CN102676750A - Method and device for compositely modifying medical titanium alloy by laser gas nitriding and impacting - Google Patents
Method and device for compositely modifying medical titanium alloy by laser gas nitriding and impacting Download PDFInfo
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Abstract
The invention discloses a method and device for compositely modifying medical titanium alloy by laser gas nitriding and impacting, and relates to the field of laser composite surface modification. A composite surface modification process combining laser gas nitriding and laser impact strengthening treatment is adopted to carry out surface modification on the medical titanium alloy. The device disclosed by the invention comprises a computer monitoring unit, a laser gas nitriding unit, a laser impact treatment unit, a numerical control work system and a measurement feedback system, wherein the computer monitoring unit comprises a computer, a continuous laser controller, a pulse laser controller and a workbench controller. Certain residual stress and highly dislocated tissues are introduced on the surface of a nitration layer by the high-amplitude shock wave pressure generated by laser impact treatment, so that the stress distribution state and the arborescent structure shape of the nitration layer are changed within a certain depth range of the nitration layer, the quality of the nitration layer can be effectively improved, and the service life of the nitration layer can be effectively prolonged.
Description
Technical field
The present invention relates to Laser Combined surface-treated field; Refer in particular to a kind of medical titanium alloy material that is directed against and carry out laser gas nitriding and laser impact intensified surface modifying method; With effective Laser Combined surface modifying method and device that improves its comprehensive use properties, be specially adapted to the surface treatment of plate, club shaped structure medical titanium alloy material.
Background technology
Titanium alloy is one of best metallic substance of present known bioaffinity, has good mechanical performance, specific tenacity, fatigue resistance and biocompatibility, has a wide range of applications at aspects such as knochenbruch joint, spinal fixation, joint prosthesises at present.Yet, how further to improve its wear-resistant resistance to corrosion, the bonding force of enhancing and biological tissue, improving the safe handling property is the subject matter that the biological titanium alloy material is applied.Coenocorrelation is very complicated physics, a chemical electrolysis matter environment, and medical titanium alloy goods long-term existence in human body various forms of wearing and tearing and corrosion can take place.Wearing and tearing and corrosion make the size of material reduce, the smooth finish of failure surface; Even make material surface produce local defect and cause stress concentration; Thereby cause crackle or fracture, and the loosening and fracture failure of implantation goods that the greatest problem of clinical use is caused by corrosion and overstress just.Meanwhile, even the good metallic element of consistency, ion stripping and abrasive dust gathering also require to be controlled in certain safety range.Because the interaction of embedded material and medical environment only limits to several atomic shell places of material surface, therefore, except the composition and preparation technology that improve alloy, process for modifying surface is that biomedical metal material is learned an important developing direction and research focus.Surface-treated through to biomedical beta-titanium alloy material can be improved its various performances effectively, the Special metallic features of matrix and the biological property on top layer is combined better, for the application of biomedical beta-titanium alloy material is laid a good foundation.
At present, raising medical titanium alloy material wear-resistant is anti-corrosion mainly contains sol-gel method, ion sputtering/injection method, acid/alkaline purification method, electrochemical deposition method, plasma pyrolytic coating method and laser surface modification method etc. with the process for modifying surface physiologically acceptable performance.Yet except plasma pyrolytic coating Win 40350 (HA) obtains the clinical application, other seldom obtains practical application.The HA coating that sol-gel method makes is very evenly, crystal grain is very tiny, but and the bonding force between the matrix alloy less relatively, in use come off easily; Traditional is ion implantation because of receiving the restriction of ion implantation energy, and strengthening layer is more shallow; Ion carburizing, glowdischarge carburizing, boronising and nitriding etc. exist shortcomings such as long processing period and the high part of temperature be yielding; Plasma pyrolytic coating process efficiency is high, coating is even, good reproducibility; But pyrolytic coating causes the phase transformation and the embrittlement of coating easily; Become other calcium phosphate salt to reduce surfactivity thereby produce non-crystalline state or thermolysis, and the modified layer weave construction is loose and can't have the bonding interface than high-bond with matrix formation.The laser surface modification technology is laser technology and the product that metallic surface processing combines, and is to apply high energy at material surface to make it to take place physicochemical change, thereby significantly changes wear resistance, solidity to corrosion and the surface hardness of material.Because laser energy density is high, its rate of heating is exceedingly fast, power output is accurately controlled, and alternative modification local surface, and the laser surface modification technology has caused to be paid close attention to widely and pay attention to.
Laser gas nitriding is to utilize high energy laser beam irradiation workpiece surface to make its fusing form the liquid metal molten bath; Simultaneously nitrogen is under the high energy laser beam effect of irradiation and the high-temperature liquid-phase metal generation intensive chemistry/metallurgical reaction in the molten bath; Thereby significantly change the chemical ingredients and the composition of liquid metal in the molten bath; The final hard nitride layer that forms dendritic crystal state to improve the wear resistance and corrosion resistance of workpiece surface, is the process for modifying surface that a kind of extremely has application prospect and potentiality after rapid condensation.Carrying out number of research projects aspect this both at home and abroad; Man H.C. etc. place 3.5%NaCl solution to carry out the experiment of anti-spot corrosion behavior the pure titanium and the T6Al4V alloy of laser gas nitriding; The result shows that the spot corrosion drag of the purer titanium or titanium alloy of nitride layer of formation has improved 12 times more than, has improved its corrosion resisting property greatly.Because this technology belongs to hot-work, unavoidably must produce deleterious residual tension and microcrack, thereby reduce plasticity, fatigue strength and the solidity to corrosion of workpiece, even shorten its work-ing life at finished surface.Laser impact intensified processing can improve the substructure of parts list layer material and produce useful residual compressive stress, thereby improves the fatigue lifetime and enhancing stress corrosion resistant ability of part.2004; The LSP that F/A-22 and F119 mover titanium alloy damaged blade have been carried out in U.S. laser impact technology company and United States Air Force laboratory repairs research; Damaged blade fatigue strength after laser-impact is handled is 413.7MPa; Satisfy the design requirements 379MPa that blade uses fully, obtained immense success.At present, the LSP technology has been applied to the F119-PW-100 engine line.Medically, the titanium alloy artificial knee joint can be brought up to 5-6 from original 2-3 work-ing life after laser impact intensified, and has reduced patient's operation number of times.Though the hardness and the solidity to corrosion on shock treatment surface have had raising, for the part of under wearing and tearing and corrosive environment, being on active service for a long time, surface property still is apparent not enough.Therefore these two kinds of technology are combined; Not only can obtain the remarkable TN modified layer of performance; And can remove the residual tension of nitriding treatment generation and introduce useful residual compressive stress; Further hardened surface and the antifatigue and the anticorrosion stress-resistant ability that increase the modified layer degree of depth and improve material finally obtain high-quality modified surface.
At present; Report document about the medical material Research on Surface Modification has: publication number is that the Chinese patent of CN1712076 provides a kind of method that on the titanium alloy material surface, prepares gradient cladding, and internal layer is the zone of oxidation that under 400-700 ℃, obtains, and thickness is 0.5-5 μ m; Skin is a hydroxyapatite coating layer; Thickness is 0.1-1 μ m, but this implementation of processes cycle is long, working (machining) efficiency is low, and the degree of depth of its inside and outside modified layer is also more shallow in addition; USP U.S. 6491723 has proposed to carry out 1 pickling and with high temperature sulfuric acid (H with hydrofluoric acid (HF)
2SO
4The method that)/hydrochloric acid (HCl) mixed solution carries out 2 pickling, yet thereby pickling causes the hydrogenation of implantation material surface to reduce surface bioactive easily and the hydrogen embrittlement phenomenon takes place, and sulfuric acid (H
2SO
4), hydrofluoric acid (HF) and hydrochloric acid (HCl) is that the easy volatile strong acid of murther damages human body easily.Publication number is that the Chinese patent of CN1676658 adopts hot isostatic pressing technique to carry out the high temperature carburizing processing on the medical titanium alloy surface.Publication number is that the Chinese patent of CN101264551 is incorporated into the modification of medical titanium and titanium alloy material with femtosecond laser, and ablating at material surface forms the regular pattern of even striped, groove or the combination of compound configuration, and generates certain thickness zone of oxidation.Though above-mentioned technology has improved surface hardness, wear resistance property and the biological activity of material to a certain extent; But bring deleterious residual tension to workpiece owing to receive influence of thermal effect; Greatly reduce the fatigue resistance of implant part, increased the susceptibility of corrosion failure.
Do not retrieve at present research document and the related patent U.S. Patent No. of utilizing laser gas nitriding and the composite modified medical titanium alloy material of laser-impact as yet.
Summary of the invention
The objective of the invention is in order to overcome the gradient cladding method; Prior art such as acid wash and hot isostatic pressing technique is not enough; A kind of Laser Combined surface modifying treatment of medical titanium alloy material is provided; Modification is implemented on surface in order to plate, club shaped structure medical titanium alloy material, effectively improves its surperficial wear and corrosion behavior, improves its work-ing life.
The technical scheme that the present invention adopted is:
A kind of laser gas nitriding and the device that impacts composite modified medical titanium alloy comprise computer monitoring unit, laser gas nitriding unit, laser-impact processing unit, numerical control work system and measurement feedback system; The laser gas nitriding unit comprises continuous wave laser, optical fiber collimator, optical fiber, laser beam setter, gas hood and nitrogen pot; The laser-impact processing unit comprises ps pulsed laser and ns pulsed laser device, optical fiber collimator, optical fiber, laser beam setter, cascade sparging unit and waste water reclamation groove; Measurement feedback system is made up of unrelieved stress detector and quick corrosion tester, and the computer monitoring unit comprises computingmachine, pulse laser unit, continuous laser unit and worktable unit; Ps pulsed laser and ns pulsed laser device and continuous wave laser are connected on the computingmachine through pulse laser unit and continuous laser unit respectively, and the unrelieved stress detector of measurement feedback system directly links to each other with computingmachine with quick corrosion tester; Continuous wave laser is fixed on the oscillation isolation platform; One end of optical fiber links to each other with the light-emitting window of continuous wave laser through optical fiber collimator, and the other end of optical fiber then is connected with the laser beam setter, and the laser beam setter is regulated laser beam spot size to satisfy actual processing needs; The anchor clamps that sample is installed are fixed by bolts on five worktable, are covered with sealing in the anchor clamps periphery and use gas hood, and gas hood is fastened on five worktable with bolt; The gas hood front end face offers the transparency silica glass window that can see through laser beam, and relative with the light-emitting window front end of laser beam setter; Gas hood top has been provided with pneumatic joint, and pneumatic joint links to each other with nitrogen pot through pneumatic tube, on pneumatic tube, is provided with pneumavalve and gas meter; The ps pulsed laser and ns pulsed laser device is fixed on the oscillation isolation platform, and an end of optical fiber links to each other with the light-emitting window of ps pulsed laser and ns pulsed laser device through optical fiber collimator, and the other end of optical fiber then is connected with the laser beam setter; The cascade sparging unit is fixed on five worktable, moves to guarantee the stability of cascade with five worktable; The water outlet of cascade sparging unit is positioned at the workpiece front upper place, and the waste water reclamation groove is positioned over the below of processing sample and reclaims processing waste water.
A kind of laser gas nitriding and the method for impacting composite modified medical titanium alloy, concrete steps are following:
[1]. with the pre-treatment of medical titanium alloy workpiece surface: polishing and being polished to surfaceness is lower than Ra1.6, locatees with clamping behind acetone surface oil stain and the dirt.According to processing request, according to predetermined machining locus establishment NC program, and set each device parameter, comprising: continuous and pulse laser parameter, working table movement parameter.
[2]. by worktable unit control movable workbench, traverser is opened air feeder and gas flow 20L/min is set to the laser gas nitrogen treatment district, makes it be full of nitrogen.Set suitable gas laser nitriding process parameter: laser power 800-1800W, wavelength 1064nm, sweep velocity 10-30mm/s, at titanium alloy workpiece surface preparation hard nitride layer.
[3]. by worktable unit control movable workbench, the adjustment Working position gets into laser-impact treatment zone and location.The workpiece surface spraying 20-50 μ m thick even pitch-dark layer of computer control automatic spray-paint device after gas nitriding is handled.
[4]. through computer settings laser-impact processing parameter, pulsed laser energy 15-35J, wavelength 1064nm, PW 7-10ns, overlapping rate 50%.Drive workpiece through the multiaxis worktable and move in order, with the laser-impact processing unit hard nitride layer is carried out shock peening and handle.
[5]. utilize the nitride layer surface after the measurement feedback system impact intensified process to carry out unrelieved stress and electrochemical corrosion performance test.Control residual compressive stress value-below the 180MPa, SCE during as reference the corrosion potential in the 3.5%NaCl electrolytic solution greater than-130mV.If do not reach requirement, then continue beginning repeating step two, implement shock treatment until qualified.
The technique effect that the present invention can reach is:
[1] the present invention has kept the formed dendritic crystal state TiN of laser gas nitrogen treatment layer well, makes the wear resisting property of work material increase greatly; Simultaneously; Laser-impact is handled and is made further densification of TiN layer and refinement; And introduced useful residual compressive stress at the bill of material surface layer; Effectively improve the fatigue lifetime and reduction sensitivity of corrosion of surface in contact, the healing of wound after helping the oriented growth of cell and promoting the titanium alloy material implant into body.
[2] the present invention adopts the duplex surface modification technology that laser gas nitriding and laser-impact are handled; Have instantaneous heating, quick refrigerative characteristics; Do not change the microtexture of body material, and modified layer and matrix be the metallurgical binding that has than high-bond, difficult drop-off.
[3] because laser parameter, action time, focused beam size and machining locus are accurately controlled, and treating processes is untouchable, so the inventive method has great flexibility, determinacy and repeatability.Can realize the modified layer of demands of different, to satisfy medical titanium alloy material different clinical actual needs.
Description of drawings
Below in conjunction with accompanying drawing the present invention is described further.
Fig. 1, medical titanium alloy Laser Combined surface modification treatment schematic representation of apparatus.
Fig. 2 is along the residual stress distribution figure of laser spot diameter direction.
Fig. 3, Laser Combined is handled the microhardness distribution figure of back sample along depth direction.
Fig. 4, the sample wear rate was schemed over time before and after Laser Combined was handled.
Among the figure, 1. computingmachine; 2. pulse laser unit; 3. continuous laser unit; 4. continuous wave laser; 5. ps pulsed laser and ns pulsed laser device; 6. optical fiber collimator; 7. continuous laser is used optical fiber; 8. pulse laser is used optical fiber; 9. laser beam setter; 10. titanium alloy workpiece; 11. gas hood; 12. anchor clamps; 13. five worktable; 14. gas meter; 15. pneumatic tube; 16. nitrogen pot; 17. automatic spray-paint device; 18. pitch-dark coating (absorption layer); 19. cascade sparging unit; 20. waste water reclamation groove; 21. cascade (restraint layer); 22. unrelieved stress detector; 23. quick corrosion tester; 24. worktable unit.
Embodiment
Sample adopts the thick medical Ti 13Nb13Zr sheet alloy of 3mm.
Like Fig. 1, the device of embodiment of the present invention comprises computer monitoring unit, laser gas nitriding unit, laser-impact processing unit, numerical control work system and measurement feedback system.Wherein, the laser gas nitriding unit comprises continuous wave laser 4, optical fiber collimator 6, optical fiber 7 and 8, laser beam setter 9, gas hood 11 and nitrogen pot 16; The laser-impact processing unit comprises ps pulsed laser and ns pulsed laser device 5, optical fiber collimator 6, optical fiber 8, laser beam setter 9, cascade sparging unit 19 and waste water reclamation groove 20; Measurement feedback system is made up of unrelieved stress detector 22 and quick corrosion tester 23, and the computer monitoring unit comprises computingmachine 1, pulse laser unit 2, continuous laser unit 3 and worktable unit 24.
At first with the polished finish of Ti13Nb13Zr sheet alloy specimen surface, and place the acetone ultrasonic cleaning.With anchor clamps 12 good titanium alloy workpiece 10 clampings of surface cleaning on worktable, closed top gas hood 11 is opened air feeder, sets nitrogen flow 20L/min.Start laser gas nitriding unit, zlasing mode TEM00, setting power 1.5KW, spot diameter 3mm through computingmachine 1.Work out NC program input service platform unit 24 according to machining locus, moved by five worktable 13 of worktable unit 24 controls, sweep velocity 20mm/s realizes successively scanning by the road of gas desalination.
When sample is cooled to room temperature fully after gas nitriding is handled, spray the thick even pitch-dark coating 18 of 30 μ m through computingmachine 1 surface of control automatic spray-paint device 17 after gas nitriding is handled.Mobile five worktable 13 to laser-impact districts process the location and the curtain device of fetching boiling water sprays the thick even cascade of 3mm at specimen surface.By computingmachine 1 regulating impulse laser controller 2 and laser beam setter 9, setting pulse laser processing parameter is: pulsed laser energy 20J, PW 10ns, spot diameter 3mm, overlapping rate 50%.Computingmachine 1 starts five worktable 13 and ps pulsed laser and ns pulsed laser device 5 simultaneously, and the pulse laser that ps pulsed laser and ns pulsed laser device 5 sends is radiated at work surface after 9 adjustment of laser beam setter, implement laser impact intensified processing.Five worktable 13 stopped automatically after five worktable 13 moved to the target surface completion of processing by preset track.
After impacting end for the first time, with unrelieved stress detector 22 and quick corrosion tester 23 online detection surface stress and galvanic corrosion data.Then, with result back computingmachine 1,, determine next impact parameter with the contrast of goal-selling value.
The Ti13Nb13Zr alloy is after above-mentioned Combined Processing, and its Combined Processing zone unrelieved stress distributes as shown in Figure 2 along the laser spot diameter direction, the residual compressive stress distribution uniform, and the layer depth that influences that experiment records residual compressive stress is about 1 mm; Laser impact intensified processing has produced a large amount of dislocations and twin tissue, makes the dendritic structure shape of hard nitride layer change.Record alloy static corrosion rate of weight loss by original 0.09g/m through electrochemical corrosion experimental
2H is reduced to 0.03g/m
2H has reduced 60%, and the corrosion potential in 3.5%NaCl electrolytic solution is brought up to-92.7mV by-387.4mV.Simultaneously related experiment shows that its top layer microhardness and wear resisting property significantly improve after the Alloy by Laser Combined Processing, shown in Fig. 3 and 4.
The result shows that this method can effectively improve the wear-resistant and corrosion resistance nature of biological medical titanium alloy, and makes hard nitride layer and basal body interface bond strength also obtain certain enhancing, improves the service life of workpiece.
Claims (4)
1. laser gas nitriding and the method for impacting composite modified medical titanium alloy is characterized in that concrete steps are following:
A. with the pre-treatment of medical titanium alloy workpiece surface: polishing and being polished to surfaceness is lower than Ra1.6, with clamping location behind acetone surface oil stain and the dirt; According to processing request, according to predetermined machining locus establishment NC program, and set each device parameter, comprising: continuous and pulse laser parameter, working table movement parameter;
B. by worktable unit control movable workbench, traverser is opened air feeder to the laser gas nitrogen treatment district, makes it be full of nitrogen; Set gas laser nitriding process parameter, at titanium alloy workpiece surface preparation hard nitride layer;
C. by worktable unit control movable workbench, the adjustment Working position gets into laser-impact treatment zone and location; The workpiece surface spraying 20-50 μ m thick even pitch-dark layer of computer control automatic spray-paint device after gas nitriding is handled;
D. through computer settings laser-impact processing parameter; Drive workpiece through the multiaxis worktable and move in order, with the laser-impact processing unit hard nitride layer is carried out shock peening and handle;
E. utilize the nitride layer surface after the measurement feedback system impact intensified process to carry out unrelieved stress and electrochemical corrosion performance test; Control residual compressive stress value-below the 180MPa, SCE during as reference the corrosion potential in the 3.5%NaCl electrolytic solution greater than-130mV; If do not reach requirement, then continue to begin to be repeated to step B from step B, implement shock treatment until qualified.
2. laser gas nitriding according to claim 1 and the method for impacting composite modified medical titanium alloy; It is characterized in that; Nitrogen gas flow 20L/min among the said step B, gas laser nitriding process parameter: laser power 800-1800W, wavelength 1064nm, sweep velocity 10-30mm/s.
3. laser gas nitriding according to claim 1 and the method for impacting composite modified medical titanium alloy; It is characterized in that; Laser-impact processing parameter among the said step D: pulsed laser energy 15-35J, wavelength 1064nm, PW 7-10ns, overlapping rate 50%.
4. implement the described laser gas nitriding of claim 1 and impact the device of the method for composite modified medical titanium alloy; It is characterized in that, comprise computer monitoring unit, laser gas nitriding unit, laser-impact processing unit, numerical control work system and measurement feedback system; The laser gas nitriding unit comprises continuous wave laser (4), optical fiber collimator (6), optical fiber (7), laser beam setter (9), gas hood (11) and nitrogen pot (16); The laser-impact processing unit comprises ps pulsed laser and ns pulsed laser device (5), optical fiber collimator (6), optical fiber (8), laser beam setter (9), cascade sparging unit (19) and waste water reclamation groove (20); Measurement feedback system is made up of unrelieved stress detector (22) and quick corrosion tester (23), and the computer monitoring unit comprises computingmachine (1), pulse laser unit (2), continuous laser unit (3) and worktable unit (24); Ps pulsed laser and ns pulsed laser device (5) and continuous wave laser (4) are connected on the computingmachine (1) through pulse laser unit (2) and continuous laser unit (3) respectively, and the unrelieved stress detector (22) of measurement feedback system directly links to each other with computingmachine (1) with quick corrosion tester (23); Continuous wave laser (4) is fixed on the oscillation isolation platform; One end of optical fiber (7) links to each other with the light-emitting window of continuous wave laser (4) through optical fiber collimator (6); The other end of optical fiber (7) then is connected with laser beam setter (9), and laser beam setter (9) is regulated laser beam spot size to satisfy actual processing needs; The anchor clamps (12) that sample is installed are fixed by bolts on five worktable (13), are covered with sealing in anchor clamps (12) periphery with gas hood (11), and gas hood (11) is fastened on five worktable (13) with bolt; Gas hood (11) front end face offers the transparency silica glass window that can see through laser beam, and relative with the light-emitting window front end of laser beam setter (9); Gas hood (11) top has been provided with pneumatic joint, and pneumatic joint links to each other with nitrogen pot (16) through pneumatic tube (15), on pneumatic tube (15), is provided with pneumavalve and gas meter (14); Ps pulsed laser and ns pulsed laser device (5) is fixed on the oscillation isolation platform, and an end of optical fiber (8) links to each other with the light-emitting window of ps pulsed laser and ns pulsed laser device (5) through optical fiber collimator (6), and the other end of optical fiber (8) then is connected with laser beam setter (9); Cascade sparging unit (19) is fixed on five worktable (13), moves to guarantee the stability of cascade with five worktable (13); The water outlet of cascade sparging unit (19) is positioned at the workpiece front upper place, and waste water reclamation groove (20) is positioned over the below of processing sample and reclaims processing waste water.
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| CN108914048B (en) * | 2018-07-24 | 2020-11-20 | 南华大学 | Method for preparing titanium nitride coating by laser micro-melting in-situ reaction |
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| CN109402542A (en) * | 2018-12-05 | 2019-03-01 | 贵州大学 | A method of gradient micro/nano-scale twin is obtained on TC21 titanium alloy surface layer |
| CN110129719A (en) * | 2019-05-29 | 2019-08-16 | 河北科技大学 | A method of preparing titanium alloy surface nitration case |
| CN111286584A (en) * | 2020-04-01 | 2020-06-16 | 重庆金樾光电科技有限公司 | System and method for laser nitriding metal surfaces |
| CN113118633A (en) * | 2021-04-21 | 2021-07-16 | 吉林大学 | Method for preparing periodic microstructure on surface of titanium alloy through nanosecond laser irradiation |
| CN115341167A (en) * | 2022-08-26 | 2022-11-15 | 西安电子科技大学 | Nanometer twin crystal ZrN diffusion shielding layer and preparation method thereof |
| CN115341167B (en) * | 2022-08-26 | 2024-01-16 | 西安电子科技大学 | Nanometer twin crystal ZrN diffusion shielding layer and preparation method thereof |
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