CN106801163B - A kind of Ti-39Nb-6Zr bio-medical porous titaniums alloy and preparation method thereof - Google Patents
A kind of Ti-39Nb-6Zr bio-medical porous titaniums alloy and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Ti 39Nb 6Zr bio-medical porous titanium alloys and preparation method thereof, belong to bio-medical material and field of porous materials.The alloy is by niobium, zirconium and titanium composition, and wherein niobium 39w%, zirconium 6w%, surplus is titanium；The porosity of titanium alloy is 19.4% 42.1%.Ti 39Nb 6Zr alloy cast ingots are prepared using vacuum consumable smelting method, spherical powder particle is obtained using rotating electrode atomized method；The alloy powder of 100 150 mesh is selected, binder or ammonium hydrogen carbonate pore creating material and binder is added, is sufficiently mixed, is pressed into green compact；Green compact sintering is carried out in logical argon pipe type sintering furnace, thoroughly removes binder or pore creating material and binder, obtains porous alloy.The alloy elastic modulus is 3.6GPa~12.4GPa, and tensile strength is 123.8MPa~347.5MPa, has the advantages that elasticity modulus is low and good biocompatibility.
Description
Technical field
The present invention relates to a kind of Ti-Nb-Zr low elastic modulus porous titanium alloys and preparation method thereof, and in particular to a kind of
Ti-39Nb-6Zr bio-medical porous titanium alloys and preparation method thereof, belong to bio-medical material and field of porous materials.
Background technology
Titanium or titanium alloy because having the characteristics that good biocompatibility, high intensity, corrosion resistance, low elastic modulus,
Biologic medical field has obtained more and more applications, such as joint prosthesis, heart valve prosthesis, dental implant.Titanium and titanium close
The elasticity modulus of gold is all more much higher than body bone tissue, once and implantation material is mismatched with bone tissue elasticity modulus, implantation
Object will bear most biotic stress so that bone tissue is difficult to obtain the stimulation of biotic stress, is chronically at
Bone tissue under this environment gradually atrophy and degeneration, the loosening for ultimately causing implant will fail, cannot meet long-term
Requirement causes " stress shielding " phenomenon.According to the difference of the type of bone and measurement direction, the elasticity modulus of human body bone exists
Change between 4~30GPa, and the elasticity modulus of general fine and close titanium alloy is substantially in 50GPa or more.In order to avoid " stress shielding "
The generation of phenomenon, may be used porous structure.
Invention content
The purpose of the present invention is to provide a kind of Ti-39Nb-6Zr bio-medical porous titaniums alloys and preparation method thereof.This
Invention prepares Ti-39Nb-6Zr porous titanium alloys using powder metallurgic method makes the elasticity of material by Different Preparation parameter
Modulus and intensity reach a good matching degree with human body difference sclerotin.
A kind of Ti-39Nb-6Zr bio-medical porous titaniums alloy, by niobium, zirconium and titanium composition, weight percentage difference
For niobium 39%, zirconium 6%, surplus is titanium；The porosity of the titanium alloy be 19.4%-42.1%, elasticity modulus be 3.6GPa~
12.4GPa。
A kind of preparation method of Ti-39Nb-6Zr bio-medical porous titaniums alloy, using Ti-39Nb-6Zr titanium alloys as former material
Material, prepares porous titanium alloy, includes the following steps：
(1) it uses vacuum consumable smelting method to prepare Ti-39Nb-6Zr alloy cast ingots, is obtained using rotating electrode atomized method
Spherical powder particle；
(2) alloy powder for selecting 100-150 mesh adds binder or ammonium hydrogen carbonate pore creating material and binder, fully mixed
It closes, is pressed into green compact；
(3) green compact sintering process is carried out in logical argon pipe type sintering furnace, thoroughly removes binder or pore creating material and bonding
Agent obtains porous Ti-39Nb-6Zr alloys.
In step (1), using TiNb intermediate alloys, pure Ti, pure Zr as raw material, pass through 3 meltings of vacuum consumable electrode arc furnace
Obtain Ti-39Nb-6Zr alloy cast ingots；Consutrode is made in Ti-39Nb-6Zr alloy cast ingots, using rotating electrode atomized method,
Granularity is atomized into the spherical powder particle of 90~325 mesh, 100~150 mesh powders are filtered out using standard screen.
In step (2), the binder is polyethylene glycol, and the mass fraction of addition polyethylene glycol binder is 0.8%；
The mass fraction of the ammonium hydrogen carbonate pore creating material added is 0% or 5%~15%.
Compression moulding process carries out on super high pressure hydraulic electric tube expander, and the pressing pressure of green compact is 120MPa~160MPa, pressure
Molding jig is process by Cr12 mould steel.
In step (3), sintering process is completed in pipe type sintering furnace, and atmosphere protection is argon gas；Sintering temperature is 1000 DEG C
~1200 DEG C, sintering time 4h.
It is heated up using sublevel segmentation when sintering：120 DEG C are first warming up to, 20-30min is kept the temperature, thoroughly removes ammonium hydrogen carbonate and make
Hole agent (for being not added with the sample of pore creating material, this step can omit)；250 DEG C are continuously heating to, 20-30min is kept the temperature, removal is viscous
Tie agent polyethylene glycol；It is continuously heating to 1000~1200 DEG C of sintering temperature, sintering time 4h.Heating rate is controlled 1~10
℃/min。
The assay method of porous Ti-39Nb-6Zr alloys porosity and density that the present invention is prepared is impregnated using paraffin
Method.Usable material chamber temperature and pressure contracting Mechanics Performance Testing is according to national standard GB/T7314-2005《Metal material room temperature compression test method》,
Sample is processed into the cylinder that size is 6 × 9mm of Ф, compression speed 0.2mm/min.
It is an advantage of the invention that：Based on bio-medical Ti-39Nb-6Zr alloys, prepared using powder metallurgic method porous
Titanium alloy, preparation method is simple, by change pressing pressure, sintering temperature and Content of Pore-forming Agents come adjust material porosity with
Mechanical property realizes material and the better matching relationship of human body bone.
Specific implementation mode
The present invention prepares porous titanium alloy using Ti-39Nb-6Zr titanium alloys as raw material.Particular technique route is as follows：
1) using TiNb intermediate alloys, pure Ti, pure Zr as raw material, Ф is obtained by 3 meltings of vacuum consumable electrode arc furnace
The Ti-39Nb-6Zr alloy cast ingots of 210mm.
2) consutrode is made in Ti-39Nb-6Zr alloy cast ingots, using rotating electrode atomized method, is atomized into granularity
In the spherical powder particle of 90~325 mesh, 100~150 mesh powders are filtered out as experiment raw material using standard screen.
3) alloy powder, ammonium hydrogen carbonate pore creating material and polyethylene glycol (0.8wt.%) of suitable Ti-39Nb-6Zr are weighed
Binder be placed in grinding crucible in be fully ground it is uniformly mixed.
4) compression moulding process carries out on super high pressure hydraulic electric tube expander, and pressure parameter selects 120MPa~160MPa；Using
Compacting tool set be process by Cr12 mould steel, dies cavity sectional dimension be 55mm × 10mm, sectional area 550mm2。
5) sintering process is completed in pipe type sintering furnace, and atmosphere protection is argon gas；Keep heating rate control 5 DEG C/
Min, temperature rise to 120 DEG C, keep the temperature 30min, thoroughly remove ammonium hydrogen carbonate pore creating material (for being not added with the sample of pore creating material, this
Step can omit)；Continue to heat up, temperature rises to 250 DEG C, keeps the temperature 20min, removes binder polyethylene glycol；Continue to heat up, heat up
Speed control is in 1~10 DEG C/min, until reaching 1000~1200 DEG C required of sintering temperature, sintering time 4h.
Below by specific embodiment, the present invention will be further described：
First, alloy powder is prepared；
Alloy powder preparation method：Using TiNb intermediate alloys, pure Ti, pure Zr as raw material dispensing, alloying component Ti-
39Nb-6Zr.Ф 210mm ingot castings are obtained 3 times using vacuum consumable electrode arc furnace melting, rotation electrode is utilized after consutrode is made
Atomization is atomized into granularity in the spherical powder particle of 90~325 mesh, is sieved to obtain the powder of 100~150 mesh using standard screen
End.
Then, using the alloy powder of preparation, Ti-39Nb-6Zr biologies doctor is prepared according to the specific steps of embodiment 1-7
Use porous titanium alloy.
Embodiment 1
(1) 25g alloy powders are weighed, the polyethylene glycol binder of 0.8wt.% is added, is fully ground mixing；Utilize superelevation
Hydraulic casing roller carries out pressing process to alloyed powder, and green compact is made in pressing pressure 120MPa；
(2) green compact sintering process carries out in logical argon pipe type sintering furnace, and initial heating rate control works as temperature in 5 DEG C/min
Degree is warming up to 250 DEG C, keeps the temperature 20min, thoroughly removes binder；Continue to heat up, heating rate is controlled in 1~10 DEG C/min, directly
To reaching 1100 DEG C, sintering time 4h；
(3) after the completion of being sintered, sample is processed into the cylinder (state of 6 × 9mm of quadrat sampling and Ф of 9mm × 9mm × 10mm
Mark GB/T7314-2005) respectively carry out porosity and density measurement and room temperature compression test.
The pore character and mechanical property of material：Density 4.16g/cm3, porosity 23.6%, compression strength 217.4MPa,
Elasticity modulus 6.5GPa.
Embodiment 2
(1) 25g alloy powders are weighed, the polyethylene glycol binder of 0.8wt.% is added, is fully ground mixing；Utilize superelevation
Hydraulic casing roller carries out pressing process to alloyed powder, and green compact is made in pressing pressure 160MPa；
(2) green compact sintering process carries out in logical argon pipe type sintering furnace, and initial heating rate control works as temperature in 5 DEG C/min
Degree is warming up to 250 DEG C, keeps the temperature 20min, thoroughly removes binder；Continue to heat up, heating rate is controlled in 1~10 DEG C/min, directly
To reaching 1100 DEG C, sintering time 4h；
(3) after the completion of being sintered, sample is processed into the cylinder (state of 6 × 9mm of quadrat sampling and Ф of 9mm × 9mm × 10mm
Mark GB/T7314-2005) respectively carry out porosity and density measurement and room temperature compression test.
The pore character and mechanical property of material：Density 4.35g/cm3, porosity 19.4%, compression strength 226.3MPa,
Elasticity modulus 11.1GPa.
Embodiment 3
(1) 25g alloy powders are weighed, the polyethylene glycol binder of 0.8wt.% is added, is fully ground mixing；Utilize superelevation
Hydraulic casing roller carries out pressing process to alloyed powder, and green compact is made in pressing pressure 140MPa；
(2) green compact sintering process carries out in logical argon pipe type sintering furnace, and initial heating rate control works as temperature in 5 DEG C/min
Degree is warming up to 250 DEG C, keeps the temperature 20min, thoroughly removes binder；Continue to heat up, heating rate is controlled in 1~10 DEG C/min, directly
To reaching 1000 DEG C, sintering time 4h；
(3) after the completion of being sintered, sample is processed into the cylinder (state of 6 × 9mm of quadrat sampling and Ф of 9mm × 9mm × 10mm
Mark GB/T7314-2005) respectively carry out porosity and density measurement and room temperature compression test.
The pore character and mechanical property of material：Density 4.18g/cm3, porosity 23.2%, compression strength 210.4MPa,
Elasticity modulus 4.7GPa.
Embodiment 4
(1) 25g alloy powders are weighed, the polyethylene glycol binder of 0.8wt.% is added, is fully ground mixing；Utilize superelevation
Hydraulic casing roller carries out pressing process to alloyed powder, and green compact is made in pressing pressure 140MPa；
(2) green compact sintering process carries out in logical argon pipe type sintering furnace, and initial heating rate control works as temperature in 5 DEG C/min
Degree is warming up to 250 DEG C, keeps the temperature 20min, thoroughly removes binder；Continue to heat up, heating rate is controlled in 1~10 DEG C/min, directly
To reaching 1200 DEG C, sintering time 4h；
(3) after the completion of being sintered, sample is processed into the cylinder (state of 6 × 9mm of quadrat sampling and φ of 9mm × 9mm × 10mm
Mark GB/T7314-2005) respectively carry out porosity and density measurement and room temperature compression test.
The pore character and mechanical property of material：Density 4.32g/cm3, porosity 20.6%, compression strength 292.4MPa,
Elasticity modulus 12.4GPa.
Embodiment 5
(1) 25g alloy powders are weighed, the polyethylene glycol binder of 0.8wt.% is added, is fully ground mixing；Utilize superelevation
Hydraulic casing roller carries out pressing process to alloyed powder, and green compact is made in pressing pressure 140MPa；
(2) green compact sintering process carries out in logical argon pipe type sintering furnace, and initial heating rate control works as temperature in 5 DEG C/min
Degree is warming up to 250 DEG C, keeps the temperature 20min, thoroughly removes binder；Continue to heat up, heating rate is controlled in 1~10 DEG C/min, directly
To reaching 1100 DEG C, sintering time 4h；
(3) after the completion of being sintered, sample is processed into the cylinder point of 6 × 9mm of quadrat sampling and Ф of 9mm × 9mm × 10mm
Not carry out porosity and density measurement and room temperature compression test.
The pore character and mechanical property of material：Density 4.31g/cm3, porosity 20.8%, compression strength 235.3MPa,
Elasticity modulus 8.2GPa.
Embodiment 6
(1) 25g alloy powders are weighed, the ammonium hydrogen carbonate pore creating material that addition mass fraction is 5% is sufficiently mixed, and continue
Add the polyethylene glycol binder of 0.8wt.%；Pressing process, pressing pressure are carried out to alloyed powder using super high pressure hydraulic electric tube expander
For 140MPa, green compact is made；
(2) green compact sintering process carries out in logical argon pipe type sintering furnace, and initial heating rate control is in 5 DEG C/min, temperature
120 DEG C are risen to, 30min is kept the temperature, thoroughly removes ammonium hydrogen carbonate pore creating material；Continue to heat up, when temperature is warming up to 250 DEG C, heat preservation
20min thoroughly removes binder；Continue to heat up later, heating rate control is in 1~10 DEG C/min, until reaching 1200 DEG C, burns
The knot time is 4h；
(3) after the completion of being sintered, sample is processed into the cylinder point of 6 × 9mm of quadrat sampling and Ф of 9mm × 9mm × 10mm
Not carry out porosity and density measurement and room temperature compression test.
The pore character and mechanical property of material：Density 3.84g/cm3, porosity 29.5%, compression strength 347.5MPa,
Elasticity modulus 7.9GPa.
Embodiment 7
(1) 25g alloy powders are weighed, the ammonium hydrogen carbonate pore creating material that addition mass fraction is 15% is sufficiently mixed, and continue
Add the polyethylene glycol binder of 0.8wt.%；Pressing process, pressing pressure are carried out to alloyed powder using super high pressure hydraulic electric tube expander
For 140MPa, green compact is made；
(2) green compact sintering process carries out in logical argon pipe type sintering furnace, and initial heating rate control is in 5 DEG C/min, temperature
120 DEG C are risen to, 30min is kept the temperature, thoroughly removes ammonium hydrogen carbonate pore creating material；Continue to heat up, when temperature is warming up to 250 DEG C, heat preservation
20min thoroughly removes binder；Continue to heat up later, heating rate control is in 1~10 DEG C/min, until reaching 1200 DEG C, burns
The knot time is 4h；
(3) after the completion of being sintered, sample is processed into the cylinder point of 6 × 9mm of quadrat sampling and Ф of 9mm × 9mm × 10mm
Not carry out porosity and density measurement and room temperature compression test.
The pore character and mechanical property of material：Density 3.15g/cm3, porosity 42.1%, compression strength 123.8MPa,
Elasticity modulus 3.6GPa.
By above example, it can be seen that, the Ti-39Nb-6Zr bio-medical porous titaniums obtained by the method for the invention close
The elasticity modulus of gold is 3.6GPa~12.4GPa, and tensile strength is 123.8MPa~347.5MPa, density 3.15-4.35g/
cm3, porosity 19.4%-42.1% has the advantages that elasticity modulus is low and good biocompatibility.
Claims (7)
1. a kind of preparation method of Ti-39Nb-6Zr bio-medical porous titaniums alloy, includes the following steps：
(1) it uses vacuum consumable smelting method to prepare Ti-39Nb-6Zr alloy cast ingots, is obtained using rotating electrode atomized method spherical
Powder particle；Using TiNb intermediate alloys, pure Ti, pure Zr as raw material, Ti- is obtained by 3 meltings of vacuum consumable electrode arc furnace
39Nb-6Zr alloy cast ingots；Consutrode is made in Ti-39Nb-6Zr alloy cast ingots, using rotating electrode atomized method, by its mist
Granularity is melted into the spherical powder particle of 90~325 mesh, 100~150 mesh powders are filtered out using standard screen；
(2) alloy powder for selecting 100-150 mesh, adds binder or ammonium hydrogen carbonate pore creating material and binder, the bonding
Agent is polyethylene glycol, is sufficiently mixed, and green compact is pressed into；
(3) green compact sintering is carried out in logical argon pipe type sintering furnace, sintering temperature is 1000 DEG C~1200 DEG C, sintering time 4h,
Binder or pore creating material and binder are thoroughly removed, obtains porous Ti-39Nb-6Zr alloys, the alloy is by niobium, zirconium and titanium group
At weight percentage is respectively niobium 39%, and zirconium 6%, surplus is titanium, and the porosity of the titanium alloy is 19.4%-
42.1%.
2. the preparation method of Ti-39Nb-6Zr bio-medical porous titaniums alloy according to claim 1, it is characterised in that：
The mass fraction for adding polyethylene glycol binder is 0.8%；The mass fraction for adding ammonium hydrogen carbonate pore creating material is 5%~15%.
3. the preparation method of Ti-39Nb-6Zr bio-medical porous titaniums alloy according to claim 1, it is characterised in that：
Green compact is pressed on super high pressure hydraulic electric tube expander, compacting tool set is process by Cr12 mould steel.
4. the preparation method of Ti-39Nb-6Zr bio-medical porous titaniums alloy according to claim 3, it is characterised in that：
The pressing pressure of green compact is 120MPa~160MPa.
5. the preparation method of Ti-39Nb-6Zr bio-medical porous titaniums alloy according to claim 1, it is characterised in that：
It is heated up using sublevel segmentation when sintering, is first warming up to 250 DEG C, keep the temperature 20-30min, remove binder polyethylene glycol；Continue to heat up
To sintering temperature.
6. the preparation method of Ti-39Nb-6Zr bio-medical porous titaniums alloy according to claim 1, it is characterised in that：
It is heated up using sublevel segmentation when sintering：120 DEG C are first warming up to, 20-30min is kept the temperature, removes ammonium hydrogen carbonate pore creating material；Continue to heat up
To 250 DEG C, 20-30min is kept the temperature, removes binder polyethylene glycol；It is continuously heating to sintering temperature.
7. the preparation method of Ti-39Nb-6Zr bio-medical porous titaniums alloy according to claim 5 or 6, feature exist
In：Heating rate is 1~10 DEG C/min.
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| RU2765044C1 (en) * | 2021-03-29 | 2022-01-25 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method for obtaining porous and permeable ring-shaped blanks from a superelastic titanium-zirconium-niobium system alloy |
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| CN107824790A (en) * | 2017-10-25 | 2018-03-23 | 成都先进金属材料产业技术研究院有限公司 | A kind of preparation method of porous vanadium chromium titanium material |
| CN109847110A (en) * | 2018-12-19 | 2019-06-07 | 云南大学 | A kind of porous Ti-Nb-Zr composite artificial bone implant material and its preparation method and application |
| RU2687352C1 (en) * | 2018-12-25 | 2019-05-13 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method of producing permeable foam material from super elastic alloys of titanium-zirconium-niobium system |
| CN111441007B (en) * | 2020-04-29 | 2023-09-01 | 安徽江南泵阀集团有限公司 | Treatment process for improving damage of fluid medium to mortar pump impeller |
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| RU2765044C1 (en) * | 2021-03-29 | 2022-01-25 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method for obtaining porous and permeable ring-shaped blanks from a superelastic titanium-zirconium-niobium system alloy |
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