CN111304648B - TiBw-NiTi composite coating and preparation method thereof - Google Patents

TiBw-NiTi composite coating and preparation method thereof Download PDF

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CN111304648B
CN111304648B CN202010273669.3A CN202010273669A CN111304648B CN 111304648 B CN111304648 B CN 111304648B CN 202010273669 A CN202010273669 A CN 202010273669A CN 111304648 B CN111304648 B CN 111304648B
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composite coating
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CN111304648A (en
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林英华
林振衡
陈庆堂
唐群华
窦景欣
雷永平
符寒光
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Nanhua University
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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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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Abstract

The invention relates to a TiBw-NiTi composite coating and preparation method thereof. The TiBw-NiTi composite coating containing TiBwGrains and NiTi grains, TiBwThe area fraction of the crystal grains is 30-50%, the area fraction of the NiTi crystal grains is 40-60%, and the area fraction of the Ti crystal grains isGrains and TiB2The total area fraction of the crystal grains is not higher than 10%. The preparation method comprises the following steps: (1) mixing TiB2Uniformly mixing the powder and Ti powder to obtain mixed powder; (2) conveying the mixed powder obtained in the step (1) to the surface of a substrate in an inert atmosphere to prepare a cladding layer; (3) pre-placing Ni powder on the surface of the cladding layer obtained in the step (2) to obtain TiBw-a NiTi composite coating. The TiB obtainedwThe NiTi composite coating greatly eliminates the Ti matrix and TiB in the composite coating2The toughness, dry sliding wear resistance and fatigue resistance of the steel can be obviously improved.

Description

TiBw-NiTi composite coating and preparation method thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a TiBw-NiTi composite coating and preparation method thereof.
Background
TiBwAs the in-situ authigenic reinforcing phase commonly used for preparing the titanium-based composite material, the titanium-based composite material has the following advantages: TiBwThe diameter of the titanium alloy is very small, so that the crystal contains few defects, the atoms are highly ordered, and the strength is close to the theoretical value of a complete crystal, so that the Young modulus and the tensile strength of TiB are far higher than those of titanium and titanium alloy; chemical reaction does not occur between the TiB and the Ti matrix, a fixed orientation relation can be obtained, and the interface structure can be combined in a coherent or semi-coherent form, so that the mechanical property and the fatigue property of the composite coating can be improved; the density and the thermal expansion coefficient of TiB are similar to those of Ti and titanium alloy, so that the composite coating with high stability and low residual stress can be obtained.
The NiTi alloy has shape memory effect and excellent mechanical property (super elasticity), and the recoverable strain of the NiTi alloy can reach 8 percent at most. The shape memory effect of the NiTi alloy can be realized by promoting martensite to generate phase transformation through temperature rise and fall and stress application and unloading. And the superelastic behavior can be achieved by applying and removing stress to cause reversible martensitic transformation of the NiTi alloy. In order for NiTi alloys to exhibit superelastic properties, the material must be in the original state in the austenite phase, then stress-induced transformation of the austenite phase into the martensite phase is induced, and when the stress is relieved, the martensite phase returns to the austenite phase. During the stress application and unloading, in addition to the phase transformation behavior, the elastic deformation behavior of the austenite and martensite phases occurs, and thus a higher strain change amount than that of a general material can be obtained.
At present, Ni powder and TiB are adopted2The powder and Ti powder are mixed to be used as cladding material, and the composite coating is prepared on the surface of the titanium alloy by laser cladding. Although NiTi and TiB can be formedwPhase, also capable of suppressing Ni by process optimization3Ti、Ni3B、Ni4B3And Ni20Ti3B6Formation of equivalent phases, but also the presence of higher amounts of Ti matrix and TiB2. When the Ti matrix and the NiTi exist in the composite coating, particularly when the content of the Ti matrix is high, the Ti matrix is plastically deformed in the service process of the composite coating to cause dislocation slippage, and when the dislocation slips to the interface of the NiTi matrix, atomic scale high stress concentration is caused at the interface, so that the super-elastic property of the NiTi cannot be exerted. This requires that the composite coating contain no or low Ti matrix to ensure that the matrix material does not undergo dislocation glide during plastic deformation. The NiTi alloy generates stress to induce martensite phase transformation in the plastic deformation process, and the microstructure mechanism is lattice shear rather than dislocation slip, so that the NiTi alloy can exert super-elasticity performance when compounded with other strengthening phases difficult to deform plastically. However, TiB2Is a ceramic brittle phase, and poor fatigue resistance is easily caused by poor plastic deformation resistance and toughness. Therefore, in the preparation process of the composite coating, TiB formation is ensuredwAnd in the case of NiTi, how to eliminate the Ti matrix and TiB2The existence of the metal oxide and the reduction of the crack sensitivity in the solidification process of the laser molten pool become key technologies which need to be solved urgently.
In view of this, the invention is particularly proposed.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a TiBw-NiTi composite coatingAnd a method for preparing the same. TiB obtained by the preparation methodwThe NiTi composite coating greatly eliminates the Ti matrix and TiB in the composite coating2The toughness, dry sliding wear resistance and fatigue resistance of the steel can be obviously improved.
The scheme of the invention is to provide a TiBw-NiTi composite coating comprising TiBwGrains and NiTi grains, TiBwThe area fraction of the crystal grains is 30-50%, the area fraction of the NiTi crystal grains is 40-60%, and the Ti crystal grains and the TiB crystal grains2The total area fraction of the crystal grains is not higher than 10%; the thickness of the composite coating is 0.8-1.5 mm, and the composite coating can provide toughness, dry sliding wear resistance and fatigue resistance for the titanium alloy. The composite coating can be applied to a manufacturing layer and a repairing layer of a component manufactured by titanium alloy materials.
Preferably, the average microhardness of the composite coating is 500-600 HV0.2And a porosity area fraction of less than 3%.
Preferably, the TiBwThe crystal grains are in the form of fine needles, and the diameter of the fine needles is 300-500 nm.
Based on the same technical conception, the invention also provides a TiBwThe preparation method of the NiTi composite coating comprises the following steps: firstly TiB is added2Powder and Ti powder are taken as raw materials, the raw materials are sent into a processing chamber through coaxial powder feeding equipment or a preset mode, and a laser beam is adopted to prepare a cladding layer on the surface of a substrate; then, pre-coating Ni powder on the surface of the cladding layer, and preparing the composite coating on the surface of the original cladding layer in a synergistic mode of induction heating and laser cladding.
The method specifically comprises the following steps:
(1) mixing TiB2Uniformly mixing the powder and Ti powder to obtain mixed powder;
(2) conveying the mixed powder obtained in the step (1) to the surface of a substrate in an inert atmosphere to prepare a cladding layer;
(3) pre-placing Ni powder on the surface of the cladding layer obtained in the step (2) to obtain TiBw-a NiTi composite coating.
Wherein, the mixed powder in the step (2) can also be adhered to the surface of the substrate by adopting a preset method.
Preference is given toEarth, TiB2The particle size of the powder is 0.5-150 μm, the particle size of the Ti powder is 1-200 μm, and the particle size of the Ni powder is 1-100 μm.
Preferably, TiB2The weight ratio of the powder to the Ti powder is 1: 2-3. TiB2Too large or too small amounts of powder and Ni powder do not result in Ti grains and TiB2The total area fraction of the crystal grains is not higher than 10%.
Preferably, in the step (2), the amount of the mixed powder conveyed is 10-30 g/min.
Preferably, in the step (2), a laser beam heat source is started to prepare a cladding layer; the laser beam spot size is 4-5 mm, the laser beam power is 1.5-3.5 kW, the scanning speed is 4-8 mm/s, the defocusing amount is-1-0 mm, the dilution rate of the laser melting substrate is 5-25%, and the thickness of the obtained cladding layer is 0.4-1.0 mm.
Preferably, in the step (3), the Ni powder is heated to a temperature of 200 to 400 ℃ for 3 to 5min during coating.
Preferably, in the step (3), a laser beam heat source is started to prepare the composite coating; the laser beam spot size is 4 ~ 5mm, and laser beam power is 1.0 ~ 3.0kW, and scanning speed is 4 ~ 8mm/s, and the defocus volume moves 1 ~ 2mm downwards.
It is emphasized that, through repeated verification by the inventor, the composite coating must be prepared by 2 times of laser processing, otherwise, the content of Ti crystal grains cannot be effectively eliminated, and meanwhile, the second time of laser processing needs a synergistic induction heating device to effectively inhibit the crack initiation in the solidification process of a laser molten pool.
The method for preparing the composite coating needs the following equipment to be realized: a device that can provide a laser beam as a heat source; equipment capable of coaxially conveying mixed powder; closed processing equipment capable of performing inert atmosphere protection; the induction heating equipment can heat the substrate and monitor the temperature in real time.
The invention has the beneficial effects that:
TiB of the inventionwThe preparation method of the-NiTi composite coating comprises the steps of firstly taking Ti powder and TiB2Preparing a TiBw/Ti cladding layer on the surface of a substrate by using powder as a raw material, then pre-coating Ni powder on the surface of the cladding layer, and finally coating the original cladding layer with Ni powderPreparing a TiBw/NiTi composite coating on the surface. The preparation method greatly eliminates Ti matrix and TiB in the composite coating2The toughness, dry sliding wear resistance and fatigue resistance of the steel can be obviously improved. The TiBw-NiTi composite coating can be applied to a titanium alloy material surface modification layer and a repair layer.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a Scanning Electron Microscope (SEM) image of the cladding layer prepared in example 1.
FIG. 2 is a Scanning Electron Microscope (SEM) image of a composite coating prepared in example 1.
FIG. 3 is a graph of microhardness of the composite coating prepared in example 1 from the top and the bottom.
FIG. 4 is a graph comparing the dry sliding wear resistance of the composite coating prepared in example 1 with that of titanium alloy.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
This example provides a TiBwThe preparation method of the NiTi composite coating comprises the following steps:
(1) early preparation: the Ti-6Al-4V alloy is selected as a substrate, and comprises the following components in percentage by weight: 6.01 percent of aluminum, 3.84 percent of vanadium, 0.3 percent of iron, 0.15 percent of sulfur,0.1% of carbon, 0.1% of oxygen, 0.15% of nickel and the balance of titanium; placing the Ti-6Al-4V alloy substrate into a processing protection chamber with controllable closed atmosphere, and placing and fastening an induction heater at the lower part of the substrate; mixing TiB with purity of 99.9%2Compounding the powder and Ti powder with the purity of 99% according to the weight ratio of 1:3 to obtain mixed powder, TiB2The particle size of the powder is 0.5-10 mu m, and the particle size of the Ti powder is 1-10 mu m; mixing the mixed powder in a vertical high-energy ball mill for 120min, drying at 120 ℃ for 60min, and then putting into a coaxial powder feeder; argon with the atomizing size of 48-75 microns and the purity of 99.9 percent is selected as protective gas and mixed powder conveying gas, and the conveyed mixed powder amount is 10 g/min;
(2) preparing a cladding layer: starting a laser beam heat source to prepare a cladding layer, wherein the laser cladding process parameters are that the spot size of a laser beam is 5 multiplied by 5mm (square spot), the power of the laser beam is 1.5kW, the scanning speed is 4mm/s, the defocusing amount is 0mm, the dilution rate of a laser melting substrate is 5%, and the thickness of the obtained cladding layer is 0.8 mm-1.0 mm;
(3) preparing a composite coating: presetting Ni powder with the granularity of 1-5 mu m on the surface of the cladding layer, wherein the thickness of the preset layer is 0.5-0.7 mm; adjusting the preheating temperature of the preset layer to 300 ℃ by adopting an induction heating device, and preheating for 3 min; the laser process parameters are as follows: the laser beam spot size is 5 multiplied by 5mm (square spot), the laser power is 1.0kW, the scanning speed is 4mm/s, the defocusing amount moves downwards by 2mm, and the thickness of the prepared composite coating is about 1.3 mm-1.5 mm in a dynamic sealed atmosphere controllable processing protection room.
Example 2
The present embodiment provides a TiBwThe preparation method of the NiTi composite coating comprises the following steps:
(1) early preparation: the TA2 alloy is selected as a substrate, and comprises the following components in percentage by weight: 0.03% of nitrogen, 0.015% of hydrogen, 0.3% of iron, 0.25% of oxygen, 0.1% of carbon and the balance of titanium; mixing TiB with purity of 99.9%2Compounding the powder and Ti powder with the purity of 99.1% in the weight ratio of 1 to 2 to obtain mixed powder TiB2The particle size of the powder is 130-150 μm, and the particle size of the Ti powder is 180-200 μm; mixing the powder in vertical high energyMixing for 150min in a ball milling device, drying for 90min at 120 ℃, and then putting into a coaxial powder feeder; argon with the atomizing size of 50-70 mu m and the purity of 99.99 percent is selected as protective gas and mixed powder conveying gas, and the conveyed mixed powder amount is 30 g/min;
(2) preparing a cladding layer: starting a laser beam heat source to prepare a cladding layer, wherein the laser cladding process parameters are that the diameter of a laser beam spot is 4mm (a circular spot), the power of the laser beam is 3.5kW, the scanning speed is 8mm/s, the defocusing amount is-1 mm, the dilution rate of a laser melting substrate is 25%, and the thickness of the obtained cladding layer is 0.6-0.8 mm;
(3) preparing a composite coating: adopting Ni powder to preset on the surface of a cladding layer, wherein the thickness of the preset layer is 0.3-0.4 mm; adjusting the preheating temperature of the preset layer to 400 ℃ by adopting an induction heating device, and preheating for 4 min; the laser process parameters are as follows: the laser beam spot size is 4 multiplied by 4mm (square spot), the laser power is 3.0kW, the scanning speed is 8mm/s, the defocusing amount moves downwards by 1mm, and the thickness of the prepared composite coating is about 0.8 mm-1.0 mm in a dynamic sealed atmosphere controllable processing protection room.
Example 3
This example provides a TiBwThe preparation method of the NiTi composite coating comprises the following steps:
(1) early preparation: the Ti-6Al-4V alloy is selected as a substrate, and comprises the following components in percentage by weight: 6.01 percent of aluminum, 3.84 percent of vanadium, 0.3 percent of iron, 0.15 percent of sulfur, 0.1 percent of carbon, 0.1 percent of oxygen, 0.15 percent of nickel and the balance of titanium; placing the Ti-6Al-4V alloy substrate into a processing protection chamber with controllable closed atmosphere, and placing and fastening an induction heater at the lower part of the substrate; mixing TiB with purity of 99.9%2Compounding the powder and Ti powder with the purity of 99.1% in the weight ratio of 1 to 2.5 to obtain mixed powder TiB2The granularity of the powder is 90-100 mu m, and the granularity of the Ti powder is 80-90 mu m; mixing the mixed powder in a vertical high-energy ball mill for 120min, and then adopting a proper amount of 2123 phenolic resin as a binder to mix TiB2Presetting the powder and Ti powder on a cylinder of a sample, wherein the thickness of the preset layer is 0.4-0.6 mm, and then drying for 100min at 120 ℃; argon with the atomizing size of 5-10 mu m and the purity of 99.9 percent is selectedAs a shielding gas;
(2) preparing a cladding layer: starting a laser beam heat source to prepare a cladding layer, wherein the laser cladding process parameters are that the spot size of a laser beam is 5 multiplied by 5mm (circular spot), the power of the laser beam is 2.7kW, the scanning speed is 6mm/s, the defocusing amount is 0mm, the dilution rate of a laser melting substrate is 15%, and the thickness of the obtained cladding layer is 0.6-0.8 mm;
(3) preparing a composite coating: adopting Ni powder to preset on the surface of a cladding layer, wherein the thickness of the preset layer is 0.3-0.4 mm; adjusting the preheating temperature of the preset layer to 200 ℃ by adopting an induction heating device, and preheating for 5 min; the laser process parameters are as follows: the laser beam spot size is 5 multiplied by 5mm (square spot), the laser power is 2.4kW, the scanning speed is 4mm/s, the defocusing amount moves downwards by 1mm, and the thickness of the prepared composite coating is about 0.8 mm-1.0 mm in a dynamic sealed atmosphere controllable processing protection room.
FIG. 1 is an SEM photograph of the cladding layer prepared in example 1, and TiB can be seenwThe shape of the needle-like structure is fine needle-like, and the diameter and the length of the needle-like structure are respectively 300-500 nm and 5-8 mu m.
FIG. 2 and Table 1 show the SEM and EPMA test results, respectively, of the composite coating prepared in example 1, and it can be seen that the composite coating has TiB as a main componentw(2 and 3 in the figure) and NiTi (1 and 4 in the figure), and also contains small amount of Ti and TiB2Phase, TiBwThe form of the NiTi is fine needle-shaped, the diameter and the length of the NiTi are respectively 300-500 nm and 5-8 mu m, the form of the NiTi is dendritic, and the average size of the NiTi is 6 mu m. Meanwhile, the composite coating is found to be compact in structure, and the porosity area fraction is lower than 3%.
FIG. 3 is a graph of the microhardness of the composite coating prepared in example 1, and it can be seen that the microhardness of the composite coating is slightly reduced from the surface to the inside, but the microhardness values from the surface to the inside are 500-600 HV0.2Mean microhardness of 556HV0.2。
FIG. 4 is a graph comparing the dry sliding wear resistance of the composite coating prepared in example 1 with that of titanium alloy, and it can be seen that the abrasion load is 200N, and the rotation speed is 500 r.min-1And under the condition of 30min of abrasion time, the abrasion loss of the composite coating is only 12% of that of the titanium alloy. Illustrating the TiBw-NiTi compositeThe coating has excellent wear resistance.
TABLE 1 EPMA test results
Position of Ti/％ B/％ Ni/％ Al/％ V/％
1 47.5 1.2 49.7 0.9 0.7
2 50.2 48.3 0.4 0.6 0.5
3 50.2 47.1 0.8 1.0 0.9
4 47.7 0.7 49.2 1.1 1.3
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (9)

1. TiBw-a NiTi composite coating, characterized in that it contains TiBwGrains and NiTi grains, TiBwThe area fraction of the crystal grains is 30-50%, the area fraction of the NiTi crystal grains is 40-60%, and the Ti crystal grains and the TiB crystal grains2The total area fraction of the crystal grains is not higher than 10%;
the TiBwThe preparation method of the NiTi composite coating comprises the following steps:
(1) mixing TiB2Uniformly mixing the powder and Ti powder to obtain mixed powder;
(2) conveying the mixed powder obtained in the step (1) to the surface of a substrate in an inert atmosphere to prepare a cladding layer;
(3) pre-placing Ni powder on the surface of the cladding layer obtained in the step (2) to obtain TiBw-a NiTi composite coating;
preparing a cladding layer on the surface of a substrate by adopting a laser beam, then pre-coating Ni powder on the surface of the cladding layer, and preparing a composite coating on the surface of the original cladding layer in a synergistic mode of induction heating and laser cladding; and the composite coating must be prepared by 2 times of laser processing, otherwise, the content of Ti crystal grains cannot be effectively eliminated, and meanwhile, the secondary laser processing can effectively inhibit the crack initiation in the solidification process of a laser molten pool only by needing a synergistic induction heating device.
2. The TiB of claim 1w-a NiTi composite coating, characterized in that the thickness of the composite coating is 0.8-1.5 mm.
3. The TiB of claim 1w-a NiTi composite coating, characterized in that the composite coating has an average microhardness of 500 to 600HV0.2 and a porosity area fraction of less than 3%.
4. The TiB of claim 1w-a NiTi composite coating, characterized in that the TiBwThe crystal grains are in the form of fine needles, and the diameter of the fine needles is 300-500 nm.
5. The TiB of claim 1w-NiTi composite coating, characterized in that TiB2The particle size of the powder is 0.5-150 μm, the particle size of the Ti powder is 1-200 μm, and the particle size of the Ni powder is 1-100 μm; TiB2The weight ratio of the powder to the Ti powder is 1: 2-3.
6. The TiB of claim 1wThe NiTi composite coating is characterized in that in the step (2), the amount of the conveyed mixed powder is 10-30 g/min.
7. The TiB of claim 1wThe NiTi composite coating is characterized in that in the step (2), a laser beam heat source is started to prepare a cladding layer; the laser beam spot size is 4-5 mm, the laser beam power is 1.5-3.5 kW, the scanning speed is 4-8 mm/s, the defocusing amount is-1-0 mm, the dilution rate of the laser melting substrate is 5-25%, and the thickness of the obtained cladding layer is 0.4-1.0 mm.
8. The TiB of claim 1wThe NiTi composite coating is characterized in that in the step (3), when the Ni powder is coated, the temperature is heated to 200-400 ℃ and maintained for 3-5 min.
9. The TiB of claim 1wThe NiTi composite coating is characterized in that in the step (3), a laser beam heat source is started to prepare the composite coating; the laser beam spot size is 4 ~ 5mm, and laser beam power is 1.0 ~ 3.0kW, and scanning speed is 4 ~ 8mm/s, and the defocus volume moves 1 ~ 2mm downwards.
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