CN110344052A - A method of superhard Ti10CoCrNiFeNbx high entropy alloy coating is prepared on high purity titanium surface - Google Patents
A method of superhard Ti10CoCrNiFeNbx high entropy alloy coating is prepared on high purity titanium surface Download PDFInfo
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- CN110344052A CN110344052A CN201910691988.3A CN201910691988A CN110344052A CN 110344052 A CN110344052 A CN 110344052A CN 201910691988 A CN201910691988 A CN 201910691988A CN 110344052 A CN110344052 A CN 110344052A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
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Abstract
The invention discloses one kind to prepare superhard Ti on high purity titanium surface10CoCrNiFeNbxThe method of high entropy alloy coating, comprising the following steps: pre-process high purity titanium workpiece；Using PVA organic solvent by ingredient be Ti10CoCrFeNiNbxMetal powder be mixed into paste, be coated in pretreated workpiece surface, be then coated with Ti10CoCrFeNiNbxThe workpiece of high entropy alloy coating, which is placed in drying box, dries, the Ti10CoCrFeNiNbxHigh-entropy alloy is made of Ti, Co, Cr, Fe, Ni and Nb, wherein Co, Cr, Fe and Ni molar fraction having the same, and the molar fraction of Ti is 10at.%, x=0-2at.%；Treated workpiece preset to coating carries out cladding laser surfaces processing；The workpiece handled through cladding laser surfaces is taken out, the surface of workpiece is polished flat.It is provided by the invention to prepare superhard Ti on high purity titanium surface10CoCrNiFeNbxThe method of high entropy alloy coating, meet the performance variation law of high purity titanium material, the mechanical properties such as high purity titanium microhardness and intensity can be effectively improved, make its case depth and tissue more fine uniform, and method process is easy to operate, equipment is simple, economical and practical, technically reliable is high-efficient, quality stabilization is, it can be achieved that preferable economic benefit.
Description
Technical field
The present invention relates to metal material surface working process technical fields, and in particular to a kind of super in the preparation of high purity titanium surface
Hard Ti10CoCrNiFeNbxThe method of high entropy alloy coating.
Background technique
Cladding laser surfaces technology, as a kind of modern process for modifying surface, because can obtain thickness is controllable, quality is high,
The good coating with matrix conjugation, to significantly change the surface hardness of material, wearability, corrosion resistance and high-temperature behavior.In recent years
Come, cladding laser surfaces technology is also widely paid close attention to by researcher due to having the advantages that easy to operate, processing cost is low etc.
With application, it is the laser beam using high-energy density, and one or more alloying elements and substrate surface rapidly solidification are formed
The metallurgical bonding layer of even compact, so as to improve metal and the surface property of alloy.
Pure titanium has many advantages, such as specific strength height, fine corrosion resistance, good biocompatibility, aerospace, ocean and
The fields such as chemical industry are widely used.However, compared with other high-intensitive titanium alloys, the abrasion resistance properties of pure titanium compared with
Difference often shows lower tribological property under friction duty, and surface abrasion fails frequent occurrence, and this severely limits it
Service reliability.With pure titanium in the industry using increasing, higher want is proposed to the performance of pure titanium material
It asks, including abrasion resistance properties, corrosion resistance, biocompatibility etc., it is therefore desirable to improve the surface property of pure titanium material.
Summary of the invention
Present invention seek to address that the above-mentioned technical problems in the prior art, are intended to provide a kind of intensive treatment process behaviour
Work is convenient, equipment is simple, economical and practical, technically reliable, the high-efficient method for obtaining superhard coating on high purity titanium surface, improves
The surface mechanical properties such as microhardness, intensity and the wear-resisting property of high purity titanium material surface.
In order to realize above-mentioned purpose of the invention, the present invention the following technical schemes are provided:
One kind preparing superhard Ti on high purity titanium surface10CoCrFeNiNbxThe method of high entropy alloy coating, including following step
It is rapid:
1) preparation of workpiece: high purity titanium workpiece is pre-processed；
2)Ti10CoCrFeNiNbxThe preset processing of high entropy alloy coating: it is by ingredient using PVA organic solvent
Ti10CoCrFeNiNbxMetal powder be mixed into paste, be coated in pretreated workpiece surface, be then coated with
Ti10CoCrFeNiNbxThe workpiece of high entropy alloy coating, which is placed in drying box, dries, the Ti10CoCrFeNiNbxHigh-entropy alloy by
Ti, Co, Cr, Fe, Ni and Nb composition, wherein Co, Cr, Fe and Ni molar fraction having the same, the molar fraction of Ti are
10at.%, x=0-2at.%；
3) the cladding laser surfaces processing of workpiece: treated workpiece preset to coating carries out cladding laser surfaces processing；
4) workpiece handled through cladding laser surfaces is taken out, the surface of workpiece is polished flat.
In a preferred embodiment of the present invention, the pretreatment of step 1) the high purity titanium workpiece includes: successively to select
400#, 800#, 1000#, 1200#, 2000# and 3000# sand paper are clear with dehydrated alcohol after the completion of polishing by grinding workpieces to light
It washes, and dries up the surface of workpiece.
In a preferred embodiment of the present invention, in the step 2): the PVA organic solvent concentration is 6-10wt.%,
The Ti10CoCrFeNiNbxThe pre-set thickness of high entropy alloy coating is 500-600 μm, and drying temperature is 100-130 DEG C, dry
Time 4-6h.
In a preferred embodiment of the present invention, the cladding laser surfaces processing of the step 3) workpiece includes: using lazy
Property gas be protective gas, laser power 50-250W, pulse width 3-6ms, defocusing amount 0-4mm, scanning speed 5-
10mm/s。
In a preferred embodiment of the present invention, the cladding laser surfaces processing of the step 3) workpiece includes: using lazy
Property gas be protective gas, laser power 100W, pulse width 5ms, defocusing amount 2mm, scanning speed 8mm/s.
In a preferred embodiment of the present invention, inert gas described in the step 3) is argon gas.
Compared with prior art, the invention has the following beneficial effects:
The present invention prepares certain depth in high purity titanium material surface using the method that pulse laser surface cladding is handled
Ti10CoCrFeNiNbx(molar fraction of x=0-2at.%, Ti are 10at.%, and having the same mole of Co, Cr, Fe, Ni
Score) high entropy alloy coating, and control effectively by adjusting laser processing parameter and coating pre-set thickness.The present invention passes through
The high purity titanium material surface of pulse laser surface cladding high entropy alloy coating forms dendritic crystalline institutional framework, and modified layer depth reaches
500 μm, hardness is up to 800~1200HV, and more high-purity Titanium base promotes 6~10 times.Test result is shown, provided by the invention to swash
The processing method of optical surface cladding high entropy alloy coating meets the performance variation law of high purity titanium material, can be effectively improved high purity titanium
The mechanical properties such as microhardness and intensity make its case depth and tissue more fine uniform.And intensive treatment process operates
Convenient, equipment is simple, economical and practical, technically reliable, high-efficient, and quality stabilization is, it can be achieved that preferable economic benefit.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 a to Fig. 1 c is the XRD test knot of the high-entropy alloy metal powder and coating after processing before laser treatment of the present invention
Fruit.
Fig. 2 is Ti of the present invention10CoCrFeNiNbxThe metallurgical microscopic image of high entropy alloy coating.
Fig. 3 is the high-purity Titanium base of the present invention and coating Ti10CoCrFeNiNbxThe hardness test of the workpiece of high entropy alloy coating
As a result.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not thereby limiting the invention.
Experimental method in following embodiments is unless otherwise instructed conventional method.
Embodiment 1
The high purity titanium sample of 9 × 17mm of preparation is chosen, successively selects 400#, 800#, 1000#, 1200#, 2000# first
Sample is polishing to light with 3000# sand paper.Washes of absolute alcohol is used after the completion of sample polishing, finally dries up its surface.By table
Sample after face cleans up is placed on dedicated carrier, using PVA organic solvent by ingredient be Ti10CoCrFeNiNbx(x=
The molar fraction of 0at.%, Ti be 10at.%, and Co, Cr, Fe, Ni molar fraction having the same) metal powder be mixed into
Paste is coated in workpiece surface, is subsequently placed in drying box and dries, the technological parameter of the preset processing of coating are as follows: PVA organic solvent
Concentration is 6wt.%, 500-600 μm of coating pre-set thickness；Drying temperature is 120 DEG C, drying time 6h.Wherein, dry temperature
Degree and the adjustment of the drying time property of can be chosen, for example, dry temperature is 100-130 DEG C, drying time 4-6h.
By the sample clamping after drying on dedicated fixture, it is put on the station of the operating room of pulse laser equipment, and
Using purity is 99.9% argon gas as protective gas.Starting impulse laser equipment, on-load voltage, to the table of high purity titanium material
Face carries out the processing of pulse laser surface cladding.The major parameter of pulse laser surface cladding processing are as follows: laser power 100W, energy
Density 12.5J/mm2, pulse width 5ms, defocusing amount 2mm, scanning speed 8mm/s.Wherein, pulse laser surface cladding is handled
The adjustment of the main technologic parameters property of can be chosen, for example, laser power can be 50-250W, pulse width can be 3-6ms, defocus
Amount can be 0-4mm, and scanning speed can be 5-10mm/s.
The workpiece handled through cladding laser surfaces is taken out, the surface of workpiece is polished flat, is coated with
Ti10CoCrFeNiNbx(molar fraction of x=0at.%, Ti are 10at.%, and having the same mole point of Co, Cr, Fe, Ni
Number) alloy coat workpiece.
Ti before laser treatment10CoCrFeNiNbx(molar fraction of x=0at.%, Ti be 10at.%, and Co, Cr, Fe,
Ni molar fraction having the same) the XRD test result of coating is as shown in Figure 1a after metal powder and processing, and it is wherein bent in Fig. 1 a
Line A is the test result of the metal powder of the present embodiment, and curve B is the test result of coating after the present embodiment processing.After tested
The modified layer of pine-tree structure tissue is formed using cladding laser surfaces processing method of the present invention treated high purity titanium surface, it is modified
Layer depth reaches 500 μm.
Embodiment 2
The high purity titanium sample of 9 × 17mm of preparation is chosen, successively selects 400#, 800#, 1000#, 1200#, 2000# first
Sample is polishing to light with 3000# sand paper.Washes of absolute alcohol is used after the completion of sample polishing, finally dries up its surface.By table
Sample after face cleans up is placed on dedicated carrier, using PVA organic solvent by ingredient be Ti10CoCrFeNiNbx(x=
The molar fraction of 1at.%, Ti are 10at.%, and Co, Cr, Fe, Ni molar fraction having the same；That is, in this embodiment,
Co, Cr, Fe, Ni, Nb molar fraction having the same) metal powder be mixed into paste, be coated in workpiece surface, be subsequently placed in
It is dried in drying box, the technological parameter of the preset processing of coating are as follows: PVA organic solvent concentration 8wt.%, coating pre-set thickness 500-
600 μm, 120 DEG C of drying temperature, drying time 6h.The adjustable range of drying temperature is 100-130 DEG C, and drying time is adjustable
Range be 4-6h.
By the sample clamping after drying on dedicated fixture, it is put on the station of the operating room of pulse laser equipment, and
Using purity is 99.9% argon gas as protective gas.Starting impulse laser equipment, on-load voltage, to the table of high purity titanium material
Face carries out the processing of pulse laser surface cladding.The major parameter of pulse laser surface cladding processing are as follows: laser power 100W, energy
Density 12.5J/mm2, pulse width 5ms, defocusing amount 2mm, scanning speed 8mm/s.Wherein, pulse laser surface cladding is handled
The adjustment of the main technologic parameters property of can be chosen, for example, laser power can be 50-250W, pulse width can be 3-6ms, defocus
Amount can be 0-4mm, and scanning speed can be 5-10mm/s.
The workpiece handled through cladding laser surfaces is taken out, the surface of workpiece is polished flat, is coated with
Ti10CoCrFeNiNbx(molar fraction of x=1at.%, Ti are 10at.%, and having the same mole point of Co, Cr, Fe, Ni
Number) alloy coat workpiece.
Ti before laser treatment10CoCrFeNiNbx(molar fraction of x=1at.%, Ti be 10at.%, and Co, Cr, Fe,
Ni molar fraction having the same) the XRD test result of coating is as shown in Figure 1 b after metal powder and processing, and it is wherein bent in Fig. 1 b
Line A is the test result of the metal powder of the present embodiment, and curve B is the test result of coating after the present embodiment processing.High purity titanium
The Ti of surface laser cladding10CoCrFeNiNbx(molar fraction of x=1at.%, Ti are 10at.%, and Co, Cr, Fe, Ni have
Having identical molar fraction) metallurgical microscopic image of high entropy alloy coating is as shown in Fig. 2, from Figure 2 it can be seen that utilize this hair after tested
Bright cladding laser surfaces processing method treated high purity titanium surface forms the modified layer of pine-tree structure tissue, and modified layer depth reaches
To 500 μm.
Embodiment 3
The high purity titanium sample of 9 × 17mm of preparation is chosen, successively selects 400#, 800#, 1000#, 1200#, 2000# first
Sample is polishing to light with 3000# sand paper.Washes of absolute alcohol is used after the completion of sample polishing, finally dries up its surface.By table
Sample after face cleans up is placed on dedicated carrier, using PVA organic solvent by ingredient be Ti10CoCrFeNiNbx(x=
The molar fraction of 2at.%, Ti be 10at.%, and Co, Cr, Fe, Ni molar fraction having the same) metal powder be mixed into
Paste is coated in workpiece surface, is subsequently placed in drying box and dries, the technological parameter of the preset processing of coating are as follows: PVA organic solvent
Concentration 10wt.%, 500-600 μm of coating pre-set thickness, 120 DEG C of drying temperature, drying time 6h.Wherein, drying temperature is adjustable
Whole range is 100-130 DEG C, and drying time adjustable range is 4-6h.
By the sample clamping after drying on dedicated fixture, it is put on the station of the operating room of pulse laser equipment, and
Using purity is 99.9% argon gas as protective gas.Starting impulse laser equipment, on-load voltage, to the table of high purity titanium material
Face carries out the processing of pulse laser surface cladding.The major parameter of pulse laser surface cladding processing are as follows: laser power 100W, energy
Density 12.5J/mm2, pulse width 5ms, defocusing amount 2mm, scanning speed 8mm/s.Wherein, pulse laser surface cladding is handled
The adjustment of the main technologic parameters property of can be chosen, for example, laser power can be 50-250W, pulse width can be 3-6ms, defocus
Amount can be 0-4mm, and scanning speed can be 5-10mm/s.
The workpiece handled through cladding laser surfaces is taken out, the surface of workpiece is polished flat, is coated with
Ti10CoCrFeNiNbx(molar fraction of x=2at.%, Ti are 10at.%, and having the same mole point of Co, Cr, Fe, Ni
Number) alloy coat workpiece.
Ti before laser treatment10CoCrFeNiNbx(molar fraction of x=2at.%, Ti be 10at.%, and Co, Cr, Fe,
Ni molar fraction having the same) after metal powder and processing coating XRD test result as illustrated in figure 1 c, it is wherein bent in Fig. 1 c
Line A is the test result of the metal powder of the present embodiment, and curve B is the test result of coating after the present embodiment processing.After tested
The modified layer of pine-tree structure tissue is formed using cladding laser surfaces processing method of the present invention treated high purity titanium surface, it is modified
Layer depth reaches 500 μm.
Hardness test result such as Fig. 3 institute of the cated workpiece of the tool obtained of high purity titanium workpiece substrate and embodiment 1-3
Show.Wherein, the hardness of pure Titanium base is 120HV or so, and embodiment 1 is obtained to have Ti10CoCrFeNiNbx(x=0at.%,
The molar fraction of Ti is 10at.%, and Co, Cr, Fe, Ni molar fraction having the same) workpiece hardness of surface covering is up to
800HV (indicates) that purer Titanium base promotes 6 times or more with Nb0 in Fig. 3.Embodiment 2 is obtained to have Ti10CoCrFeNiNbx(x
The molar fraction of=1at.%, Ti be 10at.%, and Co, Cr, Fe, Ni molar fraction having the same) coating workpiece it is hard
Degree is up to 1000HV (indicating in Fig. 3 with Nb1), and purer Titanium base promotes 8 times or more.Have made from embodiment 3
Ti10CoCrFeNiNbx(molar fraction of x=2at.%, Ti are 10at.%, and having the same mole point of Co, Cr, Fe, Ni
Number) hardness of workpiece of coating is up to 1200HV (being indicated in Fig. 3 with Nb2), and purer Titanium base promotes 10 times or more.
The present invention coats a kind of specific high-entropy alloy Ti on high-purity Titanium base10CoCrFeNiNbx(x=0-2at.%,
The molar fraction of Ti be 10at.%, and Co, Cr, Fe, Ni molar fraction having the same), by adjusting the composition of high-entropy alloy
Ingredient, coating pre-set thickness and laser melting coating parameter etc. control effectively to high purity titanium matrix surface coating.The present invention is logical
Extra pulse cladding laser surfaces are by special high-entropy alloy Ti10CoCrFeNiNbx(molar fraction of x=0-2at.%, Ti is
10at.%, and Co, Cr, Fe, Ni molar fraction having the same) it is coated in high purity titanium workpiece surface, gained high entropy alloy coating
High purity titanium material surface form dendritic crystalline institutional framework, modified layer depth reaches 500 μm, and hardness is up to 800~1200HV, compared with
High-purity Titanium base promotes 6~10 times.Test result shows, the processing of cladding laser surfaces high entropy alloy coating provided by the invention
Method meets the performance variation law of high purity titanium material, can be effectively improved the mechanical properties such as high purity titanium microhardness and intensity, make
Its case depth and tissue more fine uniform.And intensive treatment process is easy to operate, equipment is simple, economical and practical, technology
Reliably, high-efficient, quality stabilization is, it can be achieved that preferable economic benefit.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that: not
A variety of change, modification, replacement and modification can be carried out to these embodiments in the case where being detached from the principle of the present invention and objective, this
The range of invention is defined by the claims and their equivalents.
Claims (5)
1. one kind prepares superhard Ti on high purity titanium surface10CoCrNiFeNbxThe method of high entropy alloy coating, which is characterized in that packet
Include following steps:
1) preparation of workpiece: high purity titanium workpiece is pre-processed；
2)Ti10CoCrFeNiNbxThe preset processing of high entropy alloy coating: it is by ingredient using PVA organic solvent
Ti10CoCrFeNiNbxMetal powder be mixed into paste, be coated in pretreated workpiece surface, be then coated with
Ti10CoCrFeNiNbxThe workpiece of high entropy alloy coating, which is placed in drying box, dries, the Ti10CoCrFeNiNbxHigh-entropy alloy by
Ti, Co, Cr, Fe, Ni and Nb composition, wherein Co, Cr, Fe and Ni molar fraction having the same, the molar fraction of Ti are
10at.%, x=0-2at.%；
3) the cladding laser surfaces processing of workpiece: treated workpiece preset to coating carries out cladding laser surfaces processing；
4) workpiece handled through cladding laser surfaces is taken out, the surface of workpiece is polished flat.
2. one kind as described in claim 1 prepares superhard Ti on high purity titanium surface10CoCrNiFeNbxThe side of high entropy alloy coating
Method, which is characterized in that the pretreatment of step 1) the high purity titanium workpiece include: successively select 400#, 800#, 1000#, 1200#,
Grinding workpieces to light are used washes of absolute alcohol after the completion of polishing by 2000# and 3000# sand paper, and dry up the surface of workpiece.
3. one kind as described in claim 1 prepares superhard Ti on high purity titanium surface10CoCrNiFeNbxThe side of high entropy alloy coating
Method, which is characterized in that in the step 2): the PVA organic solvent concentration is 6-10wt.%, the Ti10CoCrFeNiNbx
The pre-set thickness of high entropy alloy coating is 500-600 μm, and drying temperature is 100-130 DEG C, drying time 4-6h.
4. one kind as described in claim 1 prepares superhard Ti on high purity titanium surface10CoCrNiFeNbxThe side of high entropy alloy coating
Method, which is characterized in that the cladding laser surfaces processing of the step 3) workpiece includes: to use inert gas for protective gas, is swashed
Optical power is 50-250W, pulse width 3-6ms, defocusing amount 0-4mm, scanning speed 5-10mm/s.
5. one kind as described in claim 1 prepares superhard Ti on high purity titanium surface10CoCrNiFeNbxThe side of high entropy alloy coating
Method, which is characterized in that the cladding laser surfaces processing of the step 3) workpiece includes: to use inert gas for protective gas, is swashed
Optical power is 100 W, pulse width 5ms, defocusing amount 2mm, scanning speed 8mm/s.
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| CN111139471A (en) * | 2020-02-10 | 2020-05-12 | 重庆理工大学 | Method for preparing superhard Zr on surface of zirconium alloyxMethod for CrCoFeNi high-entropy alloy coating |
| CN111172532A (en) * | 2020-02-18 | 2020-05-19 | 重庆理工大学 | Method for preparing medium-entropy alloy coating on surface of pure titanium plate |
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Application publication date: 20191018 |