CN110747427B - Method for improving corrosion resistance of amorphous coating and application - Google Patents

Method for improving corrosion resistance of amorphous coating and application Download PDF

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CN110747427B
CN110747427B CN201911113958.0A CN201911113958A CN110747427B CN 110747427 B CN110747427 B CN 110747427B CN 201911113958 A CN201911113958 A CN 201911113958A CN 110747427 B CN110747427 B CN 110747427B
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amorphous coating
amorphous
coating
polarization treatment
prepared
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CN110747427A (en
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周正
余文锦
贺定勇
谈震
郭星晔
吴旭
王国红
王曾洁
邵蔚
崔丽
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Shandong Jiabeide Metal Technology Co ltd
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Beijing University of Technology
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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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/129—Flame spraying
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/02—Amorphous alloys with iron as the major constituent
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/06—Metallic material
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/18—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
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Abstract

The invention relates to the technical field of amorphous coatings, and particularly discloses a method for improving the corrosion resistance of an amorphous coating and application thereof. The method for improving the corrosion resistance of the amorphous coating forms a passivation film by pre-polarizing the amorphous coating, the amorphous coating is prepared by a thermal spraying mode, and the porosity of the amorphous coating is lower than 0.6%. On the basis of not adopting an external hole sealing material, the method of forced pre-polarization is adopted to forcibly accelerate the further passivation of the passivation film, so that the problems of weak bonding interface, defect positions and weak and uneven passivation films nearby the defect positions of the amorphous coating are solved, the generation and homogenization of the passivation film at the positions are promoted, the weak positions which are easy to preferentially corrode are reduced, and the aim of improving the long-term corrosion resistance of the amorphous coating is fulfilled. And the method is simple, convenient, low in cost and suitable for industrial popularization.

Description

Method for improving corrosion resistance of amorphous coating and application
Technical Field
The invention relates to the technical field of amorphous coatings, in particular to a method for improving the corrosion resistance of an amorphous coating and application thereof.
Background
The exploitation of marine resources is an important way to improve the comprehensive competitiveness of economy. The development of marine economy is promoted by the construction of a large number of marine facilities, cross-sea bridges, ships, port facilities, ocean platforms and the like. In a complex marine environment, corrosion of marine facilities has become an important factor that hinders development of marine resources, reduces reliability and life of equipment, affects construction safety, and the like. In order to protect marine facilities from the elements of the marine environment, a protective layer is typically applied to the surface of the equipment. Currently, protective layers are mainly classified into two types: an organic coating protective layer and a metal protective layer. However, the organic coating has the problems of easy aging, short service life and the like, needs to be maintained and replaced frequently, needs a large amount of time and materials, has high labor intensity and high maintenance cost, and is not suitable for harsh marine environments. The metal protective layer capable of resisting corrosion for a long time is mainly an amorphous material at present, and the amorphous material has a uniform organization structure, does not have the crystal boundary defect like the traditional crystal material, has high strength and hardness and good wear-resisting and corrosion-resisting properties, and becomes a focus of wide attention.
Although amorphous materials have a plurality of excellent properties, the amorphous alloys have limited forming capability, limited size and shape, and intrinsic toughness and brittleness and preparation cost, so that the amorphous alloys are limited in a plurality of application fields, the realization of the amorphous coating prepared by thermal spraying successfully solves the problems, a large number of weak bonding interfaces and inevitable pores are generated among particles due to rapid cooling and shrinkage of the particles in the thermal spraying process, when the defects are positioned on the surface of the coating, a passivation film on the surface and nearby the surface of the coating is very weak and uneven, a corrosion medium usually breaks through the weak position of the passivation film and slowly permeates into the coating, finally reaches the bonding interface of the coating and a substrate, and the further acceleration effect of the potential difference between the coating and the substrate causes rapid corrosion of the substrate to fail. At present, aiming at the problems of weak passive film at the surface defects of the coating and a large number of weak bonding interfaces between particles, hole sealing treatment is usually adopted to reduce the influence of the defects on the corrosion resistance of the coating. The sealing treatment not only needs the addition of external sealing agent, but also can only seal the surface of the coating, and the sealing agent on the surface is easy to age or fall off under the influence of external force to cause the corrosion resistance of the coating to be reduced.
Therefore, it is desirable to provide a new amorphous coating and a method of processing and application thereof to solve the above problems.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a method for treating an amorphous coating, which can solve the problems of weak and uneven passivation film at the surface defect of the amorphous coating and a large number of weak bonding interfaces among particles and improve the long-term corrosion resistance and wear resistance of the amorphous coating.
In order to achieve the purpose of the invention, the technical scheme of the invention is as follows:
a method for improving corrosion resistance of an amorphous coating is characterized in that a passivation film is formed by pre-polarizing the amorphous coating, the amorphous coating is prepared by a thermal spraying mode, and the porosity of the amorphous coating is lower than 0.6%.
The research of the invention finds that after the surface of the amorphous coating with extremely low porosity prepared by the thermal spraying mode is subjected to pre-polarization treatment, the generation and the homogenization of the amorphous coating weak bonding interface, the defect and the passive film nearby the defect are promoted, the weak position easy for preferential corrosion is reduced, and the purpose of improving the corrosion resistance of the amorphous coating is realized.
In the method, the electrolyte solution for the pre-polarization treatment is 0.35-0.45 wt.% of NaCl solution.
The pre-polarization is carried out under the electrolyte solution with the specific concentration, the structure of the amorphous coating is not damaged, the in-situ self-hole sealing effect of the amorphous coating can be realized, a compact and uniform passive film is obtained more quickly, and the ideal protection effect on the coating is achieved.
Preferably, the NaCl solution is prepared by mixing NaCl crystals and deionized water, and the mass concentration of NaCl is more than 99.5% so as to avoid the influence of impurities on the pre-polarization treatment effect.
The method of the invention comprises the following steps: and exposing the surface of the amorphous coating to the electrolyte solution to carry out the pre-polarization treatment until the amorphous coating is passivated, wherein the initial voltage of the pre-polarization treatment is-0.2 to-0.3V relative to the open circuit potential, and the scanning speed is 0.333 to 0.5 mV/s.
In the present invention, it is preferable that the passivation region of the amorphous coating of a specific composition to be treated is obtained by a polarization treatment, and then when the amorphous coating of the same composition is pre-polarized, the coating is polarized until the polarization curve is significantly passivated (i.e., V)SCENear the upper limit of the passivation interval) to stop the pre-polarization treatment.
In the method, the step of pre-treating the amorphous coating is further included before the pre-polarization treatment, and the pre-treatment comprises wet grinding, polishing, ultrasonic cleaning, acetone degreasing, alcohol cleaning and blow-drying. The pretreatment can remove grease and stains on the surface of the amorphous coating, and the effect of the pre-polarization treatment is prevented from being influenced.
In the method, the thermal spraying mode is a supersonic flame spraying mode.
The method is one of the most advantageous methods for preparing the wear-resistant and corrosion-resistant amorphous coating. The amorphous coating prepared by supersonic flame spraying has the advantages of low cost, low porosity, uniform structure, high bonding strength, wear resistance and the like, and is the first choice of metal protective materials. After the method is used for the amorphous coating prepared by the supersonic flame spraying method, a more corrosion-resistant and wear-resistant metal protective layer can be further obtained.
Preferably, in the method of the present invention, theThe amorphous coating is prepared by taking amorphous alloy powder as a raw material, and the amorphous alloy powder comprises Fe48Cr15Mo14C15B6Y2。
The amorphous alloy powder comprises the following components: fe 48 wt.%, Cr 15 wt.%, Mo 14 wt.%, C15 wt.%, B6 wt.%, Y2 wt.%.
The method is particularly suitable for the iron-based amorphous coating, and the iron-based amorphous coating with high corrosion resistance can be obtained.
In the method, the amorphous alloy powder is prepared by an air atomization method, and the particle size of the amorphous alloy powder is 25-45 mu m, so that the physical property and the bonding property of the coating are improved.
In the method, the pre-polarization treatment further comprises the steps of water cleaning, alcohol cleaning and blow drying.
Another object of the present invention is to provide an amorphous coating with high corrosion resistance, which is prepared by the above method.
It is a further object of the present invention to provide the use of the above method or amorphous coating in the manufacture of marine facilities.
The invention has the beneficial effects that:
on the basis of not adopting an external hole sealing material, the method of forced pre-polarization is adopted to forcibly accelerate the further passivation of the passivation film, so that the problems of weak bonding interface, defect positions and weak and uneven passivation films nearby the defect positions of the amorphous coating are solved, the generation and homogenization of the passivation film at the positions are promoted, the weak positions which are easy to preferentially corrode are reduced, and the aim of improving the long-term corrosion resistance of the amorphous coating is fulfilled. And the method is simple, convenient, low in cost and suitable for industrial popularization.
Drawings
FIG. 1 is an SEM topography of amorphous alloy powder of example 1 of the present invention;
FIG. 2 is XRD patterns of an amorphous alloy Powder (Powder) of example 1 of the present invention and an amorphous Coating (Coating) prepared in example 1; wherein, the ordinate is diffraction Intensity (Intensity), and the abscissa is diffraction angle (2 theta);
FIG. 3 is a sectional SEM topography of a composite substrate with an amorphous coating prepared in example 1 of the invention;
FIG. 4 is a graph comparing the polarization curves of the pre-polarized amorphous coatings of example 1 and comparative example 1 of the present invention with those of the non-pre-polarized amorphous coatings; wherein, the abscissa is Current Density (Current Density), and the ordinate is Potential (Potential);
FIG. 5 is a graph comparing Electrochemical Impedance Spectroscopy (EIS) of pre-polarized amorphous coatings of example 1 and comparative example 1.
Detailed Description
Preferred embodiments of the present invention will be described in detail with reference to the following examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and alterations of this invention will become apparent to those skilled in the art without departing from the spirit and scope of this invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
The embodiment provides a processing method of an amorphous coating and tests the corrosion resistance of the amorphous coating, and the specific steps are as follows:
(1) matrix treatment: cleaning a substrate (carbon steel) by using ultrasonic acetone to remove oil stains on the surface, and then performing sand blasting treatment on the substrate by using brown corundum with the granularity of 400 meshes to remove oxide skin on the surface of the substrate and increase the roughness;
(2) preparing a coating: amorphous alloy powder Fe prepared by gas atomization48Cr15Mo14C15B6Y2(25-45 μm) as a spraying material. FIG. 1 is an SEM (scanning electron microscope) morphology of the amorphous alloy powder, and it can be seen from FIG. 1 that most of the powder is spherical and has high sphericity, and only a few of the powder has satellite structures, so that the flowability of the powder in the spraying process is ensured. In the sand blasting treatmentAnd preparing an amorphous coating on the substrate by adopting JP-5000 type supersonic flame spraying equipment of Praxair-TAFA to obtain the substrate (sample) compounded with the amorphous coating. The specific spraying process parameters are as follows: oxygen 2000SCFH, kerosene 6.2GPH, nitrogen 26SCFH, powder feeding rate of 5r/min, spraying distance: 380 mm.
Fig. 2 is XRD patterns of the amorphous alloy powder of this example and the amorphous coating prepared in this example, and the XRD curve in fig. 2 shows that neither the amorphous coating prepared in this example nor the amorphous alloy powder has a distinct crystallization peak, and a distinct broadening phenomenon is observed at a diffraction angle of 35-50 °, which indicates that the amorphous degree of the coating and the powder is very high.
FIG. 3 is a SEM image of the cross-section of the sample prepared in this example, which shows that the amorphous coating is uniform and dense, the porosity is very low (0.58%), and the combination with the matrix is good.
(3) Preparing an electrolyte solution for amorphous coating pre-polarization treatment: 4g of NaCl crystal for experiment is added into 1000g of deionized water, and the mixture is stirred until the crystal is completely dissolved, so that NaCl electrolyte solution (0.4 wt.%) for pre-polarization treatment is prepared.
Preparing an electrolyte solution for polarization treatment of the amorphous coating: 36.27g of NaCl crystal for experiment is added into 1000g of deionized water, and the mixture is stirred until the crystal is completely dissolved, thus preparing the NaCl electrolyte solution for polarization treatment.
(4) Amorphous coating pretreatment: wet grinding the amorphous coating prepared in the step (2) to 1500# with sand paper, polishing, ultrasonic cleaning, acetone degreasing, alcohol cleaning and blow-drying.
(5) Determining the passivation interval of the amorphous coating: taking the sample (25X 10 mm) prepared in step (4)3) Carrying out polarization treatment, wherein the specific treatment process comprises the following steps: immersing the surface of the amorphous coating layer in the NaCl electrolyte solution for polarization treatment prepared in the step (3) to test the open circuit for one hour until the open circuit potential is stable, and scanning the sample from the position of-0.3V relative to the open circuit at the scanning rate of 0.333mV/s to 1.2V after the open circuit potential is stableSCEThe polarization curve of the non-pre-polarized amorphous coating was obtained, see fig. 4. From FIG. 4, it can be obtained that the self-etching potential Ecorr of the amorphous coating without pre-polarization treatment is-301 mV, self-corrosion current Icorr of 2.75 multiplied by 10-3mA/cm2Passivation Current of 4.02X 10-1mA/cm2The passivation interval is 0.4-0.9VSCE。
(6) Pre-polarization treatment of the amorphous coating: performing pre-polarization treatment on the sample prepared in the step (4), wherein the specific treatment process comprises the following steps: immersing the surface of the amorphous coating layer in the NaCl electrolyte solution for pre-polarization treatment prepared in the step (3) to test the open circuit for one hour until the open circuit potential is stable, and scanning the sample from the position of-0.3V relative to the open circuit at the scanning rate of 0.4mV/s to 0.7V after the open circuit potential is stableSCEStopping immediately, taking out the sample, and then cleaning with distilled water, cleaning with alcohol and drying.
And (5) carrying out polarization treatment on the sample subjected to the pre-polarization treatment in the step (6), and obtaining a polarization curve of the pre-polarized amorphous coating in the same specific step as the step (5), and referring to fig. 4.
As can be seen from the comparison of the polarization curves in FIG. 4, after the pre-polarization treatment with 0.4 wt.% NaCl solution, the self-corrosion potential of the amorphous coating shifted up 103mV compared to that before the pre-polarization (without pre-polarization treatment), and the self-corrosion current shifted left compared to that before the pre-polarization by 1.41X 10-3mA/cm2With passivation current shifted to the left by 6.5X 10-2mA/cm2. Therefore, the corrosion resistance of the amorphous coating after the pre-polarization treatment is improved.
The Electrochemical Impedance Spectroscopy (EIS) test is performed on the amorphous coating which is subjected to the pre-polarization treatment and the non-pre-polarization treatment in the embodiment, and the specific test process is as follows: before impedance test, the surface of the amorphous coating to be tested is exposed to 3.5 wt.% NaCl electrolyte solution for testing open circuit for one hour until the open circuit potential is stable, and impedance is tested under the open circuit potential, wherein the frequency range is 10kHz to 0.01Hz, the amplitude is 10mV, and the soaking time is 7 days. The test results are shown in FIG. 5.
Fig. 5 is an impedance comparison graph of the amorphous coating before and after the pre-polarization, the larger the capacitive arc resistance radius represents the better the corrosion resistance, and it can be seen from fig. 5 that the capacitive arc resistance radius of the amorphous coating subjected to the pre-polarization treatment by 0.4 wt.% NaCl solution is obviously larger than that of the amorphous coating not subjected to the pre-polarization treatment after the soaking in the same time, which shows that the long-term corrosion resistance of the amorphous coating is further improved after the pre-polarization treatment.
Comparative example 1
This comparative example provides a treatment method of amorphous coating and tests the corrosion resistance, and the specific steps are the same as example 1, except that: the electrolyte solution prepared in the step (3) and subjected to the pre-polarization treatment of the amorphous coating is a 1 wt.% NaCl electrolyte solution.
The sample after the pre-polarization treatment of the comparative example was subjected to the polarization treatment in the same manner as in example 1, and a polarization curve of the pre-polarized amorphous coating was obtained, as shown in fig. 4. As can be seen from the polarization curve in FIG. 4, the self-corrosion potential of the amorphous coating after pre-polarization treatment with 1 wt.% NaCl solution shifted up by 50mV compared to the pre-polarization direction, the self-corrosion current did not change significantly compared to the pre-polarization direction, and the passivation current shifted left by 2X 10-2mA/cm2Although the passivation current becomes smaller, the self-corrosion current does not change significantly.
The sample after the pre-polarization treatment of the comparative example was subjected to Electrochemical Impedance Spectroscopy (EIS) test in the same manner as in example 1, and the test results are shown in fig. 5. As can be seen from fig. 5, the impedance of the amorphous coating after the pre-polarization treatment with 1 wt.% NaCl solution does not increase much than before the pre-polarization, which is far less than the increase after the pre-polarization treatment with 0.4 wt.% NaCl solution.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (8)

1. A method for improving the corrosion resistance of an amorphous coating is characterized in that a passivation film is formed by pre-polarizing the amorphous coating, the amorphous coating is prepared by a thermal spraying mode, and the porosity of the amorphous coating is lower than 0.6%;
the method comprises the following steps:
firstly obtaining the passivation region of the amorphous coating to be treated by polarization treatment, and then waiting V when the amorphous coating with the same composition is subjected to pre-polarization treatmentSCEStopping the pre-polarization treatment when the upper limit value of the passivation interval is close to the vicinity;
the pre-polarization treatment is carried out by exposing the surface of the amorphous coating to an electrolyte solution, the initial voltage of the pre-polarization treatment is-0.2 to-0.3V relative to the open circuit potential, and the scanning speed is 0.333 to 0.5 mV/s;
the electrolyte solution for the pre-polarization treatment is 0.35-0.45 wt.% of NaCl solution.
2. The method of claim 1, further comprising a step of pre-treating the amorphous coating prior to the pre-poling treatment, the pre-treating comprising wet milling, polishing, ultrasonic cleaning, acetone degreasing, alcohol cleaning and blow drying.
3. The method of claim 1, wherein the thermal spray is a supersonic flame spray.
4. The method according to any one of claims 1 to 3, wherein the amorphous coating is prepared from amorphous alloy powder as a raw material, and the amorphous alloy powder comprises Fe48Cr15Mo14C15B6Y2。
5. The method according to claim 4, wherein the amorphous alloy powder is prepared by a gas atomization method, and the particle size of the amorphous alloy powder is 25-45 μm.
6. The method according to any one of claims 1 to 3, wherein the pre-polarization treatment further comprises the steps of water washing, alcohol washing and blow drying.
7. An amorphous coating, prepared according to the method of any one of claims 1 to 6.
8. Use of the method according to any one of claims 1-6 or the amorphous coating according to claim 7 in the manufacture of a marine facility.
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