JP5999549B2 - Wet developer for penetration flaw detection test and development method using the developer - Google Patents

Wet developer for penetration flaw detection test and development method using the developer Download PDF

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JP5999549B2
JP5999549B2 JP2012123642A JP2012123642A JP5999549B2 JP 5999549 B2 JP5999549 B2 JP 5999549B2 JP 2012123642 A JP2012123642 A JP 2012123642A JP 2012123642 A JP2012123642 A JP 2012123642A JP 5999549 B2 JP5999549 B2 JP 5999549B2
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津葉本 寿博
寿博 津葉本
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本発明は、自動車部材などの各種部材の表面に存在する微細な開口欠陥部の探傷に適用される浸透探傷試験に用いられる湿式現像剤及び該現像剤を使用した現像方法に関する。   The present invention relates to a wet developer used in a penetrant flaw detection test applied to flaw detection of fine opening defect portions existing on the surface of various members such as automobile members, and a developing method using the developer.

周知のとおり、非破壊検査方法の一種である「JIS Z 2343−1〜4」に規格化されている浸透探傷試験は、自動車部材(例えば、ピストンロッド)などの各種部材の表面に存在する微細な開口欠陥部(例えば、微細なクラックやピンホール)の探傷に汎用されており、その基本的態様は、当該JIS規格に示されているように、染色浸透液(通常、油溶性赤色染料を溶剤に溶解させた浸透性の強い液体が用いられる)を用いる方法又は蛍光浸透液(通常、紫外線灯:ブラックライト:照射下で黄緑色蛍光を発する油溶性蛍光染料を溶剤に溶解させた浸透性の強い液体が用いられる)を用いる方法がある。   As is well known, the penetrant flaw detection standardized in “JIS Z 234-1-4”, which is a kind of nondestructive inspection method, is a fine method that exists on the surface of various members such as automobile members (for example, piston rods). It is widely used for flaw detection of fine opening defects (for example, fine cracks and pinholes), and the basic mode is as shown in the JIS standard. A method using a highly penetrating liquid dissolved in a solvent or a fluorescent penetrating liquid (usually ultraviolet light: black light: penetrating oil-soluble fluorescent dye that emits yellow-green fluorescence under irradiation in a solvent) A strong liquid is used).

染色浸透液を用いる探傷試験方法では、染色浸透液を被検査物表面に付着させて開口欠陥部に浸透させた後、当該欠陥部内に浸透せずに被検査物表面に残留している余剰染色浸透液を除去し、次いで当該被検査物表面に炭酸マグネシウム粉末や炭酸カルシウム粉末などの無機質白色粉末を分散媒に分散させて界面活性剤を添加して製造した現像剤を塗布して、前記無機質白色粉末の薄層を形成して、該薄層によって開口欠陥部内に浸透している染色浸透液を薄層表面に吸い出させることによって欠陥指示模様を現出させ、自然光又は白色光の下で観察して当該欠陥指示模様によって開口欠陥部の存在・位置を探傷する。   In the flaw detection test method using the dye penetrant, after the dye penetrant is adhered to the surface of the object to be infiltrated and penetrated into the opening defect portion, the excess dye remaining on the surface of the object to be inspected without penetrating into the defect portion. After removing the penetrating liquid, and then applying a developer produced by dispersing an inorganic white powder such as magnesium carbonate powder or calcium carbonate powder in a dispersion medium and adding a surfactant to the surface of the object to be inspected. A thin layer of white powder is formed, and the defect indicating pattern is revealed by sucking the dye permeation solution penetrating into the opening defect portion by the thin layer to the surface of the thin layer, under natural light or white light. Observe and detect the presence / position of the opening defect by the defect indication pattern.

蛍光浸透液を用いる探傷試験方法では、蛍光浸透液を被検査物表面に付着させて開口欠陥部に浸透させた後、当該欠陥部に浸透せずに被検査物表面に残留している余剰蛍光浸透液を除去した後、前記現像剤を適用することなく、暗所において被検査物表面にブラックライトを照射して開口欠陥部内に残留している蛍光浸透液を黄緑色に発光させ該黄緑色の欠陥指示模様によって開口欠陥部の存在・位置を探傷する態様と、余剰浸透液を除去した後、前記染色浸透液を用いる場合と同様に現像剤を適用して開口欠陥部に残留している蛍光浸透液を薄層表面に吸い出させた後に暗所においてブラックライトを照射して、該薄層表面に吸い出されている蛍光浸透液を黄緑色に発光させ該黄緑色の欠陥指示模様によって開口欠陥部の存在・位置を探傷する態様とがあり、現像剤を適用する態様の方がより微細な開口欠陥部が探傷できる。   In the flaw detection test method using a fluorescent penetrating liquid, after attaching the fluorescent penetrating liquid to the surface of the inspection object and penetrating into the opening defect portion, the excess fluorescence remaining on the surface of the inspection object without penetrating the defect portion. After removing the penetrating liquid, without applying the developer, the surface of the object to be inspected is irradiated with black light in a dark place to cause the fluorescent penetrating liquid remaining in the opening defect portion to emit yellow-green light. The defect detection pattern is used to detect the presence / position of the opening defect portion, and after removing the excess permeation liquid, the developer is applied and remains in the opening defect portion in the same manner as in the case of using the dyeing permeation liquid. After the fluorescent penetrating liquid is sucked out on the surface of the thin layer, it is irradiated with black light in the dark, and the fluorescent penetrating liquid sucked out on the surface of the thin layer emits yellowish green, and the defect indication pattern of the yellowish green Detects the presence and position of opening defects That there is a manner, the developer can be more minute opening defect portion flaw better aspect to apply.

染色浸透液及び蛍光浸透液(以下単に『浸透液』ということがある)には、種々様々な処方の製品が市販・汎用されており、当業者において汎用されている市販品を、油溶性赤色染料(例えば、オイルレッド5B:商品名:オリエント株式会社やSudan Red 462:商品名:BASF社)及び油溶性蛍光染料(例えば、Fluorol 7GA:商品名:GAF社:やフロレッセントブライトニスエージェント68:商品名:日本化薬株式会社)を溶解している主溶剤によって大別すれば、水及び水と相溶する水溶性有機溶剤を主溶剤とする水ベース染色浸透液・水ベース蛍光浸透液と可燃性の非水溶性有機溶剤(通常、高沸点有機溶剤)を主溶剤とする油ベース染色浸透液・油ベース蛍光浸透液とに分類できる。なお、油ベース染色浸透液・油ベース蛍光浸透液には希釈溶剤(通常、揮発性低・中沸点有機溶剤)が配合されている。   For dyeing penetrants and fluorescent penetrants (hereinafter sometimes referred to simply as “penetrants”), products with a variety of prescriptions are commercially available and widely used, and those commercially used by those skilled in the art are oil-soluble red. Dye (for example, oil red 5B: trade name: Orient Corporation or Sudan Red 462: trade name: BASF) and oil-soluble fluorescent dye (for example, Fluorol 7GA: trade name: GAF: Fluorescent Bright Varnish Agent 68) : Product name: Nippon Kayaku Co., Ltd.), water-based dyeing penetrant / water-based fluorescent penetrant containing water and water-soluble organic solvent as main solvent And oil-based dyeing penetrants and oil-based fluorescent penetrants containing flammable water-insoluble organic solvents (usually high-boiling organic solvents) as main solvents. A dilution solvent (usually a volatile low / medium boiling organic solvent) is blended in the oil-based dyeing permeation solution and the oil-based fluorescent permeation solution.

油ベース染色浸透液・油ベース蛍光浸透液は、水ベース染色浸透液・水ベース蛍光浸透液と比べて、開口欠陥部に浸透した浸透液を過剰に除去することがないので、一般的には水ベース染色浸透液・水ベース蛍光浸透液よりも探傷精度が高く、微細な開口欠陥部を検出するために用いられているが、溶剤として有機溶剤を使用するため、消防法において取り扱いや貯蔵量の規制がある。   Oil-based dye penetrant / oil-based fluorescent penetrant generally does not remove the penetrant that has penetrated into the opening defect, compared to water-based dye penetrant / water-based fluorescent penetrant. It has higher flaw detection accuracy than water-based dyeing penetrants and water-based fluorescent penetrants, and is used to detect fine opening defects. There are regulations.

一方、水ベース染色浸透液・水ベース蛍光浸透液は、主溶剤が水と水溶性有機溶剤とを引火点を有しない割合にて混合されているので、消防法の規格を満たして取り扱いや貯蔵量の問題がない。そして、同じく分散媒が水であり引火点を有さない湿式現像剤で現像すれば、浸透探傷試験実施場所周辺の火気の使用に注意する必要がないので、水ベース浸透液と湿式現像剤との組み合わせは、自動車工場で汎用されており、また製鉄所でのスラブの探傷にも適している。   On the other hand, water-based dye penetrant and water-based fluorescent penetrants contain water and water-soluble organic solvents in a proportion that does not have a flash point. There is no problem of quantity. Similarly, if the dispersion medium is water and development is performed with a wet developer that does not have a flash point, there is no need to pay attention to the use of fire around the penetration test site. This combination is widely used in automobile factories and is suitable for flaw detection of slabs at steelworks.

しかし、前記湿式現像剤を使用する現像方法では、現像剤の分散媒が水であるため欠陥指示模様が時間の経過とともに大きく拡大されすぎる傾向がある。これは、水が乾燥するまでに時間がかかるため、湿式現像剤の粉末の隙間に染色浸透液・蛍光浸透液が浸透して広がりすぎるからである(以下この現象を本明細書中では『ニジミ』という)。   However, in the developing method using the wet developer, since the dispersion medium of the developer is water, the defect indicating pattern tends to be greatly enlarged as time passes. This is because it takes time for the water to dry, so that the dye penetrating solution / fluorescent penetrating solution permeates into the gaps of the powder of the wet developer and spreads too much. 』)).

ニジミの発生は探傷精度に悪影響を及ぼし、例えば2個の開口欠陥部が隣接する場合には、2つの欠陥指示模様として現出しても、時間の経過とともにニジミにより重なり合って1つの欠陥指示模様になってしまったり、開口欠陥部が線状である場合には、太い線状の欠陥指示模様として現出しても、時間の経過とともにニジミにより楕円形の欠陥指示模様になってしまったりする。このように時間の経過とともに欠陥指示模様の大きさや形が変化してしまうという問題点がある。   The occurrence of blemishes adversely affects the flaw detection accuracy. For example, when two opening defect portions are adjacent to each other, even if they appear as two defect indication patterns, they overlap with each other over time and become one defect indication pattern. If the opening defect portion is linear, even if it appears as a thick linear defect instruction pattern, it will become an elliptical defect instruction pattern due to blurring over time. As described above, there is a problem in that the size and shape of the defect indicating pattern changes with time.

また、一般的に使用される湿式現像剤に含有される無機質白色粉末の平均粒子径は約4μm未満の微細粉末であり、その含有量は約5〜15重量%であるが、被検査物が大形であったり、加熱できない材質であったり等の理由により、湿式現像剤の塗布後に被検査物を乾燥機で乾燥させることができないときには、エアブロー等で乾燥させているが、この場合乾燥時間を短縮するため湿式現像剤中の水分量を減少させ粉末含有量を約40〜60重量%まで増加させた現像剤が用いられている。   Moreover, the average particle diameter of the inorganic white powder contained in the commonly used wet developer is a fine powder of less than about 4 μm, and its content is about 5 to 15% by weight. When the object to be inspected cannot be dried with a dryer after applying the wet developer due to the large size or the material that cannot be heated, it is dried by air blow etc. In order to shorten the length of the developer, a developer in which the moisture content in the wet developer is reduced and the powder content is increased to about 40 to 60% by weight is used.

そして、粉末含有量が約40〜60重量%の現像剤の場合、一般的に使用されている平均粒子径が約4μm未満の微細粉末であると、粘度が上昇して均一な薄層が形成できず、厚くなりムラができて現像剤として機能しなくなるので、粉末含有量が多くても粘度が上昇しないように平均粒子径約4〜8μmの大きな粉末が用いられている。   In the case of a developer having a powder content of about 40 to 60% by weight, when the average particle size is generally used, it is a fine powder having a mean particle size of less than about 4 μm, and the viscosity increases and a uniform thin layer is formed. Since it cannot thicken and becomes uneven and does not function as a developer, a large powder having an average particle diameter of about 4 to 8 μm is used so that the viscosity does not increase even if the powder content is large.

しかし、粉末の平均粒子径が大きくなると粉末同士の隙間が大きくなり、開口欠陥部に残存した染色浸透液・蛍光浸透液が薄層中に吸い出される際、この大きな隙間に染色浸透液・蛍光浸透液が浸透するので、一般的な平均粒子径約4μm未満の微細粉末を使用した湿式現像剤と比較してさらにニジミが拡大し、開口欠陥部の正確な検出(探傷)が一層困難になるといった問題点がある。   However, as the average particle size of the powder increases, the gap between the powders increases, and when the staining penetrating solution / fluorescent penetrating solution remaining in the opening defect portion is sucked into the thin layer, the dyeing penetrating solution / fluorescent solution is absorbed into the large gap. Since the penetrating liquid penetrates, the blurring is further expanded as compared with a general wet developer using a fine powder having an average particle size of less than about 4 μm, and accurate detection (flaw detection) of an opening defect portion becomes more difficult. There is a problem.

本発明者は、前記諸問題点を解決することを技術的課題とし、試行錯誤的な数多くの試作・実験を重ねた結果、湿式現像剤であっても水溶性樹脂を添加することで、薄層に含まれる粉末の周囲に水溶性樹脂を存在させて、当該水溶性樹脂が開口欠陥部から隙間に浸透する染色浸透液・蛍光浸透液を取り込み固めるので欠陥指示模様のニジミが広がり過ぎず、かつ、水溶性樹脂の種類及び/又は添加量を選定して使用することでニジミの広がりを調節して、欠陥指示模様を所望の大きさに調整することができるという刮目すべき知見を得て、前記技術的課題を達成したものである。   The present inventor has made it a technical subject to solve the above-mentioned problems, and as a result of many trial and error trial manufactures and experiments, the inventors have added a water-soluble resin even if it is a wet developer. The presence of a water-soluble resin around the powder contained in the layer, and the water-soluble resin takes in and hardens the dye permeation solution / fluorescent permeation solution that penetrates into the gap from the opening defect portion, so the defect indication pattern blurring does not spread too much, In addition, we have obtained a remarkable knowledge that the defect indication pattern can be adjusted to a desired size by adjusting the spread of blistering by selecting and using the type and / or addition amount of the water-soluble resin. The technical problem has been achieved.

前記技術的課題は、次のとおり本発明によって解決できる。   The technical problem can be solved by the present invention as follows.

即ち、本発明は、水溶性樹脂が溶解している水に無機質白色粉末が分散している浸透探傷試験用湿式現像剤であって、前記現像剤における前記水溶性樹脂の含有量が0.1〜5重量%であり、前記無機質白色粉末の含有量が40〜60重量%であり、前記無機質白色粉末の平均粒子径が4〜8μmである浸透探傷試験用湿式現像剤である(請求項1)。 That is, the present invention is a wet developer for penetrant flaw testing in which an inorganic white powder is dispersed in water in which a water-soluble resin is dissolved, and the content of the water-soluble resin in the developer is 0.1 to 5 The wet developer for penetrant flaw detection, wherein the inorganic white powder content is 40% by weight to 60% by weight, and the inorganic white powder has an average particle size of 4 to 8 μm (Claim 1).

また、本発明は、前記水溶性樹脂が水溶性アクリル酸エステル系樹脂、水溶性カルボキシメチルセルロース樹脂及び水溶性ポリビニルアルコール樹脂から選択される1種以上である請求項1記載の浸透探傷試験用湿式現像剤である(請求項2)。 Further, the present invention provides the wet development for penetrant flaw detection test according to claim 1 , wherein the water-soluble resin is at least one selected from a water-soluble acrylic ester resin, a water-soluble carboxymethyl cellulose resin and a water-soluble polyvinyl alcohol resin. (Claim 2).

また、本発明は、前記無機質白色粉末が炭酸マグネシウム及び/又は炭酸カルシウムである請求項1又は2記載の浸透探傷試験用湿式現像剤である(請求項3)
また、本発明は、さらにノニオン系界面活性剤を添加することを特徴とする請求項1乃至3いずれか記載の浸透探傷試験用湿式現像剤である(請求項4)。
The present invention is the wet developer for penetrant flaw detection according to claim 1 or 2 , wherein the inorganic white powder is magnesium carbonate and / or calcium carbonate (claim 3) .
Further, the present invention provides the wet developer for penetrant flaw detection according to any one of claims 1 to 3, further comprising a nonionic surfactant (claim 4).

また、本発明は、請求項1乃至4いずれか記載の浸透探傷試験用湿式現像剤を使用することを特徴とする浸透探傷試験における現像方法である(請求項5)。 The present invention also relates to a developing method in a penetrant flaw detection test characterized in that the wet developer for penetrant flaw testing according to any one of claims 1 to 4 is used (claim 5).

また、本発明は、前記水溶性樹脂の含有量及び/又は種類を選定して使用することにより欠陥指示模様の大きさを調整する請求項5記載の浸透探傷試験における現像方法である(請求項6)。 Further, the present invention is a developing method in penetrant testing according to claim 5, wherein adjusting the size of the defect indication pattern by use selected content and / or type of the water-soluble resin (claim 6).

本発明は、水溶性樹脂が溶解している水に無機質白色粉末が分散していることを特徴とする浸透探傷試験用湿式現像剤であるので、粉末同士の隙間に水溶性樹脂が存在し、当該水溶性樹脂が、粉末同士の隙間に浸透する染色浸透液・蛍光浸透液を取り込み固めてニジミの過度な拡大を抑制するので、時間が経過しても欠陥指示模様の大きさや形が変化しにくくなり、開口欠陥部を正確に検出(探傷)することができる。   Since the present invention is a wet developer for penetrant flaw testing characterized in that an inorganic white powder is dispersed in water in which the water-soluble resin is dissolved, the water-soluble resin is present in the gap between the powders, The water-soluble resin takes in the dyeing and fluorescent penetrating liquids that penetrate into the gaps between the powders and hardens them to suppress the excessive expansion of the blisters, so the size and shape of the defect indication pattern changes over time. This makes it difficult to accurately detect (detect flaws) the opening defect portion.

また、本発明の湿式現像剤に添加する前記水溶性樹脂を0.1〜5重量%の範囲で変化させれば、ニジミの広がりを調節することができるので、例えば、目視による検出が容易な大きさであり、かつ、隣接する開口欠陥部の欠陥指示模様が重なり合うことがないといった所望の欠陥指示模様の大きさに調整することができる。   In addition, if the water-soluble resin added to the wet developer of the present invention is changed in the range of 0.1 to 5% by weight, the spread of blurring can be adjusted, so that, for example, visual detection is easy. It is possible to adjust the size of the defect indication pattern to a desired size so that the defect indication patterns of the adjacent opening defect portions do not overlap.

また、添加する水溶性樹脂が水溶性アクリル酸エステル系樹脂、水溶性カルボキシメチルセルロース樹脂、水溶性ポリビニルアルコール樹脂から選択される1種以上であれば、水に溶解しやすく、かつ、湿式現像剤自体の粘度を上昇させにくいので現像剤に添加しても均一な薄層を形成することができる。   Further, if the water-soluble resin to be added is at least one selected from water-soluble acrylic ester resins, water-soluble carboxymethyl cellulose resins, and water-soluble polyvinyl alcohol resins, it is easy to dissolve in water and the wet developer itself. Therefore, even if added to the developer, a uniform thin layer can be formed.

また、前記無機質白色粉末含有量が40〜60重量%、平均粒子径4〜8μmの粉末を用いた湿式現像剤は、粉末の平均粒子径が大きいため粒子間の隙間が大きくなってニジミが拡大しやすいが、水溶性樹脂が浸透する染色浸透液・蛍光浸透液を取り囲んで固めることでニジミの過度な拡大を抑制することができるので、開口欠陥部を正確に検出(探傷)することができる。   Further, the wet developer using the powder having the inorganic white powder content of 40 to 60% by weight and the average particle size of 4 to 8 μm has a large average particle size of the powder, so that the gap between the particles becomes large and the blurring is enlarged. However, it is possible to accurately detect (flaw detection) an opening defect because it is possible to suppress the excessive expansion of bleeding by surrounding and solidifying the dye penetrant / fluorescent penetrant into which the water-soluble resin penetrates. .

また、無機質白色粉末を白色度が高く速乾性に優れている炭酸マグネシウム及び/又は炭酸カルシウムとすることで均一な白色薄層が形成できるので、欠陥指示模様を明確に現出させることができ、開口欠陥部を正確に検出(探傷)することができる。   Moreover, since a uniform white thin layer can be formed by making the inorganic white powder magnesium carbonate and / or calcium carbonate having high whiteness and excellent quick drying properties, a defect indication pattern can be clearly revealed, An opening defect can be accurately detected (flaw detection).

さらに、本発明の湿式現像剤を使用した浸透探傷試験方法は、染色浸透液・蛍光浸透液のニジミの過度な拡大を抑制できるとともに、必要に応じて、湿式現像剤に含有させる水溶性樹脂の量及び/又は種類を選定して使用することによって欠陥指示模様を所望の大きさに調整することができる。   Furthermore, the penetrant flaw detection test method using the wet developer of the present invention can suppress the excessive expansion of the staining penetrant / fluorescent penetrant, and if necessary, the water-soluble resin contained in the wet developer. By selecting and using the quantity and / or type, the defect indicating pattern can be adjusted to a desired size.

加えて、本発明は、市販の染色浸透液・蛍光浸透液と組合せて用いることができるので、種々の大きさ及び深さの開口欠陥部の浸透探傷試験に使用することができる。   In addition, since the present invention can be used in combination with a commercially available dye penetrant / fluorescent penetrant, it can be used for penetrant testing of opening defects of various sizes and depths.

水溶性樹脂の添加に伴って、ほぼ円形状の欠陥指示模様の直径が小さくなることを示した図である。It is the figure which showed that the diameter of the substantially circular defect instruction pattern became small with addition of water-soluble resin.

本発明の実施の形態は次の通りである。   The embodiment of the present invention is as follows.

本発明の浸透探傷試験用湿式現像剤は、水に無機質白色粉末を分散させ、水溶性樹脂を添加して製造する。   The wet developer for penetrant flaw detection test of the present invention is produced by dispersing an inorganic white powder in water and adding a water-soluble resin.

本発明に使用する無機質白色粉末は特に限定されるものではないが、炭酸マグネシウム粉末、炭酸カルシウム粉末、無水ケイ酸粉末、含水ケイ酸粉末等を例として挙げることができる。特に炭酸マグネシウム粉末及び炭酸カルシウム粉末は白色度が高いため好適に用いることができる。   The inorganic white powder used in the present invention is not particularly limited, and examples thereof include magnesium carbonate powder, calcium carbonate powder, anhydrous silicic acid powder, and hydrous silicic acid powder. In particular, magnesium carbonate powder and calcium carbonate powder can be suitably used because of their high whiteness.

無機質白色粉末の平均粒子径は特に限定されるものではなく、一般的に使用されている平均粒子径が約4μm未満の微細粉末はもとより、粉末含有量が約40〜60重量%の場合に用いられている平均粒子径約4〜8μmの粉末も用いることができる。   The average particle size of the inorganic white powder is not particularly limited, and is used when the powder content is about 40 to 60% by weight as well as the fine powder generally used with an average particle size of less than about 4 μm. A powder having an average particle size of about 4 to 8 μm can also be used.

なお、粉末の平均粒子径が約8μmより大きくなると、現像剤の製造時や薄層形成時の分散性が悪くなる。   In addition, when the average particle diameter of the powder is larger than about 8 μm, the dispersibility at the time of producing the developer or forming the thin layer is deteriorated.

本発明における無機質白色粉末の含有量は5〜60重量%であり、好ましくは40〜60重量%である。5重量%より少なければ、現像剤の薄層が形成されない虞があり、また60重量%より多ければ、湿式現像剤の粘度が上昇して薄層とならずまたムラもできるので、いずれも現像剤として機能せず好ましくない。   The content of the inorganic white powder in the present invention is 5 to 60% by weight, preferably 40 to 60% by weight. If the amount is less than 5% by weight, a thin layer of the developer may not be formed. If the amount is more than 60% by weight, the viscosity of the wet developer increases, and the developer does not become a thin layer. It is not preferable because it does not function as an agent.

本発明における水溶性樹脂には、天然系、半合成系、合成系いずれの水溶性樹脂も使用することができるが、アクリル酸エステル系の水溶性ポリマーが好ましい。好ましいアクリル酸エステル系の水溶性ポリマーとしてはスチレンーアクリル酸エステル共重合樹脂、スチレン―アクリル酸エステル特殊共重合樹脂、スチレン−(メタ)−アクリル酸エステル共重合樹脂、酢酸ビニル−アクリル酸共重合樹脂、アクリル酸エステル共重合樹脂、アクリル酸エステル特殊共重合樹脂等を挙げることができる。   As the water-soluble resin in the present invention, any of natural, semi-synthetic and synthetic water-soluble resins can be used, but acrylate-based water-soluble polymers are preferred. Preferred acrylate-based water-soluble polymers include styrene-acrylate copolymer resins, styrene-acrylate ester special copolymer resins, styrene- (meth) -acrylate ester copolymer resins, and vinyl acetate-acrylic acid copolymers. Examples thereof include resins, acrylic ester copolymer resins, and acrylic ester special copolymer resins.

また、水溶性カルボキシメチルセルロース、水溶性ヒドロキシメチルセルロース等のセルロース系の半合成系水溶性樹脂、水溶性ポリビニルアルコール等の合成系水溶性樹脂も好適に用いることができる。   In addition, cellulose-based semi-synthetic water-soluble resins such as water-soluble carboxymethyl cellulose and water-soluble hydroxymethyl cellulose, and synthetic water-soluble resins such as water-soluble polyvinyl alcohol can also be suitably used.

水溶性樹脂の含有量は、0.1重量%以上が好ましく、さらに好ましいのは0.1〜5重量%である。0.1重量%未満であると粉末同士の隙間に浸透する浸透液を十分に吸収することができず、ニジミが広がりすぎる虞があり、また、5重量%より多く添加してもニジミの拡大に対する抑制効果に変化はなく、かつ、湿式現像剤の粘度が上昇すると均一な薄層を形成しにくくなるためいずれも好ましくない。   The content of the water-soluble resin is preferably 0.1% by weight or more, and more preferably 0.1 to 5% by weight. If it is less than 0.1% by weight, the penetrating liquid penetrating into the gaps between the powders cannot be sufficiently absorbed, and there is a possibility that the bleeding will spread too much. There is no change in the inhibitory effect on the toner, and when the viscosity of the wet developer increases, it becomes difficult to form a uniform thin layer, which is not preferable.

また、本発明には、無機質白色粉末を十分に分散させるため界面活性剤を添加することができる。添加する界面活性剤はノニオン系界面活性剤が好ましく、例として、ノイゲンXL−40,HLB:10.5(商品名:第一工業製薬株式会社)、ノイゲンLF−30X,HLB:9.4 (商品名:第一工業製薬株式会社)、ノイゲンDKS NL−60,HLB:11.5(商品名:第一工業製薬株式会社)を挙げることができる。界面活性剤の添加量は限定されないが、0.1〜3.0重量%が好ましく、より好ましくは0.5〜1.0重量%である。   In the present invention, a surfactant can be added to sufficiently disperse the inorganic white powder. The surfactant to be added is preferably a nonionic surfactant. For example, Neugen XL-40, HLB: 10.5 (trade name: Daiichi Kogyo Seiyaku Co., Ltd.), Neugen LF-30X, HLB: 9.4 ( Trade name: Daiichi Kogyo Seiyaku Co., Ltd.), Neugen DKS NL-60, HLB: 11.5 (trade name: Daiichi Kogyo Seiyaku Co., Ltd.). Although the addition amount of surfactant is not limited, 0.1 to 3.0 weight% is preferable, More preferably, it is 0.5 to 1.0 weight%.

(湿式現像剤の調製)
本実施の形態に係る浸透探傷試験用湿式現像剤の調製は容易であり、水をプロペラ式撹拌機を用いて撹拌しながら無機質白色粉末と界面活性剤を投入し、水溶性樹脂を添加した後、全体が均一になるまで撹拌して製造する。
(Preparation of wet developer)
Preparation of a wet developer for penetrant testing according to the present embodiment is easy, after adding an inorganic white powder and a surfactant while stirring water using a propeller-type stirrer, and adding a water-soluble resin Stir until the whole is uniform.

(浸透探傷試験方法)
本実施の形態に係る浸透探傷試験方法は、先ず、市販の浸透探傷試験用浸透液を被検査物表面に塗布して付着させて開口欠陥部に浸透させ(浸透処理)、次いで、当該被検査物表面を水圧:約0.1〜0.3Mpa・流量:1〜3L/minにて当該欠陥部内に浸透せずに被検査物表面に残っている余剰浸透液を洗浄・除去する(洗浄処理)。
(Penetration testing method)
In the penetrant testing method according to the present embodiment, first, a commercially available penetrant for penetrant testing is applied to the surface of an object to be inspected and permeated into an opening defect portion (penetration treatment). Washing / removing excess permeate remaining on the surface of the object without penetrating into the defective part at a water pressure of about 0.1 to 0.3 Mpa and a flow rate of 1 to 3 L / min (cleaning process) ).

エアブロー等により被検査物表面に残存する水滴を除去した後、湿式現像剤を塗布し、乾燥機やエアブローにて乾燥させて現像剤の薄層を形成する(現像処理)。   After removing water droplets remaining on the surface of the object to be inspected by air blow or the like, a wet developer is applied and dried by a dryer or air blow to form a thin layer of developer (development process).

開口欠陥部に残存していた浸透液は現像剤の薄層に吸い出されて欠陥指示模様を現出する。現出した指示模様の直径はノギスを使用して測定する。   The penetrating liquid remaining in the opening defect portion is sucked out by a thin layer of the developer and a defect indicating pattern appears. The diameter of the displayed indication pattern is measured using a caliper.

現出した欠陥指示模様のニジミが広がりすぎて、隣接する欠陥指示模様同士が重なり合うような場合には、水溶性樹脂の添加量及び/または種類を変更して適切な大きさとなるよう調整する。   In the case where the appearance of the defect indicating pattern appears to be too wide and the adjacent defect indicating patterns overlap each other, the amount and / or type of the water-soluble resin is changed and adjusted to an appropriate size.

水溶性樹脂の添加量及び/または種類を選定し、決定した後、同一の湿式現像剤を使用すれば、開口欠陥部の大きさ及び深さ等を比較して検出(探傷)することができる。   After selecting and determining the addition amount and / or type of the water-soluble resin, if the same wet developer is used, the size and depth of the opening defect can be compared (detected). .

(湿式現像剤の調製)
ガラス製ビーカーに所要量の水を充填してプロペラ式撹拌機を用いて300rpmで撹拌しながら所要量の界面活性剤(ノイゲンXL−40(HLB:10.5))と所要量の炭酸カルシウム白色粉末(平均粒子径6μm)を添加し、その後、所要量のスチレン−アクリル酸エステル共重合樹脂(ポリゾールSE−1420:商品名:昭和電工株式会社)を添加し、全体が均一になるまで撹拌を続けて湿式現像剤を製造した。また、水溶性樹脂を添加しない外は前記と同様にして製造した湿式現像剤を比較例とした。各添加量及び水の量は表1に記載したとおりである。
(Preparation of wet developer)
Fill a glass beaker with the required amount of water and stir at 300 rpm using a propeller-type stirrer with the required amount of surfactant (Neugen XL-40 (HLB: 10.5)) and the required amount of white calcium carbonate. Powder (average particle size 6 μm) is added, and then the required amount of styrene-acrylic ester copolymer resin (Polysol SE-1420: trade name: Showa Denko KK) is added and stirred until the whole becomes uniform. Subsequently, a wet developer was produced. Further, a wet developer produced in the same manner as described above except that no water-soluble resin was added was used as a comparative example. Each addition amount and the amount of water are as described in Table 1.

(欠陥指示模様の大きさの評価方法)
厚さ10mmのアルミ板に直径0.5mm、深さ5mmのドリルホールをあけた人工欠陥試験片を使用し、染色浸透液としてスーパーチェックP−LK(商品名:マークテック株式会社)を用い、人工欠陥試験片に刷毛にて塗布し、5分間浸透させた後、余剰染色浸透液を水圧150kPaにてスプレー洗浄により除去し、次いでエアブローにより人工欠陥試験片表面に付着している水滴を除去した後、湿式現像剤をスプレーガンによって人工欠陥試験片にスプレー塗布し、熱風循環式乾燥機で、70℃、5分間乾燥させて現れたほぼ円形状の欠陥指示模様の直径をノギスで測定した。
(Evaluation method of the size of defect indication pattern)
Using an artificial defect test piece having a drill hole with a diameter of 0.5 mm and a depth of 5 mm on an aluminum plate having a thickness of 10 mm, and using Super Check P-LK (trade name: Marktech Co., Ltd.) as a dyeing penetrant, After applying to the artificial defect test piece with a brush and infiltrating for 5 minutes, the excess dyeing permeate was removed by spray cleaning at a water pressure of 150 kPa, and then water droplets adhering to the surface of the artificial defect test piece were removed by air blowing. Thereafter, the wet developer was spray-applied to the artificial defect test piece with a spray gun, and the diameter of the substantially circular defect indicating pattern which appeared after drying at 70 ° C. for 5 minutes was measured with a caliper using a hot air circulation dryer.

上記操作を3回繰り返して測定したほぼ円形状の欠陥指示模様の直径の平均値を指示模様の大きさ(mm)として表1及び図1に示した。   Table 1 and FIG. 1 show the average value of the diameter of the substantially circular defect indicating pattern measured by repeating the above operation three times as the size (mm) of the indicating pattern.

なお、市販の浸透探傷試験用蛍光浸透液であるスーパーグローOD−18S(商品名:マークテック株式会社)を用いた場合には、前記(現像処理)後に、暗所におけるブラックライト照射下で現出した欠陥指示模様の直径をノギスにて測定する。   When Super Glow OD-18S (trade name: Marktec Co., Ltd.), which is a commercially available fluorescent penetrant for penetrant flaw detection test, was used, it was exposed to black light in a dark place after (development processing). Measure the diameter of the defect indication pattern with a caliper.

Figure 0005999549
Figure 0005999549

ポリゾールSE−1420を添加すれば、添加しない場合(比較例)と比べてほぼ円形状の欠陥指示模様の直径の平均値がいずれも小さくなっていることから、無機質白色粉末の平均粒子径が大きい場合においてもニジミの過度な拡大を抑制して、正確に開口欠陥部を検出(探傷)することができる。   If Polysol SE-1420 is added, the average particle diameter of the inorganic white powder is large because the average value of the diameter of the substantially circular defect indicating pattern is smaller than when not added (Comparative Example). Even in such a case, it is possible to accurately detect (detect flaws) the opening defect portion while suppressing the excessive expansion of bleeding.

さらに、ポリゾールSE−1420の添加量が0.1〜0.5重量%においては、添加量の増加に伴いほぼ円形状の欠陥指示模様の直径が小さくなっていることから、開口欠陥部の大きさによって水溶性樹脂の添加量を調節することで隣接する欠陥指示模様同士の重なりを抑制して、正確に開口欠陥部を検出(探傷)することができる。   Further, when the amount of polyzole SE-1420 added is 0.1 to 0.5% by weight, the diameter of the substantially circular defect indicating pattern becomes smaller with the increase in the amount added, so that the size of the opening defect portion is increased. By adjusting the addition amount of the water-soluble resin depending on the thickness, it is possible to suppress the overlapping of adjacent defect indicating patterns and accurately detect (detect flaws) the opening defect portion.

(水溶性樹脂の種類の比較)
水50ccと界面活性剤(ノイゲンXL−40(HLB:10.5))0.5gと炭酸カルシウム白色粉末(平均粒子径6μm)47.5gと各種水溶性樹脂2.0gを用い、前記と同様にして湿式現像剤を製造し、前記評価方法と同一の方法でほぼ円形状の欠陥指示模様の直径を3回測定し、平均値を指示模様の大きさ(mm)とした。
(Comparison of water-soluble resin types)
Same as above, using 50 cc of water, 0.5 g of surfactant (Neugen XL-40 (HLB: 10.5)), 47.5 g of calcium carbonate white powder (average particle size 6 μm), and 2.0 g of various water-soluble resins. The wet developer was manufactured, and the diameter of the substantially circular defect indicating pattern was measured three times by the same method as the evaluation method, and the average value was taken as the size (mm) of the indicating pattern.

使用した水溶性樹脂は、酢酸ビニル−アクリル酸エステル共重合樹脂(ポリゾールP−503:商品名:昭和電工株式会社)、アクリル酸エステル共重合樹脂(ポリゾールAM−200:商品名:昭和電工株式会社)、スチレン−アクリル酸エステル共重合樹脂(ポリゾールAM−610:商品名:昭和電工株式会社)、アクリル酸エステル特殊共重合樹脂(ポリゾールAE−710DF:商品名:昭和電工株式会社)、スチレン―(メタ)アクリル酸エステル共重合樹脂とポリエステル樹脂の混合物(ポリゾールFP−3000A:商品名:昭和電工株式会社)、スチレンーアクリル酸エステル特殊共重合樹脂(ポリゾールSE−1440:商品名:昭和電工株式会社)、カルボキシメチルセルロース(CMCダイセル1120:商品名:ダイセルファインケム株式会社)、ポリビニルアルコール(ゴセノールGL−03:商品名:日本合成化学工業株式会社)である。   The water-soluble resins used were vinyl acetate-acrylic ester copolymer resin (Polysol P-503: trade name: Showa Denko KK), acrylic ester copolymer resin (Polysol AM-200: trade name: Showa Denko KK). ), Styrene-acrylic acid ester copolymer resin (Polysol AM-610: trade name: Showa Denko KK), acrylic ester special copolymer resin (Polysol AE-710DF: trade name: Showa Denko KK), styrene ( A mixture of a meth) acrylic ester copolymer resin and a polyester resin (Polysol FP-3000A: trade name: Showa Denko KK), styrene-acrylic ester special copolymer resin (Polysol SE-1440: trade name: Showa Denko KK) ), Carboxymethyl cellulose (CMC Daicel 1120: trade name: Lee cell FineChem Co., Ltd.), polyvinyl alcohol (Gosenoru GL-03: product name: a Nippon Synthetic Chemical Industry Co., Ltd.).

結果を表2に示す。   The results are shown in Table 2.

Figure 0005999549
Figure 0005999549

水溶性樹脂を添加した湿式現像剤のほぼ円形状の欠陥指示模様の直径はいずれも比較例と比べて小さくなるので、無機質白色粉末の平均粒子径が大きい場合においてもニジミの過度な拡大を抑制し、隣接する欠陥指示模様の重なりを防いで正確に開口欠陥部を検出(探傷)することができる。   Since the diameter of the almost circular defect indication pattern of the wet developer with water-soluble resin is smaller than that of the comparative example, excessive spread of blurring is suppressed even when the average particle size of the inorganic white powder is large. In addition, it is possible to accurately detect (detect flaws) the opening defect portion by preventing overlapping of adjacent defect instruction patterns.

本発明に係る湿式現像剤は水溶性樹脂を添加することで、当該水溶性樹脂が開口欠陥部から現像剤の薄層中の粉末の隙間に浸透する浸透液を取り込み固めるので、欠陥指示模様のニジミが広がりすぎず、また、水溶性樹脂の種類及び/又は添加量によってニジミの広がりを調節して、欠陥指示模様を所望の大きさに調整することができ、正確に開口欠陥部の検出(探傷)ができるから、自動車会社や製鉄所等における浸透探傷試験用湿式現像剤に適しているので本発明の産業上の利用可能性は大きいといえる。
In the wet developer according to the present invention, by adding a water-soluble resin, the water-soluble resin takes in and solidifies the penetrating liquid that permeates into the gaps of the powder in the thin layer of the developer from the opening defect portion. It is possible to adjust the defect indication pattern to a desired size by adjusting the spread of the blur according to the type and / or addition amount of the water-soluble resin, and accurately detecting the opening defect portion ( Therefore, it can be said that the present invention has great industrial applicability because it is suitable for a wet developer for penetrant flaw testing in automobile companies and steelworks.

Claims (6)

水溶性樹脂が溶解している水に無機質白色粉末が分散している浸透探傷試験用湿式現像剤であって、前記現像剤における前記水溶性樹脂の含有量が0.1〜5重量%であり、前記無機質白色粉末の含有量が40〜60重量%であり、前記無機質白色粉末の平均粒子径が4〜8μmである浸透探傷試験用湿式現像剤A wet developer for penetrant flaw detection in which an inorganic white powder is dispersed in water in which a water-soluble resin is dissolved , wherein the content of the water-soluble resin in the developer is 0.1 to 5% by weight, A wet developer for penetrant flaw testing, wherein the content of the inorganic white powder is 40 to 60% by weight, and the average particle size of the inorganic white powder is 4 to 8 μm . 前記水溶性樹脂が水溶性アクリル酸エステル系樹脂、水溶性カルボキシメチルセルロース樹脂及び水溶性ポリビニルアルコール樹脂から選択される1種以上である請求項1記載の浸透探傷試験用湿式現像剤。 2. The wet developer for penetrant flaw detection test according to claim 1, wherein the water-soluble resin is at least one selected from a water-soluble acrylic ester resin, a water-soluble carboxymethyl cellulose resin, and a water-soluble polyvinyl alcohol resin. 前記無機質白色粉末が炭酸マグネシウム及び/又は炭酸カルシウムである請求項1又は2記載の浸透探傷試験用湿式現像剤。 3. The wet developer for penetration flaw detection test according to claim 1 , wherein the inorganic white powder is magnesium carbonate and / or calcium carbonate. さらにノニオン系界面活性剤を添加することを特徴とする請求項1乃至3いずれか記載の浸透探傷試験用湿式現像剤。4. The wet developer for penetrant flaw detection according to any one of claims 1 to 3, further comprising a nonionic surfactant. 請求項1乃至4いずれか記載の浸透探傷試験用湿式現像剤を使用することを特徴とする浸透探傷試験における現像方法。 5. A developing method in a penetrant flaw test using the wet developer for penetrant flaw test according to any one of claims 1 to 4 . 前記水溶性樹脂の含有量及び/又は種類を選定して使用することにより欠陥指示模様の大きさを調整する請求項5記載の浸透探傷試験における現像方法。 6. The developing method in the penetrant flaw detection test according to claim 5, wherein the size of the defect indicating pattern is adjusted by selecting and using the content and / or type of the water-soluble resin.
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