CN114112884A - Detection method for steel corrosion performance under simulated seawater environment - Google Patents

Detection method for steel corrosion performance under simulated seawater environment Download PDF

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CN114112884A
CN114112884A CN202111486888.0A CN202111486888A CN114112884A CN 114112884 A CN114112884 A CN 114112884A CN 202111486888 A CN202111486888 A CN 202111486888A CN 114112884 A CN114112884 A CN 114112884A
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steel
sample
seawater
corrosion
analyzing
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贾仁萍
赵炳南
陆林和
雒国强
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Jiangsu Rongda Material Corrosion Inspection Co ltd
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Jiangsu Rongda Material Corrosion Inspection Co ltd
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/006Investigating resistance of materials to the weather, to corrosion, or to light of metals

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Abstract

The invention discloses a detection method for steel corrosion performance under a simulated seawater environment, which comprises the following steps of preparing a steel sample according to experimental requirements; polishing and sealing with epoxy resin; cleaning the steel sample to obtain a bare steel sample; sampling seawater, and measuring to obtain water quality parameters of the sampled seawater; placing a bare steel sample into sampled seawater to obtain a fully immersed sample and a dry-wet alternate immersed sample; carrying out polarization performance analysis to obtain a polarization curve; analyzing the appearance and the components of the rust layer; fitting the polarization curve to obtain corrosion current density; analyzing the appearance and the components of the rust layer to obtain a appearance pattern and a corresponding XRD pattern; analyzing and summarizing the corrosion resistance of the steel sample in a seawater environment; according to the method, the steel sample is placed in a seawater environment, the corrosion condition of seawater on the steel sample under different conditions is simulated, equipment and instruments are adopted for analyzing and obtaining corresponding data, corresponding parameter values are summarized and summarized, and a reference basis is provided for optimizing the steel.

Description

Detection method for steel corrosion performance under simulated seawater environment
Technical Field
The invention relates to a detection method for steel corrosion performance under a simulated seawater environment, and belongs to the technical field of environment simulation tests.
Background
In the process of development and utilization of marine resources, steel plays an indispensable role, such as tidal current power generation, seawater temperature difference power generation equipment, large coastal bridges on seashore, submarine containers related to marine development, various large marine components for resource development, shipbuilding steel and other fields, the marine environment is complex and harsh, steel equipment exposed in the marine environment can be seriously corroded, the corrosion resistance of seawater steel is an important index for evaluating steel types in China, the adaptability and the corrosion resistance effect of alloy elements can be known through the research on the corrosion resistance, and further the chemical composition design of the steel types is guided and optimized, so that the corrosion resistance detection of the seawater steel under different conditions is necessary.
Disclosure of Invention
In view of the above technical problems, the present invention aims to: the method for detecting the corrosion performance of the steel in the simulated seawater environment can simulate the corrosion condition of the steel in the seawater environment, analyze and obtain corresponding data, and provide a reference basis for optimizing the steel.
The technical solution of the invention is realized as follows: a method for detecting the corrosion performance of steel in a simulated seawater environment comprises the following steps,
s01, preparing a steel sample according to the experiment requirement, and shearing the steel sample to the required size;
s02, welding a lead at one end of the steel sample, polishing the steel sample smoothly and sealing the steel sample by using epoxy resin;
s03, cleaning the steel sample, sequentially cleaning the steel sample by using distilled water, absolute ethyl alcohol and acetone, and drying the steel sample after the cleaning is finished to obtain a bare steel sample;
s04, sampling seawater, and measuring by using a multi-parameter water quality detector to obtain water quality parameters of the sampled seawater;
s05, placing the bare steel sample into sampled seawater to obtain a fully immersed sample and a dry-wet alternately immersed sample;
s06, analyzing the polarization performance, and analyzing by adopting a potentiostat and test software to obtain a polarization curve;
s07, analyzing the appearance and components of the rust layer after the bare steel sample, the fully immersed sample and the dry-wet alternate immersed sample are polarized;
s08, fitting the polarization curve to obtain corrosion current density; analyzing the appearance and components of the rust layer to obtain the appearance diagram and the corresponding XRD diagram of corrosion of the three steel samples in seawater;
and S09, integrating the obtained corrosion current density, morphology pattern and XRD pattern, and analyzing and summarizing the corrosion resistance of the steel sample in the seawater environment.
Preferably, the steel product sample has a dimensional requirement of 30 mm to X20 mm to X3 mm.
Preferably, when the steel sample is polished, the water sand paper is used for polishing the steel sample step by step until the mirror surface is bright.
Preferably, the fully immersed test sample is a bare steel test sample which is immersed in sampling seawater and is continuously immersed for more than 10 days.
Preferably, the dry-wet alternate immersion test sample is a bare steel test sample obtained by sealing the periphery of the bare steel test sample with wax, dripping a drop of sampling seawater, naturally drying in the air, dripping the sampling seawater once again after 12 hours, and repeatedly operating for more than 10 days.
Preferably, during polarization performance analysis, a three-electrode system is adopted, and a working electrode is a bare steel sample, a full immersion sample and a dry-wet alternate immersion sample; the auxiliary motor is a Pt electrode, and the reference electrode is a saturated calomel electrode.
Preferably, during polarization curve analysis, a strong polarization curve is adopted for scanning in a range of-350 to 350mV, and the scanning speed is 1.0 mV/s; scanning orientation is-100 mV by adopting a weak polarization curve, scanning speed is 0.5mV/s, and temperature is 26 ℃.
Preferably, in step S08, observing the appearance of the rust layer of the three steel samples by using a scanning electron microscope to obtain a topography; the components of three steel samples are analyzed by an X-ray diffractometer, the anode is a Cu target, the power is 5kW, the scanning range is 10-80 degrees, the scanning speed is 5 degrees/mi < n >, and the step length is 0.03 degrees.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the detection method for simulating the corrosion performance of the steel in the seawater environment, the steel sample is placed in the seawater environment, the corrosion condition of seawater on the steel sample under different conditions is simulated, equipment and instruments are adopted for analyzing and obtaining corresponding data, corresponding parameter values are summarized and summarized, and a reference basis is provided for optimizing the steel.
Drawings
The technical scheme of the invention is further explained by combining the accompanying drawings as follows:
FIG. 1 is a schematic flow chart of a method for detecting corrosion performance of steel in a simulated seawater environment according to the present invention;
FIG. 2 is a chemical composition diagram of DH36 steel of the present invention;
FIG. 3 is a water quality parameter diagram of sampled seawater according to the present invention;
FIG. 4 is a strong polarization curve of 3 samples in seawater 1 and seawater 2;
FIG. 5 is a weak polarization curve of 3 samples in seawater 1 and seawater 2;
FIG. 6 is a graph of corrosion current density obtained after fitting a weak polarization curve according to the present invention;
FIG. 7 is an SEM topography of corrosion products of DH36 steel of the present invention in 2 Zhonghai water;
FIG. 8 is an XRD spectrum of corrosion products of DH36 steel of the present invention in 2 seawater.
Detailed Description
The invention is described below with reference to the accompanying drawings.
As shown in the attached figure 1, the method for detecting the corrosion performance of the steel in the simulated seawater environment comprises the following steps,
sample preparation
According to experimental requirements, preparing a steel material sample, such as a DH63 steel as a base material, and shearing the steel material sample until the required dimension is one of 30 mm X20 mm X3 mm, 40 mm X40 mm X3 mm or 10 mm X10 mm X2 mm, wherein the chemical composition of the DH36 steel is shown in figure 2; welding a lead on one end of a steel sample, polishing the steel sample step by using water sand paper until the surface of the steel sample is bright, and sealing the steel sample by using epoxy resin; cleaning a steel sample, sequentially cleaning the steel sample by using distilled water, absolute ethyl alcohol and acetone, and drying the steel sample after the cleaning to obtain a bare steel sample; putting a bare steel sample into sampled seawater to obtain a fully immersed sample and a dry-wet alternate immersed sample, wherein the fully immersed sample is the bare steel sample immersed in the sampled seawater for more than 10 days; the dry-wet alternate immersion test sample is a bare steel test sample obtained by sealing the periphery of the bare steel test sample with wax, dripping a drop of sampling seawater, naturally drying in the air, dripping the sample once again after 12 hours, and repeatedly operating for more than 10 days;
simulation of corrosive environment
Sampling seawater, wherein the seawater sample can be natural seawater retrieved from sea or artificial seawater prepared after analyzing the components of the natural seawater, and the coastal seawater in southeast of China mainly comprises the following components: 26.518g/L NaCl, MgSO4 3.305g/L,MgCl2 2.447g/L,CaCl2 1.141g/L,KCl 0.725g/L,NaHCO30.202g/L, 0.083g/L NaBr, 1300mmol/L osmotic pressure, 8.2 pH and 1.05-1.06g/ml density; and a multi-parameter water quality detector is adopted to measure and obtain the water quality parameters of the sampled seawater, which is shown in the attached figure 3; carrying out polarization performance analysis, adopting a three-electrode system, and using a working electrode as a bare steel sample and a fully immersed and dry-wet alternately immersed sample; the auxiliary motor is a Pt electrode, the reference electrode is a saturated calomel electrode, a constant potential rectifier and test software are adopted for analysis to obtain a polarization curve, and during analysis, a strong polarization curve is adopted for scanning in a range of-350 mV at a scanning speed of 1.0mV/s relative to an open circuit potential; scanning by using a weak polarization curve at the azimuth of-100 mV, the scanning speed of 0.5mV/s and the temperature of 26 ℃ relative to an open circuit telegraph text; analyzing the appearance and components of the rust layer after the bare steel sample, the fully immersed sample and the dry-wet alternate immersion sample are polarized; fitting the polarization curve to obtain corrosion current density; analyzing the appearance and components of the rust layer to obtain the appearance diagram of corrosion of the three steel samples in seawater and corresponding XRD (X-ray diffraction) diagrams, and observing the appearance of the rust layer of the three steel samples by adopting a scanning electron microscope to obtain the appearance diagram; analyzing the components of three steel samples by adopting an X-ray diffractometer, wherein the anode is a Cu target, the power is 5kW, the scanning range is 10-80 degrees, the scanning speed is 5 degrees/min, and the step length is 0.03 degrees; comprehensively obtaining the corrosion current density, the morphology graph and the XRD graph, analyzing and summarizing the corrosion resistance of the steel sample in the seawater environmentAnd (4) performance.
According to the graph shown in FIG. 4, a platform area appears in the cathode process of the steel in the seawater 1, the limited diffusion characteristic of dissolved oxygen is shown, the electrochemical dissolution controlled by charge transfer occurs on the iron surface under the anodic polarization, the electrochemical retardation in 2 kinds of seawater is very small, and the anode current is rapidly increased; the limiting diffusion characteristic of dissolved oxygen is also exhibited upon cathodic polarization in seawater 2, but is not evident in seawater 1; the limit diffusion control characteristic of dissolved oxygen reduction in the process of immersing the sample completely and immersing the sample in dry and wet alternately is basically disappeared, and the anode polarization behavior shows certain passivation characteristic under the control of charge transfer mainly by the reduction of corrosion products.
FIG. 6 shows the corrosion current density obtained after fitting the weak polarization curve, and it can be seen from FIG. 6 that the corrosion rates of DH36 steel in 2 kinds of seawater are not much different, the corrosion rate of the fully immersed sample is much greater than that of the bare steel sample, the corrosion rate of the dry-wet alternate immersion pattern is much greater than that of the fully immersed sample, this is probably because the corrosion products generated by DH36 steel under the alternation of dry and wet are more, the cathode current is increased by the action of the oxidizing agent of the rust layer, the corrosion rate of the fully immersed test sample is higher than that of the bare steel test sample just immersed in seawater, because the immersion time of the fully immersed test sample is shorter, and the protective rust layer is not formed on the surface of DH36 steel, in the medium of 2, the corrosion rates of the fully-submerged samples are basically consistent, the corrosion rate in the seawater 1 is slightly larger than that in the seawater 2 when the steel is alternately dry and wet, and the alternate dry and wet corrosion rate of the steel in the seawater medium 2 is 2-4 times that of the fully-submerged samples.
FIG. 7 is an SEM image of corrosion products of DH36 steel in seawater of 2, and it can be seen from FIG. 7 that the corrosion products fully submerged are in a cluster structure of platelet crystal stacking, loose and with a large number of holes; the corrosion products of the alternation of dry and wet cover most of the steel matrix, but the structure is not compact and is in a cracked layered or flaky shape, and the DH36 steel also has a caking phenomenon which is a possible magnesium protective layer, but the structure is still not compact and has a large number of holes.
FIG. 8 is an XRD spectrum of corrosion products of DH36 steel in 2 seawater; as can be seen from FIG. 8, the corrosion products of the fully submerged DH36 steel are mainly gamma-FeOOH and contain a small amount of alpha-FeOOH and Fe3O4FeOCl, etc.; dry-wet alternative corrosion products with Fe3O4And gamma-FeOOH, and contains a small amount of alpha-FeOOH, beta-FeOOH, FeOCl, etc., so that the reason why the corrosion rate of the DH36 steel with alternation of wetting and drying is 2-4 times that of the fully immersed specimen can be well explained: the fully immersed corrosion product is mainly loose and porous gamma-FeOOH, and the dry-wet alternative corrosion product is Fe in a layered or flaky shape3O4And gamma-FeOOH as main components; under the wet condition, the metal is an anode area, the rust layer is a cathode area, electrolyte solution in the gaps of the rust layer forms an ion channel connected with a cathode and an anode, the anode reaction is corrosion of a steel matrix, and Cl-Electrolyte solution passing through the holes of the rust layer reaches the matrix to damage a protective film on the surface of the steel and accelerate the corrosion of the matrix; polarization of full immersion is similar to that of bare steel, with substantial absence of oxidation-reduction of corrosion products, Fe3O4The content is less, the corrosion products of dry-wet alternation are more, and the cathode current is increased under the action of the self oxidant of the rust layer; the redox of the corrosion product is Fe3O4And gamma-FeOOH, Fe in the wet stage3O4Oxidized into gamma-FeOOH, and the gamma-FeOOH is converted into Fe in the drying stage3O4,Fe3O4As a good conductor, an electron path is formed, and the generation of corrosion is accelerated; corrosion products such as FeOCl, beta-FeOOH, etc. have appeared in both fully submerged and wet-dry alternation, and these are unstable intermediates, both in the presence of oxygen and Cl-Typical intermediates in the environment.
According to the detection method for simulating the corrosion performance of the steel in the seawater environment, the steel sample is placed in the seawater environment, the corrosion condition of seawater on the steel sample under different conditions is simulated, equipment and instruments are adopted for analyzing and obtaining corresponding data, corresponding parameter values are summarized and summarized, and a reference basis is provided for optimizing the steel.
The above-mentioned embodiments are merely illustrative of the technical idea and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered in the scope of the present invention.

Claims (8)

1. A detection method for steel corrosion performance under simulated seawater environment is characterized in that: comprises the following steps of (a) carrying out,
s01, preparing a steel sample according to the experiment requirement, and shearing the steel sample to the required size;
s02, welding a lead at one end of the steel sample, polishing the steel sample smoothly and sealing the steel sample by using epoxy resin;
s03, cleaning the steel sample, sequentially cleaning the steel sample by using distilled water, absolute ethyl alcohol and acetone, and drying the steel sample after the cleaning is finished to obtain a bare steel sample;
s04, sampling seawater, and measuring by using a multi-parameter water quality detector to obtain water quality parameters of the sampled seawater;
s05, placing the bare steel sample into sampled seawater to obtain a fully immersed sample and a dry-wet alternately immersed sample;
s06, analyzing the polarization performance, and analyzing by adopting a potentiostat and test software to obtain a polarization curve;
s07, analyzing the appearance and components of the rust layer after the bare steel sample, the fully immersed sample and the dry-wet alternate immersed sample are polarized;
s08, fitting the polarization curve to obtain corrosion current density; analyzing the appearance and components of the rust layer to obtain the appearance diagram and the corresponding XRD diagram of corrosion of the three steel samples in seawater;
and S09, integrating the obtained corrosion current density, morphology pattern and XRD pattern, and analyzing and summarizing the corrosion resistance of the steel sample in the seawater environment.
2. The method for detecting the corrosion performance of the steel in the simulated seawater environment according to claim 1, wherein the method comprises the following steps: the steel product sample has a dimensional requirement of 30 mm to X20 mm to X3 mm.
3. The method for detecting the corrosion performance of the steel in the simulated seawater environment according to claim 1, wherein the method comprises the following steps: when the steel sample is polished, the water sand paper is used for polishing the steel sample step by step until the mirror surface is bright.
4. The method for detecting the corrosion performance of the steel in the simulated seawater environment according to claim 1, wherein the method comprises the following steps: the fully immersed test sample is a bare steel test sample which is immersed in sampling seawater and is continuously immersed for more than 10 days.
5. The method for detecting the corrosion performance of the steel in the simulated seawater environment according to claim 1, wherein the method comprises the following steps: the dry-wet alternate immersion test sample is a bare steel test sample obtained by sealing the periphery of the bare steel test sample with wax, dripping a drop of sampling seawater, naturally drying in the air, dripping the sample once again after 12 hours, and repeatedly operating for more than 10 days.
6. The method for detecting the corrosion performance of the steel in the simulated seawater environment according to claim 1, wherein the method comprises the following steps: during polarization performance analysis, a three-electrode system is adopted, and a working electrode is a bare steel sample, a full immersion sample and a dry-wet alternate immersion sample; the auxiliary motor is a Pt electrode, and the reference electrode is a saturated calomel electrode.
7. The method for detecting the corrosion performance of the steel in the simulated seawater environment according to claim 1, wherein the method comprises the following steps: when the polarization curve is analyzed, a strong polarization curve is adopted for scanning in the range of-350 mV, and the scanning speed is 1.0 mV/s; scanning orientation is-100 mV by adopting a weak polarization curve, scanning speed is 0.5mV/s, and temperature is 26 ℃.
8. The method for detecting the corrosion performance of the steel in the simulated seawater environment according to claim 1, wherein the method comprises the following steps: in step S08, observing the appearance of the rust layers of the three steel samples by adopting a scanning electron microscope to obtain a topography; the components of three steel samples are analyzed by an X-ray diffractometer, the anode is a Cu target, the power is 5kW, the scanning range is 10-80 degrees, the scanning speed is 5 degrees/min, and the step length is 0.03 degrees.
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Application publication date: 20220301