CN105132840B - The method that laser quenching technology prepares enhancing medical beta titanium alloy elastic performance - Google Patents

The method that laser quenching technology prepares enhancing medical beta titanium alloy elastic performance Download PDF

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CN105132840B
CN105132840B CN201510390534.4A CN201510390534A CN105132840B CN 105132840 B CN105132840 B CN 105132840B CN 201510390534 A CN201510390534 A CN 201510390534A CN 105132840 B CN105132840 B CN 105132840B
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titanium alloy
laser
laser quenching
beta titanium
elastic performance
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CN105132840A (en
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马晓丽
王立强
姚成武
吕维洁
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Shanghai Jiaotong University
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Abstract

The invention provides a kind of method that laser quenching technology prepares enhancing medical beta titanium alloy elastic performance, surface hardening processing is carried out to medical beta titanium alloy by semiconductor laser, the technological parameter of laser quenching is power 450W~600W, 6~16mm/s of sweep speed, and processing passage is 1 passage.The method of the present invention significantly improves the elastic performance of medical beta titanium alloy, and surface it is modified medical beta titanium alloy surface it is smooth, be not required to carry out Surface Finishing again to can be used to subsequent process flow.

Description

The method that laser quenching technology prepares enhancing medical beta titanium alloy elastic performance
Technical field
The present invention relates to a kind of surface modification side of the low elastic modulus medical beta titanium alloy for Srgery grafting field Method, surface modification is specifically carried out to Ti-35Nb-2Ta-3Zr (wt.%) beta-titanium alloy using laser quenching process for treating surface, By laser-quenching technique, the elastic performance of medical beta titanium alloy is improved.
Background technology
Phase early 1950s, in Britain and the U.S., pure titanium is used to manufacture bone plate, hip joint, intramedullary nail first With the bio-medical material such as screw.But clinical discovery, the hip joint of pure titanium manufacture and intensity, the rigidity of intramedullary nail are substantially insufficient. Since nineteen nineties, the development of new titanium alloy just turns into the developing focus of medical material.However, titanium closes If the modulus of elasticity of gold is too high, it is placed in organism and is also easy to produce " stress shielding " effect.Titanium alloy is in biomedical aspect It is required using more than having to its biocompatibility, corrosion resistance etc., on the basis of biological safety is ensured, to its mechanical property Can also there is specific requirement.
Also there is such as hardness is low, heat-resisting quantity is poor, electric conductivity and can for the bio-medical titanium or titanium alloy prepared at present The defects of weldering property is bad, wearability is bad, it is also higher to the performance requirement of its material due to the particularity of its application field.It is logical Often we need to improve the use characteristic of titanium or titanium alloy, prior art using the method that surface treatment or surface are modified In mainly pass through micro-arc oxidation, Carburization Treatment, collosol and gel, vapour deposition, plasma spraying, ion implanting, agitating friction The technologies such as welding are surface-treated or are modified to titanium or titanium alloy, but effect is less desirable.Therefore, a kind of new table is developed Face is handled or method of modifying is to improve the elastic performance of bio-medical titanium or titanium alloy, it is met requirement, will have wide Wealthy application prospect.
The content of the invention
For limitation of the prior art, it is an object of the invention to provide a kind of laser quenching technology to strengthen medical beta titanium The method of alloy elastic performance.This technology is applied in the medical beta titanium alloy of self-control research and development, and this beta-titanium alloy has low elasticity mould Amount, nontoxicity, for being implanted into surgery medical field.For prior art and application requirement, by laser quenching technology to medical beta titanium Alloy surface modifying, improve the elastic performance of material.
The present invention is achieved by the following technical solutions:
The invention provides a kind of method that laser quenching technology prepares enhancing medical beta titanium alloy elastic performance, including with Lower step:
(a), material surface is handled:By beta-titanium alloy surface polishing scale removal, the aligning after mill-annealed, protect simultaneously Demonstrate,prove that surface is smooth and flatness, then cleaned with acetone to keep specimen surface to clean;
(b), fixed processing sample:Sample is fixed on the workbench of semi-conductor laser equipment with fixture, through step (a) The surface of processing upward, and sets the technological parameter of laser quenching, ensure in process laser quenching process in which materials not by Oxidation;
(c), material surface is handled:Laser quenching surface modification is carried out to the medical beta titanium alloy after fixed in step (b); Protected in process with argon gas, processing passage is 1 passage.Titanium alloy has the characteristics of inspiratory in Process of Surface Modification, Protected in process with argon gas, effectively prevent titanium alloy and corrode in fusion process with air contact.
Preferably, the composition of described medical beta titanium alloy and mass percent are:Nb:35%, Ta:2%, Zr:3%, Ti:60%.Nb:35%, Ta:2%, Zr:3%, Ti:60%.In beta-titanium alloy, the addition of the element such as Nb, Ta, Zr is on the one hand With preferable biocompatibility, can reduce or avoid being chronically implanted in vivo can to caused by body toxic action, turn into doctor The emphasis developed with beta titanium alloy material;On the other hand, with Ti-Nb, Ti-Ta, Ti-Zr are that the beta-titanium alloy of matrix compares other Conventional titanium alloy, lower modulus of elasticity and Geng Gao intensity can be obtained, it is possible to reduce or to avoid titanium alloy from having larger Modulus of elasticity, implant and cause " stress shielding " phenomenon.So the beta titanium alloy material of proportioning have it is larger medical latent Power.
Beta-titanium alloy structure is Ti-35Nb-2Ta-3Zr.Due to the addition of Nb, Ta and Zr element, this beta titanium alloy has The advantage of low elastic modulus and biocompatibility (nontoxic).
Preferably, described beta-titanium alloy Ti-35Nb-2Ta-3Zr preparation method includes:
Step 1: using vacuum consumable smelting Technology design Nb, Ta and Zr content, it is pressed into after being mixed with titanium sponge Type, and ingot casting is at least quenched twice;
Step 2: by the ingot casting after quenching it is machined after with argon arc welding and auxiliary electrode soldering, again in vacuum consumable Arc melting;
It is Step 3: the spindle after melting is right at 920 DEG C~950 DEG C in 950 DEG C of hot forgings, removal material surface oxide skin Material carries out rolling deformation after annealing processing.
Preferably, in order to ensure the quenching degree of laser quenching, the beta-titanium alloy thickness after step (a) mill-annealed is 0.5~1mm.
Preferably, the annealing time of step (a) mill-annealed is 3~5min, to obtain original state tissue.
Preferably, in described step (b), the laser type used swashs for ROFIN DL 035Q semiconductor lasers Light peak power is 3.5 kilowatts, and it is 808nm~940nm that it, which exports the wavelength of laser,.
Preferably, in described step (b), the technological parameter of laser quenching is power 450W~600W, sweep speed 6~ 16mm/s.When laser power is less than 450W and sweep speed is less than 6mm/s, the modified layer of beta-titanium alloy occurs melting and refreezing and consolidated, Quenching structure can not be formed.
Preferably, in described step (c), laser beam energy distribution when carrying out laser quenching is slow-axis direction into high cap Distribution, is in Gaussian Profile in quick shaft direction.
Preferably, in described step (c), carry out laser quenching when laser spot at spot be rectangle, its size is 2.0mm×3.3mm;Laser and the distance on beta-titanium alloy surface are 5mm.
Preferably, in described step (c), the gas flow of argon gas is set as 20~30L/min.
Laser Cladding of the present invention is one kind of laser surface modification method, and Laser Surface Modification Technology can change Kind material surface performance, has prominent superiority in terms of the materials'use life-span is improved.After Laser Surface Modification Technology processing Modified layer dilution rate it is low, modified layer thickness is easily controlled, and modified layer and matrix are in firm metallurgical binding, and laser surface changes Property processing speed is fast, heat affected area is small, will not cause the change of matrix material performance and size.It is main using laser quenching technology It is the laser beam using high-energy-density, material surface is heated to more than transformation temperature, material is quickly cooled down, austenite transformation For martensite, so that the mechanical property of material changes.
The present invention carries out surface modification by laser quenching technology to self-control beta-titanium alloy Ti-35Nb-2Ta-3Zr, for titanium Alloy has the characteristics of inspiratory in Process of Surface Modification, prevents titanium alloy from oxygen occurs with air contact in fusion process Change, experiment shows that shield gas flow rate is set as that 20-30L/min is more suitable.The case depth of laser surface hardening is general For 0.3~1.5mm, according to the thickness range of titanium alloy in this patent, in order to ensure the quenching degree of material, quenching times are 1 It is secondary.The superlastic Journal of Sex Research of beta-titanium alloy is found by laser quenching technology, the geneva body interface formed is induced by laser quenching and is moved Dynamic and reorientation causes the super elastic characteristics of material.
Compared with prior art, the present invention has following beneficial effect:
1st, method of the invention is to carry out laser quenching on medical beta titanium alloy surface, significantly improves the superlastic of titanium alloy Performance.
2nd, method of the invention is simple to operation, and process cycle is short, it is not necessary to extra hardening media, workpiece deformation is small, Modified layer smooth pieces, without carrying out follow-up finishing processing.With very big marketing and application value.
3rd, the homemade medical beta titanium alloy of the present invention, due to its specific composition and weight ratio, closed with the β titaniums of prior art Metallographic ratio, there is the advantage of low elastic modulus, high intensity, corrosion resistance and biocompatibility.
Brief description of the drawings
The detailed description made by reading with reference to the following drawings to non-limiting example, further feature of the invention, Objects and advantages will become more apparent upon:
Fig. 1 is the elastic performance of medical beta titanium alloy mother metal;
Fig. 2 is elastic performance of the medical beta titanium alloy after laser quenching;
Fig. 3 is macroscopical metallograph of the medical beta titanium alloy after laser quenching;
Fig. 4 is the metallographic structure figure of medical beta titanium alloy mother metal;
Fig. 5 is metallographic structure figure of the medical beta titanium alloy after laser quenching;
Fig. 6 is the surface reforming layer figure obtained using friction stir welding method;
Fig. 7 is macroscopical metallograph of the medical beta titanium alloy of comparative example 2 after laser quenching.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection domain.
Embodiment 1
The present embodiment is related to one kind and medical beta titanium alloy surface is modified using laser quenching technology, is comprised the following steps that:
(a), it is surface-treated:By the medical beta titanium alloy surface polishing scale removal that thickness after mill-annealed is 1mm, use Material surface is polished down to smooth state by sander;The annealing time of the mill-annealed is 3~5min.
(b), processing sample is installed:Sample is fixed on the workbench of semi-conductor laser equipment with fixture, and set Each technological parameter of processing;Design the technological parameter of laser quenching processing:Laser quenching power is 500W, and sweep speed is 12mm/s。
(c), material surface modifying:Laser quenching surface modification is carried out to the medical beta titanium alloy confirmed in step (b);Examination Shown in sample procedure of processing (a), protected in process with argon gas, flow 20L/min, the distance of laser and workpiece surface is 5mm, laser sweep 1 passage soon.
The composition and mass percent of described medical beta titanium alloy be:Nb:35%, Ta:2%, Zr:3%, Ti:60%; Its preparation method includes:Using vacuum consumable smelting Technology design Nb, Ta and Zr content, it is pressed into after being mixed with titanium sponge Type, and ingot casting is at least quenched twice;Ingot casting after quenching is machined afterwards with argon arc welding and auxiliary electrode soldering, exist again Vacuum consumable electrode arc furnace melting;By the spindle after melting in 950 DEG C of hot forgings, removal material surface oxide skin, 920 DEG C~950 DEG C to material carry out rolling deformation after annealing processing.
The super elastic characteristics of sample are represented by pure elastic strain and superelastic strain.In uninstall process, unloading curve It is made up of linear processes two parts, this linear elastic recovery strain is pure elastic strain (E);Rather than Linear Recovery rank Strain caused by section is superelastic strain (SE).Fig. 1 and Fig. 2 show medical beta titanium alloy mother metal and after laser quenching Medical beta titanium alloy elastic performance contrast.Compare Fig. 1, Fig. 2 and understand that after laser quenching, the elastic performance of titanium alloy shows Write and improve.
Embodiment 2
Medical beta titanium alloy surface is modified using laser quenching processing, specific steps are with reference to embodiment 1, with embodiment 1 Difference is as follows:
Thickness is 0.8mm medical beta titanium alloy laser-quenching technique parameter after mill-annealed:Laser quenching power is 450W, sweep speed 6mm/s, argon gas protection, flow 20L/min.Fig. 3 show medical beta titanium alloy and carries out 1 passage laser Macroscopical metallograph after quenching.From the figure 3, it may be seen that after laser quenching is handled, while above-mentioned martensite is formed, titanium alloy Crystal grain substantially grow up, and surface smooth pieces, tissue than more uniform.
Embodiment 3
Medical beta titanium alloy surface is modified using laser quenching processing, specific steps are with reference to embodiment 1, with embodiment 1 Difference is as follows:
Thickness is 0.5mm medical beta titanium alloy laser-quenching technique parameter after mill-annealed:Laser quenching power is 600W, sweep speed 16mm/s, argon gas protection, flow 30L/min.Similarly improve the superelastic properties of titanium alloy. Fig. 4 and Fig. 5 show the metallographic structure figure of medical beta titanium alloy mother metal and the medical beta titanium alloy after laser quenching.Compare figure 4 and Fig. 5 understands that after laser quenching, titanium alloy has organized the formation of more martensite, and this is to improve titanium alloy super-elasticity The main reason for energy.
Comparative example 1
Surface modification is carried out to medical beta titanium alloy described in embodiment 1 using the friction stir welding method of prior art, obtained The surface reforming layer obtained is as shown in fig. 6, the face of weld obtained is rough, it is impossible to which directly application is, it is necessary to carry out follow-up table Face finishes;And the modified layer any surface finish for utilizing laser-quenching method to obtain is smooth, it can directly apply, reduce surface finish The technique of work.
Comparative example 2
Handled using laser remolten and medical beta titanium alloy surface described in embodiment 1 is modified, specific steps reference embodiment 1, Difference is as follows:
Thickness is 0.8mm medical beta titanium alloy laser-quenching technique parameter after mill-annealed:Laser quenching power is 400W, when sweep speed is 2mm/s, when argon gas is protected and flow is 20L/min, titanium alloy surface melts, it is impossible to obtains Quenching structure, as shown in Figure 7.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring the substantive content of the present invention.

Claims (7)

1. a kind of method that laser quenching technology prepares enhancing medical beta titanium alloy elastic performance, it is characterised in that including following step Suddenly:
A, material surface is handled:By medical beta titanium alloy surface polishing scale removal, the aligning after mill-annealed, then use acetone Cleaning;
B, fixed processing sample:Sample is fixed on the workbench of semi-conductor laser equipment, the surface through processing upward, and is set Put the technological parameter of laser quenching;
C, material surface is handled:Laser quenching surface modification is carried out to medical beta titanium alloy under argon gas protection, processing passage is 1 Passage;
In described step b, the wavelength of the output laser of semi-conductor laser equipment is 808nm~940nm;
In described step b, the technological parameter of laser quenching is power 450W~600W, 6~16mm/s of sweep speed;
In described step c, carry out laser quenching when laser spot at spot be rectangle;Laser and beta-titanium alloy surface away from From for 5mm.
2. the method that laser quenching technology as claimed in claim 1 prepares enhancing medical beta titanium alloy elastic performance, its feature exist In the composition and mass percent of described beta-titanium alloy are:Nb:35%, Ta:2%, Zr:3%, Ti:60%.
3. the method that laser quenching technology as claimed in claim 1 or 2 prepares enhancing medical beta titanium alloy elastic performance, it is special Sign is that the preparation method of described beta-titanium alloy includes:
Step 1: using vacuum consumable smelting Technology design Nb, Ta and Zr content, it is compressing after being mixed with titanium sponge, and Ingot casting is at least quenched twice;
Step 2: by the ingot casting after quenching it is machined after with argon arc welding and auxiliary electrode soldering, again in vacuum consumable electric arc Stove melting;
Step 3: by the spindle after melting in 950 DEG C of hot forgings, removal material surface oxide skin, at 920 DEG C~950 DEG C to material Carry out rolling deformation after annealing processing.
4. the method that laser quenching technology as claimed in claim 1 prepares enhancing medical beta titanium alloy elastic performance, its feature exist In the beta-titanium alloy thickness after mill-annealed described in step a is 0.5~1mm.
5. the method that laser quenching technology as claimed in claim 1 prepares enhancing medical beta titanium alloy elastic performance, its feature exist In the annealing time of mill-annealed described in step a is 3~5min.
6. the method that laser quenching technology as claimed in claim 1 prepares enhancing medical beta titanium alloy elastic performance, its feature exist In in described step c, laser beam energy distribution when carrying out laser quenching is is distributed in slow-axis direction into high cap, in fast axle Direction is in Gaussian Profile.
7. the method that laser quenching technology as claimed in claim 1 prepares enhancing medical beta titanium alloy elastic performance, its feature exist In in described step c, the gas flow of argon gas is set as 20~30L/min.
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CN103084714A (en) * 2013-02-03 2013-05-08 梁建波 Laser preprocessing wire filling tungsten inert gas (TIG) welding method of titanium alloy and pure aluminum sheets

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