CN114657550B - Preparation process of refractory high-entropy alloy coating resistant to high temperature friction and wear - Google Patents
Preparation process of refractory high-entropy alloy coating resistant to high temperature friction and wear Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 84
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
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- 239000002184 metal Substances 0.000 claims abstract description 61
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- 238000004372 laser cladding Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 23
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- 238000005299 abrasion Methods 0.000 claims abstract description 12
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000011261 inert gas Substances 0.000 claims description 20
- 150000003839 salts Chemical class 0.000 claims description 20
- 239000012752 auxiliary agent Substances 0.000 claims description 19
- 238000005253 cladding Methods 0.000 claims description 17
- 239000001307 helium Substances 0.000 claims description 17
- 229910052734 helium Inorganic materials 0.000 claims description 17
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 13
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
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- 239000011780 sodium chloride Substances 0.000 claims description 6
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- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
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Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Powder Metallurgy (AREA)
- Coating By Spraying Or Casting (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention discloses a preparation process of a refractory high-entropy alloy coating resistant to high temperature friction and wear, wherein the coating comprises W, mo, ta, nb raw materials which are all simple metals; then placing the refractory simple substance powder after the drying pretreatment in a planetary ball mill, and ball milling to obtain the required refractory high-entropy alloy powder raw material; then, carrying out substrate treatment; finally, the high-temperature friction and abrasion resistant refractory high-entropy alloy coating is prepared by laser cladding and forming, the surface hardness of the coating is more than or equal to 1000HV, the abrasion rate is less than or equal to 1.0X10 ‑5mm3N‑1m‑1, and the bonding strength of the coating is more than or equal to 90N. The refractory high-entropy alloy coating with high-temperature friction and wear resistance prepared by the method is difficult to generate cracks, so that the wear resistance is ensured.
Description
Technical Field
The invention relates to the technical field of high-entropy alloy coatings, in particular to a preparation process of a high-temperature friction and wear resistant refractory high-entropy alloy coating.
Background
The high-entropy alloy has excellent high-temperature mechanical properties due to strong high-entropy effect, lattice distortion effect, diffusion hysteresis effect and interaction among multiple principal elements. The refractory high-entropy alloy not only has excellent high-temperature mechanical property and thermal stability, but also has better toughness and specific strength, can keep higher yield strength at higher temperature, meets the rigor of high-temperature service environment of aerospace, and has the potential of replacing ceramic high-temperature protective coatings.
The laser cladding refers to a process method that external materials are added into a molten pool formed after a substrate is irradiated by laser in a synchronous or preset material mode, and the external materials and the molten pool are solidified together to form a coating layer, so that the wear resistance, corrosion resistance, heat resistance, oxidation resistance or electrical characteristics of the surface of the substrate material can be obviously improved, the purpose of surface modification or repair is achieved, the specific performance requirement of the surface of the material is met, and a large amount of material cost can be saved. Compared with surfacing, spraying, electroplating and vapor deposition, the laser cladding has the characteristics of small dilution, compact structure, good combination of a coating and a matrix, suitability for cladding materials, large granularity and content change and the like, so the application prospect of the laser cladding technology is very broad. Typically, laser cladding techniques are applied to high-entropy alloys to produce coatings having refractory high-entropy alloys that are resistant to high temperatures.
However, the cooling rate of the high-temperature refractory high-entropy alloy coating produced by the laser cladding technology in the prior art is too high, so that thermal stress is generated among molecules in the coating, the thermal stress tends to accelerate the movement among the molecules in the coating, so that the high-temperature refractory high-entropy alloy coating generates local cracks, and the cracks are accelerated to diffuse due to the characteristics of higher melting point of the high-temperature refractory high-entropy alloy coating and the characteristic of overlarge difference of thermal expansion coefficients compared with a base material, so that the diffused cracks can lead to the fact that the high-temperature refractory high-entropy alloy coating is not resistant to abrasion.
Disclosure of Invention
In view of the above problems, the invention provides a preparation process of a refractory high-temperature friction and wear resistant high-entropy alloy coating, which can reduce local cracks generated in the preparation process of the refractory high-entropy alloy coating, so that the produced refractory high-entropy alloy coating has the performance of friction and wear resistance.
The technical scheme of the invention is as follows:
A preparation process of a refractory high-entropy alloy coating resistant to high temperature friction and wear comprises the following steps:
s1, preparation of powder
Weighing 15.62-38.64% of W, 14.72-22.64% of Mo, 14.72-40.62% of Ta14.72-40.82% of Nb, and pure metals with the purity of more than or equal to 99.95% of each pure metal, preparing refractory simple substance powder by using a plasma rotary electrode atomization method, sieving the powder, and drying and pre-treating the powder;
S2, ball milling mixed powder
Placing the refractory simple substance powder after the drying pretreatment in a planetary ball mill, and ball milling to obtain a required refractory high-entropy alloy powder raw material;
S3, substrate treatment
S3-1, polishing the surface of the substrate to be smooth, removing oil stains on the surface of the substrate, performing sand blasting treatment, cleaning the substrate in an ultrasonic cleaner for 30min to remove surface adhesion impurities, and finally drying in a blast drying oven at 120-250 ℃ for 1-2h for later use;
S3-2, uniformly coating the active auxiliary agent on the surface of the base material treated in the step S3-1, wherein the coating thickness of the active auxiliary agent is 0.2-0.4mm;
S4, laser cladding forming
The refractory high-entropy alloy powder obtained in the step S2 is laser-clad on the substrate obtained in the step S3 to form a refractory high-entropy alloy coating resistant to high-temperature friction and abrasion; wherein the laser power is 800-1200W, the light spot diameter is 1mm, the scanning speed is 600-1500mm/s, the cladding overlap ratio is 50-60%, the powder feeding speed is 0.2-0.5r/min, and the gas flow of the shielding gas is 3-5L/min.
Further, in the step 1, 2.4 to 6.8 mass percent of pure metal V is also weighed, and the purity of the pure metal V is more than or equal to 99.95 percent. The V simple substance pure metal is used as the mixed metal of the high-entropy alloy, and the structural performance of the whole high-entropy alloy can be improved because the V simple substance pure metal has good ductility.
Further, the specific steps of step S1 are:
S1-1, machining all simple substance pure metals into bar stock by using a lathe;
S1-2, placing the bar blank obtained in the step S1-1 into atomization powder making equipment, vacuumizing, and when the vacuum degree in the atomization chamber is 5 multiplied by 10 -3 Pa, filling inert gas and metal salt powder mixture into the atomization chamber, wherein the inert gas is mixed gas of argon and helium, and the metal salt powder is NaCl powder;
S1-3: heating and melting the bar blank rotating at a high speed by using a plasma torch, and finally cooling the melted liquid drops to obtain refractory simple substance metal powder; wherein, the plasma arc current is 1200-1800A, the voltage is 120-180V, and the rotating speed of the metal electrode is 10000-15000r/min. Wherein, the plasma arc current is 1200-1800A, the voltage is 120-180V, and the rotating speed of the metal electrode is 10000-15000r/min. The refractory simple metal powder prepared by the plasma rotary electrode atomization method has the advantages that the particle diameters are uniformly distributed and are between 10 mu m and 80 mu m, so that the metal powder can be well fused with each other, and the finally prepared refractory high-entropy alloy coating can not mutually aggravate movement due to thermal stress among metal particles in the subsequent working procedure, namely in the laser cladding process, thereby effectively reducing the generation of cracks.
Further, in the step S1, after being dried for 2 hours by a blast drying heating furnace at 110 ℃, the particle size of each refractory simple metal is 28-73 mu m, and the powder flowability is 19.07S/50g. The diameter difference of the metal particles can be further reduced through heating and drying treatment, and the rapid fusion of the metal elements in the subsequent process is ensured.
Further, in the step S2, the ball-material ratio in the ball milling process is 5:4, and the ball milling and powder mixing time is 4 hours.
Further, in step S3, the material of the base material is a Ni-based superalloy. The nickel-based alloy has good oxidation resistance, so that the oxidation resistance of the refractory high-entropy alloy coating material is further improved by selecting the base material as the nickel-based alloy.
Further, before the refractory high-entropy alloy coating is coated, the printing bin is required to be filled with a protective gas, wherein the protective gas is a mixed gas of nitrogen and helium, and the oxygen content of air is ensured to be less than or equal to 0.5%. High temperature oxidation during cladding is avoided.
Further, the coagent of S3-2 comprises SiO 2: 25-30 parts of MnO:20-25 parts of TiO 2: 15-18 parts; the preparation method of the active auxiliary agent comprises the following steps: and (3) respectively weighing the SiO 2、MnO、TiO2 in parts by weight, putting into a glass container, then adding 18-24 parts of dimethyl ketone, and uniformly stirring. The active auxiliary agent with the proportion is coated on the surface of the base material, so that the penetration of refractory high-entropy alloy powder and the base material during welding is improved, and the bonding strength of the high-entropy alloy coating and the base material is improved.
Compared with the prior art, the invention has the beneficial effects that: the high-temperature resistant refractory high-entropy alloy coating prepared by the method can reach the requirements that the surface hardness is more than or equal to 1000HV, the coating wear rate is less than or equal to 1.0X10 -5mm3N-1m-1, and the coating bonding strength is more than or equal to 90N, namely, on the basis of fully ensuring the oxidation resistance and high temperature resistance, the coating is well bonded with a base material, the structure is compact, the uniform distribution of the diameters of alloy metal particles is ensured under the condition that the laser cladding causes the thermal stress in the coating, and the acceleration of movement among the particles is not ensured, so that the difficulty in cracking is ensured. And the produced refractory high-entropy alloy coating has the advantages of flat and smooth surface, low roughness and high forming quality, and can be put into industrial application. The preparation method provided by the invention utilizes plasma rotary electrode atomization and a laser cladding method to enable metal particles to be uniformly fused with each other, provides a new thought for preparing the refractory high-entropy alloy coating with high temperature resistance and wear resistance, and has the advantages of simple process, high efficiency, high forming quality, high powder material utilization rate, excellent properties of formed parts and the like.
Drawings
FIG. 1 is a flow chart of a method of preparing a refractory high entropy alloy coating of the present invention that is resistant to high temperatures and abrasion;
FIG. 2 is an SEM image of the powder of the various metal raw materials of the present invention;
FIG. 3 is an SEM image of a refractory high entropy alloy coating laser clad at optimum parameters for example 1;
FIG. 4 is a graph of XRD analysis test results of a wear-resistant refractory high-entropy alloy coating laser cladding under optimal parameters in example 1;
FIG. 5 is an SEM image of a refractory high entropy alloy coating of example 2;
FIG. 6 is a scan of the surface roughness of the refractory high entropy alloy coating of example 2;
FIG. 7 is a first linear diagram of FIG. 6;
FIG. 8 is a second linear diagram of FIG. 6;
Fig. 9 is a data parameter diagram of fig. 6.
Detailed Description
The following detailed description of embodiments of the invention is, therefore, to be taken in conjunction with the accompanying drawings, and it is to be understood that the scope of the invention is not limited to the specific embodiments.
Example 1
A preparation process of a refractory high-entropy alloy coating resistant to high temperature friction and wear comprises the following steps:
s1, preparation of powder
The method comprises the steps of weighing W35.19%, mo18.65%, ta30.49% and Nb15.67% of simple substance pure metals according to the following mass percentages, preparing refractory simple substance powder by a plasma rotary electrode atomization method, sieving the powder with the particle size of less than 50 mu m, and drying and preprocessing the powder, wherein the SEM (scanning electron microscope) pictures of the raw metal materials are shown in figure 2, and the SEM pictures of W, mo, ta, nb raw materials are respectively from the upper left, the upper right, the lower left and the lower right.
The specific operation is as follows:
S1-1, machining all simple substance pure metals into bar stock by using a lathe;
s1-2, placing the bar blank obtained in the step S1-1 into atomization powder making equipment, vacuumizing, and when the vacuum degree in the atomization chamber is 5 multiplied by 10 -3 Pa, filling inert gas and metal salt powder into the atomization chamber, wherein the mass ratio of the inert gas to the metal salt powder is 1:4, 10 parts of inert gas and 40 parts of metal salt powder are taken, the inert gas is mixed gas of argon and helium, the mixed mass ratio of the argon is 67%, and the metal salt powder is NaCl powder;
S1-3: heating and melting the bar blank rotating at a high speed by using a plasma torch, and finally cooling the melted liquid drops to obtain refractory simple substance metal powder; wherein, the plasma arc current 1200A, the voltage is 120V, the rotating speed of the metal electrode is 10000r/min.
S2, ball milling mixed powder
Taking 351.9gW, 186.5gMo, 304.9gTa and 156.7gNb simple substance powder prepared in the step S1 respectively, putting the simple substance powder into a cleaned planetary ball mill, and then putting steel balls into the planetary ball mill for ball milling and powder mixing, wherein the ball-to-material ratio is 5: 4, mixing powder for 4 hours.
S3, substrate treatment
S3-1, polishing the surface of a substrate to be smooth by taking an Inconel 718 alloy plate as the substrate, removing greasy dirt on the surface of the substrate, and then performing sand blasting treatment, wherein the technological parameters of the abrasive are as follows: the grinding material is cast iron sand with the grain diameter of 0.5mm-1.5mm, and compressed air subjected to injection treatment is subjected to cooling and oil-water separation treatment to ensure that the compressed air is dry and oilless, wherein the pressure of the compressed air is 0.7MPa; then placing the substrate in an ultrasonic cleaning machine for cleaning for 30min to remove surface adhesion impurities, wherein the parameters of ultrasonic cleaning are as follows: the cleaning temperature is 30 ℃ and the ultrasonic frequency is 20KHz; finally, placing the base material and the powder raw material at 120 ℃ for 2 hours for standby;
S3-2, uniformly coating the active auxiliary agent on the surface of the base material treated in the step S3-1, wherein the coating thickness of the active auxiliary agent is 0.2mm; the preparation process of the active auxiliary agent comprises the following steps: 25 parts by weight of SiO 2, 20 parts by weight of MnO, and 15 parts by weight of TiO 2 were weighed into a glass container, and 18 parts by weight of dimethyl ketone was added.
S4, laser cladding forming
And (3) placing the substrate obtained in the step (S3) into a printing bin of LDM-8060 laser cladding forming equipment, setting cladding parameter laser power to be 800W, 1000W, 1200W and 1500W, scanning the substrate at 600, 900, 1200 and 1500mm/S, and carrying out cladding lap joint at 50, 60 and 70%, and carrying out powder feeding at 0.2, 0.3 and 0.5r/min, wherein a scanning strategy is single-channel reciprocation. And (3) introducing protective gas which is mixed gas of nitrogen and helium, wherein the mixing mass ratio is 2:5, and 2 parts of nitrogen and 5 parts of helium are added into the cleaned blower, starting a procedure when the oxygen content is reduced to below 0.5%, and finally obtaining the refractory high-entropy alloy coating with high-temperature friction and abrasion resistance.
And finally, taking out the sample after the refractory high-entropy alloy coating resistant to high temperature friction and abrasion is naturally cooled to room temperature, and performing subsequent characterization by cutting the sample into uniform sizes through wire cutting after the surface is cleaned.
Through subsequent experimental tests and characterization, WMoTaNb wear-resistant refractory high-entropy alloy coating laser cladding optimal parameters are selected by utilizing a single-factor variable method: the laser power is 1000W, the scanning speed is 900mm/s, the cladding overlap ratio is 50%, and the powder feeding speed is 0.3r/min.
The cladding parameter selection results are shown in table 1:
Table 1: cladding parameter selection table
As shown in an SEM image of the wear-resistant refractory high-entropy alloy coating shown in figure 3 and an XRD analysis test result image of the wear-resistant refractory high-entropy alloy coating shown in figure 4, the coating and the substrate form metallurgical bonding, the thickness of the coating is uniform, no impurity peak appears as can be seen by XRD on the surface of the coating, and the coating is completely composed of WMoTaNb, so that the expected effect is achieved. The wear-resistant refractory high-entropy alloy coating has an average friction coefficient of 0.5, a wear cross-sectional area of less than 7635.821 mu m < 2 >, a wear rate of less than 5.5X10-7 mm 3/N.m and good wear resistance at 600 ℃.
Example 2
A preparation process of a refractory high-entropy alloy coating resistant to high temperature friction and wear comprises the following steps:
s1, atomizing and pulverizing by using plasma rotary electrode
Weighing 15.62% of W, 14.72% of Mo, 40.62% of Ta40.62% of Nb10.25% of W and 6.8% of pure metal by mass percent, preparing refractory simple substance powder by using a plasma rotary electrode atomization method, sieving the powder with the particle size of less than 50 mu m, and drying and preprocessing the powder; the specific operation is as follows:
S1-1, machining all simple substance pure metals into bar stock by using a lathe;
s1-2, placing the bar blank obtained in the step S1-1 into atomization powder making equipment, vacuumizing, and when the vacuum degree in the atomization chamber is 5 multiplied by 10 -3 Pa, filling inert gas and metal salt powder mixture into the atomization chamber, wherein the mass ratio of the inert gas to the metal salt powder is 1:4, 20 parts of inert gas, 80 parts of metal salt powder, the inert gas is argon and helium mixed gas, the mixed mass ratio of the argon is 67%, and the metal salt powder is NaCl powder;
S1-3: heating and melting the bar blank rotating at a high speed by using a plasma torch, and finally cooling the melted liquid drops to obtain refractory simple substance metal powder; wherein, the plasma arc current 1800A, the voltage is 180V, and the rotating speed of the metal electrode is 15000r/min.
S2, ball milling mixed powder
Respectively taking 156.2gW, 147.2gMo, 406.2gTa, 102.5gNb and 680gV simple substance powder prepared in the step S1, putting the simple substance powder into a cleaned planetary ball mill, and then putting steel balls for ball milling and powder mixing, wherein the ball-material ratio is 5;4, mixing powder for 4 hours.
S3, substrate treatment
S3-1, polishing the surface of a substrate to be smooth by taking an Inconel 718 alloy plate as the substrate, removing greasy dirt on the surface of the substrate, and then performing sand blasting treatment, wherein the technological parameters of the abrasive are as follows: the grinding material is cast iron sand with the grain diameter of 0.5mm-1.5mm, and compressed air subjected to injection treatment is subjected to cooling and oil-water separation treatment to ensure that the compressed air is dry and oilless, wherein the pressure of the compressed air is 0.7MPa; then placing the substrate in an ultrasonic cleaning machine for cleaning for 30min to remove surface adhesion impurities, wherein the parameters of ultrasonic cleaning are as follows: the cleaning temperature is 40 ℃ and the ultrasonic frequency is 20KHz; finally, placing the base material and the powder raw material at 120 ℃ for 2 hours for standby;
S3-2, uniformly coating the active auxiliary agent on the surface of the base material treated in the step S3-1, wherein the coating thickness of the active auxiliary agent is 0.2mm; the preparation process of the active auxiliary agent comprises the following steps: 25 parts by weight of SiO 2, 20 parts by weight of MnO, and 15 parts by weight of TiO 2 were weighed into a glass container, and 18 parts by weight of dimethyl ketone was added.
S4, laser cladding forming
And (3) placing the substrate obtained in the step (S3) into a printing bin of LDM-8060 laser cladding forming equipment, setting cladding parameter laser power to be 1000W, scanning speed to be 1200mm/S, cladding overlap ratio to be 50%, powder feeding speed to be 0.2r/min, and scanning strategy to be single-channel reciprocation. And (3) introducing protective gas which is a mixed gas of nitrogen and helium, wherein the mass ratio of the nitrogen to the helium is 2:3, wherein 2 parts of nitrogen and 3 parts of helium are added into a cleaned blower, and starting a procedure when the oxygen content is reduced to below 0.5%, so as to melt the high-entropy alloy coating.
The finally obtained alloy coating is shown in figures 5-9, and the prepared coating has the advantages of smooth surface, low roughness, small friction coefficient, stable process with high Wen Masun and good wear resistance.
The average friction coefficient of the coating is between 0.5 and 0.8, the abrasion cross-sectional area is smaller than 7635.821 mu m < 2 >, the abrasion rate is smaller than 5.5X10 -7mm3/N.m, and the abrasion resistance is good.
Example 3
A preparation process of a refractory high-entropy alloy coating resistant to high temperature friction and wear comprises the following steps:
s1, preparation of powder
Weighing W38.64%, mo22.64%, ta14.72% and Nb25.82% of simple substance pure metals according to the following mass percentages, wherein the purity of each simple substance pure metal is more than or equal to 99.95%, preparing refractory simple substance powder by using a plasma rotary electrode atomization method, sieving the powder with a particle size of less than 50 mu m, and drying and preprocessing the powder;
the specific operation is as follows:
S1-1, machining all simple substance pure metals into bar stock by using a lathe;
s1-2, placing the bar blank obtained in the step S1-1 into atomization powder making equipment, vacuumizing, and when the vacuum degree in the atomization chamber is 5 multiplied by 10 -3 Pa, filling inert gas and metal salt powder into the atomization chamber, wherein the mass ratio of the inert gas to the metal salt powder is 1:4, 15 parts of inert gas, 60 parts of metal salt powder, the inert gas is mixed gas of argon and helium, the mixed mass ratio of the argon is 67%, and the metal salt powder is NaCl powder;
S1-3: heating and melting the bar blank rotating at a high speed by using a plasma torch, and finally cooling the melted liquid drops to obtain refractory simple substance metal powder; wherein, the plasma arc current 1300A, the voltage is 150V, and the rotating speed of the metal electrode is 20000r/min.
S2, ball milling mixed powder
And (3) respectively taking 386.4gW, 226.4gMo, 147.2gTa and 258.2gNb simple substance powder prepared in the step (S1), putting the simple substance powder into a clean planetary ball mill, and then putting steel balls into the planetary ball mill for ball milling and powder mixing, wherein the ball-material ratio is 5:4, and the powder mixing time is 4h.
S3, substrate treatment
S3-1, polishing the surface of a substrate to be smooth by taking an Inconel 718 alloy plate as the substrate, removing greasy dirt on the surface of the substrate, and then performing sand blasting treatment, wherein the technological parameters of the abrasive are as follows: the grinding material is cast iron sand with the grain diameter of 0.5mm-1.5mm, and compressed air subjected to injection treatment is subjected to cooling and oil-water separation treatment to ensure that the compressed air is dry and oilless, wherein the pressure of the compressed air is 0.7MPa; then placing the substrate in an ultrasonic cleaning machine for cleaning for 30min to remove surface adhesion impurities, wherein the parameters of ultrasonic cleaning are as follows: the cleaning temperature is 35 ℃, and the ultrasonic frequency is 20KHz; finally, placing the base material and the powder raw material at 120 ℃ for 2 hours for standby;
S3-2, uniformly coating the active auxiliary agent on the surface of the base material treated in the step S3-1, wherein the coating thickness of the active auxiliary agent is 0.2mm; the preparation process of the active auxiliary agent comprises the following steps: 30 parts by weight of SiO 2, 25 parts by weight of MnO, and 18 parts by weight of TiO 2 were weighed into a glass container, and 24 parts by weight of dimethyl ketone was added.
S4, laser cladding forming
And (3) placing the substrate obtained in the step (S3) into a printing bin of LDM-8060 laser cladding forming equipment, setting cladding parameter laser power to be 1100W, scanning speed to be 700mm/S, cladding overlap ratio to be 55%, powder feeding speed to be 0.5r/min, and scanning strategy to be single-channel reciprocating. And (3) introducing protective gas which is mixed gas of nitrogen and helium, wherein the mixing mass ratio is 2:5, namely 4 parts of nitrogen and 10 parts of helium, adding the dried refractory high-entropy alloy powder into a cleaned blower, and starting a starting procedure when the oxygen content is reduced to below 0.5%, so as to carry out cladding of the high-entropy alloy coating. The average friction coefficient of the finally obtained high-entropy alloy coating is between 0.5 and 0.7.
Example 4
A preparation process of a refractory high-entropy alloy coating resistant to high temperature friction and wear comprises the following steps:
s1, preparation of powder
Weighing the simple substance pure metals of 30.52% W, 18.68% Mo, 24.65% Ta24.65% Nb15.67% by mass, preparing refractory simple substance powder by a plasma rotary electrode atomization method, sieving the powder with the particle size of less than 50 mu m, and drying and preprocessing the powder;
the specific operation is as follows:
S1-1, machining all simple substance pure metals into bar stock by using a lathe;
s1-2, placing the bar blank obtained in the step S1-1 into atomization powder making equipment, vacuumizing, and when the vacuum degree in the atomization chamber is 5 multiplied by 10 -3 Pa, filling inert gas and metal salt powder into the atomization chamber, wherein the mass ratio of the inert gas to the metal salt powder is 1:4, 10 parts of inert gas and 40 parts of metal salt powder are taken, the inert gas is mixed gas of argon and helium, the mixed mass ratio of the argon is 67%, and the metal salt powder is NaCl powder;
S1-3: heating and melting the bar blank rotating at a high speed by using a plasma torch, and finally cooling the melted liquid drops to obtain refractory simple substance metal powder; wherein, the plasma arc current 1700A, the voltage is 150V, and the rotating speed of the metal electrode is 12500r/min.
S2, ball milling mixed powder
And (3) respectively taking 305.2gW, 186.8gMo, 246.5gTa and 156.7gNb simple substance powder prepared in the step (S1), putting the simple substance powder into a clean planetary ball mill, and then putting the simple substance powder into a steel ball for ball milling and powder mixing, wherein the ball-material ratio is 5:4, and the powder mixing time is 4h.
S3, substrate treatment
S3-1, polishing the surface of a substrate to be smooth by taking an Inconel 718 alloy plate as the substrate, removing greasy dirt on the surface of the substrate, and then performing sand blasting treatment, wherein the technological parameters of the abrasive are as follows: the grinding material is cast iron sand with the grain diameter of 0.5mm-1.5mm, and compressed air subjected to injection treatment is subjected to cooling and oil-water separation treatment to ensure that the compressed air is dry and oilless, wherein the pressure of the compressed air is 0.7MPa; then placing the substrate in an ultrasonic cleaning machine for cleaning for 30min to remove surface adhesion impurities, wherein the parameters of ultrasonic cleaning are as follows: the cleaning temperature is 38 ℃, and the ultrasonic frequency is 20KHz; finally, placing the base material and the powder raw material at 120 ℃ for 2 hours for standby;
s3-2, uniformly coating the active auxiliary agent on the surface of the base material treated in the step S3-1, wherein the coating thickness of the active auxiliary agent is 0.2mm; the preparation process of the active auxiliary agent comprises the following steps: 28 parts by weight of SiO 2, 24 parts by weight of MnO and 17 parts by weight of TiO 2 are weighed respectively and put into a glass container, and then 20 parts of dimethyl ketone is added.
S4, laser cladding forming
And (3) placing the substrate obtained in the step (S3) into a printing bin of LDM-8060 laser cladding forming equipment, setting cladding parameter laser power to be 1000W, scanning speed to be 600mm/S, cladding overlap ratio to be 60%, powder feeding speed to be 0.5r/min, and scanning strategy to be single-channel reciprocation. And (3) introducing protective gas which is mixed gas of nitrogen and helium, wherein the mixing mass ratio is 3:4, namely 3 parts of nitrogen and 4 parts of helium, adding the dried refractory high-entropy alloy powder into a cleaned blower, and starting a starting procedure when the oxygen content is reduced to below 0.5%, so as to carry out cladding of the high-entropy alloy coating. The average friction coefficient of the finally obtained high-entropy alloy coating is between 0.5 and 0.6.
The embodiment shows that the refractory high-entropy alloy coating with high-temperature friction and wear resistance prepared by the method can reach the requirements that the surface hardness is more than or equal to 1000HV, the coating wear rate is less than or equal to 1.0X10 -5mm3N-1m-1, and the coating bonding strength is more than or equal to 90N, namely, on the basis of fully ensuring the oxidation resistance and high-temperature resistance, the coating is well bonded with a base material, has a compact structure, ensures that the diameters of alloy metal particles are uniformly distributed under the condition that the laser cladding causes thermal stress in the coating, and does not accelerate movement among the particles, thereby ensuring that cracks are difficult to generate. And the produced refractory high-entropy alloy coating has the advantages of flat and smooth surface, low roughness and high forming quality, and can be put into industrial application. The preparation method provided by the invention utilizes plasma rotary electrode atomization and a laser cladding method to enable metal particles to be uniformly fused with each other, provides a new thought for preparing refractory high-entropy alloy coating resistant to high-temperature friction and abrasion, and has the advantages of simple process, high efficiency, high forming quality, high utilization rate of powder materials, excellent performances of formed parts and the like.
Meanwhile, the above embodiments are only for illustrating the technical scheme of the present invention, and are not limited thereto; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (2)
1. A preparation process of a refractory high-entropy alloy coating resistant to high temperature friction and wear is characterized by comprising the following steps:
s1, preparation of powder
Weighing 15.62-38.64% of W, 14.72-22.64% of Mo, 14.72-40.62% of Ta14.72-40.82% of Nb, and pure metals with the purity of more than or equal to 99.95% of each pure metal, preparing refractory simple substance powder by using a plasma rotary electrode atomization method, sieving the powder, and drying and pre-treating the powder;
S2, ball milling mixed powder
Placing the refractory simple substance powder after the drying pretreatment in a planetary ball mill, and ball milling to obtain a required refractory high-entropy alloy powder raw material;
S3, substrate treatment
S3-1, polishing the surface of the substrate to be smooth, removing oil stains on the surface of the substrate, performing sand blasting treatment, cleaning the substrate in an ultrasonic cleaner for 30min to remove surface adhesion impurities, and finally drying in a blast drying oven at 120-250 ℃ for 1-2h for later use;
s3-2, uniformly coating a reactive auxiliary agent on the surface of the base material treated in the step S3-1, wherein the coating thickness of the reactive auxiliary agent is 0.2-0.4mm;
S4, laser cladding forming
The refractory high-entropy alloy powder obtained in the step S2 is laser-clad on the substrate obtained in the step S3 to form a refractory high-entropy alloy coating resistant to high-temperature friction and abrasion; wherein the laser power is 800-1500W, the light spot diameter is 1mm, the scanning speed is 600-1500mm/s, the cladding overlap ratio is 50-60%, the powder feeding speed is 0.2-0.5r/min, and the gas flow of the shielding gas is 3-5L/min;
In the step S1, 2.4 to 6.8 mass percent of V simple substance pure metal is also weighed, and the purity of the V simple substance pure metal is more than or equal to 99.95 percent;
The specific steps of the step S1 are as follows:
S1-1, machining all simple substance pure metals into bar stock by using a lathe;
S1-2, placing the bar blank obtained in the step S1-1 into atomization powder making equipment, vacuumizing, and when the vacuum degree in the atomization chamber is 5 multiplied by 10 -3 Pa, filling inert gas and metal salt powder mixture into the atomization chamber, wherein the inert gas is mixed gas of argon and helium, and the metal salt powder is NaCl powder;
s1-3: heating and melting the bar blank rotating at a high speed by using a plasma torch, and finally cooling the melted liquid drops to obtain refractory simple substance metal powder; wherein, the plasma arc current is 1200-1800A, the voltage is 120-180V, and the rotating speed of the metal electrode is 10000-15000r/min;
The particle size of each refractory simple substance metal is 28-73 mu m after being dried for 2 hours by a blast drying heating furnace at 110 ℃ in the step S1, and the powder flowability is 19.07S/50g;
in the step S2, the ball-material ratio in the ball milling process is 5:4, and the ball milling and powder mixing time is 4 hours;
The material of the base material in the step S3 is Ni-based superalloy;
Before the refractory high-entropy alloy coating is clad, the printing bin is required to be filled with protective gas, wherein the protective gas is mixed gas of nitrogen and helium, and the oxygen content of air is ensured to be less than or equal to 0.5%.
2. The process for preparing a refractory high-entropy alloy coating resistant to high temperature frictional wear as set forth in claim 1, wherein said S3-2 coagent comprises SiO 2: 25-30 parts of MnO:20-25 parts of TiO 2: 15-18 parts; the preparation method of the active auxiliary agent comprises the following steps: and (3) respectively weighing the SiO 2、MnO、TiO2 in parts by weight, putting into a glass container, then adding 18-24 parts of dimethyl ketone, and uniformly stirring.
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