CN109652692B - Hydrogen-embrittlement-resistant tantalum alloy for biomedical implantation, and production method, application and material thereof - Google Patents
Hydrogen-embrittlement-resistant tantalum alloy for biomedical implantation, and production method, application and material thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of hydrogen embrittlement resistant tantalum alloys and production methods thereof, and particularly relates to a hydrogen embrittlement resistant tantalum alloy for biomedical implantation and a production method, application and material thereof. The production method comprises the following steps: 1) producing a hydrogen embrittlement resistant tantalum alloy material; 2) carrying out soaking treatment, rough rolling, finish rolling, laminar cooling, coiling, heat treatment after rolling and quenching on the hydrogen embrittlement resistant tantalum alloy material obtained in the step 1) in sequence to obtain the hydrogen embrittlement resistant tantalum alloy material. The hydrogen-embrittlement-resistant tantalum alloy for biomedical implantation provided by the invention has the yield strength of 800-920 MPa, the tensile strength of 1000-1100 MPa and the elongation of 18-24%; the hydrogen embrittlement resistance is far higher than that of pure Ta of a comparative example; under the condition of basically consistent hydrogen charging concentration, the hydrogen placing fatigue life is far longer than that of the pure Ta of the comparative example. The product performance completely meets the use requirement, and the hydrogen embrittlement resistance of the product is far superior to that of the pure Ta of the comparative example.
Description
Technical Field
The invention belongs to the technical field of hydrogen embrittlement resistant tantalum alloys and production methods thereof, and particularly relates to a hydrogen embrittlement resistant tantalum alloy for biomedical implantation and a production method, application and material thereof.
Background
The tantalum has a series of excellent performances of high melting point, low steam pressure, good cold processing performance, high chemical stability, strong liquid metal corrosion resistance, large dielectric constant of a surface oxide film and the like, and has important application in high and new technical fields of medical sanitation, scientific research and the like. Tantalum is used as an orthopedic and surgical material, for example, because it grows on tantalum strips as a result of their replacement of bone muscles in the human body, and therefore it has a "bio-compatible metal". In the service environment of a human body, hydrogen atoms can easily diffuse inwards from the surface of the tantalum alloy and gather, so that the strength of the tantalum alloy is reduced, and the tantalum alloy is finally cracked through hydrogen embrittlement even under the action of cyclic stress. . In recent years, with the large application of tantalum alloy in the field of biomedical implantation, the frequent occurrence of hydrogen embrittlement fracture of tantalum alloy causes a serious problem of a large number of fracture fractures, and in order to ensure the safety and reliability of biomedical implantation tantalum alloy, the development of a biomedical implantation tantalum alloy capable of resisting the generation of hydrogen embrittlement is urgently needed.
Disclosure of Invention
The invention aims to solve the problem that the existing tantalum alloy for biomedical implantation cannot fundamentally resist hydrogen embrittlement, and provides a hydrogen embrittlement resistant tantalum alloy for biomedical implantation containing Nd-rich second-phase particles and a production method thereof, so that a large number of Nd-rich second-phase particles are produced and used as irreversible hydrogen traps to fix diffused hydrogen atoms in the tantalum alloy, and the hydrogen embrittlement resistance of the tantalum alloy is realized. The hydrogen embrittlement resistant tantalum alloy can be used for manufacturing various biomedical implantation tantalum alloy structural parts used in human body environment.
The technical scheme provided by the invention is as follows:
the hydrogen embrittlement resistant tantalum alloy material comprises the following chemical components in percentage by weight: 12-14% of Al, 10-12% of Si, 6-8% of Cr, 5-7% of Ni, 1-3% of Cu, 1-3% of Nd, and the balance of Ta and inevitable impurities.
Based on the technical scheme, 1-3% of Nd is added into the tantalum alloy, so that a large number of Nd-rich second-phase particles (the number of the Nd-rich second-phase particles contained in each cubic centimeter is 3000-3500) which are uniformly dispersed and distributed are precipitated in a tantalum alloy matrix, and the Nd-rich second-phase particles can be used as irreversible hydrogen traps to firmly fix diffused hydrogen atoms, and the hydrogen embrittlement resistance of the tantalum alloy material is fundamentally realized.
Further, the mechanical property of the material reaches yield strength ReLNot less than 800MPa, tensile strength RmNot less than 1000MPa, and the elongation A not less than 18 percent.
The invention also provides a production method of the hydrogen-embrittlement-resistant tantalum alloy for biomedical implantation, which comprises the following steps:
1) producing the hydrogen embrittlement resistant tantalum alloy material provided by the invention;
2) carrying out soaking treatment, rough rolling, finish rolling, laminar cooling, coiling, heat treatment after rolling and quenching on the hydrogen embrittlement resistant tantalum alloy material obtained in the step 1) in sequence to obtain the hydrogen embrittlement resistant tantalum alloy material.
Through the technical scheme, the produced hydrogen embrittlement-resistant tantalum alloy for biomedical implantation contains a large amount of Nd-rich second phase particles which are uniformly dispersed and distributed, so that the hydrogen embrittlement-resistant performance requirement is met, and the mechanical performance requirements of high strength and high toughness are met.
Specifically, in step 1): smelting tantalum alloy by adopting a vacuum consumable melting furnace, mixing alloy materials according to a formula, pressing an electrode, welding the electrode and residual materials into a consumable electrode, alloying, melting and casting into a plate blank to obtain the tantalum alloy, wherein the melting temperature is 2300-2400 ℃.
Specifically, in the step 2):
soaking treatment is carried out at the heating temperature of 1500-1600 ℃ for 100-110 min;
the rough rolling finishing temperature is not lower than 1300 ℃;
the finish rolling temperature is 900-950 ℃.
The final cooling temperature of laminar cooling is 600-650 ℃, and the cooling speed is 50-55 ℃/s;
the heat treatment after rolling is heating to 1100-1200 ℃, and keeping the temperature for 0.8-1.0 hour;
in the technical scheme, the size and the shape of Nd-rich second-phase particles (the average particle size of the particles is 80-100 mu m, the shape of the particles is ellipsoidal) are accurately controlled by adopting a proper rolling and heat treatment process, so that a maximized irreversible hydrogen trap is provided for the tantalum alloy, and the strength and the toughness of the tantalum alloy are improved through the precipitation strengthening effect of the second phase;
specifically, in the step 2): by using Na2SiO3And (5) quenching with alkaline aqueous solution. Na (Na)2SiO3The concentration is 20-25 wt%, and the solvent is water.
In the technical scheme, Na is adopted2SiO3The alkaline aqueous solution is quenched, so that on one hand, oily impurities on the surface of the tantalum alloy can be removed by using alkali liquor, and the surface quality and the safety during tempering of the product are improved; on the other hand, Na at high temperature2SiO3In an alkaline aqueous solution, a thin chemical conversion coating can be formed on the surface of the tantalum alloy, so that the generation efficiency of a secondary Nd second phase of the alloy can be improved to a certain extent; in a further aspect, Na2SiO3The alkaline aqueous solution can also play a cooling role, thereby ensuring the mechanical property of the product.
The invention also provides the hydrogen embrittlement resistant tantalum alloy for biomedical implantation, which is produced by the production method of the hydrogen embrittlement resistant tantalum alloy for biomedical implantation provided by the invention.
The tantalum alloy for biomedical implantation provided by the invention contains a large amount of Nd-rich second phase particles which are uniformly dispersed and distributed, meets the performance requirements of hydrogen embrittlement resistance and mechanical performance requirements of high strength and high toughness, and provides an optimal production raw material for various biomedical implantation tantalum alloy structural members used in human environment.
Further, the yield strength is 800 to 920MPa, and the tensile strength is 1000 to E1100MPa, and elongation of 18-24%; hydrogen diffusion coefficient of 1.15X 10-7～1.45×10-7cm2/s。
The invention also provides application of the hydrogen embrittlement resistant tantalum alloy for biomedical implantation provided by the invention as a structural member material of the biomedical implantation tantalum alloy.
The tantalum alloy for biomedical implantation produced according to the invention contains a large amount of Nd-rich second phase particles which are uniformly dispersed and distributed, so that the performance requirement of hydrogen embrittlement resistance is met, the mechanical performance requirements of high strength and high toughness are met, and an optimal production raw material is provided for various biomedical implantation tantalum alloy structural members used in human environment.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
In one embodiment, a method for making a hydrogen embrittlement resistant tantalum alloy for biomedical implantation comprises:
1. preparing a hydrogen-embrittlement-resistant tantalum alloy for biomedical implantation: the alloy comprises, by weight, 12-14% of Al, 10-12% of Si, 6-8% of Cr, 5-7% of Ni, 1-3% of Cu, 1-3% of Nd, and the balance of Ta and inevitable impurities. The thickness specification of the tantalum alloy is 20 mm; the mechanical property satisfies yield strength ReLNot less than 800MPa, tensile strength RmNot less than 1000MPa, and the elongation A not less than 18 percent.
2. A method for producing a hydrogen embrittlement resistant tantalum alloy for biomedical implantation, comprising the steps of:
1) smelting tantalum alloy by using a vacuum consumable melting furnace, welding a consumable electrode by mixed alloy materials, pressing the electrode, the electrode and residual materials, alloying and melting (the melting temperature is 2300-2400 ℃), and casting into a plate blank;
2) heating the plate blank at 1500-1600 ℃ for 100-110 min;
3) carrying out rough rolling, and controlling the finish temperature of the rough rolling to be not lower than 1300 ℃;
4) carrying out finish rolling, and controlling the finish rolling temperature to be 900-950 ℃;
5) carrying out laminar cooling, wherein the final cooling temperature is 600-650 ℃, and the cooling speed is as follows: 50-55 ℃/s;
6) coiling to obtain a hot rolled plate coil;
7) heat treatment is carried out, the temperature is heated to 1100-1200 ℃, and Na is added after heat preservation for 0.8-1.0 hour2SiO3And (5) quenching with alkaline aqueous solution.
3. Finishing, inspecting and packaging the hydrogen-embrittlement-resistant tantalum alloy for biomedical implantation.
1) Finishing and trimming: and cutting the tantalum alloy plate according to the standard specification, and cutting off 8%.
G. Packaging: and (5) carrying out circumferential and radial packing and delivery by using the binding belt.
Detecting the produced hydrogen-embrittlement-resistant tantalum alloy for biomedical implantation, wherein the yield strength is 800-920 MPa, the tensile strength is 1000-1100 MPa, and the elongation is 18-24%; hydrogen embrittlement resistance (hydrogen diffusion coefficient 1.15X 10)-7～1.45×10-7cm2Are all much higher than the pure Ta (hydrogen diffusion coefficient 2.37X 10) of the comparative example-3) And the product performance completely meets the use requirement.
Table 1 is a table of chemical compositions of hydrogen embrittlement resistant tantalum alloys for biomedical implantation according to various embodiments of the present invention;
table 2 is a list of melting processes of the hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to embodiments of the present invention;
table 3 is a list of rolling processes of the hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to embodiments of the present invention;
table 4 is a table of the heat treatment process of the hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to various embodiments of the present invention;
table 5 is a table of mechanical properties of hydrogen embrittlement resistant tantalum alloys for biomedical implantation according to embodiments of the present invention;
table 6 is a table of hydrogen embrittlement resistance of the hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to embodiments of the present invention;
table 7 is a table listing the hydrogen fatigue performance of the hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to various embodiments of the present invention.
Examples 1 to 6 were carried out according to the contents of tables 1 to 4:
TABLE 1 chemical composition (wt%) of hydrogen embrittlement resistant tantalum alloy for biomedical implantation of various embodiments of the present invention
| Examples | Al | Si | Cr | Ni | Cu | Nd | Ta |
| 1 | 12.5 | 12.0 | 8.0 | 6.0 | 3.0 | 2.0 | 56.5 |
| 2 | 12.0 | 10.8 | 7.5 | 6.3 | 2.8 | 2.6 | 58.0 |
| 3 | 13.5 | 11.5 | 7.0 | 7.0 | 2.0 | 3.0 | 56.0 |
| 4 | 14.0 | 11.0 | 6.7 | 6.5 | 2.5 | 1.8 | 57.5 |
| 5 | 13.0 | 10.0 | 6.3 | 5.0 | 1.5 | 1.0 | 63.2 |
| 6 | 13.8 | 11.9 | 6.0 | 5.8 | 1.0 | 1.2 | 60.3 |
TABLE 2 melting process of hydrogen embrittlement resistant tantalum alloy for biomedical implantation in accordance with various embodiments of the present invention
| Examples | Melting temperature (. degree.C.) |
| 1 | 2310 |
| 2 | 2300 |
| 3 | 2340 |
| 4 | 2390 |
| 5 | 2400 |
| 6 | 2370 |
TABLE 3 Rolling Process of hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to embodiments of the present invention
TABLE 4 Heat treatment Process of hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to embodiments of the present invention
The results of testing the hydrogen embrittlement resistant tantalum alloys for biomedical implantation obtained in examples 1 to 6 are shown in Table 5
TABLE 5 mechanical properties of hydrogen embrittlement resistant tantalum alloys for biomedical implants according to embodiments of the invention
TABLE 6 list of hydrogen embrittlement resistance of hydrogen embrittlement resistant tantalum alloys for biomedical implantation according to embodiments of the present invention
TABLE 7 Hydrogen placement fatigue Performance of hydrogen embrittlement resistant tantalum alloys for biomedical implants of various embodiments of the present invention
As can be seen from tables 5 to 7, the hydrogen embrittlement resistant tantalum alloy for biomedical implantation disclosed by the invention has the yield strength of 800-920 MPa, the tensile strength of 1000-1100 MPa and the elongation of 18-24%; hydrogen embrittlement resistance (hydrogen diffusion coefficient 1.15X 10)-7～1.45×10-7cm2Are all much higher than the pure Ta (hydrogen diffusion coefficient 2.37X 10) of the comparative example-3) (ii) a Under the condition of basically consistent hydrogen charging concentration, the hydrogen storage fatigue life (41419-45511 times) is far higher than that of pure Ta (11438 times) of a comparative example. The product performance completely meets the use requirement, and the hydrogen embrittlement resistance of the product is far superior to that of the pure Ta of the comparative example.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The hydrogen embrittlement resistant tantalum alloy material is characterized by comprising the following chemical components in percentage by weight: 12-14% of Al, 10-12% of Si, 6-8% of Cr, 5-7% of Ni, 1-3% of Cu, 1-3% of Nd, and the balance of Ta and inevitable impurities.
2. The hydrogen embrittlement resistant tantalum alloy material of claim 1, wherein: the mechanical property of the material reaches yield strength ReLNot less than 800MPa, tensile strength RmNot less than 1000MPa, and the elongation A not less than 18 percent.
3. A production method of hydrogen embrittlement resistant tantalum alloy for biomedical implantation is characterized by comprising the following steps:
1) producing the hydrogen embrittlement resistant tantalum alloy material of claim 1 or 2;
2) carrying out soaking treatment, rough rolling, finish rolling, laminar cooling, coiling, heat treatment after rolling and quenching on the hydrogen-embrittlement-resistant tantalum alloy material obtained in the step 1) in sequence to obtain the hydrogen-embrittlement-resistant tantalum alloy material;
in step 2):
soaking treatment is carried out at the heating temperature of 1500-1600 ℃ for 100-110 min;
the heat treatment after rolling is heating to 1100-1200 ℃, and keeping the temperature for 0.8-1.0 hour;
the rough rolling finishing temperature is not lower than 1300 ℃;
the finish rolling temperature is 900-950 ℃;
the final cooling temperature of laminar cooling is 600-650 ℃, and the cooling speed is 50-55 ℃/s; by using Na2SiO3And (5) quenching with alkaline aqueous solution.
4. The method for producing a hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to claim 3, wherein in step 1): smelting tantalum alloy by using a vacuum consumable melting furnace, welding a consumable electrode by mixing alloy materials, pressing the electrode, electrodes and residual materials according to chemical components of the hydrogen embrittlement resistant tantalum alloy material, alloying and smelting, and pouring into a plate blank, wherein the smelting temperature is 2300-2400 ℃.
5. A hydrogen embrittlement-resistant tantalum alloy for biomedical implantation, produced by the method for producing a hydrogen embrittlement-resistant tantalum alloy for biomedical implantation according to claim 3 or 4.
6. The hydrogen embrittlement resistant tantalum alloy for biomedical implantation according to claim 5, wherein: the yield strength is 800-920 MPa, the tensile strength is 1000-1100 MPa, and the elongation is 18-24%; hydrogen diffusion coefficient of 1.15X 10-7～1.45×10-7cm2/s。
7. Use of a hydrogen embrittlement resistant tantalum alloy according to claim 5 or 6, for biomedical implants, wherein: the material is used as a biomedical implanted tantalum alloy structural part material.
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