JP4277715B2 - Method for inspecting adhesion between rubber and adherend - Google Patents
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Description
本発明は、非破壊的に行われる、ゴムと被着体との間の接着検査方法に関するものである。 The present invention relates to a method for inspecting adhesion between rubber and an adherend, which is performed nondestructively.
従来より、構造体の内部の状態を非破壊的に検査する方法として、Ｘ線を利用した検査方法が知られている（例えば、特許文献１参照）。 Conventionally, an inspection method using X-rays is known as a method for nondestructively inspecting the internal state of a structure (for example, see Patent Document 1).
例えば、ゴムシートと樹脂シートとを接着剤で接着したシート状構造体の接着状態を、上記検査方法により検査する場合には、上記接着剤として、鉛化合物が含有されているものを使用する。すなわち、上記構造体にＸ線を照射して、接着剤に含有されている鉛化合物から発生する特性Ｘ線を検出器により検出し、Ｘ線による検出像を得、その検出像から接着剤の存在状態を検査する。例えば、上記検出像が樹脂シート側に入り込んでいると、樹脂層に割れが発生していると判断でき、また、その検出像がゴムシート等の表面に沿わずに湾曲していると、ゴムシートと樹脂シートとが剥離していると判断できる。
しかしながら、上記鉛化合物は、環境問題から、その使用を避けることが望まれている。 However, it is desired to avoid the use of the lead compound due to environmental problems.
そこで、本発明者らは、上記鉛化合物に代わるものについて、鋭意研究を重ねた結果、亜鉛化合物が適しているのではないかと想起した。そして、これについて、さらに鋭意研究を重ねた結果、つぎのような知見を得た。すなわち、一般に市販されている亜鉛化合物含有接着剤を単にそのまま使用した場合には、Ｘ線による検出像が不明瞭となり、接着剤の存在状態を充分な精度で検査することができない。その原因は、亜鉛の含有量が少なく、Ｘ線の検出強度が弱いことにある。そこで、上記知見に基づき、さらに研究を重ねた結果、上記接着剤に亜鉛化合物を単に添加しただけでは、Ｘ線の亜鉛に対する検出強度は強まるものの、添加量によっては、両者間の接着力が弱まったり、検査精度の充分な向上効果が得られないことを突き止めた。 Thus, as a result of intensive research on alternatives to the lead compounds, the present inventors have recalled that zinc compounds may be suitable. As a result of further earnest research on this, the following findings were obtained. That is, when a commercially available zinc compound-containing adhesive is simply used as it is, the detection image by X-rays becomes unclear, and the presence state of the adhesive cannot be inspected with sufficient accuracy. The cause is that the zinc content is low and the X-ray detection intensity is weak. Therefore, as a result of further research based on the above findings, simply adding a zinc compound to the adhesive increases the detection strength against X-ray zinc, but depending on the amount added, the adhesive strength between the two is weak. It was found that the effect of improving the inspection accuracy could not be obtained.
本発明は、このような事情に鑑みなされたもので、ゴム用の接着剤として、亜鉛化合物が含有された接着剤を使用し、しかも、ゴムと被着体との間の接着力を弱めることなく、その接着状態のＸ線による検査を充分な精度で行うことができる、ゴムと被着体との間の接着検査方法の提供をその目的とする。 The present invention has been made in view of such circumstances, and uses an adhesive containing a zinc compound as an adhesive for rubber, and further weakens the adhesive force between the rubber and the adherend. It is another object of the present invention to provide a method for inspecting the adhesion between a rubber and an adherend, which can inspect the adhesion state with X-rays with sufficient accuracy.
上記の目的を達成するため、本発明のゴムと被着体との間の接着検査方法は、ゴムと被着体とを接着剤で接着した構造体の接着状態を、接着剤中にＸ線で検出することができるＸ線検出物質を含有させ、Ｘ線による上記Ｘ線検出物質含有接着剤の存在状態を示す検出像から検査する方法であって、上記Ｘ線検出物質として亜鉛化合物を選択し、接着剤中の亜鉛含有量を、ＥＰＭＡにより分析した亜鉛検出量が２３〜３５重量％となるように設定し、上記Ｘ線を上記構造体の側面から上記接着剤の層に沿って照射し、上記検出像として線状の検出像を得、その得られた線状検出像の湾曲状態または線の太さの変化度合いを基準にし、ゴムと被着体との接着状態を検査するという構成をとる。 In order to achieve the above object, the method for inspecting adhesion between a rubber and an adherend according to the present invention is based on an X-ray analysis of an adhesive state of a structure obtained by adhering a rubber and an adherend with an adhesive. A method for inspecting from a detection image showing the presence state of the X-ray detection substance- containing adhesive by X-rays, which contains an X-ray detection substance that can be detected by X-ray, wherein a zinc compound is selected as the X-ray detection substance Then, the zinc content in the adhesive is set so that the detected amount of zinc analyzed by EPMA is 23 to 35% by weight, and the X-ray is irradiated along the adhesive layer from the side surface of the structure. Then, a linear detection image is obtained as the detection image, and the adhesion state between the rubber and the adherend is inspected based on the curve state of the obtained linear detection image or the change in the thickness of the line. Take the configuration.
本発明者らは、先の突き止めた結果に基づき、亜鉛の含有量に着目し、さらに研究を重ねた。その結果、接着剤中の亜鉛含有量が、ＥＰＭＡによる分析の結果、亜鉛検出量２３〜３５重量％であれば、ゴムと被着体との間の接着力を弱めることなく、Ｘ線を利用して両者間の接着状態を充分に検査できることを見出し、本発明に到達した。 The inventors of the present invention focused on the zinc content based on the results of the previous determination, and further studied. As a result, when the zinc content in the adhesive is 23 to 35% by weight as a result of analysis by EPMA, the X-ray is used without weakening the adhesive force between the rubber and the adherend. As a result, the inventors have found that the adhesion state between the two can be sufficiently inspected, and have reached the present invention.
なお、上記ＥＰＭＡ（Electron Probe Micro Analyzer ）とは、電子線マイクロアナライザであり、電子線を試料に照射することにより、その試料から発生する特性Ｘ線（元素に固有な波長をもつＸ線）を測定し、元素分析等を行う装置である。具体的には、特性Ｘ線の波長から元素の種類が特定でき、その強度からその元素の存在割合を知ることができる。 The above-mentioned EPMA (Electron Probe Micro Analyzer) is an electron beam microanalyzer, which emits characteristic X-rays (X-rays having a wavelength unique to the element) generated from the sample by irradiating the sample with the electron beam. It is a device that performs measurement and elemental analysis. Specifically, the type of element can be specified from the wavelength of the characteristic X-ray, and the existence ratio of the element can be known from the intensity.
本発明のゴムと被着体との間の接着検査方法によれば、接着剤中のＸ線検出物質として亜鉛化合物を選択し、接着剤中の亜鉛含有量を、ＥＰＭＡによる分析の結果、亜鉛検出量が２３〜３５重量％となるように設定するため、ゴムと被着体との間の接着力を弱めることなく、Ｘ線を利用して両者間の接着状態を充分に検査することができる。 According to the method for inspecting adhesion between a rubber and an adherend of the present invention, a zinc compound is selected as an X-ray detection substance in the adhesive, and the zinc content in the adhesive is analyzed by EPMA. Since the detection amount is set to be 23 to 35% by weight, it is possible to sufficiently inspect the adhesive state between the two using X-rays without weakening the adhesive force between the rubber and the adherend. it can.
つぎに、本発明の実施の形態を図面にもとづいて詳しく説明する。 Next, embodiments of the present invention will be described in detail with reference to the drawings.
図１は、本発明のゴムと被着体との間の接着検査方法の一実施の形態を示している。この実施の形態では、ゴムシート１と樹脂シート（被着体）２とを接着剤３で接着したシート状構造体Ａの接着状態を、Ｘ線１０を利用して検査する。この場合、上記接着剤３には、Ｘ線検出物質として亜鉛化合物を含有させ、接着剤中の亜鉛含有量を、ＥＰＭＡによる分析結果が亜鉛検出量２３〜３５重量％の範囲内となるように設定する。それ以外は、従来の検査方法と同様である。 FIG. 1 shows an embodiment of a method for inspecting adhesion between rubber and an adherend of the present invention. In this embodiment, the adhesion state of the sheet-like structure A in which the rubber sheet 1 and the resin sheet (adhered body) 2 are bonded with the adhesive 3 is inspected using the X-ray 10. In this case, the adhesive 3 contains a zinc compound as an X-ray detection substance, and the zinc content in the adhesive is determined so that the analysis result by EPMA is within the range of the zinc detection amount of 23 to 35% by weight. Set. Other than that, it is the same as the conventional inspection method.
すなわち、Ｘ線発生装置１１から上記シート状構造体Ａの側面にＸ線１０を照射する。このとき、Ｘ線１０の照射方向がシート状構造体Ａの表面と平行になるようにする。そして、シート状構造体Ａの接着剤３中の亜鉛から発生する特性Ｘ線１０ａを検出器１２で検出することにより、シート状構造体Ａの接着剤３中における亜鉛化合物の検出像（線状に現れる）が得られる。この検出像は、Ｘ線１０が接着剤３に含有された亜鉛化合物の亜鉛を検出して形成されたものであるため、接着剤３の適正もしくは不適性な存在状態を知ることができる。例えば、検出像が直線的であれば接着剤が適正に存在していて接着状態は適正であり、湾曲していたり、直線が太くなったり細くなったりしていると、接着剤３の層に剥離部分が存在していて不適性であることがわかる。 That is, the X-ray 10 is irradiated from the X-ray generator 11 to the side surface of the sheet-like structure A. At this time, the irradiation direction of the X-ray 10 is set to be parallel to the surface of the sheet-like structure A. Then, by detecting the characteristic X-rays 10a generated from the zinc in the adhesive 3 of the sheet-like structure A by the detector 12, the detection image of the zinc compound in the adhesive 3 of the sheet-like structure A (linear) To appear). Since this detection image is formed by detecting the zinc of the zinc compound contained in the adhesive 3 by the X-ray 10, it is possible to know the proper or inappropriate presence state of the adhesive 3. For example, if the detected image is a straight line, the adhesive is properly present and the bonding state is appropriate. If the detection image is curved, or if the straight line is thick or thin, It can be seen that there is an exfoliation part and it is inappropriate.
本発明では、接着剤３として、ＥＰＭＡにより分析した亜鉛の検出量が２３〜３５重量％の範囲内にあるものを使用するが、それは、下記の理由による。すなわち、上記検出量が２３重量％を下回ると、亜鉛の含有量が少な過ぎて、亜鉛に対するＸ線１０の検出強度が弱く、接着剤３の存在状態を示す検出像が不明瞭となる。このため、接着剤３の存在状態を充分な精度で検査することができなくなるからである。また、上記検出量が３５重量％を上回ると、上記検出像が明瞭となり、検査精度は向上するものの、ゴムシート１と樹脂シート２との接着力が弱まり、製品として不充分なものとなるからである。 In the present invention, the adhesive 3 used is one in which the detected amount of zinc analyzed by EPMA is in the range of 23 to 35% by weight, for the following reason. That is, when the detected amount is less than 23% by weight, the content of zinc is too small, the detection intensity of the X-ray 10 with respect to zinc is weak, and the detection image indicating the presence state of the adhesive 3 becomes unclear. For this reason, the presence state of the adhesive 3 cannot be inspected with sufficient accuracy. Further, if the detected amount exceeds 35% by weight, the detected image becomes clear and the inspection accuracy is improved, but the adhesive force between the rubber sheet 1 and the resin sheet 2 is weakened, which is insufficient as a product. It is.
このように、本発明のゴムと被着体との間の接着検査方法によれば、ＥＰＭＡにより分析した亜鉛の検出量が２３〜３５重量％の範囲内にある接着剤３を使用するため、ゴムシート１と樹脂シート２との間の接着力を弱めることなく、Ｘ線１０を利用して両者間の接着状態を充分な精度で検査することができる。しかも、上記接着剤３は、鉛化合物を含有していないため、環境を悪化させない。 Thus, according to the adhesion inspection method between the rubber and the adherend of the present invention, since the adhesive 3 in which the detected amount of zinc analyzed by EPMA is in the range of 23 to 35% by weight is used, Without weakening the adhesive force between the rubber sheet 1 and the resin sheet 2, the X-ray 10 can be used to inspect the adhesive state between them with sufficient accuracy. And since the said adhesive agent 3 does not contain a lead compound, it does not worsen an environment.
なお、上記亜鉛化合物としては、例えば、酸化亜鉛，脂肪酸亜鉛，硝酸亜鉛，燐酸亜鉛，炭酸亜鉛，珪酸亜鉛等があげられる。 As the above-mentioned zinc compound include zinc oxide, fatty acid zinc, zinc nitrate, zinc phosphate, zinc carbonate, zinc silicate, and the like.
また、上記ゴムとしては、例えば、天然ゴム（ＮＲ），スチレン−ブタジエン共重合ゴム（ＳＢＲ），ブタジエンゴム（ＢＲ），エチレン−プロピレン−ジエン三元共重合ゴム（ＥＰＤＭ），ブチルゴム（ＩＩＲ），塩素化ブチルゴム（Ｃｌ−ＩＩＲ），アクリロニトリル−ブタジエンゴム（ＮＢＲ），水素添加アクリロニトリル−ブタジエンゴム（Ｈ−ＮＢＲ）等があげられる。 Further, as the rubber, for example, natural rubber (NR), styrene - butadiene copolymer rubber (SBR), butadiene rubber (BR), ethylene - propylene - diene terpolymer rubber (EPDM), a butyl rubber (IIR), a Examples include chlorinated butyl rubber (Cl-IIR), acrylonitrile-butadiene rubber (NBR), and hydrogenated acrylonitrile-butadiene rubber (H-NBR).
また、上記実施の形態では、被着体として樹脂シート２を用いたが、その材料や形状は、他でもよい。例えば、材料は、ゴムや金属（場合によっては非鉄系金属）等でもよく、形状は、シート状に限らず立体状でもよい。 Further, in the above-described embodiment, a resin sheet 2 as the adherend and the material and shape, have good other times. For example, the material may be rubber, metal (in some cases, non-ferrous metal), and the shape is not limited to a sheet shape but may be a three-dimensional shape.
つぎに、実施例について比較例と併せて説明する。 Next, examples will be described together with comparative examples.
〔実施例１〕
３層構造のシート状積層構造体を準備した。この積層構造体の作製は、ポリアミド（ＰＡ）製樹脂シートの上下両面に、酸化亜鉛含有接着剤を塗布し、プレス成形により作製したＮＢＲ製シート（ゴムシート）を加硫接着（１５０℃×３０分間）することにより行った。ここで、上記接着剤としては、酸化亜鉛含有のポリオレフィン系接着剤〔ロード社製、Ｃ６１００、亜鉛含有量：１７．３重量％（ＥＰＭＡ）〕に酸化亜鉛を添加し、接着剤中の亜鉛含有量を２３．０重量％（ＥＰＭＡ）に調製したものを使用した。
[Example 1]
A sheet-like laminated structure having a three-layer structure was prepared. This laminated structure was produced by applying a zinc oxide-containing adhesive on the upper and lower surfaces of a polyamide (PA) resin sheet and vulcanizing and bonding an NBR sheet (rubber sheet) produced by press molding (150 ° C. × 30 Minutes). Here, as the adhesive, zinc oxide is added to a zinc oxide-containing polyolefin-based adhesive [R6, C6100, zinc content: 17.3% by weight (EPMA)], and zinc contained in the adhesive is contained. The amount prepared to 23.0% by weight (EPMA) was used.
〔実施例２〕
上記実施例１において、接着剤中の亜鉛含有量を２５．６重量％（ＥＰＭＡ）に調製したものを使用した。それ以外は、上記実施例１と同様にした。
[Example 2]
In the said Example 1, what adjusted the zinc content in an adhesive agent to 25.6 weight% (EPMA) was used. Other than that, it was the same as in Example 1 above.
〔実施例３〕
上記実施例１において、接着剤中の亜鉛含有量を３２．６重量％（ＥＰＭＡ）に調製したものを使用した。それ以外は、上記実施例１と同様にした。
Example 3
In the said Example 1, what adjusted the zinc content in an adhesive agent to 32.6 weight% (EPMA) was used. Other than that, it was the same as in Example 1 above.
〔実施例４〕
上記実施例１において、接着剤中の亜鉛含有量を３５．０重量％（ＥＰＭＡ）に調製したものを使用した。それ以外は、上記実施例１と同様にした。
Example 4
In the said Example 1, what adjusted the zinc content in an adhesive agent to 35.0 weight% (EPMA) was used. Other than that, it was the same as in Example 1 above.
〔比較例１〕
上記実施例１において、接着剤に酸化亜鉛を添加することなく、市販状態のまま使用した〔亜鉛含有量：１７．３重量％（ＥＰＭＡ）〕。それ以外は、上記実施例１と同様にした。
[Comparative Example 1]
In the said Example 1, it was used with a commercially available state, without adding a zinc oxide to an adhesive agent [Zinc content: 17.3 weight% (EPMA)]. Other than that, it was the same as in Example 1 above.
〔比較例２〕
上記実施例１において、接着剤中の亜鉛含有量を２１．３重量％（ＥＰＭＡ）に調製したものを使用した。それ以外は、上記実施例１と同様にした。
[Comparative Example 2]
In the said Example 1, what adjusted the zinc content in an adhesive agent to 21.3% weight (EPMA) was used. Other than that, it was the same as in Example 1 above.
〔比較例３〕
上記実施例１において、接着剤中の亜鉛含有量を３６．６重量％（ＥＰＭＡ）に調製したものを使用した。それ以外は、上記実施例１と同様にした。
[Comparative Example 3]
In the said Example 1, what adjusted the zinc content in an adhesive agent to 36.6 weight% (EPMA) was used. Other than that, it was the same as in Example 1 above.
〔接着剤の酸化亜鉛含有量の測定〕
上記実施例１〜４および比較例１〜３において使用する各接着剤の亜鉛含有量の測定には、測定機器として、ＥＰＭＡ１６００（島津製作所社製）を用いた。そして、測定は、各接着剤を検査板上に塗布後固化させたものに対して行った。また、測定条件は、加速電圧１５ｋＶ，測定範囲１００μｍ，ビーム電流０．１２μＡに設定した。
[Measurement of zinc oxide content of adhesive]
EPMA 1600 (manufactured by Shimadzu Corporation) was used as a measuring instrument for measuring the zinc content of each adhesive used in Examples 1 to 4 and Comparative Examples 1 to 3. And the measurement was performed with respect to what solidified after apply | coating each adhesive agent on a test | inspection board. Measurement conditions were set to an acceleration voltage of 15 kV, a measurement range of 100 μm, and a beam current of 0.12 μA.
〔Ｘ線を利用した接着検査〕
上記実施例１〜４および比較例１〜３で得られた各シート状積層構造体の側面にＸ線を照射した。この検査には、検査機器として、ＳＭＸ−１３０（島津製作所社製）を用いた。そして、検査条件は、加速電圧６０ｋＶ，ビーム電流８０μＡに設定した。その結果、接着剤の存在状態を示す検出像が明瞭となり充分な精度で検査できるものを○、上記検出像が不明瞭となり検査精度が不充分なものを×として評価し、下記の表１に表記した。
[Adhesion inspection using X-rays]
X-rays were irradiated to the side surfaces of the respective sheet-like laminated structures obtained in Examples 1 to 4 and Comparative Examples 1 to 3. For this inspection, SMX-130 (manufactured by Shimadzu Corporation) was used as an inspection device. The inspection conditions were set to an acceleration voltage of 60 kV and a beam current of 80 μA. As a result, the detection image indicating the presence state of the adhesive was evaluated as “◯”, and the inspection image was evaluated as “x” when the detection image was unclear and the inspection accuracy was insufficient. Indicated.
〔接着力の評価〕
上記各シート状積層構造体から１ｃｍ幅の帯状に切り取ったものに対して、引張試験機（オリエンテック社製）を用い、１８０°ピール強度測定を行った。その結果、破断面が１００％ＮＢＲ製シート（ゴムシート）内部であったものを○、破断面の一部がＮＢＲ製シート（ゴムシート）と樹脂シートとの界面（接着剤部分）であったものを×として評価し、下記の表１に表記した。
[Evaluation of adhesive strength]
A 180 ° peel strength measurement was performed on a piece cut from each of the above sheet-like laminated structures into a 1 cm wide band using a tensile tester (manufactured by Orientec Corp.). As a result, the fracture surface was inside the 100% NBR sheet (rubber sheet), and a part of the fracture surface was the interface (adhesive part) between the NBR sheet (rubber sheet) and the resin sheet. Things were evaluated as x and listed in Table 1 below.
上記表１の結果より、接着剤として、亜鉛含有量が２３．０〜３５．０重量％（ＥＰＭＡ）のものを使用すると、ゴムシートと樹脂シートとの間の接着力を弱めることなく、Ｘ線を利用して両者間の接着状態を充分な精度で検査できることがわかる。 From the results in Table 1 above, when an adhesive having a zinc content of 23.0 to 35.0% by weight (EPMA) is used, the adhesive force between the rubber sheet and the resin sheet is not weakened. It can be seen that the adhesion state between the two can be inspected with sufficient accuracy using the wire.
接着剤に亜鉛化合物を特定量含有させることにより、Ｘ線を利用して検査できるようになり、接着検査が簡単かつ短時間でできる。しかも、接着力が弱まらないため、接着強度の高い構造体を製造することができる。また、環境問題となる鉛化合物含有接着剤の使用を避けることができる。 By including a specific amount of a zinc compound in the adhesive, inspection can be performed using X-rays, and the adhesion inspection can be performed easily and in a short time. In addition, since the adhesive strength is not weakened, a structure with high adhesive strength can be manufactured. In addition, it is possible to avoid the use of lead compound-containing adhesives that cause environmental problems.
Ａ 構造体
１ ゴムシート
２ 樹脂シート
３ 接着剤
１０ Ｘ線
A Structure 1 Rubber sheet 2 Resin sheet 3 Adhesive 10 X-ray
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