CN110724949A - Preparation method of high-entropy alloy layer on surface of medical beta titanium alloy - Google Patents
Preparation method of high-entropy alloy layer on surface of medical beta titanium alloy Download PDFInfo
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- CN110724949A CN110724949A CN201911106992.5A CN201911106992A CN110724949A CN 110724949 A CN110724949 A CN 110724949A CN 201911106992 A CN201911106992 A CN 201911106992A CN 110724949 A CN110724949 A CN 110724949A
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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
- C23C24/02—Coating starting from inorganic powder by application of pressure only
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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
- C22C30/06—Alloys containing less than 50% by weight of each constituent containing zinc
Abstract
The invention provides a preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy, wherein the high-entropy alloy layer comprises titanium, niobium, hafnium, zinc and zirconium, and the preparation method comprises the following steps: A. performing ball milling treatment on the high-entropy alloy powder; B. processing the medical beta titanium alloy, and then paving the high-entropy alloy powder treated in the step A; C. performing first stirring friction processing by adopting a needleless stirring head; D. and (5) carrying out secondary friction stir processing by adopting a pin stirring head. The preparation method is simple, the prepared surface high-entropy alloy layer can effectively improve the mechanical property of the medical beta titanium alloy, simultaneously reduces the application cost of the high-entropy alloy, and can be widely applied to the preparation of the alloy surface high-entropy alloy layer.
Description
Technical Field
The invention belongs to the field of high-entropy alloy materials, and particularly relates to a preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy.
Background
Medical beta titanium and titanium alloys are widely used in the field of dental and orthopedic implants because of their high strength, low Young's modulus, excellent corrosion resistance and good biocompatibility. The traditional metal and the alloy thereof can bring the problem of poor alloy plasticity and toughness while obviously improving the alloy strength and hardness.
Recent studies have shown that a solid-solution high-entropy alloy in which five or more metal elements are mixed at an equal atomic ratio or a near-equal atomic ratio has excellent properties in strength, hardness, work hardening, wear resistance, high-temperature stability, corrosion resistance, and the like, as compared with conventional alloys.
In the prior art, a high-entropy alloy layer is generally formed on a titanium alloy surface by laser melting, for example, patent document CN106591626A discloses a TA18 titanium alloy composite material composed of a TA18 titanium alloy substrate and a high-entropy alloy layer, wherein the high-entropy alloy layer comprises the following components in percentage by atom: ti: v is 1: 1.5-2, V: cr is 1: 0.9 to 1.1, V: al is 1: 0.9 to 1.1, V: mn is 1: 0.9 to 1.1; the composite material is obtained by depositing a high-entropy alloy on the surface of a titanium alloy by using a laser. But this method can only yield similar high entropy alloy layers.
The invention prepares the high-entropy alloy layer on the surface of the medical beta titanium alloy, and has important significance for developing the preparation technology of the high-entropy alloy, promoting the research of the high-entropy alloy and the application in the field of biological materials.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy, which has simple preparation process flow and effectively improves the mechanical property of the medical beta titanium alloy.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy, which comprises the following steps:
A. performing ball milling treatment on the high-entropy alloy powder;
B. processing the medical beta titanium alloy, and then paving the high-entropy alloy powder treated in the step A;
C. performing first stirring friction processing by adopting a needleless stirring head;
D. and (5) carrying out secondary friction stir processing by adopting a pin stirring head.
Preferably, in the step A, the high-entropy alloy powder is prepared by mixing titanium, niobium, hafnium, zinc and zirconium element powder in an equimolar way, and the particle size of each element powder is 20-200nm, and is more preferably 50 nm.
Preferably, in the step A, the ball milling treatment time is 24 hours, the ball-to-material ratio is 4:1-10:1, and the ball milling rotation speed is 200-400 r/min.
Preferably, in the step a, the processing specifically includes processing a groove on the surface of the medical beta titanium alloy; the width of the groove is 1-3mm, and the depth is 0.5-2 mm.
Preferably, in steps C and D, the material of the pin-less stirring head and the pin-containing stirring head is tungsten-rhenium alloy.
Preferably, in step C, the diameter of the shaft shoulder of the pin-free stirring head is 8-14mm, and more preferably 12 mm.
Preferably, in the step D, the shaft shoulder of the pin stirring head is 8-14mm, and more preferably 12 mm; the diameter of the root part of the stirring pin with the pin stirring head is 4-6mm, the diameter of the end part of the stirring pin is 3-4mm, and the length of the stirring pin is 1.5-1.8 mm.
Preferably, in the step C, the first friction stir processing is performed along the groove direction, and the rotating speed of the stirring head is controlled to be 100-. The advancing speed is 30-60mm/min, so that the problem that the local temperature of the plate is too high due to too low advancing speed or the protective layer cannot be formed due to too high advancing speed is solved. And processing for 1 pass to prevent the powder laid in the groove from being extruded in the stirring and friction processing process of the pin-containing stirring head.
Preferably, in the step D, the second friction stir processing is performed along the groove direction, the rotation speed of the stirring head is controlled to be 200-500r/min, the advancing speed is 30-60mm/min, and the high-entropy alloy layer is formed by processing for 1 pass.
The invention adopts the technology of friction stir processing to simultaneously change the matrix structure performance and obtain the high-entropy alloy layer.
The invention also provides a high-entropy alloy layer on the surface of the medical beta titanium alloy, which is obtained by mixing the powders of titanium, niobium, hafnium, zinc and zirconium in equal mol.
Compared with the prior art, the invention has the following beneficial effects:
1. the method provides a multi-principal-element high-entropy alloy material, and the high-entropy alloy material is a titanium niobium hafnium zinc zirconium multi-principal-element system.
2. The high-entropy alloy layer prepared by the method has the advantages of simple process, low cost of required materials and low energy consumption, and effectively promotes the industrial application of the high-entropy alloy.
3. The method of the invention prepares the high-entropy alloy layer on the surface of the medical beta titanium alloy, and can effectively improve the mechanical property of the titanium alloy.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The following embodiment provides a preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy, which comprises the following steps:
A. performing ball milling treatment on the high-entropy alloy powder;
B. processing the medical beta titanium alloy, and then paving the high-entropy alloy powder treated in the step A;
C. performing first stirring friction processing by adopting a needleless stirring head;
D. and (5) carrying out secondary friction stir processing by adopting a pin stirring head.
In the step A, the high-entropy alloy powder is prepared by mixing titanium, niobium, hafnium, zinc and zirconium element powder in equal molar ratio, and the granularity of each element powder is 20-200.
In the step A, the ball milling treatment time is 24 hours, the ball-material ratio is 4:1-10:1, and the ball milling rotating speed is 200-.
In the step A, the processing is specifically to process a groove on the surface of the medical beta titanium alloy; the width of the groove is 1-3mm, and the depth is 0.5-2 mm.
In the steps C and D, the needle-free stirring head and the needle-containing stirring head are made of tungsten-rhenium alloy.
In the step C, the diameter of the shaft shoulder of the needleless stirring head is 8-14 mm.
In the step D, the shaft shoulder of the stirring head with the needle is 8-14 mm; the diameter of the root part of the stirring pin with the pin stirring head is 4-6mm, the diameter of the end part of the stirring pin is 3-4mm, and the length of the stirring pin is 1.5-1.8 mm.
In the step C, the first friction stir processing is carried out along the groove direction, and the rotating speed of the stirring head is controlled to be 100-300r/min, so that the problem that the stirring head is difficult to advance due to too low rotating speed and too low plate temperature or more fins are generated on the plate due to too high rotating speed is solved. The advancing speed is 30-60mm/min, so that the problem that the local temperature of the plate is too high due to too low advancing speed or the protective layer cannot be formed due to too high advancing speed is solved. And processing for 1 pass to prevent the powder laid in the groove from being extruded in the stirring and friction processing process of the pin-containing stirring head.
In the step D, the second stirring friction processing is carried out along the groove direction, the rotating speed of the stirring head is controlled to be 200-.
The high-hardness high-entropy alloy layer can be prepared on the surface of the titanium alloy under the conditions.
Example 1
The embodiment relates to a preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy, which comprises the following specific steps:
step one, selecting titanium, niobium, hafnium, zinc and zirconium as raw materials, weighing the raw materials according to equal molar ratio, and uniformly mixing the raw materials, wherein the granularity of the raw materials is 50nm, and the purity of the raw materials is more than 99.9%; and (3) carrying out ball milling by using a QM-WX04 horizontal planetary ball mill, wherein the ball-to-material ratio in the ball milling process is 4:1, the rotating speed is 200r/min, and the high-entropy alloy powder is taken out after ball milling is carried out for 24 hours.
Fixing the medical beta titanium alloy plate on a workbench of friction stir processing equipment by using a clamp, processing a groove and paving high-entropy alloy powder; the width of the groove is 1mm, and the depth is 1 mm.
Step three, the first friction stir processing process treatment: and under the argon protection atmosphere, performing friction stir processing in the groove direction by using a needleless stirring head, wherein the processing pass is 1 pass. The stirring head is made of tungsten-rhenium alloy, the shaft shoulder of the stirring head is 12mm, and the diameter of the stirring head is 12 mm. The friction stir processing is realized by the high-speed rotation and movement of the stirring head, the rotating speed of the stirring head is 150r/min, and the advancing speed is 30 mm/min.
Step four, the second friction stir processing process treatment: and under the argon protection atmosphere, carrying out friction stir processing in the groove direction of the pin-containing stirring head, wherein the processing pass is 1 pass. The stirring head is made of tungsten-rhenium alloy, the shaft shoulder of the stirring head is 12mm, the diameter of the root of the stirring head is 5mm, the diameter of the end part of the stirring head is 3mm, and the length of the needle is 1.7 mm. In the process of friction stir processing, the rotating speed of the stirring head is 225r/min, and the advancing speed is 40 mm/min.
The mechanical property test result of the medical beta titanium alloy with the high-entropy alloy layer on the surface prepared by the embodiment is as follows: the hardness of the high-entropy alloy layer can reach 2.96GPa measured by a nano indentation experiment,
compared with the prior medical beta titanium alloy with the hardness of 2.36GPa, the hardness is improved by 25.4 percent.
Example 2
The embodiment relates to a preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy, which comprises the following specific steps:
step one, selecting titanium, niobium, hafnium, zinc and zirconium as raw materials, weighing the raw materials according to equal molar ratio, and uniformly mixing the raw materials, wherein the granularity of the raw materials is 50nm, and the purity of the raw materials is more than 99.9%; and (3) carrying out ball milling by using a QM-WX04 horizontal planetary ball mill, wherein the ball-to-material ratio in the ball milling process is 4:1, the rotating speed is 200r/min, and the high-entropy alloy powder is taken out after ball milling is carried out for 24 hours.
Fixing the medical beta titanium alloy plate on a workbench of friction stir processing equipment by using a clamp, processing a groove and paving high-entropy alloy powder; the width of the groove is 1.5mm, and the depth is 1.5 mm.
Step three, the first friction stir processing process treatment: and under the argon protection atmosphere, performing friction stir processing along the groove direction by using a needleless stirring head, wherein the processing pass is 1 pass. The stirring head is made of tungsten-rhenium alloy, the shaft shoulder of the stirring head is 12mm, and the diameter of the stirring head is 12 mm. The friction stir processing is realized by the high-speed rotation and movement of the stirring head, the rotating speed of the stirring head is 225r/min, and the advancing speed is 40 mm/min.
Step four, the second friction stir processing process treatment: and under the argon protection atmosphere, carrying out friction stir processing in the groove direction of the pin-containing stirring head, wherein the processing pass is 1 pass. The stirring head is made of tungsten-rhenium alloy, the shaft shoulder of the stirring head is 12mm, the diameter of the root of the stirring head is 5mm, the diameter of the end part of the stirring head is 3mm, and the length of the needle is 1.7 mm. In the process of friction stir processing, the rotating speed of the stirring head is 300r/min, and the advancing speed is 50 mm/min.
The mechanical property test result of the medical beta titanium alloy with the high-entropy alloy layer on the surface prepared by the embodiment is as follows: the hardness of the high-entropy alloy layer can reach 3.34GPa measured by a nano indentation experiment,
compared with the prior medical beta titanium alloy with the hardness of 2.36GPa, the hardness is improved by 41.5 percent.
Example 3
The embodiment relates to a preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy, which comprises the following specific steps:
step one, selecting titanium, niobium, hafnium, zinc and zirconium as raw materials, weighing the raw materials according to equal molar ratio, and uniformly mixing the raw materials, wherein the granularity of the raw materials is 50nm, and the purity of the raw materials is more than 99.9%; and (3) carrying out ball milling by using a QM-WX04 horizontal planetary ball mill, wherein the ball-to-material ratio in the ball milling process is 4:1, the rotating speed is 200r/min, and the high-entropy alloy powder is taken out after ball milling is carried out for 24 hours.
Fixing the medical beta titanium alloy plate on a workbench of friction stir processing equipment by using a clamp, processing a groove and paving high-entropy alloy powder; the groove width is 2mm, and the depth is 2 mm.
Step three, the first friction stir processing process treatment: and under the argon protection atmosphere, performing friction stir processing in the groove direction by using a needleless stirring head, wherein the processing pass is 1 pass. The stirring head is made of tungsten-rhenium alloy, the shaft shoulder of the stirring head is 12mm, and the diameter of the stirring head is 12 mm. The friction stir processing is realized by the high-speed rotation and movement of the stirring head, the rotating speed of the stirring head is 300r/min, and the advancing speed is 50 mm/min.
Step four, the second friction stir processing process treatment: and under the argon protection atmosphere, carrying out friction stir processing in the groove direction of the pin-containing stirring head, wherein the processing pass is 1 pass. The stirring head is made of tungsten-rhenium alloy, the shaft shoulder of the stirring head is 12mm, the diameter of the root of the stirring head is 5mm, the diameter of the end part of the stirring head is 3mm, and the length of the needle is 1.7 mm. In the process of friction stir processing, the rotating speed of the stirring head is 375r/min, and the advancing speed is 60 mm/min.
The mechanical property test result of the medical beta titanium alloy with the high-entropy alloy layer on the surface prepared by the embodiment is as follows: the hardness of the high-entropy alloy layer can reach 3.22GPa measured by a nano indentation experiment,
compared with the prior medical beta titanium alloy with the hardness of 2.36GPa, the hardness is improved by 36.4 percent.
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (10)
1. A preparation method of a high-entropy alloy layer on the surface of a medical beta titanium alloy is characterized by comprising the following steps:
A. performing ball milling treatment on the high-entropy alloy powder;
B. processing the medical beta titanium alloy, and then paving the high-entropy alloy powder treated in the step A;
C. performing first stirring friction processing by adopting a needleless stirring head;
D. and (5) carrying out secondary friction stir processing by adopting a pin stirring head.
2. The method for preparing the high-entropy alloy layer on the surface of the medical beta titanium alloy according to claim 1, wherein in the step A, the high-entropy alloy powder is prepared by mixing titanium, niobium, hafnium, zinc and zirconium element powder in an equimolar way, and the granularity of each element powder is 20-200 nm.
3. The method for preparing the high-entropy alloy layer on the surface of the medical beta titanium alloy as claimed in claim 1, wherein in the step A, the ball milling time is 24 hours, the ball-to-material ratio is 4:1-10:1, and the ball milling rotation speed is 200-.
4. The method for preparing the high-entropy alloy layer on the surface of the medical beta titanium alloy according to claim 1, wherein in the step A, the processing is specifically to process a groove on the surface of the medical beta titanium alloy; the width of the groove is 1-3mm, and the depth is 0.5-2 mm.
5. The method for preparing a high-entropy alloy layer on the surface of a medical beta titanium alloy according to claim 1, wherein in the steps C and D, the material of the pin-less stirring head and the pin-containing stirring head is tungsten-rhenium alloy.
6. The method for preparing a high-entropy alloy layer on the surface of a medical beta titanium alloy according to claim 1, wherein in the step C, the diameter of a shaft shoulder of the pin-less stirring head is 8-14 mm.
7. The method for preparing a high-entropy alloy layer on the surface of a medical beta titanium alloy according to claim 1, wherein in the step D, the shoulder of the stirring head with the needle is 8-14 mm; the diameter of the root part of the stirring pin with the pin stirring head is 4-6mm, the diameter of the end part of the stirring pin is 3-4mm, and the length of the stirring pin is 1.5-1.8 mm.
8. The method for preparing a high-entropy alloy layer on the surface of a medical beta titanium alloy as claimed in claim 1, wherein in the step C, the first friction stir processing is performed along the groove direction, the rotation speed of the stirring head is controlled to be 100-300r/min, the advancing speed is controlled to be 30-60mm/min, and the processing is performed for 1 pass.
9. The method for preparing a high-entropy alloy layer on the surface of a medical beta titanium alloy as claimed in claim 1, wherein in the step D, the second friction stir processing is performed along the groove direction, the rotation speed of the stirring head is controlled to be 200-500r/min, the advancing speed is controlled to be 30-60mm/min, and the processing is performed for 1 pass.
10. A high-entropy alloy layer on the surface of medical beta titanium alloy is characterized in that the high-entropy alloy layer is obtained by mixing powders of titanium, niobium, hafnium, zinc and zirconium in equal mol.
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