JP2005114626A - Corrosive liquid for exposing austenitic grain boundary - Google Patents
Corrosive liquid for exposing austenitic grain boundary Download PDFInfo
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本発明は、ボロン鋼あるいは高炭素クロム軸受鋼の焼入材などの結晶粒界、特にオーステナイト結晶粒界を顕出するために使用する鋼表面の腐食液に関する。 The present invention relates to a corrosive solution for a steel surface used for revealing grain boundaries such as hardened materials of boron steel or high carbon chromium bearing steel, particularly austenite grain boundaries.
鋼の凝固組織あるいは焼入材などの金属組織を顕出することは、鋼の凝固状態や焼入材の組織状態を把握する上に欠くことのできない事柄であり、研究や品質間の面から極めて重要である。このような鋼の凝固組織の顕出方法としては、例えば、a.低炭素鋼などを含む普通鋼などは、ピクリン酸飽和水溶液1リットルにライポンF(商品名:ライオン油脂製)などの洗剤2〜3滴を加えた腐食液を80℃に加熱し、その中に鋼片より採取して鏡面研磨を行った試料を1〜3分間浸漬する方法が知られている。(非特許文献1、非特許文献2参照)。b.一方、炭素濃度が50ppm以下の極低炭素鋼鋳片のデンドライトの顕出方法としては、試料を700℃以上、780℃以下に加熱した後、冷却した試料を腐食液で腐食してエッチングする方法が知られている(特許文献1参照)。 It is indispensable to reveal the solidification structure of steel or the metal structure such as hardened material in order to understand the solidification state of steel and the structure of hardened material. Very important. As a method for revealing such a solidified structure of steel, for example, a. For ordinary steel, including low-carbon steel, etc., heat a corrosive solution containing 2 to 3 drops of detergent such as Raipon F (trade name: Lion Oil) to 1 liter of a saturated aqueous solution of picric acid to 80 ° C. A method of immersing a sample taken from a steel piece and mirror-polished for 1 to 3 minutes is known. (See Non-Patent Document 1 and Non-Patent Document 2). b. On the other hand, as a method for revealing dendrites of ultra low carbon steel slabs having a carbon concentration of 50 ppm or less, a sample is heated to 700 ° C. or more and 780 ° C. or less, and then the cooled sample is etched by etching with a corrosive liquid. Is known (see Patent Document 1).
さらに出願人は、炭素鋼あるいは低合金鋼鋳片の凝固組織のデンドライトを顕出する腐食液として、60〜80℃の温水500mlに対してピクリン酸を6〜8g溶解し、これにライポンFなどの洗剤を3〜5mlを加え、さらに界面活性剤としてドデシルベンゼンスルフォン酸ナトリウム2〜4gを加えるもの開発している(特許文献2参照)。 Furthermore, the applicant dissolved 6-8 g of picric acid in 500 ml of hot water at 60 to 80 ° C. as a corrosive solution for revealing the dendrite of the solidified structure of the carbon steel or low alloy steel slab. 3-5 ml of this detergent is added, and 2-4 g of sodium dodecylbenzenesulfonate is added as a surfactant (see Patent Document 2).
ところでオーステナイト結晶粒度の顕出のためのエッチングは、通常、飽和ピクリン酸水溶液とライポンFで行われるが、ボロン鋼あるいは高炭素クロム軸受鋼の焼入材などのオーステナイト結晶粒界の顕出は十分でなく、試行錯誤で薬品により化学腐食する問題があった。 By the way, etching for revealing the austenite grain size is usually performed with a saturated picric acid aqueous solution and Lipon F, but austenite grain boundaries such as hardened materials of boron steel or high carbon chromium bearing steel are sufficiently revealed. However, there was a problem of chemical corrosion by chemicals through trial and error.
そこで、ボロン鋼あるいは高炭素クロム軸受鋼の焼入材などのオーステナイト結晶粒界の顕出は沸騰ピクリン酸水溶液とドデシルベンゼンスルフォン酸ナトリウムと過酸化水素とからなる腐食液で腐食している。この腐食液によるとき、結晶粒はきれいに顕出できる。しかし、この腐食液は沸騰型のため、腐食液の消耗と組成の変化が激しく、かつ腐食時間が30秒と短いので、腐食程度のコントロールが難しく、使いにくい面があった。 Therefore, the appearance of austenite grain boundaries such as a hardened material of boron steel or high carbon chromium bearing steel is corroded with a corrosive solution composed of a boiling picric acid aqueous solution, sodium dodecylbenzenesulfonate and hydrogen peroxide. When this corrosive solution is used, the crystal grains can be clearly revealed. However, since the corrosive liquid is a boiling type, the consumption of the corrosive liquid and the change in composition are severe, and the corrosive time is as short as 30 seconds. Therefore, it is difficult to control the degree of corrosion and it is difficult to use.
そこで、本発明が解決しようとする課題は、これらの腐食液に代えて、ボロン鋼あるいは高炭素クロム軸受鋼の焼入材などのオーステナイト結晶粒界の顕出を的確にかつ容易に行える腐食液を提供することである。 Therefore, the problem to be solved by the present invention is to replace the corrosive liquid with a corrosive liquid capable of accurately and easily revealing austenite grain boundaries such as a hardened material of boron steel or high carbon chromium bearing steel. Is to provide.
上記の課題を解決するための本発明の手段は、請求項1の発明では、ボロン鋼の焼入材のオーステナイト結晶粒界を顕出する腐食液において、400mlのH2Oに対してピクリン酸を15〜25gを溶解し、これに洗剤のライポンF(商品名:ライオン油脂製)20〜40mlを加え、さらに界面活性剤としてドデシルベンゼンスルフォン酸ナトリウムを4〜10gを加えてなることを特徴とするオーステナイト結晶粒界顕出用の腐食液である。なお、本願発明におけるボロン鋼とは、質量%でBを0.0005%以上含有する鋼からなる機械構造用鋼を指している。 The means of the present invention for solving the above-mentioned problems is that, in the invention of claim 1, picric acid is used for 400 ml of H 2 O in a corrosive solution that reveals the austenite grain boundaries of the hardened material of boron steel. It is characterized by adding 15 to 25 g of detergent, adding 20 to 40 ml of detergent Rypon F (trade name: manufactured by Lion Oil), and adding 4 to 10 g of sodium dodecylbenzenesulfonate as a surfactant. This is a corrosive solution for revealing austenite grain boundaries. In addition, the boron steel in this invention has pointed out the steel for machine structures which consists of steel which contains B 0.0005% or more by mass%.
請求項2の発明では、高炭素クロム軸受鋼の焼入材のオーステナイト結晶粒界を顕出する腐食液において、400mlのH2Oに対してピクリン酸を15〜25gを溶解し、これに洗剤のライポンF(商品名:ライオン油脂製)20〜40mlを加え、さらに界面活性剤としてドデシルベンゼンスルフォン酸ナトリウムを4〜10gを加えてなることを特徴とするオーステナイト結晶粒界顕出用の腐食液である。なお、本発明における高炭素クロム軸受鋼はJISで規定するSUJ鋼をいう。 In the invention of claim 2, 15-25 g of picric acid is dissolved in 400 ml of H 2 O in a corrosive solution that reveals the austenite grain boundaries of the hardened material of high-carbon chromium bearing steel, and a detergent No. Raipon F (trade name: manufactured by Lion Yushi) 20-40 ml, and 4-10 g of sodium dodecylbenzenesulfonate as a surfactant is further added. Corrosive solution for revealing austenite grain boundaries It is. In addition, the high carbon chromium bearing steel in this invention means SUJ steel prescribed | regulated by JIS.
本発明のオーステナイト結晶粒界顕出用の腐食液を使用することで、従来は上記した沸騰型でしか顕出が難しかったボロン鋼や非ボロン鋼である高炭素クロム軸受鋼の焼入材のオーステナイト結晶粒界の顕出が、低炭素鋼鋳片のデンドライトの顕出に対して使用する従来のライポンFと飽和ピクリン酸水溶液の場合と同様の作業で的確かつ容易に好結果を得てできるようになった。 By using the austenite grain boundary revealing corrosion liquid of the present invention, the hardened material of the high carbon chromium bearing steel, which is a boron steel or non-boron steel, which has been difficult to reveal only with the above-described boiling type. Appearance of austenite grain boundaries can be obtained accurately and easily with the same operation as in the case of conventional Lipon F and saturated picric acid aqueous solution used for the appearance of dendrites of low carbon steel slabs. It became so.
本発明を実施するための最良の形態を図面を参照して説明する。図1の(a)は本発明におけるオーステナイト結晶粒界顕出用の腐食液で顕出したボロン鋼のオーステナイト結晶粒界を400倍で示す顕微鏡写真で、図1の(b)は本発明におけるオーステナイト結晶粒界顕出用の腐食液で顕出したボロン鋼のオーステナイト結晶粒界を1000倍で示す顕微鏡写真である。図2の(a)は本発明の腐食液とは組成を変えた腐食液で顕出したボロン鋼のオーステナイト結晶粒界を400倍で示す顕微鏡写真で、図2の(b)は本発明の腐食液とは組成を変えた腐食液で顕出したボロン鋼のオーステナイト結晶粒界を1000倍で示す顕微鏡写真である。図3は本発明におけるオーステナイト結晶粒界顕出用の腐食液で顕出した高炭素クロム軸受鋼のオーステナイト結晶粒界を1000倍で示す顕微鏡写真である。図4は本発明の上記の腐食液とは組成を変えた腐食液で顕出した高炭素クロム軸受鋼のオーステナイト結晶粒界を1000倍で示す顕微鏡写真である。
本発明を実施するための最良の形態を下記の実施例1および実施例2を通じて、比較例1および比較例2と対比して説明する。
The best mode for carrying out the present invention will be described with reference to the drawings. FIG. 1 (a) is a photomicrograph showing the austenite grain boundary of boron steel revealed by the corrosive solution for revealing austenite grain boundaries in the present invention at 400 times, and FIG. 1 (b) is a diagram in the present invention. It is a microscope picture which shows the austenite grain boundary of boron steel revealed with the corrosive liquid for austenite grain boundary appearance by 1000 time. FIG. 2 (a) is a photomicrograph showing the austenite grain boundary of boron steel revealed by a corrosive liquid having a composition different from that of the present invention at a magnification of 400, and FIG. The corrosive liquid is a photomicrograph showing the austenite grain boundary of boron steel revealed by a corrosive liquid having a different composition at a magnification of 1000 times. FIG. 3 is a photomicrograph showing the austenite grain boundary of the high carbon chromium bearing steel 1000 times as revealed with the austenite grain boundary revealing liquid in the present invention. FIG. 4 is a photomicrograph showing the austenite grain boundary of the high carbon chromium bearing steel 1000 times as revealed by a corrosive liquid having a different composition from the above corrosive liquid of the present invention.
The best mode for carrying out the present invention will be described in comparison with Comparative Example 1 and Comparative Example 2 through Example 1 and Example 2 below.
ボロン鋼の焼入材のオーステナイト結晶粒界を顕出するための本発明の腐食液は、ピクリン酸20g、ライポンF30ml、ドデシルベンゼンスルフォン酸ナトリウム6gを水400mlに溶解してエッチング用の腐食液とした。 The corrosive liquid of the present invention for revealing the austenite grain boundaries of the hardened boron steel is obtained by dissolving 20 g of picric acid, 30 ml of Raipon F, and 6 g of sodium dodecylbenzenesulfonate in 400 ml of water, did.
この腐食液を適用するボロン鋼は、例えば、質量%で、C:0.20%、Si:0.11%、Mn:0.28%、P:0.012%、S:0.015%、Cr:1.05%、Mo:0.01%、B:0.0015%、Al:0.009%、N:0.0052%、O:0.0018%を含有し、残部Feおよび不可避不純物からなる鋼である。このボロン鋼からなる鋼試片を研磨して鏡面とし、次いで上記腐食液の63℃とした溶液に浸漬して研磨して得た鏡面を4分間エッチングし、ボロン鋼のオーステナイト結晶粒界を顕出した。顕出したエッチング面を顕微鏡で400倍にして撮影した写真を図1の(a)に、さらに1000倍にして撮影した写真を図1の(b)に示す。これらの顕微鏡写真に見られるとおり、従来の沸騰型としなくとも、ボロン鋼のオーステナイト結晶粒界は明瞭に顕出された。 The boron steel to which this corrosive liquid is applied is, for example, in mass%, C: 0.20%, Si: 0.11%, Mn: 0.28%, P: 0.012%, S: 0.015% , Cr: 1.05%, Mo: 0.01%, B: 0.0015%, Al: 0.009%, N: 0.0052%, O: 0.0018%, the balance Fe and inevitable Steel made of impurities. The steel specimen made of boron steel is polished to a mirror surface, and then the mirror surface obtained by immersing and polishing in a solution of the above-mentioned corrosion solution at 63 ° C. is etched for 4 minutes to reveal the austenite grain boundaries of boron steel. I put it out. A photograph of the exposed etched surface taken at a magnification of 400 with a microscope is shown in FIG. 1A, and a photograph taken at a magnification of 1000 times is shown in FIG. As can be seen from these micrographs, the austenite grain boundaries of boron steel were clearly revealed without using the conventional boiling type.
これに対比して、比較例1として、上記の特許文献2に記載の炭素鋼あるいは低合金鋼鋳片の凝固組織のデンドライトを顕出する腐食液をボロン鋼の焼入材に適用しても好ましいオーステナイト結晶粒界が顕出できなかった。また本発明の腐食液とは組成を変えて比較例として効果を確認した。先ず、ピクリン酸を15g溶解し、これにライポンFなどの洗剤を10mlを加え、400mlの水に溶解して腐食液とした。次いで上記の腐食液を70℃の温水とした溶液に上記と同じ組成のボロン鋼の鋼試片を上記と同様に研磨して得た鏡面を浸漬して4分間エッチングして顕微鏡試片とした。この試片のエッチング面を顕微鏡で400倍にして撮影した写真を図2の(a)に、さらに1000倍にして撮影した写真を図2の(b)に示す。これらの顕微鏡写真に見られるように、この比較例の腐食液ではボロン鋼のオーステナイト結晶粒界は明瞭には顕出することはできなかった。 In contrast to this, as Comparative Example 1, the corrosive liquid that reveals the dendrite of the solidified structure of the carbon steel or low alloy steel slab described in Patent Document 2 is applied to the hardened material of boron steel. A preferred austenite grain boundary could not be revealed. Moreover, the effect was confirmed as a comparative example by changing the composition of the corrosive liquid of the present invention. First, 15 g of picric acid was dissolved, 10 ml of detergent such as Lipon F was added thereto, and dissolved in 400 ml of water to obtain a corrosive solution. Next, a mirror surface obtained by polishing a steel specimen of boron steel having the same composition as above to a solution in which the above corrosive solution was heated to 70 ° C. was immersed in the same manner as above and etched for 4 minutes to obtain a microscope specimen. . FIG. 2A shows a photograph taken at 400 times the etched surface of this specimen with a microscope, and FIG. 2B shows a photograph taken at a magnification of 1000 times. As can be seen from these micrographs, the austenite grain boundaries of boron steel could not be clearly revealed with the corrosion solution of this comparative example.
高炭素クロム軸受鋼であるSUJ2鋼の焼入材のオーステナイト結晶粒界を顕出するための本発明の腐食液は、実施例1と同様に、ピクリン酸20g、ライポンF30ml、ドデシルベンゼンスルフォン酸ナトリウム6gを水400mlに溶解してエッチング用の腐食液とした。 The corrosive liquid of the present invention for revealing the austenite grain boundaries of the hardened material of SUJ2 steel, which is a high carbon chromium bearing steel, is 20 g picric acid, 30 ml rypon F, sodium dodecylbenzene sulfonate as in Example 1. 6 g was dissolved in 400 ml of water to obtain a corrosive solution for etching.
この腐食液を適用する高炭素クロム軸受鋼であるSUJ2鋼は、例えば、質量%で、C:1.00%、Si:0.30%、Mn:0.25%、P:0.015%、S:0.015%、Cr:1.40%を含有し、残部Feおよび不可避不純物からなる鋼である。この高炭素クロム軸受鋼の焼入材からなる鋼試片を研磨して鏡面とし、次いで上記腐食液の65℃とした溶液に研磨して得た鏡面を40秒間浸漬してエッチングし、オーステナイト結晶粒界を顕出した。顕出したエッチング面を顕微鏡で1000倍にして撮影した写真を図3に示す。この顕微鏡写真に見られるとおり、高炭素クロム軸受鋼の焼入材のオーステナイト結晶粒界は明瞭に顕出された。 SUJ2 steel, which is a high carbon chromium bearing steel to which this corrosion solution is applied, is, for example, in mass%, C: 1.00%, Si: 0.30%, Mn: 0.25%, P: 0.015% , S: 0.015%, Cr: 1.40%, and the balance Fe and inevitable impurities. A steel specimen made of a hardened material of this high carbon chromium bearing steel is polished to a mirror surface, and then the mirror surface obtained by polishing in a solution of the above corrosive solution at 65 ° C. is immersed and etched for 40 seconds to obtain an austenite crystal. The grain boundary was revealed. A photograph of the exposed etched surface taken with a microscope at a magnification of 1000 is shown in FIG. As can be seen from this micrograph, the austenite grain boundaries of the hardened material of high carbon chromium bearing steel were clearly revealed.
これに対比して、上記の特許文献2に記載の炭素鋼あるいは低合金鋼鋳片の凝固組織のデンドライトを顕出する腐食液もボロン鋼の焼入材には適さなかったので、比較例1の腐食液でその効果を調べた。先ず、ピクリン酸を15g溶解し、これにライポンFなどの洗剤を10mlを加え、400mlの水に溶解して腐食液とした。次いで上記の腐食液を70℃の温水とした溶液に上記と同じ組成の高炭素クロム軸受鋼で焼入材からなる鋼試片を上記と同様に研磨し、得られた鏡面を浸漬して4分間エッチングして顕微鏡試片とした。この試片のエッチング面を顕微鏡で1000倍にして撮影した写真を図4に示す。この顕微鏡写真に見られるように、この腐食液では高炭素クロム軸受鋼の焼入材のオーステナイト結晶粒界は明瞭には顕出することはできなかった。 In contrast, the corrosive liquid that reveals the dendrite of the solidified structure of the carbon steel or low alloy steel slab described in Patent Document 2 is not suitable for the quenching material of boron steel. The effect was investigated with a corrosive solution. First, 15 g of picric acid was dissolved, 10 ml of detergent such as Lipon F was added thereto, and dissolved in 400 ml of water to obtain a corrosive solution. Next, a steel specimen made of a hardened material with a high carbon chromium bearing steel having the same composition as described above was polished in a solution in which the above corrosive solution was heated to 70 ° C. in the same manner as described above, and the obtained mirror surface was immersed in 4 Etching for a minute to obtain a microscope specimen. FIG. 4 shows a photograph of the etched surface of this specimen taken with a microscope at a magnification of 1000 times. As can be seen in this micrograph, the austenite grain boundaries of the hardened material of the high carbon chromium bearing steel could not be clearly revealed with this corrosion solution.
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CN108866549A (en) * | 2018-04-13 | 2018-11-23 | 河南中原特钢装备制造有限公司 | Austenite grain boundary corrosive agent and its preparation method and application method |
CN114018920A (en) * | 2021-10-29 | 2022-02-08 | 河南中原特钢装备制造有限公司 | Method for displaying delta ferrite in P91 and P92 steel |
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