CN115656013A - Method for detecting preferential corrosion phase in high-aluminum zinc aluminum magnesium coating - Google Patents

Method for detecting preferential corrosion phase in high-aluminum zinc aluminum magnesium coating Download PDF

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CN115656013A
CN115656013A CN202211112764.0A CN202211112764A CN115656013A CN 115656013 A CN115656013 A CN 115656013A CN 202211112764 A CN202211112764 A CN 202211112764A CN 115656013 A CN115656013 A CN 115656013A
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corrosion
coating
phase
aluminum
detected
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邵蓉
黎敏
刘永壮
董妮妮
刘武华
李学涛
曹建平
王长成
何万定
刘新华
王伟
刘洋
刘向明
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Shougang Group Co Ltd
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Shougang Group Co Ltd
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Abstract

The invention provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium coating, belonging to the technical field of coating detection and analysis, and the method comprises the following steps: carrying out first microscopic scanning on the high aluminum zinc aluminum magnesium coating to be detected to obtain a curve L of the content of different characteristic elements i in the high aluminum zinc aluminum magnesium coating to be detected along with the change of depth i (ii) a Corroding the high aluminum zinc aluminum magnesium coating to be detected after the first microscopic scanning is carried out to obtain a corrosion coating; carrying out second microscopic scanning on the corrosion coating to obtain a curve L of the content of different characteristic elements i in the corrosion coating changing along with the depth i (ii) a According to said curve L i And said curve L i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected. The method has the advantages of high accuracy and good repeatability, shows wide application prospect, and effectively solves the technical problem that the prior corrosion phase in the high-aluminum-zinc-aluminum-magnesium coating is difficult to judge by the traditional corrosion observation means.

Description

Method for detecting preferential corrosion phase in high-aluminum zinc aluminum magnesium coating
Technical Field
The application relates to the technical field of plating detection and analysis, in particular to a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium plating layer.
Background
The zinc-aluminum-magnesium plating layer is a ternary alloy plating layer formed by adding a small amount of aluminum and magnesium elements on the basis of a pure zinc plating layer, and compared with the traditional pure zinc plating layer, the zinc-aluminum-magnesium plating layer has more excellent corrosion resistance.
At present, for the corrosion resistance evaluation of a plating material, an accelerated corrosion test is generally carried out on the plating material, and the corrosion weight loss rate is calculated by adopting a chemical method for rust removal. The method has the following disadvantages: (1) In the corrosion test process, the corrosion rate of a base body at a notch of a coated steel plate is far greater than that of a coating, in order to avoid the influence of notch corrosion, edge sealing treatment is usually carried out on the notch around the coated steel plate, so that large errors can be brought in weight loss weighing before and after corrosion and calculation of the corrosion rate, and particularly, when corrosion products at the initial corrosion stage are less, the corrosion rate can be greatly deviated. (2) The method can only calculate the average corrosion rate of the coating material, and is suitable for the uniform coating on the surface and the uniform corrosion of the coatingThe high aluminum zinc aluminum magnesium plating layer has aluminum-rich phase, zinc-rich phase and MgZn on the surface 2 The phase composition, which is different in corrosion rate of different phases in different corrosion tests due to different corrosion potentials between different phases, is not uniform corrosion. Therefore, the relative corrosion sequence between different phases of the traditional corrosion weight loss method is difficult to judge, and the influence of local corrosion on the durability of the plating material is more serious.
Disclosure of Invention
The embodiment of the application provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium plating layer, and aims to solve the technical problem that the preferential corrosion phase in the high aluminum zinc aluminum magnesium plating layer is difficult to judge by the traditional corrosion observation means.
In a first aspect, the present application provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium plating layer, where the method includes:
carrying out first microscopic scanning on the high aluminum zinc aluminum magnesium coating to be detected to obtain a curve L of the content of different characteristic elements i in the high aluminum zinc aluminum magnesium coating to be detected along with the change of depth i
Corroding the high aluminum zinc aluminum magnesium coating to be detected after the first microscopic scanning is carried out to obtain a corrosion coating;
carrying out second microscopic scanning on the corrosion plating layer to obtain a curve L 'of the content of different characteristic elements i in the corrosion plating layer changing along with the depth' i
According to said curve L i And the curve L' i Obtaining a preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected;
wherein the different characteristic elements i are Al elements, zn elements or Mg elements.
Further, the content of zinc element in the high aluminum zinc aluminum magnesium coating to be detected is 38-48wt.%, the content of aluminum element is 50-60wt.%, and the content of magnesium element is less than 2wt.%.
Further, carrying out first microscopic scanning on the high aluminum zinc aluminum magnesium coating to be detected to obtain the content of different characteristic elements i in the high aluminum zinc aluminum magnesium coating to be detected, which changes along with the depthCurve L of i The method specifically comprises the following steps:
carrying out first cleaning on the surface of the high aluminum zinc aluminum magnesium coating to be detected to obtain a first cleaned high aluminum zinc aluminum magnesium coating to be detected;
carrying out first drying on the high aluminum zinc aluminum magnesium coating to be detected after the first cleaning to obtain a first dried high aluminum zinc aluminum magnesium coating to be detected;
carrying out progressive first microscopic scanning on the surface of the first dried high aluminum zinc aluminum magnesium coating to be detected along the radial depth by adopting a glow spectrometer to obtain a curve L of the content of different characteristic elements i in the high aluminum zinc aluminum magnesium coating to be detected along with the change of the depth i
Furthermore, the size diameter of the high aluminum zinc aluminum magnesium coating to be detected is more than or equal to 2cm, the surface roughness Ra value is less than or equal to 3, and the sputtering depth is greater than the coating thickness.
Further, corroding the to-be-detected high aluminum zinc aluminum magnesium coating after the first microscopic scanning to obtain a corrosion coating; the method specifically comprises the following steps:
corroding the to-be-detected high aluminum zinc aluminum magnesium coating after the first microscopic scanning, and then carrying out second cleaning to obtain a second cleaned corrosion coating;
carrying out second drying on the corrosion coating after the second cleaning to obtain a corrosion coating;
wherein the second cleaning comprises: and soaking and cleaning the corroded surface by using a rust remover, and then washing the corroded surface by using deionized water.
Further, the rust remover includes at least one of glycine, ammonium chloride, chromium trioxide, hydroiodic acid, and ammonium persulfate.
Further, the corrosion mode comprises at least one of week immersion corrosion, full immersion corrosion and erosion corrosion.
Further, carrying out second microscopic scanning on the corrosion plating layer to obtain a curve L 'of the content of different characteristic elements i in the corrosion plating layer changing along with the depth' i The method specifically comprises the following steps:
using glow spectrometerCarrying out progressive second microscopic scanning on the surface of the corrosion plating layer along the radial depth to obtain a curve L 'of the content of different characteristic elements i in the corrosion plating layer changing along with the depth' i
Further, the curve L is used for i And the curve L' i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected, which specifically comprises the following steps:
according to said curve L i To obtain a curve L i Integral area S of i
According to the curve L' i To give a curve L' i Integrated area S 'of' i
According to the integral area S i And the integrated area S' i Obtaining the integral area reduction rate H of different characteristic elements I before and after corrosion by the formula (I) i
The formula (I):
H i =(S i -S’ i )/S i x is 100%; wherein H i Representing the integral area reduction rate of different characteristic elements i, wherein i is Al element, zn element or Mg element;
according to the integral area reduction rate H of the different characteristic elements i i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected.
Further, the integral area reduction rate H according to the different characteristic elements i i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected, which specifically comprises the following steps:
according to the integral area reduction rate H of the different characteristic elements i i Obtaining a preferential corrosion phase in the high aluminum zinc aluminum magnesium plating layer to be detected through a judgment formula (II);
the decision formula (II):
if H is Mg >H Zn >H Al And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: mgZn 2 Phase (C)>Zinc rich phase>An aluminum-rich phase;
if H Mg >H Al >H Zn Then it is statedThe order of preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: mgZn 2 Phase (C)>Phase rich in aluminum>A zinc-rich phase;
if H Zn >H Mg >H Al And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: zinc rich phase>MgZn 2 Phase (C)>An aluminum-rich phase;
if H is Zn >H Al >H Mg And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: zinc rich phase>Rich in aluminium>MgZn 2 Phase (1);
if H is Al >H Mg >H Zn And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: phase rich in aluminum>MgZn 2 Phase (C)>A zinc-rich phase;
if H is Al >H Zn >H Mg And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: phase rich in aluminum>Zinc rich phase>MgZn 2 And (4) phase(s).
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
the embodiment of the application provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium coating, and a curve L of content variation with depth of different characteristic elements i (Al element, zn element or Mg element) in the high aluminum zinc aluminum magnesium coating before and after corrosion is respectively obtained through microscopic scanning detection i And curve L' i Therefore, the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected is obtained, and the technical problem that the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating is difficult to judge by the traditional corrosion observation means is effectively solved. The method has the advantages of high accuracy and good repeatability, and shows wide application prospect.
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The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a schematic flow chart of a method for detecting a preferential corrosion phase in a high Al-Zn-Al-Mg coating according to an embodiment of the present invention;
FIG. 2 is a graph showing the content of different characteristic elements in the Al-Mg-Al coating before and after etching according to example 1 of the present application as a function of depth; wherein 0h is a corresponding curve before corrosion; 168h is a corresponding curve after corrosion;
FIG. 3 is a graph showing the content of different characteristic elements in the Al-Mg-Al coating before and after etching according to example 2 of the present application as a function of depth; wherein 0h is a corresponding curve before corrosion; and 240h is a curve corresponding to the corroded part.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, 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. If there is a conflict, the present specification will control.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention may be commercially available or may be prepared by existing methods.
The zinc-aluminum-magnesium plating layer is a ternary alloy plating layer formed by adding a small amount of aluminum and magnesium elements on the basis of a pure zinc plating layer, and compared with the traditional pure zinc plating layer, the zinc-aluminum-magnesium plating layer has more excellent corrosion resistance.
At present, the corrosion resistance of the coating materialAnd (4) evaluating, generally performing an accelerated corrosion test on the alloy, and calculating the corrosion weight loss rate by adopting a chemical derusting method. The method has the following disadvantages: (1) In the corrosion test process, the corrosion rate of a base body at a notch of a coated steel plate is far greater than that of a coating, edge sealing treatment is usually carried out on the notch around the coated steel plate in order to avoid the influence of notch corrosion, so that great errors can be brought in weight loss weighing before and after corrosion and calculation of the corrosion rate, and particularly, when corrosion products at the initial stage of corrosion are less, great deviation can be caused in the corrosion rate. (2) The method can only calculate the average corrosion rate of the coating material, is suitable for products with uniform coating on the surface and uniform corrosion on the coating, and for high-aluminum zinc aluminum magnesium coating, the surface of the coating comprises an aluminum-rich phase, a zinc-rich phase and MgZn 2 The phase composition, due to the different corrosion potentials between the different phases, differs in corrosion rates of the different phases in different corrosion tests, and does not corrode uniformly. Therefore, the relative corrosion sequence between different phases of the traditional corrosion weight loss method is difficult to judge, and the influence of local corrosion on the durability of the plating material is more serious.
In order to solve the technical problems, the embodiment of the invention provides the following general ideas:
in a first aspect, the present application provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium coating, as shown in fig. 1, the method includes:
carrying out first microscopic scanning on the high aluminum zinc aluminum magnesium coating to be detected to obtain a curve L of the content of different characteristic elements i in the high aluminum zinc aluminum magnesium coating to be detected, which changes with the depth i
Corroding the high aluminum zinc aluminum magnesium coating to be detected after the first microscopic scanning to obtain a corrosion coating;
carrying out second microscopic scanning on the corrosion plating layer to obtain a curve L 'of the content of different characteristic elements i in the corrosion plating layer changing along with the depth' i
According to said curve L i And the curve L' i Obtaining a preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected;
wherein the different characteristic elements i are Al elements, zn elements or Mg elements.
The embodiment of the application provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium coating, and a curve L of content variation with depth of different characteristic elements i (Al element, zn element or Mg element) in the high aluminum zinc aluminum magnesium coating before and after corrosion is respectively obtained through microscopic scanning detection i And curve L' i Therefore, the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected is obtained, and the technical problem that the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating is difficult to judge by the traditional corrosion observation means is effectively solved. The method has the advantages of high accuracy and good repeatability, and shows wide application prospect.
As an implementation manner of the embodiment of the present application, in terms of mass fractions, the content of zinc element in the to-be-detected high aluminum zinc aluminum magnesium plating layer is 38 to 48wt.%, the content of aluminum element is 50 to 60wt.%, and the content of magnesium element is less than 2wt.%.
In the application, the zinc-aluminum-magnesium coating is a high-aluminum-zinc-aluminum-magnesium coating, and the content of zinc element, the content of aluminum element and the content of magnesium element in the high-aluminum-zinc-aluminum-magnesium coating to be detected are respectively 38-48wt.%, 50-60wt.% and 50-60wt.%, respectively<2wt.%. In the high aluminum zinc aluminum magnesium plating layer, the MgZn in the high aluminum zinc aluminum magnesium is 2 The phase content is small, and therefore the reduction rate of the Zn element content can be approximated to the reduction rate of the Zn-rich phase content.
As an implementation manner of the embodiment of the application, a first microscopic scanning is performed on a to-be-detected high aluminum zinc aluminum magnesium plating layer to obtain a curve L of the to-be-detected high aluminum zinc aluminum magnesium plating layer with the content of different characteristic elements i changing with the depth i The method specifically comprises the following steps:
carrying out first cleaning on the surface of the high aluminum zinc aluminum magnesium coating to be detected to obtain a first cleaned high aluminum zinc aluminum magnesium coating to be detected;
carrying out first drying on the high aluminum zinc aluminum magnesium coating to be detected after the first cleaning to obtain a first dried high aluminum zinc aluminum magnesium coating to be detected;
adopting a glow spectrometer to perform radial depth feeding on the surface of the first dried high aluminum zinc aluminum magnesium coating to be detectedPerforming progressive first microscopic scanning to obtain a curve L of the content of different characteristic elements i in the high aluminum zinc aluminum magnesium coating to be detected along with the change of depth i
In this application, in some embodiments, the specific process of the first cleaning may be: ultrasonic cleaning with ethanol to remove oil stain and impurities on the surface of the coating; the specific process of the first drying can be cold air drying.
As an implementation mode of the embodiment of the application, the size diameter of the high aluminum zinc aluminum magnesium plating layer to be detected is more than or equal to 2cm, the surface roughness Ra value is less than or equal to 3, and the sputtering depth is greater than the thickness of the plating layer.
In the application, the sputtering depth specifically refers to the element detection depth of the glow discharge spectrometer, and the sputtering depth needs to be larger than the thickness of the coating because the integral is the integral of the whole coating, so that the area reduction rate is convenient to calculate.
In the application, the effect of controlling the size diameter of the high aluminum zinc aluminum magnesium coating to be detected to be more than or equal to 2cm is that the detection diameter of a glow discharge spectrometer is 0.1-0.8cm, and the high aluminum zinc aluminum magnesium coating to be detected is too small to be detected.
As an implementation manner of the embodiment of the present application, the high aluminum zinc aluminum magnesium plating layer to be detected after the first microscopic scanning is etched to obtain an etched plating layer; the method specifically comprises the following steps:
corroding the to-be-detected high aluminum zinc aluminum magnesium coating after the first microscopic scanning, and then carrying out second cleaning to obtain a second cleaned corrosion coating;
carrying out second drying on the corrosion coating after the second cleaning to obtain a corrosion coating;
wherein the second cleaning comprises: and soaking and cleaning the corroded surface by using a rust remover, and then washing the corroded surface by using deionized water.
In this application, adopt the rust remover to soak the washing to corroding the surface, later use deionized water to wash corroding the surface, be favorable to follow-up carry out the second microscopic scanning to corroding the cladding material, improve measurement accuracy.
As an implementation of the embodiments herein, the rust remover includes at least one of glycine, ammonium chloride, chromium trioxide, hydroiodic acid, and ammonium persulfate.
As an implementation manner of the embodiment of the present application, the etching manner includes at least one of an immersion etching, a full immersion etching, and a erosion etching.
In the present application, the weekly immersion corrosion can be carried out according to the periodic immersion corrosion test method described in Standard HB 5194-1981.
In the application, the full immersion corrosion is also called full immersion zone corrosion, and particularly refers to the corrosion of a full immersion part of a metal component, which can be carried out according to a uniform corrosion full immersion test method in a metal material laboratory described in the standard GB 10124-1988.
Erosion corrosion in this application is metal damage caused by high speed relative motion between the metal surface and the corrosive fluid. Typically in a static or low velocity flowing corrosive medium, corrosion is not severe, but when the corrosive fluid moves at high velocity, it destroys the surface film or corrosion product film that the metal surface can provide protection against, and the thinning or removal of the surface film accelerates the corrosion process of the metal, so that erosive corrosion is a result of the synergistic effect of the erosive and corrosive fluids. The method mainly comprises the following steps: a rotary method, a pipe flow method, an impact jet method, a high-speed scouring method, and the like.
As an implementation manner of the embodiment of the application, the corrosion coating layer is subjected to second microscopic scanning to obtain a curve L 'of the content of different characteristic elements i in the corrosion coating layer along with the change of the depth' i The method specifically comprises the following steps:
carrying out progressive second microscopic scanning on the surface of the corrosion coating along the radial depth by adopting a glow spectrometer to obtain a curve L 'of the content of different characteristic elements i in the corrosion coating along with the change of the depth' i
As an implementation manner of the embodiment of the present application, the curve L is obtained according to the above i And the curve L' i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium plating layer to be detected, which specifically comprises:
according to said curve L i To obtain a curve L i Integral area S of i
According to the curve L' i To give a curve L' i Integrated area S 'of' i
According to the integral area S i And the integrated area S' i Obtaining the integral area reduction rate H of different characteristic elements I before and after corrosion by the formula (I) i
The formula (I):
H i =(S i -S’ i )/S i x is 100%; wherein H i Representing the integral area reduction rate of different characteristic elements i, wherein i is Al element, zn element or Mg element;
according to the integral area reduction rate H of the different characteristic elements i i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected.
In the present application, according to the curve L i To obtain a curve L i Integral area S of i Can be directly aligned with the curve L on a glow spectrometer i Integrating to obtain an integral area S i (ii) a Or by following the curve L in Origin mapping software i Integrated area S i . "according to the curve L' i To obtain a curve L i Integrated area S 'of' i "according to said curve L i To obtain a curve L i Integral area S of i The process is the same.
As an implementation manner of the embodiment of the present application, the integral area reduction rate H according to the different feature elements i i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected, which specifically comprises the following steps:
according to the integral area reduction rate H of the different characteristic elements i i Obtaining a preferential corrosion phase in the high aluminum zinc aluminum magnesium plating layer to be detected through a judgment formula (II);
the decision formula (II):
if H is Mg >H Zn >H Al And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: mgZn 2 Phase (C)>Zinc rich phase>An aluminum-rich phase;
if H is Mg >H Al >H Zn And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: mgZn 2 Phase (C)>Phase rich in aluminum>A zinc-rich phase;
if H is Zn >H Mg >H Al And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: zinc rich phase>MgZn 2 Phase (C)>An aluminum-rich phase;
if H is Zn >H Al >H Mg And then the order of the preferential corrosion phase in the high aluminum zinc aluminum magnesium plating layer to be detected is as follows: zinc rich phase>Rich in aluminium>MgZn 2 Phase (1);
if H is Al >H Mg >H Zn And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: phase rich in aluminum>MgZn 2 Phase(s)>A zinc-rich phase;
if H is Al >H Zn >H Mg And then the order of the preferential corrosion phase in the high aluminum zinc aluminum magnesium plating layer to be detected is as follows: phase rich in aluminum>Zinc rich phase>MgZn 2 And (4) phase(s).
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental methods of the following examples, which are not specified under specific conditions, are generally determined according to national standards. If there is no corresponding national standard, it is carried out according to the usual international standards, to the conventional conditions or to the conditions recommended by the manufacturer.
Example 1
The embodiment provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium coating, which specifically comprises the following steps:
the processing object is as follows: the high aluminum zinc plating material is subjected to a 168-hour soaking test (a sodium bisulfite system); wherein, the content of zinc element in the high aluminum zinc aluminum magnesium coating to be detected is 38-48wt.%, the content of aluminum element is 50-60wt.%, and the content of magnesium element is less than 2wt.%.
1. Firstly, carrying out ethanol ultrasonic cleaning on a high-aluminum zinc aluminum magnesium plated steel plate to remove surface oil stains and impurities, then carrying out progressive scanning on the zinc aluminum magnesium plated steel plate from the surface along the radial depth by adopting a glow spectrometer to obtain a curve of the change of the contents of Zn, al and Mg elements of the plating along with the depth, wherein the result is shown in figure 2 (specifically, the curve is shown by 0 h), and the curves are respectively integrated, wherein the integral area of the Zn element curve is 325.9, the integral area of the Al element curve is 234.3, and the integral area of the Mg element curve is 11.5.
2. Carrying out a periimmersion accelerated corrosion test on a sample according to the GB/T19746-2005 'periimmersion test of corrosive salt solution of metal and alloy', sampling after 168 hours for derusting, carrying out immersion cleaning on a corrosion product by adopting an ammonium acetate cleaning solution (the mass ratio of ammonium acetate to deionized water is 1:4), flushing residual cleaning solution by adopting deionized water, and drying by cold air.
3. The coating steel plate after rust removal is subjected to depth distribution scanning of Zn, al and Mg elements by using a glow spectrometer, as shown in figure 2 (specifically, a curve shown by 168 h), and curves of the coating steel plate are respectively integrated to obtain the integral area of a Zn element curve of 195.9, the integral area of an Al element curve of 158.3 and the integral area of an Mg element curve of 1.2.
4. Calculating the reduction rate of the Zn element content according to the integral result: (325.9-195.9)/325.9X 100% =39.9%
Reduction rate of Al element content: (234.3-158.3)/234.3X 100% =32.4%
Reduction rate of Mg element content: (11.5-1.2)/11.5X 100% =89.6%
5. Because Mg element is mainly MgZn 2 Form exists, from which MgZn can be obtained 2 Preferential corrosion is carried out, and simultaneously, because the eutectic phase content in the high aluminum zinc aluminum magnesium is less, the reduction rate of the Zn element content can be approximate to the reduction rate of the zinc-rich phase content, so the corrosion rate MgZn 2 >Zinc rich phase>An aluminum-rich phase; i.e. the order of preferential corrosion phases is MgZn 2 >Zinc rich phase>An aluminum-rich phase.
Example 2
The embodiment provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium coating, which specifically comprises the following steps:
the processing object is as follows: the high aluminum zinc plating material is subjected to a 240-hour soaking test (sodium bisulfite system); wherein, the content of zinc element in the high aluminum zinc aluminum magnesium coating to be detected is 38-48wt.%, the content of aluminum element is 50-60wt.%, and the content of magnesium element is less than 2wt.%.
1. Firstly, carrying out ethanol ultrasonic cleaning on a zinc-aluminum-magnesium coating steel plate to remove oil stains and impurities on the surface, then carrying out progressive scanning on the zinc-aluminum-magnesium coating steel plate from the surface along the radial depth by adopting a glow spectrometer to obtain a curve of the content of Zn, al and Mg elements of the coating along with the depth, wherein the result is shown in figure 3 (specifically a curve shown by 0 h), and the curve is respectively integrated, wherein the integral area of the Zn element curve is 325.9, the integral area of the Al element curve is 234.3, and the integral area of the Mg element curve is 11.5.
2. Carrying out a periimmersion accelerated corrosion test on a sample according to the GB/T19746-2005 'periimmersion test of corrosive salt solution of metal and alloy', sampling after 240h for derusting, carrying out immersion cleaning on a corrosion product by adopting an ammonium acetate cleaning solution (the mass ratio of ammonium acetate to deionized water is 1:4), flushing residual cleaning solution by adopting deionized water, and drying by cold air;
3. the coating steel plate after rust removal is subjected to deep distribution scanning of Zn, al and Mg elements by using a glow spectrometer, as shown in figure 3 (specifically, a curve shown by 240 h), and the curve is respectively integrated to obtain that the integral area of the Zn element curve is 91.3, the integral area of the Al element curve is 121.1, and the integral area of the Mg element curve is 0.78.
4. Calculating the reduction rate of the Zn element content according to the integral result: (325.9-91.3)/325.9 × 100% =72.0%
Reduction rate of Al element content: (234.3-121.1)/234.3 × 100% =48.3%
Reduction rate of Mg element content: (11.5-0.78)/11.5X 100% =93.2%
5. Because Mg element is mainly MgZn 2 Form exists, from which MgZn can be obtained 2 Preferential corrosion is carried out, and simultaneously, because the content of the eutectic phase of the high aluminum zinc aluminum magnesium is less, the reduction rate of the Zn element content can be approximate to the reduction rate of the zinc-rich phase content, so the corrosion rate MgZn 2 >Zinc rich phase>An aluminum-rich phase; i.e. the order of preferential corrosion phases is MgZn 2 >Zinc rich phase>An aluminum rich phase.
Comparative example 1
The embodiment provides a method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium plating layer by adopting a traditional method, which specifically comprises the following steps:
the processing object is as follows: the high aluminum zinc aluminum magnesium material is subjected to a weekly soaking test for 240h (sodium bisulfite system); wherein, the content of zinc element in the high aluminum zinc aluminum magnesium coating to be detected is 38-48wt.%, the content of aluminum element is 50-60wt.%, and the content of magnesium element is less than 2wt.%.
1. Ultrasonically cleaning a high-aluminum zinc aluminum magnesium plated steel plate with ethanol, removing oil stains and impurities on the surface of the steel plate, measuring the size of a sample, and calculating the corrosion area to be 4cm multiplied by 10cm =40cm 2 Weighing the weight m of the original plate before the corrosion test 0 Is 20.3356g.
2. Carrying out accelerated corrosion test by GB/T19746-2005 'Metal and alloy corrosive salt solution Weekly immersion test', sampling after 240h for derusting, soaking and cleaning corrosion products by ammonium acetate cleaning liquid (the mass ratio of ammonium acetate to deionized water is 1:4), flushing residual cleaning liquid by deionized water, and drying by cold air;
3. weighing the derusted sample by using an electronic balance to obtain a weight m 1 For 19.8586g, the formula for the etch rate calculation is (20.3356-19.8586)/(40X 240X 2) g cm -2 h -1 =2.48×10 -5 g cm -2 h -1 =0.25g m -2 h -1 . The calculated corrosion rate is the average corrosion rate of the whole steel plate, and the preferential corrosion phase cannot be judged.
It should be understood that the endpoints of the ranges and any values disclosed herein are not limited to the precise range or value and that such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
It is noted that, in this document, relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. In addition, the term "and/or" appearing herein is merely one type of association that describes an associated object, meaning that three relationships may exist, e.g., a and/or B, may mean: a exists alone, A and B exist simultaneously, and B exists alone.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. A method for detecting a preferential corrosion phase in a high aluminum zinc aluminum magnesium plating layer, comprising:
carrying out first microscopic scanning on the high aluminum zinc aluminum magnesium coating to be detected to obtain a curve L of the content of different characteristic elements i in the high aluminum zinc aluminum magnesium coating to be detected along with the change of depth i
Corroding the high aluminum zinc aluminum magnesium coating to be detected after the first microscopic scanning is carried out to obtain a corrosion coating;
carrying out second microscopic scanning on the corrosion plating layer to obtain a curve L 'of the content of different characteristic elements i in the corrosion plating layer changing along with the depth' i
According to said curve L i And the curve L' i Obtaining the height to be detectedA preferential corrosion phase in the aluminum-zinc-aluminum-magnesium coating;
wherein the different characteristic elements i are Al elements, zn elements or Mg elements.
2. The method for detecting the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating as claimed in claim 1, wherein the content of zinc element in the high aluminum zinc aluminum magnesium coating to be detected is 38-48wt.%, the content of aluminum element is 50-60wt.%, and the content of magnesium element is less than 2wt.%.
3. The method for detecting the preferential corrosion phase in the AlMgAl layer of claim 1, wherein the AlMgAl layer to be detected is first scanned to obtain a curve L of the depth variation of the content of different characteristic elements i in the AlMgAl layer to be detected i The method specifically comprises the following steps:
carrying out first cleaning on the surface of the high aluminum zinc aluminum magnesium coating to be detected to obtain a first cleaned high aluminum zinc aluminum magnesium coating to be detected;
carrying out first drying on the high aluminum zinc aluminum magnesium coating to be detected after the first cleaning to obtain a first dried high aluminum zinc aluminum magnesium coating to be detected;
carrying out progressive first microscopic scanning on the surface of the first dried high aluminum zinc aluminum magnesium coating to be detected along the radial depth by adopting a glow spectrometer to obtain a curve L of the content of different characteristic elements i in the high aluminum zinc aluminum magnesium coating to be detected along with the change of the depth i
4. The method for detecting the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating according to claim 1, wherein the size diameter of the high aluminum zinc aluminum magnesium coating to be detected is more than or equal to 2cm, the surface roughness Ra value is less than or equal to 3, and the sputtering depth is greater than the coating thickness.
5. The method for detecting the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating according to claim 1, wherein the high aluminum zinc aluminum magnesium coating to be detected after the first microscopic scanning is corroded to obtain a corrosion coating; the method specifically comprises the following steps:
corroding the to-be-detected high aluminum zinc aluminum magnesium coating after the first microscopic scanning, and then carrying out second cleaning to obtain a second cleaned corrosion coating;
carrying out second drying on the corrosion coating after the second cleaning to obtain a corrosion coating;
wherein the second cleaning comprises: and soaking and cleaning the corroded surface by using a rust remover, and then washing the corroded surface by using deionized water.
6. The method of detecting preferential corrosion phases in a high aluminum zinc aluminum magnesium coating of claim 5 wherein said rust removing agent comprises at least one of glycine, ammonium chloride, chromium trioxide, hydroiodic acid, and ammonium persulfate.
7. The method of detecting preferential corrosion phases in a high aluminum zinc aluminum magnesium coating of claim 1 wherein said corrosion mode comprises at least one of a week dip corrosion, a full dip corrosion and a wash-out corrosion.
8. The method for detecting the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating according to claim 1, wherein the corrosion coating is subjected to a second microscopic scanning to obtain a curve L 'of the content of different characteristic elements i in the corrosion coating along with the depth' i The method specifically comprises the following steps:
carrying out progressive second microscopic scanning on the surface of the corrosion coating along the radial depth by adopting a glow spectrometer to obtain a curve L 'of the content of different characteristic elements i in the corrosion coating along with the change of the depth' i
9. The method of claim 1, wherein said detecting a preferential corrosion phase in said high al-zn-al-mg coating is according to said curve L i And the curve L' i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected, which specifically comprises the following steps:
according to said curve L i To obtain a curve L i Integral area S of i
According to the curve L' i To give a curve L' i Integrated area S 'of' i
According to the integral area S i And the integrated area S' i Obtaining the integral area reduction rate H of different characteristic elements I before and after corrosion by the formula (I) i
The formula (I):
H i =(S i -S’ i )/S i x is 100%; wherein H i Represents the integral area reduction rate of different characteristic elements i, wherein i is Al element, zn element or Mg element;
according to the integral area reduction rate H of the different characteristic elements i i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected.
10. The method of claim 9, wherein the reduction rate H is an integral area of the different characteristic elements i i And obtaining the preferential corrosion phase in the high aluminum zinc aluminum magnesium coating to be detected, which specifically comprises the following steps:
according to the integral area reduction rate H of the different characteristic elements i i Obtaining a preferential corrosion phase in the high aluminum zinc aluminum magnesium plating layer to be detected through a judgment formula (II);
the decision formula (II):
if H is Mg >H Zn >H Al And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: mgZn 2 Phase (C)>Zinc rich phase>An aluminum-rich phase;
if H is Mg >H Al >H Zn And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: mgZn 2 Phase (C)>Phase rich in aluminum>A zinc-rich phase;
if H is Zn >H Mg >H Al And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: rich inZinc phase>MgZn 2 Phase (C)>An aluminum-rich phase;
if H is Zn >H Al >H Mg And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: zinc rich phase>Rich in aluminium>MgZn 2 Phase (1);
if H is Al >H Mg >H Zn And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: phase rich in aluminum>MgZn 2 Phase (C)>A zinc-rich phase;
if H is Al >H Zn >H Mg And then, the order of the preferential corrosion phases in the high aluminum zinc aluminum magnesium coating to be detected is as follows: phase rich in aluminum>Zinc rich phase>MgZn 2 And (4) phase(s).
CN202211112764.0A 2022-09-14 2022-09-14 Method for detecting preferential corrosion phase in high-aluminum zinc aluminum magnesium coating Pending CN115656013A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117907562A (en) * 2024-03-19 2024-04-19 张家港扬子江冷轧板有限公司 Method for simultaneously detecting contents of multiple elements in coating

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117907562A (en) * 2024-03-19 2024-04-19 张家港扬子江冷轧板有限公司 Method for simultaneously detecting contents of multiple elements in coating
CN117907562B (en) * 2024-03-19 2024-06-04 张家港扬子江冷轧板有限公司 Method for simultaneously detecting contents of multiple elements in coating

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