JPH0369989B2 - - Google Patents
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- Publication number
- JPH0369989B2 JPH0369989B2 JP14800488A JP14800488A JPH0369989B2 JP H0369989 B2 JPH0369989 B2 JP H0369989B2 JP 14800488 A JP14800488 A JP 14800488A JP 14800488 A JP14800488 A JP 14800488A JP H0369989 B2 JPH0369989 B2 JP H0369989B2
- Authority
- JP
- Japan
- Prior art keywords
- sputtering
- copper foil
- electrolytic copper
- foil
- electrolytic
- 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
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- Physical Vapour Deposition (AREA)
Description
〔発明の目的〕
(産業上の利用分野)
本発明は、汚染防止材を配設したスパツタリン
グ装置に関するものである。
(発明の背景)
従来より、集積回路の電極や拡散バリヤ等用の
薄膜、磁気記録媒体用磁性薄膜、液晶表示装置の
ITO透明導電膜などの多くの薄膜形成にスパツタ
リング技術が使用されている。スパツタリング
は、陽極と陰極との間に高電圧を印加して放電を
生じさせ、陰極に配置されたターゲツトからその
構成物質をイオン衝撃によつて叩出し、これを対
向する基板上に堆積させることにより薄膜を形成
する技術である。
現在、このようなスパツタリングプロセスは大
量生産技術として確立されているが、同様な成膜
プロセスであるCVDプロセス形成された膜上に
一般にパーテイクルと言われている粗大粒子が堆
積するという問題がクローズアツプされている。
このパーテイクルとは、ターゲツトをスパツタ
リングした場合、クラスター化した微粒子が基板
上に堆積したものを言うものであるが、この微粒
子の直径が数μm程度までに大きくなるものが多
いので、これが基板上に堆積すると、例えばLSI
の場合は配線の短絡あるいは逆に断線を引き起こ
すなどの問題を生じ不良率増大の原因となる。そ
してこれらのパーテイクルは、ターゲツト自体に
起因するものや、スパツタリング装置に起因する
もの等の種々の要因があつて、その原因究明と低
減のための各種工夫がなされているのが現状であ
る。
(従来技術とその問題点)
スパツタリング装置に起因するパーテイクルと
しては、基板周辺やチヤンバー内壁(炉壁)やシ
ヤツター、シールド板等に付着したスパツタリン
グ薄膜が剥離し、それが飛散して基板に堆積して
汚染源となることも1つの大きな要因である。こ
のような付着物質の再剥離に起因するパーテイク
ルを防止するため、スパツタリング装置の内壁を
常に清浄しておく必要がある。
このような内壁を常にクリーンに保つのは実際
には非常に難しく、完全にクリーンにするには大
変な時間を必要とし、また内壁の部位によつては
クリーン化が実際にはできないところもある。そ
のために考えだされたのが、Al箔や電解Fe箔の
デイスポーザブル(使い捨て)箔による汚染防止
材である。前記の箔をあらかじめ内壁にはりつけ
ておき、スパツタリング終了後これを除去すれ
ば、一応内壁をクリーンな状態に保つことが可能
と考えられた。
しかし、これらの使い捨て箔には致命的な欠陥
が見出された。それは、設置された箔に堆積した
スパツタリング飛散物質膜が剥離し易く、基板上
への堆積膜上でのパーテイクル発生が依然として
起つたからである。この使い捨て箔(フオイル)
を用いた場合の剥離現象は飛散物質の膜厚が厚い
ほど発生が顕著となり、また生成物がシリサイド
やITO(インジウム−錫酸化物)のようなセラミ
ツク系の場合ほど生じ易いことが分つた。この剥
離を防止するためには頻繁に箔を交換しなければ
ならずスパツタリングの操業性が著しけ悪化し
た。このようなことから画期的な内壁をおおう箔
用汚染防止材の出現が熱望されていた。
(問題点を解決するための手段)
上記の問題を解決するためスパツタリングチヤ
ンバー内の汚染を防止する材料としての箔を種々
検討した結果、トリート電解銅箔が汚染防止材と
して最適である、との知見を得た。すなわち、本
願発明は、(イ)電解銅箔のマツト面に銅めつきによ
る銅又は及び銅酸化物微細粒子薄層を形成した電
解銅箔からなるスパツタリングチヤンバー内汚染
防止材を内部に配設したスパツタリング装置及び
(ロ)電解銅箔のマツト面側の表面粗さRzが5μm〜
10μmである前記(イ)のスパツタリング装置及び(ハ)
微細粒子薄層形成面をスパツタリング飛散粒子捕
獲面とした前記(イ)及び(ロ)のスパツタリング装置並
びに(ニ)使い捨て用電解銅箔である前記(イ)、(ロ)、(
ハ)
のスパツタリング装置を提供するものである。
(発明の具体的説明)
本発明の電解銅箔を使用することによりスパツ
タリング装置内(炉)壁の汚染がなく、かつこの
内壁からの飛散生成物の剥離に起因するパーテイ
クル発生が著しく減少し良好なスパツタリングを
実施することが可能となつた。
電解銅箔のマツト面に形成する微細粒子薄層は
アメリカ特許第3220897号あるいはアメリカ特許
第3293109号などの電気めつき処理によつて行な
うことができる。
この処理自体は公知であるが、本願発明におい
ては、従来のAl箔や鉄箔でしか考えられなかつ
た箔にかえて本願発明の汚染防止材を用いること
により、著大な効果をもたらすことが可能となつ
た。
微細粒子薄層は電解銅箔(生箔)のマツト面に
形成されるが、これを形成する電気めつきの条件
の一例を下記に示す。
水溶銅硫酸塩めつき浴
CuSO4・5H2O,g/(as Cu) …23
NaCl,p.p.m.(as Cl) …32
H2SO4,g/ …70
にかわ,g/ …0.75
純水 …Ba.
めつき条件
電流密度 60〜100a.s.f
時 間 10〜60秒
浴 温 70〜80〓
電解銅箔(生箔)のマツト面(無光沢面)は、
該箔の製造工程におけるロール等の接触面(光沢
面)の反対側の面で、電子顕微鏡で観察すると前
記マツト面は無数のノブ状(塊状と突出部)粗面
を呈している。
さらにこの面に前記微細粒子薄層を形成すると
銅又は及び銅酸化物の微細粒(ノジユラー)がラ
ンダムに上記電解銅箔(生箔)のノブ状粗面に析
出しているのが同様に電子顕微鏡により観察され
る。
(参考資料 電子技術,1985年6月増刊号 97P.
〜105P.)
上記のような条件で形成した銅箔はさらに特公
昭54−6701号に示すような耐熱特性をもたせるた
めの黄銅又は亜鉛のバリヤー層を形成したり、さ
らにこの上に銅箔運搬又は保管中の酸化等を防止
するための防錆処理を施すこともできる。
本願発明は、これらの工程によつて製造された
電解銅箔を全て包含するものである。電解銅箔の
表面粗さはRz5.0〜10.0μmの範囲とするのが望ま
しい。この粗さによる突起が存在するために、ア
ンカー効果によつて飛散物質が析出して形成され
た生成物との密着性が改善され、剥離現象が生じ
なくなる。
本願発明のスパツタリング装置における汚染防
止材として使用される材料は、厚さ10μm〜100μ
mが適し、10〜70μmが好適である。薄すぎると
炉壁へセツトする時にしわが生じ易く、しわ部が
できると剥離の原因となるので避ける必要があ
る。厚いとしわは生じにくくなるが、炉壁へのセ
ツト時の操作性が悪くなり、また価格的にも不利
である。
上記のように電解銅箔はにかわ質の電解浴中で
製造されるので、箔表面にはにわが付着している
ことがある。したがつてにわかによるスパツタリ
ング装置内の汚染を防止するために、あらかじめ
アセトンやアルコール等の有機溶媒または熱した
超純水を用いて超音波洗浄をしてから使用するこ
とが望ましい。なお、洗浄後の乾燥を目的として
真空加熱をしても良い。真空加熱をする場合は、
表面突起が成長現象によつて変化しないよう最高
400℃までにおさえる必要がある。
次に実施例にもとづいて本願発明を説明する。
実施例 1
透明導電膜用ITOターゲツトを用いて第1表に
示す各種の箔をスパツタリング装置チヤンバー内
壁に取りつけスパツタリングを実施した。
390w・Hrのスパツタリング終了後に箔を取り出
した。前記の箔にも飛散したITO膜が形成されて
いた。この膜をスコツチテープによるピールテス
トを行つたところ、本願発明の電解銅箔と、電解
銅箔のみがピールテストの結果、ITO膜の剥離が
起こらなかつた。試験材料と結果を第1表に示
す。
[Object of the Invention] (Industrial Application Field) The present invention relates to a sputtering device provided with a pollution prevention material. (Background of the Invention) Conventionally, thin films for electrodes and diffusion barriers in integrated circuits, magnetic thin films for magnetic recording media, and thin films for liquid crystal display devices have been used.
Sputtering technology is used to form many thin films such as ITO transparent conductive films. Sputtering is a process in which a high voltage is applied between an anode and a cathode to generate a discharge, and constituent substances are ejected from a target placed on the cathode by ion bombardment, and then deposited on the opposing substrate. This is a technology that forms thin films using Currently, this type of sputtering process has been established as a mass production technology, but there is a problem that coarse particles, generally called particles, accumulate on the film formed by the CVD process, which is a similar film formation process. Closed up. Particles are clustered fine particles that are deposited on a substrate when a target is sputtered, and since these fine particles often have a diameter of several micrometers, they are deposited on the substrate. When deposited, e.g. LSI
In this case, problems such as wiring short-circuiting or, conversely, wire breakage may occur, leading to an increase in the defective rate. These particles are caused by various factors, such as those caused by the target itself and those caused by the sputtering device, and various efforts are currently being made to investigate the causes and reduce them. (Prior art and its problems) Particles caused by sputtering equipment include peeling of the sputtering thin film attached to the periphery of the substrate, the inner wall of the chamber (furnace wall), the shutter, the shield plate, etc., which scatters and accumulates on the substrate. Another major factor is that it becomes a source of pollution. In order to prevent particles caused by such re-peeling of the adhered substances, it is necessary to constantly clean the inner wall of the sputtering apparatus. It is actually very difficult to keep these inner walls clean at all times, it takes a lot of time to completely clean them, and there are some parts of the inner walls that cannot be cleaned. . To this end, we devised a pollution prevention material using disposable foils such as Al foil and electrolytic Fe foil. It was thought that it would be possible to keep the inner wall clean by attaching the foil to the inner wall in advance and removing it after sputtering. However, a fatal flaw was discovered in these disposable foils. This is because the sputtering scattered material film deposited on the installed foil was easily peeled off, and particles still occurred on the deposited film on the substrate. This disposable foil
It has been found that the peeling phenomenon occurs more prominently when the film of the scattered substance is thicker, and is more likely to occur when the product is ceramic-based such as silicide or ITO (indium-tin oxide). In order to prevent this peeling, the foil had to be replaced frequently, and the operability of sputtering deteriorated significantly. For this reason, there has been a desire for the emergence of an innovative anti-fouling material for covering inner walls. (Means for solving the problem) In order to solve the above problem, we investigated various foils as a material to prevent contamination inside the sputtering chamber, and as a result, we found that Treat electrolytic copper foil is the most suitable material for preventing contamination. , we obtained the following knowledge. That is, the present invention provides (a) a sputtering chamber contamination prevention material made of an electrolytic copper foil on which a thin layer of copper or copper oxide fine particles is formed by copper plating on the matte surface of the electrolytic copper foil; The installed sputtering equipment and
(b) The surface roughness Rz of the matte side of the electrolytic copper foil is 5 μm or more
The sputtering device of (a) and (c) above, which has a thickness of 10 μm.
The sputtering apparatus of (a) and (b) above, in which the fine particle thin layer forming surface is the sputtering scattering particle capture surface, and (d) the above (a), (b), (d) is a disposable electrolytic copper foil
c)
The present invention provides a sputtering device. (Detailed Description of the Invention) By using the electrolytic copper foil of the present invention, there is no contamination of the walls in the sputtering equipment (furnace), and the generation of particles caused by the peeling of scattered products from the inner walls is significantly reduced, which is good. It has become possible to carry out sputtering. The thin layer of fine particles formed on the matte surface of the electrolytic copper foil can be formed by an electroplating process such as US Pat. No. 3,220,897 or US Pat. No. 3,293,109. Although this treatment itself is well known, in the present invention, by using the pollution prevention material of the present invention in place of conventional foils that could only be used with Al foil or iron foil, it is possible to bring about significant effects. It became possible. A fine particle thin layer is formed on the matte surface of electrolytic copper foil (raw foil), and an example of the electroplating conditions for forming this is shown below. Aqueous copper sulfate plating bath CuSO 4・5H 2 O, g/(as Cu)…23 NaCl, ppm (as Cl)…32 H 2 SO 4 , g/…70 Glue, g/…0.75 Pure water…Ba .. Plating conditions Current density: 60 to 100 a.sf Time: 10 to 60 seconds Bath temperature: 70 to 80〓 The matte side (matte side) of electrolytic copper foil (raw foil)
When observed with an electron microscope on the surface opposite to the contact surface (glossy surface) of a roll or the like in the manufacturing process of the foil, the matte surface exhibits a rough surface with numerous knob-like shapes (clumps and protrusions). Furthermore, when a thin layer of fine particles is formed on this surface, fine grains (nodulars) of copper or copper oxide are randomly deposited on the knob-shaped rough surface of the electrolytic copper foil (raw foil), which is similar to the electrolytic copper foil. Observed with a microscope. (Reference material: Electronic Technology, June 1985 Special Issue, 97 pages.
~105P.) The copper foil formed under the above conditions is further coated with a barrier layer of brass or zinc to provide heat resistance properties as shown in Japanese Patent Publication No. 54-6701, and further coated with copper foil. Alternatively, antirust treatment can be applied to prevent oxidation during storage. The present invention includes all electrolytic copper foils manufactured by these steps. The surface roughness of the electrolytic copper foil is preferably in the range of Rz5.0 to 10.0 μm. Due to the presence of the protrusions due to this roughness, the adhesion with the product formed by the precipitation of scattered substances is improved due to the anchor effect, and the peeling phenomenon does not occur. The material used as the contamination prevention material in the sputtering device of the present invention has a thickness of 10 μm to 100 μm.
m is suitable, and 10 to 70 μm is preferable. If it is too thin, wrinkles will easily form when it is set on the furnace wall, and wrinkles will cause peeling, so it must be avoided. If it is thick, wrinkles are less likely to occur, but it becomes difficult to operate when setting it on the furnace wall, and it is also disadvantageous in terms of cost. As mentioned above, since electrolytic copper foil is manufactured in a glue electrolytic bath, glue may adhere to the surface of the foil. Therefore, in order to prevent contamination of the inside of the sputtering apparatus due to splashes, it is preferable to perform ultrasonic cleaning using an organic solvent such as acetone or alcohol or heated ultrapure water before use. Note that vacuum heating may be performed for the purpose of drying after washing. When performing vacuum heating,
It is best to ensure that the surface protrusions do not change due to growth phenomena.
It is necessary to keep the temperature below 400℃. Next, the present invention will be explained based on examples. Example 1 Using an ITO target for transparent conductive films, various foils shown in Table 1 were attached to the inner wall of the chamber of a sputtering apparatus, and sputtering was performed.
After completing sputtering at 390W/Hr, the foil was removed. A scattered ITO film was also formed on the foil. When this film was subjected to a peel test using Scotch tape, only the electrolytic copper foil of the present invention and the electrolytic copper foil did not cause peeling of the ITO film. The test materials and results are shown in Table 1.
【表】
実施例 2
シリサイドターゲツトを用いて電解鉄箔と、本
願発明の電解銅箔とを同時にスパツタリング装置
内壁にセツトしてスパツタリングを実施した。ス
パツタリング終了後には、どちらの箔にも厚さ約
1μmのシリサイド膜が形成されていた。その試
料をスコツチテープ及び粘着力の強い両面テープ
(No.500)を用いてピールテストをしたところ、本
願発明の電解銅箔だけが、いずれのテストにおい
ても剥離しなかつた。その結果を第2表に示す。[Table] Example 2 Using a silicide target, an electrolytic iron foil and an electrolytic copper foil of the present invention were simultaneously set on the inner wall of a sputtering apparatus and sputtering was carried out. After sputtering, both foils should have a thickness of approx.
A 1 μm silicide film was formed. When the sample was subjected to a peel test using Scotch tape and a strong adhesive double-sided tape (No. 500), only the electrolytic copper foil of the present invention did not peel off in any of the tests. The results are shown in Table 2.
【表】
実施例 3
ITOターゲツトをスパツタリング装置内にセツ
トし、基板位置に電解銅箔(微細粒子層を形成し
た本願発明の汚染防止材と同形成しないものとの
両方)と電解鉄箔、純Al箔の4種を同時にセツ
トし、ITOのスパツタリングを実施した。
100w・Hr毎にスパツタリングを中断し、試料
の状況を確認した。本願発明の微細粒子層を形成
した電解銅箔は800w・Hrまでスパツタリングを
実施しても剥離は全く起こつていないが、他の3
種の試料は400w・Hrスパツタリングを継続する
と剥離が生じてきた。また本願発明の箔のみ、繰
返し曲げによる剥離試験でも剥離は全く認められ
なかつた。
(発明の効果)
以上の実施例からも明らかなように本願発明の
汚染防止材を内部に配設したスパツタリング装置
は、従来のAl箔や鉄箔などに比較してスパツタ
リング薄膜の汚染物質となるパーテイクルの発生
を著しく抑制することができる。
また、電解銅箔は熱伝導性に富み、帯電するこ
ともないので、スパツタリングチヤンバー内に設
置する汚染防止材として最適である。[Table] Example 3 An ITO target was set in a sputtering device, and electrolytic copper foil (both the pollution prevention material of the present invention with and without a fine particle layer formed thereon), electrolytic iron foil, pure Four types of Al foil were set at the same time and ITO sputtering was performed. Sputtering was interrupted every 100W/Hr and the condition of the sample was checked. The electrolytic copper foil on which the fine particle layer of the present invention was formed did not peel off at all even after sputtering up to 800 W/Hr, but other 3
Seed samples began to peel when sputtering was continued at 400W/Hr. Moreover, only in the foil of the present invention, no peeling was observed in the peeling test by repeated bending. (Effects of the Invention) As is clear from the above examples, the sputtering device in which the contamination prevention material of the present invention is disposed inside is more contaminant of the sputtering thin film than conventional Al foils, iron foils, etc. The generation of particles can be significantly suppressed. In addition, electrolytic copper foil has high thermal conductivity and is not charged with electricity, so it is ideal as a pollution prevention material installed in a sputtering chamber.
Claims (1)
及び銅酸化物微細粒子薄層を形成した電解銅箔か
らなるスパツタリングチヤンバー内汚染防止材を
内部に配設したスパツタリング装置。 2 電解銅箔のマツト面側の表面粗さRzが5μm
〜10μmである特許請求の範囲第1項記載のスパ
ツタリング装置。 3 微細粒子薄層形成面をスパツタリング飛散粒
子捕獲面とした特許請求の範囲第1項乃至第2項
記載のスパツタリング装置。 4 使い捨て用電解銅箔である特許請求の範囲第
1項乃至第3項記載のスパツタリング装置。[Claims] 1. A sputtering chamber contamination prevention material made of an electrolytic copper foil with a thin layer of copper or copper oxide fine particles formed by copper plating on the matte surface of the electrolytic copper foil is disposed inside. sputtering equipment. 2 The surface roughness Rz of the matte side of the electrolytic copper foil is 5μm
The sputtering apparatus according to claim 1, which has a thickness of 10 μm. 3. The sputtering apparatus according to claims 1 and 2, wherein the fine particle thin layer forming surface is the sputtering scattering particle capturing surface. 4. The sputtering apparatus according to claims 1 to 3, which is a disposable electrolytic copper foil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14800488A JPH01316456A (en) | 1988-06-17 | 1988-06-17 | Sputtering device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14800488A JPH01316456A (en) | 1988-06-17 | 1988-06-17 | Sputtering device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01316456A JPH01316456A (en) | 1989-12-21 |
| JPH0369989B2 true JPH0369989B2 (en) | 1991-11-06 |
Family
ID=15442958
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14800488A Granted JPH01316456A (en) | 1988-06-17 | 1988-06-17 | Sputtering device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01316456A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03177561A (en) * | 1989-09-19 | 1991-08-01 | Nippon Mining Co Ltd | Thin-film forming device |
| JP3449459B2 (en) | 1997-06-02 | 2003-09-22 | 株式会社ジャパンエナジー | Method for manufacturing member for thin film forming apparatus and member for the apparatus |
| JP2005330566A (en) * | 2004-05-21 | 2005-12-02 | Sumitomo Bakelite Co Ltd | Vacuum film deposition method using deposition preventive film |
-
1988
- 1988-06-17 JP JP14800488A patent/JPH01316456A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01316456A (en) | 1989-12-21 |
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