CN118028657A - Medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy and bar, and preparation methods and applications thereof - Google Patents
Medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy and bar, and preparation methods and applications thereof Download PDFInfo
- Publication number
- CN118028657A CN118028657A CN202410186985.5A CN202410186985A CN118028657A CN 118028657 A CN118028657 A CN 118028657A CN 202410186985 A CN202410186985 A CN 202410186985A CN 118028657 A CN118028657 A CN 118028657A
- Authority
- CN
- China
- Prior art keywords
- temperature
- alloy
- titanium alloy
- ingot
- smelting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 152
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000956 alloy Substances 0.000 claims abstract description 137
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 127
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000005266 casting Methods 0.000 claims abstract description 24
- 239000010936 titanium Substances 0.000 claims abstract description 19
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 238000003723 Smelting Methods 0.000 claims description 101
- 238000005242 forging Methods 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 46
- 238000001816 cooling Methods 0.000 claims description 31
- 206010040844 Skin exfoliation Diseases 0.000 claims description 30
- 229910017305 Mo—Si Inorganic materials 0.000 claims description 26
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 26
- 229910052710 silicon Inorganic materials 0.000 claims description 26
- 238000005098 hot rolling Methods 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- 239000010955 niobium Substances 0.000 claims description 19
- 229910052726 zirconium Inorganic materials 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052750 molybdenum Inorganic materials 0.000 claims description 17
- 239000010703 silicon Substances 0.000 claims description 17
- 229910002804 graphite Inorganic materials 0.000 claims description 15
- 239000010439 graphite Substances 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 238000005498 polishing Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 15
- 230000032683 aging Effects 0.000 claims description 14
- 229910052758 niobium Inorganic materials 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 238000003754 machining Methods 0.000 claims description 12
- 229910052718 tin Inorganic materials 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 11
- 239000010949 copper Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910001257 Nb alloy Inorganic materials 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 238000003466 welding Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims description 5
- 244000046052 Phaseolus vulgaris Species 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 5
- 230000007547 defect Effects 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 5
- 238000010894 electron beam technology Methods 0.000 claims description 5
- 239000000314 lubricant Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000009853 pyrometallurgy Methods 0.000 claims description 5
- 239000013589 supplement Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 230000001276 controlling effect Effects 0.000 description 8
- 230000009286 beneficial effect Effects 0.000 description 7
- 210000000988 bone and bone Anatomy 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 4
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 3
- 239000003870 refractory metal Substances 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001040 Beta-titanium Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 230000037182 bone density Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000003832 thermite Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 230000008733 trauma Effects 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy, a bar and a preparation method and application thereof, and belongs to the technical field of titanium alloy materials. The titanium alloy comprises the following components ：Al6.0-7.0％,Sn1.80-2.20％,Zr2.80-3.20％,Mo4.80-5.20％,Nb0.80-1.20％,Si0.40-0.60％,C0.03-0.05％,Fe＜0.015％,O0.07-0.14％,Ti by mass percent and the balance. According to the invention, the mixing method of the mixer is used for ensuring the uniformity of alloy components of the intermediate alloy in the axial direction and the radial direction of the ingot in the ingot casting and the three-time vacuum self-consumption ingot casting process is adopted, so that the uniformity and consistency of alloy elements in the titanium alloy ingot are improved, the crystallization speed of the ingot is regulated, the size and the direction of crystal grains of the ingot are controlled, and the prepared medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy meets the requirements.
Description
Technical Field
The invention belongs to the technical field of titanium alloy materials, and particularly relates to a medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy, a bar, a preparation method and application thereof.
Background
Titanium and titanium alloys based on an alpha-phase pure titanium and an alpha+beta-type Ti-6Al-4V component are widely used in the medical field, the pure titanium is used in oral medical treatment, the Ti-6Al-4V alloy is widely used in artificial joints and bone fixation, and in the medical instrument field, a specially developed titanium alloy material is basically blank.
The ultrasonic osteotome is a new surgical instrument in the medical field in recent years, is widely used in the bone cutting occasion in the treatment process, and has the characteristics of small trauma, shortened operation time and no damage to blood vessels, nerves and soft tissues. Generally, the ultrasonic osteotome made of the Ti-6Al-4V titanium alloy material can meet the use requirement of the material strength with the heat-resistant temperature of about 400 ℃. However, at the position with high bone density, the ultrasonic osteotome material has not only enough normal temperature strength and rigidity, but also high heat resistance at 600 ℃. This is because the ultrasonic osteotome material must have high thermosetting properties because of the high heat generation during cutting of high density bone tissue. In the actual use process, the heat-resistant temperature of the titanium alloy material of the ultrasonic osteotome is required to be more than or equal to 600 ℃, but the heat-resistant temperature of most titanium alloys in the current markets at home and abroad can not meet the requirement. Traditionally, heat resistant titanium alloys are important materials for aerospace and are also hot spot materials developed in various countries. In particular to a heat-resistant titanium alloy material for manufacturing a compressor wheel disc and a blade of an aircraft engine, which has high heat-resistant requirement and is used at the temperature of 500-550 ℃. However, when a titanium alloy with a higher heat resistance temperature is required for manufacturing medical devices, no special alternative heat resistant titanium alloy brand is available.
As for the titanium alloy rod for manufacturing the ultrasonic osteotome material, not only is the strength high enough, but also the structure and the performance of the titanium alloy material are stable and reliable, and the manufacturing of the heat-resistant titanium alloy needs higher content of heat-resistant alloy elements, the uniformity of components is difficult to control, and the heat processing is difficult.
Therefore, how to develop a medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy, a rod, a preparation method and application thereof are technical problems to be solved by the technicians in the field.
Disclosure of Invention
In view of the above, the invention provides a medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy and bar, and a preparation method and application thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy comprises the following components ：Al：6.0-7.0％,Sn：1.80-2.20％,Zr：2.80-3.20％,Mo：4.80-5.20％,Nb：0.80-1.20％,Si：0.40-0.60％,C：0.03-0.05％,Fe：＜0.015％,O：0.07-0.14％,Ti percent by mass and the balance.
The invention has the beneficial effects that: ① The heat-resistant titanium alloy must have a considerable amount of alloy elements with stable alpha phase represented by aluminum, and must also have a certain amount of alloy elements with stable beta phase represented by molybdenum, so that the stability of the structure is ensured, and the occurrence of brittle phases is avoided, thereby affecting the mechanical properties.
② The high temperature resistant titanium alloy is a titanium alloy which is difficult to break through at home and abroad, and because the heat resistance at 50 ℃ is very difficult to improve, molybdenum and niobium elements with high melting points must be added, and the component ranges of the two elements play a key role in the influence of the heat resistant titanium alloy, so the titanium alloy must be distinguished from other similar titanium alloys at home and abroad in component ranges.
③ The high temperature resistant titanium alloy is mainly used for airplanes and rocket engines, has high requirement on fatigue strength, is a material for ultrasonic bone knives, has low requirement on fatigue strength and high requirement on heat strength, so silicon must be accurately added to match with control of the carbon content range, and titanium carbide formed in the ingot casting smelting process is also a high temperature resistant compound, so that the heat strength of the titanium alloy is greatly influenced. This is why the silicon and carbon composition is strictly controlled.
The composition of a near-alpha titanium alloy and a very small portion of a solid-solution-strengthened alpha+beta titanium alloy is theoretically the best heat resistance because the content of aluminum in the stable alpha phase is relatively high, and the contents of Al, sn and Zr are determined in combination with other neutral alloy elements, and in order to prevent the occurrence of an alpha' brittle phase in the titanium alloy, it is necessary to add an alloy element for stabilizing the beta phase and an element for improving heat resistance, and the contents of Mo, nb and Si are determined.
The medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy mark is specified to be Ti65321.
Further, the Al equivalent > 8.0, and the equivalent value is calculated by the following expression:
al equivalent = al+sn/3+zr/6+10×o.
The invention also provides a preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy, which comprises the following steps:
(1) Manufacturing an Al-Mo-Si ternary master alloy:
A. Putting pure aluminum beans, molybdenum and silicon into a graphite crucible, carrying out pyrometallurgy to obtain a master alloy casting, peeling off a riser, crushing, mixing the obtained master alloy casting ingot to obtain a master alloy crushed material, and analyzing the components of the master alloy crushed material;
B. Placing the analyzed intermediate alloy crushed aggregates into a high-purity graphite crucible of a vacuum induction furnace for vacuum smelting, adding silicon according to the components of the intermediate alloy crushed aggregates to supplement burnt silicon in the smelting process, adjusting to a proper proportion, casting alloy ingots, peeling and crushing the ingots, analyzing the components to obtain an Al-Mo-Si ternary intermediate alloy, and controlling the mass ratio of Mo to Si to be 10:1 and the balance of Al;
(2) Manufacturing a Ti-Nb-Sn ternary master alloy:
a. Smelting titanium sponge and metallic niobium by a vacuum electron beam furnace, peeling the smelted cast ingot, analyzing components, and carrying out mechanical processing and cutting to obtain Ti-Nb alloy blocks;
b. Placing the cut Ti-Nb alloy blocks into a water-cooled copper crucible induction furnace for melting, pressing the tin blocks into a molten pool under the protection of argon after thoroughly melting, adjusting the temperature of molten metal, casting alloy ingots, cooling the ingot furnace, discharging the ingot furnace, peeling the ingot, analyzing the components, carrying out mechanical processing and crushing to obtain a Ti-Nb-Sn ternary intermediate alloy, controlling the mass ratio of the components Nb to Sn to be 1:2, and balancing Ti;
(3) Accurately weighing titanium sponge, al-Mo-Si ternary intermediate alloy, ti-Nb-Sn ternary intermediate alloy and zirconium sponge, mixing in a mixer, placing the uniformly mixed materials into a hydraulic extruder die, extruding into consumable electrode blocks by a hydraulic extruder of two thousand tons, and placing the extruded consumable electrode blocks into a vacuum welding box for assembly welding to form consumable electrodes;
(4) And (3) placing the consumable electrode into a vacuum consumable arc furnace for three times of vacuum consumable smelting, cooling to obtain a titanium alloy cast ingot, detecting a flaw of the titanium alloy cast ingot, removing a riser, performing machining and peeling treatment on the surface of the titanium alloy cast ingot to obtain a titanium alloy finished product cast ingot, sampling three points of the titanium alloy finished product cast ingot up, down, and analyzing the components of the titanium alloy cast ingot to obtain the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy.
The invention has the beneficial effects that: the invention is a high temperature resistant high strength titanium alloy, which needs to add 6 alloy elements, belonging to titanium alloy with high alloy content, wherein molybdenum and niobium are refractory metals with high melting point, especially niobium, if added in the form of simple substance pure niobium, metal inclusion and component segregation are easy to form in the process of titanium alloy casting. Tin and aluminum are low-melting-point metals, and are added as simple substance pure metals, so that volatilization burning loss is serious, and the component stability of the titanium alloy cast ingot cannot be ensured. The alloying elements must therefore be added in the form of a master alloy, and the composition and production method of the master alloy are the subject that each titanium alloy production enterprise must face. The traditional production method of the intermediate alloy used at home and abroad is a thermite method, and because the production method is smelting in the atmosphere, the impurity components such as oxygen, nitrogen and the like are difficult to control, the stability and consistency of the intermediate alloy are poor, and the use requirement of the titanium alloy with high alloy content cannot be met. In many cases, for high alloy content titanium alloys, master alloy composition selection, process recipe and quality control are determinants of the quality of the titanium alloy melted ingot.
The invention adopts Al-Mo-Si ternary intermediate alloy and Ti-Nb-Sn ternary intermediate alloy to respectively add five alloy elements Al, mo, si, nb, sn, and because Zr and Ti are infinitely solid-solved and have little difference in melting point, the zirconium sponge is used for adding Zr in pure metal.
The high-quality titanium alloy ingot casting is the most basic work of high-performance processing materials, and has decisive effects on the uniformity, consistency and stability of the performance of the titanium alloy materials. The consistency index of the domestic titanium alloy material performance is lower than that of the developed national product for a long time, and the key factor is that the quality of the titanium alloy cast ingot is lower than the foreign level, so that each link of the titanium alloy cast ingot production must be emphasized.
Consumable electrode manufacturing for the first smelting is the most important and fundamental operation. The invention is different from the domestic traditional feeding process of the intermediate alloy package, ensures the uniformity of alloy components of the intermediate alloy in the axial direction and the radial direction of the ingot in the ingot casting process by using a mixer mixing method, and is a basic process for ensuring the quality of the ingot.
The titanium alloy is further refined on the basis of the first consumable ingot by adopting a three-time vacuum consumable smelting ingot casting process, the second vacuum consumable smelting and the third vacuum consumable smelting, the uniformity and the consistency of alloy elements in the titanium alloy ingot are improved, the ingot crystallization speed is regulated, and the grain size and the grain direction of the ingot are controlled.
The titanium alloy thin rod used for manufacturing the ultrasonic osteotome has high requirements on uniformity of components and consistency of performance of titanium alloy materials because of ultrasonic conduction, and the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy prepared by the invention meets the requirements.
Further, the sponge zirconium comprises more than 99.90% of Zr in percentage by mass;
the granularity of the Al-Mo-Si ternary intermediate alloy and the granularity of the Ti-Nb-Sn ternary intermediate alloy are controlled to be 2.0-6.0mm, and the contents of gas and impurity components of the two ternary intermediate alloys are controlled to be as follows according to mass percent: o is less than 0.060, N is less than 0.005%, H is less than 0.002%, C:0.03-0.04%;
The sponge titanium is 0-grade sponge titanium, the granularity is controlled to be 3.0-8.0mm, and the impurity component content is controlled as follows according to the mass percent: o is less than 0.05%, N is less than 0.002%, and Fe is less than 0.010%.
The beneficial effect of adopting the further technical scheme is that: as the amount of the added alloy elements of the titanium alloy is relatively high, the quality of the intermediate alloy has an important influence on the quality of the titanium alloy cast ingot, so that the gas and impurities of the Al-Mo-Si ternary intermediate alloy and the Ti-Nb-Sn ternary intermediate alloy are controlled, and the uniform distribution of the intermediate alloy during electrode extrusion can be ensured only when the granularity of the Al-Mo-Si ternary intermediate alloy and the granularity of the Ti-Nb-Sn ternary intermediate alloy are consistent.
Further, in the step (4), the vacuum degree of the three times of vacuum consumable smelting is 3.0 multiplied by 10 -3-1.0×10-3 mmHg;
Wherein, the smelting current of the first vacuum consumable smelting is 9000A-10000A, the smelting voltage is 25-40V, and the diameter of the first vacuum consumable ingot is 220-225mm;
The smelting current of the secondary vacuum consumable smelting is 13000A-14000A, the smelting voltage is 25-42V, and the diameter of the secondary vacuum consumable ingot is 310-315mm;
The smelting current of the third vacuum consumable smelting is 18000A-20000A, the smelting voltage is 25-45V, the diameter of the third vacuum consumable ingot is 400-405mm, and the cooling water temperature of the copper crucible is controlled to be less than 36 ℃.
The beneficial effect of adopting the further technical scheme is that: the primary vacuum consumable smelting process has great influence on ingot quality, and because the smelting power is changed greatly in the smelting process, the arc length and the vacuum degree are unstable, different smelting process changes are adopted according to different titanium alloy element compositions. In the titanium alloy, the vacuum degree is changed severely in different smelting stages due to the fact that the titanium alloy contains volatile element tin. In the initial stage of smelting, arc stabilization must be adopted, and measures of improving vacuum degree with high air extraction rate are taken to ensure the purity of the titanium alloy metal liquid. In the smelting process, the smelting current is changed from low to high to stable and then from stable to low.
The third vacuum consumable smelting also needs to consider the cooling intensity of the cast ingot, the solidification speed, the cast ingot feeding, the cast ingot yield improvement, the cooling intensity of the water-cooled copper crucible and the like, and ensures that refractory metals are uniformly distributed in the cast ingot.
The size of the vacuum consumable ingot can be selected according to the size of a crucible of a smelting furnace and the alloy content in the titanium alloy, and the size of the ingot is determined by combining various factors because the refractory metal content of the titanium alloy is high, the electromagnetic stirring time of a molten pool is long.
Further, in the step (4), according to mass percent, the components and design errors in the finished titanium alloy ingot are controlled as follows: al < 0.02%, sn < 0.02%, zr < 0.01%, mo < 0.01%, nb < 0.01%, si < 0.001%, and C < 0.010%.
The beneficial effect of adopting the further technical scheme is that: the uniformity, accuracy and consistency of the components have great influence on the performance of the titanium alloy. The axial upper, middle and lower parts of the ingot have large deviation of radial surface and central components, which indicates that the components have substantial segregation, and the method is also the root cause that the performance of the Chinese titanium alloy is always lower than that of imported products. The component error value of the invention is far superior to the standard and actual production control values of the titanium alloy cast ingots at home and abroad.
The invention also provides a preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar, which comprises the following steps:
① Cogging of titanium alloy cast ingot: heating, forging and cogging the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy according to any one of claims 3 to 6 by using a 3000 ton hydraulic rapid forging machine and a high-temperature resistance furnace with the power of 120KW, grinding the blank, removing oxide scales and forging defects by machining, sawing and blanking;
② Finish forging the bar material: heating and forging by using an 800-ton hydraulic rapid forging machine and a 75KW resistance furnace, mechanically processing a bar stock, removing surface oxide skin, sawing and blanking to obtain a hot-rolled blank;
③ And (3) hot rolling: heating and hot rolling a hot rolled blank by using a 460 type high-speed wire rod hot rolling mill and a box type resistance furnace with the power of 75KW, and water-cooling;
④ And (5) hot finish drawing: hot stretching and air cooling are carried out by using an80 ton adjustable speed flat drawing stretcher and a 10m horizontal high-temperature alloy tubular resistance heating furnace with the power of 85 KW;
⑤ And (3) heat treatment: heating by using a resistance furnace with the power of 75KW, and sequentially carrying out solution treatment, air cooling, aging treatment and air cooling;
⑥ Thermal straightening: carrying out thermal straightening by using an electric heating straightener with the power of 45 KW;
⑦ Peeling, polishing and flaw detection: rough machining is carried out by using a centerless grinder, fine grinding is carried out by using a high-precision grinder, polishing is carried out by using a polishing machine, and the obtained bar is detected by an ultrasonic flaw detector, so that the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar is obtained.
The invention has the beneficial effects that: the titanium alloy is heat-resistant high-strength titanium alloy, and has high heat strength and high deformation resistance, so that the cogging, hot rolling and stretch forming of a titanium alloy ingot are all carried out on bars, compared with other alpha-phase, near-alpha-phase and alpha+beta-phase titanium alloys, the heat processing difficulty is much higher, and the processing capacity of required processing equipment is generally higher. The stability and consistency of the mechanical properties of the bars are further improved by heat treatment.
Further, in step ①, the heating temperature is 1190 ℃, the heat preservation time is 1.5 hours, the forging temperature is 1050-1180 ℃, the deformation rate of one firing time is 30-45%, and the cross section of the blank is square with side length of 230 mm;
In the step ②, the heating temperature is 1120 ℃, the forging temperature is 1020-1120 ℃, the deformation rate of one firing time is 30-50%, and the diameter of the bar stock is 85-87mm;
in the step ③, the heating temperature is 1120 ℃, the hot rolling temperature is 1000-1120 ℃, the hot rolling linear speed is 3-6 m/S, the pass deformation rate is 20-30%, and the diameter of the finished product is 12mm;
In the step ④, the hot stretching temperature is 950-1050 ℃, the pass deformation rate is 15-25%, emulsified graphite is adopted as a lubricant, and the diameter of a finished product is 3.0-5.0mm;
in the step ⑤, the solution treatment temperature is 980-1030 ℃ plus or minus 10 ℃, the heat preservation time is 30 minutes, the aging treatment temperature is 650-690 ℃, and the heat preservation time is 45-60 minutes;
In step ⑥, the thermal straightening temperature is 580-600 ℃, and the diameter shrinkage error is 0.01mm.
Further, in step ①, the forging deformation speed is changed: low-speed, medium-speed, high-speed, low-speed, deformation change: high- & gt low- & gt high;
in step ②, the forging deformation speed is changed: medium speed→fast, deformation change: high- & gtlow.
The invention also provides the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar prepared by the method.
The invention has the beneficial effects that: the physical properties of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar prepared by the invention are as follows: ① density: ρ=4.6-4.62 g/cm 3;② elastic modulus E:20 ℃,118-121GPa;600 ℃,90-94GPa; ③ thermal conductivity: 6.18-6.22W/m at 100deg.C; 600 ℃ 11.20-11.60W/m; ④ Linear thermal expansion: 20-600 ℃ and 0.49-0.53%;
mechanical properties (after solution+aging treatment) ① room temperature tensile properties: sigma b 1080-1150MPa, sigma 0.2980-1020MPa, delta 12-14%, psi 22-25%;
② Tensile properties at 600 ℃): sigma b 660-700MPa, sigma 0.2550-600MPa, delta 16-18%, and psi 35-37%.
The invention also provides application of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar in preparation of a medical high-temperature-resistant high-strength ultrasonic osteotome.
Drawings
Fig. 1 is a photograph of a metallographic structure of a solid solution state of a medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar according to example 1 of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy comprises the following components ：Al：6.50％,Sn：2.10％,Zr：3.20％,Mo：4.95％,Nb：1.20％,Si：0.47％,C：0.03％,Fe：0.012％,O：0.070％,N：0.0015％,H：0.0010％,Ti percent by mass and the balance.
Al equivalent > 8.0, equivalent value is calculated from the following expression:
al equivalent = al+sn/3+zr/6+10×o.
The preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy comprises the following steps:
(1) Manufacturing an Al-Mo-Si ternary master alloy:
A. Placing pure aluminum beans, molybdenum and silicon into a graphite crucible, carrying out pyrometallurgy to obtain a master alloy casting, wherein the smelting temperature is 2700 ℃, and carrying out peeling riser, crushing and mixing on the obtained master alloy casting ingot to obtain master alloy crushed aggregates and analyzing the components of the master alloy crushed aggregates;
B. Placing the analyzed intermediate alloy crushed aggregates into a high-purity graphite crucible of a vacuum induction furnace for vacuum smelting, wherein the smelting temperature is 2200 ℃, adding silicon according to the components of the intermediate alloy crushed aggregates to supplement burnt silicon in the smelting process, adjusting the proportion to a proper level, casting alloy ingots, peeling and crushing the ingots, analyzing the components to obtain an Al-Mo-Si ternary intermediate alloy, controlling the mass ratio of the components Mo and Si to be 10:1, and balancing Al;
(2) Manufacturing a Ti-Nb-Sn ternary master alloy:
a. Smelting titanium sponge and metallic niobium by a vacuum electron beam furnace, wherein the smelting temperature is 2600 ℃, peeling the smelted cast ingot, analyzing components, and carrying out mechanical processing and cutting to obtain Ti-Nb alloy blocks;
b. placing the cut Ti-Nb alloy blocks into a water-cooled copper crucible induction furnace for melting, pressing the tin blocks into a molten pool under the protection of argon after thoroughly melting, adjusting the temperature of molten metal to 1700 ℃, pouring alloy ingots, cooling the ingot furnace, discharging the ingot furnace, peeling the ingot, analyzing the components, carrying out mechanical processing and crushing to obtain a Ti-Nb-Sn ternary intermediate alloy, controlling the mass ratio of the components Nb to Sn to be 1:2, and the balance Ti;
(3) Accurately weighing titanium sponge, al-Mo-Si ternary intermediate alloy, ti-Nb-Sn ternary intermediate alloy and zirconium sponge, mixing in a mixer, placing the uniformly mixed materials into a hydraulic extruder die, extruding into consumable electrode blocks by a hydraulic extruder of two thousand tons, and placing the extruded consumable electrode blocks into a vacuum welding box for assembly welding to form consumable electrodes;
the sponge zirconium comprises Zr in percentage by mass: 99.91%;
The granularity of the Al-Mo-Si ternary intermediate alloy and the granularity of the Ti-Nb-Sn ternary intermediate alloy are controlled to be 2.0-6.0mm, and the contents of gas and impurity components of the Al-Mo-Si ternary intermediate alloy are as follows by mass percent: o:0.050%, N:0.003%, H:0.001%, C:0.035%, the content of Ti-Nb-Sn ternary master alloy gas and impurity components are: o: 0.04%, N:0.002%, H:0.001%, C:0.03%;
The titanium sponge is 0-grade titanium sponge, the granularity is controlled to be 3.0-8.0mm, and the impurity components of the titanium sponge are as follows in percentage by mass: o:0.04%, N:0.001%, fe:0.009%.
(4) Placing the consumable electrode into a vacuum consumable arc furnace for three times of vacuum consumable smelting, wherein the smelting temperature of the first time of vacuum consumable smelting is 1800 ℃, the smelting current is 9500A, the smelting voltage is 30V, and the diameter of a first time of vacuum consumable ingot is 220-225mm;
The smelting temperature of the secondary vacuum consumable smelting is 1850 ℃, the smelting current is 13500A, the smelting voltage is 32V, and the diameter of the secondary vacuum consumable ingot is 310-315mm;
The smelting temperature of the third vacuum consumable smelting is 1900 ℃, the smelting current is 19000A, the smelting voltage is 34V, the diameter of the third vacuum consumable ingot is 400-405mm, the cooling temperature of copper crucible cooling water is controlled to 34 ℃, the titanium alloy ingot is obtained, flaw detection and riser removal are carried out on the titanium alloy ingot, the surface of the titanium alloy ingot is subjected to mechanical processing and peeling treatment, the titanium alloy finished ingot is obtained, the upper, middle and lower three points of the titanium alloy finished ingot are sampled, and the components of the titanium alloy finished ingot are analyzed, so that the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy is obtained.
The components and design errors in the titanium alloy finished product cast ingot are as follows by mass percent: al:0.01%, sn:0.01%, zr:0.007%, mo:0.008%, nb:0.005%, si:0.0008%, C:0.005%.
The preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar comprises the following steps:
① Cogging of titanium alloy cast ingot: heating, forging and cogging a medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy with the size phi of 390mm by using a 3000-ton hydraulic rapid forging machine and a high-temperature resistance furnace with the power of 120KW, grinding the blank, removing oxide scales and forging defects by machining, sawing and blanking;
heating temperature is 1190 ℃, heat preservation time is 1.5 hours, initial forging temperature is 1170 ℃, final forging temperature is 1050 ℃, one-firing deformation rate is 35%, and blank size is as follows: 230X 2000mm;
Forging deformation speed change: low-speed, medium-speed, high-speed, low-speed, deformation change: high- & gt low- & gt high;
② Finish forging the bar material: heating and forging by using an 800-ton hydraulic rapid forging machine and a 75KW resistance furnace, mechanically processing a bar stock, removing surface oxide skin, sawing and blanking to obtain a hot-rolled blank;
The heating temperature is 1120 ℃, the initial forging temperature is 1120 ℃, the final forging temperature is 1020 ℃, the first-time deformation rate is 30%, and the bar size is as follows: phi 85-87mm multiplied by 1500mm;
forging deformation speed change: medium speed→fast, deformation change: high- & gt low;
③ And (3) hot rolling: heating and hot rolling a hot rolled blank by using a 460 type high-speed wire rod hot rolling mill and a box type resistance furnace with the power of 75KW, and water-cooling;
the heating temperature is 1120 ℃, and the rolling temperature is as follows: 1120 ℃, finishing temperature: the hot rolling line speed is 5 m/S at 1010 ℃, the pass deformation rate is 25%, and the diameter of a finished product is 12mm;
④ And (5) hot finish drawing: hot stretching and air cooling are carried out by using an80 ton adjustable speed flat drawing stretcher and a 10m horizontal high-temperature alloy tubular resistance heating furnace with the power of 85 KW;
The hot stretching temperature is 980 ℃, the pass deformation rate is 18%, emulsified graphite is adopted as a lubricant, and the size of a finished product is: phi 3.2mm x 5000mm;
⑤ And (3) heat treatment: heating by using a resistance furnace with the power of 75KW, and sequentially carrying out solution treatment, air cooling, aging treatment and air cooling;
the solution treatment temperature is 980 ℃, the heat preservation time is 30 minutes, the aging treatment temperature is 680 ℃, and the heat preservation time is 45 minutes;
⑥ Thermal straightening: carrying out thermal straightening by using an electric heating straightener with the power of 45 KW;
the thermal straightening temperature is 580 ℃, and the diameter shrinkage error is 0.01mm;
⑦ Peeling, polishing and flaw detection: rough machining is carried out by using a centerless grinder, fine grinding is carried out by using a high-precision grinder, polishing is carried out by using a polishing machine, and the obtained bar is detected by using an ultrasonic flaw detector to obtain the finished product size: phi 2.5+0.010mm×1500mm medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar.
Mechanical properties of medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bars:
Physical properties: ① density: ρ=4.61 g/cm 3;② elastic modulus E:20 ℃ and 119GPa;600 ℃,92GPa; ③ thermal conductivity: 6.20W/m DEG C at 100 ℃;600 ℃ 11.50W/m. DEGC; ④ Linear thermal expansion: 20-600 ℃ and 0.51%;
Mechanical properties (after solution+aging treatment) ① room temperature tensile properties: sigma b 1150MPa, sigma 0.21020MPa, delta 13 percent, and psi 23 percent;
② Tensile properties at 600 ℃): sigma b 690MPa, sigma 0.2585MPa, delta 18 percent and psi 37 percent.
Example 2
The medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy comprises the following components ：Al：6.0％,Sn：1.80％,Zr：2.80％,Mo：4.80％,Nb：0.80％,Si：0.40％,C：0.04％,Fe：0.012％,O：0.11％,N：0.0015％,H：0.0010％,Ti percent by mass and the balance.
Al equivalent > 8.0, equivalent value is calculated from the following expression:
al equivalent = al+sn/3+zr/6+10×o.
The preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy comprises the following steps:
(1) Manufacturing an Al-Mo-Si ternary master alloy:
A. Placing pure aluminum beans, molybdenum and silicon into a graphite crucible, carrying out pyrometallurgy to obtain a master alloy casting, wherein the smelting temperature is 2700 ℃, and carrying out peeling riser, crushing and mixing on the obtained master alloy casting ingot to obtain master alloy crushed aggregates and analyzing the components of the master alloy crushed aggregates;
B. Placing the analyzed intermediate alloy crushed aggregates into a high-purity graphite crucible of a vacuum induction furnace for vacuum smelting, wherein the smelting temperature is 2200 ℃, adding silicon according to the components of the intermediate alloy crushed aggregates to supplement burnt silicon in the smelting process, adjusting the proportion to a proper level, casting alloy ingots, peeling and crushing the ingots, analyzing the components to obtain an Al-Mo-Si ternary intermediate alloy, controlling the mass ratio of the components Mo and Si to be 10:1, and balancing Al;
(2) Manufacturing a Ti-Nb-Sn ternary master alloy:
a. Smelting titanium sponge and metallic niobium by a vacuum electron beam furnace, wherein the smelting temperature is 2600 ℃, peeling the smelted cast ingot, analyzing components, and carrying out mechanical processing and cutting to obtain Ti-Nb alloy blocks;
b. placing the cut Ti-Nb alloy blocks into a water-cooled copper crucible induction furnace for melting, pressing the tin blocks into a molten pool under the protection of argon after thoroughly melting, adjusting the temperature of molten metal to 1700 ℃, pouring alloy ingots, cooling the ingot furnace, discharging the ingot furnace, peeling the ingot, analyzing the components, carrying out mechanical processing and crushing to obtain a Ti-Nb-Sn ternary intermediate alloy, controlling the mass ratio of the components Nb to Sn to be 1:2, and the balance Ti;
(3) Accurately weighing titanium sponge, al-Mo-Si ternary intermediate alloy, ti-Nb-Sn ternary intermediate alloy and zirconium sponge, mixing in a mixer, placing the uniformly mixed materials into a hydraulic extruder die, extruding into consumable electrode blocks by a hydraulic extruder of two thousand tons, and placing the extruded consumable electrode blocks into a vacuum welding box for assembly welding to form consumable electrodes;
The sponge zirconium comprises Zr in percentage by mass: 99.92%;
The granularity of the Al-Mo-Si ternary intermediate alloy and the granularity of the Ti-Nb-Sn ternary intermediate alloy are controlled to be 2.0-6.0mm, and the contents of gas and impurity components of the Al-Mo-Si ternary intermediate alloy are as follows by mass percent: o:0.040%, N:0.003%, H:0.001%, C:0.03 percent of Ti-Nb-Sn ternary master alloy gas and the impurity components with the contents of: o:0.050%, N:0.004%, H:0.001%, C:0.04%;
The titanium sponge is 0-grade titanium sponge, the granularity is controlled to be 3.0-8.0mm, and the impurity components of the titanium sponge are as follows in percentage by mass: o:0.04%, N:0.001%, fe:0.009%.
(4) Placing the consumable electrode into a vacuum consumable arc furnace for three times of vacuum consumable smelting, wherein the smelting temperature of the first time of vacuum consumable smelting is 1800 ℃, the smelting current is 9500A, the smelting voltage is 30V, and the diameter of a first time of vacuum consumable ingot is 220-225mm;
The smelting temperature of the secondary vacuum consumable smelting is 1850 ℃, the smelting current is 13500A, the smelting voltage is 32V, and the diameter of the secondary vacuum consumable ingot is 310-315mm;
The smelting temperature of the third vacuum consumable smelting is 1900 ℃, the smelting current is 19000A, the smelting voltage is 34V, the diameter of the third vacuum consumable ingot is 400-405mm, the cooling water temperature of the copper crucible is controlled to 35 ℃, the titanium alloy ingot is obtained, flaw detection and riser removal are carried out on the titanium alloy ingot, the surface of the titanium alloy ingot is subjected to mechanical processing and peeling treatment, the titanium alloy finished ingot is obtained, the upper, middle and lower three points of the titanium alloy finished ingot are sampled, and the components of the titanium alloy finished ingot are analyzed, so that the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy is obtained.
The components and design errors in the titanium alloy finished product cast ingot are as follows by mass percent: al:0.01%, sn:0.01%, zr:0.007%, mo:0.008%, nb:0.005%, si:0.0008%, C:0.005%.
The preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar comprises the following steps:
① Cogging of titanium alloy cast ingot: heating, forging and cogging a medical high-temperature-resistant high-strength ultrasonic bone knife titanium alloy by using a 3000-ton hydraulic quick forging machine and a high-temperature resistance furnace with the power of 120KW, grinding the blank, removing oxide scales and forging defects by machining, sawing and blanking;
Heating temperature is 1190 ℃, heat preservation time is 1.5 hours, initial forging temperature is 1170 ℃, final forging temperature is 1050 ℃, one-firing deformation rate is 30%, and blank size is as follows: 230X 2000mm;
Forging deformation speed change: low-speed, medium-speed, high-speed, low-speed, deformation change: high- & gt low- & gt high;
② Finish forging the bar material: heating and forging by using an 800-ton hydraulic rapid forging machine and a 75KW resistance furnace, mechanically processing a bar stock, removing surface oxide skin, sawing and blanking to obtain a hot-rolled blank;
The heating temperature is 1120 ℃, the initial forging temperature is 1120 ℃, the final forging temperature is 1020 ℃, the first-time deformation rate is 40%, and the diameter of the bar stock is 85-87mm;
forging deformation speed change: medium speed→fast, deformation change: high- & gt low;
③ And (3) hot rolling: heating and hot rolling a hot rolled blank by using a 460 type high-speed wire rod hot rolling mill and a box type resistance furnace with the power of 75KW, and water-cooling;
The heating temperature is 1120 ℃, and the rolling temperature is as follows: 1120 ℃, finishing temperature: the hot rolling line speed is 4 m/S at 1010 ℃, the pass deformation rate is 25%, and the diameter of a finished product is 12mm;
④ And (5) hot finish drawing: hot stretching and air cooling are carried out by using an80 ton adjustable speed flat drawing stretcher and a 10m horizontal high-temperature alloy tubular resistance heating furnace with the power of 85 KW;
the hot stretching temperature is 950 ℃, the pass deformation rate is 20%, emulsified graphite is adopted as a lubricant, and the size of the finished product is as follows: phi 3.2mm x 5000mm;
⑤ And (3) heat treatment: heating by using a resistance furnace with the power of 75KW, and sequentially carrying out solution treatment, air cooling, aging treatment and air cooling;
The solution treatment temperature is 980 ℃, the heat preservation time is 30 minutes, the aging treatment temperature is 650 ℃, and the heat preservation time is 45 minutes;
⑥ Thermal straightening: carrying out thermal straightening by using an electric heating straightener with the power of 45 KW;
the thermal straightening temperature is 580 ℃, and the diameter shrinkage error is 0.01mm;
⑦ Peeling, polishing and flaw detection: rough machining is carried out by using a centerless grinder, fine grinding is carried out by using a high-precision grinder, polishing is carried out by using a polishing machine, and the obtained bar is detected by using an ultrasonic flaw detector to obtain the finished product size: phi 2.5+0.010mm×1500mm medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar.
Mechanical properties of medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bars:
Physical properties: ① density: ρ=4.60 g/cm 3;② elastic modulus E:20 ℃,118GPa;600 ℃,90GPa; ③ thermal conductivity: 6.18W/m at 100deg.C; 600 ℃ 11.20W/m. DEGC; ④ Linear thermal expansion: 20-600 ℃ and 0.49%;
Mechanical properties (after solution+aging treatment) ① room temperature tensile properties: sigma b 1150MPa, sigma 0.21020MPa, delta 14%, psi 25%;
② Tensile properties at 600 ℃): sigma b 700MPa, sigma 0.2600MPa, delta 18 percent and psi 37 percent.
Example 3
The medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy comprises the following components ：Al：7.0％,Sn：2.20％,Zr：3.0％,Mo：5.20％,Nb：1.0％,Si：0.60％,C：0.05％,Fe：0.012％,O：0.14％,N：0.0015％,H：0.0010％,Ti percent by mass and the balance.
Al equivalent > 8.0, equivalent value is calculated from the following expression:
al equivalent = al+sn/3+zr/6+10×o.
The preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy comprises the following steps:
(1) Manufacturing an Al-Mo-Si ternary master alloy:
A. Placing pure aluminum beans, molybdenum and silicon into a graphite crucible, carrying out pyrometallurgy to obtain a master alloy casting, wherein the smelting temperature is 2700 ℃, and carrying out peeling riser, crushing and mixing on the obtained master alloy casting ingot to obtain master alloy crushed aggregates and analyzing the components of the master alloy crushed aggregates;
B. Placing the analyzed intermediate alloy crushed aggregates into a high-purity graphite crucible of a vacuum induction furnace for vacuum smelting, wherein the smelting temperature is 2200 ℃, adding silicon according to the components of the intermediate alloy crushed aggregates to supplement burnt silicon in the smelting process, adjusting the proportion to a proper level, casting alloy ingots, peeling and crushing the ingots, analyzing the components to obtain an Al-Mo-Si ternary intermediate alloy, controlling the mass ratio of the components Mo and Si to be 10:1, and balancing Al;
(2) Manufacturing a Ti-Nb-Sn ternary master alloy:
a. Smelting titanium sponge and metallic niobium by a vacuum electron beam furnace, wherein the smelting temperature is 2600 ℃, peeling the smelted cast ingot, analyzing components, and carrying out mechanical processing and cutting to obtain Ti-Nb alloy blocks;
b. placing the cut Ti-Nb alloy blocks into a water-cooled copper crucible induction furnace for melting, pressing the tin blocks into a molten pool under the protection of argon after thoroughly melting, adjusting the temperature of molten metal to 1700 ℃, pouring alloy ingots, cooling the ingot furnace, discharging the ingot furnace, peeling the ingot, analyzing the components, carrying out mechanical processing and crushing to obtain a Ti-Nb-Sn ternary intermediate alloy, controlling the mass ratio of the components Nb to Sn to be 1:2, and the balance Ti;
(3) Accurately weighing titanium sponge, al-Mo-Si ternary intermediate alloy, ti-Nb-Sn ternary intermediate alloy and zirconium sponge, mixing in a mixer, placing the uniformly mixed materials into a hydraulic extruder die, extruding into consumable electrode blocks by a hydraulic extruder of two thousand tons, and placing the extruded consumable electrode blocks into a vacuum welding box for assembly welding to form consumable electrodes;
The sponge zirconium comprises Zr in percentage by mass: 99.93%;
the granularity of the Al-Mo-Si ternary intermediate alloy and the granularity of the Ti-Nb-Sn ternary intermediate alloy are controlled to be 2.0-6.0mm, and the contents of gas and impurity components of the Al-Mo-Si ternary intermediate alloy are as follows by mass percent: o:0.050%, N:0.004%, H:0.001%, C:0.04%;
the content of the Ti-Nb-Sn ternary master alloy gas and the impurity components are as follows: o:0.040%, N:0.003%, H:0.001%, C:0.03%;
The titanium sponge is 0-grade titanium sponge, the granularity is controlled to be 3.0-8.0mm, and the impurity components of the titanium sponge are as follows in percentage by mass: o:0.04%, N:0.001%, fe:0.009%.
(4) Placing the consumable electrode into a vacuum consumable arc furnace for three times of vacuum consumable smelting, wherein the smelting temperature of the first time of vacuum consumable smelting is 1800 ℃, the smelting current is 9500A, the smelting voltage is 30V, and the diameter of a first time of vacuum consumable ingot is 220-225mm;
The smelting temperature of the secondary vacuum consumable smelting is 1850 ℃, the smelting current is 13500A, the smelting voltage is 32V, and the diameter of the secondary vacuum consumable ingot is 310-315mm;
The smelting temperature of the third vacuum consumable smelting is 1900 ℃, the smelting current is 19000A, the smelting voltage is 34V, the diameter of the third vacuum consumable ingot is 400-405mm, the cooling water temperature of the copper crucible is controlled to 35 ℃, the titanium alloy ingot is obtained, flaw detection and riser removal are carried out on the titanium alloy ingot, the surface of the titanium alloy ingot is subjected to mechanical processing and peeling treatment, the titanium alloy finished ingot is obtained, the upper, middle and lower three points of the titanium alloy finished ingot are sampled, and the components of the titanium alloy finished ingot are analyzed, so that the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy is obtained.
The components and design errors in the titanium alloy finished product cast ingot are as follows by mass percent: al:0.01%, sn:0.01%, zr:0.007%, mo:0.008%, nb:0.005%, si:0.0008%, C:0.005%.
The preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar comprises the following steps:
① Cogging of titanium alloy cast ingot: heating, forging and cogging a medical high-temperature-resistant high-strength ultrasonic bone knife titanium alloy by using a 3000-ton hydraulic quick forging machine and a high-temperature resistance furnace with the power of 120KW, grinding the blank, removing oxide scales and forging defects by machining, sawing and blanking;
the heating temperature is 1190 ℃, the heat preservation time is 1.5 hours, the initial forging temperature is 1170 ℃, the final forging temperature is 1050 ℃, the deformation rate of one firing is 45%, and the cross section of the blank is square with the side length of 230 mm;
Forging deformation speed change: low-speed, medium-speed, high-speed, low-speed, deformation change: high- & gt low- & gt high;
② Finish forging the bar material: heating and forging by using an 800-ton hydraulic rapid forging machine and a 75KW resistance furnace, mechanically processing a bar stock, removing surface oxide skin, sawing and blanking to obtain a hot-rolled blank;
The heating temperature is 1120 ℃, the initial forging temperature is 1120 ℃, the final forging temperature is 1020 ℃, the first-time deformation rate is 50%, and the diameter of the bar stock is 85-87mm;
forging deformation speed change: medium speed→fast, deformation change: high- & gt low;
③ And (3) hot rolling: heating and hot rolling a hot rolled blank by using a 460 type high-speed wire rod hot rolling mill and a box type resistance furnace with the power of 75KW, and water-cooling;
The heating temperature is 1120 ℃, and the rolling temperature is as follows: 1120 ℃, finishing temperature: the hot rolling line speed is 6 m/S at 1010 ℃, the pass deformation rate is 30%, and the diameter of a finished product is 12mm;
④ And (5) hot finish drawing: hot stretching and air cooling are carried out by using an80 ton adjustable speed flat drawing stretcher and a 10m horizontal high-temperature alloy tubular resistance heating furnace with the power of 85 KW;
the hot stretching temperature is 1050 ℃, the pass deformation rate is 25%, emulsified graphite is adopted as a lubricant, and phi 5mm is multiplied by 5000mm;
⑤ And (3) heat treatment: heating by using a resistance furnace with the power of 75KW, and sequentially carrying out solution treatment, air cooling, aging treatment and air cooling;
the solution treatment temperature is 1030 ℃, the heat preservation time is 30 minutes, the aging treatment temperature is 690 ℃, and the heat preservation time is 60 minutes;
⑥ Thermal straightening: carrying out thermal straightening by using an electric heating straightener with the power of 45 KW;
the thermal straightening temperature is 600 ℃, and the diameter shrinkage error is 0.01mm;
⑦ Peeling, polishing and flaw detection: rough machining is carried out by using a centerless grinder, fine grinding is carried out by using a high-precision grinder, polishing is carried out by using a polishing machine, and the obtained bar is detected by using an ultrasonic flaw detector to obtain the finished product size: phi 2.5+0.010mm×1500mm medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar.
Mechanical properties of medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bars:
Physical properties: ① density: ρ=4.62 g/cm 3;② elastic modulus E:20 ℃ and 121GPa;600 ℃,94GPa; ③ thermal conductivity: 6.22W/m at 100deg.C; 600 ℃ 11.60W/m. DEGC; ④ Linear thermal expansion: 20-600 ℃ and 0.53%;
mechanical properties (after solution+aging treatment) ① room temperature tensile properties: sigma b 1080MPa, sigma 0.2980MPa, delta 12 percent, and psi 22 percent;
② Tensile properties at 600 ℃): sigma b 660MPa, sigma 0.2550MPa, delta 16 percent and psi 35 percent.
The description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy is characterized by comprising the following components ：Al：6.0-7.0％,Sn：1.80-2.20％,Zr：2.80-3.20％,Mo：4.80-5.20％,Nb：0.80-1.20％,Si：0.40-0.60％,C：0.03-0.05％,Fe：＜0.015％,O：0.07-0.14％,Ti percent by mass and the balance.
2. The medical high temperature and high strength ultrasonic osteotome titanium alloy of claim 1, wherein Al equivalent is > 8.0, the equivalent value calculated by the following expression:
al equivalent = al+sn/3+zr/6+10×o.
3. A method for preparing the medical high-temperature and high-strength ultrasonic osteotome titanium alloy according to any one of claims 1 to 2, which is characterized by comprising the following steps:
(1) Manufacturing an Al-Mo-Si ternary master alloy:
A. Putting pure aluminum beans, molybdenum and silicon into a graphite crucible, carrying out pyrometallurgy to obtain a master alloy casting, peeling off a riser, crushing, mixing the obtained master alloy casting ingot to obtain a master alloy crushed material, and analyzing the components of the master alloy crushed material;
B. Placing the analyzed intermediate alloy crushed aggregates into a high-purity graphite crucible of a vacuum induction furnace for vacuum smelting, adding silicon according to the components of the intermediate alloy crushed aggregates to supplement burnt silicon in the smelting process, adjusting to a proper proportion, casting alloy ingots, peeling and crushing the ingots, analyzing the components to obtain an Al-Mo-Si ternary intermediate alloy, and controlling the mass ratio of Mo to Si to be 10:1 and the balance of Al;
(2) Manufacturing a Ti-Nb-Sn ternary master alloy:
a. Smelting titanium sponge and metallic niobium by a vacuum electron beam furnace, peeling the smelted cast ingot, analyzing components, and carrying out mechanical processing and cutting to obtain Ti-Nb alloy blocks;
b. Placing the cut Ti-Nb alloy blocks into a water-cooled copper crucible induction furnace for melting, pressing the tin blocks into a molten pool under the protection of argon after thoroughly melting, adjusting the temperature of molten metal, casting alloy ingots, cooling the ingot furnace, discharging the ingot furnace, peeling the ingot, analyzing the components, carrying out mechanical processing and crushing to obtain a Ti-Nb-Sn ternary intermediate alloy, controlling the mass ratio of the components Nb to Sn to be 1:2, and balancing Ti;
(3) Accurately weighing titanium sponge, al-Mo-Si ternary intermediate alloy, ti-Nb-Sn ternary intermediate alloy and zirconium sponge, mixing in a mixer, placing the uniformly mixed materials into a hydraulic extruder die, extruding into consumable electrode blocks by a hydraulic extruder of two thousand tons, and placing the extruded consumable electrode blocks into a vacuum welding box for assembly welding to form consumable electrodes;
(4) And (3) placing the consumable electrode into a vacuum consumable arc furnace for three times of vacuum consumable smelting, cooling to obtain a titanium alloy cast ingot, detecting a flaw of the titanium alloy cast ingot, removing a riser, performing machining and peeling treatment on the surface of the titanium alloy cast ingot to obtain a titanium alloy finished product cast ingot, sampling three points of the titanium alloy finished product cast ingot up, down, and analyzing the components of the titanium alloy cast ingot to obtain the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy.
4. The method for preparing the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy according to claim 3, wherein the sponge zirconium comprises more than 99.90% of Zr by mass percent;
The granularity of the Al-Mo-Si ternary intermediate alloy and the granularity of the Ti-Nb-Sn ternary intermediate alloy are controlled to be 2.0-6.0mm, and the contents of gas and impurity components of the two ternary intermediate alloys are respectively controlled as follows by mass percent: o is less than 0.060, N is less than 0.005%, H is less than 0.002%, C:0.03-0.04%;
The sponge titanium is 0-grade sponge titanium, the granularity is controlled to be 3.0-8.0mm, and the impurity component content is controlled as follows according to the mass percent: o is less than 0.05%, N is less than 0.002%, and Fe is less than 0.010%.
5. The method for preparing the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy according to claim 3, wherein in the step (4), the vacuum degree of three times of vacuum consumable smelting is 3.0×10 -3-1.0×10-3 mmHg;
Wherein, the smelting current of the first vacuum consumable smelting is 9000A-10000A, the smelting voltage is 25-40V, and the diameter of the first vacuum consumable ingot is 220-225mm;
The smelting current of the secondary vacuum consumable smelting is 13000A-14000A, the smelting voltage is 25-42V, and the diameter of the secondary vacuum consumable ingot is 310-315mm;
the smelting current of the third vacuum consumable smelting is 18000A-20000A, the smelting voltage is 25-45V, the diameter of the third vacuum consumable ingot is 400-405mm, and the cooling is to control the temperature of the copper crucible cooling water to be less than 36 ℃.
6. The method for preparing the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy according to claim 3, wherein in the step (4), the components and design errors in the finished titanium alloy ingot are controlled as follows by mass percent: al < 0.02%, sn < 0.02%, zr < 0.01%, mo < 0.01%, nb < 0.01%, si < 0.001%, and C < 0.010%.
7. The preparation method of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar is characterized by comprising the following steps of:
① Cogging of titanium alloy cast ingot: heating, forging and cogging the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy according to any one of claims 3 to 6 by using a 3000 ton hydraulic rapid forging machine and a high-temperature resistance furnace with the power of 120KW, grinding the blank, removing oxide scales and forging defects by machining, sawing and blanking;
② Finish forging the bar material: heating and forging by using an 800-ton hydraulic rapid forging machine and a 75KW resistance furnace, mechanically processing a bar stock, removing surface oxide skin, sawing and blanking to obtain a hot-rolled blank;
③ And (3) hot rolling: heating and hot rolling a hot rolled blank by using a 460 type high-speed wire rod hot rolling mill and a box type resistance furnace with the power of 75KW, and water-cooling;
④ And (5) hot finish drawing: hot stretching and air cooling are carried out by using an80 ton adjustable speed flat drawing stretcher and a 10m horizontal high-temperature alloy tubular resistance heating furnace with the power of 85 KW;
⑤ And (3) heat treatment: heating by using a resistance furnace with the power of 75KW, and sequentially carrying out solution treatment, air cooling, aging treatment and air cooling;
⑥ Thermal straightening: carrying out thermal straightening by using an electric heating straightener with the power of 45 KW;
⑦ Peeling, polishing and flaw detection: rough machining is carried out by using a centerless grinder, fine grinding is carried out by using a high-precision grinder, polishing is carried out by using a polishing machine, and the obtained bar is detected by an ultrasonic flaw detector, so that the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar is obtained.
8. The method for preparing the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar according to claim 7, wherein in the step ①, the heating temperature is 1190 ℃, the heat preservation time is 1.5 hours, the forging temperature is 1050-1180 ℃, the deformation rate at one firing time is 30-45%, and the cross section of the blank is square with the side length of 230 mm;
In the step ②, the heating temperature is 1120 ℃, the forging temperature is 1020-1120 ℃, the deformation rate of one firing time is 30-50%, and the diameter of the bar stock is 85-87mm;
in the step ③, the heating temperature is 1120 ℃, the hot rolling temperature is 1000-1120 ℃, the hot rolling linear speed is 3-6 m/S, the pass deformation rate is 20-30%, and the diameter of the finished product is 12mm;
In the step ④, the hot stretching temperature is 950-1050 ℃, the pass deformation rate is 15-25%, emulsified graphite is adopted as a lubricant, and the diameter of a finished product is 3.0-5.0mm;
In the step ⑤, the solution treatment temperature is 980-1030 ℃, the heat preservation time is 30 minutes, the aging treatment temperature is 650-690 ℃, and the heat preservation time is 45-60 minutes;
In step ⑥, the thermal straightening temperature is 580-600 ℃, and the diameter shrinkage error is 0.01mm.
9. A medical high temperature and high intensity ultrasonic osteotome titanium alloy bar prepared by the method of any one of claims 7-8.
10. Use of the medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy bar according to claim 9 in preparing a medical high-temperature-resistant high-strength ultrasonic osteotome.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410186985.5A CN118028657A (en) | 2024-02-20 | 2024-02-20 | Medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy and bar, and preparation methods and applications thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410186985.5A CN118028657A (en) | 2024-02-20 | 2024-02-20 | Medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy and bar, and preparation methods and applications thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118028657A true CN118028657A (en) | 2024-05-14 |
Family
ID=90988871
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410186985.5A Pending CN118028657A (en) | 2024-02-20 | 2024-02-20 | Medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy and bar, and preparation methods and applications thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118028657A (en) |
-
2024
- 2024-02-20 CN CN202410186985.5A patent/CN118028657A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100567534C (en) | The hot-work of the high-temperature titanium alloy of a kind of high heat-intensity, high thermal stability and heat treating method | |
| JP3395443B2 (en) | High creep strength titanium alloy and its manufacturing method | |
| CN105925842B (en) | A kind of manufacture method of high-quality titanium alloy | |
| CN114645162A (en) | Manufacturing method of fine-grain homogeneous disc forging of high-temperature alloy difficult to deform | |
| CN108546850A (en) | A kind of production method of 6101 aluminum alloy plate materials of high conductivity | |
| WO2020195049A1 (en) | Method for producing ni-based super-heat-resistant alloy, and ni-based super-heat-resistant alloy | |
| JPH05214470A (en) | Rhombic titanium niobium aluminide containing vanadium | |
| CN111910103A (en) | Titanium alloy sheet material and method for producing same | |
| CN111549244A (en) | Preparation method of Ti35 titanium alloy ingot | |
| CN108251693A (en) | A kind of High-strength high-plasticity three-phase TiAl alloy and preparation method thereof | |
| WO2021046928A1 (en) | Large pipe-diameter ni-v rotary target material containing trace elements and preparation method therefor | |
| CN115198162B (en) | Entropy alloy in high-toughness heterogeneous multi-phase core-shell organization structure and preparation method thereof | |
| CN113846247A (en) | W-Mo-Co reinforced high-temperature alloy hot-rolled bar and preparation method thereof | |
| CN106636746A (en) | High-strength and high-elongation high-temperature titanium alloy and preparing technology thereof | |
| CN118028657A (en) | Medical high-temperature-resistant high-strength ultrasonic osteotome titanium alloy and bar, and preparation methods and applications thereof | |
| US4370299A (en) | Molybdenum-based alloy | |
| CN113278812B (en) | Vacuum consumable melting method for high-Mo-content Ti-Mo alloy homogeneous ingot | |
| CN111394606B (en) | Gold-based high-resistance alloy, alloy material and preparation method thereof | |
| CN114905010A (en) | Nickel-based alloy wire and preparation method thereof | |
| JP4371201B2 (en) | β-type titanium alloy and method for producing the same | |
| CN113481418B (en) | Nickel-aluminum-molybdenum-chromium-vanadium-iron eutectic high-entropy alloy and preparation method thereof | |
| CN115852267B (en) | High-strength high-conductivity low-expansion iron-nickel-molybdenum alloy wire and production method thereof | |
| CN115821171B (en) | Trace B element doped modified high-strength high-plasticity multicomponent alloy, and preparation method and application thereof | |
| CN115369286B (en) | Alpha + beta type titanium alloy for fastener, preparation method and preparation method of bar thereof | |
| CN115233063B (en) | High-strength high-temperature NbSiTiCx alloy and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |