JP2008216058A - Surface inspection method of magnesium containing material - Google Patents

Surface inspection method of magnesium containing material Download PDF

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JP2008216058A
JP2008216058A JP2007054243A JP2007054243A JP2008216058A JP 2008216058 A JP2008216058 A JP 2008216058A JP 2007054243 A JP2007054243 A JP 2007054243A JP 2007054243 A JP2007054243 A JP 2007054243A JP 2008216058 A JP2008216058 A JP 2008216058A
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magnesium
containing material
color
compound
inspection method
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Katsuyuki Iijima
勝之 飯島
Hironobu Nakanishi
裕信 中西
Masanori Ikeda
昌則 池田
Shinsuke Murao
伸介 村尾
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Kobe Steel Ltd
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Kobe Steel Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a surface inspection method of a magnesium containing material capable of visually recognizing even a minute defect without using an expensive machine. <P>SOLUTION: A magnesium color coupler which reacts with magnesium or magnesium compound and colors is made to react with magnesium or magnesium compound existing in a surface of the magnesium containing material, thereby selectively coloring the magnesium color coupler. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明は、マグネシウムを含むアルミニウム合金等のマグネシウム含有材の表面検査方法に関する。   The present invention relates to a surface inspection method for a magnesium-containing material such as an aluminum alloy containing magnesium.

近年、アルミニウム合金に対する品質要求は非常に高度になってきている。その中でも、特に、マグネシウムを含むアルミ合金圧延材（以下、「Ｍｇ／Ａｌ合金」と略す）は品質要求が最も厳しいものの一つである。一般的なＭｇ／Ａｌ合金の品質不良の原因の一つに表面欠陥がある。表面欠陥としては、ひっかき傷、穴、ふくらみ、異物の付着などがその例として挙げられる。Ｍｇ／Ａｌ合金のこすれによって生じたひっかき傷などのマクロな欠陥は、光沢の違いから目視にて発見することができる。しかし、目視で発見できる傷は少ない。そこで、ミクロな欠陥を発見するために、被検査物に光を当ててその反射光を受光手段で受け取って表面欠陥の有無を機械的に測定する方法が提案されている。   In recent years, quality requirements for aluminum alloys have become very high. Among them, in particular, an aluminum alloy rolled material containing magnesium (hereinafter abbreviated as “Mg / Al alloy”) is one of the strictest quality requirements. One of the causes of poor quality of general Mg / Al alloys is surface defects. Examples of surface defects include scratches, holes, bulges, and adhesion of foreign matter. Macro defects such as scratches caused by rubbing the Mg / Al alloy can be found visually from the difference in gloss. However, few scratches can be found visually. Therefore, in order to find a micro defect, a method has been proposed in which light is applied to an object to be inspected, its reflected light is received by a light receiving means, and the presence or absence of a surface defect is mechanically measured.

また、アルマイト処理による表面欠陥を検査する方法も行われている。アルマイト処理とは、Ａｌ合金を硫酸浴中で陽極酸化させることにより表面に光沢を付与する処理であるが、表面欠陥を有するＭｇ／Ａｌ合金をアルマイト処理すると、欠陥部分と非欠陥部分とで異なる光沢を目視で確認できるため、表面欠陥の検査方法として、特にＡｌ合金製造現場で広く行われている。しかし、アルマイト処理は高電圧や硫酸等の酸性物質が必要であるため、取り扱いが容易でない。さらに、欠陥部分と非欠陥部分の光沢の違いが非常に小さくわかりにくいため、区別できるようになるためには長年の経験が必要である。そこで、特許文献１には、アルマイト処理を行ったＡｌ合金の光沢の読みとりを簡便に行うために、被検査物に光をあて、その反射光を受光手段で感知し、感知した光を波長別に分類してその強度と反射面積などを数値化し、波長別に分類した前記数値をヒストグラム化し、理論正規分布式を利用した演算処理を行うことにより、表面欠陥の有無を判断し、表面欠陥の数、面積などと前記反射面積などとの関連づけにより、表面欠陥レベルを判断するＡｌ板の表面欠陥自動検査法が提案されている。
特開平９−１０１２６５号公報 In addition, a method for inspecting surface defects by anodizing is also performed. Alumite treatment is a treatment that imparts gloss to the surface by anodizing an Al alloy in a sulfuric acid bath. However, when an alumite treatment is performed on a Mg / Al alloy having surface defects, it differs between a defective portion and a non-defect portion. Since the gloss can be visually confirmed, it is widely used as an inspection method for surface defects, particularly at an Al alloy manufacturing site. However, alumite treatment is not easy to handle because it requires an acidic substance such as high voltage or sulfuric acid. Furthermore, since the difference in gloss between the defective part and the non-defective part is very small and difficult to understand, many years of experience are required to be able to distinguish them. Therefore, in Patent Document 1, in order to easily read the gloss of an Al alloy that has been anodized, light is applied to the object to be inspected, the reflected light is detected by a light receiving means, and the detected light is classified by wavelength. By classifying and quantifying the intensity and reflection area, etc., by making a histogram of the numerical values classified according to wavelength, by performing arithmetic processing using the theoretical normal distribution formula, determine the presence or absence of surface defects, the number of surface defects, An automatic inspection method for surface defects of an Al plate for determining the surface defect level by associating the area and the like with the reflection area has been proposed.
JP-A-9-101265

しかしながら、非欠陥部分との色彩の相違が少ない場合が多く、欠陥部と非欠陥部の判別が困難である。また、比較的高価な機械を用いる必要があるか、または微小な傷を発見することができない問題があった。   However, there are many cases where the color difference from the non-defect portion is small, and it is difficult to distinguish between the defect portion and the non-defect portion. In addition, there is a problem that it is necessary to use a relatively expensive machine or a minute scratch cannot be found.

そこで、本発明の課題は、マグネシウム含有材の表面欠陥を、アルマイト処理等の処理を行うことなく、しかも高価な機械を用いることなく微小な欠陥でも目視で発見することができるマグネシウム含有材の表面検査方法を提供することにある。   Therefore, the problem of the present invention is that the surface of the magnesium-containing material can be found by visual inspection even for a minute defect without using an alumite treatment or the like, and without using an expensive machine. To provide an inspection method.

前記課題を解決するために、請求項１に係る発明は、マグネシウム含有材の表面検査方法であって、マグネシウムまたはマグネシウム化合物と反応して発色するマグネシウム発色剤を、前記マグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させて、前記マグネシウム発色剤を選択的に発色させる工程を含むことを特徴とする。   In order to solve the above-mentioned problem, the invention according to claim 1 is a surface inspection method for a magnesium-containing material, wherein a magnesium color former that reacts with magnesium or a magnesium compound and develops color is present on the surface of the magnesium-containing material. And a step of selectively developing the magnesium color former by reacting with magnesium or a magnesium compound.

このマグネシウム含有材の表面検査方法では、マグネシウムまたはマグネシウム化合物と反応して発色するマグネシウム発色剤を、マグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させて、マグネシウム発色剤を選択的に発色させることによって、マグネシウム含有材の表面欠陥を目視で発見することができる。   In this magnesium-containing material surface inspection method, a magnesium color former that reacts with magnesium or a magnesium compound and reacts with magnesium or a magnesium compound present on the surface of the magnesium-containing material to selectively color the magnesium colorant. By making it, the surface defect of a magnesium containing material can be discovered visually.

請求項２に係る発明は、前記のマグネシウム含有材の表面検査方法において、前記マグネシウム発色剤を含む検査液を前記マグネシウム含有材の表面に塗布して、前記マグネシウム発色剤を前記マグネシウムまたはマグネシウム化合物と反応させることを特徴とする。   According to a second aspect of the present invention, in the surface inspection method for a magnesium-containing material, a test liquid containing the magnesium color former is applied to a surface of the magnesium-containing material, and the magnesium color former is combined with the magnesium or the magnesium compound. It is made to react.

このマグネシウム含有材の表面検査方法では、マグネシウム発色剤を含む検査液をマグネシウム含有材の表面に塗布して、マグネシウム発色剤をマグネシウムまたはマグネシウム化合物と反応させて、マグネシウム発色剤を選択的に発色させることによって、マグネシウム含有材の表面欠陥を目視で発見することができる。   In this surface inspection method for a magnesium-containing material, a test solution containing a magnesium color former is applied to the surface of the magnesium-containing material, and the magnesium color former is reacted with magnesium or a magnesium compound to selectively color the magnesium color former. By this, the surface defect of a magnesium containing material can be discovered visually.

請求項３に係る発明は、前記のマグネシウム含有材の表面検査方法において、前記マグネシウム発色剤を含む検査液を含浸した担体を前記マグネシウム含有材に接触させることによって、前記マグネシウム発色剤を前記マグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させることを特徴とする。   According to a third aspect of the present invention, in the method for inspecting a surface of a magnesium-containing material, the magnesium colorant is contained in the magnesium-containing material by bringing the carrier impregnated with the test solution containing the magnesium colorant into contact with the magnesium-containing material. It is characterized by reacting with magnesium or a magnesium compound present on the surface of the material.

このマグネシウム含有材の表面検査方法では、マグネシウム発色剤を含む検査液を含浸した担体をマグネシウム含有材に接触させることによって、マグネシウム発色剤をマグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させて、マグネシウム発色剤を選択的に発色させることによって、マグネシウム含有材の表面欠陥を目視で発見することができる。   In this magnesium-containing material surface inspection method, a carrier impregnated with a test solution containing a magnesium color former is brought into contact with the magnesium-containing material, so that the magnesium color former reacts with magnesium or a magnesium compound present on the surface of the magnesium-containing material. Thus, the surface defects of the magnesium-containing material can be visually found by selectively coloring the magnesium color former.

請求項４に係る発明は、前記のマグネシウム含有材の表面検査方法において、前記マグネシウムまたはマグネシウム化合物と反応して発色した前記マグネシウム発色剤を、被転写体に転写することを特徴とする。   The invention according to claim 4 is characterized in that, in the method for inspecting a surface of a magnesium-containing material, the magnesium color-developing agent that has developed color by reacting with the magnesium or the magnesium compound is transferred to a transfer target.

このマグネシウム含有材の表面検査方法では、マグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応して発色したマグネシウム発色剤を、被転写体に転写することによって、発色したマグネシウム発色剤の色を確認するとともに、色を保存することが可能となる。   In this surface inspection method for a magnesium-containing material, the color of the magnesium colorant developed by transferring the magnesium colorant that has developed color by reacting with the magnesium or the magnesium compound present on the surface of the magnesium-containing material to the transfer target. It is possible to check and save the color.

請求項５に係る発明は、前記のマグネシウム含有材の表面検査方法において、発色した前記マグネシウム発色剤の色を色差計を用いて測定することを特徴とする。   The invention according to claim 5 is characterized in that, in the surface inspection method for a magnesium-containing material, the color of the colored magnesium color former is measured using a color difference meter.

このマグネシウム含有材の表面検査方法では、発色した前記マグネシウム発色剤の色を色差計を用いて測定することによって、より定量的に色の相違を判別して明確に表面欠陥を発見することが可能となる。   In this surface inspection method for magnesium-containing materials, the color of the developed magnesium color former can be measured using a color difference meter, so that the color difference can be distinguished more quantitatively and surface defects can be clearly found. It becomes.

請求項６に係る発明は、前記のマグネシウム含有材の表面検査方法において、表面にマグネシウム金属またはマグネシウム化合物が存在する前記マグネシウム含有材の表面の一部を除去した後、前記マグネシウム発色剤を含む検査液を、前記マグネシウム含有材と接触させることを特徴とする。   The invention according to claim 6 is the above-described method for inspecting a surface of a magnesium-containing material, wherein the magnesium colorant is removed after removing a part of the surface of the magnesium-containing material in which magnesium metal or a magnesium compound is present. A liquid is brought into contact with the magnesium-containing material.

このマグネシウム含有材の表面検査方法では、マグネシウム含有材の表面の一部を除去（図３の状態を図４の状態にする）した後、マグネシウム発色剤を含む検査液を、前記マグネシウム含有材と接触させてマグネシウム発色剤の発色の有無によって、表面にMgが偏析している部分の一部にのみ欠陥がある場合に、欠陥部分をわかりやすくすることも可能である。   In this magnesium-containing material surface inspection method, after removing a part of the surface of the magnesium-containing material (the state of FIG. 3 is changed to the state of FIG. 4), a test solution containing a magnesium color former is used as the magnesium-containing material. Depending on the presence or absence of coloration of the magnesium color former, it is possible to make the defective portion easy to understand when there is a defect only in a part of the portion where Mg is segregated on the surface.

請求項７に係る発明は、前記のマグネシウム含有材の表面検査方法において、前記マグネシウム含有材が、アルミニウム合金圧延材からなるものであることを特徴とする。   The invention according to claim 7 is characterized in that, in the surface inspection method for a magnesium-containing material, the magnesium-containing material is made of a rolled aluminum alloy material.

このマグネシウム含有材の表面検査方法は、マグネシウムを含有するアルミニウム合金に適用して、表面欠陥を目視によって発見することができる。   This surface inspection method for a magnesium-containing material can be applied to an aluminum alloy containing magnesium to detect surface defects visually.

請求項８に係る発明は、前記のマグネシウム含有材の表面検査方法において、前記マグネシウム発色剤がアゾ化合物であることを特徴とする。特に、前記マグネシウム発色剤が、下記式（１）で表される化合物であることが好ましい。

Figure 2008216058
The invention according to claim 8 is characterized in that, in the surface inspection method for a magnesium-containing material, the magnesium color former is an azo compound. In particular, the magnesium color former is preferably a compound represented by the following formula (1).
Figure 2008216058

このマグネシウム含有材の表面検査方法では、マグネシウム発色剤として、アゾ化合物、特に、前記式（１）で表される化合物が好適である。   In this method for inspecting a surface of a magnesium-containing material, an azo compound, particularly a compound represented by the formula (1) is suitable as a magnesium color former.

本発明の方法によれば、マグネシウムまたはマグネシウム化合物が表面に存在するマグネシウム含有材の表面欠陥を、高価な機器を使うことなく、目視で検査することができる。特に、Ｍｇ／Ａｌ合金に適用して、表面欠陥の有無を検査する方法として好適である。   According to the method of the present invention, a surface defect of a magnesium-containing material in which magnesium or a magnesium compound is present can be visually inspected without using an expensive device. In particular, it is suitable as a method for inspecting for the presence or absence of surface defects by applying to Mg / Al alloys.

以下、本発明のマグネシウム含有材の表面検査方法（以下、「本発明の方法」という）について詳細に説明する。   The magnesium-containing material surface inspection method of the present invention (hereinafter referred to as “the method of the present invention”) will be described in detail below.

本発明の方法は、マグネシウムまたはマグネシウム化合物と反応して発色するマグネシウム発色剤を、前記マグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させて、前記マグネシウム発色剤を選択的に発色させることによって、マグネシウム含有材の表面を検査する方法である。   According to the method of the present invention, a magnesium color former that reacts with magnesium or a magnesium compound and reacts with magnesium or a magnesium compound present on the surface of the magnesium-containing material to selectively develop the magnesium color former. This is a method for inspecting the surface of a magnesium-containing material.

本発明において、マグネシウム含有材とは、マグネシウムを必須成分とし、他の成分を含む合金材、または表面にマグネシウムメッキがなされた材である。その中でも、特に、Ｍｇ／Ａｌ合金に適用して、表面欠陥を検査する場合に好適である。本発明の方法を適用するＭｇ／Ａｌ合金はマグネシウムを含むアルミニウム合金であれば、特に限定されない。例えば、本発明の方法は、ＪＩＳに規定される２０００系、３０００系、４０００系、５０００系、６０００系、７０００系等のマグネシウムを含むアルミニウム合金に適用が可能である。   In the present invention, the magnesium-containing material is an alloy material containing magnesium as an essential component and containing other components, or a material having a surface plated with magnesium. Among them, it is particularly suitable when applied to Mg / Al alloy and inspecting surface defects. The Mg / Al alloy to which the method of the present invention is applied is not particularly limited as long as it is an aluminum alloy containing magnesium. For example, the method of the present invention can be applied to 2000-series, 3000-series, 4000-series, 5000-series, 6000-series, 7000-series aluminum alloys containing magnesium specified by JIS.

本発明の方法において、マグネシウム発色剤をマグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させる方法は、マグネシウム発色剤とマグネシウムまたはマグネシウム化合物と接触させて反応させることが可能な方法であれば、いずれの方法でもよい。例えば、前記マグネシウム発色剤を含む検査液をマグネシウム含有材の表面に塗布する方法、前記マグネシウム発色剤を含む検査液を含浸した担体を前記マグネシウム含有材に接触させる方法、例えば検査液を吸収させた布でマグネシウム含有材の表面を覆うなどによって、マグネシウム発色剤をマグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させることができる。   In the method of the present invention, the method of reacting the magnesium color former with magnesium or a magnesium compound present on the surface of the magnesium-containing material may be any method that allows the magnesium color former and the magnesium or magnesium compound to react with each other. Any method may be used. For example, a method of applying a test liquid containing the magnesium color former on the surface of the magnesium-containing material, a method of contacting a carrier impregnated with the test liquid containing the magnesium color developer, and the test liquid absorbed, for example, The magnesium color former can be reacted with magnesium or a magnesium compound present on the surface of the magnesium-containing material, such as by covering the surface of the magnesium-containing material with a cloth.

マグネシウム発色剤を含む検査液をマグネシウム含有材の表面に塗布する場合には、刷毛やバーコーターを用いて、マグネシウム含有材の表面に検査液を均一にのばすことが好ましい。また、マグネシウム発色剤を含む検査液を含浸した担体を前記マグネシウム含有材に接触させる場合には、金属不純物の少ない素材からなる担体を用いることが好ましい。例えば、合成繊維等からなる布、不織布などが挙げられる。具体的には、旭化成せんい（株）から市販されているキュプラ不織布（ビスコースレーヨン不織布）ＢＥＭＣＯＴ（商品名）シリーズなどを用いることができる。金属不純物が多い担体を用いると、マグネシウム発色剤を含む検査液を担体に含浸させた場合にマグネシウム発色剤が発色する虞があるためである。   When applying a test solution containing a magnesium color former to the surface of the magnesium-containing material, it is preferable to uniformly extend the test solution to the surface of the magnesium-containing material using a brush or a bar coater. In the case where a carrier impregnated with a test solution containing a magnesium color former is brought into contact with the magnesium-containing material, it is preferable to use a carrier made of a material with few metal impurities. For example, a cloth or a non-woven fabric made of synthetic fiber or the like can be used. Specifically, a cupra nonwoven fabric (viscose rayon nonwoven fabric) BEMCOT (trade name) series and the like commercially available from Asahi Kasei Fibers Corporation can be used. This is because if a carrier with a large amount of metal impurities is used, the magnesium color former may develop color when the carrier is impregnated with a test solution containing a magnesium color former.

また、マグネシウム含有材の表面で発色したマグネシウム発色剤を被転写体に転写して、発色した色を長期的に保存することが可能である。被転写体としては、前記金属不純物の少ない素材からなる担体を用いることが好ましい。金属不純物が多い素材を用いると、転写させた場合に色が変化してしまう虞があるためである。   In addition, it is possible to store the color that has developed on the surface of the magnesium-containing material by transferring the color developer that has developed on the surface of the magnesium-containing material to the transfer target. As the material to be transferred, it is preferable to use a carrier made of a material with few metal impurities. This is because if a material with many metal impurities is used, the color may change when transferred.

マグネシウム発色剤を含む検査液は、マグネシウム発色剤およびその発色剤を溶解するための溶媒、さらに、必要に応じて助剤等を含む。   The test solution containing a magnesium color former includes a magnesium color former, a solvent for dissolving the color former, and an auxiliary agent as necessary.

マグネシウム発色剤としては、Ｍｇ金属やＭｇ化合物とだけ反応する薬剤であるか、もしくはＭｇ金属やＭｇ化合物と反応して示す色と下地であるＡｌおよびＡｌ化合物と反応して示す色が異なる薬剤であれば特に限定されない。例えば、アゾ化合物などを用いることができる。特に、アゾ化合物の中でも、前記式（１）で表されるSodium 1-azo-2-hydroxy-3-(2,4-dimethylcarboxanilido)-naphthalene-1’-(2-hydroxybenzene-5-sulfonate)（以下、「ＸＢＩ」と略す）が好ましい。また、フタロシアニン、エリオクロムブラックＴ、チモールフタレインコンプレクソン、メチルチモールブルーなどを用いることができる。   The magnesium color former is an agent that reacts only with Mg metal or Mg compound, or an agent that reacts with Mg metal or Mg compound and has a different color when reacted with Al or Al compound as a base. If there is no particular limitation. For example, an azo compound can be used. In particular, among azo compounds, sodium 1-azo-2-hydroxy-3- (2,4-dimethylcarboxanilido) -naphthalene-1 ′-(2-hydroxybenzene-5-sulfonate) represented by the above formula (1) ( Hereinafter, it is abbreviated as “XBI”). Further, phthalocyanine, eriochrome black T, thymolphthalein complexone, methylthymol blue and the like can be used.

検査液におけるマグネシウム発色剤の濃度は、０．００１質量％〜１質量％の範囲である。マグネシウム発色剤の濃度が０．００１質量％未満では濃度が低すぎる為に発色の確認ができない。一方、１質量％よりも高くなると、発色の程度に変化が見られないため、これ以上添加することは非経済的である。   The concentration of the magnesium color former in the test solution is in the range of 0.001% by mass to 1% by mass. If the concentration of the magnesium color former is less than 0.001% by mass, the color development cannot be confirmed because the concentration is too low. On the other hand, when the content is higher than 1% by mass, no change is observed in the degree of color development, so it is uneconomical to add more.

溶媒としては、水、アルコール、炭化水素系溶媒など特に発色剤および場合によっては助剤を溶かす事が可能な溶媒であれば特に限定されない。アルコールや炭化水素系溶媒の例としては、メチルアルコール、エチルアルコール、１−プロパノール、２−プロパノール、ペンタン、ヘキサン、ヘプタン、オクタン、ノナン、デカン、ベンゼン、トルエン、ジメチルスルホキシド、シクロヘキサン、シクロオクタン、ジクロロベンゼン、ジエチルエーテル、ジメチルエーテル、酢酸メチル、酢酸エチル、酢酸などを用いることができる。   The solvent is not particularly limited as long as it is a solvent capable of dissolving a color former and, in some cases, an auxiliary agent, such as water, alcohol, and a hydrocarbon solvent. Examples of alcohols and hydrocarbon solvents include methyl alcohol, ethyl alcohol, 1-propanol, 2-propanol, pentane, hexane, heptane, octane, nonane, decane, benzene, toluene, dimethyl sulfoxide, cyclohexane, cyclooctane, di Chlorobenzene, diethyl ether, dimethyl ether, methyl acetate, ethyl acetate, acetic acid and the like can be used.

溶媒の濃度は、９９．９９９質量％〜４０質量％の範囲で使用することができる。９９．９９９質量％を超えると、溶解されるマグネシウム発色剤の濃度が低くなるため発色の確認ができない。一方、４０質量％未満では、マグネシウム発色剤を十分に溶解させるには量が少なすぎる。   The concentration of the solvent can be used in the range of 99.999 mass% to 40 mass%. If it exceeds 99.999% by mass, the concentration of the magnesium color former to be dissolved becomes low, and color development cannot be confirmed. On the other hand, if it is less than 40% by mass, the amount is too small to sufficiently dissolve the magnesium color former.

また、助剤としては、検査液の粘性を調整し板に塗布しやすくするための増粘剤、溶媒中へのマグネシウム発色剤の溶解を促進するための界面活性剤、ｐＨ調整剤としての酸やアルカリ溶液などを用いることができる。増粘剤としては、三洋化成製メルポールＦ−２２０・ＰＥＧシリーズ（ＰＥＧ−２００，−３００，−４００，−６００等：商品名）、住友精化製ＰＥＯシリーズ（ＰＥＯ−１，−３，−８，−１５，−１８：商品名）ヒドロキシエチルセルロースなどが挙げられる。増粘剤の濃度は、用いる増粘剤の種類、粘度に合わせて使用することが可能である。例えば、０質量％〜３０質量％、より好ましくは１質量％〜１５質量％の範囲で使用することが好ましい。これは、増粘剤は用いなくても発色による傷の発見は可能であるが、１質量％〜１５質量％の間で添加すると適度な粘性を持つようになる為塗布しやすくなるが、粘性が高くなりすぎると、検査液をマグネシウム含有材の表面に塗布する事が困難となる虞があるため３０質量％以内とするのが好ましい。また、界面活性剤としては、ポリオキシエチレンイソオクチルフェニルエーテルなどを用いることができる。用いる界面活性剤の濃度としては、０質量％〜１質量％の範囲である。これは、１質量％より多く添加しても、効果が変わらないためである。   The auxiliary agent includes a thickener for adjusting the viscosity of the test solution and facilitating application to the plate, a surfactant for promoting the dissolution of the magnesium color former in the solvent, and an acid as a pH adjuster. Or an alkaline solution can be used. As a thickener, Sanyo Chemical's Melpol F-220 / PEG series (PEG-200, -300, -400, -600, etc .: trade name), Sumitomo Seika PEO series (PEO-1, -3,- 8, -15, -18: trade name) hydroxyethyl cellulose and the like. The concentration of the thickener can be used according to the type and viscosity of the thickener used. For example, it is preferably used in the range of 0% by mass to 30% by mass, more preferably 1% by mass to 15% by mass. Although it is possible to detect scratches due to color development without using a thickener, it becomes easy to apply when added between 1% by mass and 15% by mass. If it becomes too high, it may be difficult to apply the test solution to the surface of the magnesium-containing material. As the surfactant, polyoxyethylene isooctyl phenyl ether or the like can be used. The concentration of the surfactant used is in the range of 0% by mass to 1% by mass. This is because the effect does not change even if it is added in an amount of more than 1% by mass.

また、発色剤の中には色の変化を示すｐＨ域が限られているものがあるため、ｐＨ調整剤として酸・アルカリを使用できる。ｐＨ調整剤としては、特に限定されないが、塩酸、硫酸、酢酸、硝酸、水酸化ナトリウム、水酸化カリウム、炭酸ナトリウム、炭酸カリウムなどを用いることができる。用いる酸またはアルカリ溶液の濃度は、０質量％〜３０質量％の範囲である。酸やアルカリは用いなくてもよい場合もあるが、３０質量％を超える濃度にしても効果が変わらないため、経済的に使用する意味はない。   Further, since some color formers have a limited pH range showing a color change, acids and alkalis can be used as pH adjusters. Although it does not specifically limit as a pH adjuster, Hydrochloric acid, a sulfuric acid, an acetic acid, nitric acid, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate etc. can be used. The concentration of the acid or alkali solution to be used is in the range of 0% by mass to 30% by mass. Acid or alkali may not be used in some cases, but even if the concentration exceeds 30% by mass, the effect does not change, so there is no point in using it economically.

発色したマグネシウム発色剤の色は、目視にて色の変化を観測することが可能である。また、カメラやその他の機材を用いて観察することも可能である。さらに、定量的に色の違いを判断するためには、色差計を用いて測定することが好ましい。   The color change of the developed magnesium color former can be visually observed. It is also possible to observe using a camera or other equipment. Further, in order to quantitatively determine the color difference, it is preferable to measure using a color difference meter.

本発明の方法において、マグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と、マグネシウム発色剤との反応によって、マグネシウム発色剤を発色させて、マグネシウム含有材の表面欠陥を発見できる理由は、以下のように考えられる。
。 In the method of the present invention, the reason that the magnesium color former can be colored by the reaction of magnesium or a magnesium compound present on the surface of the magnesium-containing material with the magnesium color former to detect the surface defects of the magnesium-containing material is as follows. I think so.
.

一般に、Ｍｇ／Ａｌ合金は加熱処理されると、表面に合金含有成分が偏析することが知られている。例えば、Ｍｇ／Ａｌ合金が熱延工程時に高温のロールで延ばされると、表面には多くのＭｇが偏析すると言われている。参考文献（Applications of Surface Science,17,344(1984)）によると、特に、図１に示すように、ＭｇＯに代表されるＭｇ化合物部１で表面が占有されていると考えられている。そのため、同状態の合金表面部分に傷がついた場合、図２に示すように、ＭｇＯに代表されるＭｇ化合物部１が削られ、非Ｍｇ化合物部分２が露出する場合がある。そこで、Ｍｇ化合物部１にのみ選択的に発色する発色剤を添加すると、Ｍｇ化合物部１は色が変わり、非Ｍｇ化合物部２は色が変わらないことからキズ部分を目視で発見することが可能となる。   In general, it is known that when an Mg / Al alloy is heat-treated, alloy-containing components are segregated on the surface. For example, it is said that when Mg / Al alloy is stretched by a high-temperature roll during the hot rolling process, a large amount of Mg is segregated on the surface. According to the reference (Applications of Surface Science, 17, 344 (1984)), it is considered that the surface is occupied by the Mg compound portion 1 represented by MgO, as shown in FIG. Therefore, when the alloy surface portion in the same state is damaged, as shown in FIG. 2, the Mg compound portion 1 represented by MgO may be scraped and the non-Mg compound portion 2 may be exposed. Therefore, if a color former that selectively develops color is added only to the Mg compound part 1, the color of the Mg compound part 1 changes and the color of the non-Mg compound part 2 does not change, so it is possible to visually detect the scratched part. It becomes.

しかしながら、傷が付いた場合にＭｇ化合物部１が全て除去されるのでは無く、図３に示すように、一部のみ除去される程度の傷Ｄが付く場合も考えられる。この状態のＭｇ／Ａｌ合金３にＭｇ金属やＭｇ化合物と反応して発色するマグネシウム発色剤を含む検査液を塗布すると、ＭｇＯが厚い部分４は色が大きく変わり、ＭｇＯが薄い部分５は色の変わりが少なくなるため、特にＭｇＯが薄い部分５のエッチングを行わずとも色の違いにより目視で区別することが可能である。また、図４に示すように、表面のＭｇ化合物部１の一部を酸やアルカリによって均一にエッチングした後に発色剤を塗布することにより、よりはっきりとキズ部分６を発見することも可能である。さらに、図５に示すように、下地のＭｇ／Ａｌ合金３まで深いキズ７が付いた場合でも、Ｍｇ化合物部１とＭｇ／Ａｌ合金３ではＭｇ濃度が異なるため、キズ７を目視で発見することが可能となる。   However, when the scratch is attached, not all of the Mg compound portion 1 is removed, but as shown in FIG. When a test solution containing a magnesium color former that reacts with Mg metal or a Mg compound is applied to the Mg / Al alloy 3 in this state, the color of the thick MgO portion 4 changes greatly, and the thin MgO portion 5 changes the color. Since the change is reduced, it is possible to visually distinguish by the difference in color without performing etching of the portion 5 where MgO is particularly thin. Moreover, as shown in FIG. 4, it is also possible to discover the flaw part 6 more clearly by applying a color former after etching a part of the Mg compound part 1 on the surface uniformly with acid or alkali. . Further, as shown in FIG. 5, even when deep scratches 7 are formed up to the underlying Mg / Al alloy 3, the Mg compound portion 1 and the Mg / Al alloy 3 have different Mg concentrations. It becomes possible.

一方、本発明の方法では、図６に示すように、Ｍｇ化合物８が一部だけ特異的に膨らんでいる部分８ａがある場合にも適用できる。これは、マグネシウム発色剤を含む検査液を塗布した場合、膨らみの部分８ａはＭｇ化合物濃度が高いため、その他の部分よりも色が濃く変色することで確認できる。また、膨らみの程度が小さく、色の濃淡の差が小さい場合には、図７に示すように、表面層のＭｇ化合物の一部を均一にエッチングして、非Ｍｇ化合物部２を露出させた後でマグネシウム発色剤を含む検査液を塗布することにより、よりはっきりとふくらみ部分を目視で区別することが可能である。
ミクロな欠陥の場合であっても発色剤により、中間的色に着色され、欠陥を判別する事は可能である。例えば、ミクロな欠陥部を持つ材にマグネシウム発色剤を塗布したときに、ミクロな欠陥部が青くミクロな非欠陥部が赤くなった場合、全体的には青紫色に見える。この時、欠陥部が無い材に発色剤を塗布した時の色と比べると青みがかった色に見えるため、ミクロな欠陥部があるかどうかを判別することができる。 On the other hand, as shown in FIG. 6, the method of the present invention can also be applied to the case where there is a portion 8a in which only a part of the Mg compound 8 swells specifically. This can be confirmed by applying a test solution containing a magnesium color former, because the swollen portion 8a has a higher Mg compound concentration, and thus the color changes darker than other portions. Further, when the degree of swelling is small and the difference in color shading is small, as shown in FIG. 7, a part of the Mg compound on the surface layer is uniformly etched to expose the non-Mg compound part 2. By subsequently applying a test solution containing a magnesium color former, it is possible to visually distinguish the bulging portion more clearly.
Even in the case of a micro defect, it is colored in an intermediate color by the color former and it is possible to determine the defect. For example, when a magnesium color former is applied to a material having a micro defect portion, if the micro defect portion is blue and the micro non-defect portion is red, the whole appears blue-purple. At this time, since the color looks bluish compared to the color when the color former is applied to a material having no defect, it is possible to determine whether there is a micro defect.

実施例１
ＸＢＩ０．１ｇとエタノール１００ｇの混合溶液、およびＮａ２ＣＯ３１０．６ｇと水１８９．４ｇの混合溶液をそれぞれ作製した。ＸＢＩとエタノールの混合溶液６０ｍｌと、Ｎａ２ＣＯ３の混合溶液１００ｍｌとを混合して検査液を調製した。この検査液のｐＨは１２であり、液の色は青紫色を示した。 Example 1
A mixed solution of 0.1 g of XBI and 100 g of ethanol, and a mixed solution of 10.6 g of Na 2 CO 3 and 189.4 g of water were prepared. A test solution was prepared by mixing 60 ml of a mixed solution of XBI and ethanol and 100 ml of a mixed solution of Na 2 CO 3 . The pH of this test solution was 12, and the color of the solution showed a bluish purple color.

予め硫酸浴を用いてアルマイト処理を行った結果、色調が異なった部分が観測されたＭｇ／Ａｌ合金材と同一のロットから採取したＭｇ／Ａｌ合金材の試料片（大きさ：３０ｍｍ×２１００ｍｍ×５ｍｍ）の表面に、前記検査液１５０ｍｌを塗布して、キュプラ不織布（旭化成せんい（株）製、ＢＥＭＣＯＴ（ＴＲ−７Ｆ））の上に載置した。６０秒経過後、検査液の色が青紫色から濃い赤紫色に変化した。色差計（ミノルタ（株）製、ＣＲ−２００）でL*a*b*表色系で測定したところ、ａ＊値は２５を示した。なお、目視では全体が赤みがかった色に見えた。 As a result of alumite treatment using a sulfuric acid bath in advance, a specimen of Mg / Al alloy material (size: 30 mm × 2100 mm ×) taken from the same lot as the Mg / Al alloy material in which a portion having a different color tone was observed On the surface of 5 mm), 150 ml of the test solution was applied and placed on a cupra non-woven fabric (BEMCOT (TR-7F) manufactured by Asahi Kasei Fibers Co., Ltd.). After 60 seconds, the color of the test solution changed from blue purple to deep red purple. When measured with a color difference meter (Minolta, CR-200) in the L * a * b * color system, the a * value was 25. In addition, visually, the whole looked reddish.

一方、予め硫酸浴を用いてアルマイト処理を行った結果、色調が異なった部分が観測されなかったＭｇ／Ａｌ合金材と同一のロットから採取したＭｇ／Ａｌ合金材の試料片（大きさ：８００ｍｍ×８００ｍｍ×５ｍｍ）の表面に、前記と同様に、検査液を塗布して、６０秒経過後の検査液の色差を測定したところ、ａ＊値は２１を示した。目視では、[0042] 色調が異なった部分が観測されたＭｇ／Ａｌ合金材に比べて赤みが薄く、少し青紫がかってみえた。   On the other hand, as a result of alumite treatment using a sulfuric acid bath in advance, a sample piece of Mg / Al alloy material (size: 800 mm) taken from the same lot as the Mg / Al alloy material in which a portion having a different color tone was not observed. As described above, the test solution was applied to the surface of × 800 mm × 5 mm), and the color difference of the test solution after 60 seconds was measured. As a result, the a * value was 21. Visually, [0042] The redness was lighter than that of the Mg / Al alloy material in which a portion having a different color tone was observed.

これらの結果から、アルマイト処理で色調が異なった部分が観測されたＭｇ／Ａｌ合金と、色調が異なった部分が観測されなかったＭｇ／Ａｌ合金とを、発色の違いにより目視（目視および色差計での測定）で区別できることが分かった。   From these results, the Mg / Al alloy in which a portion with a different color tone was observed by anodizing and the Mg / Al alloy in which a portion with a different color tone was not observed were visually observed (visual and color difference meter). It was found that it can be distinguished by measurement in

実施例２
ＸＢＩ０．１ｇとエタノール１００ｇの混合溶液、およびＮａ２ＣＯ３５．３ｇと水９４．７ｇの混合溶液をそれぞれ作製した。ＸＢＩとエタノールの混合溶液３ｍｌと、Ｎａ２ＣＯ３の混合溶液５ｍｌとを混合して検査液を調製した。この検査液のｐＨは１２であり、液の色は青紫色を示した。 Example 2
A mixed solution of 0.1 g of XBI and 100 g of ethanol, and a mixed solution of 5.3 g of Na 2 CO 3 and 94.7 g of water were prepared. A test solution was prepared by mixing 3 ml of a mixed solution of XBI and ethanol and 5 ml of a mixed solution of Na 2 CO 3 . The pH of this test solution was 12, and the color of the solution showed a bluish purple color.

１０質量％塩酸に１０分間浸して表面に存在するＭｇの一部をあらかじめ除去して、下地のアルミニウムの一部を露出させたＭｇコーティング材（大きさ：３０ｍｍ×４０ｍｍ×２ｍｍ、アセトンにより脱脂済み、表面に５００ÅのＭｇ膜を持つアルミニウム材）の表面に、前記の検査液１ｍｌを滴下した。次に、バーコーターを用いて、液厚が１μｍになるように、Ｍｇコーティング材の表面に検査液を均一に展開した。６０秒経過後、塩酸によりＭｇを除去してアルミニウムを露出させた部分は青紫色のままで色は変わらず、その他の部分は濃い赤紫色に発色したことが目視で確認できた。   Mg coating material (size: 30 mm x 40 mm x 2 mm, degreased with acetone) in which a part of Mg existing on the surface is removed beforehand by dipping in 10% by mass hydrochloric acid for 10 minutes to expose a part of the underlying aluminum 1 ml of the above test solution was dropped on the surface of an aluminum material having a 500-mm Mg film on the surface. Next, using a bar coater, the test liquid was uniformly spread on the surface of the Mg coating material so that the liquid thickness was 1 μm. After 60 seconds, it was confirmed by visual observation that the portion where the aluminum was exposed by removing Mg with hydrochloric acid remained blue-purple and the color did not change, and the other portions were colored deep red-purple.

キュプラ不織布（旭化成せんい（株）製、ＢＥＭＣＯＴ（ＴＲ−７Ｆ））を、Ｍｇコーティング材の表面で発色した検査液に押し当て、検査液を不織布に吸収させた。不織布に吸収された検査液の色差を色差計（ミノルタ（株）製、ＣＲ−２００）でL*a*b*表色系で測定したところ、濃い赤紫色に発色した部分はａ＊＝３０であり、青紫色の部分はａ＊＝１０であった。これによって、色の違いを色差計により判別することが可能であることが分かった。 A cupra nonwoven fabric (BEMCOT (TR-7F) manufactured by Asahi Kasei Fibers Co., Ltd.) was pressed against the test solution colored on the surface of the Mg coating material, and the test solution was absorbed into the nonwoven fabric. When the color difference of the test solution absorbed by the non-woven fabric was measured with a color difference meter (CR-200, manufactured by Minolta Co., Ltd.) in the L * a * b * color system, the portion colored in deep reddish purple was a * = 30 The blue-violet part was a * = 10. As a result, it has been found that the color difference can be discriminated by a color difference meter.

実施例３
ＸＢＩ０．１ｇとエタノール１００ｇの混合溶液と、Ｎａ２ＣＯ３５．３ｇと水９４．７ｇの混合溶液をそれぞれ作製した。ＸＢＩとエタノールの混合溶液３ｍｌと、Ｎａ２ＣＯ３の混合溶液５ｍｌとを混合して検査液を調製した。この検査液のｐＨは１２であり、液の色は青紫色を示した。 Example 3
A mixed solution of 0.1 g of XBI and 100 g of ethanol and a mixed solution of 5.3 g of Na 2 CO 3 and 94.7 g of water were prepared. A test solution was prepared by mixing 3 ml of a mixed solution of XBI and ethanol and 5 ml of a mixed solution of Na 2 CO 3 . The pH of this test solution was 12, and the color of the solution showed a bluish purple color.

前記の検査液１ｍｌを含浸させたキュプラ不織布（旭化成せんい（株）製、ＢＥＭＣＯＴ（ＴＲ−７Ｆ））を、１０質量％塩酸に浸して表面に存在するＭｇの一部をあらかじめ除去して、下地のアルミニウムの一部を露出させたＭｇコーティング材（大きさ：３０ｍｍ×４０ｍｍ×２ｍｍ、アセトンにより脱脂済み）の表面に載せた。６０秒経過後、Ｍｇコーティング材の表面に載せた不織布のうち、塩酸によりエッチングした部分に接触した部分は青紫色のままで色は変わらず、その他の部分は濃い赤紫色に発色したことが目視で確認できた。   A cupra nonwoven fabric impregnated with 1 ml of the above test solution (Asahi Kasei Fibers Co., Ltd., BEMCOT (TR-7F)) is immersed in 10% by mass hydrochloric acid to remove a part of Mg existing on the surface in advance. The aluminum coating was exposed on the surface of a Mg coating material (size: 30 mm × 40 mm × 2 mm, degreased with acetone). After 60 seconds, the non-woven fabric placed on the surface of the Mg coating material was in contact with the portion etched with hydrochloric acid, and the color did not change and the other portions were colored deep red purple. I was able to confirm.

発色した不織布の表面の色を色差計（ミノルタ（株）製、ＣＲ−２００）で測定したところ、濃い赤紫色部分はａ＊＝３０となり、青紫色部分はａ＊＝１０となった。これによって、色の違いを色差計により判別することが可能であることが分かった。   When the color of the surface of the developed nonwoven fabric was measured with a color difference meter (CR-200, manufactured by Minolta Co., Ltd.), the dark red-purple portion was a * = 30 and the blue-purple portion was a * = 10. As a result, it has been found that the color difference can be discriminated by a color difference meter.

熱延工程後のＭｇ／Ａｌ合金の表面におけるＭｇの偏析を示す概念図である。It is a conceptual diagram which shows the segregation of Mg in the surface of the Mg / Al alloy after a hot rolling process. Ｍｇ／Ａｌ合金の表面における非Ｍｇ化合物部の露出を示す概念図である。It is a conceptual diagram which shows the exposure of the non-Mg compound part in the surface of Mg / Al alloy. Ｍｇ／Ａｌ合金の表面の一部に傷が付いた状態を示す概念図である。It is a conceptual diagram which shows the state where a part of surface of Mg / Al alloy was damaged. Ｍｇ／Ａｌ合金の表面のＭｇ化合物の一部を均一にエッチングした状態を示す概念図である。It is a conceptual diagram which shows the state which etched a part of Mg compound of the surface of Mg / Al alloy uniformly. Ｍｇ／Ａｌ合金のＭｇ／Ａｌ合金部まで深いキズが付いた状態を示す概念図である。It is a conceptual diagram which shows the state with the deep flaw to the Mg / Al alloy part of Mg / Al alloy. Ｍｇ／Ａｌ合金において、Ｍｇ化合物が一部だけ特異的に膨らんでいる場合を示す概念図である。In Mg / Al alloy, it is a conceptual diagram which shows the case where only a part of Mg compound is swollen. 表面層のＭｇ化合物の一部を均一にエッチングして、非Ｍｇ化合物部を露出させた状態を示す概念図である。It is a conceptual diagram which shows the state which etched a part of Mg compound of the surface layer uniformly, and exposed the non-Mg compound part.

符号の説明Explanation of symbols

１ Ｍｇ化合物部
２ 非Ｍｇ化合物部
３ Ｍｇ／Ａｌ合金 1 Mg compound part 2 Non-Mg compound part 3 Mg / Al alloy

Claims (9)

マグネシウム含有材の表面検査方法であって、
マグネシウムまたはマグネシウム化合物と反応して発色するマグネシウム発色剤を、前記マグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させて、前記マグネシウム発色剤を選択的に発色させる工程を含むことを特徴とするマグネシウム含有材の表面検査方法。 A surface inspection method for a magnesium-containing material,
Including a step of reacting magnesium or a magnesium compound that reacts with magnesium or a magnesium compound to react with magnesium or a magnesium compound present on the surface of the magnesium-containing material to selectively color the magnesium colorant. A surface inspection method for magnesium-containing materials. 前記マグネシウム発色剤を含む検査液を前記マグネシウム含有材の表面に塗布して、前記マグネシウム発色剤を前記マグネシウムまたはマグネシウム化合物と反応させることを特徴とする請求項１に記載のマグネシウム含有材の表面検査方法。   2. The surface inspection of a magnesium-containing material according to claim 1, wherein a test liquid containing the magnesium color former is applied to a surface of the magnesium-containing material, and the magnesium color former is reacted with the magnesium or the magnesium compound. Method. 前記マグネシウム発色剤を含む検査液を含浸した担体を前記マグネシウム含有材に接触させることによって、前記マグネシウム発色剤を前記マグネシウム含有材の表面に存在するマグネシウムまたはマグネシウム化合物と反応させることを特徴とする請求項１に記載のマグネシウム含有材の表面検査方法。   The magnesium color former is reacted with magnesium or a magnesium compound present on the surface of the magnesium-containing material by bringing a carrier impregnated with a test solution containing the magnesium color former into contact with the magnesium-containing material. Item 8. A method for inspecting a surface of a magnesium-containing material according to Item 1. 前記マグネシウムまたはマグネシウム化合物と反応して発色した前記マグネシウム発色剤を、被転写体に転写することを特徴とする請求項１〜請求項３のいずれか１項に記載のマグネシウム含有材の表面検査方法。   The surface inspection method for a magnesium-containing material according to any one of claims 1 to 3, wherein the magnesium color-developing agent that has developed color by reacting with the magnesium or the magnesium compound is transferred to a transfer target. . 発色した前記マグネシウム発色剤の色を色差計を用いて測定することを特徴とする請求項１〜請求項４のいずれか１項に記載のマグネシウム含有材の表面検査方法。   The surface inspection method for a magnesium-containing material according to any one of claims 1 to 4, wherein the color of the magnesium color former that has developed color is measured using a color difference meter. 表面にマグネシウム金属またはマグネシウム化合物が存在する前記マグネシウム含有材の表面の一部を除去した後、前記マグネシウム発色剤を含む検査液を、前記マグネシウム含有材と接触させることを特徴とする請求項１〜請求項５のいずれか１項に記載のマグネシウム含有材の表面検査方法。   The test liquid containing the magnesium color former is brought into contact with the magnesium-containing material after removing a part of the surface of the magnesium-containing material in which magnesium metal or a magnesium compound is present on the surface. The surface inspection method of the magnesium containing material of any one of Claim 5. 前記マグネシウム含有材が、アルミニウム圧延材からなるものであることを特徴とする請求項１〜請求項６のいずれか１項に記載のマグネシウム含有材の表面検査方法。   The said magnesium containing material consists of aluminum rolling materials, The surface inspection method of the magnesium containing material of any one of Claims 1-6 characterized by the above-mentioned. 前記マグネシウム発色剤がアゾ化合物であることを特徴とする請求項１〜請求項７のいずれか１項に記載のマグネシウム含有材の表面検査方法。   The surface inspection method for a magnesium-containing material according to any one of claims 1 to 7, wherein the magnesium color former is an azo compound. 前記マグネシウム発色剤が、下記式（１）で表される化合物であることを特徴とする請求項１〜請求項７のいずれか１項に記載のマグネシウム含有材の表面検査方法。
Figure 2008216058
 The said magnesium color former is a compound represented by following formula (1), The surface inspection method of the magnesium containing material of any one of Claims 1-7 characterized by the above-mentioned.
Figure 2008216058
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