CN101724764B - Process for preparing biomedical beta-titanium alloy - Google Patents
Process for preparing biomedical beta-titanium alloy Download PDFInfo
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- CN101724764B CN101724764B CN2009103111984A CN200910311198A CN101724764B CN 101724764 B CN101724764 B CN 101724764B CN 2009103111984 A CN2009103111984 A CN 2009103111984A CN 200910311198 A CN200910311198 A CN 200910311198A CN 101724764 B CN101724764 B CN 101724764B
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Abstract
The invention discloses a process for preparing a biomedical beta-titanium alloy. The process comprises the following steps: A) alloy preparation; B) surface coating; C) hot forging and cogging; D) hot rolling; E) cold rolling and molding; and F) heat treatment. In the process, the material is manufactured to a 2mm plate after the beta-titanium alloy is subjected to high vacuum electric arc melting, repeated stirring, casting, phase transformation point measuring, homogenization under the protection of vacuum and argon, coating, hot forging, hot rolling, cold rolling, solid solution, water quenching, artificial aging and water cooling so as to prepare the biomedical beta-titanium alloy with excellent comprehensive performance. The process is a biomedical beta-titanium preparation process capable of improving the material strength, abrasion resistance and corrosion resistance, reducing the elasticity modulus of the material, and maintaining excellent manufacturing and molding performance of the material.
Description
Technical field
The present invention relates to a kind of preparation technology of titanium alloy, relate in particular to a kind of preparation technology of beta-titanium alloy material in biology medical application.
Background technology
Bio-medical material is an important branch of Materials science, being to be used to diagnose, treat or alternative tissue, organ or the novel carriers material promoting its function, have high technology content and high economic worth, is frontier that is developing in the material science and technology.Bio-medical material is made bigger contribution for exploration human life secret, guarantee human health longevity.Nearly 10 for many years, does the growth rate of market of bio-medical material and goods remain on 20% always? about 5%, estimate to comprise that the medical apparatus industry of bio-medical material will reach the pharmaceutical products market scale in following 10 years-15 years, become the mainstay industry of 21 century world economy.In the bio-medical metallic substance, titanium and alloy thereof rely on excellent comprehensive performances, become the preferred material of medical implants products such as joint prosthesis (hip, knee, shoulder, ankle, elbow, wrist, articulations digitorum manus etc.), bone wound product (intramedullary nail, steel plate, screw etc.), backbone correcting internal fixation system, tooth implant, denture fixing device, tooth orthopedic wire, heart valve prosthesis, intervention angiocarpy bracket.At present, also be not used for clinical than the better metallic substance of titanium alloy.In the exploitation of medical titanium alloy, to research and develop low elastic modulus on the one hand, high-wear resistance, corrosion resistance and high-fracture toughness hang down crack growth rate, high damage tolerance, and have the biomedical beta-titanium alloy material of good biocompatibility; The component of alloy should be to pay attention to the prerequisite that is added to of nontoxic element on the other hand.The Ti-Nb-Zr-Fe-Ta series titanium alloy becomes the first-selection of biological medical titanium alloy of new generation owing to have the Young's modulus that more approaches human body bone.But owing to added refractory metal Ta in the alloy, the fusing point height of itself and matrix metal Ti more than 1300 degree, generally add and be difficult to dissolve in form of pure metal, can be present in the alloy with simple substance form, and in the following process process, this simple substance comes off mutually easily, the effect that does not have, can have influence on the composition and the performance of material simultaneously, therefore the method that will seek a kind of Ta of adding.In addition, the titanium alloy specific activity is higher, is easy to oxidation in hot procedure, influences its over-all properties, expects that a kind of new technology prevents the technology of surface oxidation in the time of guaranteeing titanium alloy hot-work, thereby guarantees alloy processing characteristics and use properties.
Summary of the invention
Technical problem to be solved by this invention provides and a kind ofly can improve the strength of materials, wear resistance and corrosion stability, reduces elasticity modulus of materials, keeps the preparation technology of the bio-medical beta-titanium alloy of material well processed forming property.
In order to solve the problems of the technologies described above, the preparation technology of bio-medical beta-titanium alloy provided by the invention comprises the steps:
A) alloy preparation
Ti, Nb, Zr, Fe, Ta pure metal and Ti-Ta master alloy are by alloying constituent mass percent batching, melting in the high vacuum arc heating furnace, fully stir, be cast into ingot blank, fully the sampling of cooling back is analyzed alloy solid-liquid phase temperature through DTA, add the Ar gas shiled and carry out homogenizing annealing in vacuum oven, homogenization temperature is 950～1050 ℃, and the time is 8～12h;
B) surface-coated
At ingot blank surface-coated one deck is the oxidation and increase lubricated when preventing high temperature process of the coating of main component with the boron nitride;
C) forge hot cogging
1050～1150 ℃ of ingot blank Heating temperatures are incubated 1～2 hour, adopt flat-die forging, and 780～820 ℃ of final forging temperatures are swaged into the 10mm heavy-gauge sheeting after the repeated multiple times;
D) hot rolling
Forge back sheet material and be heated to 1050～1150 ℃, be incubated beginning hot rolling in 0.5～1.5 hour, be rolled into 3mm sheet material through multi-pass;
E) cold roll forming
After the hot rolled plate annealing, it is cold rolling to carry out multi-pass then, and being rolled to final thickness is 2mm;
F) thermal treatment
Cold rolling back sample carries out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 800～850 ℃, and solution time is 1～2 hour, carries out shrend after the solid solution, and the artificial aging temperature is 320～360 ℃, and aging time is 3～5 hours, uses water cooling after the timeliness.
Adopt the preparation technology of the bio-medical beta-titanium alloy of technique scheme, by adding the Ti-Ta master alloy, the one, guarantee that high-meltiing alloy element T a adds back composition accuracy, the 2nd, guarantee that Ta is solid-solubilized in the alloy, come off with simple substance point particle form when being unlikely to following process, could really guarantee the alloy low elastic modulus like this; When preventing alloy hot-work surface oxidation and reduce with its processing units between friction, forge hot is preceding armor coated at alloy surface, has improved the processability of material, thereby has helped improving the alloy over-all properties.The preparation technology that the present invention proposes improves on the basis that traditional titanium alloy melting processing alloy element all adds with the form of simple substance pure metal, adopt Ti-Ta master alloy form to add, all the other elements use pure metal, guaranteed so fully to be dissolved in the alloy after high-melting-point element T a adds, carried out follow-up cold and hot working again and be unlikely to from alloy, to come off; On the basis of conventional alloys complete processing, increase coating for surface protection technology before the forge hot, heat following process such as forge hot after the coating again.
The advantage and the positively effect of invention: after beta-titanium alloy of the present invention adopts the high vacuum arc melting to add repeatedly to stir, cast, survey transformation temperature, vacuum to add argon shield homogenizing, coating, forge hot, hot rolling, cold rolling, solid solution, shrend, artificial aging, water-cooled; materials processing is become the thick sheet material of 2mm, prepare beta-titanium alloy bio-medical material with excellent comprehensive performance.
Material performance index is as follows respectively:
Young's modulus (GPa): 40-60; Breaking tenacity: 600-910; Yield strength (MPa): 480-650; Elongation (%): 14-18; Relative reduction in area (%): 40-52.
In sum, the present invention a kind ofly can improve the strength of materials, wear resistance and corrosion stability, reduces elasticity modulus of materials, keeps the preparation technology of the bio-medical beta-titanium alloy of material well processed forming property.
Description of drawings
Fig. 1 is tensile property specimen size of the present invention (GB3076-82) synoptic diagram.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1:
A) alloy preparation
The Ti-25Nb-5Zr-0.2Fe-15Ta alloy, Ti, Nb, Zr, Fe pure metal and Ti-Ta master alloy are by alloying constituent mass percent batching, melting in the high vacuum arc heating furnace, fully stir, be cast into 100 * 60 * 20mm ingot blank, fully the sampling of cooling back is analyzed alloy solid-liquid phase temperature through DTA, carries out homogenizing annealing (adding the Ar gas shiled) in vacuum oven, homogenization temperature is 1000 ℃, and the time is 10h;
B) surface-coated
Applying one deck at alloy surface is the oxidation and increase lubricated when preventing high temperature process of the coating of main component with the boron nitride;
C) forge hot cogging
1100 ℃ of ingot blank Heating temperatures are incubated 2 hours, adopt flat-die forging, and 800 ℃ of final forging temperatures are swaged into the 10mm heavy-gauge sheeting after the repeated multiple times;
D) hot rolling
Forge back sheet material and be heated to 1100 ℃, be incubated beginning hot rolling in 1 hour, be rolled into 3mm sheet material through multi-pass;
E) cold roll forming
After the hot rolled plate annealing, it is cold rolling to carry out multi-pass then, and being rolled to final thickness is 2mm;
F) thermal treatment
Cold rolling back sample carries out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 800 ℃, and solution time is 2.5 hours, carries out shrend after the solid solution, and the artificial aging temperature is 340 ℃, and aging time is 5 hours, uses water cooling after the timeliness;
G) material property
Referring to Fig. 1, Young's modulus (GPa): 40; Breaking tenacity (MPa): 650; Yield strength (MPa): 520; Elongation (%): 16; Relative reduction in area (%): 42.
Embodiment 2:
A) alloy preparation
The Ti-28Nb-3Zr-0.6Fe-12Ta alloy, Ti, Nb, Zr, Fe pure metal and Ti-Ta master alloy are by alloying constituent mass percent batching, melting in the high vacuum arc heating furnace, fully stir, be cast into 100 * 60 * 20mm ingot blank, fully the sampling of cooling back is analyzed alloy solid-liquid phase temperature through DTA, carries out homogenizing annealing (adding the Ar gas shiled) in vacuum oven, homogenization temperature is 950 ℃, and the time is 12h;
B) surface-coated
Applying one deck at alloy surface is the oxidation and increase lubricated when preventing high temperature process of the coating of main component with the boron nitride;
C) forge hot cogging
1150 ℃ of ingot blank Heating temperatures are incubated 2 hours, adopt flat-die forging, and 780 ℃ of final forging temperatures are swaged into the 10mm heavy-gauge sheeting after the repeated multiple times;
D) hot rolling
Forge back sheet material and be heated to 1050 ℃, be incubated beginning hot rolling in 1 hour, be rolled into 3mm sheet material through multi-pass;
E) cold roll forming
After the hot rolled plate annealing, it is cold rolling to carry out multi-pass then, and being rolled to final thickness is 2mm;
F) thermal treatment
Cold rolling back sample carries out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 800 ℃, and solution time is 2 hours, carries out shrend after the solid solution, and the artificial aging temperature is 360 ℃, and aging time is 3 hours, uses water cooling after the timeliness;
G) material property
Young's modulus (GPa): 50; Breaking tenacity (MPa): 780; Yield strength (MPa): 650; Elongation (%): 17; Relative reduction in area (%): 48.
Embodiment 3:
A) alloy preparation
The Ti-30Nb-1Zr-1Fe-10Ta alloy, Ti, Nb, Zr, Fe pure metal and Ti-Ta master alloy are by alloying constituent mass percent batching, melting in the high vacuum arc heating furnace, fully stir, be cast into 100 * 60 * 20mm ingot blank, fully the sampling of cooling back is analyzed alloy solid-liquid phase temperature through DTA, carries out homogenizing annealing (adding the Ar gas shiled) in vacuum oven, homogenization temperature is 980 ℃, and the time is 8h;
B) surface-coated
At ingot blank surface-coated one deck is the oxidation and increase lubricated when preventing high temperature process of the coating of main component with the boron nitride;
C) forge hot cogging
1100 ℃ of ingot blank Heating temperatures are incubated 1.5 hours, adopt flat-die forging, and 800 ℃ of final forging temperatures are swaged into the 10mm heavy-gauge sheeting after the repeated multiple times;
D) hot rolling
Forge back sheet material and be heated to 1100 ℃, be incubated beginning hot rolling in 1 hour, be rolled into 3mm sheet material through multi-pass;
E) cold roll forming
After the hot rolled plate annealing, it is cold rolling to carry out multi-pass then, and being rolled to final thickness is 2mm
F) thermal treatment
Cold rolling back sample carries out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 850 ℃, and solution time is 1 hour, carries out shrend after the solid solution, and the artificial aging temperature is 320 ℃, and aging time is 4 hours, uses water cooling after the timeliness;
G) material property
Young's modulus (GPa): 55; Breaking tenacity (MPa): 850; Yield strength (MPa): 620; Elongation (%): 15; Relative reduction in area (%): 42.
Embodiment 4:
A) alloy preparation
The Ti-30Nb-5Zr-1Fe-15Ta alloy, Ti, Nb, Zr, Fe pure metal and Ti-Ta master alloy are by alloying constituent mass percent batching, melting in the high vacuum arc heating furnace, fully stir, be cast into 100 * 60 * 20mm ingot blank, fully the sampling of cooling back is analyzed alloy solid-liquid phase temperature through DTA, carries out homogenizing annealing (adding the Ar gas shiled) in vacuum oven, homogenization temperature is 1000 ℃, and the time is 9h;
B) surface-coated
At ingot blank surface-coated one deck is the oxidation and increase lubricated when preventing high temperature process of the coating of main component with the boron nitride;
C) forge hot cogging
1150 ℃ of ingot blank Heating temperatures are incubated 2 hours, adopt flat-die forging, and 800 ℃ of final forging temperatures are swaged into the 10mm heavy-gauge sheeting after the repeated multiple times;
D) hot rolling
Forge back sheet material and be heated to 1100 ℃, be incubated beginning hot rolling in 0.5 hour, be rolled into 3mm sheet material through multi-pass;
E) cold roll forming
After the hot rolled plate annealing, it is cold rolling to carry out multi-pass then, and being rolled to final thickness is 2mm;
F) thermal treatment
Cold rolling back sample carries out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 850 ℃, and solution time is 1 hour, carries out shrend after the solid solution, and the artificial aging temperature is 330 ℃, and aging time is 5 hours, uses water cooling after the timeliness;
G) material property
Young's modulus (GPa): 60; Breaking tenacity (MPa): 910; Yield strength (MPa): 650; Elongation (%): 14; Relative reduction in area (%): 40.
Embodiment 5:
A) alloy preparation
The Ti-25Nb-1Zr-0.2Fe-10Ta alloy, Ti, Nb, Zr, Fe pure metal and Ti-Ta master alloy are by alloying constituent mass percent batching, melting in the high vacuum arc heating furnace, fully stir, be cast into 100 * 60 * 20mm ingot blank, fully the sampling of cooling back is analyzed alloy solid-liquid phase temperature through DTA, carries out homogenizing annealing (adding the Ar gas shiled) in vacuum oven, homogenization temperature is 1050 ℃, and the time is 11h;
B) surface-coated
At ingot blank surface-coated one deck is the oxidation and increase lubricated when preventing high temperature process of the coating of main component with the boron nitride;
C) forge hot cogging
1100 ℃ of ingot blank Heating temperatures are incubated 1 hour, adopt flat-die forging, and 820 ℃ of final forging temperatures are swaged into the 10mm heavy-gauge sheeting after the repeated multiple times;
D) hot rolling
Forge back sheet material and be heated to 1050 ℃, be incubated beginning hot rolling in 1 hour, be rolled into 3mm sheet material through multi-pass;
E) cold roll forming
After the hot rolled plate annealing, it is cold rolling to carry out multi-pass then, and being rolled to final thickness is 2mm;
F) thermal treatment
Cold rolling back sample carries out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 850 ℃, and solution time is 1 hour, carries out shrend after the solid solution, and the artificial aging temperature is 350 ℃, and aging time is 5 hours, uses water cooling after the timeliness;
G) material property
Young's modulus (GPa): 40; Breaking tenacity (MPa): 600; Yield strength (MPa): 480; Elongation (%):; Relative reduction in area (%): 52.
Claims (1)
1. the preparation technology of a bio-medical beta-titanium alloy is characterized in that: comprise the steps:
A) alloy preparation
Ti, Nb, Zr, Fe pure metal and Ti-Ta master alloy are by alloying constituent mass percent batching, melting in the high vacuum arc heating furnace, fully stir, be cast into ingot blank, fully the sampling of cooling back is analyzed alloy solid-liquid phase temperature through DTA, add the Ar gas shiled and carry out homogenizing annealing in vacuum oven, homogenization temperature is 950～1050 ℃, and the time is 8～12h;
B) surface-coated
At ingot blank surface-coated one deck is the oxidation and increase lubricated when preventing high temperature process of the coating of main component with the boron nitride;
C) forge hot cogging
1050～1150 ℃ of ingot blank Heating temperatures are incubated 1～2 hour, adopt flat-die forging, and 780～820 ℃ of final forging temperatures are swaged into the 10mm heavy-gauge sheeting after the repeated multiple times;
D) hot rolling
Forge back sheet material and be heated to 1050～1150 ℃, be incubated beginning hot rolling in 0.5～1.5 hour, be rolled into 3mm sheet material through multi-pass;
E) cold roll forming
After the hot rolled plate annealing, it is cold rolling to carry out multi-pass then, and being rolled to final thickness is 2mm;
F) thermal treatment
Cold rolling back sample carries out solution treatment in chamber type electric resistance furnace, solid solubility temperature is 800～850 ℃, and solution time is 1～2 hour, carries out shrend after the solid solution, and the artificial aging temperature is 320～360 ℃, and aging time is 3～5 hours, uses water cooling after the timeliness.
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Assignee: Hunan Maidike Novel Materials Co., Ltd. Assignor: Central South University Contract record no.: 2011430000075 Denomination of invention: Process for preparing biomedical beta-titanium alloy License type: Exclusive License Open date: 20100609 Record date: 20110601 |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110720 Termination date: 20151210 |
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| EXPY | Termination of patent right or utility model |