CN115011840B - Production method of beta-type titanium alloy bar for femoral stem human body implantation - Google Patents
Production method of beta-type titanium alloy bar for femoral stem human body implantation Download PDFInfo
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000002513 implantation Methods 0.000 title claims abstract description 15
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 22
- 239000000956 alloy Substances 0.000 claims abstract description 22
- 238000005242 forging Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 229910011214 Ti—Mo Inorganic materials 0.000 claims abstract description 3
- 238000005098 hot rolling Methods 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 5
- 230000007547 defect Effects 0.000 claims description 5
- 229910001040 Beta-titanium Inorganic materials 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 230000009466 transformation Effects 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 229910011212 Ti—Fe Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000002844 melting Methods 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 5
- 238000005204 segregation Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000005096 rolling process Methods 0.000 abstract description 2
- 239000007943 implant Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 210000000988 bone and bone Anatomy 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 230000001054 cortical effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 210000004394 hip joint Anatomy 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Transplantation (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dermatology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
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- Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Forging (AREA)
Abstract
The invention provides a production method of a beta-type titanium alloy bar for human body implantation of a femoral stem, belonging to the technical field of titanium alloy bar production. The method is adjusted in the aspects of controlling the chemical composition of the cast ingot, controlling the processing technologies of forging, rolling and heat treatment, and the like, and meanwhile, the Ti-Mo intermediate alloy is adopted, so that the melting point of Mo element is reduced, the risk of inclusion and segregation is reduced, the tensile strength of the prepared TMZrF bar is 1030-1070 Mpa, the Rockwell hardness HRC is about 30, the elastic modulus is 88Gpa, the strength is higher, the biocompatibility and the wear resistance are better, and the elastic modulus is closer to that of human skeleton.
Description
Technical Field
The invention relates to the technical field of titanium alloy bar production, in particular to a production method of a beta type titanium alloy bar for femoral stem human body implantation.
Background
The biomedical material is one of novel high-tech materials, can be used as an implant to be applied in a living body so as to replace diseased tissues, and is widely used for manufacturing various medical implants. The biomedical titanium alloy has wide medical application due to the excellent biocompatibility, excellent mechanical property and low Young's modulus close to human cortical bone. Recent studies in biomedical titanium alloys have shown that the novel beta titanium alloys have better biocompatibility and lower stress shielding effect, and thus are believed to be more effective in promoting bone healing and remodeling.
The Ti-12Mo-6Zr-2Fe (TMZF) alloy is a metastable beta-type titanium alloy, has high strength, low elastic modulus, excellent corrosion resistance and wear resistance, better biocompatibility and no harmful elements, is an ideal artificial bone implant biomaterial and has been approved in clinical medical field. At present, molybdenum element is usually added in a molybdenum powder mode in the traditional preparation process of Ti-12Mo-6Zr-2Fe (TMZF) alloy, but the granularity of Mo powder is less than 0.6mm, the molybdenum element is high-density refractory metal, the melting point is 2617 ℃, the temperature of a molten pool is about 1800 ℃ in the smelting process, the non-uniform melting is easy to occur, and the inclusion phenomenon is easy to occur. In addition, the existing material for the human body implant femoral stem is TC4, but the tensile strength, the elastic modulus, the Rockwell hardness and the like of the TC4 titanium alloy can not meet the requirements for preparing the human body implant femoral stem.
Disclosure of Invention
In view of the above, the invention provides a method for producing a beta-type titanium alloy bar for human implantation of a femoral stem, which mainly solves the problems of inclusion and segregation of high-molybdenum element particles by controlling the chemical components of an ingot and the scientific and reasonable proportioning design of the components and changing the adding mode of a molybdenum element in an intermediate alloy, ensures the uniformity of the components of the ingot, and controls the processing technologies of forging, rolling, heat treatment and the like, so that the produced titanium alloy bar meets the application requirements of human implantation of the femoral stem. Meanwhile, the femoral stem made of the Ti-12Mo-6Zr-2Fe titanium alloy bar prepared by the method has the advantages of lower elastic modulus, high strength, higher fracture toughness, better wear resistance and excellent corrosion resistance, and is an excellent material for manufacturing the femoral stem in a hip joint prosthesis system.
The invention provides a method for producing a beta-type titanium alloy bar for human implantation of a femoral stem, which comprises the following steps:
step S1, smelting an ingot: preparing alloy components, pressing electrodes, and smelting into cast ingots with the diameter of 500mm by a vacuum consumable electrode arc furnace; the cast ingot comprises the following components in percentage by weight: mo:10.7% -12.5%; zr:5.2% -6.8%; fe:1.7 to 2.5 percent; al: less than or equal to 0.05 percent; si: less than or equal to 0.03 percent; o:0.16% -0.24%; c: less than or equal to 0.02 percent; n: less than or equal to 0.02 percent; h: less than or equal to 0.02 percent; the balance being Ti;
step S2, cogging and forging: after the cast ingot is subjected to ultrasonic flaw detection, sawing a cap bottom and a cap opening for forging, heating the cast ingot to a beta phase region through an electric furnace, forging the cast ingot into a bar blank with the diameter of 150mm by one fire in a 1600-ton press, and then deforming the bar blank into a required square blank;
step S3, first hot rolling: sawing the square billet, repairing surface defects, and then hot rolling at 940-960 ℃ to obtain a bar billet with phi of 55 mm; the total deformation is 85-95%;
step S4, second hot rolling: sawing the bar blank in the step S3, repairing surface defects, and hot rolling at 900-930 ℃ to obtain a bar blank with phi of 18.5 mm; the total deformation is 85-95%, and the crystal grains are further refined.
Step S5, hot drawing: heating the bar billet obtained in the step S4 at the temperature of 30-100 ℃ above the phase transformation point, drawing the bar billet into a bar billet with the diameter of 18.2mm by multiple dies, controlling the pass deformation rate to be 5% -12%, obtaining stable size, ensuring the machining allowance and improving the yield;
and S6, cutting, solution annealing and polishing to obtain the beta-type titanium alloy bar for preparing the femoral stem for human body implantation.
Preferably, the Ti element in step S1 is titanium sponge as a raw material.
Preferably, the titanium sponge is titanium sponge of grade 0 or above.
Preferably, the Mo element in the step S1 is added in a TI-Mo intermediate alloy mode, so that the melting point of the Mo element can be effectively reduced, and the risk of inclusion and segregation can be reduced.
Preferably, the Zr element is added in the form of sponge zirconium in step S1.
Preferably, the Fe element is added in the form of a Ti — Fe master alloy in step S1.
Preferably, the forging cogging temperature in step S2 is 1150 ℃, at which the original β grains can be sufficiently crushed.
Preferably, the solution treatment in step S6 is performed at an atmospheric furnace temperature of 732 to 802 ℃ for 30 to 60min to obtain stable structure and performance.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, the Mo element is added in a TI-Mo intermediate alloy mode, so that the melting point of the Mo element is reduced, and the risk of inclusion and segregation is reduced. The beta-type titanium alloy bar prepared by the method has the tensile strength of 1030-1070 Mpa, the elastic modulus of 88Gpa, the Rockwell hardness HRC of about 30, higher strength, better biocompatibility and wear resistance, and the elastic modulus which is closer to that of human skeleton.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the starting materials and auxiliaries are, unless otherwise specified, obtained from customary commercial sources or prepared in customary manner.
Example 1
The '0-grade' sponge titanium is used as a raw material, ti-Mo, ti-Fe intermediate alloy and sponge zirconium are used as main added elements, alloy components and ingredients are designed, electrodes are pressed, and the alloy components, ingredients and the alloy components are melted three times into cast ingots with the diameter of 500mm through a vacuum consumable electrode arc furnace.
The cast ingot comprises the following components in percentage by weight:
mo:10.7% -12.5%; zr:5.2% -6.8%; 1.7 to 2.5 percent of Fe; al: less than or equal to 0.05 percent; si: less than or equal to 0.03 percent; o:0.16% -0.24%; c: less than or equal to 0.02 percent; n: less than or equal to 0.02 percent; h: less than or equal to 0.02 percent; the balance being titanium;
the alloy composition meets the ASTM F1813-13 standard, and the composition is uniform.
The phase transformation point of an ingot (delta + beta/beta) is measured to be 804 ℃ by a metallographic method, the ingot is subjected to surface peeling, cap opening sawing, heating to a beta phase region by an electric furnace, forging for one time by a 1600-ton press, coping, sawing, heating to 940-960 ℃ in a resistance furnace, hot rolling to a phi 55mm bar blank, sawing, repairing surface defects, heating to 900-930 ℃ in the resistance furnace, hot rolling to the phi 18.5mm bar blank, heating the bar blank by the electric furnace (30-100 ℃ above the phase transformation point), drawing to phi 18.2mm by multiple dies, polishing and cutting, a solution annealing method of keeping 30-60min at the furnace temperature of 732-802 ℃ is adopted, and the polished finished product phi 17.2mm is obtained.
The chemical components of the ingot casting in the example 1 and various properties of the finished bar are detected, and the detection results are shown in tables 1 and 2:
table 1: chemical composition of ingot (wt%)
Table 2: mechanical property of finished bar
As is clear from the data shown in tables 1 and 2, the ingot of example 1 has satisfactory chemical indexes, small variations in the upper and lower elements, and good uniformity of the composition.
The tensile strength of the obtained product with mechanical properties reaches about 1040MPa, the performance stability is good, the Rockwell hardness HRC is about 35, and the elastic modulus is about 88Gpa.
Comparative example 1
The difference from example 1 is that the Mo element is added as Mo powder, and other conditions are not changed.
Various properties of the chemical components of the ingot casting of comparative example 1 are detected, and the detection results are shown in table 3:
TABLE 3 ingot chemical composition (wt%)
From the data shown in Table 3, it is understood that the variation of the Mo content in the upper and lower portions of the ingot of comparative example 1 is large, whereas the variation of the Mo content in the upper and lower portions of the ingot detected in example 1 is small by the addition method of the Ti-Mo master alloy.
Comparative example 2
The TC4 titanium alloy which is a commonly used domestic human implant joint material is taken as a comparative example 2, and the performance of a finished bar of the alloy is detected, and the results are shown in a table 4:
table 4: mechanical property of finished bar
The TMZrF bar has the tensile strength of 1030-1070 Mpa, higher strength, elastic modulus of 88Gpa and Rockwell hardness HRC of about 30, better biocompatibility and wear resistance, and more approximate to the elastic modulus of human skeleton.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A production method of a beta-type titanium alloy bar for human implantation of a femoral stem is characterized by comprising the following steps:
step S1, smelting an ingot: preparing alloy components, pressing electrodes, and smelting into cast ingots with the diameter of 500mm by a vacuum consumable electrode arc furnace; the cast ingot comprises the following components in percentage by weight: mo:10.7% -12.5%; zr:5.2% -6.8%; fe:1.7 to 2.5 percent; al: less than or equal to 0.05 percent; si: less than or equal to 0.03 percent; o:0.16% -0.24%; c: less than or equal to 0.02 percent; n: less than or equal to 0.02 percent; h: less than or equal to 0.02 percent; the balance being Ti;
step S2, cogging and forging: after the cast ingot is subjected to ultrasonic flaw detection, sawing a cap bottom and a cap opening for forging, heating the cast ingot to a beta phase region through an electric furnace, forging the cast ingot into a bar blank with the diameter of 150mm by one fire in a 1600-ton press, and then deforming the bar blank into a required square blank;
step S3, first hot rolling: sawing the square billet, repairing surface defects, and then hot rolling at 940-960 ℃ to obtain a bar billet with the diameter of 55 mm;
step S4, secondary hot rolling: sawing the bar blank in the step S3, repairing surface defects, and hot rolling at 900-930 ℃ to obtain a bar blank with phi of 18.5 mm;
step S5, hot drawing: heating the bar blank obtained in the step S4 at the temperature of 30-100 ℃ above the phase transformation point, drawing the bar blank into a bar blank with the diameter of 18.2mm by multiple dies, and controlling the pass deformation rate to be 5-12%;
s6, cutting, carrying out solution annealing and polishing to obtain a beta-type titanium alloy bar for preparing the femoral stem for human body implantation;
in the step S1, the Mo element is added in a Ti-Mo intermediate alloy mode;
the Fe element in the step S1 is added in a Ti-Fe intermediate alloy mode.
2. The method for producing the beta-type titanium alloy bar for human implantation of femoral stem according to claim 1, wherein the Ti element in step S1 is titanium sponge.
3. The method for producing a beta-type titanium alloy bar for human implantation of a femoral stem according to claim 2, wherein the titanium sponge is titanium sponge of grade 0 or more.
4. The method for producing a beta titanium alloy bar for human implantation of a femoral stem according to claim 1, wherein the Zr element is added in the form of zirconium sponge in step S1.
5. The method for producing a beta titanium alloy bar for human implantation of femoral stem according to claim 1, wherein the forging temperature in step S2 is 1150 ℃.
6. The method for producing the beta titanium alloy bar for human implantation of femoral stem according to claim 1, wherein the solution annealing in the step S6 is performed at an atmospheric furnace temperature of 732 to 802 ℃ for 30 to 60min.
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