-30 | The Altalgroup, Inc | Titanium crystal and titanium |
| US6596228B2 (en) | 1997-04-30 | 2003-07-22 | Honeywell International Inc. | Titanium materials |
| US5993621A (en) * | 1997-07-11 | 1999-11-30 | Johnson Matthey Electronics, Inc. | Titanium sputtering target |
| US6302977B1 (en) | 1997-07-11 | 2001-10-16 | Johnson Matthey Electronics, Inc. | Method of making a target |
| US6509102B1 (en) | 1997-07-11 | 2003-01-21 | Honeywell International Inc. | Titanium film |
| US6210502B1 (en) | 1997-12-24 | 2001-04-03 | Toho Titanium Co., Ltd. | Processing method for high-pure titanium |
| US6984272B2 (en) * | 2002-01-15 | 2006-01-10 | Toho Titanium Co., Ltd. | Process for producing titanium material for target, titanium material for target, and sputtering target using the same |
| CN104114303A (en) * | 2012-02-14 | 2014-10-22 | 吉坤日矿日石金属株式会社 | High-purity titanium ingots, manufacturing method therefor, and titanium sputtering target |
| US10161032B2 (en) | 2012-02-14 | 2018-12-25 | Jx Nippon Mining & Metals Corporation | High-purity titanium ingots, manufacturing method therefor, and titanium sputtering target |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 20020604 |