CN106435566B - A kind of method of niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating - Google Patents
A kind of method of niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating Download PDFInfo
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- CN106435566B CN106435566B CN201610817077.7A CN201610817077A CN106435566B CN 106435566 B CN106435566 B CN 106435566B CN 201610817077 A CN201610817077 A CN 201610817077A CN 106435566 B CN106435566 B CN 106435566B
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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
Abstract
The invention discloses a kind of methods of niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating, include the following steps：（1）It is prepared by matrix of samples：Surface grinding processing and drying process are carried out to matrix of samples；（2）It is prepared by mixed powder：Mixed powder is mainly made of zirconia powder, oxidation yttrium powder and nickel-base alloy powder；After mixed powder is prepared according to corresponding proportion, mixed powder is put into ball mill, 2h is mixed, 100 DEG C of processing 5h of heat preservation are dried in mixed powder later；（3）Powder feeder parameter setting；（4）Laser parameter is arranged；（5）The parameter set according to above-mentioned steps proceeds by laser multiple tracks cladding in C103 niobium alloy disk surfaces.ZrO prepared by the present invention2Ni base composite ceramic gradient coatings are divided into equiax crystal orientation column crystal binder course, middle part branch crystal layer, surface compact ceramic layer；Coating is in metallurgical binding with matrix, is well combined, coating hardness is greatly improved compared with matrix and pure nickel coating.
Description
Technical field
The present invention relates to a kind of processes of laser multiple tracks deposited metals composite ceramics gradient coating, belong to composite material
Technical field.
Background technology
Gradient coating refers to that consecutive variations are presented in material composition, structure, density and function from matrix to coating surface
A kind of composite construction.Gradually changeable in macroscopic properties makes gradient coating internal stress small, and under high temperature difference environment, thermal stress will
Obtain certain mitigation.Gradient coating have the advantages that many single coatings it is incomparable, be particularly suitable for ceramic coating with close
Optimum performance matching between auri body.High wear-resisting, the resistance to thermal barrier coating of binding force is can get using the technology, in high temperature or the temperature difference
Change under big environment, can slow down or change thermal stress mutation and distribution, to be effectively prevented disbonding.Thermal barrier coating exists
Aerospace, atomic energy and military industry field have a wide range of applications, and gradient coating is applied as heat insulating coat in space flight earliest, and one
As be combined by metal material and ceramic material, with the excellent performance not fallen off under big temperature difference environment.Metal has
The performances such as high thermal conductivity, toughness and ductility, ceramic material hardness is high, wear-resisting, anti-corrosion, high temperature resistant, some ceramics also have
How the properties such as heat-insulated, insulation or luminous energy conversion combine metal with the excellent properties of ceramics, are always material supply section
Learn the direction with engineering research.
Protective coating is coated in alloy surface, is improving alloy high-temp inoxidizability and corrosion proof while can also have both good
Good mechanical property, gradient coating is a kind of preferable solution, and the document of related application is 1.《It is prepared on niobium tungsten alloy high
The method of warm antioxidant coating》（Application number：201110024937.9）By first cold spraying nano Si, Mo, then laser remolten
High-temperature oxidation resistant coating is prepared, coating has powerful binding force and have preferable high-temperature oxidation resistance with matrix.②《It is a kind of
Laser melting coating metal/ceramic composite coating and its preparation process》（Application number：201310392592.1）It is Ni-based by preset Ni35
Alloy powder and bulky grain niobium carbide NbC mixed powders are in steel matrix, and then 3. laser melting coating is prepared for wear-resistant coating《It is a kind of
The method of refractory metal material surface Zr base ceramic coatings protection》（Application number：201510009907.9）It is heavy by electrophoresis first
The preset Zr base ceramic coatings of method refractory metal surfaces are accumulated, then laser melting coating is prepared for anti-corrosion coating.④《It is laser induced compound
The method of cladding gradient function thermal barrier coating》（Application number：200910186673.X）Bonding is sent respectively by twin-bucket automatic powder feeding
Metal powder and ceramic powder prepare controllable thickness gradient coating.1. 2. 3. 4. it is different from patent, the present invention is one kind in niobium alloy table
The technique of face laser multiple tracks cladding single layer composite ceramics gradient coating, using the method for sending mixed powder is synchronized, single layer cladding both may be used
To prepare high-bond gradient coating, coating surface layer is continuous dense ceramic layers, and provides properties of sample analysis.
Invention content
The present invention provides a kind of method in niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating.By this hair
Graded is presented in chemical composition and texture in the coating of bright acquisition, and coating can be divided into three layers of equiax crystal orientation column crystal knot
Layer, middle part branch crystal layer, surface compact ceramic layer, coating and matrix metallurgical binding are closed, bond strength is high, the continuous fine and close pottery of outer layer
Enamel coating is engaged with matrix in sawtooth.
The invention is realized in this way：
A kind of method of niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating, it is characterised in that：Including following
Step：
（1）It is prepared by matrix of samples：It uses wire cutting method to cut thickness for the C103 niobium alloys of 3mm, a diameter of 23mm to justify
Piece sample uses the silicon carbide paper of 80#, 120#, 240#, 320#, 400#, 600# to carry out surface to C103 niobium alloy disks successively
Polishing is handled, and is carried out super wave with absolute ethyl alcohol later and is cleaned 15min, then low temperature drying C103 niobium alloys disk surfaces；
（2）It is prepared by mixed powder：Mixed powder is mainly made of zirconia powder, oxidation yttrium powder and nickel-base alloy powder；The oxygen
Change zirconium powder and match powder in 0%~20% ratio of mixed powder gross mass, the oxidation yttrium powder is matched in 10% ratio of zirconia powder quality
Powder, surplus are nickel-base alloy powder；After mixed powder is prepared according to corresponding proportion, mixed powder is put into ball mill, 2h is mixed,
100 DEG C of processing 5h of heat preservation are dried in mixed powder later；
（3）Powder feeder parameter setting：Mixed powder after drying is imported in powder feeding tank, each mixed powder is sent into 50g；Setting
Powder feeding throughput is 6~15L/min, and powder feeding voltage is 3~12V；
（4）Laser parameter is arranged：Finished surface 20mm of the focus lamp of laser away from C103 niobium alloy disks, laser work(
800~1400W of rate, 100~500mm/min of spot velocity；
（5）The parameter set according to above-mentioned steps proceeds by laser multiple tracks cladding in C103 niobium alloy disk surfaces.
It further illustrates, in step（1）In, each element content of the C103 niobium alloy disks is：Hf（Hafnium）=
9.11wt%、Ti（Titanium）=0.81wt%、Zr（Zirconium）=0.30wt%、W（Tungsten）=0.30wt%、Ta（Tantalum）=0.27wt%、C（Carbon）=
0.005wt%、N（Nitrogen）=0.010wt%、O（Oxygen）=0.019wt%, remaining be Nb（Niobium）.
It further illustrates, in step（2）In, each element content of the nickel-base alloy powder is：C（Carbon）=0.1wt%、Si
（Silicon）=3.0wt%、Cr（Chromium）=1.0wt%、B（Boron）=1.5wt%、Fe（Iron）=6.0wt%, remaining be Ni（Nickel）；The oxidation
The purity of zirconium powder is ZrO2≥99.9wt%；Aoxidize the purity Y of yttrium powder2O3≥99.9wt%；Stabilization of the yttrium oxide as zirconium oxide
Agent.
It further illustrates, the granular size of the nickel-base alloy powder is 120~420 mesh；Of the zirconia powder
Grain size is 300~320 mesh；The granular size of the oxidation yttrium powder is 300~320 mesh.
It further illustrates, in step（3）In, the powder feeding gas that powder feeder uses is 99.9% high purity argon, and as guarantor
Protect gas；The powder-feeding nozzle of powder feeder is directed at hot spot, apart from 6~12mm of hot spot.
It further illustrates, in step（4）In, laser is fiber coupling all solid state laser, focal length 20mm, spot diameter
3mm。
It further illustrates, in step（5）In, the overlapping rate of laser multiple tracks cladding is 33%.
Advantages of the present invention：
1. the present invention, which is laser melting coating, prepares composite ceramics gradient coating, coating and base layer metallurgical binding, binding force is strong,
Outer coating, which is dense ceramic layers, can effectively improve its high-temperature oxidation resistance.
2. composite ceramics gradient coating prepared by the present invention, chemical composition change in gradient with texture, effectively reduce
Because coefficient of thermal expansion difference leads to the probability of coating shedding.
3. coating hardness improves 4~7 times relative to niobium alloy matrix.
4. the present invention uses synchronous powder feeding system, the composite ceramic that outer layer is ceramic of compact coating is prepared with the less ceramic powder of content
Porcelain gradient coating effectively reduces cost, efficient, and composite powder utilization rate is high.
5. composite ceramics gradient coating corrosion resistance prepared by prepares coating of the present invention has larger promotion compared with matrix,
Two orders of magnitude of middle polarization resistance maximum lift.
Description of the drawings
Fig. 1：Whole pattern of the 2 composite ceramics gradient coating section of embodiment after corrosion treatment.
Fig. 2：2 coating outer layer dense ceramic layers of embodiment.
Fig. 3：Branch crystal layer in the middle part of 2 coating of embodiment.
Fig. 4：2 coating of embodiment orients column crystal with matrix engaging portion equiax crystal.
Fig. 5：4 outer layer dense ceramic layers of embodiment and middle part branch crystal layer combination interface.
Fig. 6：1,2,3,4 coating surface XRD spectrum of embodiment.
Fig. 7：Matrix section, pure nickel powder coating, 1,2,3,4 coating cross sections hardness profile of embodiment.
Fig. 8：Matrix, pure nickel powder coating, the electrochemical tests of 1,2,3,4 sample coatings of embodiment.
In figure 6,1 surface xrd collection of illustrative plates of a embodiments, 2 surface xrd collection of illustrative plates of b embodiments, 3 surface xrd collection of illustrative plates of c embodiments, d
4 surface xrd collection of illustrative plates of embodiment.
In the figure 7, curve 1 is undressed matrix curve, and curve 2 is without ZrO2 coating cross sections hardness
Distribution curve, curve 3 are 2 coating cross sections hardness profile of embodiment, and curve 4 is that the distribution of 1 coating cross sections hardness of embodiment is bent
Line, curve 5 are 3 coating cross sections hardness profile of embodiment, and curve 6 is 5 coating cross sections hardness profile of embodiment.
In fig. 8, curve 1,2,3,4,5,6 is respectively matrix, pure nickel powder coating, embodiment 1,2,3,4 sample coatings electricity
Chemical polarization curve.
Specific implementation mode
Present invention will be further explained below with reference to the attached drawings and examples.
Embodiment 1：
A kind of method of niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating, includes the following steps：
（1）It is prepared by matrix of samples：It uses wire cutting method to cut thickness for the C103 niobium alloys of 3mm, a diameter of 23mm to justify
Piece sample uses the silicon carbide paper of 80#, 120#, 240#, 320#, 400#, 600# to carry out surface to C103 niobium alloy disks successively
Polishing is handled, and is carried out super wave with absolute ethyl alcohol later and is cleaned 15min, then low temperature drying C103 niobium alloys disk surfaces；
（2）It is prepared by mixed powder：Mixed powder is mainly made of zirconia powder, oxidation yttrium powder and nickel-base alloy powder；The oxygen
Change zirconium powder and match powder in 5% ratio of mixed powder gross mass, the oxidation yttrium powder matches powder in 10% ratio of zirconia powder quality, remaining
Amount is nickel-base alloy powder；After mixed powder is prepared according to corresponding proportion, mixed powder is put into ball mill, 2h is mixed, later will
100 DEG C of processing 5h of heat preservation are dried in mixed powder；
（3）Powder feeder parameter setting：Mixed powder after drying is imported in powder feeding tank, each mixed powder is sent into 50g；Setting
Powder feeding throughput is 8L/min, and powder feeding voltage is 8V；
（4）Laser parameter is arranged：Finished surface 20mm of the focus lamp of laser away from C103 niobium alloy disks, laser work(
Rate 1200W, spot velocity 300mm/min；
（5）The parameter set according to above-mentioned steps proceeds by laser multiple tracks cladding in C103 niobium alloy disk surfaces,
Overlapping rate is 33%.
In step（1）In, each element content of the C103 niobium alloy disks is：Hf=9.11wt%、Ti=0.81wt%、
Zr=0.30wt%, W=0.30wt%, Ta=0.27wt%, C=0.005wt%, N=0.010wt%, O=0.019wt%, remaining be Nb.
In step（2）In, each element content of the nickel-base alloy powder is：C=0.1wt%、Si=3.0wt%、Cr=
1.0wt%, B=1.5wt%, Fe=6.0wt%, remaining be Ni；The purity of the zirconia powder is ZrO2≥99.9wt%；Yttrium oxide
The purity Y of powder2O3≥99.9wt%；Stabilizer of the yttrium oxide as zirconium oxide.
In step（3）In, the powder feeding gas that powder feeder uses is 99.9% high purity argon, and as protective gas；Powder feeding
The powder-feeding nozzle of device is directed at hot spot, apart from hot spot 8mm.
In step（4）In, laser is fiber coupling all solid state laser, focal length 20mm, spot diameter 3mm.
Embodiment 2：
The present embodiment is differed only in embodiment 1：In step（2）Described in zirconia powder press mixed powder gross mass
10% ratio match powder；In step（4）Middle laser power 1300w, spot velocity 250mm/min.
Table 1：2 coating cross sections of embodiment different parts Zr, Y, O constituent content after corroding corrosion
| Coating location | Zr contents（wt%） | Y contents（wt%） | O content（wt%） |
| Engaging portion equiax crystal dendrite | 11.44 | 6.86 | 2.19 |
| Middle part dendrite | 32.18 | 13.14 | 4.73 |
| External dense ceramic layers | 44.63 | 18.17 | 9.31 |
Embodiment 3：
The present embodiment is differed only in embodiment 1：In step（2）Described in zirconia powder press mixed powder gross mass
15% ratio match powder；In step（3）Middle powder feeding throughput is 10L/min；In step（4）Middle laser power 1200w, hot spot speed
Spend 250mm/min.
Embodiment 4：
The present embodiment is differed only in embodiment 1：In step（2）Described in zirconia powder press mixed powder gross mass
20% ratio match powder；In step（3）Middle powder feeding throughput is 10.5L/min；In step（4）Middle laser power 1300w, hot spot
Speed 300mm/min.
Embodiment 5：
The present embodiment is differed only in embodiment 1：In step（3）Middle powder feeding throughput is 6L/min, powder feeding voltage
3V；Powder-feeding nozzle is apart from hot spot 6mm；In step（4）Middle laser power 800w, spot velocity 100mm/min.
Embodiment 6：
The present embodiment is differed only in embodiment 1：In step（3）Middle powder feeding throughput is 15L/min, powder feeding voltage
12V；Powder-feeding nozzle is apart from hot spot 12mm；In step（4）Middle laser power 1400w, spot velocity 500mm/min.
Composite ceramics gradient coating Cross Section Morphology and mechanical property characterization
To embodiment 1,2,3,4 obtained samples, it is utilized respectively electron microscope, scanning electron microscope（SEM）Observe cutting for coating
Face pattern utilizes X-ray diffraction analysis instrument（XRD）Detect the phase structure of coating, EDS detection elements contents, electrochemical operation
It stands and detects coating corrosion resistance energy, the hardness that Vickers measures cladding layer is utilized to be distributed.Measurement result is shown in Table 1, Fig. 1~figure
8, measurement result shows：
1. it is showed a rising trend from coating interface to outer surface by EDS spectroscopy detection Zr, Y, O constituent content such as table 1, coating
Ingredient changes in gradient.
It, can be with clear view to applying by electron microscope, SEM 2. after corroding 2 sample in cross section of corrosion embodiment
Layer is divided into three layers, and Fig. 1 is coating global sections figure, and Fig. 2 is surface compact ceramic layer, and Fig. 3 is middle part branch crystal layer, and Fig. 4 is etc.
Axialite orient column crystal binder course, coating and matrix metallurgical binding are good, in structure from coating cross sections to coating surface, intergranular away from
Smaller and smaller, coating changes in gradient in structure.
3. 4 outer layer dense ceramic layers of embodiment are presented sawtooth with middle part branch crystal layer combination interface and are engaged as shown in Figure 5,
This sawtooth occlusion structure can greatly promote outer layer dense ceramic layers and middle part dendrite binding force.
4. by Fig. 6 each sample coating surface XRD diagram spectrum analysis, it is m- that sample coatings Surface Phases, which are made, in embodiment 1
ZrO2Embodiment 2, the object phase of 3,4 obtained sample surfaces mainly have m-ZrO2、t-ZrO2、c-ZrO2, show embodiment 1,2,3,4
The dense ceramic layers on surface are ZrO2。
5. being existed by 1 hardness number containing coating cross sections of embodiment known to 1,2,3,4,5,6 curves in Fig. 7
It is 5~6 times of matrix within the scope of 1000~1200HV；2 coating cross sections hardness number of embodiment is in 900~100HV ranges
It is interior, it is 4~5 times of matrix；3 coating cross sections hardness number of embodiment is the 5~6 of matrix within the scope of 1000~1350HV
Times；4 coating cross sections hardness number of embodiment is 7~8 times of matrix within the scope of 1200~1400HV；Curve 3,4,5,6 and song
Line 2 compares it is found that ZrO2The addition of ceramic phase is the main reason for coating hardness is promoted.
6. real by 1,2,3,4,5,6 coating electrochemical tests in Fig. 8 it is found that relative to matrix and pure nickel coating
The corrosion current for applying example 1,2,3,4 all decreases and corrosion resistance is promoted, and wherein 4 sample coatings of embodiment reduce about
2 orders of magnitude, embodiment 1,2 sample coatings reduce about 1 order of magnitude, and 4 sample coatings polarization resistance highest of embodiment is resistance to
Corrosion is best.
Claims (7)
1. a kind of method of niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating, it is characterised in that：Including following step
Suddenly：
（1）It is prepared by matrix of samples：It uses wire cutting method to cut thickness to try for the C103 niobium alloy disks of 3mm, a diameter of 23mm
Sample uses the silicon carbide paper of 80#, 120#, 240#, 320#, 400#, 600# to carry out surface grinding to C103 niobium alloy disks successively
Processing, carries out ultrasonic cleaning 15min, then low temperature drying C103 niobium alloys disk surfaces with absolute ethyl alcohol later；
（2）It is prepared by mixed powder：Mixed powder is mainly made of zirconia powder, oxidation yttrium powder and nickel-base alloy powder；The zirconium oxide
Powder matches powder in 5%~20% ratio of mixed powder gross mass, and the oxidation yttrium powder matches powder in 10% ratio of zirconia powder quality,
Surplus is nickel-base alloy powder；After mixed powder is prepared according to corresponding proportion, mixed powder is put into ball mill, 2h is mixed, later
100 DEG C of processing 5h of heat preservation are dried in mixed powder；
（3）Powder feeder parameter setting：Mixed powder after drying is imported in powder feeding tank, each mixed powder is sent into 50g；Powder feeding is set
Throughput is 6~15L/min, and powder feeding voltage is 3~12V；
（4）Laser parameter is arranged：Finished surface 20mm of the focus lamp of laser away from C103 niobium alloy disks, laser power
800~1400W, 100~500mm/min of spot velocity；
（5）The parameter set according to above-mentioned steps proceeds by laser multiple tracks cladding in C103 niobium alloy disk surfaces.
2. the method for niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating according to claim 1, feature
It is：In step（1）In, each element content of the C103 niobium alloy disks is：Hf=9.11wt%、Ti=0.81wt%、Zr=
0.30wt%, W=0.30wt%, Ta=0.27wt%, C=0.005wt%, N=0.010wt%, O=0.019wt%, remaining be Nb.
3. the method for niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating according to claim 1, feature
It is：In step（2）In, each element content of the nickel-base alloy powder is：C=0.1wt%、Si=3.0wt%、Cr=1.0wt%、
B=1.5wt%, Fe=6.0wt%, remaining be Ni；The purity of the zirconia powder is ZrO2≥99.9wt%；Aoxidize the pure of yttrium powder
Spend Y2O3≥99.9wt%；Stabilizer of the yttrium oxide as zirconium oxide.
4. the method for niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating according to claim 1 or 3, special
Sign is：The granular size of the nickel-base alloy powder is 120~420 mesh；The granular size of the zirconia powder be 300~
320 mesh；The granular size of the oxidation yttrium powder is 300~320 mesh.
5. the method for niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating according to claim 1, feature
It is：In step（3）In, the powder feeding gas that powder feeder uses is 99.9% high purity argon, and as protective gas；Powder feeder
Powder-feeding nozzle be aligned hot spot, apart from 6~12mm of hot spot.
6. the method for niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating according to claim 1, feature
It is：In step（4）In, laser is fiber coupling all solid state laser, focal length 20mm, spot diameter 3mm.
7. the method for niobium alloy surface laser multiple tracks cladding composite ceramics gradient coating according to claim 1, feature
It is：In step（5）In, the overlapping rate of laser multiple tracks cladding is 33%.
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Effective date of registration: 20210226 Address after: 545112 No.1 Xingfu Road, Xinxing Industrial Park, Liujiang District, Liuzhou City, Guangxi Zhuang Autonomous Region Patentee after: Liuzhou Hengfengli Cutting Tool Co.,Ltd. Address before: 530004 No. 100, University Road, the Guangxi Zhuang Autonomous Region, Nanning Patentee before: GUANGXI University Patentee before: GUANGXI NANNING JINBOZHOU MATERIAL Co.,Ltd. |
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