CN110747374B - Low-elasticity-modulus Ti6Al4V alloy and preparation method and application thereof - Google Patents
Low-elasticity-modulus Ti6Al4V alloy and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a low-elasticity-modulus Ti6Al4V alloy, a preparation method and application thereof, wherein the Ti6Al4V alloy comprises the following components in percentage by mass: al: 5.5-6.2 wt.%; v: 3.8-4.5 wt.%; fe: 0.16-0.22 wt.%; y: 0.01-0.1 wt.%; the balance being Ti. The preparation method comprises the steps of carrying out hot forging, hot drawing and double annealing heat treatment on a Ti6Al4V titanium alloy ingot, and machining to obtain the Ti6Al4V alloy with low elastic modulus. The elastic modulus of the Ti6Al4V alloy is 80-90 GPa. The invention increases the beta phase content through the mutual cooperation of the alloy components and the process, thereby reducing the elastic modulus of the Ti6Al4V alloy.
Description
Technical Field
The invention discloses a low-elasticity-modulus Ti6Al4V alloy, a preparation method thereof and application thereof to a medical ultrasonic knife, and belongs to the field of titanium alloy material preparation.
Background
With the continuous improvement of the medical technology level, the surgical operation development trend is fast formed by small surgical trauma, light pain and quick postoperative recovery. The minimally invasive surgery utilizes modern medical instruments such as a laparoscope, a thoracoscope and the like and related equipment to carry out the surgery, the patient is attached to the body to the greatest extent on the prior art, the purposes of small surgical wound, light pain and quick postoperative recovery are achieved, and the inconvenience brought to the patient and family members by the disease is greatly reduced.
The ultrasonic scalpel as a common instrument for minimally invasive surgery has the characteristics of high precision, less bleeding, no burn, quick postoperative recovery and the like. When in use, the temperature of the ultrasonic scalpel head is lower than 80 ℃, the peripheral propagation distance is less than 5 microns, smoke, eschar and electric spark are rarely generated, and no physiological interference is generated on organisms. Compared with the common electrotome for common operations, the ultrasonic cutter has the advantages of accurate cutting, firm hemostasis, strong controllability and the like, has better safety and effectiveness, reduces the occurrence probability of complications, and is more advanced. Therefore, the ultrasonic knife has started to gradually replace the electric knife in modern surgical operation, and the development of minimally invasive surgery is the trend.
The most commonly used material for the medical ultrasonic knife bar at present is Ti6Al4V alloy. Ti6Al4V is a typical (α + β) dual phase titanium alloy. The Ti6Al4V alloy has the characteristics of high strength, small specific gravity, good biocompatibility, excellent comprehensive mechanical property and the like, thereby being widely applied to the top scientific fields of aerospace, navigation, military equipment, medical instruments and the like. In ultrasonic blade surgery, cutting is one of its primary functions. During operation, the ultrasonic scalpel converts electric energy into mechanical energy through a special conversion device to generate high-frequency ultrasonic oscillation, so that water in contacted tissue cells is gasified, and protein hydrogen bonds are broken, thereby achieving the purpose of cutting. Relevant researches show that the minimum amplitude required for cutting different tissues is different, and the working efficiency and the application range of the ultrasonic knife can be effectively improved by improving the amplitude of the ultrasonic knife. The elastic modulus of the cutter bar material is one of the main factors influencing the amplitude of the ultrasonic cutter, but the elastic modulus of the Ti6Al4V alloy is higher than that of the beta-type titanium alloy, and the high elastic modulus can cause the problems of reduced energy transfer efficiency, reduced amplitude, increased internal stress of alloy and the like of the medical ultrasonic cutter bar, so that the fatigue life of the medical ultrasonic cutter bar is shortened, and the medical ultrasonic cutter bar is easy to break. The elastic modulus of the Ti6Al4V alloy is reduced, so that the energy transfer efficiency of the ultrasonic cutter bar is improved, the amplitude is improved, the internal stress of the alloy is reduced, the fatigue life of the ultrasonic cutter bar is prolonged, and the application range is expanded.
Therefore, the problem to be solved in the field of the current medical ultrasonic blade Ti6Al4V alloy is solved by preparing the medical ultrasonic blade Ti6Al4V alloy with the mechanical property meeting the use requirement of the ultrasonic blade and the low elastic modulus.
Disclosure of Invention
In order to solve the above problems, the present invention aims to provide a low elastic modulus Ti6Al4V alloy, and a preparation method and an application thereof, and the application thereof as an ultrasonic cutter bar can reduce the possibility of cutter bar fracture during use, and provide a strong guarantee for the safety and smooth performance of an operation.
The invention relates to a low-elasticity-modulus Ti6Al4V alloy, which comprises the following components in percentage by mass:
Al：5.5～6.2wt.％；
V：3.8～4.5wt.％；
Fe：0.16～0.22wt.％；
Y：0.01～0.1wt.％；
the balance being Ti.
The content of other impurity elements is lower than the corresponding national standard level.
In a preferred scheme, the Ti6Al4V alloy comprises the following components in percentage by mass:
Al：5.54～6.2wt.％；
V：4.44～4.5wt.％；
Fe：0.16～0.22wt.％；
Y：0.01～0.10wt.％；
the balance being Ti.
Preferably, the elastic modulus of the Ti6Al4V alloy is 80-90 GPa, and preferably 80-89 GPa.
In a preferable scheme, the tensile strength of the Ti6Al4V alloy is 980-1031 MPa; the yield strength is 905-953 MPa; the elongation is 11-15%.
The invention relates to a preparation method of a low-elasticity-modulus Ti6Al4V alloy, which comprises the following steps of:
step 1 Hot forging
Heating the Ti6Al4V titanium alloy ingot to a temperature above the transformation point, and performing hot forging for multiple times to obtain a Ti6Al4V alloy bar;
step 2 Hot drawing
Heating the Ti6Al4V alloy bar obtained in the step 1 to a temperature higher than the recrystallization temperature, and carrying out multi-pass hot drawing to obtain a Ti6Al4V alloy wire;
step 3 annealing
Carrying out double annealing heat treatment on the Ti6Al4V alloy wire material obtained in the step 2 to obtain a low-elasticity-modulus Ti6Al4V alloy;
the first annealing temperature is 900-1000 ℃, and the second annealing temperature is 700-800 ℃.
Preferably, in the step 1, the preparation method of the Ti6Al4V titanium alloy ingot comprises the following steps: and mixing pure Al powder, Al-V intermediate phase powder, pure Fe powder and pure Y powder according to a designed proportion, pressing into a blocky mixture, and smelting the blocky mixture for more than 5 times to obtain the Ti6Al4V alloy cast ingot.
Further, the purities of the pure Al powder, the Al-V intermediate phase powder, the pure Fe powder and the pure Y powder are all more than or equal to 99.9 wt%
In the actual operation process, the casting is carried out by using a non-consumable vacuum arc furnace, the massive mixture is repeatedly smelted for more than 5 times to obtain a Ti6Al4V alloy cast ingot with uniform components, then oxide skin on the surface of the Ti6Al4V alloy cast ingot is removed by turning, and a riser is cut off, so that the Ti6Al4V titanium alloy cast ingot for hot forging is obtained.
Preferably, in the step 1, the temperature is heated to 850-1050 ℃ and kept.
Further, in the step 1, heating to 850-990 ℃ and preserving heat.
In the preferable scheme, in the step 1, the total radial deformation amount of the forged rod reaches 85-98% after multiple times of upsetting, drawing and forging.
In the actual operation process, upsetting, drawing and forging the bar are all carried out in the air, the head and the tail are cut off in the middle of each fire when the bar is forged, and the bar is obtained after hot forging. The hot forging is to heat the Ti6Al4V alloy ingot with coarse grains after smelting to a temperature above the transformation point and then forge and break the original large grains.
Preferably, in the step 2, the temperature is heated to 800-1050 ℃ and kept.
Further, in the step 2, heating to 800-990 ℃.
In the step 2, the total radial deformation after the multi-pass hot drawing is 60-70%. The hot drawing is performed in air.
In the preferable scheme, in the step 3, the first annealing heat preservation time is 0.5-2.5 h, and the annealing furnace is taken out after the heat preservation time is up and is cooled to the room temperature by air; and (4) keeping the temperature for the second annealing for 1-3 hours, taking out the product after the temperature is kept for the second annealing, and air-cooling the product to room temperature.
The invention relates to application of a low-elastic-modulus Ti6Al4V alloy, in particular to application of a low-elastic-modulus Ti6Al4V alloy to an ultrasonic knife.
Further, the low-elasticity-modulus Ti6Al4V alloy is applied to the cutter bar of the medical ultrasonic cutter.
In the actual operation process, the Ti6Al4V alloy wire subjected to double annealing is machined to remove surface scale. The machining is performed using a lathe.
Principles and advantages of the invention
The modulus of elasticity of a titanium alloy depends on the phase composition and phase content of the titanium alloy. The Ti6Al4V belongs to a dual-phase titanium alloy, and comprises alpha phase and beta phase. Wherein the alpha phase is a close-packed hexagonal structure, and the beta phase is a body-centered cubic structure. Body-centered cubic beta has more slip systems than hexagonal close-packed alpha phase, so beta has good plasticity and lower elastic modulus than alpha phase. By properly increasing the beta phase content is an important way to reduce the elastic modulus of the Ti6Al4V alloy.
Among the β stabilizing elements of titanium alloys, Fe is one of the strongest β stabilizing elements, but since it is not thermally stable and easily causes segregation during melting, Fe is generally an impurity element in Ti6Al4V, and the content thereof needs to be controlled. In the invention, the content of Fe is controlled within 0.16-0.22 wt.%, so that the transition temperature of a beta phase can be reduced and the range of a beta phase region can be enlarged on the premise of not influencing other performance requirements of the Ti6Al4V alloy by the Fe element, thereby achieving the purpose of improving the content of the beta phase in the Ti6Al4V alloy and reducing the elastic modulus of the Ti6Al4V alloy.
Meanwhile, a small amount of rare earth element yttrium (Y) is added, so that the grain size of a Ti6Al4V alloy forging structure can be effectively reduced, and the section elongation and the tensile strength are increased.
The first annealing temperature of the double annealing is close to the phase transformation point, the primary alpha phase is easy to transform to the beta phase, so that a large amount of transformed beta phase appears, and the elastic modulus of the Ti6Al4V alloy is favorably reduced.
The elastic modulus of the Ti6Al4V alloy is mainly controlled by the content of beta phase in the microstructure of the alloy. The content of beta stable elements in the Ti6Al4V alloy is increased, and then the Ti6Al4V alloy is subjected to heat treatment by adopting a reasonable double heat treatment system, so that the content of beta phases in the Ti6Al4V alloy is increased, and the Ti6Al4V alloy containing a large amount of beta phases is obtained, thereby reducing the elastic modulus of the Ti6Al4V alloy. In addition, in order to prevent the reduction of other mechanical properties of the Ti6Al4V alloy due to the excessively high content of the beta phase, the Y element is added into the Ti6Al4V alloy in an alloying mode, so that the grain size of the Ti6Al4V alloy is reduced, the elastic modulus of the Ti6Al4V alloy is reduced, and meanwhile, the original good mechanical properties are maintained.
The elastic modulus of the conventional Ti6Al4V alloy is about 110GPa, and the elastic modulus of the Ti6Al4V alloy prepared by the method is reduced to 80-90 GPa when other mechanical properties meet the use standard of the medical ultrasonic knife, so that the efficiency and amplitude of energy transfer of the medical ultrasonic knife Ti6Al4V during use are greatly improved, the internal stress of the ultrasonic knife bar during use is reduced, the fatigue life of the ultrasonic knife bar is prolonged, the possibility of knife bar fracture during use is reduced, and the powerful guarantee is provided for the safety and the smoothness of an operation.
Detailed Description
Example 1
Pure aluminum with the purity of more than 99.9 wt.%, an Al-V intermediate phase, pure Fe, pure Y and high-purity sponge titanium are used as raw materials to smelt Ti6Al4V alloy, the smelting is repeated for 5 times to obtain alloy with uniform components, and the element content is respectively Al: 5.54 wt.%; v: 4.44 wt.%; fe: 0.16 wt.%; y: 0.08 wt.%; ti: the balance; the other impurity elements meet the relevant national standard. Heating the obtained titanium ingot to 950 ℃, then carrying out hot forging on the titanium ingot to obtain a bar material, wherein the total deformation is 76%, and then carrying out air cooling on the bar material to room temperature. Heating the obtained bar to 930 ℃, then carrying out hot drawing to obtain a wire, wherein the total deformation of the hot drawing is 70%, and then carrying out air cooling to room temperature. Annealing in an annealing furnace, wherein the first annealing temperature is 920 ℃ between the first annealing temperature and the annealing time is 1h, air cooling is carried out to the room temperature after the heat preservation is finished, the second annealing temperature is 780 ℃ and the annealing time is 1.5h, and air cooling is carried out to the room temperature after the heat preservation is finished. And finally, machining to remove the surface oxide skin. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 84GPa, the tensile strength is 980MPa, the yield strength is 905MPa, and the elongation is 14%.
Example 2
Pure aluminum with the purity of more than 99.9 wt.%, an Al-V intermediate phase, pure Fe, pure Y and high-purity sponge titanium are used as raw materials to smelt Ti6Al4V alloy, the smelting is repeated for 5 times to obtain alloy with uniform components, and the element content is respectively Al: 5.64 wt.%; v: 4.48 wt.%; fe: 0.18 wt.%; y: 0.04 wt.%; ti: the balance; the other impurity elements meet the relevant national standard. Heating the obtained titanium ingot to 950 ℃, then carrying out hot forging on the titanium ingot to obtain a bar material, wherein the total deformation is 77%, and then carrying out air cooling on the bar material to room temperature. Heating the obtained bar to 900 ℃, then carrying out hot drawing to obtain a wire material, carrying out hot drawing to achieve the total deformation of 75%, and then carrying out air cooling to room temperature. Annealing in an annealing furnace, wherein the first annealing temperature is 935 ℃ and the annealing time is 1h, air cooling to room temperature is carried out after the heat preservation is finished, the second annealing temperature is 770 ℃ and the annealing time is 1.5h, and air cooling to room temperature is carried out after the heat preservation is finished. And finally, machining to remove the surface oxide skin. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 80GPa, the tensile strength is 1020MPa, the yield strength is 923MPa, and the elongation is 12%.
Example 3
Pure aluminum with the purity of more than 99.9 wt.%, an Al-V intermediate phase, pure Fe, pure Y and high-purity sponge titanium are used as raw materials to smelt Ti6Al4V alloy, the smelting is repeated for 5 times to obtain alloy with uniform components, and the element content is respectively Al: 6.2 wt.%; v: 4.47 wt.%; fe: 0.18 wt.%; y: 0.01 wt.%; ti: the balance; the other impurity elements meet the relevant national standard. Heating the obtained titanium ingot to 950 ℃, then carrying out hot forging on the titanium ingot to obtain a bar material, wherein the total deformation is 73%, and then carrying out air cooling on the bar material to room temperature. Heating the obtained bar to 930 ℃, then carrying out hot drawing to obtain a wire, wherein the total deformation of the hot drawing is 71%, and then carrying out air cooling to room temperature. Annealing in an annealing furnace, wherein the first annealing temperature is 960 ℃, the annealing time is 2h, air cooling is carried out to the room temperature after the heat preservation is finished, the second annealing temperature is 710 ℃, the annealing time is 1.5h, and air cooling is carried out to the room temperature after the heat preservation is finished. And finally, machining to remove the surface oxide skin. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 86GPa, the tensile strength is 1022MPa, the yield strength is 953MPa and the elongation is 15 percent.
Example 4
Pure aluminum with the purity of more than 99.9 wt.%, an Al-V intermediate phase, pure Fe, pure Y and high-purity sponge titanium are used as raw materials to smelt Ti6Al4V alloy, the smelting is repeated for 5 times to obtain alloy with uniform components, and the element content is respectively Al: 6.03 wt.%; v: 4.50 wt.%; fe: 0.22 wt.%; y: 0.09 wt.%; ti: the balance; the other impurity elements meet the relevant national standard. Heating the obtained titanium ingot to 950 ℃, then carrying out hot forging on the titanium ingot to obtain a bar material, wherein the total deformation is 76%, and then carrying out air cooling on the bar material to room temperature. Heating the obtained bar to 930 ℃, then carrying out hot drawing to obtain a wire, carrying out hot drawing to obtain a total deformation of 72%, and then carrying out air cooling to room temperature. Annealing in an annealing furnace, wherein the first annealing temperature is 950 ℃, the annealing time is 1h, air cooling is carried out to the room temperature after the heat preservation is finished, the second annealing temperature is 780 ℃, the annealing time is 2h, and air cooling is carried out to the room temperature after the heat preservation is finished. And finally, machining to remove the surface oxide skin. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 89GPa, the tensile strength is 992MPa, the yield strength is 921MPa, and the elongation is 13%.
Example 5
Pure aluminum with the purity of more than 99.9 wt.%, an Al-V intermediate phase, pure Fe, pure Y and high-purity sponge titanium are used as raw materials to smelt Ti6Al4V alloy, the smelting is repeated for 5 times to obtain alloy with uniform components, and the element content is respectively Al: 6.11 wt.%; v: 4.49 wt.%; fe: 0.21 wt.%; y: 0.10 wt.%; ti: the balance; the other impurity elements meet the relevant national standard. Heating the obtained titanium ingot to 950 ℃, then carrying out hot forging on the titanium ingot to obtain a bar material, wherein the total deformation is 73%, and then carrying out air cooling on the bar material to room temperature. Heating the obtained bar to 930 ℃, then carrying out hot drawing to obtain a wire, wherein the total deformation of the hot drawing is 71%, and then carrying out air cooling to room temperature. Annealing in an annealing furnace, wherein the first annealing temperature is 945 ℃ and the annealing time is 1.5h, air cooling to room temperature is carried out after the heat preservation is finished, the second annealing temperature is 750 ℃, the annealing time is 3h, and air cooling to room temperature is carried out after the heat preservation is finished. And finally, machining to remove the surface oxide skin. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 81GPa, the tensile strength is 1031MPa, the yield strength is 925MPa and the elongation is 11 percent.
Comparative example 1
In this comparative example, no Fe element was added, and the other conditions were the same as in example 1. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 115GPa, the tensile strength is 984MPa, the yield strength is 860MPa and the elongation is 13 percent. Obviously, the elastic modulus of the Ti6Al4V alloy has obvious reduction effect under the condition of containing Fe element.
Comparative example 2
In this comparative example, annealing was performed only once at 780 ℃ under the same conditions as in example 1. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 100GPa, the tensile strength is 1002MPa, the yield strength is 930MPa and the elongation is 14 percent. The tensile strength and yield strength of the comparative example are somewhat improved compared to example 1, but at the same time the modulus of elasticity is also increased, indicating that the dual annealing reduces the modulus of elasticity of the Ti6Al4V alloy compared to the single annealing.
Comparative example 3
In this comparative example, only one annealing was performed at 920 ℃ under the same conditions as in example 1. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 82GPa, the tensile strength is 898MPa, the yield strength is 830MPa, and the elongation is 15%. Compared with example 1, the elastic modulus of the comparative example is not obviously changed, but the tensile strength and the yield strength of the comparative example are lower than the tensile mechanical property requirements of relevant national standards on the Ti6Al4V alloy, and the application requirements can not be met.
Comparative example 4
In this comparative example, the Y element was not added, and the other conditions were the same as in example 1. The microstructure of the obtained alloy is a two-state structure. The relative test shows that the elastic modulus is 96GPa, the tensile strength is 862MPa, the yield strength is 824MPa and the elongation is 13 percent. The modulus of elasticity was higher than that of example 1, while the tensile strength, yield strength and elongation were lower than those of example 1.
Claims (7)
1. A low modulus of elasticity Ti6Al4V alloy, characterized by: the Ti6Al4V alloy comprises the following components in percentage by mass:
Al：5.5~6.2 wt.%；
V：3.8~4.5 wt.%；
Fe：0.16~0.22 wt.%；
Y：0.01~0.1 wt.%；
ti is the rest;
the elastic modulus of the Ti6Al4V alloy is 80-90 GPa; the tensile strength of the Ti6Al4V alloy is 980-1031 MPa; the yield strength is 905-953 MPa; the elongation is 11% -15%;
the preparation method of the low-elasticity-modulus Ti6Al4V alloy comprises the following steps of:
step 1 Hot forging
Heating the Ti6Al4V titanium alloy ingot to a temperature above the transformation point, and performing hot forging for multiple times to obtain a Ti6Al4V alloy bar;
step 2 Hot drawing
Heating the Ti6Al4V alloy bar obtained in the step 1 to a temperature higher than the recrystallization temperature, and carrying out multi-pass hot drawing to obtain a Ti6Al4V alloy wire;
step 3 annealing
Carrying out double annealing heat treatment on the Ti6Al4V alloy wire material obtained in the step 2 to obtain a low-elasticity-modulus Ti6Al4V alloy; the first heavy annealing temperature is 900-1000 ℃, the first heavy annealing heat preservation time is 0.5-2.5 h, and the steel plate is taken out after the heat preservation time is up and cooled to the room temperature in air; the second annealing temperature is 700-.
2. The method for preparing the low-elastic-modulus Ti6Al4V alloy according to claim 1, wherein the method comprises the following steps: in the step 1, the preparation method of the Ti6Al4V titanium alloy ingot comprises the following steps: and mixing pure Al powder, Al-V intermediate phase powder, pure Fe powder and pure Y powder according to a designed proportion, pressing into a blocky mixture, and smelting the blocky mixture for more than 5 times to obtain the Ti6Al4V alloy cast ingot.
3. The low elastic modulus Ti6Al4V alloy of claim 1, wherein: in the step 1, heating to 850-1050 ℃ and preserving heat.
4. The low elastic modulus Ti6Al4V alloy of claim 1, wherein: in the step 1, the total radial deformation amount of the bar is 85-98% after repeated hot upsetting, drawing and bar forging.
5. The low elastic modulus Ti6Al4V alloy of claim 1, wherein: in the step 2, heating to 800-1050 ℃ and preserving heat.
6. The low elastic modulus Ti6Al4V alloy of claim 1, wherein: in the step 2, the radial total deformation after the multi-pass hot drawing is 60-70%.
7. Use of a low modulus of elasticity Ti6Al4V alloy according to any one of claims 1 to 6, wherein: the low elastic modulus Ti6Al4V alloy was applied to an ultrasonic blade.
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| CN114086028A (en) * | 2021-11-18 | 2022-02-25 | 上海睿速创生医疗科技有限公司 | Special titanium alloy wire for cutter bar of medical ultrasonic knife and preparation method thereof |
| CN114345975A (en) * | 2021-12-30 | 2022-04-15 | 深圳市世格赛思医疗科技有限公司 | TC4 titanium alloy wire for ultrasonic vibration conduction and preparation method thereof |
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| CN109023189A (en) * | 2018-09-06 | 2018-12-18 | 湖南瀚德微创医疗科技有限公司 | A kind of heat treatment process improving ultrasound knife knife bar amplitude |
| CN110106395A (en) * | 2019-05-29 | 2019-08-09 | 西北有色金属研究院 | A kind of ocean engineering can weld titanium alloy with high-strength and high ductility |
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