CN104611611B - A kind of preparation method of ultralow elasticity modulus high strength titanium alloy material - Google Patents
A kind of preparation method of ultralow elasticity modulus high strength titanium alloy material Download PDFInfo
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Abstract
Invention provides the preparation method of a kind of ultralow elasticity modulus high strength titanium alloy material, belongs to technical field of biological medical material preparation.With Ti, Mo, Fe element powders as primary raw material, it is that 6 ~ 38wt.% carries out composition proportion according to molybdenum equivalent, mixed-powder is carried out high-energy ball milling, obtain nanocrystalline titanio composite powder by adjusting milling parameters.In ball-milled powder is loaded graphite jig and carry out discharge plasma sintering, sintering temperature is 800 ~ 1000 DEG C, and after insulation, furnace cooling i.e. can get titanium alloy block materials.The advantage of the method is: the simple manufacturing cycle of technique is short, and prepared alloy is mainly by β Ti and FCC Ti two phase composition, and has the organizational structure feature of Ultra-fine Grained.The new titanium alloy tool ultralow elasticity modulus of preparation and high intensity, the feature of high-ductility, its elastic modelling quantity index is mated with natural bone, has the biomechanics adaptability of excellence.
Description
Technical field
The invention provides a kind of ultralow elasticity modulus, the preparation method of high strength titanium alloy material, belong to technical field of biological medical material preparation.
Technical background
Titanium alloy has good biocompatibility, high specific strength, low elastic modulus, the advantage such as corrosion-resistant, it has also become the development priority in biomedical materials field.The titanium alloy of clinical practice at present is mainly Ti-6Al-4V and improves alloy, but this type of alloy elastic modulus is about 80 ~ 110Gpa, and relatively tissue elastic modelling quantity (10 ~ 30GPa) is the biggest, is difficult to mate with human bone.Additionally, human body also can be caused potential hazard by the precipitation being chronically implanted internal Al or V ion.On this basis, new type beta type titanium alloy nontoxic, that elastic modelling quantity is lower is researched and developed in design becomes the Main Trends of The Development that medical titanium alloy material is current.
Report both at home and abroad about ultralow elasticity modulus, high intensity beta-titanium alloy is less at present.Wherein the design such as Yurie is prepared for β type Ti29Nb13Ta4.6Zr alloy, its elastic modelling quantity is 60-67Gpa(Mechanical Strength and
Bone Contactability of Biomedical Titanium Alloy with
Low Young's Modulus Subjected to Fine Particle Bombarding Process. The Japan
Institute of Metals and Materials, 2014,78:163-169)；Li etc. use powder metallurgy process to be prepared for Ultra-fine Grained (Ti69.7Nb23.7Zr4.9Ta1.7)94
Fe6Alloy, research show alloy by β-Ti phase and FeTi phase composition, the elastic modelling quantity of gained is 52-54Gpa(Ultrafine-grained Ti-based
composites with high strength and low modulus. Materials Science &
Engineering A, 2013,560:857-861)；Chrominski etc. are prepared for β type Ti-45Nb alloy, and its elastic modelling quantity is 57-68Gpa (Enhancement of mechanical
properties of biocompatible Ti–45Nb alloy by hydrostatic extrusion. Journal of Materials Science,
2014,49:6930-6936).There is bigger gap in the novel beta-titanium alloy elastic modelling quantity the most relatively tissue (10 ~ 30GPa) reported at present, therefore develops titanium alloy that is nontoxic and that have ultralow elasticity modulus and high intensity and have important application prospect in biomedical materials field.
This patent proposes to be greatly lowered the elastic modelling quantity of titanium alloy by preparing β+FCC-Ti biphase titanium alloy, and can improve its moulding index on the basis of keeping titanium alloy high intensity.At present, yet there are no correlational study report both at home and abroad.
Summary of the invention
In order to solve the problems referred to above, it is an object of the invention to provide the preparation method of a kind of ultralow elasticity modulus high strength titanium alloy material, can be widely applied to biomedical materials field.
The technical scheme is thatThe preparation method of a kind of ultralow elasticity modulus high strength titanium alloy material, specifically comprises the following steps that
Step 1: proportioning raw material: with Ti powder, Mo powder and Fe powder as primary raw material, being calculated as according to mass percent of various compositions: Mo content 5 ~ 12%, the content of Fe is 0 ~ 9%, composition meets Mo equivalent weight range simultaneously is that 6 ~ 38wt%, Mo equivalent computing formula is: [Mo] equivalent=%Mo+%Fe/0.35+%Cr/0.63+%Mn/0.65+%Ni/0.8+%V/
1.5+%W/2+%Nb/3.6+%Ta/4.5, surplus be Ti and and other trace alloying elements, standby；
Step 2: mixed-powder step 1 obtained carries out high-energy ball milling; mechanical milling process is carried out under inert gas shielding, and ratio of grinding media to material is 5:1 ~ 20:1, rotating speed 600 ~ 1500r/min; Ball-milling Time is 2 ~ 30h, obtains composition and is uniformly distributed and the composite powder of crystallite dimension≤150nm；
Step 3: ball-milled powder step 2 obtained loads in graphite jig, then inserts in discharge plasma sintering stove, applies the axial compressive force of 10 ~ 80MPa, uses vacuum 10-2～be sintered under the vacuum condition of 6Pa or inert gas shielding; it is that 50～300 DEG C/min heats up with speed; being warming up to 800～1000 DEG C, cool to room temperature after insulation with the furnace, i.e. available is 97.0 more than % by its consistency of titanium alloy block materials of β+FCC-Ti two phase composition.
Present invention have an advantage that
(1) novel β+FCC-Ti biphase titanium alloy material tool ultralow elasticity modulus and high intensity, the feature of high-ductility prepared by, its elastic modelling quantity index is mated with natural bone, there is the biomechanics adaptability of excellence, its consistency is more than 97.0%, its elastic modelling quantity is 15 ~ 32GPa, compressive strength is 2000 ~ 2800Mpa(2) prepared by titanium alloy there is ultrafine-grained's structure so that it is there is higher osteoblast adhesion, show as the most excellent biocompatibility.
(3) process is simple, manufacturing cycle is short, can realize numerical control operating, and preparation technology is repeatable strong.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of Ti-8Mo-3Fe alloy microscopic structure prepared by the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is described further.
Embodiment
1
With Ti, Mo and Fe element powders as raw material, granularity is-500 mesh, is 16.6wt.% according to nominal composition Ti-8Mo-3Fe(molybdenum equivalent) carry out proportioning.Mixed-powder is carried out vibration type high-energy ball milling, and mechanical milling process is carried out under high-purity argon gas is protected, ratio of grinding media to material 10:1, rotating speed 1000r/min.The composite powder that average grain size is about 15nm is collected after ball milling 10h.Ball-milled powder is put in the stone grinder mould of Φ 20, subsequently stone grinder mould is put into discharge plasma sintering stove, system is evacuated to 2Pa, additional axial compressive force is 40MPa, it is warming up to 900 DEG C with the speed of 100 DEG C/min, furnace cooling after insulation 5min, i.e. obtains Ti-8Mo-3Fe alloy block material.After testing, preparing alloy sample by β+FCC-Ti two phase composition, its consistency is 98.95%, alloy.The mechanical property of sample is: elastic modelling quantity is 23.69GPa, and comprcssive strength is 2465MPa, and compression failure strain is 34.7%.Prepare the high-resolution field emission scanning electron microscope photo of sample as shown in Figure 1.
Embodiment
2
With Ti, Mo element powders as raw material, granularity is-325 mesh, is 6 wt.% according to nominal composition Ti-6Mo(molybdenum equivalent) carry out proportioning.Mixed-powder is carried out vibration type high-energy ball milling, and mechanical milling process is carried out under high-purity argon gas is protected, ratio of grinding media to material 10:1, rotating speed 1200r/min.The composite powder that average grain size is about 32nm is collected after ball milling 8h.Being put into by ball-milled powder in the stone grinder mould of Φ 20, subsequently stone grinder mould is put into discharge plasma sintering stove, system is evacuated to 2Pa, additional axial compressive force is 40MPa, it is warming up to 1000 DEG C with the speed of 100 DEG C/min, furnace cooling after insulation 5min, i.e. obtain Ti-6Mo alloy block material.After testing, the consistency preparing sample is 98.49%.The mechanical property of sample is: elastic modelling quantity is 19.44GPa, and comprcssive strength is 2248MPa, and compression failure strain is 31.3%.
Embodiment
3
With Ti, Mo and Fe element powders as raw material, granularity is-500 mesh, is 33.7 wt.% according to nominal composition Ti-8Mo-9Fe(molybdenum equivalent) carry out proportioning.Mixed-powder is carried out vibration type high-energy ball milling, and mechanical milling process is carried out under high-purity argon gas is protected, ratio of grinding media to material 15:1, rotating speed 800r/min.The composite powder that average grain size is about 9nm is collected after ball milling 12h.Ball-milled powder is put in the stone grinder mould of Φ 20, subsequently stone grinder mould is put into discharge plasma sintering stove, system is evacuated to 2Pa, additional axial compressive force is 40MPa, it is warming up to 850 DEG C with the speed of 100 DEG C/min, furnace cooling after insulation 5min, i.e. obtains Ti-8Mo-9Fe alloy block material.After testing, preparing alloy sample by β+FCC-Ti and a small amount of TiFe phase composition, its consistency is 98.37%, and the mechanical property of alloy sample is: elastic modelling quantity is 30.71GPa, and comprcssive strength is 2591MPa, and compression failure strain is 17.9%.
Embodiment 4:
With Ti, Mo and Fe element powders as raw material, granularity is-500 mesh, is 29.2wt.% according to nominal composition Ti-9Mo-6Fe-2Cr(molybdenum equivalent) carry out proportioning.Mixed-powder is carried out vibration type high-energy ball milling, and mechanical milling process is carried out under high-purity argon gas is protected, ratio of grinding media to material 20:1, rotating speed 600r/min.The composite powder that average grain size is about 32nm is collected after ball milling 25h.Ball-milled powder is put in the stone grinder mould of Φ 20, subsequently stone grinder mould is put into discharge plasma sintering stove, system is evacuated to 6Pa, additional axial compressive force is 80MPa, it is warming up to 850 DEG C with the speed of 300 DEG C/min, furnace cooling after insulation 5min, i.e. obtains Ti-9Mo-6Fe-2Cr alloy block material.After testing, preparing alloy sample and be made up of β+FCC-Ti, its consistency is 97.7%, and the mechanical property of alloy sample is: elastic modelling quantity is 29.6GPa, and comprcssive strength is 2223MPa, and compression failure strain is 27.9%.
Embodiment 5:
With Ti, Mo and Fe element powders as raw material, granularity is-500 mesh, is 25wt.% according to nominal composition Ti-5Mo-7Fe(molybdenum equivalent) carry out proportioning.Mixed-powder is carried out vibration type high-energy ball milling, and mechanical milling process is carried out under high-purity argon gas is protected, ratio of grinding media to material 15:1, rotating speed 700r/min.The composite powder that average grain size is about 95nm is collected after ball milling 5h.Ball-milled powder is put in the stone grinder mould of Φ 20, subsequently stone grinder mould is put into discharge plasma sintering stove, system is evacuated to 5Pa, additional axial compressive force is 60MPa, it is warming up to 900 DEG C with the speed of 250 DEG C/min, furnace cooling after insulation 5min, i.e. obtains Ti-5Mo-7Fe alloy block material.After testing, preparing alloy sample by β+FCC-Ti and a small amount of TiFe phase composition, its consistency is 97.9%, and the mechanical property of alloy sample is: elastic modelling quantity is 30.9GPa, and comprcssive strength is 2346MPa, and compression failure strain is 18.7%.
Claims (1)
1. the preparation method of a ultralow elasticity modulus high strength titanium alloy material, it is characterised in that specifically comprising the following steps that of the method
Step 1: proportioning raw material: with Ti powder, Mo powder and Fe powder as primary raw material, various compositions are calculated as according to mass percent: Mo content 5-12%, the content of Fe is 0-9%, composition meets Mo equivalent weight range simultaneously is that 6-38wt%, Mo equivalent computing formula is: [Mo] equivalent=%Mo+%Fe/0.35+%Cr/0.63+%Mn/0.65+%Ni/0.8+%V/1.5+%W/2+%Nb/3 .6+%Ta/
4.5, surplus be Ti and and other trace alloying elements, standby；
Step 2: mixed-powder step 1 obtained carries out high-energy ball milling; mechanical milling process is carried out under inert gas shielding, and ratio of grinding media to material is 5:1 ~ 20:1, rotating speed 600 ~ 1500r/min; Ball-milling Time is 2 ~ 30h, obtains composition and is uniformly distributed and the composite powder of crystallite dimension≤150nm；
Step 3: ball-milled powder step 2 obtained loads in graphite jig, then inserts in discharge plasma sintering stove, applies the axial compressive force of 10 ~ 80MPa, uses vacuum 10-2It is sintered under the vacuum condition of ~ 6Pa or inert gas shielding; it is that 50 ~ 300 DEG C/min heats up with speed; it is warming up to 800 ~ 1000 DEG C; room temperature is cooled to the furnace after insulation; i.e. obtaining titanium alloy block materials, i.e. available main by the titanium alloy block materials of β+FCC-Ti two phase composition, its consistency is more than 97.0%; its elastic modelling quantity is 15 ~ 32GPa, and compressive strength is 2000 ~ 2800MPa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4857269A (en) * | 1988-09-09 | 1989-08-15 | Pfizer Hospital Products Group Inc. | High strength, low modulus, ductile, biopcompatible titanium alloy |
| CN102312129A (en) * | 2011-09-30 | 2012-01-11 | 昆明理工大学 | Method for preparing titanium niobium zirconium tin biomedical titanium alloys by discharge plasma sintering |
| CN103649350A (en) * | 2012-05-30 | 2014-03-19 | 韩国机械研究院 | Beta titanium alloy with low elasticity and high strength |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20040241037A1 (en) * | 2002-06-27 | 2004-12-02 | Wu Ming H. | Beta titanium compositions and methods of manufacture thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4857269A (en) * | 1988-09-09 | 1989-08-15 | Pfizer Hospital Products Group Inc. | High strength, low modulus, ductile, biopcompatible titanium alloy |
| CN102312129A (en) * | 2011-09-30 | 2012-01-11 | 昆明理工大学 | Method for preparing titanium niobium zirconium tin biomedical titanium alloys by discharge plasma sintering |
| CN103649350A (en) * | 2012-05-30 | 2014-03-19 | 韩国机械研究院 | Beta titanium alloy with low elasticity and high strength |
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