CN118048569A - Ti-Zr high-entropy alloy with low modulus and high ductility, and preparation method and application thereof - Google Patents
Ti-Zr high-entropy alloy with low modulus and high ductility, and preparation method and application thereof Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 138
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 124
- PMTRSEDNJGMXLN-UHFFFAOYSA-N titanium zirconium Chemical compound [Ti].[Zr] PMTRSEDNJGMXLN-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 229910008651 TiZr Inorganic materials 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 20
- 238000003723 Smelting Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 13
- 238000012360 testing method Methods 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000007943 implant Substances 0.000 claims description 8
- 238000005260 corrosion Methods 0.000 claims description 7
- 238000010314 arc-melting process Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910001182 Mo alloy Inorganic materials 0.000 claims description 2
- 229910001093 Zr alloy Inorganic materials 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 7
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 description 9
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 210000000988 bone and bone Anatomy 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000001727 in vivo Methods 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910000531 Co alloy Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 229910001040 Beta-titanium Inorganic materials 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
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- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
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- 229910052720 vanadium Inorganic materials 0.000 description 1
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- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a low-modulus high-ductility Ti-Zr high-entropy alloy and a preparation method and application thereof. The structural general formula of the high-entropy alloy is (TiZr) xMy, wherein x ranges from 40 to 49, and y ranges from 0.66 to 6.66; and M is an alloy containing 3 or more equielement metal elements in different molar ratios. The high-entropy alloy is based on the synergistic effect between the TiZr alloy and the M alloy, and the mechanical property and the chemical property of the high-entropy alloy are regulated and controlled by controlling the molar ratio of the alloy between the TiZr alloy and the M alloy, so that on one hand, the excellent mechanical property of the alloy material at room temperature is ensured, and meanwhile, the high-temperature stability of the alloy is improved, on the other hand, the elastic modulus of the alloy is effectively reduced, the ductility of the alloy is improved, and the application scene of the alloy material is further expanded.
Description
Technical Field
The invention relates to a Ti-Zr high-entropy alloy, in particular to a low-modulus high-ductility Ti-Zr high-entropy alloy, and a preparation method and application thereof, and belongs to the field of high-strength and high-toughness alloy materials.
Background
With the continued development of biomedical fields, biomedical materials have attracted considerable attention from researchers. The biomedical metal materials used in clinic at present mainly comprise stainless steel, titanium alloy, cobalt-based alloy and the like. However, the above materials have some disadvantages in that when SUS316L stainless steel is used in vivo, nickel ions are released due to abrasion and corrosion, causing adverse reactions such as inflammation or cell damage. Although the strength of the Ti-6Al-4V alloy is higher than that of CP-Ti and the alloy has good workability, the Al and V elements contained in the Ti-6Al-4V alloy material are considered as elements harmful to living organisms. Long-term wear of cobalt-based alloy materials in vivo can cause cobalt and nickel plasma to dissolve out, causing cell or tissue necrosis in vivo. Therefore, biomedical materials with excellent comprehensive properties (strength, plasticity, toughness, hardness, abrasion, corrosion and the like) are widely focused on the aspects of related material workers, clinicians, medical instrument manufacturing enterprises and the like.
Compared with the traditional alloy material, the high-entropy alloy is proposed and developed for the first time in 2004, and is expected to be widely applied in the biomedical field due to the high-entropy effect in thermodynamics, the slow diffusion effect in dynamics, the lattice distortion effect in structure and the cocktail effect in performance. At present, researchers respectively adopt a smelting process and a plasma arc additive manufacturing process to research and discover that a Ti-Zr-Nb-Ta-Mo high-entropy alloy system has excellent yield strength, but still has the problems of higher elastic modulus and lower ductility, and the Ti-Zr-Nb-Ta-Mo high-entropy alloy system is limited to be applied to the biomedical field as an implantation material. At present, few reports about good tensile properties of the as-cast Ti-Zr-Nb-Ta-Mo high-entropy alloy are provided, the microstructure and the composition relation of the Ti-Zr-Nb-Ta-Mo high-entropy alloy are studied, and the design of the compact Ti-Zr-Nb-Ta-Mo biomedical high-entropy alloy with excellent properties has very important significance.
Disclosure of Invention
Aiming at the problems existing in the prior art, the first aim of the invention is to provide a low-modulus high-ductility Ti-Zr high-entropy alloy which is based on the synergistic effect between TiZr alloy and M alloy, and the mechanical property and chemical property of the high-entropy alloy are regulated and controlled by controlling the molar ratio of the alloy between the TiZr alloy and the M alloy, so that on one hand, the excellent mechanical property of the alloy material at room temperature is ensured, and on the other hand, the high-temperature stability of the alloy is improved, the elastic modulus of the alloy is effectively reduced, the ductility of the alloy is improved, and the application scene of the alloy material is further expanded.
The second object of the invention is to provide a preparation method of the low-modulus high-ductility Ti-Zr high-entropy alloy, which is characterized in that high-entropy alloy samples with different proportions are obtained rapidly through a smelting process, and then the high-entropy alloy samples are screened according to a comprehensive performance threshold value, so that the optimal element ratio and the optimal process parameters in the high-entropy alloy are determined, the optimization period of the high-entropy alloy is shortened greatly, and the product with excellent performance is obtained rapidly and accurately.
The third object of the invention is to provide an application of the Ti-Zr high-entropy alloy with low modulus and high ductility as a biomedical implant material. Based on the excellent mechanical property and chemical property of the high-entropy alloy provided by the invention, the high-entropy alloy has good stability and rejection resistance for complex systems, especially biological systems, and can be used as biomedical implant materials, and the high-entropy alloy provided by the invention has the elongation of 16.5%, the wear rate of 6.2 multiplied by 10 -5mm3/N.m and the self-corrosion current density of 0.102 plus or minus 0.017 mu A/cm 2 on the premise that the mechanical property is basically unchanged.
In order to achieve the technical purpose, the invention provides a Ti-Zr high-entropy alloy with low modulus and high ductility, which is characterized in that: the structural general formula of the high-entropy alloy is (TiZr) xMy, wherein x ranges from 40 to 49, and y ranges from 0.66 to 6.66; and M is an alloy containing 3 or more equielement metal elements in different molar ratios.
As a preferable scheme, the ratio of x to y in the high-entropy alloy is 8.5-23.5:1.
As a preferred embodiment, the M alloy is a Nb-Ta-Mo alloy.
The invention takes TiZr alloy with equal molar ratio as a whole, the VEC of Ti and Zr is 4, the ductility of the high-entropy alloy can be regulated by regulating the valence electron concentration of the alloy through regulating the high VEC element in the M alloy, and Nb, ta and Mo in the M alloy are all beta stable elements, thus the low-elasticity modulus beta titanium alloy can be designed, and Mo can provide negative mixing enthalpy to achieve higher toughness and matching degree.
As a preferred embodiment, the crystal structure of the high-entropy alloy is a simple body-centered cubic structure.
The invention also provides a preparation method of the low-modulus high-ductility Ti-Zr high-entropy alloy, which comprises the following steps:
1) Proportioning Ti-Zr alloy and M alloy according to gradient in the value range of x, and obtaining a sample through smelting process;
2) And (3) testing the mechanical property and chemical property of a sample, and recording data when the comprehensive property of the sample exceeds a threshold value.
As a preferred scheme, the smelting process comprises the following steps: and (3) smelting the alloy raw materials through vacuum arc until the alloy raw materials are molten, and turning over and smelting after the alloy is cooled, wherein the repetition number is more than or equal to 10.
As a preferred solution, the vacuum arc melting process is: the alloy raw material is sent into a sample chamber, and when the vacuum degree reaches 5x10 -3 Pa, argon is introduced into the sample chamber to the pressure of 0.5atm.
As a preferable scheme, electromagnetic stirring is also needed in the vacuum arc melting process, and the current is 3-4A.
As a preferable scheme, the arc holding time in the vacuum arc melting process is 100-120 s, and the current is 300-450A.
As a preferable scheme, the threshold value of the comprehensive performance is that the tensile strain is more than 5%, the elastic modulus is less than or equal to 100GPa, the wear rate is less than or equal to 7.0X10 -5mm3/N.m, and the self-corrosion current density is less than 0.168+/-0.002 mu A/cm 2.
The invention also provides application of the Ti-Zr high-entropy alloy with low modulus and high ductility as a biomedical implant material.
Compared with the prior art, the technical scheme of the invention has the beneficial technical effects that:
1) The high-entropy alloy provided by the invention is based on the synergistic effect between the TiZr alloy and the M alloy, and the mechanical property and the chemical property of the high-entropy alloy are regulated and controlled by controlling the alloy molar ratio between the TiZr alloy and the M alloy, so that on one hand, the excellent mechanical property of the alloy material at room temperature is ensured, and on the other hand, the high-temperature stability of the alloy is improved, the elastic modulus of the alloy is effectively reduced, the ductility of the alloy is improved, and the application scene of the alloy material is further expanded.
2) According to the preparation method provided by the invention, the high-entropy alloy samples with different proportions are obtained rapidly through a smelting process, and then the high-entropy alloy samples are screened according to the comprehensive performance threshold value, so that the optimal element ratio and the optimal process parameters in the high-entropy alloy are determined, the optimization period of the high-entropy alloy is shortened greatly, and the product with excellent performance is obtained rapidly and accurately.
3) According to the technical scheme provided by the invention, based on the excellent mechanical property and chemical property of the high-entropy alloy, the high-entropy alloy has good stability and rejection resistance for complex systems, especially biological systems, and can be used as biomedical implant materials, and the high-entropy alloy provided by the invention has the elongation of 16.5%, the wear rate of 6.2 multiplied by 10 -5mm3/N.m and the self-corrosion current density of 0.102 plus or minus 0.017 mu A/cm 2 on the premise that the mechanical property is basically unchanged.
Drawings
FIG. 1 is a TEM image and an energy spectrum of the Ti42.5 high-entropy alloy material obtained in example 1 of the present invention;
fig. 2 is a TEM image and an energy spectrum of the Ti45 high-entropy alloy material obtained in example 1 of the present invention.
Detailed description of the preferred embodiments
The present application will be described in further detail with reference to the following examples, and all other examples, which can be obtained by one skilled in the art without making any inventive effort, are intended to fall within the scope of the present application. It should be understood that the detailed description is intended to illustrate the application, and is not intended to limit the application.
The specific conditions are not noted in the examples of the present invention, and are carried out according to conventional conditions or conditions suggested by the manufacturer. The raw materials, reagents, etc. used, which are not noted to the manufacturer, are conventional products commercially available. The reagents used in the examples are commercially available as usual unless otherwise specified.
Example 1
Gradient proportioning is carried out on the high-entropy alloy according to the value range of x, and the obtained high-entropy alloy expressions are respectively as follows: (TiZr) 42.5(NbTaMo)5、(TiZr)45(NbTaMo)3.33 and (TiZr) 47(NbTaMo)2, abbreviated as Ti42.5, ti45 and Ti47, respectively.
The preparation steps of the compact high-entropy alloy are as follows:
1) Raw material preparation: the alloy smelting raw materials adopted by the invention are high-purity (> 99.5%) Ti particles, zr particles, nb particles, ta particles and Mo particles, the accurate weighing proportion is carried out according to the molar proportion, and the balance with the accuracy of 0.001g is used for batching. And (3) placing the prepared raw materials into industrial ethanol for ultrasonic cleaning to remove organic pollutants on the surface of the materials.
2) Preparation of high-entropy alloy: feeding the raw materials prepared in the step 1) into a vacuum non-consumable vacuum smelting furnace, wherein Ti and Zr are placed at the bottom, nb, ta and Mo are placed at the top, the vacuum degree of a vacuum chamber of the vacuum smelting furnace is regulated to be 5x10 -3 Pa, argon is then filled into a furnace chamber to be half atmospheric pressure, the air suction and the air washing are repeated for more than 3 times, the vacuum smelting furnace is started to smelt the alloy raw materials, the arc current is 380A, smelting is repeated for 12 times until the alloy is fully and uniformly smelted, and the smelting time is 100s each time; and after the alloy is fully smelted and cooled, obtaining a high-entropy alloy primary sample with a simple body-centered cubic structure.
3) The two primary samples are subjected to tensile test by adopting a MTS E45.305 universal tester, wherein the length of the primary sample is 10mm, the cross section of the primary sample is 5X 3mm 2, and the initial strain rate of the test is 2.1X 10-4s-1; the Vickers hardness of the sample was measured using an HDX-1000TMC type Vickers hardness tester; the elastic modulus of the samples was measured on a TI950 trilo nanoindentation test apparatus using a Berkovich indenter and the test results of the samples are shown in table 1.
4) The high-entropy alloy abrasion performance test is carried out on the two primary samples respectively, and the test results are shown in table 2; the high-entropy alloy corrosion performance test was performed on each of the above two primary samples, and the test results are shown in table 3.
5) Comparing the test results obtained in the step 3) and the step 4) with a threshold value, and screening out the high-entropy alloy material with the best comprehensive performance, wherein the threshold value is a performance parameter value of Ti6Al4V under the same test condition.
TABLE 1
TABLE 2
TABLE 3 Table 3
The result shows that the elastic modulus of the high-entropy alloy is less than 100GPa and the elongation is more than 5% under three proportions, wherein the yield strength, the tensile strength and the elongation of the Ti45 alloy are all highest; the abrasion performance of Ti42.5 and Ti45 are better than that of Ti6Al4V alloy, but the abrasion performance of Ti47 is the worst, which is inferior to that of Ti6Al4V alloy, the abrasion rate reaches 2.1 multiplied by 10 -4, the threshold requirement is not met, the abrasion performance of Ti47 is better than that of Ti6Al4V alloy, in conclusion, the abrasion performance of Ti47 does not meet the threshold requirement, the abrasion performance of Ti47 does not meet the requirement of low modulus high ductility high entropy alloy, and the comprehensive performance of Ti45 is optimal, therefore, the scheme provided by the invention can realize the rapid and accurate proportioning and optimization of Ti-Zr high entropy alloy, greatly shorten the research and development period of materials, and has important guiding function on the development and research of new materials.
In the biomedical field, the mechanical strength requirement on the implant material is generally lower than that of the framework material in industry, but the requirement on the porosity and biocompatibility of the material is higher, when the high-entropy alloy is used as artificial bone, the yield strength is more than 120Mpa, the compression strength is more than 300Mpa, the porosity is different according to the implantation position, for example, the porosity is about 5% when being used as cortical bone implant, and the porosity is about 30% when being used as cancellous bone implant, therefore, in order to verify that the high-entropy alloy provided by the invention has wide biomedical applicability, the invention also carries out related pore-forming experiments on the Ti45 high-entropy alloy, and the process is as follows:
the preparation method of the porous Ti-Zr-Nb-Ta-Mo biomedical high-entropy alloy added with 0wt.% of pore-forming agent comprises the following steps:
The addition amount of the pore-forming agent is 0 wt%, 5wt%, 10 wt% and 15 wt%, and the rest raw materials are proportioned according to Ti45 high-entropy alloy and are placed in V-shaped powder mixing equipment for 24h under the protection of argon gas to be fully and uniformly mixed. And then sintering the mixed powder in a rapid hot-pressing sintering furnace at 1000 ℃ for 4 hours, wherein the mechanical pressure applied during sintering is 0MPa, and the protective atmosphere is vacuum. Namely, the porous Ti-Zr-Nb-Ta-Mo biomedical high-entropy alloy material added with 0wt.% of pore-forming agent is respectively recorded as 0wt.% HEAs, 5wt.% HEAs, 10wt.% HEAs and 15wt.% HEAs, and the mechanical property test results are shown in Table 4.
TABLE 4 Table 4
As shown in Table 4, the high-entropy alloy provided by the invention has yield strength of more than 120Mpa, compression strength of more than 300MPa, porosity of 5-30% and capability of meeting the performance requirement of artificial bones.
Claims (10)
1. A low-modulus high-ductility Ti-Zr high-entropy alloy is characterized in that: the structural general formula of the high-entropy alloy is (TiZr) xMy, wherein x ranges from 40 to 49, and y ranges from 0.66 to 6.66; and M is an alloy containing 3 or more equielement metal elements in different molar ratios.
2. The low modulus, high ductility Ti-Zr high entropy alloy of claim 1, wherein: the ratio of x to y in the high-entropy alloy is 8.5-23.5:1; the M alloy is Nb-Ta-Mo alloy.
3. The low modulus, high ductility Ti-Zr high entropy alloy of claim 1, wherein: the crystal structure of the high-entropy alloy is a simple body-centered cubic structure.
4. A method for producing a low modulus, high ductility Ti-Zr high entropy alloy according to any of claims 1 to 3, comprising:
1) Proportioning Ti-Zr alloy and M alloy according to gradient in the value range of x, and obtaining a sample through smelting process;
2) And (3) testing the mechanical property and chemical property of a sample, and recording data when the comprehensive property of the sample exceeds a threshold value.
5. The method for preparing the low-modulus high-ductility Ti-Zr high-entropy alloy according to claim 4, wherein the method comprises the following steps: the smelting process comprises the following steps: and (3) smelting the alloy raw materials through vacuum arc until the alloy raw materials are molten, and turning over and smelting after the alloy is cooled, wherein the repetition number is more than or equal to 10.
6. The method for preparing the low-modulus high-ductility Ti-Zr high-entropy alloy according to claim 5, wherein the method comprises the following steps: the vacuum arc melting process comprises the following steps: the alloy raw material is sent into a sample chamber, and when the vacuum degree reaches 5x10 -3 Pa, argon is introduced into the sample chamber to the pressure of 0.5atm.
7. The method for preparing the low-modulus high-ductility Ti-Zr high-entropy alloy according to claim 5, wherein the method comprises the following steps: electromagnetic stirring is also needed in the vacuum arc melting process, and the current is 3-4A.
8. The method for preparing the low-modulus high-ductility Ti-Zr high-entropy alloy according to claim 4, wherein the method comprises the following steps: the arc holding time in the vacuum arc melting process is 100-120 s, and the current is 300-450A.
9. The method for preparing the low-modulus high-ductility Ti-Zr high-entropy alloy according to claim 4, wherein the method comprises the following steps: the threshold value of the comprehensive performance is that the tensile strain is more than 5%, the elastic modulus is less than or equal to 100GPa, the wear rate is less than or equal to 7.0X10 -5mm3/N.m, and the self-corrosion current density is less than 0.168+/-0.002 mu A/cm 2.
10. Use of a low modulus, high ductility Ti-Zr high entropy alloy according to any of claims 1 to 3, characterized in that: as biomedical implant material.
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