CN101482484B - Simulated acceleration test method for coating - Google Patents
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- CN101482484B CN101482484B CN 200910103110 CN200910103110A CN101482484B CN 101482484 B CN101482484 B CN 101482484B CN 200910103110 CN200910103110 CN 200910103110 CN 200910103110 A CN200910103110 A CN 200910103110A CN 101482484 B CN101482484 B CN 101482484B
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Abstract
The invention relates to a coating simulation accelerated test method, comprising a damp heat test, a solar radiation test, a salt mist test, characterized in that the damp heat test, the solar radiation test and the salt mist test are combined in precedence order and circulate; circulation time of the damp heat test, the solar radiation test and the salt mist test is more ten. The coating simulation accelerated test method of marine environment adaptation check is reasonable, effective and rapid and obtains the outdoor long-time exposure test result using the indoor short-time testing; solves the practical problems of development and use, in favor of application and popularization of coating material.
Description
Technical field
The present invention relates to a kind of simulated acceleration test method of coating, particularly relate to a kind of simulated acceleration test method that is used for the marine environment adaptability examination of coating.
Background technology
At present, examine the method for adopting available Natural Environmental Test and lab simulation accelerated test to carry out to the environmental suitability of various coatings.Natural Environmental Test is that the sample or direct the input under typical physical environment of product that scribble coating are being exposed to the open air, by observing, test its various changes of properties, accumulation data analyzes and draw the real environmental suitability rule of coating material, but the test period is longer; Natural Environmental Test has some general standard test methods.Simulated acceleration test then is the mini-test that adopts some typical envirment factors in order to shorten the examination time, test as high and low temperature, temperature shock test, damp heat test, the solar radiation test, salt-fog tests etc., these tests all have general standard test method, resulting test findings can only reflect coating performance in a certain respect.The result of this two classes test does not have direct contact, and its correlativity still is among the exploratory development now, therefore has Natural Environmental Test cycle length and the incomplete problem of simulated acceleration test result.Comparatively speaking, be marine environment to the bigger typical physical environment of coating performance influence, its high temperature, high humidity, optical radiation and Photochemical effects, envirment factors such as salt fog atmosphere all produce great destruction to coating, and coating is used in this environment mostly.How obtaining the test findings of long-term ocean physical environment with the simulated acceleration test of short-term, to determine the environmental suitability of coating, is the practical problems that both sides of development and use of coating are badly in need of solving.
Summary of the invention
The object of the present invention is to provide a kind of rationally, effectively and rapidly, the simulated acceleration test method that is used for the marine environment adaptability examination of coating, utilize simulated acceleration test method of the present invention can reach, obtain the purpose of outdoor long term exposure test findings with short term tests in the laboratory.
The object of the present invention is achieved like this; A kind of simulated acceleration test method of coating comprises damp heat test, solar radiation test, salt-fog test, it is characterized in that: described damp heat test, described solar radiation test, described salt-fog test make up sequentially, and circulate.
The cycle index of above-mentioned damp heat test, described solar radiation test, described salt-fog test is more than 10.
Described damp heat test, described solar radiation test, round-robin test period of described salt-fog test are 72 hours, wherein:
The described damp heat test time is 24 hours, and test condition is: heated up in 2 hours: 30 ℃ are raised to 60 ℃, and 16 hours are hot and humid: 60 ℃, relative humidity cooling in 95%, 2 hour: 60 ℃ drop to 30 ℃, 4 hours low temperature and high relative humidities: 30 ℃, and relative humidity 85%;
Described solar radiation test period is 24 hours, and test condition is: solar radiation in 20 hours, light source: 1120 ± 47W/m
2Water-cooled tubulose xenon lamp, temperature: 49 ± 2 ℃, closed light source in 4 hours;
The described salt-fog test time is 24 hours, and test condition is: salt solusion: 5%NaCl, and PH:6.5～7.2, temperature: 35 ± 2 ℃, salt fog sedimentation: 1～2ml/80cm
2.h, spraying continuously.
The ageing process of simulation coating in physical environment in the laboratory, and set up short-time test and evaluation method, fundamental purpose is the test findings that acquisition and the test in the physical environment have comparability, test period weak point.Can laboratory examination obtain ideal effect, depends on method, sequence test and the condition of selection, confirmed test, but at first will consider breakdown of coating is had the environmental factor of material impact.
As everyone knows, aging the be subjected to Effect of Environmental such as temperature, humidity, optical radiation, salt fog, temperature shock of coating in the physical environment of ocean.Because range of temperature is little in the marine environment, that coating performance mainly is subjected to is damp and hot, the influence of optical radiation, salt fog: sunshine can cause the oxidation and the hydrolysis of coating, high temperature and high humidity will promote this process, chlorion in the salt fog can pass coating and substrate generation electrochemical reaction, so the speed of coating aging speed, main is by thermal effect, Photochemical effects and salt air corrosion effect decision.
Show after deliberation, other laboratory examinations such as damp heat test, optical radiation test, the same thermal aging test of salt-fog test, temperature shock are compared, has specific influence, carrying out these three kinds of tests is that necessary also being difficult to replaced by other laboratory examination, three kinds of test reasonable combination are got up, test findings in ageing failure mechanism behind the coating test, performance change trend and the physical environment is the most approaching, and the acceleration effect of composite test is also best.The laboratory examination of, optical radiation test damp and hot and three kinds of environmental factors of salt fog because of having determined than the present invention.
The sequencing of damp heat test, optical radiation test, salt-fog test is influential to test findings, and main performance is that test result in earlier stage can be different.Select damp heat test-this sequencing of optical radiation test-salt-fog test, mainly considered 2 points: the one, the change procedure of simulation actual environment condition, the 2nd, help accelerating the coating deterioration.In the physical environment of ocean, humidity value before and after morning every day is the highest, at the upper and lower noon solar radiation is arranged subsequently, salt-fog test can show the formation electrolyte membrane in coating, very similar to the condensation state of coating surface in time beyond the solar radiation, so salt-fog test is arranged in the back of optical radiation test, carry out salt-fog test rather than optical radiation test before the damp heat test, can make the damp heat test sample surfaces keep the salt corrosion medium, temperature, humidity and corrosive medium are to the summation stress efficacy of coating during the quickening damp heat test.
The main consideration of selection of the test condition in above-mentioned three test methods will have certain maturity, from handled easily, can utilize present testing equipment to carry out test to determine.Test condition in the relevant test methods through adopting national standard and GJB has carried out the test of many times contrast and has shown that the test condition that the present invention determines is comprehensive relatively, harsh, can satisfy the test needs.
The T.T. that the cyclic test of above-mentioned three test methods needs, consideration is a principle with the Changing Pattern that can reflect appearance of coat, colour index and mechanical property etc., show through experimental study, 10 circulations promptly can draw the rule that coating performance changes in 720 hours basically, and compare with 18 months coating performance result of variations of marine environment outdoor exposure test, the simulated acceleration test method of coating provided by the invention has simulation, acceleration and reappearance preferably.
When implementing the simulated acceleration test method of coating provided by the invention, to coating specimen preparation, the placement in the test routine, testing equipment, switching time, the sampling of coating sample between damp heat test, optical radiation test, salt-fog test, and test report etc. can be undertaken by existing test standard or relevant technologies documentation requirements; And the coating sample before test, test item and the result evaluation of test after the neutralization test, the detection of outward appearance and mechanical property etc. can be undertaken by the relevant technologies documentation requirements of existing examination criteria or coating material.
In sum, the simulated acceleration test method that the marine environment adaptability that is used for coating provided by the invention is examined can reach rationally, effectively, fast with short term tests in the laboratory, obtains the purpose of outdoor long term exposure test findings; Solve both sides of development and use's practical problems, helped the application and the popularization of coating material.
Description of drawings
The present invention is further illustrated below in conjunction with drawings and Examples.
The sample adhesion change curve of Fig. 1 for adopting the coating simulated acceleration test method to obtain in the embodiments of the invention 1;
The sample adhesion change curve that Fig. 2 obtains for coating Hainan outdoor exposure test method of carrying out with embodiments of the invention 1 contrast;
Sample aberration Δ E value diffusing point and the regression straight line figure of Fig. 3 for adopting the coating simulated acceleration test method to obtain in the embodiments of the invention 1;
The sample aberration Δ E value that Fig. 4 obtains for coating Hainan outdoor exposure test method of carrying out with embodiments of the invention 1 contrast is loose and is put and regression straight line figure;
The sample aberration Δ a value change curve of Fig. 5 for adopting the coating simulated acceleration test method to obtain in the embodiments of the invention 2;
The sample aberration Δ a value change curve that Fig. 6 obtains for coating Hainan outdoor exposure test method of carrying out with embodiments of the invention 2 contrast;
Sample aberration Δ a value diffusing point and the regression straight line figure of Fig. 7 for adopting the coating simulated acceleration test method to obtain in the embodiments of the invention 2;
Sample aberration Δ a value diffusing point and the regression straight line figure of Fig. 8 for adopting the coating simulated acceleration test method to obtain in the embodiments of the invention 1.
Embodiment
Embodiment 1: a kind of simulated acceleration test method of coating, comprise damp heat test, solar radiation test, salt-fog test, and it is characterized in that: described damp heat test, described solar radiation test, described salt-fog test make up sequentially, and circulate.
The cycle index of described damp heat test, described solar radiation test, described salt-fog test is 12.
Described damp heat test, described solar radiation test, round-robin test period of described salt-fog test are 72 hours, wherein:
The described damp heat test time is 24 hours, and test condition is: heated up in 2 hours: 30 ℃ are raised to 60 ℃, and 16 hours are hot and humid: 60 ℃, relative humidity cooling in 95%, 2 hour: 60 ℃ drop to 30 ℃, 4 hours low temperature and high relative humidities: 30 ℃, and relative humidity 85%;
Described solar radiation test period is 24 hours, and test condition is: solar radiation in 20 hours, light source: 1120 ± 47W/m
2Water-cooled tubulose xenon lamp, temperature: 49 ± 2 ℃, closed light source in 4 hours;
The described salt-fog test time is 24 hours, and test condition is: salt solusion: 5%NaCl, and PH:6.5～7.2, temperature: 35 ± 2 ℃, salt fog sedimentation: 1～2ml/80cm
2.h, spraying continuously.
In the present embodiment, having adopted with epoxy resin is that the coating sample of important composition is tested sample substrate sizes: 85mm * 95mm * 2.0mm; Coating color is green; Testing equipment is:
Damp heat test: SH050C moisture-heat test-box;
Solar radiation test: SH60C xenon lamp weatherability chamber;
Salt-fog test: FY10E salt spray test chamber.
Before the test sample has been carried out the initial performance detection, after finishing certain cycle index, has extracted 3 on one group of sample and carry out relevant Performance Detection by the examination criteria of being correlated with:
GB1766-95 " ranking method of paint and varnish coating aging "
GB11186.3-93 " determination method of paint film color "
GB5210-85 " the coating adhesion determination method is drawn back method "
Sample outward appearance evaluation result in test sees Table 1, and the adhesion change curve of sample is seen Fig. 1, and the aberration Δ E value testing result of sample sees Table 2, and Δ E is the total color difference value.
Outward appearance evaluation result in the salt fog cyclic test that table 1 sample is damp and hot--solar radiation--
| Test period (h) | Variable color | Efflorescence | Bubble | Get rusty | Comprehensive Assessment |
| ?0 | 0 | 0 | 0 | 0 | 0 |
| ?72 | 0 | 0 | 0 | 0 | 0 |
| ?144 | 1 | 1 | 0 | 0 | 1 |
| ?288 | 1 | 1 | 0 | 0 | 1 |
| ?432 | 2 | 2 | 0 | 0 | 2 |
| ?576 | 2 | 2 | 0 | 1(S3) | 2 |
| ?720 | 3 | 3 | 0 | 2(S2) | 3 |
| ?864 | 4 | 3 | 0 | 2(S3) | 4 |
Table 2 sample aberration Δ E value result
In addition, also adopted the same batch coating sample identical to carry out the Natural Environmental Test of 18 months outdoor exposure test field, Hainan with present embodiment, the sample outdoor exposure is towards southwards, tilt horizontal by miter angle, the adhesion change curve of test back sample is seen Fig. 2, and the aberration Δ E value testing result of sample sees Table 2.
In entire test, sample cracking do not occur and comes off, and variable color is the most important failure mode of sample.After the analysis of the sample aberration Δ E Value Data by his-and-hers watches 2, set up following Ageing Model: Y=AX+B, and obtain the value of chromatism regression equation of two kinds of test methods respectively, wherein, Y is a value of chromatism, and A, B are constant, and X is a digestion time.The A value is rate of ageing, by comparing the A value, can draw the size of two kinds of test methods to the coating influence, and with data substitution Ageing Model, diffusing point of the sample aberration Δ E value that obtains and regression straight line figure are referring to Fig. 3 and Fig. 4.
The value of chromatism regression equation of damp and hot-solar radiation-salt fog cyclic test: Y=0.0161X+1.5053
The goodness of fit R=0.922 of regression equation, R
0.01=0.917, by the significance test of α=0.01, fitting effect is fine.
The value of chromatism regression equation of seashore, Hainan outdoor exposure test: Y=0.1568X+0.8145
The goodness of fit R=0.892 of regression equation, R
0.05=0.811, by the significance test of α=0.05, fitting effect is good.
Having obtained the rate of ageing of experiment lab simulation accelerated test and Hainan outdoor exposure test by recurrence, is respectively: damp and hot--solar radiation--salt fog cyclic test 0.0161, Hainan outdoor exposure test 0.1568.Because Hainan outdoor exposure test is to be unit with the moon.And the lab simulation accelerated test is hour being unit, obtains following relation by conversion:
0.0161×24×30÷0.1568＝74
The rate of ageing of the sample of present embodiment is 74 times of Hainan outdoor exposure sample.
From Fig. 1 and Fig. 2 the adhesion change curve of sample as can be known, the form of the adhesion change curve of the sample of present embodiment and the sample of the Natural Environmental Test of Hainan outdoor exposure is similar substantially, and presents essentially identical Changing Pattern.
From above analysis as can be known, the coating simulated acceleration test method of present embodiment has simulation and acceleration preferably to ocean Natural Environmental Test method.
Embodiment 2: a kind of simulated acceleration test method of coating, present embodiment is except that the sample coating that adopts is coating of the same race with the sample different batches of embodiment 1, and the simulated acceleration test method of being implemented, test are not equipped with, extraction sample detection etc. is all identical with embodiment 1.Sample outward appearance evaluation result in test sees Table 3; The sample aberration Δ a value change curve that obtains is seen Fig. 5.
Outward appearance evaluation result in the salt fog cyclic test that table 3 sample is damp and hot--solar radiation--
| Test period (h) | Variable color | Efflorescence | Bubble | Get rusty | Integrated level |
| ?0 | 0 | 0 | 0 | 0 | 0 |
| ?72 | 0 | 0 | 0 | 0 | 0 |
| ?144 | 1 | 1 | 0 | 0 | 1 |
| ?288 | 1 | 1 | 0 | 0 | 1 |
| ?432 | 2 | 1 | 0 | 0 | 1 |
| ?576 | 3 | 2 | 0 | 0 | 2 |
| ?720 | 3 | 3 | 0 | 1(S3) | 3 |
| ?864 | 4 | 3 | 1 | 2(S3) | 4 |
The same with embodiment 1, also adopted the same batch coating sample identical to carry out the Natural Environmental Test of 18 months outdoor exposure test field, Hainan with present embodiment, the sample outdoor exposure tilts horizontal by miter angle towards southwards, and the sample aberration Δ a value change curve that obtains is seen Fig. 6.
In entire test, sample cracking do not occur and comes off, and variable color is the most important failure mode of sample.Because of the sample coating color is green, aberration Δ a is a sign amount red, greenness, and variable color mainly is the variation of Δ a value, so adopt more directly perceived with aberration Δ a value, accurate.From Fig. 5 and Fig. 6 the aberration Δ a value change curve of sample as can be known, the form of the aberration Δ a value change curve of the sample of present embodiment and the sample of the Natural Environmental Test of Hainan outdoor exposure is similar substantially, and presents essentially identical Changing Pattern.
From above analysis as can be known, the coating simulated acceleration test method of present embodiment has simulation and acceleration preferably equally to ocean Natural Environmental Test method.
From the outward appearance evaluation result of table 3 and table 1 as can be known, the sample of the sample of present embodiment and embodiment 1 is under same simulated acceleration test condition, and the appearance change process and the state of coating are basic identical.
Again after the analysis of the aberration Δ a Value Data that records by sample to the sample of present embodiment and embodiment 1, set up following Ageing Model: Y=AX+B, and obtain value of chromatism one regression equation of twice test respectively, wherein, Y is aberration Δ a eight values, B is a constant, X is a digestion time, the A value is rate of ageing, by comparing the A value, can draw twice test to the coating effect, with data substitution Ageing Model, obtain the diffusing point of sample aberration Δ a value and regression straight line Fig. 7 of present embodiment, the diffusing point of the sample aberration Δ a value of embodiment 1 and regression straight line Fig. 8.
The data model of 720 hours aberration Δs of specimen test a of present embodiment:
y
Δa＝0.0032x+2.9576
The goodness of fit of regression equation: R=0.7265, R
0.05=0.8064, by the significance test of α=0.10, fitting effect is good.
The data model of 720 hours aberration Δs of specimen test a of embodiment 1:
y
Test Δ a=0.0061x+1.319
The goodness of fit of regression equation: R=0.7592, R
0.05=0.8064, by the significance test of α=0.10, fitting effect is good.
Therefore, the simulated acceleration test method of the coating that present embodiment and embodiment 1 are used is good for the test findings correlativity, has reappearance preferably.
In addition, in present embodiment and embodiment 1, the coating sample is detected performance data after test proceeds to 10 loop ends, basically can draw the rule that coating performance changes, and had reappearance preferably, also can reflect simulation and the acceleration that ocean Natural Environmental Test method is had fully.
Claims (1)
1. the simulated acceleration test method of a coating, comprise damp heat test, solar radiation test, salt-fog test, it is characterized in that: described damp heat test, described solar radiation test, described salt-fog test make up sequentially, and circulate, described cycle index is more than 10, the test period of described circulation primary is 72 hours, wherein:
The described damp heat test time is 24 hours, and test condition is: heated up in 2 hours: 30 ℃ are raised to 60 ℃, and 16 hours are hot and humid: 60 ℃, relative humidity cooling in 95%, 2 hour: 60 ℃ drop to 30 ℃, 4 hours low temperature and high relative humidities: 30 ℃, and relative humidity 85%;
Described solar radiation test period is 24 hours, and test condition is: solar radiation in 20 hours, light source: 1120 ± 47W/m
2Water-cooled tubulose xenon lamp, temperature: 49 ± 2 ℃, closed light source in 4 hours;
The described salt-fog test time is 24 hours, and test condition is: salt solusion: 5%NaCl, and PH:6.5～7.2, temperature: 35 ± 2 ℃, salt fog sedimentation: 1～2ml/80cm
2.h, spraying continuously.
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