CN115058680A - High-corrosion-resistance high-strength high-entropy alloy coating with adjustable components and preparation method thereof - Google Patents
High-corrosion-resistance high-strength high-entropy alloy coating with adjustable components and preparation method thereof Download PDFInfo
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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
- C23C4/134—Plasma spraying
-
- 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
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Abstract
The invention discloses a high-corrosion-resistance high-strength high-entropy alloy coating with adjustable components and a preparation method thereof; the method comprises the steps of selecting 4-5 elements such as Al, Cr, Mn, Ni, Fe, Co, Ti, Cu, V and the like which are commonly used for preparing the high-entropy alloy, designing theoretical components, preparing powder for plasma cladding, and synthesizing a high-entropy alloy coating with richer actual components on the surface of structural steel in situ by using a plasma cladding technology and the dilution effect of a matrix so as to improve the surface hardness and corrosion resistance of the matrix and achieve the purpose of prolonging the service time of the matrix. Me prepared according to the invention Ⅳ‑Ⅴ Fe x C y (Me Ⅳ‑Ⅴ Means that 4-5 elements, 0, are selected from the above-mentioned elements commonly used for the preparation of high-entropy alloys<x<2，0<y<0.02,) wherein x, y are variables whose values depend on the plasma cladding process parameters and the composition of the base material composition by plasma claddingIn the process, the dilution effect of the matrix diffuses Fe and C in the matrix into the coating.
Description
Technical Field
The invention relates to the field of metal plasma surface modification, in particular to a high-corrosion-resistance high-strength high-entropy alloy coating with adjustable components and a preparation method thereof.
Background
Structural steel is an extremely important and widely applied material in the industrial field, but the structural steel is often influenced by the service site environment, such as friction, corrosion, high temperature and other factors, so that the structural steel fails, new steel has to be replaced, and great resource waste is caused. Especially, with the development of society, people carry out deep exploration and development on unconventional areas such as deep sea, plateau, outer space and the like, which requires further improvement of the radiation resistance, oxidation resistance, corrosion resistance, high temperature resistance, good structural stability and other properties of the material so as to meet the application requirements of prolonging the service time of a steel structure and in special fields.
Alloying is still one of the main ways to improve the properties of the steel such as hardness, corrosion resistance and the like. However, the addition of a large amount of alloy elements may cause the formation of complex brittle phases in the alloy, and the mechanical properties of the alloy are reduced. Unlike conventional single element based alloys, high entropy alloys contain multiple principal elements (typically 5-13), each in a certain proportion (often 5-35% mole fraction). Due to the unique component composition, the alloy has high mixed entropy, so that the alloy cannot form a complex intermetallic compound, but the crystal structure of the alloy tends to form a simple solid solution, and the advantages of main elements are all highlighted due to the synergistic effect of multiple elements, so that the high-entropy alloy has higher strength, hardness, wear resistance, corrosion resistance and the like compared with the traditional alloy, and has wide development potential and application prospect in the important engineering fields of mechanical manufacturing, transportation, ocean engineering and the like. The performance of the high-entropy alloy is superior to that of the traditional alloy, so that the processing of the blocky high-entropy alloy is more time-consuming and labor-consuming, the manufacturing cost of parts is increased, and the resource waste is caused. The high-entropy alloy coating has wide application scenes in the fields of wear resistance modification of the surface of a rotary transmission part, corrosion resistance modification of the surface of ocean engineering equipment, repair and remanufacture of damaged parts and the like due to excellent performance.
At present, magnetron sputtering, electrochemical deposition, laser cladding technology and plasma cladding technology are most applied in the preparation method of the high-entropy alloy coating. The coating prepared by magnetron sputtering and electrochemical deposition is too thin and is only in micron level, so that the coating is difficult to work for a long time in a harsh environment; the coating prepared by the laser cladding technology reaches millimeter level, but the technology has high requirements on working environment, complex equipment and high preparation cost, and is difficult to apply on a large scale.
The plasma cladding technology is one of important means of metal surface strengthening and remanufacturing engineering, has extremely high energy density, high solidification speed and cooling speed as well as laser cladding technology, but has the characteristics of low equipment cost, simple operation, low requirement on working environment, high cladding rate, high powder utilization rate, low substrate dilution rate, wide range of fusible materials, good process controllability and the like compared with the laser cladding technology, and is hopeful to realize large-scale use. The dilution of the substrate can make the actual components and the designed components of the coating come in and go out greatly, even the mixed entropy of the coating is reduced, so that the content of certain main elements can be reduced in the components of the target coating by using the dilution of the substrate according to the components of the substrate and the control of process parameters during cladding, thereby achieving the purposes of regulating and controlling the components of the coating, reducing the cost, improving the performance of metal materials and prolonging the working time.
Disclosure of Invention
The purpose of the invention is as follows: the method provided by the invention has the advantages that the chemical components of the high-entropy alloy coating can be controlled by changing the process parameters and the matrix material, so that the high-entropy alloy coating with high hardness and good corrosion resistance can be prepared.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a preparation method of a high-corrosion-resistance high-strength component-controllable high-entropy alloy coating specifically comprises the following steps:
me is formed by selecting 4-5 elements from elements commonly used for preparing high-entropy alloy Ⅳ-Ⅴ Design of high entropy alloy coatingLayer, weighing each element metal powder according to the molar ratio, and ball-milling and mixing uniformly to form powder for cladding;
cleaning the surface of the base material in a mechanical, physical and other modes;
under the protection of argon, Me is synthesized in situ on the surface of a matrix by using a plasma cladding technology through the dilution effect of the matrix material Ⅳ-Ⅴ Fe x C y High entropy coating.
Further, said step (1) is used for composing Me Ⅳ-Ⅴ The metal powder molar ratio of (a) is selected to be different according to different designs including, but not limited to, equal ratios.
Further, in the step (1), the purity of each powder is more than or equal to 99.9%, and the particle size ranges from 70 μm to 100 μm.
Further, in the step (1), a planetary ball mill is adopted for grinding and mixing for about 4 hours, and the rotating speed of the ball mill is about 400r/min, so that powder for cladding is formed;
further, it is characterized in that: in the step (2), the base material is generally structural steel.
Another objective of the present invention is to provide a method for preparing the alloy coating with high corrosion resistance, high strength and high entropy, which can prepare a large area of coating on the surface of the substrate while ensuring the quality of the coating and avoiding the occurrence of cracks, obvious pores, and other defects on the coating, so as to provide specific process parameters for plasma cladding the alloy coating with high corrosion resistance, high strength and high entropy, which can be used for protecting the metal surface, through specific experiments, and the method comprises the following steps:
step 1: polishing the base material to remove an oxide layer and oil stains;
and 2, step: cleaning a powder feeding pipeline of the plasma cladding equipment by using high-pressure gas, and putting the prepared powder for cladding into a powder storage tank of the plasma cladding equipment.
And step 3: and placing the substrate on a workbench of plasma cladding equipment, and preparing the high-entropy alloy coating on the surface of the substrate through plasma cladding.
Further, in the step 1, the substrate is subjected to treatment means such as sand paper polishing for derusting, degreasing and the like; the sandpaper adopts 400# and 1000# sandpaper to polish the surface of the substrate in turn.
Further, in step 3, the preparation process parameters of the coating are as follows: the spraying distance is 40-70 mm, the moving speed of a spray gun is 5-8 mm/s, and the cladding current is 133A; the powder feeding amount is 17 g/min; 4L/min of ion gas; 4L/min of protective gas; the transferred arc voltage is 40V; the swing amplitude is 9 mm; the wobble frequency is 53 c/min; the spraying angle is 90 degrees, and the thickness of the coating is 1-3 mm.
Further, the plasma cladding in-situ synthesis high-entropy alloy coating is Me Ⅳ-Ⅴ Fe x C y The high-entropy alloy coating is characterized in that the molar ratio of each element is determined according to the requirements of service performance, C element and part of Fe element are provided by the dilution effect of a substrate, the prefabricated cladding powder only contains Me by modifying the processing parameters of plasma cladding and selecting different substrates for control Ⅳ-Ⅴ And (4) elements.
Compared with the prior art, the invention has the advantages that: 1. the invention provides a high-corrosion-resistance high-strength high-entropy alloy coating with adjustable and controllable components, wherein elements existing in a base material are added in less or not added in each element powder required by cladding, and element C and part of element Fe in the coating are obtained by the dilution effect of the base; at the same time, the Me synthesized in situ in the invention Ⅳ-Ⅴ Fe x C y The high-entropy alloy coating is characterized in that the contents of Fe and C elements in the high-entropy alloy coating are controlled by controlling the parameters of a cladding process, so that elements existing in a matrix can be added or not added when a cladding raw material of the high-entropy alloy coating is prepared, the cost of the high-entropy alloy coating raw material is reduced, the problem that the components of the conventional cladding actual coating deviate from those of the originally designed coating is expected to be solved, the Fe content of the matrix is introduced to inhibit the formation of dendrites, the single phase structure of the coating is ensured, the introduced C element is added into the coating in the form of interstitial solid solution instead of cementite, the hardness of the coating is further enhanced while the single structure is ensured, and the service performances of the high-entropy alloy coating, such as hardness, wear resistance and corrosion resistance, can meet the use expectation.
2. When the problems that the use performance of the high-entropy alloy coating is influenced due to nonuniform microstructure of the coating, concentrated crack stress and the like caused by excessive nonuniform distribution of element content occur in the method, the moving speed is controlled to control the stirring time of the plasma beam in the molten pool in the process of synthesizing the high-entropy alloy coating in situ by plasma cladding, so that the elements in the molten pool are driven to flow in the high-entropy alloy coating, uniform distribution of the elements is realized, and the negative influence on the in-situ synthesized high-entropy alloy coating, which is caused by extremely nonuniform distribution of the elements, is reduced.
3. The preparation method of the in-situ synthesis high-entropy alloy coating is simple, is easy to operate, is quick to prepare, is low in cost, is easy to realize automation, does not need complex equipment, and has remarkable economic benefits in the field of preparing the high-entropy alloy coating by plasma cladding.
Drawings
FIG. 1 shows AlNiCrMnFe in the examples x C y An X-ray diffraction pattern of the coating;
FIG. 2 shows AlNiCrMnFe in the examples x C y Scanning electron microscope pictures of the coating;
FIG. 3 shows AlNiCrMnFe in the examples x C y Metallographic structure of the longitudinal section of the coating;
FIG. 4 shows AlNiCrMnFe in the examples x C y Hardness curves for the coating and the E32 marine steel substrate;
FIG. 5 shows AlNiCrMnFe in the examples x C y Polarization curves of the coating and the E32 marine steel substrate;
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings.
Example 1: the preparation method of the alloy coating with high corrosion resistance, high strength and high entropy provided in the embodiment specifically comprises the following steps:
(1) five elements of Al, Ni, Cr, Fe and Mn are selected to form Me V And the molar ratio of 1: 1: 1: 1: 1, weighing Al, Ni, Cr, Fe and Mn metal powder with the particle size of 70-100 mu m, and grinding and mixing for 4 hours by using a planetary ball mill at the rotating speed of 400r/min to form powder for cladding;
(2) the E32 steel substrate was polished to remove oxide layers and oil stains.
(3) Cleaning a powder feeding pipeline of the plasma cladding equipment by using high-pressure gas, putting the high-entropy alloy powder obtained in the embodiment 1 into a powder storage tank of the plasma cladding equipment, putting a substrate on a workbench of the plasma cladding equipment, and preparing a high-entropy alloy coating on the surface of the substrate through plasma cladding.
(4) In the plasma cladding process, the powder feeding mode is synchronous powder feeding. The cladding technological parameters are as follows: the spraying distance is 40-70 mm, the moving speed of a spray gun is 5-8 mm/s, and the cladding current is 133A; the powder feeding amount is 17 g/min; 4L/min of ion gas; 4L/min of protective gas; the transferred arc voltage is 40V; the swing amplitude is 9 mm; the wobble frequency is 53 c/min; the spraying angle is 90 degrees.
It should be noted that the high-entropy alloy coating can be rapidly prepared by performing plasma cladding within the experimental parameter range, and the hardness and the bonding force of the coating can be ensured. Of course, in other embodiments of the present invention, parameters of the plasma cladding may also be adjusted according to requirements, and the embodiments of the present invention are not limited.
It should be noted that, in this embodiment, the thickness of the high-entropy alloy coating layer prepared by arc ion plating on the surface of the base material is 1-3 mm. The hardness, the binding force and the substrate dilution rate of the coating within the thickness range can be effectively improved and guaranteed. Of course, in other embodiments of the present invention, the thickness of the coating layer may also be adjusted according to requirements, and the embodiments of the present invention are not limited.
Of course, the base material is structural steel, and bases such as E32 steel, 45 steel, A3 steel and the like can be selected, and the embodiment of the present invention is not limited.
Example 2: in the coating area, a sample with a matrix is taken out by using electric spark cutting, a metallographic phase is prepared, and the XRD, SEM and EDS detection are analyzed. FIG. 1 is an X-ray diffraction pattern of a high entropy alloy coating, showing that the coating is a single phase structure of BCC.
FIG. 2 shows AlNiCrMnFe x C y In the scanning electron microscope image of the longitudinal section of the high-entropy alloy coating, the part with a darker color is the coating, the part with a lighter color is the matrix, and the coating is faster due to the extremely high melting and cooling speed of the plasma claddingThe coating is compact and uniform, is tightly combined with a matrix, has no defects such as obvious holes and the like, and achieves the effect of coating preparation.
FIG. 3 shows AlNiCrMnFe x C y The longitudinal section metallographic structure of the high-entropy alloy coating is characterized in that most of alloy grains are columnar grains and a small amount of dendritic crystals.
The elemental contents of the top, middle, bottom and cladding raw material powder of the coating in example 1 are shown in table 1, and in example 1, the content of Fe in the bottom of the coating is higher than that in the top of the coating and much higher than that in the cladding raw material, which indicates that Fe in the matrix enters the coating, but the result of detecting light elements such as C by EDS is inaccurate, but steel necessarily contains a certain amount of carbon, so that a small amount of C enters the coating due to the change of Fe.
Table 1 example 1 EDS analysis results (atomic fraction,%) of coating A, B, C region
Example 3:
the microhardness of the high-entropy alloy cladding layer was measured using a microhardness tester by taking points at different distances from the surface of the cladding layer, and compared with an E32 steel substrate, wherein the results of example 3 are shown in FIG. 4, and the average hardness of the coating was 411.6HV 0.5 While the hardness of the E32 marine steel substrate was about 180.6HV compared to the E32 marine steel substrate 0.5 Compared with the traditional metal alloy, the coating prepared by the preparation method of the high-entropy alloy coating provided by the embodiment of the invention has higher hardness.
Example 4:
connecting a sample with a thin copper plate through a conductive adhesive, sealing other surfaces except a test surface by using a cold-inlaid mode for electrochemical test, measuring a polarization potential and a polarization current on a Gamry-Interface 1010E electrochemical workstation by using a detection sample as shown in figure 4, adopting a traditional three-electrode system, taking a working electrode as a test sample, an auxiliary electrode as a platinum sheet, a reference electrode as a saturated Ag/AgCl electrode, and measuring a scanning rate as1mV/s, ranging from-1.5V to 1V, with the electrolyte being a 3.5% NaCl solution, was tested at room temperature, and the sample was now soaked in the 3.5% NaCl solution for 1 hour before the test began until the open rate potential stabilized. The self-etching potential of the coating was found to be-671 mv and the self-etching current density 1.2X 10 -2 μA/cm 2 Comparison with E32 maritime work steel base material, the autogenous corrosion potential of the E32 maritime work steel base material is-886 mV, and the autogenous corrosion current density is 3.5 multiplied by 10 -2 μA/cm 2 The results are shown in FIG. 5.
The method comprises the steps of selecting 4-5 elements such as Al, Cr, Mn, Ni, Fe, Co, Ti, Cu, V and the like which are commonly used for preparing the high-entropy alloy, designing theoretical components, preparing powder for plasma cladding, and synthesizing a high-entropy alloy coating with richer actual components on the surface of structural steel in situ by using a plasma cladding technology and the dilution effect of a matrix so as to improve the surface hardness and corrosion resistance of the matrix and achieve the purpose of prolonging the service time of the matrix. Me prepared according to the invention Ⅳ-Ⅴ Fe x C y (Me Ⅳ-Ⅴ Means that 4-5 elements, 0, are selected from the above-mentioned elements commonly used for the preparation of high-entropy alloys<x<2，0<y<0.02,) wherein x, y are variables whose values depend on the plasma cladding process parameters and the composition of the substrate material, which diffuse Fe and C from the substrate into the coating by the dilution of the substrate during plasma cladding. Me prepared by the method provided by the invention Ⅳ-Ⅴ Fe x C y The coating has a phase structure of BCC single phase, does not have a complex intermetallic compound precipitated phase, has higher hardness, shows good corrosion resistance, is uniform and compact, and has good bonding state with an alloy matrix.
The present invention and the embodiments thereof have been described above, and the description is not intended to be limiting, and the embodiments shown in the drawings are only a part of the embodiments of the present invention, not all of the embodiments, and the actual configuration is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation method of a component-adjustable high-corrosion-resistance high-strength high-entropy alloy coating is characterized by comprising the following preparation steps:
(1) me is formed by selecting 4-5 elements from elements commonly used for preparing high-entropy alloy Ⅳ-Ⅴ Designing a high-entropy alloy coating, weighing each element metal powder according to a molar ratio, and performing ball milling and mixing uniformly to form powder for cladding;
(2) cleaning the surface of the base material in a mechanical, physical and other modes;
(3) under the protection of argon, Me is synthesized in situ on the surface of a matrix by using a plasma cladding technology through the dilution effect of the matrix material Ⅳ-Ⅴ Fe x C y High entropy coating.
2. The method for preparing a composition-controlled high-corrosion-resistance high-strength high-entropy alloy coating according to claim 1, wherein Me in the step (1) Ⅳ-Ⅴ The metal powder is selected according to different designs and different molar ratios include, but are not limited to, weighing the powder in equal proportion.
3. The method according to claim 1, wherein the purity of each element powder in step (1) is greater than or equal to 99.9%, and the particle size is in the range of 70 μm to 100 μm.
4. The method for preparing a composition-controllable high-corrosion-resistance high-strength high-entropy alloy coating according to claim 1, wherein the step (1) comprises grinding and mixing for about 4 hours by using a planetary ball mill at a rotation speed of about 400r/min to form the high-entropy alloy powder.
5. The method of claim 1, wherein step (2) is performed in a manner such that the composition of the alloy coating is controlled to provide a corrosion resistance, a strength, and an entropyThe body material is structural steel; in the step (1), five elements of Al, Ni, Cr, Fe and Mn are adopted to form Me V Mole ratio of elements in five is 1: 1: 1: 1: 1.
6. the method for preparing a composition-controllable high-corrosion-resistance high-strength high-entropy alloy coating according to claim 1, wherein in the step (2), the base material is subjected to surface mechanical and physical cleaning methods including shot blasting, sand paper polishing for rust removal, and oil stain removal.
7. The method for preparing the alloy coating with controllable components, high corrosion resistance, high strength and high entropy according to claim 1, wherein the preparation process parameters of the coating are as follows: the spraying distance is 40-70 mm, the moving speed of a spray gun is 5-8 mm/s, and the cladding current is 133A; the powder feeding amount is 17 g/min; 4L/min of ion gas; 4L/min of protective gas; the transferred arc voltage is 40V; the swing amplitude is 9 mm; the wobble frequency is 53 c/min; the spraying angle is 90 degrees, and the thickness of the coating is 1-3 mm.
8. The method for preparing a composition-controllable high-corrosion-resistance high-strength high-entropy alloy coating according to any one of claims 1 to 7, wherein the plasma cladding in-situ synthesis high-entropy alloy coating prepared by the method is applied.
9. The method of claim 7, wherein Me is Me in the process of forming a compositionally controlled, corrosion-resistant, high-strength, high-entropy alloy coating Ⅳ-Ⅴ Fe x C y The high-entropy alloy coating is characterized in that the molar ratio of each element is determined according to the requirements of service performance, C element and part of Fe element are provided by the dilution effect of a substrate, the plasma cladding processing parameters are modified and the substrate material is changed for control, and cladding powder only contains Me Ⅳ-Ⅴ And (4) elements.
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