JP2006119069A - Method for measuring water vapor permeability by using calcium corrosion test - Google Patents

Method for measuring water vapor permeability by using calcium corrosion test Download PDF

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JP2006119069A
JP2006119069A JP2004309252A JP2004309252A JP2006119069A JP 2006119069 A JP2006119069 A JP 2006119069A JP 2004309252 A JP2004309252 A JP 2004309252A JP 2004309252 A JP2004309252 A JP 2004309252A JP 2006119069 A JP2006119069 A JP 2006119069A
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water vapor
corrosion
calcium
vapor permeability
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JP4407466B2 (en
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Kenichi Kanemasa
賢一 兼政
Hisashi Ito
寿 伊東
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Sumitomo Bakelite Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for measuring water vapor permeability of a film by a calcium corrosion test, which can calculate the water vapor permeability without being affected by irregularities or foreign materials produced in a test piece. <P>SOLUTION: The test piece subjected to the calcium corrosion test is set in a constant-temperature and constant-humidity environment, and a plurality of test piece images are photographed at intervals of time. Feature points such as corrosion and foreign materials in respective images are extracted through an image processing step, and then the images are compared respectively, and only feature points whose areas increase with time, are extracted as the corrosion, and the water vapor permeability of the film is calculated from the areas. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

本発明は、カルシウム腐食法による水蒸気透過度測定方法、特に、腐食領域を抽出する画像処理方法に関するものである。 The present invention relates to a method for measuring water vapor permeability by a calcium corrosion method, and more particularly to an image processing method for extracting a corrosion area.

水分が透過することで材料の特性が低下する現象が昔から確認されている。例えば、鉄表面に亜鉛やアルミ等のメッキを施したメッキ鋼板や表面処理鋼板では、メッキ材の欠陥を通して水分が浸透しサビを発生させる。また、プラスチック表面に酸化ケイ素、酸化アルミまたはアルミ金属箔を蒸着した食品や薬品の包装材料では蒸着膜の欠陥を通して水蒸気が拡散し、食品または薬品に吸湿する等の問題が発生する。更に最近では、電子・電気装置の包装材料や液晶表示素子、有機ＥＬ表示素子のようなハイレベルな防湿性が要求されるプラスチックフィルムの開発がなされているため、吸湿を防止するためのバリア膜の開発が非常に活発に行なわれている。   It has been confirmed for a long time that the properties of materials deteriorate due to the permeation of moisture. For example, in a plated steel sheet or a surface-treated steel sheet in which zinc or aluminum is plated on the iron surface, moisture penetrates through defects in the plated material and generates rust. In addition, in a packaging material for foods and chemicals in which silicon oxide, aluminum oxide or aluminum metal foil is vapor-deposited on the plastic surface, water vapor is diffused through defects in the vapor deposition film, causing problems such as moisture absorption by the food or chemicals. More recently, plastic films that require high levels of moisture-proofing, such as packaging materials for electronic and electrical devices, liquid crystal display elements, and organic EL display elements, have been developed, and therefore barrier films for preventing moisture absorption. The development of is very active.

従来から検討されている水蒸気透過度の評価は、カップ法（非特許文献１）、モコン法(非特許文献２)等であるが、ハイレベルな防湿性を評価することは不可能であった。モコン法の測定限界値は0.01g/m2/day程度であり、液晶基板や有機ＥＬ基板等に要求される10-3g/m2/day以下の水蒸気透過量は評価できない。 The evaluation of water vapor permeability that has been studied conventionally is the cup method (Non-patent document 1), the mocon method (Non-patent document 2), etc., but it has been impossible to evaluate a high level of moisture resistance. . The measurement limit value of the Mocon method is about 0.01 g / m 2 / day, and the water vapor transmission rate of 10 −3 g / m 2 / day or less required for liquid crystal substrates and organic EL substrates cannot be evaluated.

近年、カルシウムの腐食により、バリア膜付きプラスチックフィルムの防湿性を評価する方法が開発されている(例えば、非特許文献３、４)。この方法はバリア膜付きプラスチックフィルムのバリア欠陥を通して侵入した水分とカルシウムの反応を利用した測定方法である。内側に金属カルシウム膜を成膜したフィルム試験片を恒温恒湿環境下に置き、フィルムを透過した水蒸気と反応して腐食したカルシウムの量を画像処理等で測定することにより、フィルムの水蒸気透過量を測定する。このカルシウム腐食法による水蒸気透過度測定は従来のモコン法等と比べ非常に高感度な水蒸気透過度測定が可能である。     In recent years, methods for evaluating moisture resistance of a plastic film with a barrier film by corrosion of calcium have been developed (for example, Non-Patent Documents 3 and 4). This method is a measurement method using the reaction between moisture and calcium that has penetrated through a barrier defect of a plastic film with a barrier film. A film specimen with a metallic calcium film formed inside is placed in a constant temperature and humidity environment. Measure. The water vapor permeability measurement by this calcium corrosion method can measure the water vapor permeability with a very high sensitivity compared to the conventional Mocon method.

カルシウム腐食法によりフィルムの水蒸気透過度を測定する際、試験片中のカルシウムの腐食面積を画像処理により自動的に測定すると、手作業で測定する場合に比べて、測定精度向上と測定時間短縮が可能となる。しかしながら、カルシウム腐食の有無による画像の明度差は小さく、単純な2値化画像処理による腐食領域の抽出は難しい。デジタル画像を３値化し、ニューラルネットワークにより欠陥パターンの分類を行う方法（例えば、特許文献１）などより高度な画像処理を行うことにより、腐食領域の抽出は可能である。しかし、高度な画像処理により高感度な腐食領域抽出を行うことにより、異物や腐食ではないわずかなムラなども抽出してしまい、精度が低下することがあるという問題がある。   When measuring the water vapor permeability of a film by the calcium corrosion method, automatically measuring the corrosion area of calcium in the test piece by image processing improves measurement accuracy and shortens the measurement time compared to manual measurement. It becomes possible. However, the difference in image brightness due to the presence or absence of calcium corrosion is small, and it is difficult to extract the corrosion area by simple binary image processing. Corrosion areas can be extracted by performing more advanced image processing such as a method of ternizing a digital image and classifying defect patterns using a neural network (for example, Patent Document 1). However, there is a problem in that, by performing highly sensitive corrosion area extraction by advanced image processing, foreign matter or slight unevenness that is not corrosion may be extracted, and accuracy may deteriorate.

特開平７−３１８５１５号公報JP 7-318515 A ＪＩＳ Ｚ ０２０８JIS Z 0208 ＪＩＳ Ｋ ７１２９ Ｂ法JIS K 7129 method B Asia Display/IDW’01 pp.1435〜1438Asia Display / IDW’01 pp.1435〜1438 藤本ら、第１２回ポリマー材料フォーラム、ｐ．２００、２００３Fujimoto et al., 12th Polymer Material Forum, p. 200, 2003

本発明は、高精度な水蒸気透過度測定方法を提供するものである。 The present invention provides a highly accurate method for measuring water vapor permeability.

本発明は、カルシウム腐食法によるフィルムの水蒸気透過度測定方法において、試験片の腐食状態を時間間隔をあけて複数回撮影し、撮影した各画像中の特徴点を抽出し、各画像間の特徴点を比較して時間とともに面積が増加している特徴点のみを腐食とみなして水蒸気透過度を算出する水蒸気透過度測定方法である。     The present invention relates to a method for measuring the water vapor permeability of a film by a calcium corrosion method, wherein the corrosion state of a test piece is photographed multiple times at time intervals, feature points in each photographed image are extracted, and features between each image are extracted. This is a method for measuring water vapor permeability in which the water vapor permeability is calculated by comparing points and considering only the feature points whose area increases with time as corrosion.

本発明によれば、カルシウム腐食法による水蒸気透過度測定方法において、異物などの影響を受けずにカルシウム腐食領域だけを画像処理にて抽出するため、精度の高い水蒸気透過度測定が可能となる。 According to the present invention, in the method for measuring water vapor permeability by the calcium corrosion method, only the calcium corrosion area is extracted by image processing without being affected by foreign matters, so that water vapor permeability can be measured with high accuracy.

本発明は、カルシウム腐食法による水蒸気透過度測定方法において、試験片の腐食状態を撮影した複数画像から異物などの影響を受けずに腐食面積の測定が可能な画像処理を用いることにより、高精度に水蒸気透過度を算出する水蒸気透過度測定方法である。   In the water vapor permeability measurement method by the calcium corrosion method, the present invention uses image processing that can measure the corrosion area without being affected by foreign matter from a plurality of images obtained by photographing the corrosion state of the test piece. This is a method for measuring water vapor permeability by calculating water vapor permeability.

以下本発明を図面によって説明する。
図１は本発明の水蒸気透過度測定方法のフロー図である。適当な時間間隔をあけて撮影した複数の試験片撮影画像１に対し、特徴点抽出処理２を行い、腐食や異物、ムラなど画像中で特徴となる点を抽出する。さらに、各画像の特徴点を特徴点比較処理３にて比較し、経時的な面積増加がある特徴点のみを腐食領域として抽出する。最後に、水蒸気透過度算出処理４にて、各画像の腐食領域の面積から水蒸気透過量を算出し、その値をもとに単位時間あたりの水蒸気透過量変化、つまり、水蒸気透過度算出する。 The present invention will be described below with reference to the drawings.
FIG. 1 is a flow diagram of the method for measuring water vapor permeability of the present invention. A feature point extraction process 2 is performed on a plurality of test piece photographed images 1 photographed at appropriate time intervals to extract points that are characteristic in the image, such as corrosion, foreign matter, and unevenness. Further, the feature points of the images are compared in the feature point comparison process 3, and only the feature points having an area increase with time are extracted as corrosion areas. Finally, in the water vapor transmission rate calculation process 4, the water vapor transmission rate is calculated from the area of the corroded area of each image, and the change in the water vapor transmission rate per unit time, that is, the water vapor transmission rate is calculated based on the value.

図２はカルシウム腐食法で用いる試験片の一例である。水蒸気透過度を測定する材料である水蒸気バリアフィルム５の片面の一部にカルシウム層６を成膜し、カルシウム層６のうち水蒸気バリアフィルム５に接していない面を封止層７で覆う。カルシウム腐食法では試験片を恒温恒湿処理し、水蒸気バリアフィルムを透過した水蒸気により腐食したカルシウムの量を算出することにより水蒸気の透過量を測定する。カルシウム層６の腐食状態を光学的に観測するために、水蒸気バリアフィルム５と封止層７のうち、少なくともどちらか一方は透明である必要がある。水蒸気バリアフィルム５が透明な場合は、封止層７には金属、ガラス、樹脂などを複数組み合わせて使用することが好ましい。
また、封止層７が透明であれば、水蒸気透過度を測定する材料である水蒸気バリアフィルム５は、透明フィルムやガラス等の透明な材料ばかりではなく、例えば金属やセラミック等、不透明な材料でも水蒸気透過度を測定することができる。 FIG. 2 is an example of a test piece used in the calcium corrosion method. The calcium layer 6 is formed on a part of one surface of the water vapor barrier film 5 which is a material for measuring the water vapor permeability, and the surface of the calcium layer 6 that is not in contact with the water vapor barrier film 5 is covered with the sealing layer 7. In the calcium corrosion method, a test piece is subjected to constant temperature and humidity treatment, and the amount of calcium corroded by water vapor that has permeated through the water vapor barrier film is calculated to measure the amount of water vapor permeated. In order to optically observe the corrosion state of the calcium layer 6, at least one of the water vapor barrier film 5 and the sealing layer 7 needs to be transparent. When the water vapor barrier film 5 is transparent, the sealing layer 7 is preferably used in combination of a plurality of metals, glasses, resins and the like.
Further, if the sealing layer 7 is transparent, the water vapor barrier film 5 which is a material for measuring the water vapor transmission rate is not only a transparent material such as a transparent film or glass but also an opaque material such as a metal or ceramic. Water vapor permeability can be measured.

試験片を恒温恒湿環境下に放置した後、水蒸気によるカルシウムの腐食状態を撮影した画像の一例を図３に示す。カルシウムが腐食していない領域８の中に、腐食領域９や異物１０が存在する。腐食していない領域８についても、素材、照明、カメラなど各種要因によるムラが存在する。   FIG. 3 shows an example of an image obtained by photographing the corrosion state of calcium by water vapor after leaving the test piece in a constant temperature and humidity environment. In the region 8 where calcium is not corroded, the corroded region 9 and the foreign material 10 exist. The non-corroded region 8 also has unevenness due to various factors such as materials, lighting, and cameras.

図４は、本発明の水蒸気透過度測定方法における画像処理の説明図である。まず、図３に示したような試験片の画像から特徴点を抽出する。特徴点を抽出する方法としては、二値化処理、多値化処理、微分処理による輪郭抽出などの各種方法やそれらを組み合わせた方法があるが、腐食がどのような画像になるかによって適切に選択すればよく、特徴点抽出処理方法に限定はない。図３の画像に対する特徴点抽出処理方法の一例としては、画像中で腐食していない領域８に比べて腐食領域９の色が中心部では白く、外周部では黒くなっていることから、画像明度について２つの閾値をつかう三値化処理をおこない、小さい閾値より明度が小さい領域と大きい閾値より明度が大きい領域を特徴点として抽出する方法があげられる。   FIG. 4 is an explanatory diagram of image processing in the water vapor transmission rate measurement method of the present invention. First, feature points are extracted from the test piece image as shown in FIG. There are various methods for extracting feature points, such as binarization processing, multi-value processing, contour extraction by differentiation processing, and combinations of these methods. The feature point extraction processing method is not limited. As an example of the feature point extraction processing method for the image of FIG. 3, the color of the corroded area 9 is white in the central portion and black in the outer peripheral portion as compared with the non-corroded area 8 in the image. There is a method of performing ternarization processing using two threshold values and extracting, as feature points, a region having a lightness smaller than a small threshold and a region having a lightness larger than a large threshold.

試験片の各画像に対し、特徴点抽出処理をおこなうことにより、特徴点画像が得られる。時刻Ｔ１における特徴点画像１１と時刻Ｔ２（Ｔ２＞Ｔ１）における特徴点画像１３を比較すると、特徴点１２は面積が増加しているものと、増加していないものに分類することが出来る。面積が増加している特徴点だけを腐食領域１５として抽出し、腐食領域画像１４を作成する。面積が増加していない特徴点は腐食とみなされない領域１６となり、水蒸気透過度算出の際に除外する。異物やムラは時間が経過しても面積は変化しないため、特徴点比較後の腐食領域画像１４からは除去される。従って、水蒸気の透過により成長している腐食領域の面積だけを用いて水蒸気透過度の算出を行うため、異なる時刻の画像を比較せずに腐食面積を抽出する一般的な方法に比べて高精度の測定が可能となる。また、特徴点抽出処理において、異物やムラが特徴点として抽出されたとしても特徴点比較処理で除去されるため、特徴点抽出処理の感度を上げ、腐食を確実に抽出するように出来る点においても精度の向上が可能となる。   A feature point image is obtained by performing feature point extraction processing on each image of the test piece. Comparing the feature point image 11 at time T1 and the feature point image 13 at time T2 (T2> T1), the feature points 12 can be classified into those having an increased area and those having not increased. Only the feature points having an increased area are extracted as the corrosion area 15 to create the corrosion area image 14. A feature point whose area has not increased becomes a region 16 that is not regarded as corrosion, and is excluded when calculating the water vapor permeability. Since the area of foreign matter and unevenness does not change over time, it is removed from the corrosion region image 14 after the feature point comparison. Therefore, since the water vapor permeability is calculated using only the area of the corroded area that is growing due to water vapor permeation, it is more accurate than the general method of extracting the corroded area without comparing images at different times. Can be measured. Also, in the feature point extraction process, even if foreign matter or unevenness is extracted as a feature point, it is removed by the feature point comparison process, so that the sensitivity of the feature point extraction process can be increased and corrosion can be reliably extracted. The accuracy can be improved.

図１の水蒸気透過度算出処理４においては、特徴点比較処理３から出力された腐食領域画像から腐食総面積を算出し、その全領域が腐食するのに要した水蒸気の量を計算することにより、水蒸気バリアフィルムの水蒸気透過度を算出する。式１に示すように、カルシウム１ｍｏｌは２ｍｏｌの水分と反応し、１ｍｏｌの水酸化カルシウムを生成する。

Ｃａ ＋ ２Ｈ２Ｏ → Ｃａ（ＯＨ）２ ＋ Ｈ２ （式１）

よって、試験片の腐食に要した水蒸気の量は、腐食総面積δ、カルシウム層の厚みｔ、カルシウムの腐食後の厚み補正係数α（式３）、腐食後の水酸化カルシウムの密度ｄ２から求めることができる。

恒温恒湿処理後の水酸化カルシウムのモル量（Ｘ）：
Ｘ＝（δ×ｔ×α×ｄ２）/Ｍ２［g/m2/day］ （式２）
１<α≦（Ｍ２/ｄ２）/（Ｍ１/ｄ１） （式３）
水蒸気透過量（Ｙ）＝Ｘ×１８×２［g/m2/day］ （式４）

時刻Ｔ１における水蒸気透過量Ｙ１、時刻Ｔ２における水蒸気透過量Ｙ２、Ｔ１とＴ２の時間差Ｔ、測定前のカルシウム膜の総面積Ａから水蒸気透過度は式５に示すとおりとなる。

水蒸気透過度＝（Ｙ２−Ｙ１）×（１０４／Ａ）*（２４／Ｔ）［g/m2/day］
（式５）

測定開始時のカルシウム総面積 ： Ａ［ｃｍ2］
カルシウムの厚み ： ｔ［ｃｍ］
厚み補正係数 ： α
腐食総面積 ： δ［ｃｍ2］
カルシウムの分子量 ： Ｍ１
水酸化カルシウムの分子量 ： Ｍ２
カルシウムの密度 ： ｄ１［ｇ／ｃｍ3］
水酸化カルシウムの密度 ： ｄ２［ｇ／ｃｍ3］
測定時間差 ： Ｔ［ｈｏｕｒ］

以上の手順により、腐食領域のみを抽出することによる高精度な水蒸気透過度測定が可能となる。 In the water vapor permeability calculation process 4 of FIG. 1, the total corrosion area is calculated from the corrosion area image output from the feature point comparison process 3, and the amount of water vapor required for the entire area to corrode is calculated. The water vapor permeability of the water vapor barrier film is calculated. As shown in Equation 1, 1 mol of calcium reacts with 2 mol of water to produce 1 mol of calcium hydroxide.

Ca + 2H 2 O → Ca (OH) 2 + H 2 (Formula 1)

Therefore, the amount of water vapor required for the corrosion of the test piece is determined from the total corrosion area δ, the calcium layer thickness t, the thickness correction coefficient α after the calcium corrosion (Equation 3), and the calcium hydroxide density d 2 after the corrosion. Can be sought.

Molar amount of calcium hydroxide after constant temperature and humidity treatment (X):
X = (δ × t × α × d 2 ) / M 2 [g / m 2 / day] (Formula 2)
1 <α ≦ (M 2 / d 2 ) / (M 1 / d 1 ) (Formula 3)
Water vapor transmission rate (Y) = X × 18 × 2 [g / m 2 / day] (Formula 4)

From the water vapor transmission amount Y1 at time T1, the water vapor transmission amount Y2 at time T2, the time difference T between T1 and T2, and the total area A of the calcium film before the measurement, the water vapor transmission rate is as shown in Equation 5.

Water vapor permeability = (Y2−Y1) × (10 4 / A) * (24 / T) [g / m 2 / day]
(Formula 5)

Total area of calcium at the start of measurement: A [cm 2 ]
Calcium thickness: t [cm]
Thickness correction factor: α
Total corrosion area: δ [cm 2 ]
Molecular weight of calcium: M 1
Molecular weight of calcium hydroxide: M 2
Calcium density: d 1 [g / cm 3 ]
Calcium hydroxide density: d 2 [g / cm 3 ]
Measurement time difference: T [hour]

By the above procedure, it is possible to measure water vapor permeability with high accuracy by extracting only the corrosion area.

本発明のカルシウム腐食法による水蒸気透過度方法は、試験片の腐食領域を画像処理で自動的に抽出する際、異物やムラの影響を排除して腐食領域のみを確実に抽出するため、非常に高精度な水蒸気透過度測定が可能である。
The water vapor permeability method by the calcium corrosion method of the present invention is very effective in extracting only the corrosion area by eliminating the influence of foreign matter and unevenness when automatically extracting the corrosion area of the test piece by image processing. Highly accurate water vapor permeability measurement is possible.

本発明の水蒸気透過度測定方法のフロー図である。It is a flowchart of the water-vapor-permeation measuring method of this invention. カルシウム腐食法で用いる試験片の一例である。It is an example of the test piece used with a calcium corrosion method. 試験片の画像の一例である。It is an example of the image of a test piece. 本発明における画像処理の説明図である。It is explanatory drawing of the image processing in this invention.

符号の説明Explanation of symbols

１ 複数の試験片撮影画像
２ 特徴点抽出画像処理
３ 特徴点比較画像処理
４ 水蒸気透過度算出処理
５ 水蒸気バリアフィルム
６ カルシウム層
７ 封止層
８ 腐食していない領域
９ 腐食領域
１０ 異物
１１ 時刻Ｔ１における特徴点抽出画像
１２ 特徴点
１３ 時刻Ｔ２における特徴点抽出画像
１４ 腐食領域画像
１５ 腐食とみなされた特徴点
１６ 腐食とみなされない特徴点 DESCRIPTION OF SYMBOLS 1 Photographed test piece 2 Feature point extraction image processing 3 Feature point comparison image processing 4 Water vapor permeability calculation processing 5 Water vapor barrier film 6 Calcium layer 7 Sealing layer 8 Non-corroded region 9 Corrosion region 10 Foreign material 11 Time T1 Feature point extraction image 12 Feature point 13 Feature point extraction image at time T2 14 Corrosion area image 15 Feature point regarded as corrosion 16 Feature point not regarded as corrosion

Claims (1)

カルシウム腐食法によるフィルムの水蒸気透過度測定方法において、（１）試験片の腐食状態を時間間隔をあけて複数回撮影する工程、（２）撮影した各画像中の特徴点を抽出する画像処理工程、（３）各画像間の特徴点を比較する画像処理工程、及び（４）水蒸気透過度を算出する工程を有し、前記各画像間の特徴点を比較する画像処理工程において、時間とともに面積が増加している特徴点のみを腐食とみなす処理を行うことを特徴とする水蒸気透過度測定方法。 In the method of measuring water vapor permeability of a film by the calcium corrosion method, (1) a step of photographing the corrosion state of the test piece a plurality of times at intervals, (2) an image processing step of extracting feature points in each photographed image , (3) an image processing step for comparing feature points between the images, and (4) an image processing step for calculating the water vapor transmission rate, and comparing the feature points between the images. A method for measuring a water vapor transmission rate, characterized in that only a feature point with an increase in the amount of corrosion is treated as corrosion.
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