JPH0829435B2 - Method for manufacturing target for sputtering device by hot isostatic pressing - Google Patents
Method for manufacturing target for sputtering device by hot isostatic pressingInfo
- Publication number
- JPH0829435B2 JPH0829435B2 JP60117547A JP11754785A JPH0829435B2 JP H0829435 B2 JPH0829435 B2 JP H0829435B2 JP 60117547 A JP60117547 A JP 60117547A JP 11754785 A JP11754785 A JP 11754785A JP H0829435 B2 JPH0829435 B2 JP H0829435B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- target
- hot isostatic
- isostatic pressing
- pressure
- 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
Links
- 238000000034 method Methods 0.000 title claims description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000004544 sputter deposition Methods 0.000 title claims description 4
- 238000001513 hot isostatic pressing Methods 0.000 title description 11
- 239000000843 powder Substances 0.000 claims description 30
- 239000011888 foil Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 229910021332 silicide Inorganic materials 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 6
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 6
- 239000003870 refractory metal Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007596 consolidation process Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 229910016006 MoSi Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Landscapes
- Press Drives And Press Lines (AREA)
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はMOS−ICに使用されるゲート電極材料を形成
するに用いるに好適な、高密度の高融点金属シリサイド
からなるスパッタリング装置用ターゲットを熱間静水圧
プレスを用いて成形する製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention provides a sputtering apparatus target comprising a high-density refractory metal silicide, which is suitable for forming a gate electrode material used in a MOS-IC. The present invention relates to a manufacturing method of molding using a hot isostatic press.
近年MOS型LSIのゲート電極に、比抵抗の小さいモリブ
デンやタングステンなどの高融点金属のシリサイド（珪
化物）が用いられるようになってきた。こうして高融点
金属のシリサイドの膜を形成するには、高融点金属のシ
リサイド製のターゲットを用いたスパッタリング法が主
として採用されている。In recent years, silicides of high melting point metals such as molybdenum and tungsten having low specific resistance have been used for gate electrodes of MOS type LSIs. In order to form a silicide film of a refractory metal in this way, a sputtering method using a target made of a refractory metal silicide is mainly adopted.
高融点金属のシリサイド特にモリブデンシリサイド製
のターゲットは、一般にモリブデン粉末とシリコン粉末
との混合粉を原料とするか、あるいはモリブデンシリサ
イド粉末を原料としてホットプレス法或いは無加圧真空
焼結法で製造されている。A refractory metal silicide, particularly a target made of molybdenum silicide, is generally produced by using a mixed powder of molybdenum powder and silicon powder as a raw material, or by using a molybdenum silicide powder as a raw material by a hot pressing method or a pressureless vacuum sintering method. ing.
ホットプレス法で相対密度90％以上であるターゲット
を製造する場合には加熱温度1400℃以上，圧力100kg/cm
2以上が必要となる。しかしながら、加圧容器にカーボ
ン材料を用いた場合には加熱温度が高いためにターゲッ
ト材へのカーボン（Ｃ）の混入が問題であり、また加圧
容器にセラミック材料を用いた場合にはターゲットへの
材料の混入は無いものの容器の破損が問題となってい
る。When manufacturing a target with a relative density of 90% or more by the hot press method, the heating temperature is 1400 ° C or more and the pressure is 100 kg / cm.
2 or more is required. However, when a carbon material is used for the pressure vessel, the heating temperature is high, so mixing of carbon (C) into the target material is a problem, and when a ceramic material is used for the pressure vessel, the target material is Although there is no mixing of the above materials, damage to the container is a problem.
また、例えば直径が180mm未満、厚み10mm未満のター
ゲットを一枚成形する場合は、直径中心まで均一に90％
以上で圧密出来るが、量産用の直径220mm、厚み40mmタ
ーゲットをホットプレス成形する場合、外周部は90％以
上の密度が得られるが中央部は80％程度となり、ターゲ
ット自体の圧密不足、圧密むらが起り、スパッタ成膜に
粒状物が付着し膜特性を損うという問題もあった。In addition, for example, when molding a single target with a diameter of less than 180 mm and a thickness of less than 10 mm, it is necessary to maintain a uniform 90%
Although it is possible to consolidate by the above, when hot-press molding a target of 220 mm in diameter and 40 mm in thickness for mass production, a density of 90% or more can be obtained in the outer peripheral part but about 80% in the center part, insufficient consolidation of target itself, uneven consolidation However, there is also a problem in that particulate matter adheres to the sputtered film to impair the film characteristics.
一方、無加圧真空焼結法による場合は、焼結温度1700
℃においても約60〜70％の密度しか得られず密度不足の
ためにほとんど実用に供し得なかった。On the other hand, when using the pressureless vacuum sintering method, the sintering temperature is 1700
Even at ℃, only about 60-70% density was obtained and it was practically unusable due to lack of density.
一方、モリブデンシリサイド粉末を圧密封入缶に封入
し熱間静水圧プレスにより圧密焼結することにより、低
温で高密度化でき均一な組成分布であり、かつ不純物の
混入のないターゲットを成形することが出来る。On the other hand, by encapsulating molybdenum silicide powder in a pressure-sealed can and compacting and sintering with hot isostatic pressing, it is possible to form a target that has a uniform composition distribution and can be densified at low temperature, and has no impurities mixed in. I can.
第１表はモリブデンシリサイド粉末をホットプレス、
無加圧焼結および熱間静水圧プレス（HIP）により焼結
成形した条件を示すもので、第１表の条件により焼結成
形したターゲットの特性を示したものが表２である。こ
れらの表より熱間静水圧プレスによる焼結成形のすぐれ
ていることが判る。Table 1 shows hot pressing of molybdenum silicide powder,
Table 2 shows the conditions for sintering and forming by pressureless sintering and hot isostatic pressing (HIP), and Table 2 shows the characteristics of the targets for sintering and forming under the conditions in Table 1. From these tables, it can be seen that the sinter molding by hot isostatic pressing is excellent.
しかし、熱間静水圧プレス成形工程において、圧密封
入缶として経済的に使用できる鉄を主体とする金属缶材
を用いることができるが、この場合は本合金のSiと容易
に1200℃で共晶反応し、缶が破壊したりあるいは缶材に
よる汚染を生じる。又、缶材と成形体の界面が接着して
いるため、缶材と成形体の熱膨張差により成形体に引張
応力が働き成形体にクラックを生じることがある。However, in the hot isostatic pressing process, it is possible to use a metal can material mainly composed of iron that can be economically used as a pressure-sealed canister. Reacts, destroying the can or contaminating the can material. Further, since the interface between the can material and the molded product is adhered, tensile stress may act on the molded product due to the difference in thermal expansion between the can material and the molded product, and cracks may occur in the molded product.
〔問題点を解決するための手段〕 上記問題を解決するために本発明においては高融点金
属シリサイド粉末を圧密用封入缶に封入し、熱間静水圧
プレス（HIP）法により成形焼結するのに用いる圧密用
封入缶の内面にあらかじめBN粉末を塗布した封入缶を用
いることにより熱間静水圧プレス工程における缶材とタ
ーゲット材の反応あるいはターゲットのクラックなどの
欠陥を防止することが出来る。 [Means for Solving the Problems] In order to solve the above problems, in the present invention, a refractory metal silicide powder is enclosed in a compacting can and is compacted and sintered by a hot isostatic pressing (HIP) method. By using an encapsulating can in which the BN powder is applied in advance on the inner surface of the encapsulating encapsulating can used for, it is possible to prevent defects such as a reaction between the can material and the target material in the hot isostatic pressing step or a crack of the target.
すなわち、本発明は原料粉末を圧密封入缶内に封入し
熱間静水圧プレス焼結するに際し、内面にBN粉末を塗布
した圧密封入缶を用いて、原料粉末と圧密封入缶との間
にBN粉末を介在させることにより、成形体と圧密封入缶
との熱膨張差によるクラックの発生を低減したことを特
徴とする熱間静水圧プレス方法である。That is, the present invention, when encapsulating the raw material powder in a pressure-sealed canister and performing hot isostatic pressing and sintering, using a pressure-sealed canister coated with BN powder on the inner surface, the BN powder between the raw material powder and the pressure-sealed canister is used. The hot isostatic pressing method is characterized in that the generation of cracks due to the difference in thermal expansion between the molded body and the pressure-sealed canister is reduced by interposing the powder.
さらに望ましくはBN粉末のはくりによる局部的な浸蝕あ
るいはBNの汚染を防ぐためにBN塗布の内側に成形体を構
成する金属の箔を内張りすることにより完全なものとな
る。More preferably, in order to prevent local erosion due to peeling of the BN powder or contamination of the BN, a metal foil constituting the compact is lined inside the BN coating to complete the BN coating.
本発明は、上述のようにシリサイド粉末を原料粉末と
して使用するものに好適であるが、HIPに使用する封入
缶からの汚染を防ぐ効果において、原料粉末を特定する
ものではない。The present invention is suitable for use of the silicide powder as the raw material powder as described above, but does not specify the raw material powder in terms of the effect of preventing contamination from the canister used for HIP.
以下、本発明を実施例に基づきより詳細に説明する。 Hereinafter, the present invention will be described in more detail based on examples.
純度99.98％のモリブデンのインゴットと、純度99.99
99％のシリコンインゴットとを、MoSi2.5（モリブデン5
7.2％、シリコン42.8％）となるように配合しプラズマ
アーク溶解炉にて溶解した。得られた合金を振動式粉砕
機にて粉砕し、得られた粉末100重量部に対して6.4重量
部のシリコン粉末（上記シリコンインゴットを同様に粉
砕したもの）を添加して焼結用原料粉とした。99.98% pure molybdenum ingot and 99.99% pure
99% silicon ingot and MoSi 2.5 (molybdenum 5
7.2%, silicon 42.8%) and melted in a plasma arc melting furnace. The obtained alloy was crushed with a vibration crusher, and 6.4 parts by weight of silicon powder (the above silicon ingot was similarly crushed) was added to 100 parts by weight of the obtained powder, and raw material powder for sintering was added. And
次にこの粉末を用いて第１表に示したと同じ条件で軟
鋼製の内面に厚み0.2mmにBN粉末を塗布した缶BN粉末塗
布した内側に厚み0.2mmのMo箔を内張りした缶およびBN
粉末を塗布しない缶とを用いてHIP成形した。BN粉末を
塗布しない缶材のFeと原料粉中のSiが共晶反応して缶壁
が溶融し形をとどめないほど変形し同時に成形体にクラ
ックが発生したがBN粉末を塗布した缶はBN膜により缶材
のFeと原料粉中のSiが隔てられているためにFeとSiのBN
粉のはくりした局部的な反応しか起らず、原料粉は所望
形状に焼結されクラックの発生はなかった。BN粉末を塗
布しさらにMo箔を内張りした缶では全く成形体と缶材の
間に反応は起きなかった。第３表は各缶材を用いたとき
のターゲットへの缶材・Feの侵入を示したものである。Using this powder, under the same conditions as shown in Table 1, mild steel inner surface coated with 0.2 mm thick BN powder can BN powder coated inside 0.2 mm thick Mo foil lined can and BN
HIP molding was performed using a can to which the powder was not applied. The eutectic reaction between Fe in the can material without applying BN powder and Si in the raw material powder melted the can wall and deformed it so that it could not keep its shape, and at the same time cracked the molded body. Since the film separates Fe in the can material from Si in the raw material powder, BN of Fe and Si
Only the localized reaction of the powder was separated, and the raw material powder was sintered into a desired shape and no crack was generated. In the can coated with BN powder and lined with Mo foil, no reaction occurred between the molded body and the can material. Table 3 shows the penetration of can material and Fe into the target when each can material was used.
〔発明の効果〕 以上の通り本発明によれば、MOS型LSIのゲート電極膜
を形成するに好適なモリブデンシリサイド合金からなる
ターゲットが提供される。このターゲットは高強度であ
り、取扱いが容易である。 [Effects of the Invention] As described above, according to the present invention, a target made of a molybdenum silicide alloy suitable for forming a gate electrode film of a MOS type LSI is provided. This target has high strength and is easy to handle.
また、本発明によれば、モリブデンシリサイド以外の
高融点金属シリサイドターゲットを容易に製造すること
ができる。Further, according to the present invention, a refractory metal silicide target other than molybdenum silicide can be easily manufactured.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ０４Ｂ 35/645 ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Internal reference number FI technical display location C04B 35/645
Claims (1)
圧プレス焼結するに際し、内面にBN粉末を塗布した圧密
封入缶を用いて、原料粉末と圧密封入缶との間にBN粉末
を介在させ、かつ前記BNを塗布した圧密封入缶の内面を
さらに成形体と反応し難い金属箔体で内張りした封入缶
を用いることにより、成形体と圧密封入缶との熱膨張差
によるクラックの発生を低減したことを特徴とする熱間
静水圧プレスによるスパッタリング装置用ターゲットの
製造方法。1. When a raw powder is sealed in a pressure-sealed can and hot isostatically pressed and sintered, a BN powder is applied to the inner surface of the can to form a BN between the raw powder and the pressure-sealed can. Cracks due to the difference in thermal expansion between the molded body and the pressure-sealed canister are used by using an enclosed can in which a powder is interposed and the inner surface of the BN-coated pressure-sealed canister is lined with a metal foil that does not easily react with the molded body. A method for manufacturing a target for a sputtering apparatus by a hot isostatic press, which is characterized by reducing the occurrence of
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60117547A JPH0829435B2 (en) | 1985-05-30 | 1985-05-30 | Method for manufacturing target for sputtering device by hot isostatic pressing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60117547A JPH0829435B2 (en) | 1985-05-30 | 1985-05-30 | Method for manufacturing target for sputtering device by hot isostatic pressing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61276798A JPS61276798A (en) | 1986-12-06 |
| JPH0829435B2 true JPH0829435B2 (en) | 1996-03-27 |
Family
ID=14714505
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60117547A Expired - Fee Related JPH0829435B2 (en) | 1985-05-30 | 1985-05-30 | Method for manufacturing target for sputtering device by hot isostatic pressing |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0829435B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010106351A (en) * | 2008-10-31 | 2010-05-13 | Kuroki Kogyosho:Kk | Treatment method for article including container by hip process |
| CN104057083B (en) | 2013-03-22 | 2016-02-24 | 通用电气公司 | For the manufacture of the method for part taking high melting point metal materials as base material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1557744A (en) * | 1976-06-01 | 1979-12-12 | Special Metals Corp | Process and apparatus for producing aticles of complex shape |
| JPS56141998A (en) * | 1980-04-03 | 1981-11-05 | Ngk Spark Plug Co Ltd | Mold for hot press |
-
1985
- 1985-05-30 JP JP60117547A patent/JPH0829435B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61276798A (en) | 1986-12-06 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |