JP2008185502A - Combined degradation test method for painting steel plate - Google Patents

Combined degradation test method for painting steel plate Download PDF

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JP2008185502A
JP2008185502A JP2007020530A JP2007020530A JP2008185502A JP 2008185502 A JP2008185502 A JP 2008185502A JP 2007020530 A JP2007020530 A JP 2007020530A JP 2007020530 A JP2007020530 A JP 2007020530A JP 2008185502 A JP2008185502 A JP 2008185502A
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humidity
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Homin Ikeda
法民 池田
Yoshihiro Tsujimoto
吉寛 辻本
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Sekisui House Ltd
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Sekisui House Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a testing method capable of extremely increasing the correlation with degradation in the actual outdoor exposure, in a combined cycle test for making a painting steel plate degrade artificially. <P>SOLUTION: A sample of the painting steel plate is fixed in an isothermal constant-humidity tank capable of keeping arbitrary temperature and humidity, and a plurality of cycles are repeated. The cycle comprises (a) a process of atomizing salt water with respect to the sample in the isothermal constant-humidity tank (preferably, 2 hours), (b) a process of continuously radiating ultraviolet rays by a metal halide lamp, sprinkling water at every fixed period, and cleaning the surface of the sample (preferably, 16 hours), and (c) a process of stopping the radiation of the ultraviolet rays and maintaining a state of high humidity (preferably, 2 hours). <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明は、外装材として用いられる塗装鋼板の耐久性や耐候性を検証するため、人工的な環境下で塗装鋼板に複合的な劣化を生じさせるサイクル試験の方法に関する。   The present invention relates to a cycle test method for causing combined deterioration of a coated steel sheet in an artificial environment in order to verify durability and weather resistance of the coated steel sheet used as an exterior material.

建築物の屋根や外壁等に用いられる外装用の塗装鋼板は、太陽光、熱、水分、塩分といった劣化因子の複合的な作用により、長期間にわたって徐々に劣化する。かかる外装材料の耐久性や耐候性を試験するための方法としては、例えばＪＩＳ・Ｄ０２０５の「自動車部品の耐候性試験」や特許文献１記載の複合サイクル試験に準じた方法、あるいは、特許文献２記載の紫外線照射装置とスプレー装置とを組み合わせた装置による方法などが知られている。   The coated steel sheet for exteriors used for the roof, outer wall, etc. of a building gradually deteriorates over a long period of time due to the combined action of deterioration factors such as sunlight, heat, moisture, and salt content. As a method for testing the durability and weather resistance of such exterior materials, for example, a method according to JIS D0205 "weather resistance test of automobile parts" and the combined cycle test described in Patent Document 1, or Patent Document 2 A method using an apparatus in which the described ultraviolet irradiation apparatus and a spray apparatus are combined is known.

また、本出願人も、実際の屋外暴露環境に近似した複合劣化を促進する試験方法として、特許文献３に記載の方法を提案している。その試験方法は、ひとつの試験装置内で、日射を想定した任意の温度環境下、任意の時間及びサイクルで、紫外線照射、塩水（中性または酸性）の噴霧、散水（中性または酸性）、湿潤、結露、休止、乾燥等を連続的または断続的に実施するものである。
特開昭５６−１２６７４０号公報 特開昭５７−２１１５２８号公報 特開２００３−２７９４６９号公報 In addition, the present applicant has also proposed a method described in Patent Document 3 as a test method for accelerating combined deterioration approximate to an actual outdoor exposure environment. The test method consists of ultraviolet irradiation, spraying of salt water (neutral or acidic), spraying water (neutral or acidic), in an arbitrary temperature environment assuming solar radiation, and at an arbitrary time and cycle in one test apparatus. Wetting, condensation, resting, drying, etc. are performed continuously or intermittently.
JP-A-56-126740 JP-A-57-2111528 JP 2003-279469 A

上記公知文献記載の試験方法を含む多くの研究や実験において、光、熱、水分等の劣化因子による作用が検証されてはいるが、劣化の度合いを客観的に数値化し得る指標は未だ確立していない。また、上記のような複合サイクル試験に際して、各劣化因子をどのような条件や時間配分で組み合わせれば、実際の屋外暴露に最も近似した劣化が生じるのかという点についても、明確化されているわけではない。複数種類の劣化因子の組み合わせ方については、きわめて多様なパターンが考えられるので、それらの多様なパターンを相互に比較して、実際の屋外暴露に最も近似した劣化状態を効率的に再現し得るパターンを見出すのは、特に時間的な面での困難が大きい。   In many studies and experiments including the test methods described in the above-mentioned known literatures, the effects of deterioration factors such as light, heat, and moisture have been verified, but an index that can objectively quantify the degree of deterioration has not yet been established. Not. In addition, in the combined cycle test as described above, it is also clarified as to what kind of conditions and time distribution are combined with each deterioration factor to cause deterioration that is most similar to actual outdoor exposure. is not. There are a wide variety of patterns that can be used to combine multiple types of deterioration factors, so these patterns can be compared with each other to efficiently reproduce the deterioration state that most closely approximates actual outdoor exposure. Finding it is particularly difficult in terms of time.

本発明者らは、長期間にわたる実験・実証結果を通じて、塗装鋼板の劣化の度合いを数値化し得る指標を確立するとともに、その指標に沿って、実際の屋外暴露による劣化結果との相関性が極めて高くなる劣化因子の組み合わせパターンを見出した。本発明は、かかる複合サイクル試験の具体的な方法を提案するものである。   The inventors established an index that can quantify the degree of deterioration of the coated steel sheet through long-term experiments and demonstration results, and along with the index, the correlation with the deterioration result due to actual outdoor exposure is extremely high. We found a combination pattern of increasing deterioration factors. The present invention proposes a specific method for such a combined cycle test.

本発明の複合劣化試験方法は、任意の温湿度を維持しうる恒温恒湿槽内に塗装鋼板の試料を定置し、この槽内で上記試料に対し、
（ａ）塩水を噴霧する工程と、
（ｂ）メタルハライドランプによる紫外線を連続的に照射するとともに、一定時間おきに散水して試料の表面を洗浄する工程と、
（ｃ）紫外線照射を停止して、温湿度制御装置により槽内を高湿に保ち、湿潤させる工程と、
からなるサイクルを複数回繰り返して試料を劣化させることを特徴とする。 In the composite deterioration test method of the present invention, a sample of a coated steel sheet is placed in a constant temperature and humidity chamber capable of maintaining an arbitrary temperature and humidity, and the sample in this tank is
(A) spraying salt water;
(B) a step of continuously irradiating with ultraviolet rays from a metal halide lamp and spraying water every predetermined time to clean the surface of the sample;
(C) stopping ultraviolet irradiation, keeping the inside of the tank at a high humidity by the temperature and humidity control device, and moistening;
It is characterized in that the sample is deteriorated by repeating the cycle consisting of a plurality of times.

より具体的には、上記複合劣化試験方法において、
（ａ）の工程では、塩化ナトリウム濃度５％の塩水を、温度３５℃に保った槽内で、１時間あたり水平面積８０ｃｍ2 に１．５±０．５ｍｌの噴霧量でＮ時間噴霧し、
（ｂ）の工程では、ブラックパネル温度８０±１０℃、槽内湿度５０％を保持しつつ、波長範囲が２９５〜７８０ｎｍで、３３０〜３９０ｎｍの波長域における照射強度が７５±２５ｍＷ／ｃｍ2 の紫外線を、４Ｎ〜１２Ｎ時間照射するとともに、２時間おきに２分間の散水を行って試料の表面を洗浄し、
（ｃ）の工程では、Ｎ時間、槽内温度を５０℃、槽内湿度を９５％以上に保持する、
のが好ましい。 More specifically, in the above composite deterioration test method,
In the step (a), salt water having a sodium chloride concentration of 5% is sprayed in a horizontal area of 80 cm 2 per hour at a spray amount of 1.5 ± 0.5 ml for N hours in a tank maintained at a temperature of 35 ° C.
In the step (b), while maintaining the black panel temperature of 80 ± 10 ° C. and the humidity in the tank of 50%, the wavelength range is 295 to 780 nm, and the irradiation intensity in the wavelength range of 330 to 390 nm is 75 ± 25 mW / cm 2 . UV light is irradiated for 4N to 12N hours, and the surface of the sample is washed by spraying water every 2 hours for 2 minutes,
In the step (c), the temperature in the tank is maintained at 50 ° C. and the humidity in the tank at 95% or more for N hours.
Is preferred.

さらには、上記複合劣化試験方法において、Ｎ＝２とし、
（ａ）の工程を２時間、
（ｂ）の工程を１６時間、
（ｃ）の工程を２時間、
実施するのが好ましい。かかる条件での実施により、実際の屋外暴露に極めて近似した劣化状態を効率的に再現することができる。 Furthermore, in the above composite deterioration test method, N = 2,
Step (a) for 2 hours,
(B) for 16 hours,
Step (c) is performed for 2 hours,
It is preferable to carry out. By carrying out under such conditions, it is possible to efficiently reproduce a deterioration state very close to actual outdoor exposure.

また、本発明は、上記複合劣化試験方法による劣化の度合いを客観的に数値化するための指標として、試料の劣化状態を、
（ア）塗膜の剥離、割れ、膨れ、腐食等にかかる外観と、
（イ）ＪＩＳ・Ｚ８７３０により測定した試験前後の表面色の色差と、
（ウ）ＪＩＳ・Ｚ８７４１により測定した試験前後の光沢度の残存率と、
（エ）表面−界面切削法（ＳＡＩＣＡＳ）による塗膜の剥離強度と、
（オ）表面−界面切削法（ＳＡＩＣＡＳ）による塗膜のみなしせん断強度と、
からなる５項目により評価することを特徴とする。 Further, the present invention provides the deterioration state of the sample as an index for objectively quantifying the degree of deterioration by the composite deterioration test method.
(A) Appearance of peeling, cracking, swelling, corrosion, etc.
(B) The color difference of the surface color before and after the test measured according to JIS Z8730,
(C) Gloss residual rate before and after the test measured according to JIS Z8741
(D) The peel strength of the coating film by the surface-interface cutting method (SAICAS),
(E) Only the coating film by surface-interface cutting method (SAICAS) and shear strength,
It is characterized by the evaluation based on 5 items.

上述のように構成される本発明の複合劣化試験方法では、長時間の紫外線照射により、塗料や樹脂塗材を構成する高分子化合物の鎖が徐々に破壊され、塗膜が硬化して割れや変色などの化学的劣化が生じる。また、紫外線照射中に塩分が乾燥して、上記の化学的劣化と鋼板の腐食とが複合的・相乗的に進行する。このような複合的作用により、実際の屋外暴露環境に近い劣化状態を比較的短時間で再現することができる。   In the composite deterioration test method of the present invention configured as described above, the polymer compound chain constituting the coating material or the resin coating material is gradually broken by ultraviolet irradiation for a long time, and the coating film is cured and cracked. Chemical deterioration such as discoloration occurs. Further, the salt content is dried during the ultraviolet irradiation, and the chemical deterioration and the corrosion of the steel sheet proceed in a complex and synergistic manner. By such a combined action, a deterioration state close to an actual outdoor exposure environment can be reproduced in a relatively short time.

また、特に請求項４の構成にかかる複数種類の指標を採用することにより、劣化の度合いを客観的に数値化して比較することが可能になる。   In particular, by adopting a plurality of types of indices according to the configuration of claim 4, it is possible to objectively quantify the degree of deterioration and compare them.

以下、本発明の実施の形態について図を参照して説明する。   Hereinafter, embodiments of the present invention will be described with reference to the drawings.

［試験装置］
図１は、本発明の複合劣化試験を実施するための試験装置の基本構成を示した概念図である。この試験装置１は、散水装置２及び照射装置３を組み込んだ恒温恒湿槽４内に、塗装鋼板の試料９が定置されるように構成される。恒温恒湿槽４は、電源部５に接続された温湿度制御装置６によって、槽内の温度及び湿度を自由に変化させ、かつ一定の温湿度状態を維持できるようになっている。 [Test equipment]
FIG. 1 is a conceptual diagram showing the basic configuration of a test apparatus for carrying out the combined deterioration test of the present invention. The test apparatus 1 is configured such that a sample 9 of a coated steel plate is placed in a constant temperature and humidity chamber 4 in which a watering device 2 and an irradiation device 3 are incorporated. The temperature and humidity chamber 4 is configured to freely change the temperature and humidity in the chamber and maintain a constant temperature and humidity state by a temperature and humidity control device 6 connected to the power supply unit 5.

散水装置２は、中性水、酸性水（希硫酸、希塩酸、蓚酸など）、塩水など、成分の異なる複数種類の水を供給することのできる給水部２１を備える。それらの水は、定置される試料９の上方に設けられたノズル部２２から試料９に向けて霧状に散布されたり、あるいは槽内全体に向けて噴霧される。   The watering device 2 includes a water supply unit 21 that can supply a plurality of types of water having different components such as neutral water, acidic water (such as dilute sulfuric acid, dilute hydrochloric acid, and oxalic acid), and salt water. These waters are sprayed in the form of a mist toward the sample 9 from the nozzle portion 22 provided above the sample 9 to be placed, or sprayed toward the entire tank.

照射装置３は、試料９に正対する位置にメタルハライドランプ３１を備え、このメタルハライドランプ３１から試料９に向けて、特に紫外光（短波長）領域に卓越したエネルギーを有する光が照射される。この試験装置の具体的な仕様を、下記表１に示す。このような試験装置により、任意の時間及びサイクルで、紫外線照射、塩水噴霧、散水、湿潤、結露、休止、乾燥等のモードを連続的に行うことが可能になる。   The irradiation device 3 includes a metal halide lamp 31 at a position directly facing the sample 9, and light having excellent energy is irradiated from the metal halide lamp 31 toward the sample 9, particularly in the ultraviolet light (short wavelength) region. Specific specifications of this test apparatus are shown in Table 1 below. Such a test apparatus makes it possible to continuously perform modes such as ultraviolet irradiation, salt spray, water spray, wetting, condensation, pause, and drying at an arbitrary time and cycle.

Figure 2008185502
Figure 2008185502

上記のような試験装置を用いて本発明者らが実施した試験結果を以下に示す。   The test results conducted by the present inventors using the above test apparatus are shown below.

［試料］
本発明者らは、表２に示す５種類の塩ビ塗装鋼板について下記条件での屋外暴露を行っており、１、２、３、４、７年暴露後の各回収品を入手していた。また、これら５種類の塗装鋼板と同一仕様の新品（同一ロットの冷暗所保管品）を保管していた。そこで、これらの新品を試料として供試した。
暴露地：鳥取市湖山町西４丁目（離岸距離：約８００ｍ）
暴露期間：１９９４年１１月〜２００１年１１月（最長７年間）
暴露方法：南面に３０度の傾斜で定置 [sample]
The present inventors have performed outdoor exposure under the following conditions for the five types of polyvinyl chloride coated steel sheets shown in Table 2, and obtained each recovered product after exposure for 1, 2, 3, 4, and 7 years. In addition, these five kinds of coated steel sheets were stored in the same specifications as new articles (cold dark place storage products of the same lot). Therefore, these new products were used as samples.
Exposed location: Koyamacho Nishi 4-chome, Tottori City (distance to shore: about 800m)
Exposure period: November 1994 to November 2001 (up to 7 years)
Exposure method: Placed on the south with a 30 degree inclination

Figure 2008185502
Figure 2008185502

塗装鋼板の試料としては、切断端面、曲げ加工、傷部での腐食を考慮して、図２に示すような形状及び寸法とした。試料９の一部に断面Ｕ字状の折り曲げ密着部９１を形成するとともに、試料の表面２カ所にＸ字状のクロスカット９２を入れ、一方のクロスカット９２の裏側から鋼球ポンチによるエリクセン９３を形成した。また、試料９の切断端面については、バリの向きによって耐食性に違いが生じる可能性があるため、表裏の向きを変えてシャーリング裁断した。図中に白三角印を付した端面は表面から、黒三角印を付した端面は裏面から裁断したことを示す。なお、上記１〜７年間の屋外暴露品についても同じ形状の試料を用いた。   As a sample of the coated steel plate, the shape and dimensions as shown in FIG. 2 were taken in consideration of the cut end face, bending work, and corrosion at the scratch. A bent contact portion 91 having a U-shaped cross section is formed in a part of the sample 9, and X-shaped crosscuts 92 are inserted into two portions of the surface of the sample 9. Formed. Further, the cut end face of the sample 9 was subjected to shearing cutting by changing the direction of the front and back since there is a possibility that the corrosion resistance varies depending on the direction of burrs. In the figure, the end face marked with a white triangle mark is cut from the front surface, and the end face marked with a black triangle mark is cut from the back face. In addition, the sample of the same shape was used also about the outdoor exposure goods for the said 1-7 years.

［試験条件］
下記の表３に示すＡ〜Ｃの３種類の条件で、（ａ）塩水噴霧−（ｂ）紫外線照射−（ｃ）湿潤の工程を繰り返す複合サイクル試験を実施した。 [Test conditions]
Under the three conditions A to C shown in Table 3 below, a combined cycle test was repeated in which the steps of (a) salt spray, (b) ultraviolet irradiation, and (c) wetting were repeated.

Figure 2008185502
Figure 2008185502

条件Ａは、既に多くの分野での試験実績があるＪＡＳＯ（日本自動車技術会規格）Ｍ６０９−９１の複合サイクル試験（塩水噴霧→乾燥→湿潤のサイクル試験。）における乾燥モードを、そのまま紫外線照射モードに置き換えたものである。塩水噴霧工程では、塩化ナトリウム濃度５％の塩水（または人工海塩の水溶液）を、温度３５℃に保った槽内で、１時間あたり水平面積８０ｃｍ2 に１．５±０．５ｍｌの噴霧量で２時間噴霧した。続く
紫外線照射工程では、槽内のブラックパネル温度８０±１０℃、槽内湿度５０％を保持しつつ、波長範囲が２９５〜７８０ｎｍ（ＫＦ−１フィルター使用）で、３３０〜３９０ｎｍの波長域における照射強度が７５±２５ｍＷ／ｃｍ2 （ウシオ電機製ＵＩＴ−１０１による測定）の紫外線を４時間照射した。このとき、２時間おきに２分間の散水を行って、槽内湿度を５０％以上に保持した。続く湿潤工程では、５０℃の水を２時間噴霧して槽内湿度を９５％以上に保持した。 Condition A is the UV irradiation mode as it is in the combined cycle test (salt spray → dry → wet cycle test) of JASO (Japan Automobile Manufacturers Association Standard) M609-91, which has already been tested in many fields. It has been replaced with. In the salt water spraying step, a spray amount of 1.5 ± 0.5 ml per hour on a horizontal area of 80 cm 2 in a tank maintained at a temperature of 35 ° C. with a sodium chloride concentration of 5% (or an artificial sea salt aqueous solution). For 2 hours. In the subsequent UV irradiation step, irradiation in the wavelength range of 330 to 390 nm with a wavelength range of 295 to 780 nm (using a KF-1 filter) while maintaining a black panel temperature of 80 ± 10 ° C. and a humidity of 50% in the bath Ultraviolet rays having an intensity of 75 ± 25 mW / cm 2 (measured with UIT-101 manufactured by USHIO INC.) Were irradiated for 4 hours. At this time, watering was performed every 2 hours for 2 minutes, and the humidity in the tank was maintained at 50% or more. In the subsequent wetting step, 50 ° C. water was sprayed for 2 hours to maintain the humidity in the tank at 95% or more.

条件Ｂは、塩水噴霧工程及び湿潤工程については上記条件Ａと同一で、紫外線照射時間を条件Ａの２倍である８時間とした。   Condition B was the same as Condition A above for the salt spraying step and the wetting step, and the ultraviolet irradiation time was 8 hours, which is twice that of Condition A.

条件Ｃは、塩水噴霧工程及び湿潤工程については上記条件Ａ、Ｂと同一で、紫外線照射時間を条件Ａの４倍である１６時間とした。   The condition C was the same as the above conditions A and B for the salt spray step and the wetting step, and the ultraviolet irradiation time was 16 hours, which is four times the condition A.

ＪＡＳＯ・Ｍ６０９−９１の複合サイクル試験では、５サイクルが都市・海岸地帯の大気暴露１年に相当するといわれている。このため、５サイクルを暴露相当年数１年として、条件Ａ、Ｂ、Ｃのいずれも、試験期間を３５サイクル（暴露相当年数７年）とした。   In the combined cycle test of JASO M609-91, it is said that 5 cycles correspond to 1 year of atmospheric exposure in cities and coastal areas. For this reason, 5 cycles were set to 1 year equivalent to exposure, and conditions A, B, and C were all set to 35 cycles (exposure equivalent years of 7 years).

［評価項目］
外観観察、色差、光沢、塗膜剥離強度、みなしせん断強度、膜厚、塗膜抵抗値を評価項目として、暴露相当年数１、２、３、４、７年経過後（塗膜剥離強度等の破壊検査については４、７年経過後）に測定を行った。それぞれの概要を以下に示す。
（ア）外観観察
塗膜の剥離・割れ・膨れ・腐食状況を目視的に観察した。
（イ）色差
試料の中央付近に測定個所３ケ所を定め、ＪＩＳ・Ｚ８７３０のＬ＊、ａ＊、ｂ＊表色系で表面色を測定した。その後、一定の試験時間経過後に試験体の表面色を同様に測定し、各時間における色差（ΔＥ）を算出した。
（ウ）光沢
試料の中央付近に測定個所３ケ所を定め、ＪＩＳ・Ｚ８７４１の光沢度（６０°鏡面反射率）を測定した。その後、一定の試験時間経過後に光沢度を同様に測定し、各時間における光沢度の残存率を算出した。
（エ）塗膜剥離強度
試料の中央付近に測定個所１ヶ所を定め、表面−界面切削法：ＳＡＩＣＡＳ（Ｓｕｒｆａｃｅ Ａｎｄ Ｉｎｔｅｒｆａｃｉａｌ Ｃｕｔｔｉｎｇ Ａｎａｌｙｓｉｓ Ｓｙｓｔｅｍ）を用いて、塗膜の剥離強度とみなしせん断強度（表層部及び内部）を測定した。
（オ）みなしせん断強度
上記と同様にＳＡＩＣＡＳを用いて、塗膜の表層部及び内部におけるみなしせん断強度を測定した。
（カ）膜厚
試料の中央付近に測定個所５ヶ所を定め、電磁膜厚計を用いて初期の膜厚を測定し、その後、一定の試験時間経過後に膜厚を同様に測定し、各時間における膜厚残存率を算出した。 [Evaluation item]
Appearance observation, color difference, gloss, paint film peel strength, deemed shear strength, film thickness, paint film resistance value as evaluation items, after exposure years 1, 2, 3, 4, 7 years (coating film peel strength etc. The destructive inspection was measured after 4 or 7 years. The outline of each is shown below.
(A) Appearance observation The peeling, cracking, swelling and corrosion of the coating film were visually observed.
(A) Color difference Three measurement points were determined near the center of the sample, and the surface color was measured using the L *, a *, b * color system of JIS Z8730. Thereafter, the surface color of the specimen was measured in the same manner after a certain test time, and the color difference (ΔE) at each time was calculated.
(C) Glossiness Three measurement points were determined near the center of the sample, and the glossiness (60 ° specular reflectance) of JIS Z8741 was measured. Thereafter, the glossiness was measured in the same manner after a certain test time, and the residual ratio of the glossiness at each time was calculated.
(D) Coating film peel strength One measurement point is set near the center of the sample, and surface-interface cutting method: SAICAS (Surface And Interfacial Cutting Analysis System) is used to determine the coating film peel strength and shear strength (surface layer part) And inside).
(E) Deemed shear strength Using SAICAS in the same manner as described above, the deemed shear strength in the surface layer portion and inside of the coating film was measured.
(F) Film thickness Five measurement points are set near the center of the sample, and the initial film thickness is measured using an electromagnetic film thickness meter. The film thickness residual ratio was calculated.

［試験結果］
条件Ａ、Ｂ、Ｃによる複合サイクル試験の各５サイクルを暴露相当年数１年とみなして、それらと屋外暴露の結果とを評価項目別に比較すると、以下のようになった。なお、屋外暴露１年経過後の色差及び光沢度の残存率に関するデータは、汚れの影響が大きかったため省略した。 [Test results]
Assuming that each of the five cycles of the combined cycle test under conditions A, B, and C was regarded as one year equivalent to exposure, the results of outdoor exposure were compared by evaluation item, and the results were as follows. Data on color difference and gloss remaining after one year of outdoor exposure were omitted because the effect of dirt was great.

（ア）外観観察
屋外暴露では、暴露期間が長くなるに従って、塩ビ皮膜の割れ、剥離、変退色や鋼板の腐食が見られた。これに対して複合サイクル試験では、進行度合いは異なるものの、条件Ａ、Ｂ、Ｃのいずれにおいても同様の現象が見られた。なかでも条件Ｃにおいて、暴露同様に塗膜の剥離と剥離部分の塗膜下での白錆が見られ、最も近似した外観が確認された。 (A) Appearance observation In outdoor exposure, cracking, peeling, discoloration, and corrosion of steel sheets were observed as the exposure period increased. On the other hand, in the combined cycle test, the same phenomenon was observed in any of the conditions A, B, and C although the degree of progress was different. In particular, under condition C, peeling of the coating film and white rust under the coating film at the peeled portion were observed as in the exposure, and the closest appearance was confirmed.

（イ）色差
試料Ｎｏ．１及びＮｏ．４についての色差の変化を、図３及び図４にそれぞれ示す。屋外暴露では、色差は２〜４年で極大となり、その後やや低下する傾向が見られた。これに対して複合サイクル試験では、条件Ｂ、Ｃで同様の傾向が見られ、特に条件Ｃでは早期（２〜３年）に色差が大きくなる傾向が見られた。条件Ａでは色差の変化が緩やかであった。 (A) Color difference Sample No. 1 and no. The change in color difference for 4 is shown in FIGS. 3 and 4, respectively. In outdoor exposure, the color difference reached a maximum in 2 to 4 years, and then tended to decrease slightly. On the other hand, in the combined cycle test, the same tendency was observed under the conditions B and C. In particular, under the condition C, the color difference tended to increase early (2 to 3 years). Under condition A, the change in color difference was gradual.

（ウ）光沢
試料Ｎｏ．１及びＮｏ．４についての光沢度の変化を、図５及び図６にそれぞれ示す。屋外暴露では、光沢度が２〜４年で大きく低下し、それ以降はあまり変化しない傾向が見られた。これに対して複合サイクル試験では、条件Ｂ、Ｃで同様の傾向が見られ、特に条件Ｃでは早期から光沢度が低下して、屋外暴露に近似した傾向が見られた。条件Ａでは光沢残存率の変化も緩やかであった。 (C) Gloss Sample No. 1 and no. The change in glossiness for No. 4 is shown in FIGS. 5 and 6, respectively. In outdoor exposure, the glossiness decreased significantly in 2 to 4 years, and after that, there was a tendency not to change much. On the other hand, in the combined cycle test, the same tendency was observed under the conditions B and C. In particular, under the condition C, the gloss decreased from an early stage, and a tendency approximated to outdoor exposure was observed. Under condition A, the change in the gloss residual ratio was also gradual.

（エ）塗膜剥離強度
試料Ｎｏ．１及びＮｏ．４についての塗膜剥離強度の変化を図７及び図８にそれぞれ示す。塗膜剥離強度は、塗膜とめっき面の界面近傍の付着力を示しており、この値が低下し始めると塗膜が剥離しやすくなっていると考えられる。試料Ｎｏ．４では、屋外暴露と条件Ｃで一旦剥離強度が増加した後、急激な低下が見られた。それ以外の試料では、屋外暴露を含めていずれの条件でも明らかな低下傾向は見られなかった。 (D) Coating film peel strength Sample No. 1 and no. The change of the coating film peeling strength about 4 is shown in FIG.7 and FIG.8, respectively. The coating film peeling strength indicates the adhesive force in the vicinity of the interface between the coating film and the plating surface, and it is considered that the coating film is easily peeled off when this value starts to decrease. Sample No. In No. 4, after the peel strength once increased under outdoor exposure and condition C, a sharp decrease was observed. The other samples did not show a clear decrease trend under any condition including outdoor exposure.

（オ）みなしせん断強度
試料Ｎｏ．１及びＮｏ．４についての表層部みなしせん断強度の変化を図９及び図１０にそれぞれ示す。表層部みなしせん断強度は、塗膜表層部の劣化（樹脂の硬化や崩壊等）の程度を示すと考えられる。表層部みなしせん断強度については、試料及び条件によりバラツキが大きく、明らかな傾向は見られなかった。また、全体的には屋外暴露と条件Ｃの傾向が近いと言えるが、塗膜剥離強度ほど明確ではなかった。 (E) Deemed shear strength Sample No. 1 and no. FIG. 9 and FIG. 10 show changes in the surface layer assumed shear strength for No. 4 respectively. The surface layer deemed shear strength is considered to indicate the degree of deterioration (curing or disintegration of the resin) of the coating surface layer. The surface layer deemed shear strength varied greatly depending on the sample and conditions, and no obvious tendency was observed. Moreover, although it can be said that the outdoors exposure and the tendency of the condition C are close as a whole, it was not as clear as coating film peeling strength.

（カ）膜厚
屋外暴露では、暴露期間が長くなるに従って徐々に膜厚の減少が見られた。これに対して複合サイクル試験でも同様の現象が見られたが、条件Ａ、Ｂでは屋外暴露に較べて変化が非常に緩やかであった。 (F) Film thickness In outdoor exposure, the film thickness gradually decreased as the exposure period increased. On the other hand, the same phenomenon was also observed in the combined cycle test, but under conditions A and B, the change was very gradual compared to outdoor exposure.

（まとめ）
上記の試験結果を総合すれば、色差、光沢、塗膜剥離強度、表層部みなしせん断強度の各項目において、条件Ｃによる結果が屋外暴露と最も近似した傾向を示した。したがって、塗装鋼板の劣化を再現する試験条件としては、今回実施した中では条件Ｃが最適であると考えられる。 (Summary)
When the above test results were combined, the results under Condition C showed the tendency closest to that of outdoor exposure in each of the items of color difference, gloss, coating film peel strength, and surface layer deemed shear strength. Therefore, it is considered that the condition C is the most suitable test condition for reproducing the deterioration of the coated steel sheet.

また、今後様々な試料に対して物性評価をおこなう場合の項目としては、特徴的な値を示すこと及び比較的測定が簡便であること等から、色差、光沢、塗膜剥離強度の３項目、または、これにみなしせん断強度を加えた４項目が適切と考えられる。   In addition, as an item for performing physical property evaluation on various samples in the future, three items of color difference, gloss, and coating film peel strength are shown because it shows characteristic values and is relatively easy to measure. Or 4 items which considered this and added shear strength are considered appropriate.

本発明の複合劣化試験を実施するための試験装置の基本構成を示した概念図である。It is the conceptual diagram which showed the basic composition of the testing apparatus for implementing the composite deterioration test of this invention. 本発明の複合劣化試験に使用する塗装鋼板の試料の形状を示した正面図及び側面図である。It is the front view and side view which showed the shape of the sample of the coated steel plate used for the composite deterioration test of this invention. 本発明の複合劣化試験の実施例にかかる試料Ｎｏ．１の色差の変化を示すグラフである。Sample No. according to the example of the composite deterioration test of the present invention. 2 is a graph showing changes in color difference of 1. 同じく、試料Ｎｏ．４の色差の変化を示すグラフである。Similarly, sample no. 4 is a graph showing changes in color difference of 4; 本発明の複合劣化試験の実施例にかかる試料Ｎｏ．１の光沢度の変化を示すグラフである。Sample No. according to the example of the composite deterioration test of the present invention. 2 is a graph showing a change in glossiness of 1. 同じく、試料Ｎｏ．４の光沢度の変化を示すグラフである。Similarly, sample no. 4 is a graph showing a change in glossiness of No. 4; 本発明の複合劣化試験の実施例にかかる試料Ｎｏ．１の塗膜剥離強度の変化を示すグラフである。Sample No. according to the example of the composite deterioration test of the present invention. It is a graph which shows the change of the coating-film peeling strength of 1. 同じく、試料Ｎｏ．４の塗膜剥離強度の変化を示すグラフである。Similarly, sample no. 4 is a graph showing changes in coating film peel strength of No. 4; 本発明の複合劣化試験の実施例にかかる試料Ｎｏ．１の表層部みなしせん断強度の変化を示すグラフである。Sample No. according to the example of the composite deterioration test of the present invention. 1 is a graph showing a change in shear strength considered as a surface layer portion of 1; 同じく、試料Ｎｏ．４の表層部みなしせん断強度の変化を示すグラフである。Similarly, sample no. 4 is a graph showing changes in the assumed shear strength of the surface layer 4 of FIG.

符号の説明Explanation of symbols

１ 試験装置
２ 散水装置
３ 照射装置
３１ メタルハライドランプ
４ 恒温恒湿槽
６ 温湿度制御装置
９ 試料 DESCRIPTION OF SYMBOLS 1 Test apparatus 2 Watering apparatus 3 Irradiation apparatus 31 Metal halide lamp 4 Constant temperature and humidity tank 6 Temperature and humidity control apparatus 9 Sample

Claims (4)

任意の温湿度を維持しうる恒温恒湿槽内に塗装鋼板の試料を定置し、この槽内で上記試料に対し、
（ａ）塩水を噴霧する工程と、
（ｂ）メタルハライドランプによる紫外線を連続的に照射するとともに、一定時間おきに散水して試料の表面を洗浄する工程と、
（ｃ）紫外線照射を停止して、温湿度制御装置により槽内を高湿に保ち、湿潤させる工程と、
からなるサイクルを複数回繰り返して試料を劣化させることを特徴とする複合劣化試験方法。 Place the sample of the coated steel plate in a constant temperature and humidity chamber that can maintain any temperature and humidity.
(A) spraying salt water;
(B) a step of continuously irradiating with ultraviolet rays from a metal halide lamp and spraying water every predetermined time to clean the surface of the sample;
(C) stopping ultraviolet irradiation, keeping the inside of the tank at a high humidity by the temperature and humidity control device, and moistening;
A compound deterioration test method characterized in that a sample is deteriorated by repeating a cycle consisting of a plurality of times. 請求項１記載の複合劣化試験方法において、
（ａ）の工程では、塩化ナトリウム濃度５％の塩水を、温度３５℃に保った槽内で、１時間あたり水平面積８０ｃｍ2 に１．５±０．５ｍｌの噴霧量でＮ時間噴霧し、
（ｂ）の工程では、ブラックパネル温度８０±１０℃、槽内湿度５０％を保持しつつ、波長範囲が２９５〜７８０ｎｍで、３３０〜３９０ｎｍの波長域における照射強度が７５±２５ｍＷ／ｃｍ2 の紫外線を、４Ｎ〜１２Ｎ時間照射するとともに、２時間おきに２分間の散水を行って試料の表面を洗浄し、
（ｃ）の工程では、Ｎ時間、槽内温度を５０℃、槽内湿度を９５％以上に保持する、
ことを特徴とする複合劣化試験方法。 In the compound deterioration test method according to claim 1,
In the step (a), salt water having a sodium chloride concentration of 5% is sprayed in a horizontal area of 80 cm 2 per hour at a spray amount of 1.5 ± 0.5 ml for N hours in a tank maintained at a temperature of 35 ° C.
In the step (b), while maintaining the black panel temperature of 80 ± 10 ° C. and the humidity in the tank of 50%, the wavelength range is 295 to 780 nm, and the irradiation intensity in the wavelength range of 330 to 390 nm is 75 ± 25 mW / cm 2 . UV light is irradiated for 4N to 12N hours, and the surface of the sample is washed by spraying water every 2 hours for 2 minutes,
In the step (c), the temperature in the tank is maintained at 50 ° C. and the humidity in the tank at 95% or more for N hours.
A composite deterioration test method characterized by the above. 請求項２記載の複合劣化試験方法において、Ｎ＝２とし、
（ａ）の工程を２時間、
（ｂ）の工程を１６時間、
（ｃ）の工程を２時間、
実施することを特徴とする複合劣化試験方法。 In the combined deterioration test method according to claim 2, N = 2,
Step (a) for 2 hours,
(B) for 16 hours,
Step (c) is performed for 2 hours,
A composite deterioration test method characterized by being carried out. 請求項１〜３のいずれかに記載の複合劣化試験方法において、試料の劣化状態を、
（ア）塗膜の剥離、割れ、膨れ、腐食等にかかる外観と、
（イ）ＪＩＳ・Ｚ８７３０により測定した試験前後の表面色の色差と、
（ウ）ＪＩＳ・Ｚ８７４１により測定した試験前後の光沢度の残存率と、
（エ）表面−界面切削法（ＳＡＩＣＡＳ）による塗膜の剥離強度と、
（オ）表面−界面切削法（ＳＡＩＣＡＳ）による塗膜のみなしせん断強度と、
からなる５項目により評価することを特徴とする複合劣化試験方法。 The composite deterioration test method according to any one of claims 1 to 3, wherein the deterioration state of the sample is
(A) Appearance of peeling, cracking, swelling, corrosion, etc.
(B) The color difference of the surface color before and after the test measured according to JIS Z8730,
(C) Gloss residual rate before and after the test measured according to JIS Z8741
(D) The peel strength of the coating film by the surface-interface cutting method (SAICAS),
(E) Only the coating film by surface-interface cutting method (SAICAS) and shear strength,
A composite deterioration test method characterized by evaluation based on 5 items.
JP2007020530A 2007-01-31 2007-01-31 Combined degradation test method for painting steel plate Pending JP2008185502A (en)

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