JP3049553B1 - Passivation treatment method in corrosive gas transfer system - Google Patents
Passivation treatment method in corrosive gas transfer systemInfo
- Publication number
- JP3049553B1 JP3049553B1 JP10368763A JP36876398A JP3049553B1 JP 3049553 B1 JP3049553 B1 JP 3049553B1 JP 10368763 A JP10368763 A JP 10368763A JP 36876398 A JP36876398 A JP 36876398A JP 3049553 B1 JP3049553 B1 JP 3049553B1
- Authority
- JP
- Japan
- Prior art keywords
- gas
- corrosive gas
- passivation film
- passivation treatment
- transfer system
- 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 - Lifetime
Links
Landscapes
- Cleaning Or Drying Semiconductors (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
【要約】
【課題】 半導体製造過程でクリーニングガスとして使
用されるフッ化水素等の腐食性ガス供給路での接ガス面
での腐食の進行を抑制する方法を提供する。
【解決手段】 腐食性ガスを流通させるガス移送経路で
の接ガス面にオゾンガスを作用させて酸化不動態膜を形
成し、酸化不動態膜にフッ素系ガスを作用させてフッ化
不動態膜を形成するようにした。The present invention provides a method for suppressing the progress of corrosion on a gas contact surface in a corrosive gas supply path such as hydrogen fluoride used as a cleaning gas in a semiconductor manufacturing process. SOLUTION: An oxidation passivation film is formed by applying an ozone gas to a gas contact surface in a gas transfer path for flowing a corrosive gas, and a fluorine-based gas is caused to act on the oxidation passivation film to form a fluoride passivation film. It was formed.
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、半導体製造工程等
で使用する半導体ガスを流通させるガス移送系での不動
態化処理方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a passivation treatment method in a gas transfer system for circulating a semiconductor gas used in a semiconductor manufacturing process or the like.
【０００２】[0002]
【従来の技術】従来、半導体製造工程で使用する半導体
ガスの移送系では、配管や機器類に酸化膜を形成して不
動態化処理した安定した表面をもつステンレス鋼やアル
ミニウム合金を使用して、防錆・純度維持等を行うよう
にしている。しかし、このような安定した表面をもつス
テンレス鋼やアルミニウム合金でも、フッ化水素等の腐
食性ガスが流通すると、ステンレス鋼やアルミニウム合
金も腐食することがあった。2. Description of the Related Art Conventionally, in a semiconductor gas transfer system used in a semiconductor manufacturing process, a stainless steel or aluminum alloy having a stable surface which has been subjected to a passivation treatment by forming an oxide film on piping or equipment has been used. , Rust prevention, purity maintenance, etc. However, even with stainless steel or aluminum alloy having such a stable surface, when a corrosive gas such as hydrogen fluoride flows, the stainless steel or aluminum alloy sometimes corrodes.
【０００３】そこで、近年、フッ素系のガスが流れるス
テンレス鋼製の配管路や構成機器における接ガス面をフ
ッ素系ガスで処理して、その表面にフッ化不動態膜を形
成するようにしたものも提案されている(特開平９−２
４６６７２号)。Therefore, in recent years, a gas passage surface of a stainless steel pipe or a component device through which a fluorine-based gas flows is treated with a fluorine-based gas to form a fluorinated passivation film on the surface. (Japanese Patent Laid-Open No. 9-2)
No. 46672).
【０００４】[0004]
【発明が解決しようとする課題】ステンレス鋼で形成し
た配管路の接ガス面にフッ化不動態膜を形成した場合、
接ガス面に形成された金属のフッ化物は、一種の腐食生
成物であり、パーティクルとして剥離したり、純水に浸
漬した際に純水への溶出金属量が増大したりすることが
判明した。When a fluoride passivation film is formed on the gas contact surface of a pipe made of stainless steel,
The metal fluoride formed on the gas contact surface is a kind of corrosion product, and it was found that the metal fluoride peeled off as particles or increased the amount of metal eluted into pure water when immersed in pure water. .
【０００５】本発明は、このような点に着目し、半導体
製造過程でクリーニングガスとして使用されるフッ化水
素等の腐食性ガス供給路での接ガス面での腐食の進行を
抑制する方法を提供することを目的とする。The present invention focuses on such a point, and proposes a method of suppressing the progress of corrosion on a gas contact surface in a corrosive gas supply path such as hydrogen fluoride used as a cleaning gas in a semiconductor manufacturing process. The purpose is to provide.
【０００６】[0006]
【課題を解決するための手段】上述の目的を達成するた
めに本発明は半導体製造過程でクリーニングガスとして
使用されるフッ化水素等の腐食性を有するガスの流通経
路での接ガス面を、５０ vol％以上の高濃度オゾンガス
を使用した酸化膜を形成する不動態化処理をした後、フ
ッ素系ガスでフッ化膜を形成する不動態化処理を施した
ことを特徴としている。SUMMARY OF THE INVENTION In order to achieve the above-mentioned object, the present invention provides a gas contacting surface in a flow path of a corrosive gas such as hydrogen fluoride used as a cleaning gas in a semiconductor manufacturing process. A passivation process for forming an oxide film using a high-concentration ozone gas of 50 vol% or more is performed, and then a passivation process for forming a fluoride film with a fluorine-based gas is performed.
【０００７】[0007]
【発明の作用】本発明では、５０ vol％以上の高濃度オ
ゾンによる不動態化処理をした後に、フッ素系ガスによ
る不動態化処理を施しているので、接ガス面にＭ(金属)
−Ｏ(酸素)−Ｆ(フッ素)の結合組織が生じ、しっかりし
た組織となって、腐食性ガス供給路の接ガス面での腐食
の進行を抑制することができることになる。According to the present invention, the passivation treatment with fluorine-based gas is performed after the passivation treatment with high-concentration ozone of 50 vol% or more.
A -O (oxygen) -F (fluorine) bond structure is generated, and a firm structure is formed, so that the progress of corrosion on the gas contact surface of the corrosive gas supply path can be suppressed.
【０００８】[0008]
【発明の実施の形態】半導体を製造する過程で、エッチ
ング用やクリーニング用のガスとして使用するフッ化水
素(HF)等の腐食性ガスの供給路を構成するステンレス電
解研磨管の内面にオゾンガスを作用させて、このステン
レス電解研磨管の内面に酸化不動態膜を形成し、この酸
化不動態膜で覆われているステンレス電解研磨管の内面
にフッ素ガスを作用させて、酸化不動態膜の上にフッ化
不動態膜を形成させる。DESCRIPTION OF THE PREFERRED EMBODIMENTS In the process of manufacturing a semiconductor, ozone gas is supplied to the inner surface of a stainless steel electropolishing tube constituting a supply path of a corrosive gas such as hydrogen fluoride (HF) used as an etching or cleaning gas. To form an oxidation passivation film on the inner surface of the stainless steel electropolishing tube, and to cause fluorine gas to act on the inner surface of the stainless steel electropolishing tube covered with the oxidation passivation film, thereby forming a film on the oxidation passivation film. To form a fluoride passivation film.
【０００９】ちなみに、オゾンによる酸化膜による不動
態化処理は、酸素でバランスさせた濃度５５vol ％のオ
ゾンガスを室温・大気圧で７２時間作用させることによ
り行い、フッ素ガスによるフッ化膜による不動態化処理
は、ヘリウムでバランスさせた濃度１５vol ％のフッ素
ガスを６０℃、圧力３.５kg/cm2・Ｇで１２０時間作用
させることにより行ったものである。Incidentally, the passivation treatment with an oxide film using ozone is performed by applying ozone gas having a concentration of 55 vol%, which is balanced with oxygen, at room temperature and atmospheric pressure for 72 hours. The treatment was carried out by applying a fluorine gas having a concentration of 15 vol% balanced with helium at 60 ° C. and a pressure of 3.5 kg / cm 2 · G for 120 hours.
【００１０】上述のように処理した電解研磨管に、圧力
０.５kg/cm2・Ｇ、温度４０℃の窒素でバランスさせた
濃度１５vol ％のフッ化水素に３日間作用させ、純水に
浸漬し、純水中に解け出した金属の溶出量を腐食量とし
た場合の溶出金属量を図１に示す。なお、フッ素だけで
処理した電解研磨管の溶出金属量及び、オゾンだけで処
理した電解研磨管の溶出金属量、無処理の電解研磨管の
溶出金属量の状態を図１に示す。The electropolished tube treated as described above is allowed to act on hydrogen fluoride at a concentration of 0.5 vol / cm 2 · G at a temperature of 40 ° C. and a concentration of 15 vol. FIG. 1 shows the amount of eluted metal when the amount of metal dissolved in pure water is taken as the amount of corrosion. FIG. 1 shows the state of the amount of eluted metal in the electrolytic polishing tube treated only with fluorine, the amount of eluted metal in the electrolytic polishing tube treated only with ozone, and the amount of eluted metal in the untreated electrolytic polishing tube.
【００１１】さらに、フッ化水素を流通させた場合、図
２に示すように、無処理の電解研磨管の場合には、経過
日数とともに溶出金属量が増大するのに対し、オゾンに
よる不動態化処理とフッ素による不動態化処理とを併せ
て行った場合には、その溶出金属量はほぼ２日目から横
ばいになる。Further, when hydrogen fluoride is circulated, as shown in FIG. 2, in the case of an untreated electrolytic polishing tube, the amount of eluted metal increases with the lapse of days. When the treatment and the passivation treatment with fluorine are performed in combination, the amount of the eluted metal becomes almost level from the second day.
【００１２】上述の実施形態では、酸化膜形成に５５vo
l％のオゾンガスを使用したが、腐食防止のために酸化
膜を形成する場合のオゾン濃度は５０vol％以上の高濃
度のものが望ましい。また、上述の実施形態では、フッ
化膜形成にフッ素を使用しているが、三フッ化塩素でフ
ッ化処理してもよい。In the above embodiment, the formation of the oxide film
Although 1% ozone gas was used, the ozone concentration when forming an oxide film to prevent corrosion is desirably as high as 50 vol% or more. In the above-described embodiment, fluorine is used for forming the fluoride film. However, the fluoride treatment may be performed with chlorine trifluoride.
【００１３】[0013]
【発明の効果】本発明では、５０ vol％以上の高濃度オ
ゾンによる不動態化処理をした後に、フッ素系ガスによ
る不動態化処理を施しているので、接ガス面にＭ−Ｏ−
Ｆの結合組織が生じ、しっかりした組織となって、腐食
性ガス供給路の接ガス面での腐食の進行を抑制すること
ができる。According to the present invention, the passivation treatment with a fluorine-based gas is performed after the passivation treatment with high-concentration ozone of 50 vol% or more, so that the MO-
The connective structure of F is generated, and the structure becomes firm, so that the progress of corrosion on the gas contact surface of the corrosive gas supply path can be suppressed.
【図１】処理条件を変えた状態での金属腐食量を示す図
である。FIG. 1 is a diagram showing the amount of metal corrosion in a state where processing conditions are changed.
【図２】腐食量の経過日数での変化を示す図である。FIG. 2 is a diagram showing a change in the amount of corrosion with the number of elapsed days.
Claims (2)
の接ガス面に５０ vol％以上の高濃度オゾンガスを作用
させて酸化不動態膜を形成し、酸化不動態膜にフッ素系
ガスを作用させてフッ化不動態膜を形成するようにした
腐食性ガス移送系での不動態化処理方法。1. An oxidation passivation film is formed by applying a high-concentration ozone gas of 50 vol% or more to a gas contact surface in a gas transfer path for flowing a corrosive gas, and a fluorine-based gas acts on the oxidation passivation film. A passivation treatment method in a corrosive gas transfer system in which a fluorinated passivation film is formed.
に記載の腐食性ガス移送系での不動態化処理方法。2. The method according to claim 1, wherein the corrosive gas is hydrogen fluoride.
3. The passivation treatment method in a corrosive gas transfer system according to item 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10368763A JP3049553B1 (en) | 1998-12-25 | 1998-12-25 | Passivation treatment method in corrosive gas transfer system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10368763A JP3049553B1 (en) | 1998-12-25 | 1998-12-25 | Passivation treatment method in corrosive gas transfer system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP3049553B1 true JP3049553B1 (en) | 2000-06-05 |
| JP2000192222A JP2000192222A (en) | 2000-07-11 |
Family
ID=18492691
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10368763A Expired - Lifetime JP3049553B1 (en) | 1998-12-25 | 1998-12-25 | Passivation treatment method in corrosive gas transfer system |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3049553B1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4912163B2 (en) * | 2007-01-12 | 2012-04-11 | ステラケミファ株式会社 | Carbon steel or special steel formed with a fluorinated passive film and method for forming the same |
| JP5317321B2 (en) * | 2008-02-21 | 2013-10-16 | 岩谷産業株式会社 | Metal material, storage container using the same, gas piping, apparatus, manufacturing method thereof, and ClF3 storage method |
| JP2014109059A (en) * | 2012-12-03 | 2014-06-12 | Iwatani Internatl Corp | Hydrogen embrittlement-resistant metal material, and surface treatment method of hydrogen embrittlement-resistant metal material |
-
1998
- 1998-12-25 JP JP10368763A patent/JP3049553B1/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP2000192222A (en) | 2000-07-11 |
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