JP2001002471A - High-density sputtering sintered target material not cracked even in high-speed film forming condition - Google Patents
High-density sputtering sintered target material not cracked even in high-speed film forming conditionInfo
- Publication number
- JP2001002471A JP2001002471A JP11173780A JP17378099A JP2001002471A JP 2001002471 A JP2001002471 A JP 2001002471A JP 11173780 A JP11173780 A JP 11173780A JP 17378099 A JP17378099 A JP 17378099A JP 2001002471 A JP2001002471 A JP 2001002471A
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- target material
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- film forming
- porosity
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、特に次世代高集
積半導体メモリーの電極として適用される高誘電体酸化
物キャパシタ用電極薄膜の形成に際して、高速成膜条件
でも割れ発生のない高密度スパッタリング燒結ターゲッ
ト材に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to high density sputtering sintering which does not generate cracks even under high-speed film forming conditions, particularly when forming an electrode thin film for a high dielectric oxide capacitor used as an electrode of a next generation highly integrated semiconductor memory. It concerns the target material.
【０００２】[0002]
【従来の技術】近年、次世代高集積半導体メモリーの電
極として高誘電体酸化物キャパシタ薄膜が注目されてい
る。また、上記の高誘電体酸化物キャパシタの電極薄膜
が、（Ｌａ，Ｓｒ）ＣｏＯ 3の組成式で表され、かつ主
構成相がぺロブスカイト構造を有する複合酸化物燒結材
をターゲット材として用い、スパッタリング法により形
成されることも知られている。さらに、上記のスパッタ
リング燒結ターゲット材が、原料粉末として、Ｌａ2Ｏ3
粉末とＳｒＣＯ3粉末、さらにＣｏＯ粉末および／また
はＣｏ3Ｏ4粉末を用い、これら原料粉末を所定の配合組
成に配合し、混合した後、大気中、１１００〜１３００
℃の温度に所定時間保持の条件で焼成して、（Ｌａ，Ｓ
ｒ）ＣｏＯ3の組成式で表され、かつ主構成相がぺロブ
スカイト構造を有する複合酸化物を形成し、粉砕して１
０μｍ以下の平均粒径とした後、１〜３ｔｏｎ／ｃｍ2
の圧力で圧粉体にプレス成形し、この圧粉体を同じく大
気中、１１００〜１３００℃の温度に１〜３時間保持
後、炉冷の条件で燒結することにより製造されることも
知られている。2. Description of the Related Art In recent years, the power of next-generation highly integrated semiconductor memories has been increasing.
High dielectric oxide capacitor thin films are attracting attention as poles
You. Also, the electrode thin film of the high dielectric oxide capacitor described above.
Is (La, Sr) CoO ThreeRepresented by the composition formula
Composite oxide sintered material whose constituent phase has perovskite structure
Is used as a target material, and is formed by sputtering.
It is also known that In addition, the above sputtering
Ring sintering target material is LaTwoOThree
Powder and SrCOThreePowder, further CoO powder and / or
Is CoThreeOFourPowders and combine these raw material powders in a prescribed
After mixing and mixing, in air, 1100-1300
(La, S)
r) CoOThreeAnd the main constituent phase is perov
A composite oxide having a skyte structure is formed and pulverized to form 1
After having an average particle size of 0 μm or less, 1 to 3 ton / cmTwo
Pressing into a green compact at a pressure of
In air, kept at 1100-1300 ° C for 1-3 hours
Later, it may be manufactured by sintering under furnace cooling conditions.
Are known.
【０００３】[0003]
【発明が解決しようとする課題】一方、スパッタリング
に限らず、その他の成膜技術分野では、成膜速度の高速
化が常に命題として掲げられ、これに対する研究がなさ
れているが、スパッタリング燒結ターゲット材の場合、
成膜速度を速くするために、高出力条件で成膜を行うと
きわめて割れが発生し易くなり、また割れ防止の目的で
空孔率を上げて低密度化すると成膜厚さに局部的に不均
一が生じるようになるのが現状である。On the other hand, not only in sputtering but also in other film forming technology fields, increasing the film forming rate has always been proposed as a proposition, and research on this has been conducted. in the case of,
If the film is formed under high power conditions to increase the film formation rate, cracks are extremely likely to occur.If the porosity is increased to reduce the density for the purpose of preventing cracks, the film thickness will be locally reduced. At present, non-uniformity occurs.
【０００４】[0004]
【課題を解決するための手段】そこで、本発明者らは、
上述のような観点から、高誘電体酸化物キャパシタ用電
極薄膜の高速生膜を可能にするスパッタリング燒結ター
ゲット材を開発すべく研究を行った結果、（ａ）上記の
公知のスパッタリング燒結ターゲット材は、約２０％の
空孔率をもつが、成膜速度の向上を図る目的で、空孔率
を小さく、すなわち密度を上げたり、成膜出力を高くし
たりすると割れが発生し易くなり、一方ターゲット材の
空孔率を上げた、すなわち密度を下げた状態で成膜出力
を高くして成膜速度の向上を試みると、割れはなくなる
が、成膜厚さに不均一が生じるようになること。Means for Solving the Problems Accordingly, the present inventors have:
From the above-mentioned viewpoints, as a result of researching to develop a sputtering sintered target material capable of high-speed deposition of an electrode thin film for a high dielectric oxide capacitor, (a) the above-mentioned known sputtering sintered target material is Has a porosity of about 20%, but if the porosity is reduced, that is, if the density is increased or the deposition output is increased for the purpose of improving the film formation rate, cracks are likely to occur. When the porosity of the target material is increased, that is, when the density is reduced, the output of the film is increased to increase the film forming speed, and cracks are eliminated, but the film thickness becomes non-uniform. thing.
【０００５】（ｂ）上記の通りスパッタリング燒結ター
ゲット材においては、高速成膜に際して、成膜厚さに均
一性から空孔率を２０％以上に上げることはできない
が、成膜出力を高くすると割れが生じるのは、不可避不
純物として含有する炭素（Ｃ）、ナトリウム（Ｎａ）、
およびカリウム（Ｋ）の含有量と密接な関係があるこ
と。(B) As described above, in the sputtering sintered target material, the porosity cannot be increased to 20% or more due to uniformity in the film thickness at the time of high-speed film formation. Is caused by carbon (C), sodium (Na),
And the content of potassium (K).
【０００６】（ｃ）上記の公知のスパッタリング燒結タ
ーゲット材は、不可避不純物として、Ｃ ：１５０〜４
００ｐｐｍ、Ｎａ：５０〜２００ｐｐｍ、Ｋ ：５〜３
０ｐｐｍ、を含有するが、これの燒結に際して、燒結雰
囲気を、大気雰囲気に変わって加圧酸素雰囲気にする
と、これらの不可避不純物含有量を低減することができ
ること。(C) The above-mentioned known sputtering sintered target material contains C: 150 to 4 as an unavoidable impurity.
00 ppm, Na: 50 to 200 ppm, K: 5 to 3
0 ppm, but when sintering, if the sintering atmosphere is changed to an atmospheric atmosphere and a pressurized oxygen atmosphere, the content of these unavoidable impurities can be reduced.
【０００７】（ｄ）これらの不可避不純物の含有量を、
Ｃ ：１００ｐｐｍ以下、Ｎａ：１０ｐｐｍ以下、Ｋ
：５ｐｐｍ以下、にすると、約２０％の通常の空孔率
は勿論のこと、空孔率を１５％以下に小さくした高密度
状態で成膜出力を高くしても割れ発生がなくなり、均一
な厚さでの高速成膜が可能になること。以上（ａ）〜
（ｄ）に示される研究結果を得たのである。(D) The content of these unavoidable impurities is
C: 100 ppm or less, Na: 10 ppm or less, K
: When the content is 5 ppm or less, cracks are eliminated even when the film formation output is increased in a high-density state where the porosity is reduced to 15% or less, as well as the normal porosity of about 20%. High-speed film formation with a thickness is possible. (A) ~
The research results shown in (d) were obtained.
【０００８】この発明は、上記の研究結果に基づいてな
されたもであって、（Ｌａ，Ｓｒ）ＣｏＯ3の組成式で
表わされ、主構成相がぺロブスカイト構造を有する複合
酸化物燒結材からなる高誘電体酸化物キャパシタ用電極
薄膜形成用スパッタリング燒結ターゲット材において、
不可避不純物として含有する炭素（Ｃ）、ナトリウム
（Ｎａ）、およびカリウム（Ｋ）の含有量を、それぞ
れ、Ｃ ：１００ｐｐｍ以下、Ｎａ： １０ｐｐｍ以
下、Ｋ ： ５ｐｐｍ以下、に低減し、空孔率を１５
％以下としてなる、高速成膜条件でも割れ発生のない高
密度スパッタリング燒結ターゲット材に特徴を有するも
である。The present invention has been made based on the above research results, and is a composite oxide sintered material represented by a composition formula of (La, Sr) CoO 3 and having a main constituent phase having a perovskite structure. In a sputtering sintered target material for forming an electrode thin film for a high dielectric oxide capacitor comprising
The contents of carbon (C), sodium (Na), and potassium (K) contained as inevitable impurities are reduced to C: 100 ppm or less, Na: 10 ppm or less, and K: 5 ppm or less, respectively, to reduce the porosity. Fifteen
% Or less, which is characterized by a high-density sputtering sintering target material that does not crack even under high-speed film forming conditions.
【０００９】なお、この発明のスパッタリング燒結ター
ゲット材において、不可避不純物として含有するＣ、Ｎ
ａ、およびＫの上限値は経験的に定められたものであっ
て、前記不可避不純物のうちのいずれかの成分でも上記
の上限値を越えるとターゲット材に割れが発生し易くな
るもである。したがってこれら不可避不純物の含有量が
上記の上限値以下であれば、通常の空孔率（約２０％）
は勿論のこと、さらに一段の高速成膜を可能ならしめる
目的で空孔率を下げて、すなわち密度を上げて１５％以
下の空孔率として、高速条件で成膜を行ってもターゲッ
ト材に割れ発生はなくなるものであり、この場合空孔率
を１５％以下にしないと、通常の空孔率である約２０％
に比して成膜速度に顕著な向上効果が得られないもので
ある。また、上記不可避不純物の上記上限値以下での含
有量の調整は、燒結時の加圧酸素雰囲気の圧力を調整す
ることによりなされるものである。In the sputtering sintered target material of the present invention, C and N contained as unavoidable impurities are contained.
The upper limits of a and K are empirically determined, and if any of the inevitable impurities exceeds the above upper limit, cracks may easily occur in the target material. Therefore, if the content of these unavoidable impurities is equal to or less than the above upper limit, the normal porosity (about 20%)
Needless to say, the porosity is reduced for the purpose of enabling one-step high-speed film formation, that is, the porosity is increased to 15% or less by increasing the density. The occurrence of cracks is eliminated. In this case, if the porosity is not reduced to 15% or less, the normal porosity of about 20%
In this case, a remarkable effect of improving the film formation rate cannot be obtained. Adjustment of the content of the unavoidable impurities below the upper limit is performed by adjusting the pressure of the pressurized oxygen atmosphere during sintering.
【００１０】[0010]
【発明の実施の態様】つぎに、この発明のスパッタリン
グ燒結ターゲット材を実施例により具体的に説明する。
原料粉末として、いずれも０．３〜５μｍの範囲内の所
定の平均粒径を有するＬａ2Ｏ3粉末、ＳｒＣＯ3粉末、
ＣｏＯ粉末、およびＣｏ3Ｏ4粉末を用意し、これら原料
粉末を所定の配合組成に配合し、混合した後、大気中、
温度：１２００℃に１２時間保持の条件で焼成して、そ
れぞれ表１に示される組成を有し、かつ主構成相がぺロ
ブスカイト構造を有する複合酸化物を形成し、粉砕して
平均粒径：１μｍとした後、１〜３ｔｏｎ／ｃｍ2の範
囲内の所定の圧力で圧粉体にプレス成形し、この圧粉体
を、それぞれ１．５〜１０ａｔｍの範囲内の所定の圧力
の加圧酸素雰囲気中、１１００〜１３００℃の範囲内の
所定の温度に２時間保持後、炉冷の条件で燒結すること
により、直径：１２５ｍｍ×厚さ：５ｍｍの寸法を有
し、かつ同じく表１に示される空孔率および不可避不純
物含有量の本発明スパッタリング燒結ターゲット材（以
下、本発明ターゲット材と云う）１〜５をそれぞれ製造
した。Next, the sputtering sintered target material of the present invention will be specifically described with reference to examples.
La 2 O 3 powder, SrCO 3 powder, each having a predetermined average particle size in the range of 0.3 to 5 μm,
A CoO powder and a Co 3 O 4 powder are prepared, and these raw material powders are blended into a predetermined blending composition and mixed.
Temperature: calcination at 1200 ° C. for 12 hours to form a composite oxide having a composition shown in Table 1 and a main constituent phase having a perovskite structure. After the thickness is set to 1 μm, the green compact is press-molded at a predetermined pressure in the range of 1 to 3 ton / cm 2 , and the green compact is pressurized oxygen having a predetermined pressure in the range of 1.5 to 10 atm. After maintaining at a predetermined temperature in the range of 1100 to 1300 ° C. for 2 hours in an atmosphere and sintering under the condition of furnace cooling, it has a size of diameter: 125 mm × thickness: 5 mm, and is also shown in Table 1. Of the present invention (hereinafter, referred to as the target material of the present invention) 1 to 5 having a porosity and an unavoidable impurity content, respectively.
【００１１】また、比較の目的で、同じく表１に示され
る通り上記本発明ターゲット材１〜５の製造に用いたと
同じ複合酸化物を用い、同じく粉砕して平均粒径：１μ
ｍとした後、１ｔｏｎ／ｃｍ2ので圧粉体にプレス成形
し、この圧粉体を、大気中、１１００〜１３００℃の範
囲内の所定の温度に２時間保持後、炉冷の条件で燒結す
ることにより、同じく直径：１２５ｍｍ×厚さ：５ｍｍ
の寸法を有し、かつ表１に示される空孔率および不可避
不純物含有量の従来スパッタリング燒結ターゲット材
（以下、従来ターゲット材と云う）１〜５をそれぞれ製
造した。For comparison purposes, as shown in Table 1, the same composite oxide as used in the production of the above-mentioned target materials 1 to 5 of the present invention was used and pulverized to obtain an average particle size of 1 μm.
m, and then press-molded into a green compact at 1 ton / cm 2 , and held in air at a predetermined temperature in the range of 1100 to 1300 ° C. for 2 hours, and then sintered under furnace cooling conditions. By doing, the same: diameter: 125 mm × thickness: 5 mm
And the conventional sintering sintered target materials (hereinafter referred to as conventional target materials) 1 to 5 having the porosity and the inevitable impurity content shown in Table 1 were produced, respectively.
【００１２】ついで、これらの各種のターゲット材を、
それぞれ純銅製バッキングプレートにＩｎ-Ｓｎ合金ろ
う材を用いてボンディングした状態でスパッタリング装
置に装入し、以下の条件、すなわち、 基板：直径１００ｍｍの単結晶Ｓｉウエハー、 基板温度：６００℃、 ターゲット材と基板間の距離：５０ｍｍ、 雰囲気ガス：Ａｒ／酸素（流量比：８／２）、 雰囲気圧力：０．８Ｐａ、 直流出力：１００Ｗ（通常成膜条件）および３００Ｗ
（高速成膜条件）、 成膜時間：５分、 の通常成膜条件および高速成膜条件でスパッタリング試
験を行い、試験後の基板上の成膜厚さから成膜速度およ
びターゲット材の割れ発生の有無を測定した。これらの
測定結果を表１に示した。Next, these various target materials are
Each was mounted on a pure copper backing plate using an In-Sn alloy brazing material and bonded to a sputtering apparatus under the following conditions: substrate: single-crystal Si wafer having a diameter of 100 mm; substrate temperature: 600 ° C; Distance between substrate and substrate: 50 mm, atmosphere gas: Ar / oxygen (flow rate ratio: 8/2), atmosphere pressure: 0.8 Pa, DC output: 100 W (normal film formation conditions) and 300 W
(High-speed film-forming conditions), film-forming time: 5 minutes, performing a sputtering test under normal film-forming conditions and high-speed film-forming conditions. Was measured. Table 1 shows the results of these measurements.
【００１３】[0013]
【表１】 [Table 1]
【００１４】[0014]
【発明の効果】表１に示される結果から、本発明ターゲ
ット材１〜５は、従来ターゲット材１〜５に比して相対
的に密度が高いので、通常成膜条件および高速成膜条件
のいずれでも相対的に高い成膜速度を示し、また高速成
膜条件でも不可避不純物含有量の低減によって割れの発
生はなく、一方従来ターゲット材１〜５ではいずれも不
可避不純物含有量が相対的に高いので、高速成膜条件で
は相対的に密度が本発明ターゲット材１〜５に比して低
いにもかかわらず、割れが発生し、スパッタリングのさ
らなる続行は困難であった。上述のように、この発明の
スパッタリング燒結ターゲット材は、スパッタリングに
よる高誘電体酸化物キャパシタ用電極薄膜の高速成膜に
十分満足に対応できるものである。According to the results shown in Table 1, since the target materials 1 to 5 of the present invention have a relatively high density as compared with the conventional target materials 1 to 5, the target materials under the normal film forming conditions and the high-speed film forming conditions are not used. In any case, a relatively high film forming rate is exhibited, and even under high-speed film forming conditions, no crack is generated due to the reduction of the unavoidable impurity content, while the conventional target materials 1 to 5 have relatively high unavoidable impurity contents. Therefore, under the conditions of high-speed film formation, cracks occurred even though the density was relatively lower than those of the target materials 1 to 5 of the present invention, and it was difficult to continue sputtering. As described above, the sputtering sintering target material of the present invention can sufficiently satisfactorily cope with high-speed deposition of an electrode thin film for a high dielectric oxide capacitor by sputtering.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 丸山 仁 埼玉県大宮市北袋町１−297 三菱マテリ アル株式会社総合研究所内 Ｆターム(参考） 4G030 AA03 AA04 AA09 AA13 AA28 AA60 BA09 CA01 GA03 GA04 GA08 GA22 GA25 GA27 4G048 AA03 AB01 AC02 AD08 AE05 4K029 AA06 BA50 BC05 BD01 CA05 DC05 DC24 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Hitoshi Maruyama 1-297 Kitabukuro-cho, Omiya-shi, Saitama F-term in Mitsubishi Materials Real Research Laboratory (reference) 4G030 AA03 AA04 AA09 AA13 AA28 AA60 BA09 CA01 GA03 GA04 GA08 GA22 GA25 GA27 4G048 AA03 AB01 AC02 AD08 AE05 4K029 AA06 BA50 BC05 BD01 CA05 DC05 DC24
Claims (1)
され、主構成相がぺロブスカイト構造を有する複合酸化
物燒結材からなる高誘電体酸化物キャパシタ用電極薄膜
形成用スパッタリング燒結ターゲット材において、 不可避不純物として含有する炭素（Ｃ）、ナトリウム
（Ｎａ）、およびカリウム（Ｋ）の含有量を、それぞ
れ、 Ｃ ：１００ｐｐｍ以下、 Ｎａ： １０ｐｐｍ以下、 Ｋ ： ５ｐｐｍ以下、 に低減し、空孔率を１５％以下としてなる、高速成膜条
件でも割れ発生のない高密度スパッタリング燒結ターゲ
ット材。1. A sputtering sintered target for forming an electrode thin film for a high dielectric oxide capacitor, which is represented by a composition formula of (La, Sr) CoO 3 and whose main constituent phase is a composite oxide sintered material having a perovskite structure. In the material, the contents of carbon (C), sodium (Na), and potassium (K) contained as unavoidable impurities are reduced to C: 100 ppm or less, Na: 10 ppm or less, and K: 5 ppm or less, respectively. A high-density sputtering sintering target material having a porosity of 15% or less and having no crack even under high-speed film forming conditions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11173780A JP2001002471A (en) | 1999-06-21 | 1999-06-21 | High-density sputtering sintered target material not cracked even in high-speed film forming condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11173780A JP2001002471A (en) | 1999-06-21 | 1999-06-21 | High-density sputtering sintered target material not cracked even in high-speed film forming condition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001002471A true JP2001002471A (en) | 2001-01-09 |
Family
ID=15967023
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11173780A Pending JP2001002471A (en) | 1999-06-21 | 1999-06-21 | High-density sputtering sintered target material not cracked even in high-speed film forming condition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001002471A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006241595A (en) * | 2005-02-01 | 2006-09-14 | Tosoh Corp | Sinter, sputtering target and molding die, and production process of sintered compact |
| TWI385139B (en) * | 2005-02-01 | 2013-02-11 | Tosoh Corp | A sintered body, a sputtering target and a forming die, and a sintered body manufacturing method using the same |
-
1999
- 1999-06-21 JP JP11173780A patent/JP2001002471A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006241595A (en) * | 2005-02-01 | 2006-09-14 | Tosoh Corp | Sinter, sputtering target and molding die, and production process of sintered compact |
| TWI385139B (en) * | 2005-02-01 | 2013-02-11 | Tosoh Corp | A sintered body, a sputtering target and a forming die, and a sintered body manufacturing method using the same |
| US8419400B2 (en) | 2005-02-01 | 2013-04-16 | Tosoh Corporation | Sintered body, sputtering target and molding die, and process for producing sintered body employing the same |
| KR101313217B1 (en) | 2005-02-01 | 2013-09-30 | 토소가부시키가이샤 | Sinter, sputtering target and molding die, and production process of sinter using the same |
| JP2014129231A (en) * | 2005-02-01 | 2014-07-10 | Tosoh Corp | Sintered compact and sputtering target |
| US9920420B2 (en) | 2005-02-01 | 2018-03-20 | Tosoh Corporation | Sintered body, sputtering target and molding die, and process for producing sintered body employing the same |
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