CN106757004B - A kind of tantalum metal surface laser multilayer cladding Ta2O5The method of ceramic coating - Google Patents
A kind of tantalum metal surface laser multilayer cladding Ta2O5The method of ceramic coating Download PDFInfo
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- CN106757004B CN106757004B CN201611224444.9A CN201611224444A CN106757004B CN 106757004 B CN106757004 B CN 106757004B CN 201611224444 A CN201611224444 A CN 201611224444A CN 106757004 B CN106757004 B CN 106757004B
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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
Abstract
The invention discloses a kind of tantalum metal surface laser multilayer cladding Ta2O5The method of ceramic coating, belongs to material manufacture technical field.This method utilizes Ta2O5The good light transmittance of ceramic powders, and its compatibility excellent with tantalum-base alloy have the single Ta of certain size thickness using the preset method of powder in the direct multilayer cladding in tantalum-base alloy surface2O5Ceramic coating.This method is easy to operate, limits less powder condition, cladding process does not need inert gas shielding, and manufacturing cost is low.Tantalum based metal surfaces laser multilayer cladding of the present invention prepares Ta2O5Excellent cladding performance and the single Ta such as ceramic coating has even tissue, compactness good, and stomata is few2O5Phase structure prepares the application fields such as implantation material coating, high-temperature wearable and optical coating suitable for Ta based metal surfaces.
Description
Technical field
The invention belongs to material manufacture technical fields, and in particular to a kind of tantalum metal surface laser multilayer cladding preparation has
Certain size thickness Ta2O5The method of ceramic coating.
Background technology
Refractory metal Ta and its alloy are because its property is stable, corrosion-resistant, high temperature resistant is widely used in human body Bones and joints and replaces
For material and high temperature aerospace material.In recent years, tantalum based metal surfaces prepare Ta2O5Ceramic coating obtains field of material preparation
Extensive concern.The study found that tantalum metal hardness is relatively low, and refractory metal oxide Ta2O5Not only fusing point is up to 1872 DEG C, but also
The high rigidity of ceramic phase makes it can be used as heat-resisting, wear-resisting, the resistance to heat etching of Ta based metal surfaces and thermal boundary protective coating；Secondly, Ta2O5
Also there is good biocompatibility, Ta is prepared in tantalum metal surface2O5Coating is implanted into for plastic surgery or human body Bones and joints
Object, coating can not only improve the corrosion wear characteristic of resistance to human body, provide more excellent bone uptake and attachment, it is often more important that can
The toxicity of generation is dissolved out under physiological environment to avoid metal ion.In addition, Ta2O5Ceramics have high light transmittance, wider light
Spectrum penetrates range (300nm-10 μm), is the most common high refractive index block of optical glass and high temp glass field and coating material
Material.At present, it was recently reported that many metal substrate surfaces prepare Ta2O5The technology of coating includes mainly：Pulsed laser deposition, hydrolysis contracting
Conjunction, atomic layer deposition, filtering cathode arc deposited, radio-frequency sputtering, direct current reaction magnetron sputtering and polymer assistant depositing etc..
However, above-mentioned technology, which concentrates on, prepares the film that thickness is limited to micron-scale.Wear out failure easily occurs for excessively thin coating, cannot
Meet its zero device surface required to mechanical property as the fields such as high-temperature wear resistant coating and body implant coating.
Existing preparation bulk prepares Ta in metal surface2O5The method of thick coating is mainly vacuum hot pressing sintering technique, by
In Ta2O5The high fusing point of ceramics, seldom report are prepared using solidification technology.China Patent Publication No. CN 1587200A are disclosed
A kind of laser heating pedestal crystal growth method passes through lifting and prepares Ta2O5The method of block crystalline ceramics, the technology first will be ceramic
For powder pressing at blank material, one end of heating ceramic blank material is then fixed using high power laser light as heat source makes ceramic blank melt,
It can make epitaxis by lifting.The technology can provide higher temperature ladder compared with conventional Bridgman crystal growths method
Degree and the speed of growth.Also it has been reported that and Ta is prepared using laser Fast Sintering technology2O5Ceramics, but above-mentioned laser technology emphasis is still
Prepare block Ta2O5Ceramics or monocrystalline, it is impossible to be used in the preparation of coating material.
Laser multilayer melting and coating technique prepares single ceramic coating, and existing research focuses primarily upon metal surface and prepares ZrO2+
Y2O3And Al2O3Equal ingredients thermal barrier coating.The problem is that since ceramics and metallic matrix thermophysical property differ greatly, gold
The direct general formability of cladding ceramic coating of metal surface is bad, easy to crack, concrete dynamic modulus.In addition, ceramic powders are mostly white or shallow
Yellow, absorptance is low, reflecting rate is high and it cannot fully be melted, the bad major reason of formability.The method of solution：1.
Ni, Co based alloy are added in ceramic coating, prepare metal-oxide composite coating；2. first with other technologies such as thermal spraying
Ceramic coating is prepared, laser remolten is then carried out；3. base metal surface first prepares alloy prime coat transition, then prepares ceramic painting
Layer.Most common bottoming composition of layer is MCrAlY etc., but for human body bone alternate material prime coat complexity metal component
Serious metal toxicity can be brought, not optimal selection.4. exploration can realize that ceramics were solidified with parent metal in laser bath
Good liquid phase reactor occurs for Cheng Zhongke, metallic matrix and ceramic coating material with excellent compatibility.But due to most metals
The significant difference of thermophysical property between ceramics need to attempt specific metal and ceramic material group in wider selection range
It closes, rare document report.As it can be seen that exploitation Ta based metal surfaces directly prepare Ta2O5Thick ceramic coating new technology answers tantalum metal
With will be significant.
Invention content
In order to overcome the deficiencies of the prior art, it is direct in tantalum metal surface that the technical problem to be solved in the present invention is to provide one kind
Laser multilayer cladding is carried out to prepare with certain size thickness Ta2O5The method of ceramic coating, it is easy to operate to this method, it is right
The limitation of powder condition is few, and cladding process does not need inert gas shielding, and manufacturing cost is low, coating cladding good quality, using neck
Domain is extensive.
It is achieved in order to solve the above technical problems, the present invention adopts the following technical scheme that.
A kind of tantalum metal surface laser multilayer cladding Ta of the present invention2O5The method of ceramic coating, utilizes Ta2O5Ceramic powders
Good light transmittance, and its compatibility excellent with tantalum-base alloy, using the preset method of powder in the direct multilayer in tantalum-base alloy surface
Cladding has the single Ta of certain size thickness2O5Ceramic coating is as follows：
(1) coating material is Ta2O5Ceramics wait for cladding Ta2O5Ceramics can be selected and be commercialized powder, Chun Du > in the market;
99%；
(2) basis material selection tantalum-base alloy or pure tantalum metal, cladding front surface carry out smooth polishing degreasing；
(3) laser multilayer cladding is prepared using fore-put powder method.Preset method process is as follows：First, by Ta2O5Ceramic powders
It is layered on Ta base metal surfaces, 0.8~2mm of powdering thickness in advance.Then, laser melting coating is carried out, it can form 0.2 after cladding~
The Ta of 0.5mm thickness2O5Ceramic coating.Subsequently, in first layer Ta2O5Clad layer surface is directly laid with second layer Ta2O5Powder
Carry out laser melting coating.Finally, according to Ta2O5The final application needs of coating layer thickness can be superimposed multilayer repeatedly, until after cladding
Ta2O5Coating reaches required thickness.
Further, the tantalum-base alloy is tantalum-tungsten alloy or tantalum-niobium alloy.
Compared with prior art, the present invention has the following technical effects：
(1) parent metal of the present invention is limited to tantalum metal alkyl materials, and coating material is limited to Ta2O5Ceramics.In view of ceramics
There are apparent thermophysical property difference between coating and metal material, generally believe that ceramics are bad with parent metal compatibility,
It is difficult to happen good liquid phase reactor.Rare success is in metal surface Direct Laser cladding high quality ceramic coating before the present invention
Report.
It is attempted using other metals such as Ti and steels as basis material cladding Ta in development process of the present invention2O5Coating is ground
Study carefully the matrix for finding only have tantalum Base Metal to be best, it can be with Ta2O5Ceramics form good liquid phase reactor and formability, Qi Tajin
Belong to matrix surface and prepares Ta2O5Coating cannot obtain good formability.Possible reason, the Ta of one side white2O5Powder
There is very high light transmittance compared with other ceramic materials, in cladding process laser heat source because reflection loss it is few, Ta can be made2O5Powder
End and tantalum metal surface fully melt in laser bath, to make coating and matrix form good liquid phase reactor and metallurgical junction
It closes.On the other hand, the Ta of Ta metals and laser irradiation fusing2O5Liquid phase has good compatibility and wetability.
(2) it is found compared with laser melting coating metal material coating during the present invention develops, due to Ta2O5Ceramic powders quality compared with
Gently, loose, pre- laying 0.8-2mm powder laser claddings are only capable of forming the coating of 0.2-0.5mm thickness, and common metal powder can
Form the coating of 0.6-1.5mm thickness.Therefore, in order to realize thick Ta2O5The standby purpose of ceramic system, this method use multiple-layer stacked
Melting and coating technique.
(3) due to Ta2O5The commercial preparation of ceramic powders prepares metal powder with vacuum atomizing very big difference, city
Sold Ta on field2O5Powder flowbility is difficult to meet the requirement of powder feeder conveying powder, and the present invention is carried out using fore-put powder method
Laser melting coating.
(4) this method prepares Ta2O5Thickness of ceramic coating is controllable, bonds closely, does not see between layers after multilayer cladding
Apparent interface, it is superior in quality.This is mainly due to Ta2O5Viscosity is higher after ceramics fusing, makes to realize between layers close
Adherency.Therefore, it is not required to can be obtained quality coating to the smooth polishing of surface progress when multilayer cladding.
(5) it can be not required to be passed through inert gas in cladding process and be protected, save manufacturing cost, it is easy to operate.Metal powder
End easily aoxidizes in laser high temperature bath, therefore need to usually carry out inert gas shielding, while need to generally add in powder
Adding additives avoid dispelling powder during inert gas shielding.And ceramic powders are lighter, are more easy to be dispelled by inert gas, bond
The addition of agent has an impact coating purity again.This method finds Ta in the course of the research2O5Ceramics are a kind of oxide in itself, i.e.,
Make to cause oxygen content in bath to increase without inert gas shielding, remains to obtain single Ta after coating solidification2O5Phase.Therefore,
It is proposed need not input inert gas shielding simultaneously in laser melting coating preparation process, need not also use binder, simplify
Technique improves efficiency and reduces cost.
(6) metal tantalum and Ta2O5The good liquid phase reactor of ceramics enables coating to realize metallurgical binding, interface cohesion with matrix
Closely, dilution rate is small.
(7) tantalum based metal surfaces laser multilayer cladding of the present invention prepares Ta2O5Ceramic coating has even tissue, compactness
It is good, excellent cladding performance and the single Ta such as stomata is few2O5Phase structure, suitable for Ta based metal surfaces prepare implantation material coating,
High-temperature wearable and optical coating application field.
Description of the drawings
Fig. 1 is 1 laser multilayer cladding Ta of embodiment2O5Ceramic coating surface pattern.
Fig. 2 is 1 laser multilayer cladding Ta of embodiment2O5Ceramic coating cross-sections scanning electron microscope tissue.
Fig. 3 is 1 laser multilayer cladding Ta of embodiment2O5Ceramic coating and tantalum metal interface scanning electron microscope mirco structure.
Fig. 4 is 1 laser multilayer cladding Ta of embodiment2O5XRD spectrum and crystal face index calibration in the middle part of ceramic coating.
Specific implementation mode
Below in conjunction with drawings and the specific embodiments, the invention will be further described, but the present invention is not limited to following realities
Apply example.
Embodiment 1
Commercialization Ta is bought from market2O5Ceramic powders and pure tantalum metal do coating material and matrix.First, laser will be waited for
It is the tantalum metal material surface decontamination of cladding, derusting, smooth.Then, by Ta2O5Ceramic powders are layered on tantalum metal surface 0.8mm in advance
It is thick.Then, CO2Cross-flow laser carries out laser melting coating to coating, and laser technical parameters are：Laser power 1.5kW, sweep speed
300mm/min, overlapping rate 30%, first layer coating layer thickness about 0.2mm after cladding.Subsequently, it repeats the above steps in first layer
Ta2O5Coating surface second, third and the 4th layer of Ta of cladding successively2O5Coating.It is respectively laser multilayer cladding shown in Fig. 1 and Fig. 2
Ta2O5Coating morphology and cross section tissue, the as seen from the figure Ta of cladding2O5Ceramic coating surface pattern is smooth, continuous.
Cladding layer cross section tissue pore-free, coating is fine and close, coating layer thickness about 1mm, and for layer with layer directly without apparent overlap joint, cladding is quality
It is good.Fig. 3 is coating and high power SEM at tantalum basal body interface is organized, and the fusing on tantalum parent metal surface layer makes coating interface, and there are Ta+
Ta2O5Miscible metallurgical binding area, interface cohesion is secured, and only about 20 μm of area's thickness, to the whole ingredient and performance shadow of coating
Sound is smaller.Fig. 4 is XRD spectrum and Ta in the middle part of ceramic coating2O5Crystal crystal face calibration result, it is seen that coating obtains single
Ta2O5Ceramic phase.
Embodiment 2
Commercialization Ta is bought from market2O5Ceramic powders and tantalum tungsten (TaW12) high-temperature alloy do matrix.First, it will wait swashing
It is the tantalum-tungsten alloy surface decontamination of light cladding, derusting, smooth.Then, by Ta2O5Ceramic powders are layered on tantalum metal surface 2mm thickness in advance.
Then, CO2Cross-flow laser carries out laser melting coating to coating, and laser technical parameters are：Laser power 2.0kW, sweep speed
200mm/min, overlapping rate 40%, first layer coating layer thickness about 0.5mm after cladding.Subsequently, it repeats the above steps in first layer
Ta2O5Coating surface 8 layers of Ta of cladding successively2O5Coating.Final thickness about 4mm after prepared coating cladding, coating cladding quality
Excellent, fine and close, pore-free, phase structure is single Ta2O5。
Embodiment 3
Commercialization Ta is bought from market2O5Ceramic powders and tantalum niobium (TaNb20) high-temperature alloy do matrix.First, it will wait for
It is the tantalum-niobium alloy surface decontamination of laser melting coating, derusting, smooth.Then, by Ta2O5Ceramic powders are layered on tantalum metal surface 1mm in advance
It is thick.Then, CO2Cross-flow laser carries out laser melting coating to coating, and laser technical parameters are：Laser power 1.8kW, sweep speed
500mm/min, overlapping rate 35%, first layer coating layer thickness about 0.3mm after cladding.Subsequently, it repeats the above steps in preceding layer
Ta2O5Coating surface six layers of Ta of continuous cladding successively2O5Coating.Final thickness about 1.8mm, coating after prepared coating cladding
Cladding is superior in quality, fine and close, pore-free, and phase structure is single Ta2O5。
Claims (2)
1. a kind of tantalum metal surface laser multilayer cladding Ta2O5The method of ceramic coating, which is characterized in that the coating material is
Ta2O5Ceramic powders, Chun Du >99%；Basis material selects tantalum-base alloy or pure tantalum metal, and substrate material surface carries out before cladding
Smooth polishing degreasing；
The laser multilayer cladding is prepared using fore-put powder method, is comprised the concrete steps that：
(1) by Ta2O5Ceramic powders are layered on tantalum-base alloy or pure tantalum metal surface, powdering thickness 0.8-2mm in advance；
(2) laser melting coating is carried out, the first layer Ta of 0.2~0.5mm thickness can be formed after cladding2O5Ceramic coating；
(3) in first layer Ta2O5Ceramic coating surface is directly laid with second layer Ta2O5Ceramic powders carry out laser melting coating；
(4) it is superimposed cladding repeatedly, until Ta after cladding2O5Ceramic coating reaches required thickness.
2. a kind of tantalum metal surface laser multilayer cladding Ta as described in claim 12O5The method of ceramic coating, feature exist
In the tantalum-base alloy is tantalum-tungsten alloy or tantalum-niobium alloy.
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| CN115281897A (en) * | 2022-07-29 | 2022-11-04 | 大连理工大学 | Metal-ceramic hip joint prosthesis lining and manufacturing method thereof |
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| FR3123364A1 (en) * | 2021-05-31 | 2022-12-02 | Centre National d'Études Spatiales | Substrate coated with a lubricious coating |
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Effective date of registration: 20210628 Address after: No.33, Lane 159, Taiye Road, Fengxian District, Shanghai, 201400 Patentee after: Shanghai Yuanbao Industrial Design Co.,Ltd. Address before: 243002 Anhui province Ma'anshan Huashan Lake District Road No. 59 Patentee before: ANHUI University OF TECHNOLOGY |
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Effective date of registration: 20230526 Address after: 721000 International New Materials Industrial Park, Comprehensive Bonded Zone, No. 600 Gaoxin Avenue, High tech Development Zone, Baoji City, Shaanxi Province Patentee after: Shaanxi Yucheng Hehui Metal Material Co.,Ltd. Address before: No.33, Lane 159, Taiye Road, Fengxian District, Shanghai, 201400 Patentee before: Shanghai Yuanbao Industrial Design Co.,Ltd. |