TW201821786A - Coating corrosion accelerating test method capable of shortening the test cycle by generating a special corrosion accelerating effect different from the corrosion factor reaction - Google Patents
Coating corrosion accelerating test method capable of shortening the test cycle by generating a special corrosion accelerating effect different from the corrosion factor reaction Download PDFInfo
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本發明是有關於一種腐蝕加速試驗方法，且特別是有關於一種金屬表面防護塗裝的實驗室加速腐蝕試驗方法。 The invention relates to an accelerated corrosion test method, and more particularly to a laboratory accelerated corrosion test method for metal surface protective coating.
金屬表面經常以塗裝的方式達到腐蝕防護之目的。針對塗裝耐蝕性的試驗方法主要有兩種，第一種是現場暴露試驗，試驗的環境條件與實際使用環境基本相同，能夠適當反映環境腐蝕因子的綜合影響。該試驗方法的結果雖然真實可靠，但試驗周期往往長達數年以上。第二種是實驗室加速腐蝕試驗，試驗條件及腐蝕因子可以嚴格控制和調整，試驗周期相對較短，而且試驗結果的再現性較佳。 Metal surfaces are often coated for corrosion protection purposes. There are two main test methods for coating corrosion resistance. The first is an on-site exposure test. The environmental conditions of the test are basically the same as the actual use environment, which can appropriately reflect the comprehensive influence of environmental corrosion factors. Although the results of this test method are true and reliable, the test cycle often takes more than several years. The second is the accelerated laboratory corrosion test. The test conditions and corrosion factors can be strictly controlled and adjusted. The test cycle is relatively short and the test results are more reproducible.
然而，目前業界習用的實驗室加速腐蝕試驗方法主要是依賴水分、鹽分、氧或其它腐蝕因子所產生的反應，仍存在諸多缺點。首先，該試驗方法的試驗周期仍然極長，例如，廣泛使用的中性鹽霧試驗可達1000小時，即使是添加了化學物質的酸性鹽霧試驗，也需要數百小時。其次，目前的實驗室加速腐蝕試驗方法主要藉由目視觀察試樣的腐蝕形貌或藉由重量損失以評鑑試樣的耐蝕性，然而，該目視觀察法缺乏定量標準，失重法則容易受到塗層吸收水分問題而影響試驗的精確度，而且，觀察法和失重法皆無法在試驗過程中獲得試樣腐蝕變化的即時資訊，不能精確掌握塗裝發生腐蝕的啟始時間。再者，目前的實驗室 加速腐蝕試驗方法普遍需要使用專門的試驗設備以達到噴霧、循環或控溫效果，不但成本較高，而且耗費能源，若再添加化學物質以加速腐蝕反應則更容易產生化學污染問題。 However, the laboratory accelerated corrosion test method currently used in the industry is mainly dependent on the reaction caused by moisture, salt, oxygen or other corrosion factors, and there are still many shortcomings. First of all, the test cycle of this test method is still extremely long. For example, the widely used neutral salt spray test can reach 1000 hours, and even the acid salt spray test with added chemicals requires hundreds of hours. Secondly, the current laboratory accelerated corrosion test method mainly evaluates the corrosion resistance of the sample by visual observation of the corrosion morphology of the sample or by weight loss. However, the visual observation method lacks a quantitative standard and the weight loss method is susceptible to coating. The problem that the layer absorbs water affects the accuracy of the test. Moreover, neither the observation method nor the weight loss method can obtain real-time information on the corrosion change of the sample during the test, and it is impossible to accurately grasp the start time of the corrosion of the coating. Furthermore, the current laboratory accelerated corrosion test methods generally require the use of special test equipment to achieve spray, cycle or temperature control effects, which is not only costly but also consumes energy. It is easier to produce chemicals if additional chemicals are added to accelerate the corrosion reaction. Chemical pollution problems.
由此可見，目前的實驗室加速腐蝕試驗方法仍有諸多缺失，而亟待加以改良，有鑑於此，業界需要一種能夠同時達到迅速、低成本、即時監測和節能環保目標的實驗室加速腐蝕試驗方法，為此，本發明乃針對上述需求，積極研究加以改良創新，終於突破傳統舊有之試驗方法，研發完成本件塗裝加速腐蝕試驗方法。 It can be seen that there are still many shortcomings in the current laboratory accelerated corrosion test methods, which need to be improved. In view of this, the industry needs a laboratory accelerated corrosion test method that can simultaneously achieve rapid, low-cost, real-time monitoring and energy conservation and environmental protection goals. To this end, the present invention is directed to the above-mentioned needs, actively researches and improves and innovates, and finally breaks through the traditional and old test methods, and develops and completes the coating accelerated corrosion test method.
本發明之目的在於提供一種塗裝加速腐蝕試驗方法，其可產生不同於腐蝕因子反應的特殊加速腐蝕效果，可縮短試驗周期。 The purpose of the present invention is to provide a coating accelerated corrosion test method, which can produce a special accelerated corrosion effect different from the response of the corrosion factor, and can shorten the test cycle.
本發明之次一目的在於提供一種塗裝加速腐蝕試驗方法，其可避免使用專門的試驗設備，可降低試驗成本並且達到節能環保。 A secondary objective of the present invention is to provide a method for accelerated corrosion testing of coatings, which can avoid the use of special testing equipment, can reduce testing costs, and achieve energy conservation and environmental protection.
本發明之又一目的在於提供一種塗裝加速腐蝕試驗方法，其具備即時監測功能以精確掌握塗裝的腐蝕起始時間，可提升評鑑塗裝試樣耐蝕性能力的準確性。 Another object of the present invention is to provide an accelerated corrosion test method for coatings, which has a real-time monitoring function to accurately grasp the corrosion initiation time of the coating, and can improve the accuracy of evaluating the corrosion resistance of the coating samples.
根據本發明之上述目的，提出一種塗裝加速腐蝕試驗方法，包括以下步驟。首先，提供試驗裝置，且試驗裝置包含附著式試驗槽、密封圈、高電位模組、參考電極及電位監測裝置。接著，進行塗裝試樣設置步驟，以將附著式試驗槽設置在塗裝試樣表面的適當區域。隨後，進行高電位模組設置步驟，以將一或若干惰性電極組合成為高電位模組。然後，進行加速腐蝕與監測步驟，利用 高電位模組與塗裝試樣之間的電位差，以加速塗裝試樣在電解液中的腐蝕反應，並且在加速腐蝕過程中即時監測塗裝試樣的複合電位。最後，進行判斷步驟，利用複合電位的轉折點來決定塗裝試樣的腐蝕起始時間，以判斷比較塗裝試樣的耐蝕性。 According to the above-mentioned object of the present invention, a coating accelerated corrosion test method is provided, which includes the following steps. First, a test device is provided, and the test device includes an attached test tank, a seal ring, a high-potential module, a reference electrode, and a potential monitoring device. Next, a coating sample setting step is performed to set an adhesion test tank in an appropriate area on the surface of the coating sample. Subsequently, a high-potential module setting step is performed to combine one or several inert electrodes into a high-potential module. Then, the accelerated corrosion and monitoring steps are performed. The potential difference between the high-potential module and the coating sample is used to accelerate the corrosion reaction of the coating sample in the electrolyte, and the coating sample is monitored immediately during the accelerated corrosion process. Compound potential. Finally, a judging step is performed, and the turning point of the composite potential is used to determine the corrosion initiation time of the coating sample, so as to judge the corrosion resistance of the comparative coating sample.
上述之附著式試驗槽採用壓克力、塑膠或其他非金屬材料加工製成；上述之密封圈可以是採用分離式密封結構設計，也可以是採用固定式密封結構設計；所述之分離式密封結構設計係使用O型橡膠圈、壓緊彈簧和固定螺栓而達成將附著式試驗槽與試樣密切結合之目的，以在試樣表面的局部區域形成一個密封的電解池；所述之固定式密封結構設計則是使用黏著劑將附著式試驗槽與試樣直接黏合，以形成一密封的電解池，所述之黏著劑係選自矽膠、環氧樹脂、丙烯酸聚合物。熟習此技藝者所熟知，在塗裝製程中，由於塗料的流動性問題以及靜電吸附的不均勻，塗裝試樣的邊緣區域非常容易產生塗裝缺陷，因而影響習用腐蝕試驗方法的準確性，藉由上述之附著式試驗槽和密封圈，能夠選擇塗裝試樣的受測試區域，避免邊緣效應對於塗裝腐蝕試驗結果造成的干擾，可有效提升塗裝耐蝕性試驗的準確性。 The above-mentioned attached test groove is made of acrylic, plastic or other non-metal materials; the above-mentioned sealing ring can be designed with a separate sealing structure, or it can be designed with a fixed sealing structure; the above-mentioned separated seal The structural design uses O-shaped rubber rings, compression springs and fixing bolts to achieve the purpose of closely combining the attached test slot with the sample to form a sealed electrolytic cell in a local area of the sample surface; the fixed type The design of the sealing structure is to use an adhesive to directly attach the attached test cell to the sample to form a sealed electrolytic cell. The adhesive is selected from the group consisting of silicone, epoxy, and acrylic polymer. Those skilled in the art are well aware that during the coating process, due to the fluidity of the coating and the uneven electrostatic adsorption, the edge area of the coating sample is very prone to coating defects, which affects the accuracy of the conventional corrosion test method. With the above-mentioned attachment test groove and sealing ring, the test area of the coating sample can be selected, interference of the edge effect on the result of the coating corrosion test can be avoided, and the accuracy of the coating corrosion resistance test can be effectively improved.
上述之高電位模組的組成，包括一或若干惰性電極、一固定夾具以及一電極引線；所述之惰性電極係選自貴金屬、鈍態金屬、碳材、導電高分子材料之其中任一種或其組合，其中該惰性電極在電解液中能夠具有相對高的開路電位而且不容易腐蝕；使用固定夾具聯結一或若干惰性電極以形成高電位模組，再經由電極引線與塗裝試樣連接，一方面可以利用高電位模組與塗裝試樣之間的電位差以加速塗裝腐蝕反應，另一方面監測兩者連接形成的複合電位之轉折變化，判斷出塗裝腐蝕的起始時間，為塗裝的耐蝕性提供一精確定量的評估指 標；其中該高電位模組可供電化學反應的面積與塗裝受測試的面積比值以0.3至3.0為宜，當低於0.3將會因為高電位模組的反應面積不足而降低塗裝加速腐蝕的效果，反之，當高於3.0雖然較大的反應面積有助於加速腐蝕反應，但是將會產生非常穏定的電位而降低了複合電位的變化量以及電位監測效果。 The composition of the above-mentioned high-potential module includes one or several inert electrodes, a fixing jig, and an electrode lead; the inert electrode is selected from any one of precious metals, passive metals, carbon materials, conductive polymer materials, or The combination, wherein the inert electrode can have a relatively high open circuit potential in the electrolyte and is not easy to corrode; a fixed fixture is used to connect one or more inert electrodes to form a high potential module, and then connected to the coating sample through the electrode lead, On the one hand, the potential difference between the high-potential module and the coating sample can be used to accelerate the coating corrosion reaction. On the other hand, the turning of the composite potential formed by the connection between the two can be monitored to determine the start time of coating corrosion. The corrosion resistance of the coating provides an accurate and quantitative assessment index; the ratio of the area available for electrochemical reaction of the high-potential module to the area tested by the coating is preferably 0.3 to 3.0. The reaction area of the group is insufficient to reduce the effect of accelerated corrosion of the coating. Conversely, when the reaction area is higher than 3.0, although the larger reaction area helps to accelerate the corrosion reaction, It will produce a very stable potential and reduce the amount of change in composite potential and the effect of potential monitoring.
上述之參考電極係選用飽和甘汞電極、銀/氯化銀電極、白金等固態參考電極，參考電極固定於附著式試驗槽的電解池中，並且通過導電引線連接到電位監測裝置，以在加速腐蝕過程中即時監測塗裝試樣的複合電位變化情形。所述之電位監測裝置係採用多通道電壓訊號自動擷取處理裝置，能够實現同時對多組塗裝試樣進行加速腐蝕試驗和即時電位監測，並藉由該複合電位的監測結果而精確得知塗裝試樣的腐蝕起始時間，以判斷比較塗裝試樣的耐蝕性。 The above-mentioned reference electrodes are solid reference electrodes such as saturated calomel electrodes, silver / silver chloride electrodes, and platinum. The reference electrodes are fixed in the electrolytic cell of the attached test cell and connected to the potential monitoring device through conductive leads to accelerate During the corrosion process, the composite potential of the coating sample is monitored in real time. The potential monitoring device adopts a multi-channel voltage signal automatic acquisition processing device, which can realize accelerated corrosion test and real-time potential monitoring of multiple sets of coating samples at the same time, and can accurately know from the monitoring result of the composite potential The corrosion initiation time of the coating sample is used to judge and compare the corrosion resistance of the coating sample.
100‧‧‧塗裝加速腐蝕試驗方法 100‧‧‧ Painting accelerated corrosion test method
101‧‧‧試驗裝置提供步驟 101‧‧‧Procedure of test device
104‧‧‧塗裝試樣設置步驟 104‧‧‧Coating Sample Setting Procedure
105‧‧‧高電位模組設置步驟 105‧‧‧High-potential module setting steps
104‧‧‧加速腐蝕與監測步驟 104‧‧‧Accelerated corrosion and monitoring steps
105‧‧‧判斷步驟 105‧‧‧Judging steps
200‧‧‧塗裝加速腐蝕試驗裝置 200‧‧‧painting accelerated corrosion test device
210‧‧‧塗裝試樣 210‧‧‧painting sample
220‧‧‧附著式試驗槽 220‧‧‧ Attached test tank
230‧‧‧密封圈 230‧‧‧sealing ring
240‧‧‧高電位模組 240‧‧‧High Potential Module
241‧‧‧惰性電極 241‧‧‧Inert electrode
243‧‧‧固定夾具 243‧‧‧Fixed fixture
245‧‧‧電極引線 245‧‧‧ electrode lead
250‧‧‧參考電極 250‧‧‧Reference electrode
260‧‧‧電位監測裝置 260‧‧‧Potential monitoring device
第1圖係本發明塗裝加速腐蝕試驗方法之流程圖；第2圖係本發明塗裝加速腐蝕試驗裝置之結構示意圖；第3圖係本發明高電位模組之結構示意圖；第4圖係本發明之一比較例的塗裝阻抗值與浸泡時間之關係圖；第5圖係本發明之一實施例的複合電位與浸泡時間之關係圖；第6圖係本發明之一實施例的塗裝腐蝕起始時間與高電位模組之關係圖。 Figure 1 is a flowchart of the method for accelerated corrosion test of the coating of the present invention; Figure 2 is a schematic diagram of the structure of the accelerated corrosion test of the coating of the present invention; Figure 3 is a schematic diagram of the structure of the high potential module of the present invention; The relationship between the coating resistance value and the immersion time of a comparative example of the present invention; FIG. 5 is the relationship between the composite potential and the immersion time of one embodiment of the present invention; and FIG. 6 is the application of one embodiment of the present invention. The relationship diagram between the corrosion start time and the high potential module.
請參閱第1圖及第2圖，第1圖係本發明之一實施方式的一種塗裝加速腐蝕試驗方法的流程圖，而第2圖係本發明之一實施方式的一種塗裝加速腐蝕試驗裝置的結構示意圖。在塗裝加速腐蝕試驗方法100中，首先進行試驗裝置提供步驟101，以提供如第2圖所示之加速腐蝕試驗裝置200。 Please refer to FIG. 1 and FIG. 2. FIG. 1 is a flowchart of an accelerated coating corrosion test method according to an embodiment of the present invention, and FIG. 2 is an accelerated coating corrosion test method according to an embodiment of the present invention. Schematic diagram of the device. In the coating accelerated corrosion test method 100, a test device providing step 101 is first performed to provide an accelerated corrosion test device 200 as shown in FIG.
請先參閱第2圖，該加速腐蝕試驗裝置200的組成包括：塗裝試樣210、附著式試驗槽220、密封圈230、高電位模組240、參考電極250及電位監測裝置260。其中，該附著式試驗槽220係藉由該密封圈230而固定於塗裝試樣210的表面以形成一封閉電解池，該高電位模組240及該參考電極250則設置於上述之封閉電解池中，又，該高電位模組240及該塗裝試樣210的導電引線係連接至該電位監測裝置260的一訊號輸入端，而該參考電極250則連接至該電位監測裝置260的另一訊號輸入端。 Please refer to FIG. 2 first. The composition of the accelerated corrosion test apparatus 200 includes: a coating sample 210, an attached test tank 220, a sealing ring 230, a high potential module 240, a reference electrode 250, and a potential monitoring device 260. The attached test tank 220 is fixed to the surface of the coating sample 210 by the sealing ring 230 to form a closed electrolytic cell, and the high-potential module 240 and the reference electrode 250 are disposed in the closed electrolytic cell described above. In the cell, the conductive leads of the high-potential module 240 and the coating sample 210 are connected to a signal input terminal of the potential monitoring device 260, and the reference electrode 250 is connected to another of the potential monitoring device 260. A signal input.
請再次參閱第1圖及第2圖，在試驗裝置提供步驟101後，接著進行塗裝試樣設置步驟102，藉由密封圈230以將附著式試驗槽220設置在塗裝試樣210表面的適當區域以形成一封閉電解池；該密封圈230可以是使用O型橡膠圈、壓緊彈簧和固定螺栓而形成的分離式密封結構設計，便于拆解與組合，也可以是使用黏著劑而形成的固定式密封結構設計。熟習此技藝者所熟知，一般塗裝試樣的邊緣區域非常容易產生塗裝缺陷，本發明提供之該附著式試驗槽220可設置在塗裝試樣的適當區域以形成一封閉電解池，以有效避免邊緣區域的塗裝缺陷對於塗裝電化學測試和腐蝕試驗的影響；上述之封閉電解池係以含有氯離子化合物之溶液作為電解液，在一較佳實施例中，所述之電解液係以含有氯化鈉重量百分比介於3.0至5.0之間的鹽水作為電解液，試驗溫度保持在室溫，浸泡於該電解 液中之塗裝試樣的受測試面積至少大於10平方公分，且上述之適當區域係距離塗裝試樣邊緣至少大於1.5公分。 Please refer to FIG. 1 and FIG. 2 again. After the test device provides step 101, the coating sample setting step 102 is performed. The seal ring 230 is used to set the adhesion test tank 220 on the surface of the coating sample 210. A suitable area to form a closed electrolytic cell; the sealing ring 230 may be a separate sealing structure design formed by using an O-shaped rubber ring, a compression spring and a fixing bolt, which is easy to disassemble and combine, or it may be formed using an adhesive Design of fixed seal structure. Those skilled in the art are familiar with the fact that the edge area of a coating sample is very prone to coating defects. The attached test tank 220 provided by the present invention can be set in an appropriate area of the coating sample to form a closed electrolytic cell. Effectively avoiding the effects of coating defects in the edge area on the coating electrochemical test and corrosion test; the above-mentioned closed electrolytic cell uses a solution containing a chloride ion compound as an electrolyte. In a preferred embodiment, the electrolyte The salt water containing sodium chloride with a weight percentage between 3.0 and 5.0 is used as the electrolyte, the test temperature is maintained at room temperature, and the test area of the coating sample immersed in the electrolyte is at least more than 10 square centimeters, and The appropriate area is at least 1.5 cm from the edge of the coating sample.
請同時參閱第1圖及第3圖，在塗裝試樣設置步驟102後，隨後進行高電位模組設置步驟103，以將一或若干惰性電極241安置在固定夾具243中，再與電極引線245共同組合成為高電位模組240。其中，該惰性電極241係選自貴金屬、鈍態金屬、碳材、導電高分子材料之其中任一種或其組合，其能夠在電解液中保持相對較高的開路電位且其不容易腐蝕；可作為惰性電極的材質可例示金、銀、鉑、不鏽鋼、鎳、鈦、碳材、石墨片、石墨紙、聚苯胺、聚吡咯等材料，但並非限定於此；雖然第3圖之惰性電極241之形狀係繪示為平板狀，然而亦可以是其它形狀，並不侷限為平板狀。上述固定夾具243係選自不易腐蝕的金屬或非金屬材質，可將複數個惰性電極241隔離且保持一定間距較佳例如是0.5公分~2.0公分，上述間距太小時，將會影響反應物質的擴散而降低惰性電極241產生的電化學反應效能，反之，當上述間距太大時，則會因為電解液的電阻而造成高電位模組240的電位降損失；電極引線245係將高電位模組240連接至塗裝試樣210，以便後續試驗流程的進行。 Please refer to FIG. 1 and FIG. 3 at the same time. After the coating sample setting step 102, the high-potential module setting step 103 is subsequently performed to place one or several inert electrodes 241 in the fixing jig 243, and then with the electrode leads. 245 together form a high-potential module 240. Wherein, the inert electrode 241 is selected from any one or a combination of precious metals, passive metals, carbon materials, and conductive polymer materials, which can maintain a relatively high open circuit potential in the electrolyte and is not easily corroded; Examples of the material of the inert electrode include gold, silver, platinum, stainless steel, nickel, titanium, carbon materials, graphite flakes, graphite paper, polyaniline, and polypyrrole, but are not limited thereto; although the inert electrode 241 of FIG. 3 The shape is shown as a flat plate, but it can also be other shapes and is not limited to a flat plate. The fixing jig 243 is selected from non-corrosive metal or non-metallic materials. It can isolate a plurality of inert electrodes 241 and maintain a certain distance. For example, 0.5 cm to 2.0 cm. The distance is too small, which will affect the diffusion of reactive materials. The electrochemical reaction efficiency generated by the inert electrode 241 is reduced. Conversely, when the distance is too large, the potential drop of the high potential module 240 will be lost due to the resistance of the electrolyte; the electrode lead 245 will be the high potential module 240 Connected to the coating sample 210 for subsequent test procedures.
如果選用的惰性電極241在電解液中的開路電位愈高，其與塗裝試樣210之間的電位差就愈大，其加速腐蝕的趨動力亦愈大，又，當惰性電極241的總面積愈大，其組合而成的高電位模組240在電解液中所能提供的電化學反應面積就愈大，其加速腐蝕的效應亦愈大；然而，如果高電位模組240與塗裝試樣210兩者的面積比值太大，其複合電位將會因為太穩定而無法呈現足夠的變化量，因而影響塗裝加速腐蝕試驗過程中的電位監測結果以及耐蝕性判斷精確性。在一較佳實施例中，上述惰性電極241的材質較佳例如是鍍鉑鈦板、碳材、石墨 紙，其在鹽水中以飽和甘汞電極量測的電位值較佳例如是大於+0.15V，又，高電位模組240與塗裝試樣210的面積比值較佳例如是介於0.3至3.0之間，當低於0.3將會因為有效反應面積不足而降低塗裝加速腐蝕的效果，反之，上述面積比值高於3.0將會降低複合電位的變化量與監測效果。藉由調整上述之高電位模組240所含之惰性電極241的材質種類、反應面積以及間距，可獲得較佳的加速腐蝕效果與電位監測精確性。 If the open-circuit potential of the selected inert electrode 241 in the electrolyte is higher, the potential difference between the inert electrode 241 and the coating sample 210 is larger, and the tendency to accelerate corrosion is greater. Also, when the total area of the inert electrode 241 is larger, The larger the combined potential of the high-potential module 240 in the electrolyte is, the larger the electrochemical reaction area is, and the greater the effect of accelerated corrosion; however, if the high-potential module 240 and the coating test The area ratio of the two samples is too large, and the composite potential will be too stable to show a sufficient amount of change, which affects the potential monitoring results and the accuracy of corrosion resistance judgment during the accelerated corrosion test. In a preferred embodiment, the material of the inert electrode 241 is, for example, platinum-plated titanium plate, carbon material, or graphite paper, and the potential value measured by the saturated calomel electrode in saline is preferably greater than +0.15, for example. V. Also, the area ratio of the high-potential module 240 and the coating sample 210 is preferably between 0.3 and 3.0. When it is lower than 0.3, the effect of accelerated corrosion of coating will be reduced due to insufficient effective reaction area. Conversely, the above-mentioned area ratio value higher than 3.0 will reduce the change amount of the composite potential and the monitoring effect. By adjusting the material type, the reaction area, and the pitch of the inert electrode 241 included in the high-potential module 240 described above, a better accelerated corrosion effect and better potential monitoring accuracy can be obtained.
在高電位模組設置步驟103後，接著進行加速腐蝕與監測步驟104，係使用電極引線245將高電位模組240連接至塗裝試樣210，然後利用兩者之間形成的電位差作為趨動力，以加速塗裝試樣210在電解池中的腐蝕反應，同時，在加速腐蝕過程中，利用參考電極250與電位監測裝置260，以即時監測塗裝試樣210的複合電位，並根據擷取記錄的複合電位數據而繪製複合電位-時間曲線，以便後續之判斷流程的進行。 After the high-potential module setting step 103 is followed by an accelerated corrosion and monitoring step 104, an electrode lead 245 is used to connect the high-potential module 240 to the coating sample 210, and then the potential difference formed between the two is used as the driving force. In order to accelerate the corrosion reaction of the coating sample 210 in the electrolytic cell, at the same time, during the accelerated corrosion process, the reference electrode 250 and the potential monitoring device 260 are used to monitor the composite potential of the coating sample 210 in real time, and according to the extraction The recorded composite potential data is used to draw a composite potential-time curve to facilitate the subsequent determination process.
在一較佳實施例中，上述之封閉電解池係以3.0重量百分比至5.0重量百分比的鹽水作為電解液，以充分利用氯離子半徑小和穿透能力強的特性，在該電解液中，當塗裝試樣210與高電位模組240因導線連接而形成了電位差之後，就會產生特別的加速腐蝕效果；首先，在塗層尚未劣化之前的第一階段，鹽水所含的氯離子將會受到上述電位差的趨動而增大在塗層中的擴散速度，接著進入加速腐蝕的第二階段，當氯離子穿透塗層而到達金屬表面之後，將會促使塗層劣化以及金屬發生腐蝕，然後，因塗層劣化而曝露的低電位金屬與高電位模組240之間又會產生另一更大的電位差，該電位差引起的電偶效應將會大幅度增加金屬的腐蝕反應速度，最後，塗層因快速腐蝕而遭受較大規模的破壞並且釋放出可供監測的電化學訊息；可知，本發明利用高電位模組240產生之特別的加速腐 蝕效果，實際上包含了第一階段的氯離子加速塗層劣化，以及第二階段的電偶效應加速金屬腐蝕等兩種不同的加速機制，相較於一般腐蝕試驗方法，能夠有效縮減塗裝加速腐蝕的試驗周期。 In a preferred embodiment, the above-mentioned closed electrolytic cell uses 3.0% by weight to 5.0% by weight of brine as the electrolyte to fully utilize the characteristics of small chloride ion radius and strong penetrability. In this electrolyte, when After the coating sample 210 and the high-potential module 240 form a potential difference due to the wire connection, a special accelerated corrosion effect will occur. First, in the first stage before the coating has not deteriorated, the chloride ions contained in the brine will Affected by the above potential difference, the diffusion rate in the coating is increased, and then the second stage of accelerated corrosion is entered. When chloride ions penetrate the coating and reach the metal surface, it will promote the degradation of the coating and the corrosion of the metal. Then, another large potential difference will be generated between the low-potential metal exposed by the coating degradation and the high-potential module 240. The galvanic effect caused by the potential difference will greatly increase the corrosion reaction speed of the metal. Finally, The coating suffered large-scale damage due to rapid corrosion and released electrochemical information that can be monitored; it can be known that the present invention uses the special Accelerated corrosion effect, in fact, includes two different acceleration mechanisms such as accelerated chloride ion degradation in the first stage and galvanic effect in the second stage to accelerate metal corrosion. Compared with the general corrosion test method, it can effectively reduce the coating Install accelerated corrosion test cycle.
在加速腐蝕與監測步驟104後，接著進行判斷步驟105，係根據上述之複合電位-時間曲線所呈現的電位轉折變化，決定塗裝試樣的腐蝕起始時間，並利用該腐蝕起始時間作為一定量指標，以判斷塗裝試樣的耐蝕性；首先，在加速腐蝕與監測步驟104的第一階段，塗裝試樣210的塗層由於尚未遭受破壞而處於電絕緣狀態，因此，上述之複合電位必然非常接近高電位模組240的開路電位而呈現出相對較高的電位值，接著，在加速腐蝕與監測步驟104的第二階段，當塗裝試樣210因為上述之特別的加速腐蝕效果而遭受破壞之後，上述之複合電位將會由原先的高電位轉折朝向金屬的低電位移動，該複合電位轉折點的發生時間，即可視為塗裝試樣210的腐蝕起始時間；上述之腐蝕起始時間愈長，即代表該塗裝試樣的耐蝕性愈佳。 After the accelerated corrosion and monitoring step 104, a determination step 105 is then performed. Based on the potential change shown in the composite potential-time curve described above, the corrosion start time of the coating sample is determined, and the corrosion start time is used as A quantitative index to judge the corrosion resistance of the coating sample. First, in the first stage of the accelerated corrosion and monitoring step 104, the coating of the coating sample 210 is in an electrically insulated state because it has not yet been damaged. The composite potential must be very close to the open-circuit potential of the high-potential module 240 and present a relatively high potential value. Then, in the second stage of the accelerated corrosion and monitoring step 104, when the coating sample 210 is due to the above-mentioned special accelerated corrosion After the effect is damaged, the above composite potential will move from the original high potential to the low potential of the metal. The occurrence time of the composite potential turning point can be regarded as the corrosion start time of the coating sample 210; the above corrosion The longer the starting time, the better the corrosion resistance of the coating sample.
為使本技藝人士更清楚本發明之特徵，特舉例於下述之實施例，但應瞭解的是，下述之實施例僅為例示說明之用，而不應被解釋為本發明實施例之限制。 In order to make those skilled in the art clearer the features of the present invention, the following embodiments are specifically exemplified, but it should be understood that the following embodiments are only for illustrative purposes and should not be interpreted as the embodiments of the present invention. limit.
比較例1 Comparative Example 1
首先，以鋁合金作為塗裝之金屬基材，進行50、75及100微米之三種不同膜厚的聚酯(Polyester)粉體塗裝；製作完成的塗裝試樣尺寸為10×10×0.2公分。接著，針對上述三種不同膜厚之塗裝試樣進行一般腐蝕試驗，以便將上述試驗結果與本發明之塗裝加速腐蝕試驗方法作一對照比較。熟習此技藝者所熟知，鹽水浸泡試驗以及電化學交流阻抗測試係一般習用的腐蝕試驗方法，本比較例 所使用的鹽水浸泡試驗與電化學交流阻抗測試係以3.5重量百分比的鹽水作為電解液，試驗溫度保持在室溫，並於電解池中設置參考電極和輔助電極以構成常規的三極式電化學測試體系，該參考電極係選用飽和甘汞電極，該輔助電極則是選用碳棒。另外，熟習此技藝者所熟知，電化學交流阻抗測試所測得之特定的低頻率阻抗值較佳例如是|Z|0.01Hz可作為評量塗裝耐蝕性的特定指標，如果塗裝發生劣化腐蝕，其|Z|0.01Hz就會明顯降低；本發明之比較例用以量測|Z|0.01Hz的電化學交流阻抗測試設備包括恆電位儀(Potentiostat)及頻率響應分析儀(Frequency response analyzer,FRA)，測試頻率由105Hz至10-2Hz，測試電位為塗裝試樣的開路電位且電壓振幅為10mV。 First, using aluminum alloy as the coating metal substrate, coating polyester powders with three different thicknesses of 50, 75, and 100 microns; the finished coating sample size is 10 × 10 × 0.2 Cm. Next, a general corrosion test is performed on the three coating samples with different film thicknesses in order to compare the above test results with the coating accelerated corrosion test method of the present invention. Those skilled in the art are familiar with the salt water immersion test and electrochemical AC impedance test which are commonly used corrosion test methods. The salt water immersion test and electrochemical AC impedance test used in this comparative example use 3.5% by weight of saline as the electrolyte. The test temperature was maintained at room temperature, and a reference electrode and an auxiliary electrode were set in the electrolytic cell to form a conventional three-electrode electrochemical test system. The reference electrode was a saturated calomel electrode, and the auxiliary electrode was a carbon rod. In addition, those skilled in the art are familiar with the specific low-frequency impedance value measured by the electrochemical AC impedance test. For example, | Z | 0.01Hz can be used as a specific index to evaluate the corrosion resistance of the coating. Corrosion, its | Z | 0.01Hz will be significantly reduced; the comparative example of the present invention is used to measure the | Z | 0.01Hz electrochemical AC impedance test equipment including a potentiometer (Potentiostat) and a frequency response analyzer (Frequency response analyzer) , FRA), the test frequency is from 10 5 Hz to 10 -2 Hz, the test potential is the open circuit potential of the coating sample and the voltage amplitude is 10 mV.
請參閱第4圖，係上述三種不同膜厚之塗裝試樣在鹽水浸泡過程中的|Z|0.01Hz與浸泡時間之關係圖。如圖所示，在長達40天的鹽水浸泡過程中，100微米膜厚及75微米膜厚的塗裝阻抗值|Z|0.01Hz皆無降低的現象，顯示該塗裝試樣的耐蝕性維持穩定且並未發生腐蝕現象；另一方面，50微米膜厚的塗裝試樣在鹽水浸泡17天後，其|Z|0.01Hz出現了明顯的轉折下降。此一結果顯示，對於上述之耐蝕性不佳的50微米膜厚塗裝試樣而言，一般的鹽水浸泡試驗方法至少需要17天才足够促使該塗裝試樣開始發生劣化與腐蝕，且30天後才能夠以肉眼觀察到腐蝕起泡現象，因此其試驗周期需要長達30天以上；另外，為了掌握塗裝的腐蝕起始時間，在鹽水浸泡試驗過程中使用上述之電化學阻抗測試方法，能夠比習用的肉眼目視方法更提早反映塗裝試樣的腐蝕發生現象，進一步將試驗周期縮短至17天以上，但是該電化學阻抗測試方法卻需要使用專門的測試設備以及熟習此技藝的技術人員，不但物力和人力的成本較為昂貴，而且該測試方法不能夠同時針 對多個塗裝試樣進行無間斷的即時監測，無法精確地掌握塗裝試樣發生腐蝕的關鍵轉折時間。 Please refer to Figure 4 for the relationship between the | Z | 0.01Hz and the immersion time of the above three different coating thickness coating samples during salt water immersion. As shown in the figure, during the 40-day salt water immersion process, the coating resistance value | Z | 0.01Hz of 100 micron film thickness and 75 micron film thickness did not decrease, indicating that the corrosion resistance of the coating sample was maintained. Stable and no corrosion phenomenon occurred. On the other hand, after 50 days of immersion in a 50-micron-thick coating sample, its | Z | 0.01 Hz showed a significant turning down. This result shows that for the above-mentioned 50-micrometer-thick coating sample with poor corrosion resistance, the general salt water immersion test method needs at least 17 days to sufficiently promote the coating sample to begin to deteriorate and corrode, and 30 days After that, the corrosion foaming phenomenon can be observed with the naked eye, so the test cycle needs more than 30 days; In addition, in order to grasp the corrosion initiation time of the coating, the above-mentioned electrochemical impedance test method is used during the salt water immersion test. It can reflect the occurrence of corrosion of the coating sample earlier than the conventional naked eye method, and further shorten the test period to more than 17 days. However, this electrochemical impedance test method requires the use of specialized test equipment and technicians who are familiar with this technique Not only is the cost of material resources and manpower relatively expensive, but the test method cannot simultaneously perform uninterrupted real-time monitoring of multiple coating samples, and it is impossible to accurately grasp the critical turning time of corrosion of the coating samples.
實施例1 Example 1
採用與比較例相同方法製作上述三種不同膜厚之塗裝試樣以進行塗裝加速腐蝕試驗。首先，如圖1之塗裝試樣設置步驟102以及圖2之塗裝加速腐蝕試驗裝置200，於塗裝試樣210的表面安裝附著式試驗槽220，該裝附著式試驗槽220係以內徑4公分的壓克力管作為主體，並利用中性矽膠作為密封圈230以直接固定於塗裝試樣210表面的適當區域而形成一封閉的電解池，且該電解池距離試樣邊緣至少大於1.5公分，以避免邊緣區域之塗裝缺陷對於試驗結果的影響，然後，注入3.5重量百分比的鹽水於電解池以作為電解液，試驗溫度保持在室溫，並且於電解池中安置一飽和甘汞電極以作為參考電極250。 In the same manner as in the comparative example, the above three coating samples with different film thicknesses were prepared for the accelerated coating corrosion test. First, as shown in the coating sample installation step 102 in FIG. 1 and the coating accelerated corrosion test apparatus 200 in FIG. 2, an attachment test tank 220 is installed on the surface of the coating sample 210, and the attachment test tank 220 has an inner diameter. A 4 cm acrylic tube is used as the main body, and a neutral silicon gel is used as the sealing ring 230 to directly fix an appropriate area on the surface of the coating sample 210 to form a closed electrolytic cell, and the electrolytic cell is at least greater than the edge of the sample. 1.5 cm to avoid the effect of coating defects in the edge area on the test results. Then, inject 3.5% by weight of brine into the electrolytic cell as the electrolyte. The test temperature was kept at room temperature, and a saturated calomel was placed in the electrolytic cell. The electrode is used as a reference electrode 250.
接著，進行如圖1之高電位模組設置步驟103，請同時參閱第2圖與第3圖之高電位模組240，首先，將一或若干惰性電極241平行並列安裝於固定夾具243以組合成為高電位模組240，然後，將該高電位模組240浸入電解池中，並且使用電極引線245將高電位模組240連接至塗裝試樣210，注意調整高電位模組240的浸泡高度以將其反應面積與塗裝試樣210的浸入面積之間的面積比值控制在較佳例如是0.3~3.0；本實施例之該惰性電極241係選用尺寸為10×1×0.05公分的石墨紙，固定夾具243係選自不鏽鋼材質並將複數個惰性電極241的間距控制在0.5公分。 Next, perform the high-potential module setting step 103 shown in FIG. 1. Please refer to the high-potential module 240 in FIGS. 2 and 3 at the same time. First, one or several inert electrodes 241 are installed in parallel to the fixing fixture 243 in parallel for assembly. Become a high-potential module 240. Then, immerse the high-potential module 240 in the electrolytic cell, and use electrode leads 245 to connect the high-potential module 240 to the coating sample 210. Pay attention to adjust the immersion height of the high-potential module 240. The area ratio between the reaction area and the immersion area of the coating sample 210 is preferably controlled to be, for example, 0.3 to 3.0. The inert electrode 241 in this embodiment is a graphite paper with a size of 10 × 1 × 0.05 cm. The fixing jig 243 is selected from stainless steel and controls the interval between the plurality of inert electrodes 241 to 0.5 cm.
隨後，進行如圖1之加速腐蝕與監測步驟104，上述以石墨紙作為惰性電極之高電位模組240與塗裝試樣210在鹽水電解液中的開路電位相差0.2V以上，兩者連接之後，該電位差首先驅動氯離子加速穿透塗層而產生塗層劣化效 果，塗層隨後失去保護性而致使基材鋁合金曝露於電解液中，接著，由於曝露的鋁合金與石墨紙在鹽水電解液中的電位差高達1.0V，因此在上述兩種導電體之間重新形成一顯著的電偶效應而大幅增加了鋁合金的腐蝕反應速度。 Subsequently, the accelerated corrosion and monitoring step 104 shown in FIG. 1 is performed. The open-circuit potential of the above-mentioned high-potential module 240 using graphite paper as an inert electrode and the coating sample 210 in the brine electrolyte is more than 0.2V. After the two are connected, The potential difference first drives chloride ions to accelerate through the coating to produce a coating degradation effect. The coating subsequently loses its protective properties and the substrate aluminum alloy is exposed to the electrolyte. Then, the exposed aluminum alloy and graphite paper are electrolyzed in brine. The potential difference in the liquid is as high as 1.0V, so a significant galvanic effect is re-formed between the two above-mentioned conductors, which greatly increases the corrosion reaction speed of the aluminum alloy.
請參閱第2圖，在上述之塗層劣化與基材金屬的加速腐蝕過程中，利用參考電極250與電位監測裝置260，以即時監測塗裝試樣210的複合電位；在上述塗層劣化之前的第一階段，由於塗裝試樣210處於不反應的絕緣狀態，因此該階段的複合電位主要受到高電位模組240的開路電位控制，將會呈現較高的電位值，接著，在上述塗層劣化之後的第二階段，該複合電位因為同時受到高電位模組240以及基材金屬之低腐蝕電位的影響，將由原先的高電位轉折朝向低腐蝕電位移動變化，且該複合電位能否產生足够的轉折變化量與上述之面積比值有關係，諸如，當電解液中的惰性電極241與塗裝試樣210的面積比值太大，其複合電位將會因為太過穩定而無法呈現足夠的變化量，所述之足夠的變化量係指複合電位在1天內的下降幅度較佳例如是大於0.2V，適當的面積比值較佳例如是0.3~3.0能夠使得上述複合電位產生足够的轉折變化量，本實施例採用的面積比值為1.0，電位監測裝置260係採用多通道電壓訊號自動擷取處理裝置，其每一通道之訊號擷取的間隔時間為1分鐘。 Please refer to FIG. 2. During the coating degradation and accelerated corrosion of the base metal described above, the reference electrode 250 and the potential monitoring device 260 are used to monitor the composite potential of the coating sample 210 in real time. In the first stage, because the coating sample 210 is in a non-reactive insulation state, the composite potential at this stage is mainly controlled by the open-circuit potential of the high-potential module 240, and will exhibit a higher potential value. In the second stage after layer degradation, the composite potential is affected by the low corrosion potential of the high-potential module 240 and the base metal at the same time, and it will change from the original high-potential turn to a low-corrosion potential. A sufficient amount of turning change is related to the above-mentioned area ratio. For example, when the area ratio of the inert electrode 241 in the electrolyte to the coating sample 210 is too large, its composite potential will not show sufficient changes because it is too stable. The sufficient change means that the decrease range of the composite potential within 1 day is preferably greater than 0.2V, for example, and the appropriate area ratio is preferably 0. .3 ~ 3.0 can make the above composite potential produce sufficient turning change. The area ratio used in this embodiment is 1.0. The potential monitoring device 260 is a multi-channel voltage signal automatic acquisition processing device. The signal acquisition of each channel is The interval is 1 minute.
然後，進行如圖1之判斷步驟105，利用電位監測裝置260以即時擷取上述之複合電位並且繪製複合電位-時間曲線，該曲線呈現的電位轉折點如果具備了足夠的變化量，即可視為塗裝試樣的腐蝕起始時間，該腐蝕起始時間愈長，代表該塗裝的耐蝕性愈佳。 Then, the judgment step 105 shown in FIG. 1 is performed, and the potential monitoring device 260 is used to instantly capture the above composite potential and draw a composite potential-time curve. If the potential turning point shown in the curve has a sufficient change amount, it can be regarded as a coating. The corrosion initiation time of the mounted sample. The longer the corrosion initiation time, the better the corrosion resistance of the coating.
請參閱第5圖，係上述三種不同膜厚試樣在塗裝加速腐蝕試驗中的複合電位與浸泡時間之關係圖。如圖所示，在為期7天的塗裝加速腐蝕試驗過 程中，100微米膜厚及75微米膜厚的複合電位皆無明顯的變化，另一方面，50微米膜厚的塗裝在1.7天後，其複合電位出現了具備足夠變化量的轉折點，且3.5天後能夠以肉眼觀察到腐蝕起泡現象。結果顯示，本發明之塗裝加速腐蝕試驗方法能夠在小於2天的試驗周期內，有效篩選出耐蝕性不佳的50微米膜厚塗裝；與上述比較例1之大於17天的試驗周期比較，可知，本發明之塗裝加速腐蝕試驗方法與一般塗裝腐蝕試驗方法相比，兩者需要的試驗周期相差可達到10倍，從結果可以明顯看出，本發明之塗裝加速腐蝕試驗方法可以大幅縮減試驗周期，而且，藉由複合電位的轉折點，能够提供非常精確的塗裝腐蝕起始時間以作為評鑑的定量指標，提升評鑑塗裝試樣耐蝕性能力的準確性。 Please refer to Figure 5, which is the relationship between the composite potential and the immersion time of the three different film thickness samples in the accelerated coating corrosion test. As shown in the figure, during the 7-day accelerated coating corrosion test, there was no significant change in the composite potential of the 100 micron film thickness and the 75 micron film thickness. On the other hand, the 50 micron film thickness was applied after 1.7 days. The compound potential showed a turning point with a sufficient amount of change, and corrosion and blistering could be observed with the naked eye after 3.5 days. The results show that the coating accelerated corrosion test method of the present invention can effectively screen out coatings with a 50 micron film thickness with poor corrosion resistance in a test period of less than 2 days; compared with the test period of greater than 17 days in Comparative Example 1 above It can be seen that compared with the general coating corrosion test method of the present invention, the accelerated test method of the coating requires a test cycle difference of up to 10 times. From the results, it can be clearly seen that the coating accelerated corrosion test method of the present invention The test period can be greatly reduced, and the turning point of the composite potential can provide a very accurate coating corrosion start time as a quantitative index for evaluation, improving the accuracy of evaluating the corrosion resistance of the coating sample.
實施例2 Example 2
分別採用304不鏽鋼、鍍鉑鈦板、碳布、碳材作為惰性電極241的材質以進行塗裝加速腐蝕試驗，且該試驗的實施方式與實施例1相同，在此不再重述；將上述比較例1、實施例1和實施例2之50微米膜厚塗裝試樣的腐蝕起始時間相互比較，比較結果如第6圖所示，不同的惰性電極材質產生了不同的塗裝加速腐蝕效果，實施例的塗裝腐蝕起始時間分別介於0.5天至2.9天之間，明顯小於比較例的17天，另外，根據肉眼觀察的比較結果，比較例的開始起泡時間為30天，而實施例的開始起泡時間則小於4天，換言之，即便是依靠肉眼觀察作為判斷方法，實施例的試驗周期僅需要4天，由此可知，本發明的塗裝加速腐蝕試驗方法能夠在不使用昂貴或專門測試設備的狀況下，達到顯著的加速腐蝕之功能，而且，可以選用廉價材質較佳例如是碳材或石墨紙作為惰性電極241，以進一步降低試驗成本。 304 stainless steel, platinum-plated titanium plate, carbon cloth, and carbon material were used as the materials of the inert electrode 241 for the accelerated coating corrosion test, and the implementation of the test is the same as that of Example 1, and will not be repeated here; The corrosion initiation times of the 50 micron-thick coating samples of Comparative Example 1, Example 1, and Example 2 were compared with each other. The comparison results are shown in Figure 6. Different inert electrode materials produced different coating accelerated corrosion. Effect, the coating corrosion initiation time of the example is between 0.5 days and 2.9 days, which is significantly shorter than the 17 days of the comparative example. In addition, according to the comparison result observed by the naked eye, the foaming time of the comparative example is 30 days. However, the foaming time of the embodiment is less than 4 days. In other words, even if the visual observation method is used as a judgment method, the test cycle of the embodiment only needs 4 days. Therefore, it can be seen that the accelerated corrosion test method of the present invention can Under the condition of using expensive or special testing equipment, it can achieve significant acceleration corrosion function. Moreover, a cheap material such as carbon material or graphite paper can be used as the inert electrode 241 for further improvement. Step to reduce test costs.
本發明所提供之塗裝加速腐蝕試驗方法，與其他習用技術相互比較時，更具備下列優點： Compared with other conventional technologies, the accelerated corrosion test method provided by the present invention has the following advantages:
1. 本發明之塗裝加速腐蝕試驗方法具備顯著的加速腐蝕效果，能夠有效縮減試驗周期。 1. The coating accelerated corrosion test method of the present invention has a significant accelerated corrosion effect and can effectively reduce the test cycle.
2. 本發明之塗裝加速腐蝕試驗方法不需要使用昂貴或專門的測試設備及器材，能夠有效降低試驗成本及耗能。 2. The coating accelerated corrosion test method of the present invention does not require the use of expensive or specialized test equipment and equipment, and can effectively reduce the test cost and energy consumption.
3. 本發明之塗裝加速腐蝕試驗方法具備即時監測的功能，可以精確掌握塗裝試樣的腐蝕起始時間，能夠有效提升評鑑塗裝試樣耐蝕性能力的準確性。 3. The coating accelerated corrosion test method of the present invention has the function of real-time monitoring, can accurately grasp the corrosion start time of the coating sample, and can effectively improve the accuracy of evaluating the corrosion resistance of the coating sample.
上列詳細說明乃針對本創作之一可行實施例進行具體說明，惟該實施例並非用以限制本創作之專利範圍，凡未脫離本創作技藝精神所為之等效實施或變更，均應包含於本案之專利範圍中。 The above detailed description is a specific description of one of the feasible embodiments of this creation, but this embodiment is not intended to limit the scope of patents for this creation. Any equivalent implementation or change that does not depart from the spirit of this creation should be included in Within the scope of the patent in this case.
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