CN113933232B - Material corrosion acceleration test method for simulating south China sea island reef environment - Google Patents

Material corrosion acceleration test method for simulating south China sea island reef environment Download PDF

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CN113933232B
CN113933232B CN202111136756.5A CN202111136756A CN113933232B CN 113933232 B CN113933232 B CN 113933232B CN 202111136756 A CN202111136756 A CN 202111136756A CN 113933232 B CN113933232 B CN 113933232B
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王荣祥
张博
邓俊豪
龚雨荷
王春辉
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China Electronic Product Reliability and Environmental Testing Research Institute
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Abstract

The invention relates to a material corrosion accelerated test method for simulating a south sea island reef environment, which comprises the following steps: circulating the material to be testedThe method comprises the following steps of (1) performing a circular acceleration test, wherein test items in one period of the circular acceleration test are a coral salt coating test, a salt spray test and a solar radiation test in sequence; wherein, the conditions of the salt spray test comprise: the temperature is 45-55 ℃, and the salt spray sedimentation rate is as follows: 1-2 mL/h.80cm 2 (ii) a The conditions of the solar radiation test include: irradiance adopts 1110-1130W/m 2 Instantaneous extreme value or 5700-5710W/m 2 The intensity conversion values are accumulated. The accelerated experiment method can better accord with the atmospheric corrosion characteristics of the south sea island reef of typical equipment materials, and the test result has strong correlation with the actual environment and higher result validity.

Description

Material corrosion acceleration test method for simulating south China sea island reef environment
Technical Field
The invention relates to the technical field of material environment testing, in particular to a material corrosion acceleration test method for simulating a south sea island reef environment.
Background
The south-sea island reef is located in a low-latitude area close to the equator and belongs to tropical marine climate. The main climatic characteristics of the south sea island reef are as follows: long sunshine time, strong radiation, high temperature in the whole year, abundant rainfall, high humidity, strong wind and less fog. Part of equipment structures are continuously subjected to the actions of high temperature, high humidity, high salt and strong solar radiation of south China sea and splashing seawater dry/wet cycle corrosion, the corrosion problem is serious, and the service life of the equipment structures and the safe use of the equipment are greatly influenced.
Because the traditional natural environment test period is too long, and the sensitivities of different structural materials to the environment are different, in order to determine the corrosion influence of the natural environment to the equipment structure, the equivalent relation between a natural environment spectrum and a laboratory accelerated environment spectrum needs to be established, and a corresponding accelerated test spectrum is designed, so that the corrosion damage rule of the equipment structural materials and the protection system in the south sea island and reef environment can be quickly obtained.
Conventional corrosion acceleration tests include: the standard GB/T25834-2010 outdoor atmospheric corrosion acceleration test for corrosion steel of metals and alloys, wherein the specified test is preferably carried out under the station condition in a dry season or region, and comprises the general requirements of the accelerated corrosion test for the steel in the atmospheric environment, such as test steps, requirements, devices and the like; the corrosion of metals and alloys according to standard GB/T20853-2007 specifies test values for the relevant components of sodium chloride solutions for accelerated tests, wherein the test solutions are prepared by dissolving sodium chloride in distilled or deionized water having a conductivity of not more than 2mS/m at 25 ℃. + -. 2 ℃, and the method for testing the corrosion resistance of metals in the presence of chloride ions is described. Above-mentioned traditional corrosion accelerated test is all unsuitable for south sea island reef actual environment, is difficult to the accurate corrosion conditions who reflects south sea island reef actual environment.
In addition, according to the marine environment corrosion problem faced by typical equipment, students compile an acceleration spectrum composed of cyclic acceleration spectrum of periodic infiltration, ultraviolet irradiation and periodic infiltration together based on a typical marine atmospheric environment spectrum. A study also researches the performance change rule of typical aviation materials after different periods of tests in the south sea marine environment, and the south sea environment accelerated test method combining the damp-heat test, the light aging test and the salt spray test is obtained through calculation. However, in the practical application process of the research, the correlation between the acceleration spectrum and the test result of the practical environment of the south sea island reef is still weak.
Disclosure of Invention
Based on the method, the material corrosion acceleration test method for simulating the environment of the south sea island is provided, which accords with the atmospheric corrosion characteristics of the south sea island of typical equipment materials, and has strong correlation and high result effectiveness.
The specific technical scheme is as follows:
a material corrosion accelerated test method for simulating a south sea island reef environment comprises the following steps:
carrying out a cyclic acceleration test on a material to be tested, wherein test items in one period of the cyclic acceleration test are a coral salt coating test, a salt spray test and a solar radiation test in sequence;
wherein, the conditions of the salt spray test comprise: the temperature is 45-55 ℃, and the salt spray sedimentation rate is as follows: 1-2 mL/h.80cm 2
The conditions of the solar radiation test include: irradiance is 1110-1130W/m 2 Instantaneous extreme value or 5700-5710W/m 2 The intensity conversion values are accumulated.
In one embodiment, the conditions of the salt spray test include: the temperature is 50 ℃, and the salt spray sedimentation rate is as follows: 1-2 mL/h.80cm 2
In one embodiment, the salt spray test uses a neutral modified ASTM-D1141 artificial seawater simulation solution of salt spray solution, wherein Cl - The mass fraction of (A) is 3% -4%.
In one embodiment, the conditions of the solar radiation test include: the instantaneous extreme value of irradiance is 1120W/m 2 Or 5708.16W/m 2 The intensity conversion value is accumulated.
In one embodiment, the conditions of the solar radiation test further comprise: the temperature is 45-50 ℃.
In one embodiment, the solar radiation test employs a temperature of 49 ℃.
In one embodiment, the step of coating the coral salt comprises:
mixing coral salt powder with artificial seawater simulation solution to prepare coral salt solution;
and coating the coral salt solution on the surface of the material to be detected.
In one embodiment, the mesh number of the coral salt powder is 800-1200 meshes.
In one embodiment, the coral salt solution contains coral salt powder in an amount of 8-12 wt%.
In one embodiment, the coral salt solution contains coral salt powder in an amount of 10 wt%.
In one embodiment, in one cycle, the time of the salt spray test is 14-15 hours, and the time of the solar radiation test is 9-10 hours.
In one embodiment, the salt spray test is carried out for 14.5h and the solar radiation test is carried out for 9.5h in one cycle.
The accelerated test method for simulating the material corrosion of the south sea island reef environment determines an accelerated test scheme capable of accurately simulating the material corrosion condition of the south sea island reef environment from multiple aspects such as test items, test sequences, test quantity values and the like, can effectively guarantee the relativity and effectiveness of a test acceleration spectrum and an actual south sea island reef environment test, can be directly used for accelerated test of key equipment structural materials in the south sea island reef environment, can quickly predict the corrosion condition in the use process of the materials, and provides data support and technical guidance for corrosion protection design and corrosion life extension work of equipment development units, production units, use units and maintenance units.
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FIG. 1 is an acceleration spectrum of a material corrosion acceleration test method for simulating a south-sea island reef environment in accordance with an embodiment of the present invention.
Detailed Description
The accelerated corrosion testing method for materials simulating the south sea island environment according to the present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In the present invention, the technical features described in the open type include a closed technical solution including the listed features, and also include an open technical solution including the listed features.
In the present invention, the numerical intervals are regarded as continuous, and include the minimum and maximum values of the range and each value between the minimum and maximum values, unless otherwise specified. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.
The percentage contents referred to in the present invention mean, unless otherwise specified, mass percentages for solid-liquid mixing and solid-solid phase mixing, and volume percentages for liquid-liquid phase mixing.
The percentage concentrations referred to in the present invention refer to the final concentrations unless otherwise specified. The final concentration refers to the ratio of the added component in the system after the component is added.
The temperature parameter in the present invention is not particularly limited, and is allowed to be a constant temperature treatment or a treatment within a certain temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
The invention provides a material corrosion accelerated test method for simulating a south sea island reef environment, which comprises the following steps:
carrying out a cyclic acceleration test on a material to be tested, wherein test items in one period of the cyclic acceleration test are a coral salt coating test, a salt spray test and a solar radiation test in sequence;
wherein, the conditions of the salt spray test comprise: the temperature is 45-55 ℃, and the salt spray sedimentation rate is as follows: 1-2 mL/h.80cm 2
The conditions of the solar radiation test include: irradiance is 1110-1130W/m 2 Instantaneous extreme value of 5700-5710W/m 2 The intensity conversion value is accumulated.
Specifically, the material to be tested is a typical aerospace material. Further, the material to be measured is a base material subjected to surface treatment. The material of the substrate includes but is not limited to aluminum or aluminum alloy, structural steel stainless steel, composite material, etcThe surface treatment means includes, but is not limited to, chemical conductive oxidation treatment, epoxy coating.
According to the accelerated test method for the corrosion of the material, aiming at the environment test characteristics of the south sea island reef of the material to be tested, on the basis of determining a test item set, test item arrangement is carried out according to the sequence of the corrosion factors suffered by the material summarized from a large amount of experience in the actual use process of the material. Specifically, the salt spray test is arranged before the solar radiation test because the salt spray test can generate corrosion products and the solar radiation test can modify the corrosion products; since the coated coral salt is prone to salt formation, moisture accumulation, and corrosion, the coated coral salt was discarded before the salt spray test. Based on this, the determined test sequence was: coating coral salt → salt spray test → solar radiation test, and so on. Meanwhile, the fact that the key parameters influencing the test result in the salt spray test are temperature and salt spray settlement rate, the key parameters influencing the test result in the solar radiation test are irradiance is found, the key parameters are reasonably controlled, and the correlation and effectiveness of the test accelerated spectrum and the actual south sea island reef environment test can be effectively guaranteed.
Specifically, the temperature of the salt spray test is 45-55 ℃. Such temperatures include, but are not limited to: 45 deg.C, 46 deg.C, 47 deg.C, 48 deg.C, 49 deg.C, 50 deg.C, 51 deg.C, 52 deg.C, 53 deg.C, 54 deg.C, 55 deg.C. Further, the conditions of the salt spray test include: the temperature is 50 ℃, and the salt spray sedimentation rate is as follows: 1-2 mL/h.80cm 2
In some specific examples, the salt spray test uses a salt spray solution as a neutral modified ASTM-D1141 artificial seawater simulant with Cl - The mass fraction of (A) is 3% -4%. Further, cl - The mass fraction of (b) is 3.034%. Thus, the acceleration effect can be improved.
Specifically, the composition of the neutral modified ASTM-D1141 artificial seawater simulation liquid is shown in the following table 1 by taking 40L as an example:
TABLE 1 40L Artificial seawater chemical content (unit g)
Figure BDA0003282293820000061
In some specific examples, the conditions of the solar radiation test include: the instantaneous extreme value of irradiance is 1120W/m 2 Or 5708.16W/m 2 The intensity conversion value is accumulated. Furthermore, the instantaneous extreme value of irradiance adopted in the solar radiation test is 1120W/m 2 . Therefore, the feasibility of the accelerated test is higher, and the popularization and the application are convenient.
In some specific examples, the conditions of the solar radiation test further include: the temperature is 45-50 ℃. Such temperatures include, but are not limited to: 45 deg.C, 46 deg.C, 47 deg.C, 48 deg.C, 49 deg.C, 50 deg.C. Further, the solar radiation test employed a temperature of 49 ℃.
In some specific examples, the step of coating the coral salt comprises:
mixing coral salt powder with artificial seawater simulation solution to prepare coral salt solution;
and coating the coral salt solution on the surface of the material to be detected.
In some specific examples, the artificial seawater simulation liquid is ASTM-D1141 artificial seawater simulation liquid.
In some specific examples, the coral salt powder has a mesh size of 800-1200 mesh. Specifically, the mesh number of the coral salt powder includes, but is not limited to: 800 meshes, 900 meshes, 1000 meshes, 1100 meshes and 1200 meshes. Furthermore, the mesh number of the coral salt powder is 1000 meshes.
In some specific examples, the coral salt solution contains 8 to 12 mass% of the coral salt powder. Specifically, the mass fractions of the coral salt powder in the coral salt solution include but are not limited to: 8%, 9%, 10%, 11%, 12%. Further, the mass fraction of coral salt powder in the coral salt solution is 10%.
In some specific examples, the time of the salt spray test is 14-15 h and the time of the solar radiation test is 9-10 h in one period. Further, in one period, the time of the salt spray test is 14.5h, and the time of the solar radiation test is 9.5h.
In some specific examples, the acceleration spectrum of the accelerated corrosion test method for materials simulating the south-ocean island reef environment is shown in fig. 1: taking 24h as a cycle period, wherein the salt spray test time is 14.5h, and the solar radiation test time is 9.5h; coating coral salt before salt spray test; the temperature of the salt spray test is 50 ℃, and the salt spray solution is a neutral modified ASTM-D1141 artificial seawater simulation solution (Cl) - The mass fraction reaches 3.304%), the salt spray sedimentation rate is: 1-2 mL/h.80cm 2 (ii) a The instantaneous extreme value adopted by solar radiation test irradiance is 1120W/m 2 The temperature was 49 ℃.
Specific examples are as follows.
Example 1
Sample piece: the base material is 2524 aluminum alloy, and the surface treatment mode of the base material is chemical conductive oxidation treatment.
Test procedure and conditions:
(1) Spraying coral salt solution: grinding real coral salt into powder, screening with a 1000-mesh sieve to obtain coral powder, mixing with ASTM-D1141 artificial seawater simulation solution, and preparing into 10 wt% coral salt solution. And (3) loading the mixture into a magnetic stirring device, uniformly rotating, and spraying the mixture onto the surface of the sample piece until the film is uniformly formed.
(2) Salt spray test:
temperature: 50 deg.C, salt spray solution is neutral modified ASTM-D1141 artificial seawater simulation solution (with ASTM-D1141 artificial seawater as base solution, adding NaCl for neutral modification to make Cl - The mass fraction reaches 3.034 percent), and the salt spray sedimentation rate is 1.0-2.0 ml/h.80cm 2
(3) Solar radiation test:
temperature: at 49 ℃, the solar radiation test adopts 1120W/m 2 An instantaneous extreme value. 24h is a cycle period, the salt spray test time is 14.5h, and the solar radiation test time is 9.5h.
(4) The number of cycles of the accelerated environmental test was 30.
The weight, electrochemical impedance spectrum and polarization curve were tested during the test. Wherein, the weight loss analysis is to firstly utilize the rust removing liquid to remove rust, and the preparation of the rust removing liquid is carried out according to the relevant requirements in GB/T16545-1996 clear of corrosion products on corrosion samples of metals and alloys. After rust removal, washing the steel by distilled water, drying the steel by cold air, weighing the steel by an analytical balance, and recording the mass W after rust removal 1 . Electrochemical testing the electrochemical impedance spectrum and polarization curve of the sample after the test is tested by using an electrochemical workstation. During electrochemical test, a traditional three-electrode system is adopted, a saturated calomel electrode is used as a reference electrode, a 20mm multiplied by 20mm Pt electrode is used as an auxiliary electrode, a test sample is used as a working electrode, and the working area of the test sample is 10mm multiplied by 10mm. The disturbance voltage of the electrochemical impedance test is 20mV, and the scanning frequency range is 100 KHz-0.01 Hz. Potentiodynamic electrodeThe scan rate of the chemical test was 0.5 mV.s -1 The voltage scanning range (vs OCP) is-0.5V-1.5V. The test solution was a 5% (mass fraction) NaCl solution.
In order to verify the effectiveness of the test, the weight and electrochemical test results in the accelerated environment test process are compared with the natural environment test results of the island in south China sea, and the results are shown in table 2.
Table 2 test results
Figure BDA0003282293820000081
Figure BDA0003282293820000091
Weightlessness and low-frequency impedance mode values are respectively taken as characteristic parameters, and a rank correlation coefficient method is adopted to evaluate the correlation between an accelerated environment test and a south sea island reef natural environment test, wherein the rank correlation coefficient R is 1.01 and 0.82, and the average rank correlation coefficient is 0.91, which is extremely strong correlation.
The weightlessness and low-frequency impedance mode values are taken as characteristic parameters, the results of the south sea island reef natural environment test for 12 months are basically consistent with the results of the accelerated environment test for 22 days, the accelerating factor AF is 13.78, and the acceleration is better.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, so as to understand the technical solutions of the present invention specifically and in detail, but not to be understood as the limitation of the protection scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. It should be understood that the technical solutions provided by the present invention, which are obtained by logical analysis, reasoning or limited experiments, are within the scope of the appended claims. Therefore, the protection scope of the present invention should be subject to the content of the appended claims, and the description and the drawings can be used for explaining the content of the claims.

Claims (11)

1. A material corrosion accelerated test method for simulating a south sea island reef environment is characterized by comprising the following steps:
carrying out a cyclic acceleration test on a material to be tested, wherein test items in one period of the cyclic acceleration test are a coral salt coating test, a salt spray test and a solar radiation test in sequence;
wherein, the conditions of the salt spray test comprise: the temperature is 45-55 ℃, and the salt spray sedimentation rate is as follows: 1 to 2mL/h.80cm 2 (ii) a The salt spray test adopts a salt spray solution as a neutral modified ASTM-D1141 artificial seawater simulation solution, wherein Cl is contained in the salt spray solution - The mass fraction of the organic silicon compound is 3% -4%;
the conditions of the solar radiation test include: the temperature is 45-50 ℃, and the irradiance is 1110-1130W/m 2 Instantaneous extreme value or 5700-5710W/m 2 Accumulating the intensity conversion values;
the step of coating the coral salt comprises: mixing coral salt powder with artificial seawater simulation liquid to prepare a coral salt solution, and coating the coral salt solution on the surface of the material to be detected, wherein the mass fraction of the coral salt powder in the coral salt solution is 8-12%;
in one cycle, the time of the salt spray test is 14h to 15h, and the time of the solar radiation test is 9h to 10h.
2. The method for accelerated testing of corrosion of materials simulating the south sea island environment according to claim 1, wherein the conditions of the salt spray test comprise: the temperature is 50 ℃, and the salt spray sedimentation rate is as follows: 1 to 2mL/h.80cm 2
3. The method for accelerated corrosion testing of materials simulating the south sea island reef environment of claim 1 wherein the material to be tested is a typical aerospace material.
4. The method for accelerated testing of corrosion of materials simulating the environment of the south sea island according to claim 1, wherein the conditions of the solar radiation test comprise: the instantaneous extreme value of irradiance is 1120W/m 2 Or 5708.16W/m 2 The intensity conversion values are accumulated.
5. The method for simulating the south sea island reef environment for the accelerated test of the material corrosion as claimed in claim 1, wherein the instantaneous extreme value of irradiance adopted in the solar radiation test is 1120W/m 2
6. The method for accelerated corrosion testing of materials simulating the south sea island environment according to claim 1, wherein the solar radiation test is performed at a temperature of 49 ℃.
7. The method for accelerated corrosion testing of materials simulating the south sea island environment according to claim 1, wherein Cl in said salt spray solution - The mass fraction of (a) is 3.034%.
8. The accelerated test method for material corrosion according to claim 1, wherein the coral salt powder has a mesh size of 800-1200 meshes.
9. The method according to claim 8, wherein the coral salt powder has a mesh size of 1000 meshes.
10. The method for accelerated testing of corrosion of materials according to claim 9, wherein the coral salt solution contains coral salt fines in an amount of 10% by weight.
11. The method for accelerated testing of corrosion of materials simulating the south sea island environment according to claim 10, wherein the time of the salt spray test is 14.5 hours and the time of the solar radiation test is 9.5 hours in one cycle.
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