CN109468562A - Improve the method and beta titanium alloy of beta titanium alloy hardness and biocompatibility - Google Patents
Improve the method and beta titanium alloy of beta titanium alloy hardness and biocompatibility Download PDFInfo
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- CN109468562A CN109468562A CN201811524770.0A CN201811524770A CN109468562A CN 109468562 A CN109468562 A CN 109468562A CN 201811524770 A CN201811524770 A CN 201811524770A CN 109468562 A CN109468562 A CN 109468562A
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- 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
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- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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Abstract
The present invention discloses a kind of method for improving beta titanium alloy hardness and biocompatibility; it is related to Alloy Processing field; it is that casting Ti-Nb-Sn-Zr-Mo titanium alloy hardness is smaller; it can lead to the problem of abrasive dust because wearability is bad when being implanted into as joint replacement materials and propose; the following steps are included: (1) is placed on Ti-Nb-Sn-Zr-Mo titanium alloy template is cast in vacuum tube furnace, and logical inert gas shielding；(2) temperature of tube furnace is warming up to 730-850 DEG C, heat preservation；(3) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；(4) tube furnace, and logical argon gas protection are reopened, 400-480 DEG C is warming up to and keeps the temperature；(5) tube furnace is closed, and the taking-up of titanium alloy template is placed in cooling in air；The present invention also provides by the above method treated beta titanium alloy, the beneficial effects of the present invention are: heat treatment methods through the invention, and the hardness of β type Ti-Nb-Sn-Zr-Mo titanium alloy surface can be made to improve 81%, and can improve osteoblast stick and bone is to differentiation.
Description
Technical field
The present invention relates to Alloy Processing fields, and in particular to a kind of raising beta titanium alloy hardness and biocompatibility
Method.
Background technique
Current clinically most widely used pure titanium has biggish elasticity modulus due to comparing with natural bone, thus is implanted into
To bear bigger stress after human body, and bone due to for a long time cannot by power stimulation and be unfavorable for the formation and life of new bone
Long, this phenomenon is known as stress shielding effect.For the generation for avoiding stress shielding effect as far as possible, biomaterial researchers
It constantly develops novel beta titanium alloy in recent years to go to substitute clinically medical pure titanium, because beta titanium alloy is with smaller
Closer to the elasticity modulus of bone, thus it can preferably avoid the generation of stress shielding effect.Based on the studies above background, Yi Zhongxin
The beta titanium alloy Ti-Nb-Sn-Zr-Mo of type is developed, and the extensive concern by researchers.
However, being implanted into since casting Ti-Nb-Sn-Zr-Mo titanium alloy hardness is often smaller as joint replacement materials
When can be bad due to wearability and generate abrasive dust, inflammation in primosome causes implant failure to fall off.
Summary of the invention
The problem to be solved by the present invention is that casting Ti-Nb-Sn-Zr-Mo titanium alloy hardness is smaller, replaced as joint
For material implantation when can be bad due to wearability and generate abrasive dust, inflammation in primosome causes implant failure to fall off.
The present invention adopts the following technical solutions solves above-mentioned technical problem:
The present invention provides a kind of method for improving beta titanium alloy hardness and biocompatibility, comprising the following steps:
(1) casting Ti-Nb-Sn-Zr-Mo titanium alloy template is placed in vacuum tube furnace, and logical inert gas shielding；
(2) temperature of tube furnace is warming up to 730-850 DEG C, heat preservation；
(3) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；
(4) tube furnace, and logical argon gas protection are reopened, 400-480 DEG C is warming up to and keeps the temperature；
(5) tube furnace is closed, and the taking-up of titanium alloy template is placed in cooling in air.
Preferably, the inert gas in the step (1) is one of argon gas, helium, neon.
Preferably, the heating rate of tube furnace is 10-20 DEG C/min in the step (2).
Preferably, the soaking time in the step (2) is 2h.
Preferably, the heating rate of tube furnace is 10-20 DEG C/min in the step (4).
Preferably, the soaking time in the step (4) is 8h.
Preferably, the size of the Ti-Nb-Sn-Zr-Mo titanium alloy template is 100mm × 100mm × 5mm.
Preferably, a method of improving beta titanium alloy hardness and biocompatibility, comprising the following steps:
(1) vacuum will be placed on having a size of 100mm × 100mm × 5mm casting Ti-Nb-Sn-Zr-Mo titanium alloy template
In tube furnace, and logical argon gas protection；
(2) temperature schedule of tube furnace is set as rising to 800 DEG C with the heating rate of 20 DEG C/min；
(3) 2h is kept the temperature in 800 DEG C of temperature；
(4) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；
(5) tube furnace, and logical argon gas protection are reopened, is warming up to 420 DEG C with the heating rate of 10 DEG C/min, and keep the temperature
8h；
(6) tube furnace is closed, and titanium alloy template is quickly removed and is placed in cooling in air.
The present invention also provides one kind by the above method treated beta titanium alloy.
The beneficial effects of the present invention are:
(1) casting Ti-Nb-Sn-Zr-Mo titanium alloy is in greatly micron order by single β phase composition and crystallite dimension very much,
Vickers microhardness is 264 ± 12HV0.02, osteoblast is rounded after 2h is cultivated on its surface, and osteoblast is on its surface
Alkali formula phosphatase (ALP) activity is relatively low after cultivating 7d and 14d；And be heat-treated after Ti-Nb-Sn-Zr-Mo titanium alloy by α+
Two phase composition of β, heat treatment cause the α phase being precipitated to be embedded in β phase matrix with the cobblestone-appearance of 40nm or so, and Vickers hardness increases
Greatly 478 ± 19HV0.02, osteoblast is flat in what is elongated after 2h is cultivated on its surface, and it is thick to form obvious cytoplasm
Side, and osteoblast alkali formula phosphatase (ALP) activity after 7d and 14d is cultivated on its surface significantly improves；
(2) heat treatment method can make the hardness of β type Ti-Nb-Sn-Zr-Mo titanium alloy surface improve 81%, and can improve
Osteoblast stick and bone is to differentiation, provide theoretical foundation to develop more excellent performance of titanium-based planting body.
Detailed description of the invention
Fig. 1 is the Ti-Nb-Sn-Zr-Mo titanium alloy of (b) and (a) before heat treatment after being heat-treated in the embodiment of the present invention
XRD spectrum；
Fig. 2 is the heterogeneous microstructure figure of the Ti-Nb-Sn-Zr-Mo titanium alloy before being heat-treated in the embodiment of the present invention；
Fig. 3 is the heterogeneous microstructure figure of the Ti-Nb-Sn-Zr-Mo titanium alloy after being heat-treated in the embodiment of the present invention；
Fig. 4 is the Ti-Nb-Sn-Zr-Mo titanium alloy sample surface training of osteoblast before heat treatment in the embodiment of the present invention
Aspect graph after supporting 2h；
Fig. 5 is the Ti-Nb-Sn-Zr-Mo titanium alloy sample surface training of osteoblast after heat treatment in the embodiment of the present invention
Aspect graph after supporting 2h；
Fig. 6 is the osteoblast on heat treatment front and back Ti-Nb-Sn-Zr-Mo titanium alloy sample surface after hatching 7 and 14 days
ALP activity figure intracellular.
Specific embodiment
The present invention is described in further details below with reference to Figure of description and embodiment.
Test material and reagent as used in the following examples etc., unless otherwise specified, commercially obtain.
Comparative example 1
(1) vacuum will be placed on having a size of 100mm × 100mm × 5mm casting Ti-Nb-Sn-Zr-Mo titanium alloy template
In tube furnace, and logical argon gas protection；
(2) temperature schedule of tube furnace is set as being warming up to 800 DEG C with the heating rate of 20 DEG C/min；
(3) 2h is kept the temperature in 800 DEG C of temperature；
(4) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template.
Test: by two kinds of titanium alloy template (cast sheets of heat treatment front and back；Cast sheet+heat treatment) through 100#, 400#,
800#, 2500# sand paper sanding and polishing are to mirror surface and are cut into 1mm × 1mm × 5mm small cube as sample progress microhardness
Test；Small cube sample is placed on progress osteoblast co-culture experiments in 24 porocyte culture plates through ultraviolet lighting.
Comparative example 2
(1) vacuum will be placed on having a size of 100mm × 100mm × 5mm casting Ti-Nb-Sn-Zr-Mo titanium alloy template
In tube furnace, and logical argon gas protection；
(2) temperature schedule of tube furnace is set as being warming up to 800 DEG C with the heating rate of 20 DEG C/min；
(3) 2h is kept the temperature in 800 DEG C of temperature；
(4) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；
(5) tube furnace, and logical argon gas protection are reopened, is warming up to 270 DEG C with the heating rate of 10 DEG C/min, and keep the temperature
8h；
(6) tube furnace is closed, and titanium alloy template is quickly removed and is placed in cooling in air.
Test: by two kinds of titanium alloy template (cast sheets of heat treatment front and back；Cast sheet+heat treatment) through 100#, 400#,
800#, 2500# sand paper sanding and polishing are to mirror surface and are cut into 1mm × 1mm × 5mm small cube as sample progress microhardness
Test；Small cube sample is placed on progress osteoblast co-culture experiments in 24 porocyte culture plates through ultraviolet lighting.
Comparative example 3
(1) vacuum will be placed on having a size of 100mm × 100mm × 5mm casting Ti-Nb-Sn-Zr-Mo titanium alloy template
In tube furnace, and logical argon gas protection；
(2) temperature schedule of tube furnace is set as being warming up to 800 DEG C with the heating rate of 20 DEG C/min；
(3) 2h is kept the temperature in 800 DEG C of temperature；
(4) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；
(5) tube furnace, and logical argon gas protection are reopened, is warming up to 570 DEG C with the heating rate of 10 DEG C/min, and keep the temperature
8h；
(6) tube furnace is closed, and titanium alloy template is quickly removed and is placed in cooling in air.
Test: by two kinds of titanium alloy template (cast sheets of heat treatment front and back；Cast sheet+heat treatment) through 100#, 400#,
800#, 2500# sand paper sanding and polishing are to mirror surface and are cut into 1mm × 1mm × 5mm small cube as sample progress microhardness
Test；Small cube sample is placed on progress osteoblast co-culture experiments in 24 porocyte culture plates through ultraviolet lighting.
Embodiment 1
(1) vacuum will be placed on having a size of 100mm × 100mm × 5mm casting Ti-Nb-Sn-Zr-Mo titanium alloy template
In tube furnace, and logical argon gas protection；
(2) temperature schedule of tube furnace is set as rising to 800 DEG C with the heating rate of 20 DEG C/min；
(3) 2h is kept the temperature in 800 DEG C of temperature；
(4) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；
(5) tube furnace, and logical argon gas protection are reopened, is warming up to 420 DEG C with the heating rate of 10 DEG C/min, and keep the temperature
8h；
(6) tube furnace is closed, and titanium alloy template is quickly removed and is placed in cooling in air.
Test: by two kinds of titanium alloy template (cast sheets of heat treatment front and back；Cast sheet+heat treatment) through 100#, 400#,
800#, 2500# sand paper sanding and polishing are to mirror surface and are cut into 1mm × 1mm × 5mm small cube as sample progress microhardness
Test；Small cube sample is placed on progress osteoblast co-culture experiments in 24 porocyte culture plates through ultraviolet lighting.
Hardness test: using the hardness of Mvs-1000JMT2 type micro Vickers measurement sample surfaces, loaded load
For 20g, the load retention time is 5s, and the sample surfaces of every kind of state select 5 points to be tested, and final hardness is averaged；
Cellular morphology observation and ALP active testing:
(1) sample for being heat-treated both front and back state is put into 24 orifice plates, every kind three groups of state sample after sterilizing
Parallel sample；
(2) by the osteoblast of people (hFOB1.19) with 105The density of/well is planted in every hole, is put into incubator
It takes out, is softly rinsed with PBS after being transferred to new bore three times when culture is to 2h, the glutaraldehyde of 300 μ L2.5% is added at 4 DEG C in every hole
Lower fixed 1h is inhaled and is successively dehydrated in 30%, 50%, 70%, 90%, 95% and 100% graded ethanol after abandoning glutaraldehyde
10min, is put into overnight after vacuum oven, after metal spraying processing, is placed under JSM-6700F type field emission scanning electron microscope and observes cell
Form；
(3) 24 porocyte culture plates of culture to 7d and 14d are taken out, inhales and abandon culture solution, with phosphate (PBS) buffer
It cleans three times and is transferred to sample in new emptying aperture, 100 μ L RIPA lysates are added in every hole, and phenylmethylsulfonyl fluoride is added
(PMSF) it keeps protein stabilized, supernatant liquor is collected after centrifugation；
(4) it is operated according to Human ALP elisa Kit (R&D company), the supernatant liquor of extraction is added to
It is coated in the orifice plate of ALP antibody；
(5) under enzyme-linked immunosorbent assay instrument, the OD value of reaction solution is detected under 450nm wavelength, wherein * is represented and is heat-treated
Preceding sample relatively has significant difference.
Measurement result:
Table 1 is the preceding microhardness with Ti-Nb-Sn-Zr-Mo titanium alloy surface after heat treatment of heat treatment
As can be seen from Table 1, comparative example 1, comparative example 2, be heat-treated in comparative example 3 after sample hardness value be heat-treated before do not have
There is significant difference；And its Vickers hardness is increased to 478 ± 19HV in embodiment 10.02, close β type Ti-Nb-Sn-Zr-Mo titanium
The hardness of gold surface improves 81%.
Simultaneously according to measurement result, comparative example 1 is in 2h, 7d and 14d to osteoblast adhesion and bone to the effect of differentiation
Effect function and effect compared with before heat treatment are close, comparative example 2, comparative example 3 in 2h, 7d and 14d to osteoblast adhesion and
Function and effect from bone to differentiation with heat treatment before compared with no significant difference.
Fig. 1 is the XRD spectrum of (b) and the Ti-Nb-Sn-Zr-Mo titanium alloy of (a) before heat treatment after being heat-treated in the present embodiment
Line；Fig. 2 is the heterogeneous microstructure of the Ti-Nb-Sn-Zr-Mo titanium alloy before being heat-treated in the present embodiment, it can be seen that its surface
Crystal grain be micron-sized pure β-Ti, Fig. 3 is microcosmic group of Ti-Nb-Sn-Zr-Mo titanium alloy after being heat-treated in the present embodiment
Knit structure, it can be seen that the α phase of cobblestone-appearance is embedded in β-Ti, and the Ti-Nb-Sn-Zr-Mo titanium alloy after heat treatment is by alpha+beta two
Phase composition, heat treatment cause the α phase being precipitated to be embedded in β phase matrix with the cobblestone-appearance of 40nm or so；
Fig. 4 is that the form after 2h is cultivated on the Ti-Nb-Sn-Zr-Mo titanium alloy sample surface of osteoblast before heat treatment,
Fig. 5 is form of the osteoblast after 2h is cultivated on the Ti-Nb-Sn-Zr-Mo titanium alloy sample surface after the present embodiment heat treatment,
Fig. 6 is the osteoblast on heat treatment front and back Ti-Nb-Sn-Zr-Mo titanium alloy sample surface ALP intracellular after hatching 7 and 14 days
Activity, it can be seen that heat treatment preosteoblast is rounded after 2h is cultivated on its surface, and osteoblast cultivates 7d on its surface
And alkali formula phosphatase (ALP) activity is relatively low after 14d, osteoblast cultivates 2h on its surface after being heat-treated through this embodiment
It is flat in what is elongated afterwards, form obvious cytoplasm webbing, and osteoblast alkali formula phosphorus after 7d and 14d is cultivated on its surface
Sour enzyme (ALP) activity significantly improves.
Embodiment 2
(1) vacuum will be placed on having a size of 100mm × 100mm × 5mm casting Ti-Nb-Sn-Zr-Mo titanium alloy template
In tube furnace, and logical argon gas protection；
(2) temperature schedule of tube furnace is set as rising to 730 DEG C with the heating rate of 20 DEG C/min；
(3) 2h is kept the temperature in 800 DEG C of temperature；
(4) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；
(5) tube furnace, and logical argon gas protection are reopened, is warming up to 480 DEG C with the heating rate of 10 DEG C/min, and keep the temperature
8h；
(6) tube furnace is closed, and titanium alloy template is quickly removed and is placed in cooling in air.
The above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
It is within the scope of the invention with present inventive concept without the various process programs of substantial differences.
Claims (9)
1. a kind of method for improving beta titanium alloy hardness and biocompatibility, it is characterised in that: the following steps are included:
(1) casting Ti-Nb-Sn-Zr-Mo titanium alloy template is placed in vacuum tube furnace, and logical inert gas shielding；
(2) temperature of tube furnace is warming up to 730-850 DEG C, heat preservation；
(3) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；
(4) tube furnace, and logical argon gas protection are reopened, 400-480 DEG C is warming up to and keeps the temperature；
(5) tube furnace is closed, and the taking-up of titanium alloy template is placed in cooling in air.
2. the method according to claim 1 for improving beta titanium alloy hardness and biocompatibility, it is characterised in that: described
Inert gas in step (1) is one of argon gas, helium, neon.
3. the method according to claim 1 for improving beta titanium alloy hardness and biocompatibility, it is characterised in that: described
The heating rate of tube furnace is 10-20 DEG C/min in step (2).
4. the method according to claim 1 for improving beta titanium alloy hardness and biocompatibility, it is characterised in that: described
Soaking time in step (2) is 2h.
5. the method according to claim 1 for improving beta titanium alloy hardness and biocompatibility, it is characterised in that: described
The heating rate of tube furnace is 10-20 DEG C/min in step (4).
6. the method according to claim 1 for improving beta titanium alloy hardness and biocompatibility, it is characterised in that: described
Soaking time in step (4) is 8h.
7. the method according to claim 1 for improving beta titanium alloy hardness and biocompatibility, it is characterised in that: described
The size of Ti-Nb-Sn-Zr-Mo titanium alloy template is 100mm × 100mm × 5mm.
8. the method according to claim 1 for improving beta titanium alloy hardness and biocompatibility, it is characterised in that: including
Following steps:
(1) electron tubes type will be placed on having a size of 100mm × 100mm × 5mm casting Ti-Nb-Sn-Zr-Mo titanium alloy template
In furnace, and logical argon gas protection；
(2) temperature schedule of tube furnace is set as rising to 800 DEG C with the heating rate of 20 DEG C/min；
(3) 2h is kept the temperature in 800 DEG C of temperature；
(4) it closes tube furnace and cools to room temperature with the furnace by titanium alloy template；
(5) tube furnace, and logical argon gas protection are reopened, is warming up to 420 DEG C with the heating rate of 10 DEG C/min, and keep the temperature 8h；
(6) tube furnace is closed, and titanium alloy template is quickly removed and is placed in cooling in air.
9. using any one of claim 1-8 method treated beta titanium alloy.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111876707A (en) * | 2020-08-04 | 2020-11-03 | 安徽理工大学 | Modification method of titanium alloy with bone regeneration promoting and antibacterial functions and modified titanium alloy |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490422A (en) * | 2003-08-08 | 2004-04-21 | 西北有色金属研究院 | Beta type titanium alloy for surgical implanting piece |
| CN105420549A (en) * | 2015-12-10 | 2016-03-23 | 东南大学 | Low-elasticity-modulus high-fatigue-strength biologic implantable titanium alloy and preparation method thereof |
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- 2018-12-13 CN CN201811524770.0A patent/CN109468562B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1490422A (en) * | 2003-08-08 | 2004-04-21 | 西北有色金属研究院 | Beta type titanium alloy for surgical implanting piece |
| CN105420549A (en) * | 2015-12-10 | 2016-03-23 | 东南大学 | Low-elasticity-modulus high-fatigue-strength biologic implantable titanium alloy and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111876707A (en) * | 2020-08-04 | 2020-11-03 | 安徽理工大学 | Modification method of titanium alloy with bone regeneration promoting and antibacterial functions and modified titanium alloy |
| CN111876707B (en) * | 2020-08-04 | 2021-11-19 | 安徽理工大学 | Modification method of titanium alloy with bone regeneration promoting and antibacterial functions and modified titanium alloy |
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