CN109182811A - A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Ag alloying - Google Patents
A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Ag alloying Download PDFInfo
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- CN109182811A CN109182811A CN201810982818.6A CN201810982818A CN109182811A CN 109182811 A CN109182811 A CN 109182811A CN 201810982818 A CN201810982818 A CN 201810982818A CN 109182811 A CN109182811 A CN 109182811A
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- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
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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
Abstract
A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn-5Ag alloy of Ag alloying, it is characterised in that: its raw material for preparing is Ti powder, Nb powder, Si powder, Zr powder and Ag powder；The following steps are included: firstly, it is prepared into mixed-powder preparation through high-energy ball milling using Ti, Nb, Zr, Sn, Ag powder as raw material.Then, mixed-powder is subjected to conventional molding processing.Finally, molding gained briquetting is carried out vacuum non-pressure sintering processing, acquisition hardness, elasticity modulus, coefficient of friction are lower, and corrosion resistance is higher, the better 5wt.%Ag/TNZS titanium base material of biocompatibility.Very good solution of the present invention TNZS alloy in terms of biologic medical using there are the problem of, effectively reduce hardness, the elasticity modulus, coefficient of friction of titanium base material；Improve the corrosion resistance of material；Biocompatibility more preferably, is conducive to application of the material in terms of biologic medical.And the advantages that preparation process is simple, economical excellent.
Description
Technical field
The present invention relates to field of metal preparation, especially a kind of preparation method of TNZS sill, specifically
A kind of lower hardness, elasticity modulus, lesser friction factor, stronger corrosion resistance, the titanium-based of preferable biocompatibility
The preparation method of material.
Background technique
TNZS alloy not only has the characteristics such as lower elasticity modulus, excellent corrosion resistance, and also has excellent
Processing forming and corresponding mechanical property, these advantages make it smoothly and become nowadays medical implant preferred material it
One.But bio-medical TNZS alloy, however it remains elasticity modulus is high, friction factor height, friction and wear behavior and bio-compatible
Many defects such as property is poor, seriously limit its extensive use on clinical medicine.
Ag is that matter is soft and rich malleable metal, has good ductility, biocompatibility, it is preferable it is wear-resistant,
The performance of corrosion resistance and sterilization.Addition Ag easily weakens its integral hardness in the alloy, while dropping low-alloyed elasticity modulus.
Therefore change the Elemental redistribution of TNZS material, organizational composition usually by adding Ag member so as to improve the overall performance of TNZS material
Value with higher and important meaning.
The present invention is made using the PM technique that high-energy ball milling twice is combined with routine molding, vacuum non-pressure sintering
Standby 5wt.%Ag/TNZS titanium base material, increases substantially the comprehensive performance of TNZS sill.As far as the applicant is aware, so far
The report of 5wt.%Ag/TNZS is prepared there has been no the addition Ag metallic element in TNZS titanium base material and using powder metallurgic method
Road.
Summary of the invention
For the purpose of the present invention for existing bio-medical TNZS alloy there are elasticity modulus height, friction factor is high, rubs
Polishing machine and the poor problem of biocompatibility are invented a kind of using " high-energy ball milling-compression molding-vacuum non-pressure sintering "
The method that the Ti-24Nb-4Zr-7.9Sn alloy of Ag alloying prepares titanium-base alloy.It prepares 5wt.% by addition Ag powder
Ag/TNZS.5wt.%Ag/TNZS obtained have lower hardness, elasticity modulus, friction factor, stronger corrosion resistance,
Preferable biocompatibility, and preparation method is easy to operate, easy realization, economical.
The technical scheme is that
A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn-5Ag alloy of Ag alloying, it is characterized in that it includes following
Step:
Step 1, prepared by high-energy ball milling mixed-powder: first preparing the 5wt.%Ag/TNZS mixed-powder (quality hundred of each component
Divide than being respectively Ti powder: 59.1%, Nb powder: 24%, Zr powder: 4%, Sn powder: 7.9%, Ag powder: 5%) through high-energy ball milling (planet
Ball mill, ball material mass ratio are 10:1, and 400r/min ball milling 72h, ball milling 50min shut down 10min) after, it is placed in vacuum oven
Interior 60 DEG C of heat preservation 4h drying, is sieved (300 mesh)；
Step 2, the method for conventional molding processing: mixed-powder prepared by step 1 is manufactured in Nantong forging equipment factory
(pressing pressure 18Mpa, pressure maintaining 3min) is pressed to get required briquetting with a thickness of the left side 4mm in YB32-100 hydraulic press
It is right；
Step 3, vacuum non-pressure sintering is handled: the briquetting of step 2 compression moulding being placed on WZS-20 type double-chamber vacuum and is burnt
Freezing of a furnace carries out pressureless sintering.Wherein vacuum degree 1 × 10-1Pa, 10 DEG C/min of heating rate.Sintering process is first pre-burning to 600 ±
10 DEG C of heat preservation 2h are warming up to 800 ± 10 DEG C of heat preservation 2h, then are warming up to 1000 ± 10 DEG C of heat preservation 2h, are finally warming up to 1250 ± 10
DEG C heat preservation 2h, subsequent furnace cooling.
The beneficial effects of the present invention are:
(1) PM technique that the present invention is combined by " high-energy ball milling-routine molding-vacuum non-pressure sintering ", is obtained
Distributed components TNZS metal alkyl materials, for titanium provide one kind can industrialized production preparation method.
(2) hardness of 5wt.%Ag/TNZS titanium base material prepared by the present invention is 505.4HV ratio TNZS (560.1HV) drop
Low 9.77%；Elasticity modulus is that 40.98Gpa ratio TNZS (45.21Gpa) reduces 9.36% closer to human body natural's tissue
Elasticity modulus；Coefficient of friction reduces 6.14% than TNZS (0.5035) for 0.4726；Corrosion current is 1.91 × 10-6A·cm-2Than TNZS (4.17 × 10-6A·cm-2) reduce 54.2%；Cell attachment greatly improves.
(3) present invention is applicable not only to the preparation of TNZS base titanium alloy, applies also for the preparation of various model titaniums.
(4) easy to operate, the easy realization of 5wt.%Ag/TNZS alloy provided by the invention and preparation method thereof, economy are excellent
It is good.
Detailed description of the invention
Fig. 1 is the XRD diffraction pattern of TNZS powder (a), 5wt.%Ag/TNZS powder (b) after ball milling in comparative example of the present invention；
Fig. 2 is TNZS titanium base material (a), 5wt.%Ag/TNZS titanium base material (b) after being sintered in comparative example of the present invention
XRD diffraction pattern；
Fig. 3 is TNZS titanium base material, 5wt.%Ag/TNZS titanium base material hardness figure after being sintered in comparative example of the present invention；
Fig. 4 is TNZS titanium base material, 5wt.%Ag/TNZS titanium base material elasticity modulus after being sintered in comparative example of the present invention
Figure；
Fig. 5 is TNZS titanium base material (a) after being sintered in comparative example of the present invention, 5wt.%Ag/TNZS titanium base material (b) friction
Coefficient figure；
Fig. 6 is TNZS titanium base material (a), 5wt.%Ag/TNZS titanium base material (b) cell after being sintered in comparative example of the present invention
Attach SEM figure.
Specific embodiment
Below in conjunction with drawings and the specific embodiments, the present invention will be further described.
Embodiment 1.
A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn-5Ag alloy (5wt.%Ag/TNZS) of Ag alloying, including
Following steps:
Step 1, prepared by high-energy ball milling mixed-powder: preparing 5wt.%Ag/TNZS mixed-powder (the quality percentage of each component
Than being respectively Ti powder: 59.1%, Nb powder: 24%, Zr powder: 4%, Sn powder: 7.9%, Ag powder: 5%) through high-energy ball milling (planet ball
Grinding machine, ball material mass ratio are 10:1, and 400r/min ball milling 72h, ball milling 50min shut down 10min) after, it is placed in vacuum oven
4h is kept the temperature under the conditions of 60 DEG C, is then cooled to room temperature taking-up to it, and crossing 300 meshes can be obtained required composite powder.
Step 2, the method for conventional molding processing: mixed-powder prepared by step 1 is manufactured in Nantong forging equipment factory
(pressing pressure 18Mpa, pressure maintaining 3min) is pressed to get required briquetting with a thickness of the left side 4mm in YB32-100 hydraulic press
It is right；
Step 3, vacuum non-pressure sintering is handled: the briquetting of step 2 compression moulding being placed on WZS-20 type double-chamber vacuum and is burnt
Freezing of a furnace carries out pressureless sintering.Wherein vacuum degree 1 × 10-1Pa, 10 DEG C/min of heating rate.Sintering process is first pre-burning to 600 ±
10 DEG C of heat preservation 2h are warming up to 800 ± 10 DEG C of heat preservation 2h, then are warming up to 1000 ± 10 DEG C of heat preservation 2h, are finally warming up to 1250 ± 10
DEG C heat preservation 2h, subsequent furnace cooling.
Obvious using 5wt.%Ag/TNZS mixed-powder mechanical alloying phenomenon made from above-mentioned steps, Fig. 1 (b) is this
The XRD diffracting spectrum of resulting 5wt.%Ag/TNZS powder after embodiment high-energy ball milling, through analyzing, containing α-Ti (Nb, Zr),
Metallic compound (Sn between β-Ti (Nb, Zr), Ti-Sn3Ti5、Sn5Ti6、Sn3Ti2) and simple substance Sn, and there is width in diffraction maximum
Change, illustrates that composite granule has occurred a degree of mechanical alloying and reached the effect of powder fining after high-energy ball milling
Fruit.Fig. 2 (b) is the XRD diffracting spectrum of the 5wt.%Ag/TNZS alloy obtained after vacuum non-pressure sintering, analyzes, contains in alloy
There are α-Ti (Nb, Zr), β-Ti (Nb, Zr), SnTi3, Sn3Ti5Furthermore phase also detects Ag4Sn phase in 5wt.%Ag/TNZS, but
And the titaniferous compound of Ag is not detected, illustrate under identical external condition, Ag and Sn can react prior to Ti.
Comparative example.
The preparation method of TNZS
This comparative example and embodiment 1 are similar, the difference is that not adding Ag powder, the mass percent of each component is respectively
Ti powder: 64.1%, Nb powder: 24%, Zr powder: 4%, Sn powder: 7.9%)
Fig. 1 (a) is the XRD diffracting spectrum for the TNZS powder that high energy is asked after mill, predominantly detects α-Ti (Nb, Zr), β-Ti
(Nb, Zr) and simple substance Sn these three titanium-silicon compounds；Fig. 2 (a) is the XRD diffraction pattern of TNZS alloy after vacuum non-pressure sintering
Spectrum, predominantly detects α-Ti (Nb, Zr), β-Ti (Nb, Zr), SnTi3, Sn3Ti5Phase.
Two embodiments and comparative example comparison are found, it is obtained after addition metal nano Ag powder progress alloying
The comprehensive performance of 5wt.%Ag/TNZS alloy is better than TNZS.Wherein, the hardness of 5wt.%Ag/TNZS alloy reduces 9.77%；
Elasticity modulus reduces 9.34% elasticity modulus organized closer to human body natural；Coefficient of friction reduces 6.14%；Corrosion electricity
Stream reduces 54.2%；Cell attachment greatly improves.
Part that the present invention does not relate to is the same as those in the prior art or can be realized by using the prior art.
Claims (5)
1. a kind of preparation method of the Ti-24Nb-4Zr-7.9Sn-5Ag alloy of Ag alloying, it is characterized in that it is by high-energy ball milling
Mixed-powder preparation, conventional molding processing and vacuum non-pressure sintering composition；The mixed-powder is 5wt.%Ag/TNZS mixing
Powder；
The high-energy ball milling mixed-powder preparation refers to Ti, Nb, Zr, Sn, Ag powder by setting ratio after high-energy ball milling
It is placed in drying in vacuum oven, sieving；
The conventional molding processing, which refers to, is placed in mixed-powder in mold by certain mass, compression moulding on a hydraulic press,
Obtain briquetting；
The vacuum non-pressure sintering, which refers to, is placed on compression molding gained briquetting in vacuum sintering furnace, carries out burning without pressure to it
Knot.
2. according to the method described in claim 1, it is characterized in that the matter of the 5wt.%Ag/TNZS mixed-powder each component
Measuring percentage is respectively Ti powder: 59.1%, Nb powder: 24%, Zr powder: 4%, Sn powder: 7.9%, Ag powder: 5%.
3. according to the method described in claim 1, it is characterized in that the high-energy ball milling 5wt.%Ag/TNZS mixed-powder is used
High-energy ball milling equipment be planetary ball mill, ball milling parameter: ball material mass ratio be 10:1,400r/min ball milling 72h, ball milling
50min shuts down 10min.
4. according to the method described in claim 1, it is characterized in that mixed-powder after the described conventional molding with a thickness of
4mm；Pressing pressure is 18Mpa, pressure maintaining 3min.
5. according to the method described in claim 1, it is characterized in that the pressureless sintering parameter are as follows: vacuum degree 1 × 10-1Pa,
10 DEG C/min of heating rate；It first burns to 600 ± 10 DEG C of heat preservation 2h, then is warming up to 800 ± 10 DEG C of heat preservation 2h, then it is warming up to 1000 ±
10 DEG C of heat preservation 2h are finally warming up to 1250 ± 10 DEG C of heat preservation 2h, subsequent furnace cooling.
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| CN201810982818.6A CN109182811A (en) | 2018-08-27 | 2018-08-27 | A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Ag alloying |
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| CN201810982818.6A CN109182811A (en) | 2018-08-27 | 2018-08-27 | A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Ag alloying |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111304477A (en) * | 2020-03-31 | 2020-06-19 | 西安稀有金属材料研究院有限公司 | Preparation method of low-modulus high-toughness silver-titanium-containing alloy |
| CN113337744A (en) * | 2021-05-31 | 2021-09-03 | 上海大学 | Preparation method of Ti2448 biomedical alloy with low Young modulus |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105274375A (en) * | 2015-10-29 | 2016-01-27 | 江苏大学 | Method for compounding and preparing high-elastic-modulus Ti-based material based on nano ceramic particles |
| CN105861966A (en) * | 2016-06-27 | 2016-08-17 | 山东建筑大学 | Silver-titanium carbide-titanium boride whisker-toughened high-strength titanium alloy antibacterial medical material |
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2018
- 2018-08-27 CN CN201810982818.6A patent/CN109182811A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105274375A (en) * | 2015-10-29 | 2016-01-27 | 江苏大学 | Method for compounding and preparing high-elastic-modulus Ti-based material based on nano ceramic particles |
| CN105861966A (en) * | 2016-06-27 | 2016-08-17 | 山东建筑大学 | Silver-titanium carbide-titanium boride whisker-toughened high-strength titanium alloy antibacterial medical material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111304477A (en) * | 2020-03-31 | 2020-06-19 | 西安稀有金属材料研究院有限公司 | Preparation method of low-modulus high-toughness silver-titanium-containing alloy |
| CN111304477B (en) * | 2020-03-31 | 2021-03-05 | 西安稀有金属材料研究院有限公司 | Preparation method of low-modulus high-toughness silver-titanium-containing alloy |
| CN113337744A (en) * | 2021-05-31 | 2021-09-03 | 上海大学 | Preparation method of Ti2448 biomedical alloy with low Young modulus |
| CN113337744B (en) * | 2021-05-31 | 2022-05-06 | 上海大学 | Preparation method of Ti2448 biomedical alloy with low Young modulus |
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Application publication date: 20190111 |