CN110804711A - High-entropy alloy powder and preparation method and application of laser cladding layer - Google Patents
High-entropy alloy powder and preparation method and application of laser cladding layer Download PDFInfo
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- CN110804711A CN110804711A CN201810885314.2A CN201810885314A CN110804711A CN 110804711 A CN110804711 A CN 110804711A CN 201810885314 A CN201810885314 A CN 201810885314A CN 110804711 A CN110804711 A CN 110804711A
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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
- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
Abstract
The invention discloses a high-entropy alloy powder and a preparation method and application of a laser cladding layer. When laser cladding is carried out, H13 steel is selected as a base material, the laser power is 1300-1600 KW, the diameter of a light spot is 2-4 mm, the scanning speed is 5-7 mm/s, the defocusing amount is 10mm, and the flow of protective gas is 20-25L/min. The laser cladding high-entropy alloy coating has larger chaos and becomes larger at high temperature, and the high mixed entropy effect obviously reduces the diffusion and redistribution rate among elements, so that the phase structure in the coating is stable, the high-temperature hardness is basically kept unchanged, and the high-temperature softening resistance is good.
Description
Technical Field
The invention relates to the field of laser surface modification, in particular to the field of preparation of high-entropy alloy powder for laser cladding and a cladding layer.
Background
At present, the wide definition of the high-entropy alloy refers to an alloy consisting of 5 to 13 main elements, and the content of each element is between 5 and 30 percent. The multicomponent high-entropy alloy has become a new research hotspot in the field of metal materials because of the unique phase structure, the brand-new design concept and the excellent alloy performance, and is called three major breakthroughs in the field of alloying theories in recent years together with rubber metal and bulk metallic glass.
The high-entropy alloy has high diffusion activation energy for forming a disordered solid solution among different atoms, can seriously obstruct a diffusion process, and can still keep the structural stability under the heating condition. The high-temperature performance material in the field of materials at present has larger demand space, and the high-entropy alloy is a potential powerful choice by virtue of the advantage of thermodynamic stability.
At present, the research on high-entropy alloy mainly focuses on vacuum arc melting and casting block materials, which causes the preparation size to be greatly limited; and the metals used for preparation are expensive, so that the cost for producing large parts is too high. The preparation of the high-entropy alloy coating can not only avoid the defects, but also obtain excellent service performance. The laser cladding has high heating and cooling rates, small heat influence on a matrix, fine and uniform distribution of cladding layer grains in the matrix, metallurgical bonding between the coating and the matrix, high bonding strength and the maximum coating thickness of several millimeters.
H13(4Cr5MoSiV1) is widely used hot-work die steel, has higher hot strength and hardness, high wear resistance and toughness and better thermal fatigue resistance, and is widely applied to manufacturing various forging dies, hot extrusion dies and die-casting dies of magnesium, aluminum and alloys thereof. The H13 die casting die bears physical and chemical actions such as abrasion, thermal fatigue, erosion, stress corrosion, surface heat welding and the like in the using process, so the service life of the die casting die is short. It is known that the failure of the mold is initiated from the surface first, and thus improving the surface texture and properties is effective in increasing the useful life of the mold.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a high-entropy alloy powder material, a preparation method and application of a cladding layer, obtains the well-formed cladding layer, improves the hardness and the high-temperature oxidation resistance of the material, prepares the high-entropy alloy cladding layer on the surface of H13 steel through a laser cladding process, and effectively improves the hardness and the high-temperature oxidation resistance of H13 steel, thereby prolonging the service life of the H13 steel and reducing the material cost consumption.
The technical purpose of the invention is realized by the following technical scheme:
the high-entropy alloy powder is composed of Fe, Co, Cr, Mn, Ni and Al element powder, namely the alloy powder composition is represented as FeCoCrNiMnAl, and specifically, the Fe, Co, Cr, Mn, Ni and Al are in equal molar ratio, namely the mole numbers of the six metal elements are consistent.
When the preparation is carried out, firstly, the proportion calculation is carried out according to the molar ratio of each element, the components are weighed accurately and then are fully mixed to be uniform, for example, the powder of each element is weighed by an electronic scale and is ground in a mortar to be uniformly mixed, and the grinding time is 0.5-1 hour. Wherein, the selected components are powder with the purity of more than or equal to 99 percent and the particle size of 200-300 meshes.
The alloy powder is applied to laser cladding welding, high-entropy alloy powder and ethanol are mixed and then uniformly coated on the surface of a base material, and a cladding layer can be obtained through laser cladding after drying.
The ethanol is analytically pure absolute ethanol, and consists of 92-95% of alloy powder and 5-8% of ethanol in a mixture of six-membered high-entropy alloy powder and ethanol in percentage by mass.
After mixing, forming paste or paste to be convenient for coating on the surface of the base material, and forming a prefabricated layer on the surface of the base material after coating, wherein the thickness of the prefabricated layer is 0.8-1.2 mm.
Wherein the substrate material is descaled and oil stain removed.
When laser cladding is carried out, H13 steel is selected as a base material, and the technological parameters are as follows: the laser power is 1300-1600 KW, the diameter of a light spot is 2.0-4.0 mm, the scanning speed is 5-7 mm/s, the defocusing amount is 6-10 mm, the protective gas is argon, nitrogen or helium, and the gas flow is 20-25L/min.
The technological parameters are as follows: the laser power is 1400-1500 KW, the diameter of a light spot is 2.0-4.0 mm, the scanning speed is 6-7 mm/s, the defocusing amount is 8-10 mm, the protective gas is argon, nitrogen or helium, and the gas flow is 20-25L/min.
Compared with the prior art, the invention has the following advantages:
(1) in the alloy powder, Cr is mainly used for improving the hardness of a cladding layer through solid solution strengthening and for improving the corrosion resistance of the cladding layer, and Al plays a role in solid solution strengthening in the system. The solid solution strengthening effect is good because the atomic radius is larger. The induced lattice distortion increases with increasing Al content. Further, Al and Cr form protective Al2O3、Cr2O3Further oxidation of the matrix can be prevented, and the oxidation rate of the alloy is reduced. In addition, the disorder degree of the laser cladding high-entropy alloy coating is larger, the coating becomes larger at high temperature, and the diffusion and redistribution rate among elements is remarkably reduced by the high mixed entropy effect, so that the phase structure in the coating is stable, the high-temperature hardness is basically kept unchanged, and the high-temperature softening resistance is good.
(2) The invention provides high-entropy alloy powder consisting of metal elements, and the self-fluxing property of the powder is improved.
(3) The invention prepares the cladding layer with good forming, higher hardness and better oxidation resistance, and the performance is obviously improved compared with the base material.
Drawings
FIG. 1 is a macroscopic morphology photograph (surface) of a FeCoCrNiMnAl cladding layer prepared by the present invention.
FIG. 2 is a photograph (cross section) of the overall appearance of a FeCoCrNiMnAl cladding layer prepared by the invention.
FIG. 3 is a photograph of the metallurgical structure of the FeCoCrNiMnAl cladding layer prepared by the invention.
Detailed Description
The technical scheme of the invention is further illustrated by the following specific examples:
the matrix material is H13 steel (purchased from Tianjin Yi iron and Steel Co., Ltd.), the mechanical polishing is adopted to remove oxides, the acetone is adopted to remove oil stains, and the chemical components are shown in the following table (mass fraction%) (the components meet the national standard):
the method is implemented according to the following steps:
1. the proportion of FeCoCrNiMnAl high-entropy alloy powder is calculated according to the molar ratio, the powder of various elements is weighed by an electronic scale and is ground in a mortar for half an hour to be uniformly mixed.
2. Mixing 92-95% of laser cladding powder and 5-8% of ethanol into paste or paste, coating the paste or paste on the surface of a base material, wherein the thickness of a prefabricated layer is 1-1.2 mm, and obtaining a cladding layer through laser cladding after air drying.
3. The selection laser used model JK2003SM Nd: YAG laser cladding.
4. The metallographic structure observation equipment adopts an OLYMPUS-GX 51 metallographic microscope, and the manufacturer comprises: olympus, Inc., Japan.
Example 1
1. Calculating the proportion of FeCoCrNiMnAl high-entropy alloy powder according to the molar ratio: 16.67 mol% of Fe, 16.67 mol% of Co, 16.67 mol% of Cr, 16.67 mol% of Ni, 16.66 mol% of Mn, 16.66 mol% of Al, and a total molar ratio of 100%, and powders of the respective elements were weighed using an electronic scale.
2. Pouring into a mortar, and grinding in the mortar for half an hour to uniformly mix.
3. Mixing the prepared laser cladding powder with 92% ethanol and 8% ethanol to form paste or paste, coating the paste or paste on the surface of H13 steel, wherein the thickness of a preset layer is 1mm, and carrying out laser cladding after air drying.
4. The laser cladding process parameters are as follows: the laser power is 1550KW, the spot diameter is 2.5mm, the scanning speed is 5mm/s, the defocusing amount is 10mm, the protective gas adopts argon, and the gas flow is 25L/min.
5. After laser cladding, aqua regia is adopted for corrosion, and a metallographic photograph of the cladding layer is obtained.
The microhardness of the cladding layer is measured by adopting an automatic turret digital display hardness tester, and the experimental result is shown in the following table, and the average hardness after laser cladding reaches 655HV, which is obviously improved compared with that of the base material.
6. The prepared high-entropy alloy material is cut into samples of 10mm multiplied by 3mm in a linear mode, the samples are ground, then 600# metallographic abrasive paper is used for grinding, and the samples are washed by ethanol for later use. The intermittent constant-temperature oxidation experiment is carried out according to HB5258-83 determination method for the oxidation resistance of steel and high CN 104561718A specification 65/7 page 7 temperature alloy; weighing the weight of each sample before the high-temperature oxidation experiment, then putting the samples into a preheated high-temperature oxidation furnace (KBF 1100), statically oxidizing for 200 hours at 700 ℃, and then turning off a power supply; after the oxidation furnace is cooled to room temperature, taking out the sample, placing the sample in a precision electronic balance (XP2001S, induction capacity 0.1mg) to weigh the weight of the sample after high-temperature oxidation, and measuring the mass increase of the sample after oxidation by 3.15 multiplied by 10-3mg/mm2The matrix is obviously improved by (150 multiplied by 10)-3mg/mm2) High temperature oxidation resistance.
Example 2
1. Mixing the prepared laser cladding powder with 95% and 5% ethanol to form paste or paste, coating the paste or paste on the surface of H13 steel, wherein the thickness of the preset layer is 1.2mm, and carrying out laser cladding after air drying.
2. The laser cladding process parameters are as follows: the laser power is 1600KW, the diameter of a light spot is 3.0mm, the scanning speed is 6mm/s, the defocusing amount is 10mm, the protective gas adopts helium, and the gas flow is 20L/min.
3. The same was used for the performance tests and the results are shown in the table below.
Embodiment 3
1. Mixing the prepared laser cladding powder with 94% ethanol to form paste or paste, coating the paste or paste on the surface of H13 steel, wherein the thickness of the preset layer is 0.8mm, and carrying out laser cladding after air drying.
2. The laser cladding process parameters are as follows: the laser power is 1400KW, the diameter of a light spot is 3.5mm, the scanning speed is 7mm/s, the defocusing amount is 10mm, the protective gas is argon, and the gas flow is 22L/min.
3. The same was used for the performance tests and the results are shown in the table below.
Example 4
1. Mixing the prepared laser cladding powder with 93% and 7% ethanol to form paste or paste, coating the paste or paste on the surface of 42CrMo steel, wherein the thickness of a preset layer is 1mm, and carrying out laser cladding after air drying.
2. The laser cladding process parameters are as follows: the laser power is 1300KW, the diameter of the light spot is 4mm, the scanning speed is 5mm/min, the defocusing amount is 10mm, the protective gas adopts helium, and the gas flow is 20L/min
3. The same was used for the performance tests and the results are shown in the table below.
As shown in attached figures 1-3, the FeCoCrNiMnAl cladding layer prepared by the invention has good surface appearance and cross section appearance, the grain size of the laser cladding layer is smaller than that of the matrix grain size, the hardness of the cladding layer is effectively improved, and the high-temperature oxidation resistance of the cladding layer can be effectively improved by the dendritic crystal growth of the cladding layer along the reverse direction of laser cladding.
The preparation process parameters are adjusted according to the content of the invention, the preparation of FeCoCrNiMnAl cladding layer can be realized, and the performance which is basically consistent with the embodiment is shown by tests, namely the FeCoCrNiMnAl high-entropy alloy powder is applied to the improvement of the hardness and the high-temperature oxidation resistance of H13 steel (the hardness can reach 650-670 HV, and the oxidation weight gain at 700 ℃ can reach 3-3.2 multiplied by 10-3mg/mm2). The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The high-entropy alloy powder is characterized by consisting of Fe, Co, Cr, Mn, Ni and Al element powder, namely the alloy powder composition is represented as FeCoCrNiMnAl, and the Fe, Co, Cr, Mn, Ni and Al are in equal molar ratio, namely the mole numbers of the six metal elements are consistent.
2. A high entropy alloy powder according to claim 1, wherein each component is selected to be a powder having a purity of 99% or more and a particle size of 200 to 300 mesh.
3. A method for producing a high-entropy alloy powder as claimed in claim 1 or 2, wherein the compounding ratio is calculated in terms of the molar ratio of each element, and the respective components are mixed thoroughly after the masses thereof are accurately weighed to be uniform.
4. A method for preparing high-entropy alloy powder according to claim 3, wherein the powders of the elements are weighed by an electronic scale and ground in a mortar for uniform mixing, for example, the grinding time is 0.5-1 hour.
5. The method for carrying out laser cladding welding by using the high-entropy alloy powder as claimed in claim 1 or 2, is characterized in that the high-entropy alloy powder and ethanol are mixed and then uniformly coated on the surface of a base material, a cladding layer can be obtained by laser cladding after drying, the base material is H13 steel when laser cladding is carried out, and the process parameters are as follows: the laser power is 1300-1600 KW, the diameter of a light spot is 2.0-4.0 mm, the scanning speed is 5-7 mm/s, the defocusing amount is 6-10 mm, the protective gas is argon, nitrogen or helium, and the gas flow is 20-25L/min.
6. The method of performing laser cladding welding according to claim 5, wherein the process parameters are: the laser power is 1400-1500 KW, the diameter of a light spot is 2.0-4.0 mm, the scanning speed is 6-7 mm/s, the defocusing amount is 8-10 mm, the protective gas is argon, nitrogen or helium, and the gas flow is 20-25L/min.
7. The laser cladding welding method according to claim 5 or 6, wherein the ethanol is analytically pure absolute ethanol, and the mixture of the six-element high-entropy alloy powder and the ethanol comprises 92-95% of alloy powder and 5-8% of ethanol by mass percent.
8. The method for laser cladding welding according to claim 5, wherein the high entropy alloy powder is mixed with ethanol to form paste or paste, so as to be coated on the surface of the base material, and a prefabricated layer is formed on the surface of the base material after coating, wherein the thickness of the prefabricated layer is 0.8-1.2 mm.
9. Use of a high entropy alloy powder of claim 1 or 2 to improve hardness and high temperature oxidation resistance of H13 steel.
10. Use according to claim 10, characterised in that the hardness is up to 650-670 HV and the oxidation weight gain at 700 ℃ is up to 3-3.2 x 10-3mg/mm2。
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Cited By (8)
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CN111394721A (en) * | 2020-05-29 | 2020-07-10 | 济南大学 | High-entropy alloy powder mixture, coating and coating preparation method |
CN112662984A (en) * | 2020-12-08 | 2021-04-16 | 武汉理工大学 | High-entropy alloy coating material and preparation method and application thereof |
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CN115161637A (en) * | 2022-08-03 | 2022-10-11 | 天津大学 | Wear-resistant and corrosion-resistant coating on surface of piston rod and preparation method thereof |
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Application publication date: 20200218 |