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LU504318B1 - A refractory high-entropy alloy coating and its preparation method - Google Patents

A refractory high-entropy alloy coating and its preparation method Download PDF

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Publication number
LU504318B1
LU504318B1 LU504318A LU504318A LU504318B1 LU 504318 B1 LU504318 B1 LU 504318B1 LU 504318 A LU504318 A LU 504318A LU 504318 A LU504318 A LU 504318A LU 504318 B1 LU504318 B1 LU 504318B1
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LU
Luxembourg
Prior art keywords
entropy alloy
alloy coating
refractory high
coating
matrix
Prior art date
Application number
LU504318A
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French (fr)
Inventor
Xuanhong Hao
Yuchong Liu
Yao Fan
Xiaowei Zhang
Hongxi Liu
Yueyi Wang
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Univ Kunming Science & Technology
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Priority to LU504318A priority Critical patent/LU504318B1/en
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Publication of LU504318B1 publication Critical patent/LU504318B1/en

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C30/00Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C24/00Coating starting from inorganic powder
    • C23C24/02Coating starting from inorganic powder by application of pressure only
    • C23C24/04Impact or kinetic deposition of particles
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

The present invention discloses a refractory high entropy alloy coating, characterized in that it is prepared from the following raw materials: Ti: 4% to 20%, Zr: 20%, Mo: 20%, Nb: 20%, Cr: 20%; the invention provides a high entropy alloy coating composed of five high melting point metal elements, Ti, Zr, Mo, Nb and Cr, high hardness, high strength, high toughness, high plasticity at low temperatures The coating has excellent wear, oxidation and corrosion resistance for better application under different working conditions; it can improve the high temperature service performance of titanium alloy, enhance its surface strength, as well as its high temperature resistance and oxidation resistance.

Description

DESCRIPTION LU504318
A REFRACTORY HIGH-ENTROPY ALLOY COATING AND ITS PREPARATION
METHOD
TECHNICAL FIELD
[01] The present invention relates to the field of laser surface modification and specifically to a refractory high-entropy alloy coating and a method for its preparation.
BACKGROUND ART
[02] To improve the high temperature service performance of titanium alloys, more and more researchers have been working on the surface modification of coatings in recent years, mainly including: ion injection, spraying, vapour deposition, plating and laser cladding. The laser coating method has the advantages of high heating and cooling rates, small heat affected zone of the matrix, high metallurgical bonding strength between the coating and the matrix, adjustable coating thickness and a wide choice of materials for the coating layer. Multi-principal high-entropy alloys are new alloys made from at least five elements in an iso-atomic or near-iso-atomic ratio, resulting in a simple and stable FCC or BCC solid solution structure, or even an amorphous phase structure.
[03] At present, there are various forms of surface coatings and coating materials used to improve the high-temperature service performance of titanium alloys, but there are low strength, high-temperature wear resistance and poor oxidation resistance in general.
[04] For this reason, there is a need for a high strength, high temperature resistant, high oxidation resistance alloy coating that can overcome the shortcomings of the above mentioned alloy coatings and improve the high temperature service performance of titanium alloys.
SUMMARY
[05] To solve the above technical problems the present invention provides a refractory high entropy alloy coating to solve the above problems of low strength, high temperature wear resistance and poor oxidation resistance when conventional alloy coatings are used for surface modification of titanium alloys. LU504318
[06] To achieve the technical effect of solving the above technical problem, the invention is realized by the following technical solution: a refractory high-entropy alloy coating, characterized in that it is prepared from the following raw materials: Ti: 4% to 20%, Zr: 20%,
Mo: 20%, Nb: 20%, Cr: 20%:
[07] Further, the specific content of element Ti is 4 %, 8 %, 12 %, 18 %, 20 %, respectively;
[08] A further object of the present invention is to provide a method for the preparation of a refractory high-entropy alloy coating, characterized in that it comprises:
[09] S1. The surface of the TC4 (Ti-6Al-4V) matrix is de-rusted and de-oiled so that the surface of the matrix is clean and flat with a certain degree of roughness;
[10] S2. Mix the powders and then vacuum ball mill them to a particle size of 180~ 300 mesh;
[11] S3. And mix the resulting alloy powder with 5~10% anhydrous ethanol and evenly coat the surface of the matrix to form a prefabricated layer;
[12] S4. 10 hours in the drying oven and then laser cladding to obtain the cladding layer;
[13] Further, the vacuum ball milling time is not less than 3 hours;
[14] Further, the thickness of the prefabricated coating is 1.0 mm;
[15] Further, the process parameters during laser cladding are: laser power of 3700 W, scanning speed of 350 mm/ min, spot diameter of 3.0 mm, off-focus volume of 20 mm, protective gas of argon and gas flow rate of 8 L/min;
[16] Beneficial effects of the present invention:
[17] 1. The present invention provides a high entropy alloy coating consisting of five high melting point metal elements, Ti, Zr, Mo, Nb and Cr High hardness, high strength, high toughness, high plasticity at low temperatures, and excellent resistance to wear, oxidation and corrosion, etc., for better application under different working conditions; it can comprehensively improve the high temperature service performance of the improved titanium alloy and enhance its surface strength, as well as its high temperature resistance and oxidation resistance.
[18] 2. The coating prepared by laser cladding forms a metallurgical bond with the matrix, with good coating morphology, no obvious holes and cracks, and equiaxial crystal organization; it can cover the outer surface of the body uniformly and densely, which is beneficial to improve the comprehensive performance of the alloy coating for surface modification; LU504318
[19] 3. Combining the advantages of laser melting method and high entropy alloy, the prepared coating has high bonding strength with the matrix and excellent performance, which is not only low cost of use, but also can fully improve the shortcomings possessed by low-cost metal materials.
BRIEF DESCRIPTION OF THE DRAWINGS
[20] To illustrate more clearly the technical solutions of the embodiments of the invention, a brief description of the accompanying drawings required for the description of the embodiments is given below, and it will be apparent that the accompanying drawings in the following description are only some embodiments of the invention, and that other accompanying drawings may be obtained without creative effort on the part of those of ordinary skill in the art.
[21] FIG. 1 shows a schematic diagram of laser cladding of a refractory high entropy alloy coating;
[22] FIG. 2 shows a microstructure of the coating and matrix bonding zone in Example 1 of a refractory high entropy alloy coating;
[23] FIG. 3 shows a microstructure diagram of the coating zone in Example 1 of a refractory high entropy alloy coating;
[24] FIG. 4 shows a graph of the average hardness of the coating and the matrix in Example 1 of a refractory high entropy alloy coating;
[25] FIG. 5 shows a graph of the wear weight loss and friction coefficient of the coating in
Example 1 of a refractory high entropy alloy coating;
[26] FIG. 6 shows a coating oxidation kinetic curve in Example 1 of a refractory high entropy alloy coating.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[27] The technical solutions in the embodiments of the invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the invention, it being clear that the embodiments described are only part of the embodiments of the invention and not all of them. Based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without creative labour fall within the scope of protection of the present invention. LU504318
[28] Example 1
[29] A refractory high entropy alloy coating having a composition comprising five high melting point metal powders of Ti, Zr, Mo, Nb and Cr, wherein the molar ratios of the components are Ti: 4% to 20%, Zr: 20%:, Mo: 20%, Nb: 20%, Cr: 20%.
[30] Where, specific Ti content of 4, 8, 12, 18 and 20 per cent were selected for group preparation experiments;
[31] A method for preparing a refractory high-entropy alloy coating comprising the steps:
[32] (1) Mix the individual powders in proportion and then vacuum ball mill the powders for 3 hours so that the powders are fully mixed uniformly;
[33] (2) Mixture of the alloy powder obtained in step (1) with anhydrous ethanol to obtain the coating material, which comprises 92% by mass of the alloy powder with 8% anhydrous ethanol,
[34] (3) The TC4 matrix is coarsely ground with 200~400 grit sandpaper to remove surface oxidation, and then cleaned by ultrasonic alcohol to remove surface stains. The mixed powder is prefabricated on the matrix with a prefabricated layer thickness of 1.0 mm and placed in a drying phase for 10 hours;
[35] (4) The dried powder is laser coated with the matrix, wherein the laser coating process parameters are: excitation power of 3700 W, scanning speed of 350 mm/min, optical shift diameter of 3 mm, off-focus volume of 20 mm, protective gas of argon, gas flow rate of 8 L/min.
[36] Example 2
[37] Based on the above described in embodiment 1, the obtained specimens were wire cut to make a sample of the molten cladding layer and the sample was etched with aqua regia for 1 min for the next step of microscopic characterization and performance testing.
[38] (1) The coating obtained in Example 1 was photographed and observed by SEM, and it was found that the coating was dense and uniform, with no obvious defects and roughly equiaxed crystal organization;
[39] The HVS-1000A microhardness tester was used to measure the microhardness of the coatings of the five components, as shown in Figure 4, with the increase in Ti content, the hardness showed an increasing trend, with the highest microhardness at 20% Ti content, with an average hardness of 1066.7 HV.
[40] (2) The coatings obtained in Example 1 were subjected to a high temperature frictid:504318 wear test at 600°C, with a friction matrix of 5 mm Si3N4, a load of 5 N, a test frequency of 0 .1
Hz and a test time of 20 min, after which the wear weight loss of each coating was obtained, as shown in Figure 5. 0.65mg, which is approximately 1/2 of the matrix;
[41] (3) The high temperature oxidation resistance of the high entropy alloy coating obtained in Example 1 was measured using a tubular resistance furnace at 800°C for 100 h. The oxidation kinetic curve was obtained as shown in Figure 6, which shows that the coating has the best oxidation resistance (12.36 mg/(cm3)-1) when the Ti content is 20%, and the oxidation weight gain is less than that of the matrix (38.44 mg/(cm3)-1). The oxidation weight gain was less than 1/3 of that of the matrix ( 38.44 mg/(cm3)-1).
[42] Itis concluded that a refractory high-entropy alloy coating with a molar ratio of Ti: 20%,
Zr: 20%, Mo: 20%, Nb: 20% and Cr: 20% has the best overall performance of the alloy coating in all aspects.
[43] In summary, 1. the invention provides a high entropy alloy coating composed of Ti, Zr,
Mo, Nb and Cr, high hardness, high strength, high toughness, high plasticity at low temperatures, and excellent resistance to wear, oxidation and corrosion, etc., for better application under different working conditions; it can comprehensively improve the high temperature service performance of titanium alloy, enhance its surface strength, as well as its high temperature resistance and oxidation resistance.
[44] 2. The coating prepared by laser cladding forms a metallurgical bond with the matrix, with good coating morphology, no obvious holes and cracks, and equiaxed crystal organization; it can cover the outer surface of the body uniformly and densely, which is beneficial to enhance the comprehensive performance of the alloy coating for surface modification.
[45] 3. Combining the advantages of laser cladding with those of high entropy alloys, the coating is prepared with high bonding strength to the matrix and excellent performance, which not only has a lower cost of use, but also can fully improve the shortcomings of low-cost metal materials.
[46] In the description of this specification, reference to the description of the term "an embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the invention. The term "embodimentU504318 "example", "specific example", etc. is used to describe specific features, structures, materials or characteristics described in connection with the embodiment or example. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials or characteristics described may be combined in a suitable manner in any one or more embodiments or examples.
[47] The above disclosure of preferred embodiments of the invention is intended only to assist in the description of the invention. The preferred embodiments are not an exhaustive recitation of all details, nor do they limit the invention to the specific embodiments described.
Obviously, many modifications and variations can be made in accordance with the contents of this specification. These embodiments have been selected and described specifically in this specification in order to better explain the principles and practical applications of the invention and thus to enable those skilled in the art to understand and make good use of the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (6)

CLAIMS LU504318
1. À refractory high entropy alloy coating, characterized in that it is prepared from the following raw materials: Ti: 4% to 20%, Zr: 20%, Mo: 20%, Nb: 20%, Cr: 20%.
2. A refractory high entropy alloy coating according to claim 1, characterized in that the specific content of said Ti element is 4%, 8%, 12%, 18%, 20% respectively.
3. A method for preparing a refractory high-entropy alloy coating according to any one of claims 1 to 2, characterized in that it comprises:
S1. subjecting the surface of the TC4 (Ti-6AI-4V) matrix to a rust and oil removal treatment, so that the surface of the matrix is clean and flat and has a certain roughness;
S2. mixing the powders and then vacuum ball milling them to a powder particle size of 180 ~300 mesh;
S3.and mix the obtained alloy powder with 5-10% anhydrous ethanol, evenly coated on the surface of the matrix, line into a prefabricated layer;
S4. put into the drying oven for 10 hours and then obtain the cladding layer by laser melting.
4. A method of preparing a refractory high entropy alloy coating according to claim 3, characterized in that the vacuum ball milling time is not less than 3 hours.
5. A method of preparing a refractory high-entropy alloy coating according to claim 3, characterized in that the thickness of the prefabricated coating is 1.0 mm.
6. A method of preparing a refractory high-entropy alloy coating according to claim 3, characterised in that the process parameters for laser coating are: laser power of 3700 W, scanning speed of 350 mm/min, spot diameter of 3.0 mm, off-focus volume of 20 mm, protective gas of argon, gas flow rate of 8 L/min.
LU504318A 2023-05-25 2023-05-25 A refractory high-entropy alloy coating and its preparation method LU504318B1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118639179A (en) * 2024-08-15 2024-09-13 烟台大学 Preparation method of ZrNbTiCrCu high-entropy nano alloy film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118639179A (en) * 2024-08-15 2024-09-13 烟台大学 Preparation method of ZrNbTiCrCu high-entropy nano alloy film

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