JPH0634624A - Sensitization detection of austenitic stainless steel - Google Patents
Sensitization detection of austenitic stainless steelInfo
- Publication number
- JPH0634624A JPH0634624A JP4186546A JP18654692A JPH0634624A JP H0634624 A JPH0634624 A JP H0634624A JP 4186546 A JP4186546 A JP 4186546A JP 18654692 A JP18654692 A JP 18654692A JP H0634624 A JPH0634624 A JP H0634624A
- Authority
- JP
- Japan
- Prior art keywords
- sensitization
- grain boundary
- area
- width
- stainless steel
- Prior art date
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明はオーステナイト系ステン
レス鋼の応力腐食割れ感受性を測定する鋭敏化検出方法
に係り、特に、非熟練者でも容易、且つ、精度良く検出
することのできるステンレス鋼の鋭敏化検出方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sensitization detection method for measuring the stress corrosion cracking susceptibility of austenitic stainless steel, and particularly to the sensitivity of stainless steel which can be easily and accurately detected by unskilled persons. Detecting method
【０００２】[0002]
【従来の技術】オーステナイト系ステンレス鋼の応力腐
食割れ感受性を測定する従来の方法として、電気化学的
再活性化法（ＥＰＲ法，JIS G 0580）が知られている。
この方法は、オーステナイト系ステンレス鋼の０.５mol
／リットル硫酸−０.０１mol／リットルチオシアン酸カ
リウム溶液中における往復アノード分極曲線かの電気化
学的再活性化率（往路と復路の最大アノード電流密度の
比）を測定し応力腐食割れ感受性を判定するものであ
る。なお電気化学的再活性化率が高いほど応力腐食割れ
感受性が高いと判定される。2. Description of the Related Art An electrochemical reactivation method (EPR method, JIS G 0580) is known as a conventional method for measuring the stress corrosion cracking susceptibility of austenitic stainless steel.
This method uses 0.5 mol of austenitic stainless steel.
Per liter sulfuric acid-0.01 mol / liter potassium thiocyanate solution, the reciprocal anodic polarization curve or electrochemical reactivation rate (ratio of maximum anode current density of forward and backward paths) is measured to judge the stress corrosion cracking susceptibility. It is a thing. It is determined that the higher the electrochemical reactivation rate, the higher the stress corrosion cracking susceptibility.
【０００３】[0003]
【発明が解決しようとする課題】ＥＰＲ法は実機に適用
できるような小型装置を開発するのは困難であり、ま
た、測定領域内の平均的な応力腐食割れ感受性を測定し
ているという欠点があった。The EPR method has a drawback that it is difficult to develop a small apparatus that can be applied to an actual machine, and that the average stress corrosion cracking susceptibility in the measurement region is measured. there were.
【０００４】[0004]
【課題を解決するための手段】上記欠点は、顕微鏡で観
察される金属組織を画像処理することにより結晶粒界の
幅および面積を測定し、鋭敏化している粒界の数や面積
を基に、局所的な応力腐食割れ感受性を測定できる方法
を提供することにある。The above-mentioned drawbacks are that the width and area of crystal grain boundaries are measured by image-processing the metallographic structure observed by a microscope, and the number and area of the grain boundaries are sharpened. The object is to provide a method capable of measuring local stress corrosion cracking susceptibility.
【０００５】[0005]
【作用】光学顕微鏡より観察される金属組織を画像処理
することにより粒界幅を測定し、鋭敏化している粒界の
数や面積から材料の応力腐食割れ感受性を定量的に評価
できる。The grain boundary width can be measured by image-processing the metallographic structure observed by an optical microscope, and the stress corrosion cracking susceptibility of the material can be quantitatively evaluated from the number and area of grain boundaries that are sensitized.
【０００６】[0006]
【実施例】以下、本発明の一実施例を図面を参照して説
明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to the drawings.
【０００７】一般的に、オーステナイト系ステンレス鋼
は、５５０〜８５０℃の温度範囲に加熱されると、クロ
ム炭化物(Ｍ23Ｃ6型：ＭはＣｒまたはＦｅ）が結晶粒界
に析出し、耐食性が低下する。耐食性が低下するような
状態になることを鋭敏化すると言う。鋭敏化を模擬する
ための熱処理方法として、溶体化処理後に６２１℃で数
時間保持し、或いは、７５０℃で５〜６時間保持した後
に５００℃で数時間保持することが行われている。この
鋭敏化の為の熱処理時間が短いと、粒界の炭化物はそれ
ほど成長せず島状に互いに独立している。しかし、熱処
理時間が長くなると島状の炭化物が成長して合体し、粒
界全体が炭化物でつながるようになる。析出したクロム
炭化物とオーステナイト基地との間の境界において、オ
ーステナイト基地側に、クロム濃度が合金の平均成分よ
り低い領域が存在する。図１は粒界近傍のクロム濃度の
分布を示す模式図である。粒界のクロム炭化物近傍に
は、クロム濃度が１２％以下の領域が数Åの幅で形成さ
れていることが実測されている。鋭敏化は粒界近傍のク
ロム欠乏層のクロム濃度が１２％以下となることによ
り、耐食性が低下し、応力腐食割れ感受性が高くなるこ
とである。[0007] Generally, when austenitic stainless steel is heated to a temperature range of 550 to 850 ° C, chromium carbide (M 23 C 6 type: M is Cr or Fe) is precipitated at grain boundaries and corrosion resistance. Is reduced. Sensitization means that the corrosion resistance is reduced. As a heat treatment method for simulating sensitization, holding at 621 ° C. for several hours after solution treatment or holding at 750 ° C. for 5 to 6 hours and then holding at 500 ° C. for several hours is performed. When the heat treatment time for this sensitization is short, the carbides at the grain boundaries do not grow so much and are independent of each other in an island shape. However, when the heat treatment time becomes long, island-shaped carbides grow and coalesce, and the entire grain boundaries are connected by the carbides. At the boundary between the precipitated chromium carbide and the austenite matrix, there is a region on the austenite matrix side where the chromium concentration is lower than the average component of the alloy. FIG. 1 is a schematic diagram showing the distribution of chromium concentration in the vicinity of grain boundaries. It has been measured that a region with a chromium concentration of 12% or less is formed in a width of several Å near the chromium carbide at the grain boundary. Sensitization means that when the chromium concentration in the chromium-deficient layer near the grain boundary is 12% or less, the corrosion resistance decreases and the stress corrosion cracking susceptibility increases.
【０００８】鋭敏化は、粒界へのクロム炭化物の析出に
伴う粒内のクロム欠乏層のクロム濃度と欠乏層の幅とに
依存する。その両者を材料外部から直接測定することは
できないため、従来は、例えば、ＥＰＲ法がよく使用さ
れている。但し、ＥＰＲ法では、測定した面積内におけ
る平均的な鋭敏化の状態を把握できるだけである。The sensitization depends on the chromium concentration in the chromium-deficient layer in the grain and the width of the depletion layer due to the precipitation of chromium carbide at the grain boundary. Since both of them cannot be directly measured from the outside of the material, for example, the EPR method is often used conventionally. However, the EPR method can only grasp the average state of sensitization within the measured area.
【０００９】図２と図３はオーステナイト系ステンレス
鋼ＳＵＳ３０４の溶体化処理材と鋭敏化熱処理材をシュ
ー酸エッチングした金属組織の模式図である。溶体化処
理した試料の粒界の幅（黒線の部分）は非常に狭いのに
対し、鋭敏化させるために熱処理を行った試料の粒界の
幅は広くなっている箇所が見られる。したがって、粒界
の幅や粒界の面積を測定すれば、鋭敏化している粒界の
数あるいは鋭敏化している粒界の面積から、試料の鋭敏
化の程度つまり耐食性が低下した程度を判定できること
になる。FIG. 2 and FIG. 3 are schematic diagrams of the metallographic structure of austenitic stainless steel SUS304 obtained by subjecting the solution heat treated material and the sensitized heat treated material to oxalic acid etching. The width of the grain boundary (black line portion) of the solution-treated sample is very narrow, whereas the width of the grain boundary of the sample heat-treated for sensitization is wide. Therefore, by measuring the width of the grain boundary or the area of the grain boundary, it is possible to determine the degree of sensitization of the sample, that is, the degree of decrease in corrosion resistance, from the number of sensitized grain boundaries or the area of sensitized grain boundaries. become.
【００１０】そこで、エッチング処理した後の粒界の幅
Ｂと長さＬおよび面積Ｓを測定し、鋭敏化している粒界
の数ＮS と全粒界の数Ｎの比Ｒ１を数１より求める。ま
た、非鋭敏化粒界幅Ｂ0 と粒界長さＬの積を基準面積Ｓ
0 とし、基準面積Ｓ0 と全粒界の面積の比Ｒ２を数２よ
り求める。Therefore, the width B, the length L and the area S of the grain boundaries after the etching treatment are measured, and the ratio R1 of the number N S of sensitized grain boundaries and the number N of all grain boundaries is calculated from Ask. Further, the product of the desensitized grain boundary width B 0 and the grain boundary length L is the reference area S
0, and the reference area S 0 and the ratio of the area of Zentsubukai R2 obtained from the number 2.
【００１１】 Ｒ１＝Ｎ／ＮS …（数１） Ｒ２＝ΣＢ・Ｌ／Ｂ0・ΣＬ＝ΣＳ／ΣＳ0 …（数２） 本発明ではこのＲ１またはＲ２により鋭敏化程度を判定
するものである。R1 = N / N S (Equation 1) R2 = ΣB · L / B 0 · ΣL = ΣS / ΣS 0 (Equation 2) In the present invention, the degree of sensitization is determined by R1 or R2. is there.
【００１２】実施例で用いた材料は、オーステナイト系
ステンレス鋼ＳＵＳ３０４であり、その炭素量は０.０
６％ で十分に鋭敏化を生じるものである。ＳＵＳ３０
４を１１５０℃で３０分保持した後、水冷して溶体化処
理を行い、鋭敏化させるための熱処理は、６２０℃にお
いて０分，１５分，６０分，１２０分，１８０分，３０
０分，６００分，１４４０分保持することで行った。そ
の後、試料表面を鏡面仕上げし、１０％のシュー酸で電
解エッチングを行った。エッチングした後の表面組織写
真およびＲ１，Ｒ２の測定結果を図４に示す。The material used in the examples is austenitic stainless steel SUS304, the carbon content of which is 0.0.
6% gives sufficient sensitization. SUS30
4 was held at 1150 ° C. for 30 minutes, and then subjected to solution treatment by cooling with water, and heat treatment for sensitization was performed at 620 ° C. for 0 minutes, 15 minutes, 60 minutes, 120 minutes, 180 minutes, 30 minutes.
It was carried out by holding for 0 minutes, 600 minutes, and 1440 minutes. Then, the surface of the sample was mirror-finished and electrolytically etched with 10% of succinic acid. The photograph of the surface structure after etching and the measurement results of R1 and R2 are shown in FIG.
【００１３】粒界の幅や面積の測定は、四百倍で撮影し
た金属組織写真を５枚程度用意し、その中の全ての粒界
について行った。溶体化処理した試料の粒界幅は０.５
μｍ、十分に鋭敏化した試料の粒界幅は２μｍ程度とな
ったので、測定した粒界幅Ｂが１.５μｍ を超える粒界
を鋭敏化した粒界とした。また、基準面積Ｓ0 を決定す
る非鋭敏化粒界幅Ｂ0 を０.５μｍ とした。The width and area of the grain boundaries were measured by preparing about five metallographic photographs taken at a magnification of 400 times and conducting all grain boundaries therein. The grain boundary width of the solution treated sample is 0.5
Since the grain boundary width of the sample sufficiently sensitized to μm was about 2 μm, the grain boundary with the measured grain boundary width B exceeding 1.5 μm was set as the sensitized grain boundary. The desensitized grain boundary width B 0 that determines the reference area S 0 was set to 0.5 μm.
【００１４】保持時間ｔ＝１５分まではＲ１およびＲ２
はほとんど変化しない。ｔ＝６０分を超えると、急速に
Ｒ１およびＲ２は大きくなりｔ＝１８０分で飽和する傾
向にある。応力腐食割れの試験結果を基にすれば、応力
腐食割れは６２０℃の熱処理温度では約６０〜９０分で
生じるとされているので、応力腐食割れを生じる限界の
値は図４に示したようにＲ１は約４０％Ｒ２は基準面積
の２.５ 倍とすることができる。R1 and R2 up to holding time t = 15 minutes
Hardly changes. Above t = 60 minutes, R1 and R2 rapidly increase and tend to saturate at t = 180 minutes. Based on the stress corrosion cracking test results, it is said that stress corrosion cracking occurs at a heat treatment temperature of 620 ° C. in about 60 to 90 minutes, so the limit value of stress corrosion cracking is as shown in FIG. In addition, R1 can be about 40% and R2 can be 2.5 times the reference area.
【００１５】以上、鋭敏化検出方法のフローチャートを
図５に示す。The flow chart of the sensitization detecting method is shown in FIG.
【００１６】[0016]
【発明の効果】本発明によれば、分解が困難な構造物の
溶接熱影響部の金属組織の画像を顕微鏡を通して取り込
み、画像処理して金属粒界の幅を測定することにより個
々の粒界が鋭敏化しているかの判定をし、鋭敏化してい
ると判定された粒界の数および面積を測定することによ
り、応力腐食割れ感受性、言い換えれば鋭敏化の程度に
応じて、熱影響部の熱処理，機械加工による耐応力腐食
割れに対する最適な対策工法の選定が可能となる。According to the present invention, an image of a metal structure of a heat-affected zone of a structure which is difficult to decompose is taken in through a microscope, and image processing is performed to measure the width of each metal grain boundary. Of the heat-affected zone depending on the stress corrosion cracking susceptibility, in other words, the degree of sensitization, by determining the number and area of grain boundaries determined to be sensitized. Therefore, it is possible to select the optimum construction method against stress corrosion cracking caused by machining.
【図１】粒界近傍のクロム濃度の分布図。FIG. 1 is a distribution diagram of chromium concentration near the grain boundary.
【図２】オーステナイトステンレス鋼ＳＵＳ３０４の溶
体化熱処理材と鋭敏化熱処理材をシュー酸エッチングし
た金属組織の説明図。FIG. 2 is an explanatory view of a metal structure of austenitic stainless steel SUS304 obtained by subjecting a solution heat treatment material and a sensitization heat treatment material to a oxalic acid etching.
【図３】オーステナイトステンレス鋼ＳＵＳ３０４の溶
体化熱処理材と鋭敏化熱処理材をシュー酸エッチングし
た金属組織の説明図。FIG. 3 is an explanatory view of a metal structure of austenitic stainless steel SUS304 obtained by subjecting a solution heat-treated material and a sensitized heat-treated material to a oxalic acid etching.
【図４】図４は熱処理時間による金属組織と鋭敏化度の
変化を示す説明図。FIG. 4 is an explanatory diagram showing changes in metal structure and sensitization degree according to heat treatment time.
【図５】図５は鋭敏化検出方法のフローチャート。FIG. 5 is a flowchart of a sensitization detection method.
ｔ…保持時間(min）、Ｒ…鋭敏化度（％）。 t ... holding time (min), R ... sensitization degree (%).
Claims (6)
ステンレス鋼の表面を研磨し、研磨された表面をエッチ
ングし、前記エッチングされた表面の所定領域内に存在
する粒界の幅と面積を測定し、前記粒界の幅が所定の幅
よりも大きい粒界を鋭敏化した粒界と判定し、鋭敏化さ
れたと判定された粒界の数と粒界の面積に基づいて鋭敏
化程度を判定することを特徴とするオーステナイト系ス
テンレス鋼の鋭敏化検出方法。1. A surface of austenitic stainless steel that has been thermally affected by welding or the like is polished, the polished surface is etched, and the width and area of grain boundaries existing in a predetermined region of the etched surface are determined. Measured, the width of the grain boundary is determined to be a grain boundary sensitized grain boundaries larger than a predetermined width, the degree of sensitization based on the number of grain boundaries determined to be sensitized and the area of the grain boundaries. A method for detecting sensitization of austenitic stainless steel, which comprises determining.
する粒界の数と鋭敏化されたと判定された粒界の数の比
で鋭敏化程度を判定するオーステナイト系ステンレス鋼
の鋭敏化検出方法。2. The sensitization detection of austenitic stainless steel according to claim 1, wherein the degree of sensitization is determined by the ratio of the number of grain boundaries existing in the predetermined region and the number of grain boundaries determined to be sensitized. Method.
０.５μｍ とし、前記非鋭敏化粒界の幅と前記所定領域
内に存在する粒界長さの積を基準面積とし、前記基準面
積と前記所定領域内に存在する粒界の面積の比で鋭敏化
程度を判定するオーステナイト系ステンレス鋼の鋭敏化
検出方法。3. The method according to claim 1, wherein the width of the non-sensitized grain boundary is 0.5 μm, and the product of the width of the non-sensitized grain boundary and the length of the grain boundary existing in the predetermined region is a reference area, A method for detecting sensitization of austenitic stainless steel, wherein the degree of sensitization is determined by the ratio of the area of a grain boundary existing in the predetermined area to the reference area.
グされた表面の金属組織を光学顕微鏡を通して画像処理
装置にとりこむオーステナイト系ステンレス鋼の鋭敏化
検出方法。4. The method for detecting sensitization of austenitic stainless steel according to claim 1, 2, or 3, wherein the metal structure of the etched surface is taken into an image processing apparatus through an optical microscope.
内に存在する粒界の数と鋭敏化されたと判定された粒界
の数の比が４０％以上であれば、鋭敏化しており、応力
腐食割れ感受性が高いと判定するオーステナイト系ステ
ンレス鋼の鋭敏化検出方法。5. The sensitization according to claim 1, wherein the ratio of the number of grain boundaries existing in the predetermined region to the number of grain boundaries determined to be sensitized is 40% or more, A method for detecting sensitization of austenitic stainless steel, which is determined to have high susceptibility to stress corrosion cracking.
と所定領域内に存在する粒界の面積の比が２.５ 以上で
あれば、鋭敏化しており、応力腐食割れ感受性が高いと
判定するオーステナイト系ステンレス鋼の鋭敏化検出方
法。6. The method according to claim 1, wherein the ratio between the reference area and the area of the grain boundary existing in the predetermined region is 2.5 or more, the sensitization is high and the stress corrosion cracking susceptibility is high. A method for detecting sensitization of austenitic stainless steel to be judged.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4186546A JPH0634624A (en) | 1992-07-14 | 1992-07-14 | Sensitization detection of austenitic stainless steel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4186546A JPH0634624A (en) | 1992-07-14 | 1992-07-14 | Sensitization detection of austenitic stainless steel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0634624A true JPH0634624A (en) | 1994-02-10 |
Family
ID=16190403
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4186546A Pending JPH0634624A (en) | 1992-07-14 | 1992-07-14 | Sensitization detection of austenitic stainless steel |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0634624A (en) |
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|---|---|---|---|---|
| JP2010025820A (en) * | 2008-07-22 | 2010-02-04 | Nippon Steel Corp | Crystal grain analyzer, and crystal grain analysis method and computer program |
| JP2010091536A (en) * | 2008-10-10 | 2010-04-22 | Nippon Steel Corp | Crystal grain analyzer, crystal grain analysis method, and computer program |
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| CN103411972A (en) * | 2013-08-23 | 2013-11-27 | 北京科技大学 | Counting method of delta ferritic phase area content in Martensite heat resistant steel |
| CN105738272A (en) * | 2016-03-01 | 2016-07-06 | 贵州大学 | Method for simply and conveniently analyzing proportion between two phase ingredients of 1.4460 duplex stainless steel |
| CN111413185A (en) * | 2020-04-15 | 2020-07-14 | 重庆赛宝工业技术研究院 | Heat treatment method for detecting TP347HFG |
| KR20210073759A (en) * | 2019-12-11 | 2021-06-21 | 주식회사 피레타 | Austenite Stainless Steel Life Evaluation Method |
-
1992
- 1992-07-14 JP JP4186546A patent/JPH0634624A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010025820A (en) * | 2008-07-22 | 2010-02-04 | Nippon Steel Corp | Crystal grain analyzer, and crystal grain analysis method and computer program |
| JP2010091536A (en) * | 2008-10-10 | 2010-04-22 | Nippon Steel Corp | Crystal grain analyzer, crystal grain analysis method, and computer program |
| CN101846634A (en) * | 2010-04-28 | 2010-09-29 | 首钢总公司 | Method for analyzing dynamic phase transformation of low carbon steel |
| CN103411972A (en) * | 2013-08-23 | 2013-11-27 | 北京科技大学 | Counting method of delta ferritic phase area content in Martensite heat resistant steel |
| CN103411972B (en) * | 2013-08-23 | 2016-04-27 | 北京科技大学 | Delta ferrite phase area content statistical method in a kind of martensite heat-resistant steel |
| CN105738272A (en) * | 2016-03-01 | 2016-07-06 | 贵州大学 | Method for simply and conveniently analyzing proportion between two phase ingredients of 1.4460 duplex stainless steel |
| KR20210073759A (en) * | 2019-12-11 | 2021-06-21 | 주식회사 피레타 | Austenite Stainless Steel Life Evaluation Method |
| CN111413185A (en) * | 2020-04-15 | 2020-07-14 | 重庆赛宝工业技术研究院 | Heat treatment method for detecting TP347HFG |
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