CN112251639A - High-strength antibacterial titanium alloy bar, high-strength antibacterial titanium alloy wire and preparation method of high-strength antibacterial titanium alloy bar - Google Patents
High-strength antibacterial titanium alloy bar, high-strength antibacterial titanium alloy wire and preparation method of high-strength antibacterial titanium alloy bar Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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Abstract
The invention provides a high-strength antibacterial titanium alloy bar, a high-strength antibacterial titanium alloy wire and a preparation method of the high-strength antibacterial titanium alloy bar, the high-strength antibacterial titanium alloy wire comprises the following chemical components (in percentage by weight): al: 5.5 to 6.5; v: 3.5 to 4.5; cu: 2-8; the balance of Ti. The preparation method of the titanium alloy bar and the titanium alloy wire comprises the following steps: smelting in a vacuum consumable electrode furnace to obtain a raw material ingot; grinding the cast ingot, cogging and forging at the temperature of more than 1000 ℃, and finish forging to obtain a bar blank; the bar blank is quickly cooled after being kept at 800-1350 ℃ for a period of time, and the bar material obtains a superfine nano-strip structure; after quenching, carrying out hot rolling on the bar blank at the temperature of 750-850 ℃, wherein the accumulated deformation of the hot rolling is more than or equal to 90 percent, and obtaining a superfine nano-strip structure bar; after hot rolling, the bar can be drawn to a bar or a wire with a target diameter in a single pass at the drawing speed of 1-3 m/min at the temperature of 600-700 ℃. The bar and wire materials processed by the method have equiaxial crystal grains, the size is less than 500nm, and the crystal grains are not coarsened and grown within 3 hours of aging at 650 ℃ and below.
Description
Technical Field
The invention relates to the field of titanium alloy processing and preparation, in particular to a high-strength antibacterial titanium alloy bar, wire and a preparation method thereof.
Background
Titanium alloy is a metal with excellent biological safety, has low density, elastic modulus close to that of human skeleton and high strength, so that titanium and its alloy are widely applied to the medical and health field, especially the oral and orthopedic repair field, such as bracket, belt loop, orthodontic arch wire, implant for anchorage, artificial joint (μm, knee, shoulder, ankle, elbow, wrist, finger joint, etc.), bone wound product (intramedullary nail, steel plate, screw, etc.), spinal column orthopedic internal fixation system, etc.
The titanium alloy has been applied in the medical field for nearly 70 years, various titanium alloy grades are layered, updating iteration is gradually unable to keep up with the needs of people for higher medical quality, and the contradiction between the defects of the existing titanium alloy and the needs of people is more and more prominent. Firstly, titanium alloys are good in biocompatibility and do not cause damage to the human body, but at the same time provide a harmless environment for the growth of harmful microorganisms. With the wide application of medical titanium alloy, the serious complication of postoperative infection also becomes a problem which is more and more concerned and needs to be solved urgently. Secondly, the medical titanium alloy has another advantage of low density and elastic modulus close to that of a human body, but when the medical titanium alloy is used as a force-bearing implant, such as an artificial hip joint handle, the implant failure caused by fracture failure often occurs, great pain is brought to a patient, and heavy spirit and economic burden are caused. Therefore, the realization that the implant material is lighter, stronger and healthier becomes a new important proposition which is more suitable for actual and future needs.
Disclosure of Invention
The invention aims to provide a high-strength antibacterial titanium alloy bar and wire and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-strength antibacterial titanium alloy bar and wire comprises the following chemical components in percentage by weight: al: 5.5-6.5, V: 3.5-4.5, Cu: 2 to 8 (preferably 4 to 6), and the balance Ti.
The preparation process of the high-strength antibacterial titanium alloy bar and wire comprises the following steps:
the method comprises the following steps: smelting for multiple times by adopting a vacuum consumable furnace to obtain a raw material ingot. Grinding the cast ingot, cogging and forging at the temperature of more than 1000 ℃, and finish forging to obtain a bar blank;
step two: keeping the temperature of the bar blank at 800-1350 ℃ for (2.5-3.5) D min, wherein D is the effective thickness (millimeter mm) of the sample;
step three: and (4) rapidly cooling the bar blank after the heat preservation is finished, wherein the cooling rate delta T/T ranges from 20 ℃/s to 200 ℃/s. Obtaining an ultrafine nano lath structure from the bar blank;
step four: hot rolling the superfine nano lath structure bar blank at the temperature of 750-850 ℃, wherein the accumulated deformation of the hot rolling is more than or equal to 90 percent, and obtaining the superfine nano lath structure bar;
step five: the superfine nano-lath tissue bar is drawn at the drawing speed of 1-3 m/min at the temperature of 600-700 ℃ to a bar or a wire with a target diameter in a single pass.
The microstructure and the performance of the high-strength antibacterial titanium alloy bar and wire are as follows:
(1) the high-strength antibacterial titanium alloy bar and wire material provided by the invention have equiaxial crystal grains, the size is less than 500nm, and the crystal grains are not coarsened and grown within 3 hours of aging at 650 ℃ and below.
(2) When the copper content is in the preferable range, the tensile strength of the high-strength antibacterial titanium alloy bar (the diameter is more than 7 mm) reaches 1200-1500MPa, and the elongation is higher than 15%; the tensile strength of the high-strength antibacterial titanium alloy wire (1-7 mm) reaches 1500-1700MPa, and the elongation is higher than 10%.
The invention has the beneficial effects that:
(1) different from the situation of the prior art, the preparation method of the high-strength antibacterial titanium alloy bar and wire provided by the invention realizes that the bar and wire with the target diameter can be drawn in a single pass, greatly simplifies the processing technology and greatly saves the economic cost and the time cost.
(2) The high-strength antibacterial titanium alloy bar and wire provided by the invention have the advantages that the microstructure is ultrafine isometric grains, the high-structure thermal stability is realized, the preparation method of the high-strength antibacterial titanium alloy bar and wire provided by the invention does not need to depend on high-power equipment and expensive dies, and ultrafine isometric crystals can be obtained through conventional thermal deformation and thermal treatment, so that the requirement of large-scale industrial production is met.
(3) The high-strength antibacterial titanium alloy bar, the high-strength antibacterial titanium alloy wire and the preparation method thereof can obviously improve the comprehensive mechanical property of the titanium alloy material.
Drawings
FIG. 1 the metallographic microstructure of the material obtained in example 3.
Detailed Description
The present application will now be illustrated and explained by means of several groups of specific examples and comparative examples, which should not be taken to limit the scope of the present application.
Example (b): examples 1 to 6 show Ti6Al4V-Cu alloys that were smelted according to the ranges of chemical compositions provided by the present invention, in which the content of Cu element was gradually increased, and the corresponding manufacturing processes were also adjusted within the ranges of technical parameters specified by the present invention, as shown in tables 1 and 2.
Comparative example: the chemical compositions of comparative examples 1-2 were below the lower limit of the chemical composition range provided by the present invention, and the chemical composition of comparative example 10 was above the upper limit of the chemical composition range provided by the present invention. The hot rolling temperature of comparative example 3 is higher than the upper limit of the hot rolling temperature range provided by the present invention; the heating temperature for the heat treatment of the rod blank of comparative example 3 is lower than the lower limit of the heating temperature range provided by the present invention; the heat treatment holding time of the bar billet of comparative example 4 is lower than the lower limit of the holding time range provided by the invention; comparative example 5 the cooling rate of the heat-treated bar was higher than the upper limit of the cooling rate range provided by the present invention. The hot-drawing temperature of comparative example 6 is higher than the upper limit of the hot-drawing temperature range provided by the present invention; the deformation amount of comparative example 7 is lower than the deformation amount range provided by the present invention; the hot-drawing temperature of comparative example 8 is lower than the lower limit of the hot-drawing temperature range provided by the present invention; the hot drawing speed of comparative example 9 was higher than that provided by the present invention. Comparative example 11 is a conventional Ti6Al4V bar and wire having a nanocrystalline structure prepared by ECAP process, see tables 3 and 4.
Table 1 examples chemical composition, heat treatment process
Description of the drawings: d is the effective thickness of the sample (in mm)
TABLE 2 example Hot working Process and Final dimensions
Table 3 comparative example chemical composition, heat treatment process
Description of the drawings: d is the effective thickness of the sample (in mm)
Table 4 comparative example hot working process and final dimensions
1. Hardness test
The hardness of the materials of the examples and comparative examples were tested. The Vickers hardness of the annealed material samples was measured using an HTV-1000 type durometer. Before testing, the sample surface was polished. The sample was a thin sheet with dimensions of 10mm diameter and 2mm thickness. The test loading force is 9.8N, the pressurizing duration is 15s, and the hardness value is automatically calculated by measuring the diagonal length of the indentation through computer hardness analysis software. The final hardness values were averaged over 15 points and three replicates were selected for each set of samples, the specific results are shown in table 5.
2. Tensile Property test
The room temperature tensile mechanical properties of the comparative and example materials were tested using an Instron model 8872 tensile tester at a tensile rate of 0.5 mm/min. Before testing, a lathe is adopted to process the material into standard tensile samples with the thread diameter of 10mm, the gauge length of 5mm and the gauge length of 30mm, three parallel samples are taken from each group of heat treatment samples, the mechanical properties obtained by the experiment comprise tensile strength and elongation, and the specific results are shown in table 5.
3. Grain size statistics
The method comprises the steps of carrying out phase volume fraction statistics on samples before and after fatigue by adopting an Electron Back Scattering Diffraction (EBSD) analysis system of a scanning electron microscope, wherein the sample preparation method comprises the steps of firstly carrying out mechanical polishing on the samples to obtain a flat and smooth surface, then placing the samples in electrolyte (6% perchloric acid, 30% butanol and 64% methanol) for electrolytic polishing for 20s at the temperature of minus 25 ℃, and removing surface stress. When EBSD collects data, the working voltage of a scanning electron microscope is 20kV, the current is 18nA, the step length is selected to be 0.2 μm, the resolution of the scanning range is more than 80%, Channel5 software is adopted to analyze the grain size, and the specific result is shown in Table 6.
TABLE 5 mechanical properties of the materials of the examples and comparative examples
TABLE 6 texture characteristics of the materials of the examples and comparative examples and the change in texture after 1h incubation at different temperatures
As can be seen from the results of tables 5 and 6, examples 1 to 6 are equiaxed nanocrystalline structures, which make them have high strength, good plasticity and high hardness. Within the Cu content range specified in the invention, as the Cu content is increased, the grain size of the material is gradually reduced, the strength and the hardness of the material are improved, and the elongation is gradually reduced.
As can be seen from the results of tables 5 and 6, comparative examples 1, 2 and 10 have poor mechanical properties and do not have equiaxed nanocrystalline structures because the Cu content is out of the range provided by the present invention. In the comparative examples 3-9, because the technological parameter ranges of heat treatment, hot rolling, hot drawing and the like are not in the ranges provided by the invention, the multi-pass drawing is caused, the processing is difficult, the final mechanical property is poor, particularly the plasticity of the wire is the worst, and the equiaxial nanocrystalline structure is not obtained.
From the results in table 6, it can be seen that examples 1 to 6 have good thermal stability of the structure during aging at 650 ℃ and below, and the grain size does not change significantly after aging. While comparative example 11 exhibited significant coarsening growth of grains.
The above description is only for the purpose of illustrating embodiments of the present application and is not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by the contents of the specification and the drawings of the present application or are directly or indirectly applied to other related technical fields, are also included in the scope of the present application.
Claims (5)
1. A high-strength antibacterial titanium alloy bar and wire is characterized by comprising the following chemical components in percentage by weight: al: 5.5 to 6.5; v: 3.5 to 4.5; cu: 2-8; the balance of Ti.
2. The high-strength antibacterial titanium alloy rod or wire according to claim 1, wherein the copper content in the alloy is Cu: 4 to 6.
3. A preparation method of the high-strength antibacterial titanium alloy bar and wire of claim 1 or 2, which is characterized by comprising the following steps:
the method comprises the following steps: smelting for multiple times by adopting a vacuum consumable furnace to obtain a raw material ingot; grinding the cast ingot, cogging and forging at the temperature of more than 1000 ℃, and finish forging to obtain a bar blank;
step two: keeping the temperature of the bar blank at 800-1350 ℃ for (2.5-3.5) D min, wherein D is the effective thickness of the sample and the unit is millimeter mm;
step three: rapidly cooling the bar blank after the heat preservation is finished, wherein the cooling rate is 20-200 ℃/s; obtaining an ultrafine nano lath structure from the bar blank;
step four: hot rolling the superfine nano lath structure bar blank at the temperature of 750-850 ℃, wherein the accumulated deformation of the hot rolling is more than or equal to 90 percent, and obtaining the superfine nano lath structure bar;
step five: the superfine nano-lath tissue bar is drawn at the drawing speed of 1-3 m/min at the temperature of 600-700 ℃ to a bar or a wire with a target diameter in a single pass.
4. The method for preparing high-strength antibacterial titanium alloy bars and wires according to claim 3, which is characterized by comprising the following steps: the bar and wire materials obtained after the thermal deformation processing have equiaxial crystal grains, the size is less than 500nm, and the crystal grains are not coarsened and grown within 3 hours of aging at 650 ℃ and below.
5. The method for preparing high-strength antibacterial titanium alloy bars and wires according to claim 3, which is characterized by comprising the following steps: the tensile strength of the prepared antibacterial titanium alloy bar with the diameter larger than 7 mm reaches 1200-1500MPa, and the elongation is higher than 15%; the tensile strength of the antibacterial titanium alloy wire with the diameter of 1-7 mm reaches 1500-1700MPa, and the elongation is higher than 10%.
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Cited By (6)
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| WO2021093805A1 (en) * | 2019-11-15 | 2021-05-20 | 苏州森锋医疗器械有限公司 | Medical titanium alloy having high fatigue strength, and hot processing and hot treatment method therefor and device thereof |
| CN113088757A (en) * | 2021-03-02 | 2021-07-09 | 许铎 | Titanium-based alloy implant containing aluminum, vanadium and copper and preparation method thereof |
| CN114318028A (en) * | 2021-02-25 | 2022-04-12 | 白志文 | Manufacturing method of antibacterial titanium and titanium alloy material |
| CN115976440A (en) * | 2023-01-05 | 2023-04-18 | 宝鸡鑫诺新金属材料有限公司 | Processing method of anti-infection medical copper-titanium-containing alloy rod wire |
| CN117324525A (en) * | 2023-12-01 | 2024-01-02 | 苏州森锋医疗器械有限公司 | Intramedullary nail and preparation method thereof |
| CN117327945A (en) * | 2023-12-01 | 2024-01-02 | 北京中科万德创新科技有限公司 | Surgical staple wire with low friction coefficient and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021093805A1 (en) * | 2019-11-15 | 2021-05-20 | 苏州森锋医疗器械有限公司 | Medical titanium alloy having high fatigue strength, and hot processing and hot treatment method therefor and device thereof |
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| CN113088757A (en) * | 2021-03-02 | 2021-07-09 | 许铎 | Titanium-based alloy implant containing aluminum, vanadium and copper and preparation method thereof |
| CN115976440A (en) * | 2023-01-05 | 2023-04-18 | 宝鸡鑫诺新金属材料有限公司 | Processing method of anti-infection medical copper-titanium-containing alloy rod wire |
| CN115976440B (en) * | 2023-01-05 | 2024-05-28 | 宝鸡鑫诺新金属材料有限公司 | Processing method of anti-infection medical copper-containing titanium alloy rod wire |
| CN117324525A (en) * | 2023-12-01 | 2024-01-02 | 苏州森锋医疗器械有限公司 | Intramedullary nail and preparation method thereof |
| CN117327945A (en) * | 2023-12-01 | 2024-01-02 | 北京中科万德创新科技有限公司 | Surgical staple wire with low friction coefficient and preparation method thereof |
| CN117324525B (en) * | 2023-12-01 | 2024-02-13 | 苏州森锋医疗器械有限公司 | Intramedullary nail and preparation method thereof |
| CN117327945B (en) * | 2023-12-01 | 2024-03-08 | 苏州森锋医疗器械有限公司 | Surgical staple wire with low friction coefficient and preparation method thereof |
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