CN111763904B - High-entropy alloy powder, high-resistance coating, and preparation method and application thereof - Google Patents
High-entropy alloy powder, high-resistance coating, and preparation method and application thereof Download PDFInfo
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- CN111763904B CN111763904B CN202010553534.2A CN202010553534A CN111763904B CN 111763904 B CN111763904 B CN 111763904B CN 202010553534 A CN202010553534 A CN 202010553534A CN 111763904 B CN111763904 B CN 111763904B
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/52—Ferrous alloys, e.g. steel alloys containing chromium with nickel with cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
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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
- C23C4/04—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
- C23C4/08—Metallic material containing only metal elements
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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
Abstract
The invention relates to high-entropy alloy powder, a high-resistance coating, and a preparation method and application thereof, wherein the high-entropy alloy powder comprises the following components in percentage by mass: 17-25% of nickel, 14-25% of cobalt, 15-20% of chromium, 13-20% of manganese and the balance of iron, wherein the high-entropy alloy powder is used for preparing a high-resistance heating coating. The high-resistance coating material provided by the invention enables the coating to obtain a single-phase structure, improves the coating resistance, realizes the improvement of the heating efficiency, ensures the service reliability, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of electric heating materials, in particular to high-entropy alloy powder, a high-resistance coating, and a preparation method and application thereof.
Background
The traditional alloy usually takes a single element as a main element, but the high-entropy alloy proposed in recent years breaks through the traditional design concept, adopts multiple elements as main elements, and the novel alloy design endows the high-entropy alloy with a series of characteristics different from the traditional alloy, including a high-entropy effect, a delayed diffusion effect, a lattice distortion effect, a cocktail effect and the like. Therefore, the high-entropy alloy has excellent properties such as good strength, hardness, wear resistance, corrosion resistance and thermal stability. At present, the preparation and research of the high-entropy alloy mainly focuses on the block structural material, relatively few researches related to the coating are carried out, the wear-resistant and corrosion-resistant performances of the coating are mainly researched, and the adopted preparation methods are mainly processes such as laser/plasma cladding and the like. As is well known, metals and alloy materials are considered good conductors, so researchers have had relatively limited interest in the electrothermal performance of high entropy alloys, particularly for thermal spray coatings. At present, the conventional electrothermal alloy material is mainly resistance wire materials of nickel-chromium or iron-chromium-aluminum alloy, but the resistance of the resistance wire materials is relatively low, so that the heating efficiency is low, the reliability is insufficient, and the like. There is a need to develop a new high resistance alloy heating coating and a method for preparing the same.
Disclosure of Invention
In order to solve the technical problems, the embodiment of the invention provides high-entropy alloy powder, a high-resistance coating and a preparation method thereof. The high-resistance (heating) coating material provided by the embodiment of the invention enables the coating to obtain a single-phase structure, improves the coating resistance, realizes the improvement of the heating efficiency, ensures the service reliability, and has wide application prospect.
One aspect of the invention provides high-entropy alloy powder, which comprises the following components in percentage by mass: 17-25% of nickel, 14-25% of cobalt, 15-20% of chromium, 13-20% of manganese and the balance of iron, wherein the high-entropy alloy powder is used for preparing a high-resistance heating coating.
According to some preferred embodiments of the present invention, the manganese is present in an amount of 14 to 18% by mass.
In the invention, the inevitable impurities in the high-entropy alloy powder comprise N, P and S, and the total content of the impurities is controlled to be less than 0.5% so as not to influence the alloy components and performance remarkably.
The invention also provides a high-resistance coating, which is prepared by hot spraying high-entropy alloy powder, wherein the high-entropy alloy powder comprises the following components in percentage by mass: 17 to 25 percent of nickel, 14 to 25 percent of cobalt, 15 to 20 percent of chromium, 13 to 20 percent of manganese and the balance of iron.
According to some preferred embodiments of the present invention, the manganese is present in an amount of 14 to 18% by mass.
According to some preferred embodiments of the present invention, the high-entropy alloy powder has a particle size in the range of 25 to 55 μm.
According to some preferred embodiments of the present invention, the following ingredients are contained in mass percent: 17 to 21 percent of nickel, 12 to 21 percent of cobalt, 16 to 19 percent of chromium, 14 to 19 percent of manganese and the balance of iron. The invention adopts high-entropy alloy powder components with specific chemical components and mass ratio, is favorable for ensuring the structural characteristics of the coating, further reduces the porosity and oxygen content of the coating material, and simultaneously improves the bonding strength, resistivity and other properties of the coating.
In another aspect, the present invention provides a method for preparing the high resistance coating, including the steps of thermal spraying: and preparing the high-resistance coating from the high-entropy alloy powder by adopting an atmospheric plasma spraying method.
According to some preferred embodiments of the invention, the spray process parameters are: current: 450-600A, argon flow: 30-40L/min, hydrogen flow: 10-18L/min, powder feeding rate: 55-80g/min, spraying distance: 120-135mm.
According to some preferred embodiments of the present invention, the high-entropy alloy powder is prepared by a nitrogen atomization method; the raw materials for preparing the high-entropy alloy powder are selected from pure metal blocks of nickel, cobalt, chromium, manganese and iron or alloy materials, wherein the purity of the pure metal blocks is more than 99.0wt.%, and the alloy materials are selected from one or more of nickel-chromium, nickel-cobalt-chromium and iron-manganese.
According to some preferred embodiments of the present invention, a method of preparing an alloy coating having high electrical resistance comprises the steps of:
(1) Preparing alloy powder: preparing high-entropy alloy powder with good sphericity and a particle size range of 25-55 mu m by adopting a nitrogen atomization method;
(2) Thermal spraying: the alloy powder in the step (1) is used for preparing the high-entropy alloy coating by adopting an Atmospheric Plasma Spraying (APS) process, and in the coating preparation method, the Atmospheric Plasma Spraying (APS) has the distinct process characteristics, including wide spraying material range, the materials from a low melting point to a high melting point can be sprayed, the requirement on the granularity of the spraying powder is not high, the porosity of the coating is low, oxide inclusions are few, and the like, so that the method is one of effective methods for preparing the high-entropy alloy coating. The spraying process parameters are preferably as follows: current: 450-600A, argon flow: 30-40L/min, hydrogen flow: 10-18L/min, powder feeding rate: 55-80g/min, spraying distance: 120-135mm. The raw materials required for preparing the alloy powder comprise nickel, cobalt, chromium, manganese and iron pure metal block materials, the purity of chemical components is more than 99.0wt.%, or alloy materials such as nickel-chromium, nickel-cobalt-chromium, iron-manganese and the like. The spraying matrix is a metal base material.
The invention also provides application of the high-entropy alloy powder or the high-resistance coating prepared by the method in a heating coating.
In the present invention, the phase structure of the high-resistance alloy coating layer is a single-phase solid solution, but has high resistance. The improvement of the resistance performance of the coating is benefited by the reasonable matching of the design and the preparation method of the components. The coating material is a high-entropy alloy and comprises a multi-principal-element alloy of nickel, iron, cobalt and chromium, wherein the design of several transition group metals is that the atomic radii of the transition group metals are closer to each other so as to realize better mutual solubility, so that a single-phase solid solution structure is obtained, and the material can have better process adaptability, namely has better plastic deformation capability so that the coating keeps better compactness; meanwhile, the integral resistivity can also be improved by introducing larger lattice distortion into the alloy; the combined action of nickel, cobalt and chromium elements is also beneficial to improving the integral high-temperature oxidation resistance of the coating; the necessary addition of manganese element can increase the lattice distortion of alloy system, reduce the layer fault energy and simultaneously reduce the ferromagnetic performance of coating. The overall improvement of the coating resistance is mainly obtained by the combined action of reasonable configuration of the components of the alloy and the preparation method, is not determined by any single element, but is absent and can certainly not be obtained by only limited tests.
The invention has the beneficial effects that: 1) The alloy coating maintains a single-phase FCC stable phase structure; 2) The grain size of the coating reaches the nanometer level; 3) The resistivity of the coating is remarkably improved and can exceed 300 mu omega cm and is higher than that of the traditional nickel-chromium alloy resistance wire material (about 100-115 mu omega cm); 4) The preparation method is simple, and processing such as casting, forging, drawing and the like in the resistance wire preparation process is not needed; 5) The coating heating efficiency and reliability are higher.
Drawings
FIG. 1 is an X-ray diffraction (XRD) spectrum of the alloy powder of example 2.
FIG. 2 is an SEM morphology of the alloy powder of example 2.
FIG. 3 is a plot of the X-ray diffraction (XRD) pattern corresponding to the coating prepared in example 2.
FIG. 4 is a SEM topography corresponding to the coating prepared in example 2.
FIG. 5 is a TEM topography corresponding to the coating prepared in example 2.
Fig. 6 is an X-ray diffraction (XRD) pattern corresponding to the coating prepared in comparative example 2.
In the above figures, FCC and Oxide represent face-centered cubic single-phase solid solutions and metal Oxide phases, respectively.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications.
In the present invention, the equipment and the like used are conventional products which are available from normal vendors, and which are not indicated by manufacturers. The process is conventional unless otherwise specified, and the starting materials are commercially available from a public source. In the following examples: selecting raw materials: the purities of the nickel, iron, cobalt, chromium and manganese blocks are respectively 99.5wt, percent, the total content of N, P, S and other impurities is controlled to be less than 0.5 wt.%. The alloy powder is prepared by adopting a nitrogen atomization method, and the powder with the particle size range of 25-55 mu m and better sphericity (shown in figure 2) is used for atmospheric plasma spraying. The matrix is low-carbon steel, the surface of the matrix is pretreated to remove an oxide film and dirt on the surface, and then sand blasting is carried out; in the performance test process, the high-entropy alloy coating is prepared by adopting an atmospheric plasma spraying process, and the thickness of the coating is 400-500 mu m (for microstructure characterization and bonding strength test) or 1mm (for resistivity test). And performing structural characterization, resistivity and bonding strength performance tests on the prepared alloy powder material and the coating under the same conditions: the phase structure was obtained by X-ray diffractometer (D8 Advance) from Bruker, and the surface area of the test specimen was 10X 10mm 2 (ii) a The microstructure was observed using a Zeiss's field emission SEM electron microscope (GemininSEM 300); the resistivity test is a four-point probe method, the instrument adopts a Nippon vacuum technology company (ULVAC) ZEM-2 type conductivity meter, and the sample size is 18 multiplied by 3 multiplied by 0.9mm 3 (ii) a Coating bond strength test, according to test standards: ASTMC633-01, wherein the sample and the loading rod are 4032 aluminum alloy, the bonding material is high-temperature structural adhesive E-7, the tensile strength of the bonding material is 70MPa, the bonding material is kept for 3 hours under the curing condition of 110 ℃, and the bonding material is tested under the room temperature condition, and experimental equipment is vinpocetine QBD-100.
Example 1
In the embodiment, the alloy material comprises the following chemical components in percentage by mass: nickel: 17%, cobalt: 14%, chromium: 20%, manganese: 14%, iron: the balance, and inevitable impurities. The spraying process parameters are as follows: current: 550A, argon flow: 30L/min, hydrogen flow rate: 10L/min, powder feeding rate: 58g/min, spraying distance: 130mm.
Example 2
In the embodiment, the alloy material comprises the following chemical components in percentage by mass: nickel: 18%, cobalt: 18%, chromium: 20%, manganese: 17%, iron: the balance, and unavoidable impurities. The spraying process parameters are as follows: current: 600A, argon flow: 38L/min, hydrogen flow rate: 12L/min, powder feeding rate: 60g/min, spraying distance: 120mm. Fig. 1 is an X-ray diffraction (XRD) spectrum of the alloy powder, and fig. 2 is an SEM morphology of the alloy powder. FIG. 3 is a plot of the X-ray diffraction (XRD) pattern corresponding to the coating prepared in example 2. FIG. 4 is a SEM topography corresponding to the coating prepared in example 2. FIG. 5 is a TEM topography corresponding to the coating prepared in example 2.
Example 3
In the embodiment, the alloy material comprises the following chemical components in percentage by mass: nickel: 18%, cobalt: 18%, chromium: 18%, manganese: 17%, iron: the balance, and unavoidable impurities. The spraying process parameters are as follows: current: 550A, argon flow: 30L/min, hydrogen flow rate: 10L/min, powder feeding rate: 60g/min, spraying distance: 120mm.
Example 4
In the embodiment, the alloy material comprises the following chemical components in percentage by mass: nickel: 20%, cobalt: 20%, chromium: 16%, manganese: 17%, iron: the balance, and unavoidable impurities. The spraying process parameters are as follows: current: 550A, argon flow: 35L/min, hydrogen flow rate: 12L/min, powder feeding rate: 60g/min, spraying distance: 130mm.
Example 5
In the embodiment, the alloy material comprises the following chemical components in percentage by mass: nickel: 22%, cobalt: 15%, chromium: 20%, manganese: 16%, iron: the balance, and unavoidable impurities. The spraying process parameters are as follows: current: 600A, argon flow: 38L/min, hydrogen flow rate: 12L/min, powder feeding rate: 65g/min, spraying distance: 120mm.
Example 6
In the embodiment, the alloy material comprises the following chemical components in percentage by mass: nickel: 18%, cobalt: 18%, chromium: 19%, manganese: 17%, iron: the balance, and unavoidable impurities. The spraying process parameters are as follows: current: 580A, argon flow: 32L/min, hydrogen flow rate: 18L/min, powder feeding rate: 55g/min, spraying distance: 125mm.
Example 7
In the embodiment, the alloy material comprises the following chemical components in percentage by mass: nickel: 20%, cobalt: 18%, chromium: 20%, manganese: 15%, iron: the balance, and inevitable impurities. The spraying process parameters are as follows: current: 600A, argon flow: 32L/min, hydrogen flow rate: 10L/min, powder feeding rate: 70g/min, spraying distance: 125mm.
Comparative example 1
The alloy material in the comparative example comprises the following chemical components in percentage by mass: nickel: 20%, cobalt: 13%, chromium: 12%, manganese: 12%, iron: the balance, and inevitable impurities. The spraying process parameters are as follows: current: 600A, argon flow: 38L/min, hydrogen flow rate: 12L/min, powder feeding rate: 60g/min, spraying distance: 120mm.
Comparative example 2
The alloy material in the comparative example comprises the following chemical components in percentage by mass: nickel: 18%, cobalt: 18%, chromium: 20%, manganese: 17%, iron: the balance, and inevitable impurities. The spraying process parameters are as follows: current: 650A, argon flow: 25L/min, hydrogen flow rate: 10L/min, powder feeding rate: 50g/min, spraying distance: 100mm. Fig. 6 is an X-ray diffraction (XRD) pattern corresponding to the coating prepared in comparative example 2.
Comparative example 3
The alloy material in the comparative example comprises the following chemical components in percentage by mass: nickel: 80%, chromium: 20%, and inevitable impurities. The spraying process parameters are as follows: current: 600A, argon flow: 38L/min, hydrogen flow rate: 12L/min, powder feeding rate: 60g/min, spraying distance: 120mm.
The results of the coating phase structure, porosity, oxygen content, bond strength, and resistivity tests of examples 1-7 and comparative examples 1-3 are shown in table 1.
TABLE 1 test results of examples 1-7 and comparative examples 1-3
The high-resistance coating material provided by the embodiment of the invention enables the coating to obtain a single-phase structure by regulating and controlling each element, the content and the preparation process parameters of the element, improves the resistance of the coating, realizes the improvement of the heating efficiency, ensures the service reliability, has excellent porosity, oxygen content, bonding strength, resistivity and other aspects, and has wide application prospect.
Although the invention has been described in detail with respect to the general description and the specific embodiments thereof, it will be apparent to those skilled in the art that modifications and improvements can be made based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (2)
1. A preparation method of a high-resistance coating used in the field of electric heating is characterized in that the raw materials are selected from the following materials: the purities of the nickel, iron, cobalt, chromium and manganese blocks are respectively 99.5wt.%, and the total content of impurities containing N, P and S is controlled to be below 0.5 wt.%; preparing high-entropy alloy powder by adopting a nitrogen atomization method, wherein the high-entropy alloy powder with the particle size range of 25-55 mu m and good sphericity is used for atmospheric plasma spraying; the matrix is low-carbon steel, the surface of the matrix is pretreated to remove an oxide film and dirt on the surface, and then sand blasting is carried out; the high-entropy alloy powder comprises the following chemical components in percentage by mass: nickel: 18%, cobalt: 18%, chromium: 20%, manganese: 17%, iron: the balance, and unavoidable impurities; the spraying process parameters are as follows: current: 600A, argon flow: 38L/min, hydrogen flow rate: 12L/min, powder feeding rate: 60g/min, spraying distance: 120mm; the resistivity of the prepared high resistance coating was 334.5 μ Ω · cm.
2. Use of a high electrical resistance coating prepared by the method of claim 1 in the field of electrical heating.
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