JP3194875B2 - Stainless steel for hydrogen peroxide and method for producing the same - Google Patents
Stainless steel for hydrogen peroxide and method for producing the sameInfo
- Publication number
- JP3194875B2 JP3194875B2 JP30018096A JP30018096A JP3194875B2 JP 3194875 B2 JP3194875 B2 JP 3194875B2 JP 30018096 A JP30018096 A JP 30018096A JP 30018096 A JP30018096 A JP 30018096A JP 3194875 B2 JP3194875 B2 JP 3194875B2
- Authority
- JP
- Japan
- Prior art keywords
- stainless steel
- hydrogen peroxide
- oxide film
- producing
- metal ions
- 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
Landscapes
- ing And Chemical Polishing (AREA)
- Chemical Treatment Of Metals (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、金属イオンの溶出
を極端に嫌う半導体製造装置等の分野において使用され
る配管・機器等を構成するステンレス鋼及びその製造方
法に関し、詳しくは、過酸化水素に対する金属イオンの
溶出量が極めて少ないステンレス鋼及びその製造方法に
関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a stainless steel for piping and equipment used in the field of semiconductor manufacturing equipment and the like which extremely dislikes elution of metal ions and a method for manufacturing the same. The present invention relates to a stainless steel having a very small amount of metal ions eluted with respect to stainless steel and a method for producing the same.
【０００２】[0002]
【従来の技術および発明が解決しようとする課題】金属
イオンの溶出量が少ない材料としてチタン、タンタルや
樹脂類等が知られているが、前者材料は極めて高価であ
り、また、後者材料は耐熱性が充分でなく、パーティク
ルが出やすいという問題がある。2. Description of the Related Art Titanium, tantalum, resins, and the like are known as materials with a small amount of metal ions eluted, but the former is extremely expensive and the latter is heat-resistant. There is a problem that the properties are not sufficient and particles are easily generated.
【０００３】また、従来より、金属イオンの溶出を抑え
るために、ステンレス鋼の表面を研磨して平滑化する方
法が知られている。例えば、バフ研磨を施したステンレ
ス鋼は表面にスクラッチのある粒状の組織となるため、
Ｆｅ、Ｃｒ、Ｎｉ等の酸化物の不動態被膜は不均一に形
成され、Ｆｅイオン等の金属イオンの溶出量は多く、本
発明の対象とする分野に適用することはできない。[0003] In addition, there has been conventionally known a method of polishing and smoothing the surface of stainless steel in order to suppress elution of metal ions. For example, buffed stainless steel has a granular structure with scratches on the surface,
Passive films of oxides such as Fe, Cr and Ni are formed non-uniformly, and the amount of metal ions such as Fe ions eluted is large and cannot be applied to the field targeted by the present invention.
【０００４】さらに、電解研磨を施したステンレス鋼で
は、上記した粒状の組織は電気化学的な溶解で除去さ
れ、加工変質層を持たない平滑な健全組織が得られる
が、その表面に形成される自然酸化による不動態酸化被
膜は極めて薄く、この場合も金属イオンの溶出量は充分
に低くないので、本発明の対象とする分野に適用するこ
とはできない。Further, in stainless steel which has been subjected to electrolytic polishing, the above-mentioned granular structure is removed by electrochemical dissolution, and a smooth sound structure without a work-affected layer is obtained, but is formed on the surface thereof. The passive oxide film formed by natural oxidation is extremely thin. In this case, too, the elution amount of metal ions is not sufficiently low, so that it cannot be applied to the field targeted by the present invention.
【０００５】本発明は従来の技術の有するこのような問
題点に鑑みてなされたものであって、その目的は、過酸
化水素に対する金属イオンの溶出量が極めて少ないステ
ンレス鋼及びその製造方法を提供することにある。The present invention has been made in view of the above-mentioned problems of the prior art, and has as its object to provide a stainless steel in which the amount of metal ions eluted with respect to hydrogen peroxide is extremely small, and a method for producing the same. Is to do.
【０００６】[0006]
【課題を解決するための手段】上記目的を達成するため
に本発明は、電解研磨処理を施した表面上に１００〜２
００×１０-8ｃｍの厚みの鉄系酸化物を主とする金属酸
化物の被膜が形成されたステンレス鋼を配管・機器等の
構成材料として用いることにより、上記金属酸化物の被
膜がバリヤーとなって、過酸化水素への金属イオンの溶
出量は極めて少なくなる。In order to achieve the above-mentioned object, the present invention provides an electro-polishing surface having a thickness of 100 to 2 mm.
By using stainless steel on which a metal oxide film mainly composed of an iron-based oxide having a thickness of 00 × 10 −8 cm is formed as a constituent material for piping, equipment, etc., the metal oxide film serves as a barrier. As a result, the amount of metal ions eluted into hydrogen peroxide is extremely small.
【０００７】[0007]
【発明の実施の形態】すなわち、本発明は、電解研磨処
理を施した表面上に１００〜２００×１０-8ｃｍの厚み
の鉄系酸化物を主とする金属酸化物の被膜が形成された
過酸化水素用ステンレス鋼を第一の発明とし、ステンレ
ス鋼表面に電解研磨処理を施した後、酸化性雰囲気中で
加熱することにより、１００〜２００×１０-8ｃｍの厚
み鉄系酸化物を主とする金属酸化物の着色酸化被膜を表
面に形成することを特徴とする過酸化水素用ステンレス
鋼の製造方法を第二の発明とし、上記第二の発明におい
て、加熱条件が、４００〜５００℃で１〜３時間加熱す
るものであることを特徴とする過酸化水素用ステンレス
鋼の製造方法を第三の発明とする。DESCRIPTION OF THE PREFERRED EMBODIMENTS That is, according to the present invention, a metal oxide film mainly composed of an iron-based oxide having a thickness of 100 to 200.times.10.sup.- 8 cm is formed on a surface subjected to electrolytic polishing. The first invention is a stainless steel for hydrogen peroxide, and after subjecting the stainless steel surface to electrolytic polishing treatment and heating in an oxidizing atmosphere, an iron-based oxide having a thickness of 100 to 200 × 10 −8 cm is obtained. A second invention is a method for producing stainless steel for hydrogen peroxide, characterized by forming a colored oxide film of a main metal oxide on the surface, and in the second invention, the heating condition is 400 to 500. A third invention is a method for producing stainless steel for hydrogen peroxide, wherein the stainless steel is heated at 1 to 3 hours.
【０００８】電解研磨処理を施すことにより、ステンレ
ス鋼の表面の平滑性は向上するが、自然酸化による不動
態酸化被膜は薄く、金属イオンの溶出を抑えることはで
きない。Although the surface smoothness of stainless steel is improved by performing the electropolishing treatment, the passive oxide film formed by natural oxidation is thin, and the elution of metal ions cannot be suppressed.
【０００９】しかし、電解研磨後のステンレス鋼を酸化
性雰囲気中で一定温度で加熱することにより、図１に示
すように、表面に鉄系酸化物（ＦｅＯ、Ｆｅ3Ｏ4、Ｆｅ
2Ｏ3）を主とする金属酸化物の着色酸化被膜が形成さ
れ、着色酸化被膜と下層母材との界面ではＣｒ，Ｎｉ成
分が相対的に多くなる。この着色酸化被膜が過酸化水素
中への金属イオンの溶出を低減するものと考えられる。However, by heating the stainless steel after electropolishing at a constant temperature in an oxidizing atmosphere, as shown in FIG. 1, the surface of the stainless steel is made of iron-based oxide (FeO, Fe 3 O 4 , Fe
A colored oxide film of a metal oxide mainly composed of 2 O 3 ) is formed, and the Cr and Ni components are relatively increased at the interface between the colored oxide film and the lower base material. It is considered that this colored oxide film reduces the elution of metal ions into hydrogen peroxide.
【００１０】しかし、加熱温度が４００℃未満では、酸
化被膜の形成が不充分であり、５００℃より高温に加熱
すると、酸化被膜が過度に厚くなると同時に脆くなる。
同様に、加熱時間が１時間より短いと、酸化被膜の形成
が不充分であり、一方、３時間より長くなると、酸化被
膜が過厚となる。従って、加熱条件としては、４００〜
５００℃で１〜３時間加熱するのが好ましい。However, when the heating temperature is lower than 400 ° C., the formation of the oxide film is insufficient, and when the temperature is higher than 500 ° C., the oxide film becomes excessively thick and becomes brittle.
Similarly, if the heating time is shorter than 1 hour, formation of an oxide film is insufficient, while if it is longer than 3 hours, the oxide film becomes too thick. Therefore, the heating conditions are 400 to
It is preferable to heat at 500 ° C. for 1 to 3 hours.
【００１１】[0011]
【実施例】以下、実施例として、図２に示すように、Ｓ
ＵＳ３１６Ｌステンレス鋼製の厚み１．６５ｍｍ、外径
３４ｍｍの管体１にキャップ２を溶接で接合したもの
と、これとは別にＳＵＳ３１６Ｌステンレス鋼製の蓋３
とを、りん酸・硫酸系電解液により電解電流密度１０Ａ
／ｄｍ2 で８分間電解研磨して表面の加工変質層を１０
〜５０μｍ除去することで健全な母材表面を得、次い
で、抵抗率１８ＭΩ・ｃｍ以上の超純水により精密洗浄
を行ってから、酸化雰囲気で４５０℃×２時間の加熱処
理を行うことにより、厚みが１００〜２００×１０-8ｃ
ｍの鉄系酸化物の被膜（図１参照）が表面に形成された
本発明の試料を得た。[Embodiment] Hereinafter, as an embodiment, as shown in FIG.
US316L stainless steel tubular body 1 having a thickness of 1.65 mm and outer diameter of 34 mm with cap 2 welded thereto, and a separate SUS316L stainless steel lid 3
And an electrolytic current density of 10 A using a phosphoric acid / sulfuric acid type electrolytic solution.
/ Dm 2 for 8 minutes by electropolishing to make the surface damaged layer 10
By obtaining a sound base material surface by removing 〜50 μm, and then performing precision cleaning with ultrapure water having a resistivity of 18 MΩ · cm or more, and then performing a heat treatment at 450 ° C. × 2 hours in an oxidizing atmosphere, Thickness 100-200 × 10 -8 c
Thus, a sample of the present invention having a m-type iron-based oxide film (see FIG. 1) formed on the surface was obtained.
【００１２】また、同上材質・同上寸法のステンレス鋼
製試料について同上条件で電解研磨のみを行った、比較
例の試料を得た。A sample of a comparative example was obtained by subjecting only a stainless steel sample of the same material and dimensions as described above to electrolytic polishing only under the same conditions.
【００１３】次に、キャップ２を溶接した管体１の上面
一杯まで、２重量％過酸化水素水または４重量％過酸化
水素水を満たして蓋３で蓋をした後、図３に示すよう
に、この管体１を管体内と同じ濃度の過酸化水素水を満
たした容器４内の過酸化水素水に浸し、クリーンルーム
室内に静置した。そして、試験開始後、１２日目、２４
日目に容器内の過酸化水素水を取り出し、ＩＣＰ−ＭＳ
（誘導結合プラズマ質量分析計）で金属イオンの分析を
行った。すなわち、試験開始後１２日目に容器内の過酸
化水素水を取り出して金属イオンの分析を行い、次い
で、新しい過酸化水素水を容器内に満たし、引き続き１
３日目から２４日目までの１２日間同上試料を浸漬した
後の容器内の過酸化水素水を取り出して金属イオンの分
析を行った。金属イオンの分析結果（μｇ／リットル）
を以下の表１に示す。Next, the cap 2 is filled with 2% by weight of hydrogen peroxide solution or 4% by weight of hydrogen peroxide solution and is covered with the cover 3 until the top surface of the tube 1 to which the cap 2 is welded is fully filled, and as shown in FIG. Then, the tube 1 was immersed in a hydrogen peroxide solution in a container 4 filled with a hydrogen peroxide solution having the same concentration as that of the tube, and was left still in a clean room. And, on the 12th day after the start of the test, 24
On the day, take out the hydrogen peroxide solution in the container and use ICP-MS
(Inductively coupled plasma mass spectrometer) was used to analyze metal ions. That is, on the 12th day after the start of the test, the hydrogen peroxide solution in the container was taken out, the metal ions were analyzed, and then the container was filled with fresh hydrogen peroxide solution.
The hydrogen peroxide solution in the container after the sample was immersed for 12 days from the third day to the 24th day was taken out and analyzed for metal ions. Analysis results of metal ions (μg / liter)
Is shown in Table 1 below.
【００１４】[0014]
【表１】 [Table 1]
【００１５】表１に明らかなとおり、本実施例の試料は
比較例の試料に比して金属イオンの溶出量は少なく、過
酸化水素水に対して優れた耐性を有している。As is clear from Table 1, the sample of this example has a smaller amount of metal ions eluted than the sample of the comparative example, and has excellent resistance to aqueous hydrogen peroxide.
【００１６】本実施例ではステンレス鋼としてＳＵＳ３
１６Ｌを使用したが、ＳＵＳ３１６等であってもよく、
各種ステンレス鋼が使用できる。In this embodiment, SUS3 is used as stainless steel.
Although 16L was used, SUS316 or the like may be used.
Various stainless steels can be used.
【００１７】[0017]
【発明の効果】本発明によれば、過酸化水素に対する金
属イオンの溶出量が極めて少ないステンレス鋼及びその
製造方法を提供することができる。According to the present invention, it is possible to provide a stainless steel having a very small amount of metal ions eluted with respect to hydrogen peroxide and a method for producing the same.
【図１】電解研磨後に酸化雰囲気で加熱処理を行ったス
テンレス鋼表面の厚さ方向の原子濃度分布を示す図であ
る。FIG. 1 is a diagram showing an atomic concentration distribution in a thickness direction of a stainless steel surface subjected to a heat treatment in an oxidizing atmosphere after electrolytic polishing.
【図２】金属イオンの溶出試験で使用した試料の側面図
である。FIG. 2 is a side view of a sample used in a metal ion elution test.
【図３】金属イオンの溶出試験方法を説明する図であ
る。FIG. 3 is a diagram illustrating a metal ion elution test method.
Claims (3)
２００×１０-8ｃｍの厚みの鉄系酸化物を主とする金属
酸化物の被膜が形成された過酸化水素用ステンレス鋼。1. The method according to claim 1, further comprising the step of:
A stainless steel for hydrogen peroxide on which a metal oxide film mainly composed of an iron-based oxide having a thickness of 200 × 10 −8 cm is formed.
た後、酸化性雰囲気中で加熱することにより、１００〜
２００×１０ -8 ｃｍの厚みの鉄系酸化物を主とする金属
酸化物の着色酸化被膜を表面に形成することを特徴とす
る過酸化水素用ステンレス鋼の製造方法。Wherein after being subjected to electrolytic polishing stainless steel surfaces, by heating in an oxidizing atmosphere, 100
A method for producing stainless steel for hydrogen peroxide, comprising forming a colored oxide film of a metal oxide mainly composed of an iron-based oxide having a thickness of 200 × 10 −8 cm on the surface.
時間加熱するものであることを特徴とする請求項２記載
の過酸化水素用ステンレス鋼の製造方法。3. The heating conditions are 400 to 500 ° C. and 1 to 3
The method for producing stainless steel for hydrogen peroxide according to claim 2, wherein the heating is performed for a time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30018096A JP3194875B2 (en) | 1996-11-12 | 1996-11-12 | Stainless steel for hydrogen peroxide and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30018096A JP3194875B2 (en) | 1996-11-12 | 1996-11-12 | Stainless steel for hydrogen peroxide and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10140322A JPH10140322A (en) | 1998-05-26 |
| JP3194875B2 true JP3194875B2 (en) | 2001-08-06 |
Family
ID=17881710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30018096A Expired - Fee Related JP3194875B2 (en) | 1996-11-12 | 1996-11-12 | Stainless steel for hydrogen peroxide and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3194875B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113005499A (en) * | 2021-02-25 | 2021-06-22 | 珠海复旦创新研究院 | Corrosion-resistant oxide film and preparation method and application thereof |
-
1996
- 1996-11-12 JP JP30018096A patent/JP3194875B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10140322A (en) | 1998-05-26 |
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