JPH07197245A - Ti silicide sintered target material for sputtering hardly generating particle during film formation - Google Patents
Ti silicide sintered target material for sputtering hardly generating particle during film formationInfo
- Publication number
- JPH07197245A JPH07197245A JP35441293A JP35441293A JPH07197245A JP H07197245 A JPH07197245 A JP H07197245A JP 35441293 A JP35441293 A JP 35441293A JP 35441293 A JP35441293 A JP 35441293A JP H07197245 A JPH07197245 A JP H07197245A
- Authority
- JP
- Japan
- Prior art keywords
- tisi
- target material
- compound
- film formation
- phase
- 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- Withdrawn
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- Physical Vapour Deposition (AREA)
- Electrodes Of Semiconductors (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、半導体デバイスにお
ける電極や配線などを構成するＴｉシリサイド薄膜をス
パッタリングにより形成するのに用いた場合に、成膜中
に薄膜欠陥となるパーティクルの発生が著しく少ない焼
結ターゲット材に関するものである。BACKGROUND OF THE INVENTION The present invention, when used for forming a Ti silicide thin film which constitutes an electrode or wiring in a semiconductor device by sputtering, produces extremely few particles which become thin film defects during film formation. The present invention relates to a sintering target material.
【０００２】[0002]
【従来の技術】従来、一般に半導体デバイスの製造に際
して、スパッタリングにより低抵抗のＴｉシリサイド薄
膜を形成することが行なわれており、これにＴｉシリサ
イド焼結ターゲット材が用いられている。また、上記Ｔ
ｉシリサイド焼結ターゲット材は、例えば特開平１−１
３６９６９号公報に記載されるように、原料としてＴｉ
板材とＳｉ塊材を用い、これを所定の割合に秤量し、非
酸化性雰囲気中で電子ビーム溶解などにより溶解し、つ
いで粉砕し、ホットプレスすることにより製造されるこ
とも知られている。さらに、この結果得られたＴｉシリ
サイド焼結ターゲット材は、組成式：ＴｉＳｉｎ（ｎは
モル比で１．８〜２未満）を満足する場合、すなわち原
料としてＴｉＳｉ1.8 〜2 未満の組成を有する粉砕粉末
を用いてホットプレスした場合、Ｔｉ−Ｓｉ２元状態図
におけるＴｉＳｉ化合物相とＴｉＳｉ2 化合物相の２相
組織をもつようになることも知られている。2. Description of the Related Art Conventionally, in manufacturing a semiconductor device, a Ti silicide thin film having a low resistance is generally formed by sputtering, and a Ti silicide sintered target material is used for this. Also, the above T
The i-silicide sintering target material is, for example, Japanese Patent Application Laid-Open No. 1-1.
As described in Japanese Patent No. 36969, Ti is used as a raw material.
It is also known that a plate material and a Si lump material are used, which are weighed at a predetermined ratio, melted by electron beam melting or the like in a non-oxidizing atmosphere, then crushed and hot pressed. Further, the Ti silicide sintering target material obtained as a result is pulverized when it satisfies the composition formula: TiSin (n is a molar ratio of less than 1.8 to 2 ), that is, a raw material having a composition of TiSi 1.8 to less than 2 It is also known that when the powder is hot pressed, it has a two-phase structure of a TiSi compound phase and a TiSi 2 compound phase in the Ti-Si binary phase diagram.
【０００３】[0003]
【発明が解決しようとする課題】一方、近年のスパッタ
リング技術の進歩はめざましく、スパッタリング装置の
高出力化および大型化が可能となり、これに伴ない、Ｔ
ｉシリサイド薄膜の形成に際しても、成膜の高速化およ
び大面積化がはかられる傾向にあるが、上記の従来Ｔｉ
シリサイド焼結ターゲット材においては、これを用いて
高速成膜や大面積成膜を行なうと、成膜中にパーティク
ル（微細粒子）が発生し易くなるという問題がある。な
お、薄膜中にパーティクルが多数存在すると、これが例
えば０．５〜４μｍの線幅で形成された電極を断線させ
たり、配線内を短絡させたりするなどの原因となり、不
良率が増大するようになるものである。On the other hand, in recent years, the progress of sputtering technology has been remarkable and it has become possible to increase the output and size of a sputtering apparatus.
Even when the i-silicide thin film is formed, the film formation tends to be speeded up and the area can be increased.
When a high-speed film formation or large-area film formation is performed using the silicide sintering target material, there is a problem that particles (fine particles) are easily generated during the film formation. It should be noted that if a large number of particles are present in the thin film, this may cause, for example, disconnection of electrodes formed with a line width of 0.5 to 4 μm or short circuit in the wiring, thus increasing the defect rate. It will be.
【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、Ｔｉシリサイド薄膜のスパッタ
リングによる形成に際して、パーティクル発生の少ない
Ｔｉシリサイド焼結ターゲット材を開発すべく研究を行
なった結果、原料粉末として、予めＴｉ板材とＳｉ塊材
を所定の割合に秤量し、これを例えば電子ビーム溶解な
どにより溶解し、粉砕することにより調製した、Ｔｉ−
Ｓｉ２元状態図におけるＴｉＳｉ化合物とＴｉＳｉ2 化
合物の共晶からなるＴｉＳｉ−ＴｉＳｉ2 共晶粉末と、
同じく同状態図におけるＴｉＳｉ2 化合物とＳｉの共晶
からなるＴｉＳｉ2 −Ｓｉ共晶粉末を用い、これら両原
料粉末を所定の割合に配合し、混合した後、ホットプレ
スすることにより組成式：ＴｉＳｉｎ（ただし、ｎはモ
ル比で１．８〜２未満）を満足するＴｉシリサイド焼結
ターゲット材を製造すると、上記ホットプレス時に、上
記ＴｉＳｉ−ＴｉＳｉ2 共晶粉末とＴｉＳｉ2 −Ｓｉ共
晶粉末が反応して、これら両者間にはＴｉＳｉ2 化合物
が形成されるようになり、したがってこの結果のＴｉシ
リサイド焼結ターゲット材は、ＴｉＳｉ2 化合物の反応
生成相中に、未反応のＴｉＳｉ−ＴｉＳｉ2 共晶相が分
散分布した組織をもつようになり、このような組織を有
するＴｉシリサイド焼結ターゲット材においては、成膜
中のパーティクル発生が著しく減少し、パーティクルの
きわめて少ないＴｉシリサイド薄膜の形成が可能になる
という研究結果を得たのである。Therefore, the present inventors have
From the above viewpoints, when forming a Ti silicide thin film by sputtering, as a result of conducting research to develop a Ti silicide sintering target material with less generation of particles, as a raw material powder, a Ti plate material and a Si lump material were predetermined. Ti-, which was prepared by weighing in proportion, dissolving this by, for example, electron beam melting, and pulverizing
A TiSi-TiSi 2 eutectic powder composed of a eutectic of a TiSi compound and a TiSi 2 compound in a Si 2 state diagram,
Similarly, TiSi 2 —Si eutectic powder composed of a eutectic of TiSi 2 compound and Si in the same phase diagram is used, and both raw material powders are mixed at a predetermined ratio, mixed, and then hot pressed to form a composition formula: TiSin. When a Ti silicide sintering target material satisfying (where n is a molar ratio of less than 1.8 to 2) is manufactured, the TiSi—TiSi 2 eutectic powder and the TiSi 2 —Si eutectic powder are produced during the hot pressing. As a result of the reaction, a TiSi 2 compound is formed between them, and thus the resulting Ti silicide sintering target material is not reacted with the unreacted TiSi—TiSi 2 compound during the reaction formation phase of the TiSi 2 compound. The crystal phase has a structure in which it is dispersed and distributed, and in the Ti silicide sintered target material having such a structure, particles are generated during film formation. It was obtained the research result that the Ti silicide thin film with very few particles can be formed.
【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、ＴｉＳｉｎ（ただし、ｎはモル
比で１．８〜２未満）の組成式を満足し、かつＴｉ−Ｓ
ｉ２元状態図で示されるＴｉＳｉ2 化合物が反応生成相
として存在し、このＴｉＳｉ2 化合物反応生成相中に、
同状態図におけるＴｉＳｉ化合物とＴｉＳｉ2 化合物の
共晶からなる未反応共晶相が分散分布した組織を有する
スパッタリング用Ｔｉシリサイド焼結ターゲット材に特
徴を有するものである。なお、組成式におけるｎの値を
１．８〜２未満としたのは、ｎの値が１．８未満では所
望の低抵抗をもったＴｉシリサイド薄膜を形成すること
ができず、一方ｎ値が２以上になると上記の組成を形成
することが困難になる。The present invention was made based on the above research results, and satisfies the composition formula of TiSin (where n is a molar ratio of less than 1.8 to 2) and Ti-S.
The TiSi 2 compound shown in the i2 binary phase diagram exists as a reaction product phase, and in the TiSi 2 compound reaction product phase,
This is characterized by a Ti silicide sintering target material for sputtering having a structure in which an unreacted eutectic phase composed of a eutectic of a TiSi compound and a TiSi 2 compound in the same phase diagram is distributed. Note that the value of n in the composition formula is set to be 1.8 to less than 2 because a Ti silicide thin film having a desired low resistance cannot be formed when the value of n is less than 1.8, while Is 2 or more, it becomes difficult to form the above composition.
【０００６】[0006]
【実施例】つぎに、この発明のＴｉシリサイド焼結ター
ゲット材を実施例により具体的に説明する。まず、５Ｎ
（ナイン）の高純度Ｔｉ板材と７Ｎの高純度Ｓｉ塊材を
用い、これらを所定の割合に秤量し、真空度：１０-5to
rrの雰囲気中、水冷銅ハースにて電子ビーム溶解を行な
い、ついでジョークラッシャーにて粗粉砕し、さらにボ
ールミルで微粉砕して、それぞれＴｉ−Ｓｉ２元状態図
におけるＴｉＳｉ化合物とＴｉＳｉ2 化合物の共晶から
なるＴｉＳｉ−ＴｉＳｉ2 共晶粉末と、同じく同状態図
におけるＴｉＳｉ2 化合物とＳｉの共晶からなるＴｉＳ
ｉ2 −Ｓｉ共晶粉末を調製し、ついでこれら両共晶粉末
を原料粉末として用い、２０〜１００μｍの範囲内の所
定の平均粒径に調整した状態で、表１に示される割合に
配合し、Ｖ型ミキサーにて３０分間混合した後、温度：
１３００℃、圧力：２０ＭＰａ、保持時間：６０分の条
件でホットプレスすることにより組成式：ＴｉＳｉｎの
ｎの値がそれぞれ表１に示される値をもち、かついずれ
もＴｉＳｉ2 化合物反応生成相中に、ＴｉＳｉ−ＴｉＳ
ｉ2 共晶の未反応共晶相が分散分布した組織を有し、さ
らに直径：２５０mmφ×厚さ：１０mmの寸法をもった本
発明Ｔｉシリサイド焼結ターゲット材（以下、本発明タ
ーゲット材という）１〜３をそれぞれ製造した。EXAMPLES Next, the Ti silicide sintering target material of the present invention will be specifically described by way of examples. First, 5N
(Nine) high-purity Ti plate material and 7N high-purity Si block material are used, and these are weighed at a predetermined ratio, and the degree of vacuum is 10 −5 to
in an atmosphere of rr, performs electron beam melting at a water-cooled copper hearth, then coarsely crushed by a jaw crusher, further eutectic was finely pulverized by a ball mill, TiSi compound in Ti-Si2 binary phase diagram respectively TiSi 2 compound TiSi-TiSi 2 eutectic powder consisting of, and TiS composed of a eutectic of TiSi 2 compound and Si in the same phase diagram
i 2 -Si eutectic powder was prepared, and then both of these eutectic powders were used as raw material powders, and they were blended in the proportions shown in Table 1 in a state of being adjusted to a predetermined average particle size within the range of 20 to 100 μm. After mixing for 30 minutes with a V-type mixer, the temperature:
By hot pressing under the conditions of 1300 ° C., pressure: 20 MPa, holding time: 60 minutes, the value of n in the composition formula: TiSin has the value shown in Table 1, and both are in the TiSi 2 compound reaction formation phase. , TiSi-TiS
i 2 eutectic unreacted eutectic phase has a structure in which it is distributed, and further has a size of diameter: 250 mmφ × thickness: 10 mm, the Ti silicide sintering target material of the present invention (hereinafter referred to as the target material of the present invention) 1-3 were produced respectively.
【０００７】また、比較の目的で、上記の高純度Ｔｉ板
材と高純度Ｓｉ塊材の秤量割合をかえて組成式：ＴｉＳ
ｉｎのｎが表２に示される値のＴｉＳｉｎ粉末を調製
し、これを原料粉末として用いる以外は同一の条件で従
来Ｔｉシリサイド焼結ターゲット材（以下、従来ターゲ
ット材という）１〜３をそれぞれ製造した。この従来タ
ーゲット材１〜３は、いずれもＴｉＳｉ相とＴｉＳｉ2
相からなる組織をもつものであった。For the purpose of comparison, the composition formula: TiS is changed by changing the weighing ratios of the high-purity Ti plate material and the high-purity Si lump material.
A conventional Ti silicide sintering target material (hereinafter referred to as a conventional target material) 1 to 3 was produced under the same conditions except that TiSin powder having a value of n of in shown in Table 2 was prepared and used as a raw material powder. did. These conventional target materials 1 to 3 all have a TiSi phase and TiSi 2
It had an organization consisting of phases.
【０００８】つぎに、この結果得られた各種ターゲット
材を、スパッタリング装置に組み込み、基板：直径１５
２mmのＳｉウェハ、基板温度：１８０℃、基板とターゲ
ット材間の距離：６０mm、雰囲気：４×１０-3torrのＡ
ｒガス、直流出力：１．５ＫＷ、成膜速度：２５０nm／
min 、スパッタ時間：１分、の条件でＳｉウェハの表面
にＴｉシリサイド薄膜を形成し、Ｓｉウェハ表面の薄膜
における直径：０．３μｍ以上のパーティクル発生数を
測定した。この測定結果をそれぞれ表１，２に示した。Next, the various target materials obtained as a result were incorporated into a sputtering apparatus, and the substrate: diameter 15
2 mm Si wafer, substrate temperature: 180 ° C., distance between substrate and target material: 60 mm, atmosphere: 4 × 10 −3 torr A
r gas, DC output: 1.5 kW, film formation rate: 250 nm /
A Ti silicide thin film was formed on the surface of the Si wafer under the conditions of min and sputtering time: 1 minute, and the number of particles having a diameter of 0.3 μm or more in the thin film on the Si wafer surface was measured. The measurement results are shown in Tables 1 and 2, respectively.
【０００９】[0009]
【表１】 [Table 1]
【００１０】[0010]
【表２】 [Table 2]
【００１１】[0011]
【発明の効果】表１，２に示される結果から、ＴｉＳｉ
2 反応生成相中に、ＴｉＳｉ−ＴｉＳｉ2 共晶の未反応
共晶相が分散分布する組織を有する本発明ターゲット材
１〜３で形成されたＴｉシリサイド薄膜中には、ＴｉＳ
ｉ相−ＴｉＳｉ2 相からなる組織を有する従来ターゲッ
ト材１〜３を用いて形成された薄膜に比してパーティク
ル発生が著しく少ないことが明らかである。上述のよう
に、この発明のスパッタリング用Ｔｉシリサイド焼結タ
ーゲット材は、成膜中のパーティクル発生がきわめて少
なく、これは成膜速度を上げても、また成膜面積を大き
くしても変らないので、スパッタリング装置の高出力化
および大型化に十分満足に対応することができるもので
ある。From the results shown in Tables 1 and 2, TiSi
In the Ti silicide thin film formed of the target materials 1 to 3 of the present invention having a structure in which the unreacted eutectic phase of TiSi—TiSi 2 eutectic is distributed and distributed in the 2 reaction generated phase, TiS
It is clear that the generation of particles is significantly smaller than that of the thin films formed by using the conventional target materials 1 to 3 having the structure of i phase-TiSi 2 phase. As described above, the Ti silicide sintering target material for sputtering of the present invention has extremely few particles generated during film formation, and this does not change even if the film formation rate is increased or the film formation area is increased. It is possible to satisfactorily deal with the increase in output and the increase in size of the sputtering apparatus.
Claims (1)
８〜２未満）の組成式を満足し、かつＴｉ−Ｓｉ２元状
態図で示されるＴｉＳｉ2 化合物が反応生成相として存
在し、このＴｉＳｉ2 化合物反応生成相中に、同状態図
におけるＴｉＳｉ化合物とＴｉＳｉ2 化合物とＳｉの共
晶からなる未反応共晶相が分散分布した組織を有するこ
とを特徴とする成膜中にパーティクル発生の少ないスパ
ッタリング用Ｔｉシリサイド焼結ターゲット材。1. TiSin (where n is a molar ratio of 1.
8 to less than 2), and a TiSi 2 compound shown in the Ti-Si binary phase diagram is present as a reaction product phase. In the TiSi 2 compound reaction product phase, the TiSi compound and the TiSi compound in the phase diagram are A Ti silicide sintering target material for sputtering with less particles generated during film formation, which has a structure in which an unreacted eutectic phase composed of a TiSi 2 compound and Si is dispersed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35441293A JPH07197245A (en) | 1993-12-28 | 1993-12-28 | Ti silicide sintered target material for sputtering hardly generating particle during film formation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP35441293A JPH07197245A (en) | 1993-12-28 | 1993-12-28 | Ti silicide sintered target material for sputtering hardly generating particle during film formation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07197245A true JPH07197245A (en) | 1995-08-01 |
Family
ID=18437386
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP35441293A Withdrawn JPH07197245A (en) | 1993-12-28 | 1993-12-28 | Ti silicide sintered target material for sputtering hardly generating particle during film formation |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07197245A (en) |
-
1993
- 1993-12-28 JP JP35441293A patent/JPH07197245A/en not_active Withdrawn
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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: 20010306 |