CN116752099B - NiTiAl-X multi-element alloy coating and preparation method and application thereof - Google Patents
NiTiAl-X multi-element alloy coating and preparation method and application thereof Download PDFInfo
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Classifications
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
Abstract
The application relates to the technical field of metal coatings, in particular to a NiTiAl-X multi-element alloy coating, and a preparation method and application thereof. The coating is made of a NiTiAl-X quaternary alloy material, wherein X is one of transition group metals Nb, mo, cu or V, and the atomic ratio of Ni, ti, al, X in the coating material is as follows: 45-50:45-50:0.5-4:0.5-4. The preparation method of the coating comprises the steps of preparing a NiTiAl-X multi-element alloy cast ingot by adopting a vacuum arc melting technology, and forming the NiTiAl-X multi-element alloy coating on a substrate by adopting a magnetron sputtering method based on an alloy target. The NiTiAl-X multi-element alloy coating prepared by the method has high cavitation erosion resistance and erosion resistance, has excellent cavitation erosion resistance and erosion resistance, can be applied to the fields of ocean, ships, transportation, nuclear power and the like, and effectively prolongs the service life of high-pressure pipelines, propellers, water turbines and other overcurrent components.
Description
Technical Field
The application relates to the technical field of metal coatings, in particular to a NiTiAl-X multi-element alloy coating and a preparation method and application thereof.
Background
The over-current components such as the propeller of the marine vessel, the runner blades, the guide blades, the top ring and the bottom ring bushings and the like can be seriously damaged due to cavitation erosion and mortar erosion and the combined action of the cavitation erosion and the mortar erosion when running in the sandy water flow. Therefore, the adoption of proper surface engineering technology to strengthen cavitation erosion resistance and erosion resistance of the overcurrent element is a key for prolonging the service life of the overcurrent element.
Cavitation is also called cavitation, and the principle is that when liquid flows, the pressure of a local area suddenly drops under the condition that the temperature is basically kept unchanged to form bubbles, the bubbles suddenly collapse from a low pressure area to a high pressure area, and high-speed jet flow generated after the collapse of the bubbles continuously impacts the surface of a material, so that the material of a flow passing component is damaged and even the surface is eroded. Erosion of silt is a hydrodynamic abrasive wear. The sand-containing water flow can generate huge impact force on the water turbine running at high speed, and solid particles in the water can collide with and cut the flow channel, so that the surface of the overflow part is worn.
At present, a method for preparing a coating on an overflow part such as a water turbine is often adopted at home and abroad to improve cavitation erosion resistance and erosion resistance. The common coatings are metal coatings and nonmetal coatings according to the material distinction. Non-metallic coatings such as epoxy resin and polyurethane have low cost and simple process, but have the problems of low bonding strength with a matrix, easy flaking under long-term pulsating negative pressure in a strong cavitation zone, and the like. The metal coating mainly adopts a thermal spraying process, a build-up welding and a laser cladding technology: the thermal spraying metal ceramic coating, the matrix and the ceramic powder particles are mainly mechanically combined, and pores exist in the tissues, so that the combination strength is not high; the surfacing process has the problems that the thickness of a welding layer is uneven, a fusion area becomes brittle, cracks are easy to generate and the like, the machining allowance is large, and the requirement on the weldability of a base material is high; the laser cladding coating has high bonding strength, uniform structure and excellent abrasion resistance, but the problem of easy crack occurrence in the cladding process still exists.
In the metal coating, the NiTi alloy has good super-elasticity and shape memory effect, can absorb huge energy generated when cavitation bubbles collapse, and has excellent cavitation erosion resistance. But NiTi alloys have lower hardness, resulting in poor wear resistance. Therefore, the alloy element can be used for strengthening the NiTi matrix phase to prepare the composite coating material with cavitation erosion resistance and abrasion resistance.
Disclosure of Invention
Related researches show that when the NiTi coating added with the alloy element is in a martensitic state, the comprehensive corrosion resistance is better. Al is added into the NiTi alloy, and the NiTiAl alloy has higher yield strength and certain elasticity while retaining the shape memory effect. This is because the martensitic transformation temperature point of NiTi alloy is greatly reduced after adding Al element, and the addition of a small amount of Al can make it in the martensitic state at room temperature. In cavitation erosion, the local pressure generated by bubble collapse can reach 1.2GPa, and the high pressure can induce the formation of martensite twin crystals in NiTi phase, thereby absorbing energy and reducing the damage to the alloy surface. The NiTiAl alloy can withstand cyclic stresses of up to 1.7GPa under compression, exhibiting recoverable elastic strain exceeding 5%. Therefore, the NiTiAl alloy has cavitation erosion resistance and abrasion resistance, and has certain application potential in cavitation erosion resistance field. However, due to the high price of NiTi series alloy and poor cold workability, niTiAl alloy has the problems of grain boundary precipitation phase and element segregation, and the like, and has no application in cavitation erosion resistance and erosion abrasion resistance on the surfaces of propeller and turbine flow passage components at present. The adoption of the coating material can relieve the problems of high price, difficult processing and the like of the block material to a certain extent, and the overall performance of the coating material can be further regulated and controlled by adding alloy elements, so that the problems of segregation, inclusion and the like in the material are reduced to a certain extent.
In view of the above, a first object of the present application is to provide a NiTiAl-X multi-element alloy coating having cavitation erosion resistance and erosion resistance, which has excellent cavitation erosion resistance and erosion resistance, and can be applied to the fields of ocean, ship, transportation, nuclear power, etc., and effectively improves the service life of overcurrent components such as high-pressure pipelines, propellers, water turbines, etc.
The second object of the application is to optimize the coating preparation process based on the coating, and provide a method for preparing the NiTiAl-X multi-element alloy coating.
In order to achieve the above purpose, the present application adopts the following technical scheme:
in a first aspect, the application provides a NiTiAl-X multi-element alloy coating, which improves a cavitation erosion resistant coating of a NiTi alloy in the related art, and plays a role of solid solution strengthening by adding 0.5-4at.% of Al element, so that the wear resistance and the yield strength of the coating are enhanced. Furthermore, the microstructure of the material is regulated and controlled by adding transition elements Nb, mo, cu or V on the basis of the NiTiAl alloy, so that the fatigue damage of the coating caused by a grain boundary precipitation phase of the NiTiAl alloy coating is improved, and meanwhile, the binding force between the coating and a matrix is improved, so that the cavitation erosion resistance and the erosion resistance of the alloy are further improved.
Specifically, the NiTiAl-X multi-element alloy coating is made of a NiTiAl-X quaternary alloy material, wherein X is selected from one of transition group metals Nb, mo, cu or V, and the atomic ratio of Ni, ti, al, X in the coating is as follows: 45-50:45-50:0.5-4:0.5-4.
Preferably, when Nb is used as the X element, ni: ti: al: nb=47.5 to 50:45 to 47.5:1 to 3:2 to 4; when Mo is selected as the X element, ni: ti: al: mo=45 to 47:47 to 50:4:1 to 4; when the element X is Cu, ni: ti: al: cu=45-50:45-50:1-2:3-4; when the X element is V, ni: ti: al: v=47.5-49.5:47.5-48.5:0.5-2.5:0.5-2.5.
In a second aspect, the application provides a preparation method of the NiTiAl-X multi-element alloy coating in the first aspect, wherein an ingot of the NiTiAl-X multi-element alloy is prepared by an alloy smelting technology, a target is obtained by cutting the ingot, and then the target is deposited on the surface of a base material by a magnetron sputtering technology to obtain the NiTiAl-X multi-element alloy coating.
Specifically, the preparation method comprises the following steps:
(1) Preparing a NiTiAl-X multi-element alloy cast ingot:
preparing an atomic ratio of Ni by adopting a Ti source, a Ni source, an Al source and a pure X source with purity of more than 99 wt%: ti: al: x=45-50:45-50:0.5-4:0.5-4 NiTiAl-X multi-element alloy cast ingot; the reason for adopting the high-purity Ti, ni, al, X source is to reduce the influence of impurities in the alloy on cavitation erosion resistance and erosion resistance of the coating and improve the density of the sputtered coating.
(2) Preparing a magnetron sputtering target:
taking the NiTiAl-X multi-element alloy cast ingot obtained in the step (1) as a raw material, and cutting and processing to obtain a NiTiAl-X alloy target; preferably, the NiTiAl-X alloy target material can be obtained by cutting from a NiTiAl-X multi-element alloy cast ingot by adopting wire-cut electrical discharge machining, and the reason for adopting the wire-cut electrical discharge machining is that the knife edge of the target material after machining is very small, so that the material utilization rate is greatly improved, and the material cost is reduced.
(3) Preparing a NiTiAl-X multi-element alloy coating:
and (3) using the NiTiAl-X alloy target material obtained in the step (2) to deposit a NiTiAl-X multi-element alloy coating on the substrate by using a magnetron sputtering device.
Preferably, in the step (1), the NiTiAl-X multi-element alloy ingots are prepared by vacuum arc melting technology, and each alloy ingot needs to be turned over and melted at least four times to obtain an alloy ingot with uniform composition and microstructure. The reason for preparing the alloy cast ingot by adopting the vacuum arc melting technology is that the prepared alloy cast ingot has uniform components, no oxidation, less pollutants and short preparation time.
Preferably, the surface of the substrate used in step (3) is cleaned and sandblasted before the coating is prepared to enhance the bonding force between the coating and the substrate.
Preferably, in the step (3), the substrate pressure during the magnetron sputtering is 5×10 -6 Pa, the deposition pressure was fixed at 5.0X10 by controlling the flow rate of argon gas in the deposition chamber -1 Pa; the deposition power of the NiTiAl-X multi-element alloy coating is 1000W, and the sputtering time is 5-6 hours; the substrate temperature was maintained at 600 ℃ during sputtering, and furnace cooled to 150 ℃ after sputtering was completed. The magnetron sputtering parameters are set because the components of the coating tissue prepared by the parameters are uniform and compact, the bonding property is good, and the coating is not easy to crack. The coating has moderate thickness, and cavitation erosion resistance and erosion performance reduction caused by insufficient thickness are avoided.
In a third aspect, the present application provides a use of the NiTiAl-X multi-element alloy coating of the first aspect described above in an overcurrent element.
The beneficial effects of the application are as follows:
(1) Compared with the prior art, the NiTiAl-X multi-element alloy coating has good cavitation erosion resistance and erosion resistance, and under the standard cavitation erosion and erosion test conditions, the average cavitation erosion speed can be as low as 0.2 MDE/mu m and the average erosion speed can be as low as 1.3 MDE/mu m; meanwhile, the NiTiAl-X coating provided by the application also has higher wear resistance, high compressive strength and high corrosion resistance, and is particularly suitable for overcurrent components;
(2) The NiTiAl-X coating prepared by the magnetron sputtering technology has high bonding strength with a matrix material, is not easy to separate from the matrix, has uniform thickness, and has no pores or cracks;
(3) In addition, compared with the high-hardness ceramic phase particle reinforced NiTi matrix phase composite coating, the NiTiAl-X coating provided by the application has the advantages of simpler process and more stable components.
Drawings
FIG. 1 is a schematic diagram showing the structure of an ASTM G32-10 standard cavitation test apparatus in accordance with an embodiment of the present application;
FIG. 2 shows Ni according to example 1 of the present application 50 Ti 45 Al 2 Cu 3 SEM micrograph of the coating;
FIG. 3 shows Ni according to example 2 of the present application 48.5 Ti 48.5 Al 2.5 V 0.5 SEM micrograph of the coating;
FIG. 4 shows Ni according to example 3 of the present application 50 Ti 45 Al 3 Nb 2 SEM micrograph of the coating;
FIG. 5 shows Ni according to example 4 of the present application 45 Ti 48 Al 4 Mo 3 A cross-sectional SEM micrograph of the coating;
reference numerals:
1. a power supply; 2. a thermostat device; 3. an ultrasonic generator; 4. testing the sample; 5. testing the liquid; 6. and a supporting device.
Detailed Description
The present application will be described in further detail below in order to make the objects, technical solutions and advantages of the present application more apparent. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In industrial production, transition group metals are often used as alloying elements to improve the physicochemical properties of the original metal. In the cavitation erosion and erosion fields, related researches prove that the cavitation erosion resistance and erosion resistance of the NiTi alloy after the NiTi alloy is added with alloy elements are better. According to the application, on the basis of the NiTi alloy, the wear resistance of the material is improved by adding a proper amount of Al, the bonding strength of the microstructure of the material and the coating is regulated and controlled by adding transition elements Nb, mo, cu or V, and on the basis, the optimal design of the coating preparation process is carried out, so that the NiTiAl-X alloy coating with good cavitation erosion resistance is prepared.
The scheme of the present application will be explained below with reference to examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the present application and should not be construed as limiting the scope of the application. The specific techniques or conditions are not identified herein and are carried out according to conditions or techniques common in the art.
Example 1
Example 1 six different atomic ratios of NiTiAl-Cu coatings were prepared, the atomic ratios of the six different component coatings being: ni (Ni) 45 Ti 50 Al 1 Cu 4 ，Ni 47.5 Ti 47.5 Al 1 Cu 4 ，Ni 50 Ti 45 Al 1 Cu 4 ，Ni 45 Ti 50 Al 2 Cu 3 ，Ni 47.5 Ti 47.5 Al 2 Cu 3 ，Ni 50 Ti 45 Al 2 Cu 3 . In addition, the component Ni is also prepared 50 Ti 45 Al 0.5 Cu 4.5 With Ni 50 Ti 45 Al 3 Cu 2 As comparative example 1.
The following is made of Ni 50 Ti 45 Al 2 Cu 3 The components are examples, and the preparation method of the NiTiAl-Cu alloy coating is briefly described. The procedure not specifically described is applicable to the other components in this example/comparative example. The specific method comprises the following steps:
(1) Early preparation: the 30×30×6 304 stainless steel is cut as a substrate, and the substrate surface is cleaned and sandblasted to facilitate subsequent coating bonding.
(2) Preparing an alloy ingot: adopts high-purity titanium sponge (pure)Degree 99.76 wt%), high purity nickel mass (purity 99.95 wt%), high purity aluminum (purity 99.99 wt%), and purity 99.9wt.% or more Cu production atomic ratio of 50:45:2:3 NiTiAl-Cu alloy ingot. Alloy ingots were prepared by arc melting technique on a water-cooled copper crucible in an Ar atmosphere, and the furnace chamber was evacuated to 3X 10 -3 Pa, then backfilled with high purity Ar gas (99.99 wt%) to a pressure of 0.05 MPa. Each alloy ingot was flipped and melted four times to obtain a homogeneous NiTiAl-Cu alloy ingot of composition and microstructure.
(3) Preparing a target: a NiTiAl-Cu alloy ingot is used as a raw material, and a target material with the size of 101.6 (diameter) multiplied by 5mm (thickness) is cut from the alloy ingot by adopting wire electric discharge machining.
(4) And (3) preparing a coating: and taking the cut NiTiAl-Cu alloy cast ingot as a target material, and depositing on a substrate by using M600 magnetron sputtering equipment to obtain the NiTiAl-Cu film. The base pressure was 5X 10 -6 Pa, the pressure of the deposition process is fixed to 5.0X10 by controlling the flow of argon in the deposition chamber -1 Pa. In the magnetron sputtering deposition process, the deposition power of the NiTiAl-Cu film is 1000W, and the sputtering time is 5.5 hours. The temperature of the substrate is kept at 600 ℃ in the sputtering process, and after the sputtering is finished, the substrate is cooled to 150 ℃ along with a furnace, and a sample is taken out. The coating obtained had a target thickness of 15. Mu.m
(5) Performance test: the quality of the bond of the coating to the substrate was measured using SEM microscopy. And (3) measuring cavitation erosion accumulated mass loss of the sample after carrying out cavitation erosion experiments on the prepared sample for 2 hours by adopting a standard cavitation erosion tester. Referring to FIG. 1, a schematic structure of an ASTM G32-10 cavitation test apparatus includes 1, a power source; 2. a thermostat device; 3. an ultrasonic generator; 4. testing the sample; 5. testing the liquid; 6. and a supporting device. The test principle is as follows: the acoustic energy of the ultrasonic generator 3 is converted into mechanical vibration waves, and the liquid at the solid-liquid contact surface vibrates at a high speed, so that the hydrostatic pressure at the solid-liquid contact surface is reduced at a certain moment, and the liquid rapidly impacts the surface of the sample in a micro-jet manner, thereby causing controllable cavitation damage to the surface of the sample. The average erosion rate MDE is defined as the cavitation cumulative mass loss divided by the product of cavitation area and material density, i.e. A circular area with a radius of 8mm is taken as a cavitation area in the cavitation generation device probe as a center. The liquid/solid washout test was performed according to ASTM G73-10 standard test method. In the liquid-solid erosion test, a high-speed water jet of 100m/s was emitted from a nozzle of 4mm diameter, and a sample 15mm from the nozzle was impacted vertically, and the impact area of the sample was about 25 mm. The test results are shown in Table 1.
TABLE 1 results of Performance test of each coating in example 1/comparative example 1
Example 1/comparative example 1a NiTiAl-Cu alloy coating was prepared using a magnetron sputter deposition technique, the average thickness of the NiTiAl-Cu coating being 14.7 μm. FIG. 2 is Ni in the present embodiment 50 Ti 45 Al 2 Cu 3 A photomicrograph of the coating. The matrix structure of the coating is NiTi phase with Al dissolved therein and a small amount of Ti 2 And Ni phase. In addition, it was also observed that white lump and short rod-like Ni precipitated 3 Ti phase, and gray blocky copper-rich Ti (Ni, cu) 2 And (3) phase (C). At a lower copper content, cu element tends to precipitate in the precipitate phase. In NiTi alloy, cu can improve the plasticity of the coating, reduce the friction between lattice interfaces, and also reduce the sensitivity of the phase transition temperature of the NiTi alloy along with the change of the atomic ratio of the NiTi. Furthermore, the addition of Cu element reduces the tendency of Al element to segregate at grain boundaries. The Cu element can also reduce the diffusivity of Fe element, thereby reducing the influence of Fe element in 304 stainless steel on the NiTi coating.
For NiTiAl-Cu coating, cavitation erosion resistance and erosion resistance of all sample coating are improved to a certain extent compared with 304 stainless steel substrate, wherein Ni is used 50 Ti 45 Al 2 Cu 3 The alloy coating of the composition is optimal.
According to the test result of the applicant, when the content of Al element in the material is less than or equal to 2at.% and the content of Cu is 3-4.5 at.%, the cavitation erosion resistance and the erosion resistance of the NiTiAl-Cu coating are better, because a small amount of Cu element can improve the plasticity of the coating, reduce the tendency of segregation of Al element at the grain boundary and coordinate the deformation of crystal grains on the surface of the coating under cavitation erosion. When the Cu content in the material is more than 4.5 at%, cavitation erosion resistance and erosion resistance of the coating are deteriorated, because excessive Cu element interacts with Al element to increase the volume of a precipitated phase, and large precipitated phase causes local stress concentration, so that the mechanical property of the NiTiAl alloy is reduced. The test results of comparative example 1 and comparative example 1, the present application controls the Al content in the NiTiAl-Cu coating material to be between 1 and 2at.% and the Cu content to be between 3 and 4 at.%.
Example 2
Example 2 six different atomic ratios of NiTiAl-V coatings were prepared, the atomic ratios of the six different component coatings being: ni (Ni) 47.5 Ti 47.5 Al 2.5 V 2.5 ，Ni 48.5 Ti 48.5 Al 1.5 V 1.5 ，Ni 48.5 Ti 48.5 Al 2.5 V 0.5 ，Ni 48.5 Ti 48.5 Al 0.5 V 2.5 ，Ni 48.5 Ti 47.5 Al 2.5 V 1.5 ，Ni 49.5 Ti 47.5 Al 2.5 V 0.5 . In addition, the component Ni is also prepared 46.5 Ti 47.5 Al 2.5 V 3.5 ，Ni 46.5 Ti 48.5 Al 1.5 V 3.5 ，Ni 46.5 Ti 49.5 Al 0.5 V 3.5 As comparative example 2.
The specific preparation and performance test methods were identical to those of example 1, and the results of the performance test for the nine coatings are shown in Table 2.
TABLE 2 results of Performance test of each coating in example 2/comparative example 2
Example 2 and comparative example 2a NiTiAl-V alloy coating was prepared using magnetron sputtering techniques under an inert atmosphere, the average thickness of the NiTiAl-V coating being 15.2 μm. The matrix structure of the coating is NiTi phase, and as the V element is increased, the crystal grains of the coating are slightly refined, and the toughness of the coating is increased. The morphology of the tissue at a V content of 0.5at.% is shown in fig. 3. The coating shows B19' phase and Ti 2 The Ni phase, V is solid-dissolved in the B19' phase, and the positions of Ni atoms are replaced, thereby achieving the effect of solid-solution strengthening. When the V content is more than 0.5 at%, the coating is B19' phase, ti 2 Ni phase and softer V precipitated at grain boundaries 9 (Ni, ti) phase, and as the V content increases, the V-rich phase becomes more and more concentrated at grain boundaries, resulting in a decrease in the wear resistance of the coating. The precipitation of the second phase at the grain boundary can lead to the reduction of the binding force of the grain boundary, and surface grains are easily stripped in the cavitation erosion process, so that cavitation erosion is aggravated. In combination with the results of the tests of the coatings in example 2 and comparative example 2, the present application controls the V content in the NiTiAl-V coating material to be between 0.5 and 2.5 at.%.
For NiTiAl-V coating, cavitation erosion resistance and erosion resistance of all sample coating are improved to a certain extent compared with 304 stainless steel substrate, wherein Ni is used 48.5 Ti 48.5 Al 2.5 V 0.5 Optimally.
Example 3
Example 3 six different atomic ratios of NiTiAl-Nb coatings were prepared, the atomic ratios of the six different component coatings were: ni (Ni) 50 Ti 45 Al 1 Nb 4 ，Ni 50 Ti 45 Al 2 Nb 3 ，Ni 50 Ti 45 Al 3 Nb 2 ， Ni 47.5 Ti 47.5 Al 2 Nb 3 ，Ni 47.5 Ti 47.5 Al 1 Nb 4 , Ni 47.5 Ti 47.5 Al 3 Nb 2 . In addition, the component Ni is also prepared 45 Ti 50 Al 2 Nb 3 As comparative example 3.
The following is made of Ni 47.5 Ti 47.5 Al 3 Nb 2 The composition is exemplified by a method for coating a NiTiAl-Nb alloy. The procedure not specifically described is applicable to the other components in this example/comparative example. The specific method comprises the following steps:
(1) Early preparation: the 30×30×6 304 stainless steel is cut as a substrate, and the substrate surface is cleaned and sandblasted to facilitate subsequent coating bonding.
(2) Preparing an alloy ingot: the atomic ratio of Nb prepared from high purity titanium sponge (99.76 wt%), high purity nickel block (99.95 wt%), high purity aluminum (99.99 wt%) and purity of 99.9wt.% or more was 47.5:47.5:3: 2. Alloy ingots were prepared by arc melting technique on a water-cooled copper crucible in an Ar atmosphere, and the furnace chamber was evacuated to 3X 10 -3 Pa, then backfilled with high purity Ar gas (99.99 wt%) to a pressure of 0.05 MPa. Each alloy ingot was flipped and melted four times to obtain a homogeneous alloy ingot of composition and microstructure.
(3) Preparing a target: a NiTiAl-Nb alloy ingot is taken as a raw material, and a target material with the size of 101.6 (diameter) multiplied by 5mm (thickness) is cut from the alloy ingot by adopting wire electric discharge machining.
(4) And (3) preparing a coating: and taking the cut NiTiAl-Nb alloy cast ingot as a target material, and depositing a NiTiAl-Nb film on the substrate by using M600 magnetron sputtering equipment. The base pressure was 5X 10 -6 Pa, the pressure of the deposition process is fixed to 5.0X10 by controlling the flow of argon in the deposition chamber -1 Pa. In the magnetron sputtering deposition process, the deposition power of the NiTiAl-Nb film is 1000W, and the sputtering time is 6 hours. The temperature of the substrate is kept at 600 ℃ in the sputtering process, and after the sputtering is finished, the substrate is cooled to 150 ℃ along with a furnace, and a sample is taken out. The coating obtained had a target thickness of 17. Mu.m.
(5) The performance test method was identical to that of example 1. The test results are shown in Table 3.
TABLE 3 results of Performance test of each coating in example 3 and comparative example 3
The above examples and comparative examples used a NiTiAl-Nb alloy coating prepared by magnetron sputtering deposition technique, and the average thickness of the NiTiAl-Nb coating was 16.2. Mu.m. The addition of Nb increases the precipitation phases of NiTi (Al, nb) in the coating, and the yield strength of the coating can be greatly improved due to the solid solution strengthening effect brought by the dispersed fine precipitation phases.
FIG. 4 is Ni 50 Ti 45 Al 3 Nb 2 SEM micrograph of magnetron sputtered film. Dark grey TiNi matrix and precipitated white TiNi (Al, nb) phases and black Ti are observed in the alloy containing 2at.% Nb 2 And Ni phase. TiNi (Al, nb) and Nb-rich Ti with increasing Nb content 2 The number of Ni phases increases and the number of TiNi matrices decreases. Excessive precipitation has a negative effect on cavitation resistance of the coating, as a large amount of the second phase can cause stress concentration, leading to tip crack generation and subsequent spalling of the coating tissue. For Ni-rich NiTi alloy, nb has solid solution strengthening effect and promotes Ni 2 The TiAl phase is dispersed and separated out, so that the coating strength is improved. For NiTi alloy with equal atomic ratio, nb can be biased and precipitate Gao Jiangfu Nb phase in the alloy, so that the coating strength is increased, and the erosion resistance is improved. While for Ti-rich NiTi alloys, nb addition, although increasing the room temperature yield strength to some extent, reduces the solubility of Ti in the matrix, resulting in coarse Ti 2 Ni precipitates in the crystal, and the cavitation resistance of the material is deteriorated. By combining the test result of the coating in comparative example 3, the content of Ni and Ti in the NiTiAl-Nb coating material is controlled between 47.5 and 50:45 and 47.5, so that the Ni/Ti ratio is more than or equal to 1, and the content of Nb is controlled between 2 and 4at percent.
Example 4
Example 4 six different atomic ratios of NiTiAl-Mo coatings were prepared, the atomic ratios of the six different component coatings being: ni (Ni) 45 Ti 50 Al 4 Mo 1 ，Ni 45 Ti 49 Al 4 Mo 2 ，Ni 45 Ti 48 Al 4 Mo 3 ，Ni 45 Ti 47 Al 4 Mo 4 ，Ni 46 Ti 48 Al 4 Mo 2 ，Ni 47 Ti 47 Al 4 Mo 2 . In addition, the component Ni is also prepared 50 Ti 45 Al 4 Mo 1 ，Ni 49 Ti 45 Al 4 Mo 2 ，Ni 48 Ti 45 Al 4 Mo 3 ，Ni 47 Ti 45 Al 4 Mo 4 As comparative example 4.
The specific preparation method and the performance test method are the same as in example 3. The test results are shown in Table 4.
TABLE 4 results of Performance test of each coating in example 4/comparative example 4
FIG. 5 is Ni in the present embodiment 45 Ti 48 Al 4 Mo 3 The cross-section SEM micrograph of the coating shows that the coating bonds well to the cross-section. The average thickness of the NiTiAl-Mo coating was 15.8 μm. When the Mo content is 1 at%, the coating matrix structure is NiTi phase, and the coating matrix structure is less than Ti at the grain boundary 2 And Ni phase. As the Mo content increases, a fine granular white phase is precipitated at the grain boundary. When the Ni/Ti ratio in the coating material is smaller than 1, the Al atoms in the coating preferentially occupy Ti positions, so that the NiTi matrix has redundant Ti atoms, ti and Mo form stable Ti-Mo bonds, thereby facilitating the solid solution of the Mo element, and the solid solution strengthening effect is optimal; when the Ni/Ti ratio in the coating material is more than 1, the solid solution strengthening effect of Mo element is greatly reduced, and when the Mo content is more than 3 at%, a Mo-rich phase with larger size is precipitated in the coating matrix, which is unfavorable for cavitation erosion resistance of the coating. Therefore, in the present application, the content of Ni and Ti in the NiTiAl-Mo coating is controlled to be 45-47:47-50 by combining the test results of example 4 and comparative example 4, so that the Ni/Ti ratio is ensured to be less than or equal to 1, and the content of Mo is controlled to be 1-4at%.
Comparative example 5
NiTi coating: reference to the coating preparation method of example 3, the preparation component was Ni 47 Ti 53 ，Ni 50 Ti 50 ，Ni 53 Ti 47 As a comparative example of the NiTiAl-X alloy coating according to the application. After 6h magnetron sputtering, the average thickness of the NiTi coating was 16.4 μm. In standard cavitation erosion test experiments, ni 53 Ti 47 The coating is coated more seriouslyThe layer cracks, resulting in a large area of spalling of the coating. Ni (Ni) 47 Ti 53 With Ni 50 Ti 50 The coating had a locally weak bond, but the coating did not crack in the standard cavitation and erosion test experiments. Ni (Ni) 47 Ti 53 With Ni 50 Ti 50 The results of the standard cavitation erosion test of the coating are set forth in the following table.
TABLE 5 results of Performance test of each coating in comparative example 5
Comparative example 6
NiTiAl coating (Al between 0.5-4 at.%): with reference to the coating preparation method of example 3, a coating having a composition of Ni was prepared 49.75 Ti 49.75 Al 0.5 ，Ni 49.5 Ti 49.5 Al 1 ，Ni 49 Ti 49 Al 2 ，Ni 48 Ti 48 Al 4 As a comparative example of the NiTiAl-X alloy coating according to the present application. After 6h of magnetron sputtering, the average thickness of the NiTiAl coating is 16.1 μm. With the addition of Al element, the martensite twin crystal content of the NiTi alloy coating is increased, and the wear resistance of the coating is increased. When the Al content is less than 2 at%, the Al element is solid-dissolved in the NiTi matrix; when the Al content is 2-4at%, a small amount of Ti which is dispersed and distributed is precipitated in the coating 2 And an Al strengthening phase. The addition of Al element effectively improves the erosion resistance of the NiTi coating. Ni (Ni) 49.75 Ti 49.75 Al 0.5 ，Ni 49.5 Ti 49.5 Al 1 ，Ni 49 Ti 49 Al 2 With Ni 48 Ti 48 Al 4 The results of the erosion test experiments on the coatings are listed in the following table.
TABLE 6 results of Performance test of each coating in comparative example 6
Comparative example 7
NiTiAl coating (Al < 0.5 at.%): reference toThe coating preparation method of example 3, prepared with Ni as the constituent 49.9 Ti 49.9 Al 0.2 As a comparative example of the NiTiAl-X alloy coating according to the present application. Because the Al content is too low, the Al element is completely dissolved in the NiTi coating matrix, and the cavitation erosion resistance and the erosion resistance of the NiTi coating matrix are as follows 50 Ti 50 The alloy is not very different.
Comparative example 8
NiTiAl coating (Al > 4at%): with reference to the coating preparation method of example 3, a coating having a composition of Ni was prepared 47 Ti 47 Al 6 With Ni 46 Ti 46 Al 8 As a comparative example of the NiTiAl-X alloy coating according to the present application. After 6h of magnetron sputtering, the average thickness of the NiTiAl coating is 16.5 μm. With the addition of a large amount of Al element, the hardness of the NiTiAl coating is obviously increased, but the toughness of the coating is reduced. In addition, a large amount of precipitated phases containing Al are also observed at the grain boundary of the coating, and the precipitated phases can become cavitation erosion crack sources in the cavitation erosion process, so that the coating grains fall off, and the cavitation erosion resistance of the coating is reduced. The component is Ni 47 Ti 47 Al 6 With Ni 46 Ti 46 Al 8 The NiTiAl alloy coating has the condition of coating breakage in standard cavitation experiments.
As can be seen from the combination of comparative examples 5 and 6, by adding Al to NiTi alloy, the hardness and wear resistance of the coating can be suitably improved; further combining comparative examples 6-8, it is possible to obtain, when the Al content in the NiTiAl alloy is less than 0.5at.%, the Al content is very small and completely solid-dissolved in the NiTi matrix, the NiTiAl coating properties are not much different from the NiTi coating properties; when the Al content in the NiTiAl alloy is more than 4 at%, the hardness of the coating is obviously increased, the toughness is reduced, and the grain boundary precipitation phase is increased, so that the cavitation erosion resistance of the coating is deteriorated. In connection with the above analysis, the present application controls the Al content in the coating material to be between 0.5 and 4 at.%.
In addition, compared with a TIG method, the coating prepared by the magnetron sputtering method has the characteristics of being more compact, obviously reducing inclusions and holes, and having better cavitation erosion resistance and erosion resistance; compared with vacuum plasma spraying and laser remelting treatment, the prepared coating is lower in cost and simpler in process. The coating alloy component is also suitable for being prepared by a plasma spraying method.
The foregoing description is only illustrative of the present application and is not intended to limit the scope of the application, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present application.
Claims (9)
1. A NiTiAl-X multi-element alloy coating, wherein the coating is made of a NiTiAl-X quaternary alloy material, wherein X is selected from one of transition group metals Nb, mo, cu or V, and the atomic ratio of Ni, ti, al, X in the coating is: 45-50:45-50:0.5-4:0.5-4; under standard cavitation erosion and erosion test conditions, the cavitation erosion average erosion speed of the coating is less than or equal to 12.7 MDE/mu m, and the erosion average erosion speed is less than or equal to 9.9 MDE/mu m;
the preparation method of the coating comprises the following steps: (1) preparation of NiTiAl-X multi-element alloy cast ingot: preparing an atomic ratio of a Ti source, a Ni source, an Al source and an X source with purity of more than 99wt.% into Ni: ti: al: x=45-50:45-50:0.5-4:0.5-4 NiTiAl-X multi-element alloy cast ingot; (2) preparation of a magnetron sputtering target material: taking the NiTiAl-X multi-element alloy cast ingot obtained in the step (1) as a raw material, and cutting and processing to obtain a NiTiAl-X alloy target; (3) preparation of NiTiAl-X multi-element alloy coating: and (3) using the NiTiAl-X alloy target material obtained in the step (2) to deposit a NiTiAl-X multi-element alloy coating on the substrate by using a magnetron sputtering device.
2. The NiTiAl-X multi-element alloy coating according to claim 1, wherein when Nb is selected for X, ni: ti: al: nb=47.5-50:45-47.5:1-3:2-4, and the ratio of Ni/Ti is more than or equal to 1; under standard cavitation erosion and erosion test conditions, the cavitation erosion average erosion speed of the coating is less than or equal to 11.1 MDE/mu m, and the erosion average erosion speed is less than or equal to 9.9 MDE/mu m.
3. The NiTiAl-X multi-element alloy coating according to claim 1, wherein when Mo is selected for X, ni: ti: al: mo=45-47:47-50:4:1-4, and the ratio of Ni to Ti is less than or equal to 1; under standard cavitation erosion and erosion test conditions, the cavitation erosion average erosion speed of the coating is less than or equal to 6.0 MDE/mu m, and the erosion average erosion speed is less than or equal to 5.1 MDE/mu m.
4. The NiTiAl-X multi-element alloy coating according to claim 1, wherein when Cu is selected for X, ni: ti: al: cu=45-50:45-50:1-2:3-4; under standard cavitation erosion and erosion test conditions, the cavitation erosion average erosion speed of the coating is less than or equal to 12.7 MDE/mu m, and the erosion average erosion speed is less than or equal to 8.9 MDE/mu m.
5. The NiTiAl-X multi-element alloy coating according to claim 1, wherein when X is V, ni: ti: al: v=47.5-49.5:47.5-48.5:0.5-2.5:0.5-2.5; under standard cavitation erosion and erosion test conditions, the cavitation erosion average erosion speed of the coating is less than or equal to 9.6 MDE/mu m, and the erosion average erosion speed is less than or equal to 9.5 MDE/mu m.
6. The NiTiAl-X multi-element alloy coating according to claim 1, wherein the thickness of the NiTiAl-X multi-element alloy coating is 12-17 μm.
7. The NiTiAl-X multi-element alloy coating according to claim 1, wherein in step (1), the NiTiAl-X multi-element alloy ingots are prepared by vacuum arc melting technology, each alloy ingot being turned and melted at least four times.
8. The NiTiAl-X multi-element alloy coating according to claim 1, wherein in step (3), the substrate pressure during magnetron sputtering is 5X 10 -6 Pa, the deposition pressure was fixed at 5.0X10 by controlling the flow rate of argon gas in the deposition chamber -1 Pa; the substrate temperature is kept at 600 ℃ in the sputtering process, and the sputtering is completedAnd then cooled to 150 ℃ with the furnace.
9. Use of a NiTiAl-X multi-element alloy coating according to any one of claims 1-5 in an overcurrent element.
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