CN114606486A - Magnesium alloy CaCO3Conversion film treating agent and treating method thereof - Google Patents
Magnesium alloy CaCO3Conversion film treating agent and treating method thereof Download PDFInfo
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- CN114606486A CN114606486A CN202210237105.3A CN202210237105A CN114606486A CN 114606486 A CN114606486 A CN 114606486A CN 202210237105 A CN202210237105 A CN 202210237105A CN 114606486 A CN114606486 A CN 114606486A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/68—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous solutions with pH between 6 and 8
Abstract
The invention discloses a magnesium alloy CaCO3The treatment agent for the conversion coating comprises CaCl2Aqueous solution with NaHCO3Aqueous solution of CaCl2Aqueous solution with NaHCO3The volume ratio of the aqueous solution is 1 (1-4). The invention also discloses a magnesium alloy CaCO3The treatment method of the conversion coating treatment agent comprises the following steps: A) putting the magnesium alloy into a degreasing agent for degreasing and deoiling; B) putting the magnesium alloy after degreasing and deoiling treatment into magnesium alloy CaCO3And (3) in the conversion film treating agent, taking out after water bath treatment for 1-6h, then ultrasonically cleaning for 3-10 min by using deionized water and ethanol, and drying by hot air. The invention provides magnesium alloy CaCO3The conversion coating treating agent is particularly suitable for engineering construction, and has the characteristics of safety, environmental protection, good corrosion resistance and capability of providing long-acting protection for a magnesium alloy matrix.
Description
Technical Field
The invention belongs to the technical field of magnesium alloy surface conversion film treatment, and particularly relates to magnesium alloy CaCO suitable for the field of buildings3A conversion coating treating agent and a treating method thereof.
Background
Magnesium is one of the most abundant elements in the earth crust and the ocean, and magnesium alloy is the lightest structural metal, so that at present, magnesium alloy is widely concerned in the fields of automobiles, aerospace, electronic technology, biomedicine and the like, but the research in building engineering is very little. The magnesium alloy has the advantages of low density and high specific strength, has the potential of becoming a building material, has large chemical activity of magnesium, low standard electrode potential, and PB ratio of a surface film generated in a natural environment of less than 1, and can greatly improve the corrosion resistance of the magnesium alloy by preparing the film on the surface of the magnesium alloy through surface modification and a chemical conversion technology.
The prior magnesium alloy surface chemical conversion film mainly comprises phosphate, molybdate, chromate, stannate, phytate and the like, and most of magnesium alloys in industrial production are processed by conversion films containing chromate, so that the safety is poor. Chromium is a heavy metal with high toxicity, easily enters human body cells, damages internal organs such as liver, kidney and the like and DNA, accumulates in human body, has carcinogenicity and possibly induces gene mutation, and the method for processing the chromate-containing conversion coating has great harm to human body and is not suitable for being used in constructional engineering; although chemical conversion coating treatment methods using molybdate or phosphate instead of chromate have appeared in the prior art, which can be used to reduce the harm to human body, the thickness of molybdate is generally about 1 μm, and is thin, so that it cannot provide long-term protection for magnesium alloy matrix; the calcium phosphate film is widely developed and used in the field of biomedicine and cannot stably exist in the alkaline environment of engineering buildings.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention mainly aims to provide magnesium alloy CaCO which is safe and environment-friendly and has good corrosion resistance and can provide long-term protection for a magnesium alloy matrix in engineering construction3And (3) a conversion coating treating agent. The invention also provides the magnesium alloy CaCO3A method for treating a conversion coating treating agent.
The purpose of the invention is realized by the following technical scheme:
in a first aspect, a magnesium alloy CaCO3A conversion coating treatment agent comprising CaCl2Aqueous solution with NaHCO3Aqueous solution of said CaCl2Aqueous solution with NaHCO3The volume ratio of the aqueous solution is 1 (1-4).
Preferably, wherein said CaCl2Aqueous solution with NaHCO3The volume ratio of the aqueous solution was 1: 3.
Preferably, wherein said NaHCO3The mass concentration of the aqueous solution is 0.5-1.5mol/L, and the CaCl is2The mass concentration of the aqueous solution is 0.5-1.5 mol/L.
Preferably, wherein said NaHCO3The mass concentration of the aqueous solution is 1.0mol/L, and the CaCl is2The mass concentration of the aqueous solution was 1.5 mol/L.
In a second aspect: the magnesium alloy CaCO3The treatment method of the conversion coating treatment agent comprises the following steps:
A) putting the magnesium alloy into a degreasing agent for degreasing and deoiling;
B) putting the magnesium alloy after degreasing and deoiling treatment into the magnesium alloy CaCO3In the conversion film treating agent, after water bath treatment for 1-6hTaking out, ultrasonically cleaning with deionized water and ethanol for 3-10 minutes, and drying with hot air.
Preferably, wherein the temperature of the water bath treatment is 45-85 ℃.
Preferably, wherein the temperature of the water bath treatment is 50 ℃.
Preferably, wherein the temperature of the water bath treatment is 80 ℃.
Compared with the prior art, the invention has at least the following advantages:
1) the invention provides magnesium alloy CaCO3The raw materials of the conversion film treating agent are simple and easy to obtain, and the cost is low, namely the CaCO3The conversion film has low manufacturing cost, is safe and environment-friendly, and does not threaten the health and safety of constructors. And aiming at the mass used concrete in the construction field, the environment of the concrete is alkaline, and CaCO3The conversion coating can not corrode under the alkaline environment and can stably exist, namely CaCO attached to the surface of the magnesium alloy3The conversion film does not react in the concrete environment; when chloride ions appear, the surface film layer of the magnesium alloy is formed by tightly combining compact calcium carbonate particles, so that the chloride ions cannot pass through and cannot corrode a magnesium alloy matrix within a certain service cycle.
2) The invention provides magnesium alloy CaCO3Method for treating conversion coating agent capable of forming CaCO having excellent corrosion resistance on magnesium alloy surface by simple low-temperature water bath3The thickness of the film layer can reach 3-5 mu m, the impedance value in plain concrete is greatly improved, and the film belongs to a magnesium alloy surface protective film with good corrosion resistance and has good engineering application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention, reference will now be made briefly to the embodiments or to the accompanying drawings that are needed in the description of the prior art.
FIG. 1 is an SEM image of the surface microstructure of a magnesium alloy provided by treatment method 1 in example 2 of the present invention; (20 μm)
FIG. 2 is an SEM image of the surface microstructure of the magnesium alloy provided by the treatment method 1 in example 2 of the present invention; (2 μm)
FIG. 3 is an impedance spectrum at 1h of the magnesium alloy provided by the treatment method 1 in example 2 of the present invention;
FIG. 4 is an impedance spectrum at 96h of the magnesium alloy provided by the treatment method 1 in example 2 of the present invention;
FIG. 5 is a plot of the polarization of a magnesium alloy after 96 hours as provided by treatment method 1 in example 2 of the present invention;
FIG. 6 is an SEM image of the surface microstructure of a magnesium alloy provided by treatment method 2 in example 2 of the present invention; (10 μm)
FIG. 7 is an SEM image of the surface microstructure of a magnesium alloy provided by treatment method 2 in example 2 of the present invention; (2 μm)
FIG. 8 is an impedance spectrum at 1h of a magnesium alloy provided by the treatment method 2 in example 2 of the present invention;
FIG. 9 is an impedance spectrum at 96h of a magnesium alloy provided by treatment method 2 in example 2 of the present invention;
FIG. 10 is a plot of the polarization of the magnesium alloy provided by treatment method 2 of example 2 of the present invention after 96 hours.
Detailed Description
The present invention will be further described with reference to the following drawings and examples, which are illustrative only and not intended to be limiting, and the scope of the present invention is not limited thereby.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or upper and lower limit of preferred values, it is understood that any range by combining any pair of range upper limits or preferred values with any range lower limits or preferred values is expressly disclosed without regard to whether or not such range is expressly disclosed. Unless otherwise indicated, numerical range values set forth herein are intended to include the endpoints of the range, and all integers and fractions within the range.
The materials, methods, and examples herein are illustrative and, unless otherwise specified, are not to be construed as limiting.
In the following embodiment of the invention, a Zeiss Auriga focused ion beam field emission scanning double-beam electron microscope is adopted to scan the surface micro-morphology of the magnesium alloy;
the electrochemical performance of the magnesium alloy was tested by corrosion of GB/T40299-2021 metals and alloys in the following examples of the invention.
The invention provides a magnesium alloy CaCO3The conversion coating treating agent comprises CaCl2Aqueous solution and NaHCO3Aqueous solution of said CaCl2Aqueous solution and NaHCO3The volume ratio of the aqueous solution is 1 (1-4), further, the CaCl is2Aqueous solution and NaHCO3The volume ratio of the aqueous solution is 1: 3; wherein said NaHCO3The mass concentration of the aqueous solution is 0.5-1.5mol/L, and the CaCl is2The mass concentration of the aqueous solution is 0.5-1.5 mol/L; further, wherein said NaHCO3The mass concentration of the aqueous solution is 1.0mol/L, and the CaCl is2The mass concentration of the aqueous solution was 1.5 mol/L.
NaHCO is used in the present application3The mass concentration of the aqueous solution is set to 0.5-1.5mol/L, CaCl2The amount concentration of the aqueous solution is 0.5-1.5mol/L for ensuring 2NaHCO3+CaCl22NaCl + CaCO ═ (heating)3↓+H2O+CO2The execution of the ↓reaction, during the specific use, through adjusting the volume ratio of the coating solution to ensure the execution of the experiment, generally control NaHCO3The mass concentration of the aqueous solution is not higher than 1.5mol/L, CaCl2When the mass concentration of the aqueous solution is not higher than 1.5mol/L, the reaction is prevented from generating excessive calcium carbonate, which causes unnecessary waste.
Wherein NaHCO3Aqueous solution and CaCl2The starting materials for the aqueous solutions are either commercially available or formulated by means of conventional techniques in the art.
The magnesium alloy CaCO3The treatment method of the conversion coating treatment agent comprises the following steps:
A) putting the magnesium alloy into a degreasing agent for degreasing and deoiling;
B) putting the magnesium alloy which is degreased and deoiled intoThe above magnesium alloy CaCO3In the conversion film treating agent, taking out after water bath treatment for 1-6h, then ultrasonically cleaning for 3-10 min by using deionized water and ethanol, and drying by hot air, wherein the water bath treatment temperature is 45-85 ℃; further preferably, the temperature of the water bath treatment is 50 ℃, or further preferably, the temperature of the water bath treatment is 80 ℃.
The water bath treatment temperature is 45-85 ℃, so that the generation of calcium carbonate particles and the attachment of the calcium carbonate particles to the surface of the magnesium alloy are ensured; when the temperature rises, the effective collision among molecules is increased, which is not only beneficial to the formation of calcium carbonate particles, but also provides certain power for the combination of the calcium carbonate particles and the magnesium alloy matrix; the heating condition is favorable for the reaction, but the temperature is higher than 85 ℃, which causes the process to be complex and difficult to achieve; meanwhile, a certain time is needed for attaching calcium carbonate particles generated by chemical conversion to the surface of the magnesium alloy, and when the temperature is lower than 45 ℃, the calcium carbonate particles are not favorably attached to the surface of the magnesium alloy.
[ example 1 ] magnesium alloy CaCO3Components and proportion of conversion film treating agent
Component 1: the magnesium alloy CaCO of the invention3The conversion coating treating agent comprises CaCl with the volume ratio of 1:12Aqueous solution and NaHCO3An aqueous solution, wherein said NaHCO3The mass concentration of the aqueous solution is 1.2mol/L, and the CaCl is2The mass concentration of the aqueous solution was 0.6 mol/L.
And (2) component: the magnesium alloy CaCO of the invention3The conversion coating treatment agent comprises CaCl with the volume ratio of 1:22Aqueous solution and NaHCO3An aqueous solution, wherein said NaHCO3The mass concentration of the aqueous solution is 0.8mol/L, and the CaCl is2The mass concentration of the aqueous solution was 0.8 mol/L.
And (3) component: the magnesium alloy CaCO of the invention3The conversion coating treatment agent comprises CaCl with the volume ratio of 1:32Aqueous solution and NaHCO3An aqueous solution, wherein said NaHCO3The mass concentration of the aqueous solution is 1.0mol/L, and the CaCl is2The mass concentration of the aqueous solution was 1.5mol/L。
And (4) component: the magnesium alloy CaCO of the invention3The conversion coating treatment agent comprises CaCl with the volume ratio of 1:42Aqueous solution and NaHCO3An aqueous solution, wherein said NaHCO3The mass concentration of the aqueous solution is 0.6mol/L, and the CaCl is2The mass concentration of the aqueous solution was 1.2 mol/L.
And (5) component: the magnesium alloy CaCO of the invention3The conversion coating treatment agent comprises CaCl with the volume ratio of 1:12Aqueous solution and NaHCO3An aqueous solution, wherein said NaHCO3The mass concentration of the aqueous solution is 1.0mol/L, and the CaCl is2The mass concentration of the aqueous solution was 0.5 mol/L.
The invention provides magnesium alloy CaCO3The conversion coating treating agent is suitable for the field of industrial and civil buildings, is mainly used for magnesium alloy building templates, and improves the corrosion resistance of the magnesium alloy building templates in a concrete environment. The main component of the protective film is CaCO3The color of the film layer is grey white, the thickness of the protective film is 3-5 mu m, and the impedance value of the coated magnesium alloy in Portland cement is improved by 1.5-3 times compared with that of a bare alloy after 4 days.
In the field of civil engineering, a lot of magnesium alloys are suitable for magnesium alloy building templates, and the application takes Mg-3Nd alloy and AZ41 magnesium alloy as examples for explanation, wherein the Mg-3Nd alloy comprises the following components in percentage by weight: nd: 3%, and the balance of Mg and inevitable impurities; the AZ41 magnesium alloy comprises the following components in percentage by weight: al: 4.3 percent of Mn, 0.4 percent of Mn, 0.9 percent of Zn, and the balance of Mg and inevitable impurities.
[ example 2 ] magnesium alloy CaCO3Treatment method of conversion film treating agent
This example uses the magnesium alloy CaCO described in example 1 as component 33The conversion coating agent is described in detail as an example.
The processing method 1:
the invention relates to magnesium alloy CaCO3The treatment method of the conversion coating treatment agent selects the magnesium alloy as the Mg-3Nd alloy, and comprises the following steps:
1) sampling and slicing on an Mg-3Nd alloy plate, wherein the sizes of all samples for experiments are 10mm multiplied by 5 mm;
2) polishing the Mg-3Nd alloy sample prepared in the step 1) by using 1200# and 1500# SiC abrasive paper respectively, washing the surface by using deionized water, washing the surface by using ethanol in an ultrasonic cleaner for three minutes to remove surface impurities of the sample, and drying the sample by using hot air for later use;
3) placing the Mg-3Nd alloy sample treated in the step 2) into the magnesium alloy CaCO with the component 33And (3) treating the conversion film treating agent in a water bath at the temperature of 50 ℃ for 5 hours, taking out, then ultrasonically cleaning for 5 minutes by using deionized water and ethanol, and drying by hot air.
The performance test of the coated Mg-3Nd alloy obtained in the treatment method 1 specifically comprises the following steps: the microstructure of the surface of the coated magnesium alloy is shown in fig. 1 and 2. Carrying out electrochemical test on the magnesium alloy, wherein the test conditions are as follows: embedding the magnesium alloy in plain concrete stirred by 3.5 wt.% of NaCl, and performing electrochemical test on the impedance value and the polarization curve of the magnesium alloy, wherein the impedance value and the polarization curve are shown in fig. 3 and 4; the resistance value of bare alloy (uncoated magnesium alloy) in plain concrete is from the original 26.3 x 104Ω·cm2Up to 40.0X 104Ω·cm2. The impedance value of the coated magnesium alloy in plain concrete is 13 multiplied by 10 from the original impedance value4Ω·cm2Rises to 83.1X 104Ω·cm2The impedance value is improved by 2.1 times in 4 days; at the same time, after 96 hours, the corrosion current density was from 1.3X 10-7A·cm-2Down to 3.1X 10-8A·cm-2As shown in detail in fig. 5.
The treatment method 2 comprises the following steps:
the invention relates to magnesium alloy CaCO3The treatment method of the conversion coating treating agent selects magnesium alloy as AZ41 magnesium alloy, and comprises the following steps:
1) sampling and slicing AZ41 magnesium alloy plates, wherein the sizes of all samples for experiments are 10mm multiplied by 5 mm;
2) polishing the AZ41 magnesium alloy sample prepared in the step 1) by using 1200# and 1500# SiC abrasive paper respectively, washing the surface by using deionized water, washing the surface by using ethanol in an ultrasonic cleaner for three minutes to remove impurities on the surface of the sample, and drying the sample by using hot air for later use;
3) placing the AZ41 magnesium alloy sample treated in the step 2) into the magnesium alloy CaCO of the component 33And (3) treating the conversion film treating agent in a water bath at the temperature of 80 ℃ for 1.5h, taking out, ultrasonically cleaning for 3 minutes by using deionized water and ethanol, and drying by hot air.
And (3) carrying out performance test on the AZ41 magnesium alloy subjected to film coating obtained in the treatment method 2, wherein the performance test specifically comprises the following steps: the microstructure of the surface of the coated magnesium alloy is shown in fig. 6 and 7. Carrying out electrochemical test on the magnesium alloy, wherein the test conditions are as follows: the impedance values of the magnesium alloy embedded in 3.5 wt.% NaCl stirred plain concrete were electrochemically tested, and the results are shown in fig. 8 and 9. The resistance value of the bare alloy in plain concrete is 8.6 multiplied by 104Ω·cm2Rises to 93.2X 104Ω·cm2. The impedance value of the coated magnesium alloy in plain concrete is 27.9 multiplied by 104Ω·cm2Rising to 160.9X 104Ω·cm2The impedance value is improved by 3.2 times in 1 hour and 1.7 times in 4 days; at the same time, after 96 hours, the corrosion current density was from 2.1X 10-7A·cm-2Down to 3.6X 10-8A·cm-2As shown in detail in fig. 10.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (8)
1. Magnesium alloy CaCO3The conversion coating treating agent is characterized by comprising CaCl2Aqueous solution with NaHCO3An aqueous solution of a carboxylic acid and a carboxylic acid,said CaCl2Aqueous solution with NaHCO3The volume ratio of the aqueous solution is 1 (1-4).
2. The magnesium alloy CaCO according to claim 13The conversion coating treating agent is characterized in that: the CaCl is2Aqueous solution with NaHCO3The volume ratio of the aqueous solution was 1: 3.
3. The magnesium alloy CaCO of claim 23A conversion film treating agent characterized by said NaHCO3The mass concentration of the aqueous solution is 0.5-1.5mol/L, and the CaCl is2The mass concentration of the aqueous solution is 0.5-1.5 mol/L.
4. The magnesium alloy CaCO according to claim 33A conversion film treating agent characterized by said NaHCO3The mass concentration of the aqueous solution is 1.0mol/L, and the CaCl is2The mass concentration of the aqueous solution was 1.5 mol/L.
5. Magnesium alloy CaCO according to any one of claims 1 to 43The treatment method of the conversion coating treatment agent is characterized by comprising the following steps:
A) putting the magnesium alloy into a degreasing agent for degreasing and deoiling;
B) putting the magnesium alloy after degreasing and deoiling treatment into the magnesium alloy CaCO3And (3) in the conversion film treating agent, taking out after water bath treatment for 1-6h, then ultrasonically cleaning for 3-10 min by using deionized water and ethanol, and drying by hot air.
6. Magnesium alloy CaCO according to claim 53The treatment method of the conversion film treating agent is characterized in that the temperature of the water bath treatment is 45-85 ℃.
7. The magnesium alloy CaCO according to claim 63The treatment method of the conversion coating treatment agent is characterized in that the temperature of the water bath treatment is 50 ℃.
8. The magnesium alloy CaCO according to claim 63The treatment method of the conversion coating treatment agent is characterized in that the temperature of the water bath treatment is 80 ℃.
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2022
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