CN102335742A - Method for preparing complexly shaped biomedical porous titanium molybdenum alloy implant body - Google Patents
Method for preparing complexly shaped biomedical porous titanium molybdenum alloy implant body Download PDFInfo
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Abstract
The invention provides a method for preparing a complexly shaped biomedical porous titanium molybdenum alloy implant body and belongs to the technical field of biomedical porous metallic material preparation. The method comprises the following steps of: taking a mixture of titanium and molybdenum metallic element powder and organic polymer powder as raw materials, and then preparing the biomedical porous titanium molybdenum alloy implant body by adopting the processes, such as three-dimensional modeling, selective laser-firing rapid forming, thermal de-greasing, vacuum sintering, and the like. The processing steps are simple, the period is short, the use ratio of materials is high, the cost is low, any complexly shaped porous titanium alloy implant body can be conveniently manufactured, and the method has efficiency and economic advantages in individual design and rapid manufacturing of the implant body. A titanium molybdenum alloy material prepared by using the method has the advantages that pore space is uniform, adjustment scopes of porosity, aperture ratio and aperture are wide, elasticity modulus and compression strength are in close proximity to natural bone, and the demand on biomechanical compatibility required by a biomedical material is met.
Description
Technical field
The invention belongs to bio-medical porous technical field of metal material preparation, a kind of quick method for preparing complicated shape bio-medical porous titanium molybdenum alloy implant is provided.
Background technology
Titanium or titanium alloy has high specific strength, good corrosion resistance, enough wearability and excellent biological compatibility, is considered to the most rising biomedical metal material at present.But; The elastic modelling quantity of fine and close titanium or titanium alloy (55～110GPa) with natural bone (3.21～30GPa) do not match; Make load not to be delivered to adjacent bone tissue well, " stress shielding " phenomenon promptly occurs, cause implant to occur bone stress on every side and absorb by implant; Cause the loosening or fracture of implant, and make the implant surgery failure.The metal material of loose structure; Because the existence of hole; Not only can effectively reduce its elastic modelling quantity and intensity, the biomechanical property of itself and natural bone is complementary, and can also promote cell to grow into; And the passage of providing convenience for the exchange of the transportation of nutriment and body fluid, be a kind of even more ideal biological implantation material.
Ti-6Al-4V is that using the most extensive at present also is the titanium alloy that is used to biomedical sector the earliest; Along with research deepens continuously, find that Al and V are harmful in recent years, Al can cause abalienation and bring out senile dementia; V can react with tissue, forms Heisui River.Therefore, the novel titanium alloy material of research and development seems more and more important.Mo is the β phase stable element of Ti; And belong to isomorphism structure with Ti, can form unlimited solid solution, not only reduce temperature and elastic modelling quantity that α-Ti changes to β-Ti with Ti; And can improve intensity and the wearability of Ti, preparation Ti-Mo porous embedded material is a kind of very attractive selection.
The porous metal material of bio-medical is complex-shaped, and its size varies with each individual, and needs personalized design and makes fast.At present, traditional powder metallurgy die pressing, slurry foaming and the gel injection-moulding method of the many employings of the technology of preparing of porous titanium alloy.Wherein, die pressing adopts the titanium valve compacting of adding pore creating material to form, and preparation technology is simple, and institutional framework is even, but hole dimension is little, and porosity is low; The slurry foaming, though can obtain the POROUS TITANIUM of high porosity, only the addition through blowing agent is difficult to control hole gap structure (like pore size and distribution); The gel injection-moulding method has added multiple additives such as organic matter, antifoaming agent and dispersant when the preparation POROUS TITANIUM, not only contaminated environment increases cost, and brings a lot of problems for follow-up removing process.In a word, the traditional preparation process method of POROUS TITANIUM all needs particular manufacturing craft; Cost height and forming accuracy can't guarantee; Be not suitable for single-piece or small lot batch manufacture, can't obtain complex-shaped loose structure implant especially, RP technique can effectively address this problem.
RP technique (Rapid Prototyping is called for short the RP technology) starts from the eighties in 20th century, is that collection CAD, laser processing technology, Numeric Control Technology and new material technology are a kind of new manufacture of one.Through mapping softwares such as CAD, Pro E, or, obtain threedimensional model with the medical image that CT scan, MRI technology and other methods the obtain processing that datumizes; Adopt discrete/stack shaping principle, laser beam is processed according to pre-designed machined parameters and according to the two-dimensional silhouette information of each synusia, and this series of layers sheet is deposited in together by the shaping order under computer control, generates 3D solid.Selective laser sintering (selective laser sintering is called for short SLS) is a kind of important RP technique, adopts CO
2Laser instrument is a thermal source; In forming process, the pressure that powder receives is very little, so the material of SLS prepared loose structure normally; And rough surface; And this just biological and medicinal implant material for promoting cell and grow into and adhere to neededly that the face shaping of implant can come to change arbitrarily through three-dimensional modeling, can realize the personalized design of implant and make fast; And have that raw material are selected extensively, technical process is simple, forming efficiency is high, need not advantage such as support, the using value at medical domain is more and more come into one's own in recent years.
Adopting the multiporous biological medical material majority of SLS technology preparation is composite (the Tan K H of polymeric material or polymer/ceramic; Chua C K; Leong K F; Et al.Selective laser sintering of biocompatible polymers for applications in tissue engineering [J] .Biomedical materials and engineering, 2005,15 (1-2): 113-124; Zhang Y; Hao L; Savalani M M; Et al.Characterization and dynamic mechanical analysis of selective laser sintered hydroxyapatite filled polymeric composites [J] .Journal of Biomedical Materials Research Part A, 2008,86 (3): 607-616; Eosoly S; Brabazon D, Lohfeld S, et al.Selective laser sintering of hydroxyapatite/poly-ε-caprolactone scaffolds [J] .Acta Biomaterialia; 2010; 6 (7): 2511-2517), these material mechanical performances are generally on the low side, can not satisfy the mechanical compatibility requirement of bio-medical material; And titanium maxter alloy has excellent biological compatibility and mechanical property, does not also see the relevant report that the SLS technology is applied to prepare POROUS TITANIUM molybdenum alloy material at present.
Summary of the invention
The object of the present invention is to provide a kind of method of making the bio-medical porous titanium alloy implant of any complicated shape; To remedy the deficiency of traditional preparation process technology; Enlarge the application of Selective Laser Sintering, efficient production goes out to satisfy the titanium alloy implant of the complicated shape of medical material biocompatibility and mechanical compatibility requirement.
A kind of method for preparing complicated shape bio-medical porous titanium molybdenum alloy implant; It is characterized in that: at first adopt Auto CAD, Pro/E mapping software; Maybe will datumize, design the threedimensional model of implant through the medical photography figure that CT scan, MRI technology obtain; Ti, Mo elemental metalpowder are carried out machinery with the organic polymer powder evenly mix, Mo content is 2～15wt% in the elemental metalpowder, and surplus is Ti, and organic macromolecule content accounts for the 3wt%-15wt% of metal dust total amount; Under argon shield, adopt CO
2Laser beam carries out selective laser sintering (SLS) with mixed-powder, obtains having the preform of the Ti-Mo alloy material implant of given shape; Under vacuum or argon shield, the shaping base is carried out hot degreasing and high temperature sintering, sintering temperature is 800～1500 ℃, promptly obtains bio-medical porous Ti-Mo alloy implant.
Concrete technological process and parameter are following:
(1) adopt ball-milling technology that material powder is carried out mechanical mixture, its technological parameter is: ratio of grinding media to material is 3:1～1:1, ball milling time 3～12h, rotating speed 30～100r/min;
(2) according to different patients' needs, adopt Pro E, CAD or CT scan, MRI technology, the threedimensional model of structure implant can carry out personalized threedimensional model design to the implant (like cantilever, hollow and insert structure etc.) of any complicated shape;
(3) be under the protection of 99.0%～99.9% inert argon, in purity with CO
2Laser instrument is a thermal source, according to pre-designed processing route mixed-powder is carried out selective laser sintering (SLS), obtains the green part of required implant.The SLS technological parameter is: laser power: 10～40W, and sweep speed is 1500～2500mm/s, and sweep span is 0.08～0.25mm, and slice thickness is 0.08～0.25mm, and powder bed preheat temperature is 45～160 ℃;
(4) under vacuum or inert gas shielding, the implant green part is put into debinding furnace, directly carry out hot degreasing; The degreasing main technologic parameters is: skimming temp is 20～750 ℃, and temperature retention time is 0.5～3h, and removing speed is 1～5 ℃/min;
(5) under vacuum or inert gas shielding, implant degreasing part is put into sintering furnace, carry out high temperature sintering, finally obtain the titanium maxter alloy implant.The sintering main technologic parameters is: 800～1500 ℃ of sintering temperatures, temperature retention time are 0.5～3h, and heating rate is 1～5 ℃/min.
The particle diameter of said raw material Ti powder, Mo powder and polymeric powder is respectively: 100～325 orders, 100～500 orders and 100～800 orders.
Said high-molecular organic material is thermoplastic resin and thermosetting resin; Thermoplastic resin comprises polyethylene, high density polyethylene (HDPE), polypropylene, polystyrene, polyamide, polymethyl methacrylate, Merlon or ethylene-vinyl acetate copolymer, and thermosetting resin comprises phenolic resins, melamine, amino resins or epoxy resin.
Advantage of the present invention is:
(1) in the face of requirement of different patients, can personalized design, and directly prepare the bio-medical implant of any complicated shape and high dimensional accuracy;
(2) be easy to regulate alloying component, stock utilization height, additive level is few, little to material and environmental pollution;
(3) forming technology has digitlization and does not have the technical characterstic of modelling, and step of preparation process is simple, and operability and repeatability are strong;
(4) through regulating Mo content, SLS forming technology and sintering process parameter, can realize the control of pore character, matrix microscopic structure and the mechanical property of porous Ti-Mo alloy material;
(5) prepared titanium maxter alloy material hole even tissue, porosity, percent opening and the aperture adjustable extent that goes out is wide; Mechanical property is excellent; Its elastic modelling quantity and intensity and natural bone coupling can satisfy as the needed biomechanical compatibility requirement of bio-medical material.
The specific embodiment
Embodiment 1
Preparation raw material powder: at first adopt electronic balance to take by weighing 300 order Ti powder 340g, 200 order Mo powder 60g, 160 purpose high density polyethylene (HDPE) (HDPE) powder 35g respectively; Then above-mentioned powder is packed into and mix in the ball mill; Ratio of grinding media to material is 3:1, and the ball milling time is 10h, and rotating speed is 55r/min;
Make up threedimensional model: use Pro E software, the 3D shape of drawing implant, and adopt delamination software that threedimensional model is carried out slicing treatment, the two-dimentional lamella information that processing is obtained is with the forming machine of STL format to selective laser sintering;
Selective laser sintering (SLS): with forming accuracy and green strength is standard, and laser beam carries out selective laser sintering (SLS) according to two-dimentional lamella information, and all lamellas are successively coupled together under computer control, obtains implant.Choose the SLS technological parameter of optimization: laser power 34W, sweep speed 1650mm/s, sweep span 0.18mm, slice thickness 0.18mm, 100 ℃ of preheat temperatures;
Hot degreasing: be under 99.8% the argon shield, the implant that SLS is shaped to be put into debinding furnace in purity, to remove organic polymer, degreasing process was divided into for three steps: the first step, and 25～250 ℃, 5 ℃/min of programming rate does not need insulation; Second step, 250～420 ℃, 3 ℃/min of heating rate, insulation 1h; In the 3rd step, 420～600 ℃, 2 ℃/min of heating rate is incubated 1h, and cools off with stove;
High temperature sintering: put into the sintering furnace that vacuum is 2Pa to implant, sinter to 1200 ℃ from room temperature through degreasing, 3 ℃/min of heating rate, and,, obtain the porous implant of Ti-15Mo alloy with the stove cooling at 1200 ℃ of insulation 3h.
Through Measurement and analysis, the porosity of the Ti-15Mo alloy that this technology obtains is 52.8%, and percent opening is 48.6%, and pore size is 180 μ m; Elastic modelling quantity is 5.55GPa, and compressive yield strength is 113.56MPa, with the elastic modelling quantity of people's bone (3.21～30GPa) and compression strength (130～180MPa) is very approaching.
Embodiment 2
On the basis of embodiment 1, only change quality proportioning and high temperature sintering temperature, the i.e. Ti/Mo=9/1 of Ti powder and Mo powder; Be heated to 1500 ℃ from room temperature by the heating rate of 3 ℃/min, and be incubated 3 hours, cool off with stove afterwards; Obtain the Ti-10Mo alloy, its porosity is 18%, and percent opening is 16.3%; The aperture mean size is 30 μ m, and elastic modelling quantity is 54.89MPa, and compressive yield strength is 486.38 MPa.
Embodiment 3
Preparation raw material powder: at first adopt electronic balance to take by weighing 100 purpose Ti powder 460g, 325 purpose Mo powder 40g, 400 purpose polystyrene (PS) powder 30g respectively; Then above-mentioned powder is packed into and mix in the ball mill; Ratio of grinding media to material is 2:1, and the ball milling time is 8h, and rotating speed is 70r/min;
Make up threedimensional model: the 3D shape of using CAD to draw implant, and adopt delamination software that threedimensional model is carried out slicing treatment, the two-dimentional lamella information that processing is obtained is with the forming machine of STL format to selective laser sintering;
Selective laser sintering (SLS): with forming accuracy and green strength is standard, and laser beam carries out selective laser sintering (SLS) according to two-dimentional lamella information, and all lamellas are successively coupled together under computer control, obtains implant.Choose the SLS technological parameter of optimization: laser power 23W, sweep speed 1800mm/s, sweep span 0.20mm, slice thickness 0.20mm, 130 ℃ of preheat temperatures;
Hot degreasing: be under 99.8% the argon shield, the implant that SLS is shaped to be put into debinding furnace in purity, to remove organic polymer, degreasing process was divided into for three steps: the first step, and 25～300 ℃, 5 ℃/min of programming rate does not need insulation; Second step, 300～550 ℃, 3 ℃/min of heating rate, insulation 2h; In the 3rd step, 550～700 ℃, 2 ℃/min of heating rate is incubated 1h, and cools off with stove;
High temperature sintering: put into the sintering furnace that vacuum is 2Pa to implant, sinter to 1250 ℃ from room temperature through degreasing, 3 ℃/min of heating rate, and,, obtain the porous implant of Ti-8Mo alloy with the stove cooling at 1250 ℃ of insulation 2h.
Through Measurement and analysis, the porosity of the Ti-8Mo alloy that this technology obtains is 37.35%, and percent opening is 35.72%, and the maximum diameter of hole reaches 120 μ m; Elastic modelling quantity is 17.76GPa, and compressive yield strength is 255.96MPa
Embodiment 4
On the basis of embodiment 3, only change the content of binding agent, polystyrene becomes 10g by 30g, promptly accounts for the 2wt% of metal dust total amount, is shaped by identical SLS technological parameter, obtains the Ti-8Mo preform.
In SLS is shaped the follow-up clear powder process that finishes; Preform causes intensity too little because binder content is low excessively; The careless slightly or big city of exerting oneself is damaged during operation; Just seem difficult more for back carrying and transportation to carry out degreasing and sintering process, especially thin-wall part damages more easily.
This shows, in order to obtain enough green strengths, with convenient follow-up operational processes, the content of binding agent must be controlled at 3wt% and more than; For complicated shape and large-sized thin-wall part, the content of binding agent should increase relatively, and the upper limit can be controlled in the 15wt%.
Embodiment 5
Preparation raw material powder: at first adopt electronic balance weighing 200 purpose Ti powder 480g, 400 purpose molybdenum powder 20g, 300 purpose polyamide (PA) powder 20g; Then above-mentioned powder is packed into and mix in the ball mill; Ratio of grinding media to material is 1:1, and the ball milling time is 6h, and rotating speed is 40r/min;
Make up threedimensional model: the 3D shape of using CAD to draw implant, and adopt delamination software that threedimensional model is carried out slicing treatment, the two-dimentional lamella information that processing is obtained is with the forming machine of STL format to selective laser sintering;
Selective laser sintering (SLS): with forming accuracy and green strength is standard, and laser beam carries out selective laser sintering (SLS) according to two-dimentional lamella information, and all lamellas are successively coupled together under computer control, obtains implant.Choose the SLS technological parameter of optimization: laser power 18W, sweep speed 2000mm/s, sweep span 0.25mm, slice thickness 0.25mm, 155 ℃ of preheat temperatures;
Hot degreasing: be under 99.8% the argon shield, the implant that SLS is shaped to be put into debinding furnace in purity, to remove organic polymer, degreasing process was divided into for three steps: the first step, and 25～350 ℃, 5 ℃/min of programming rate does not need insulation; Second step, 350～500 ℃, 2 ℃/min of heating rate, insulation 2h; In the 3rd step, 500～600 ℃, 3 ℃/min of heating rate is incubated 1h, and cools off with stove;
High temperature sintering: put into the sintering furnace that vacuum is 2Pa to implant, be warming up to 1100 ℃ from room temperature, 3 ℃/min of heating rate through degreasing; And at 1100 ℃ of insulation 2h; With the stove cooling, obtain the porous implant of Ti-4Mo alloy, its porosity is 48.79%; Percent opening is 47%, and the maximum diameter of hole reaches 160 μ m; Elastic modelling quantity is 4.18GPa, and compressive yield strength is 103.74MPa.
Embodiment 6
This example preparation porous Ti-2Mo alloy is selected 200 order titanium valves, 325 order molybdenum powders for use, and 300 order phenolic resins are material powder, adopt ball mill to mix: ratio of grinding media to material 2:1, rotating speed 40r/min, ball milling 6h; Selective laser sintering (SLS), 20 ℃ of powder bed tempertaure stuck-at-s, table one are the corresponding SLS technological parameter of phenolic resins of different content.
Table 1 mixed-powder SLS forming technology
Through the preform that above SLS technological parameter obtains, degreasing in the argon gas atmosphere of purity >=99.5%, treat that binding agent decomposes fully and volatilizees after, put into vacuum drying oven and sinter to 800 ℃, and insulation 2h, with the stove cooling, obtain porous Ti-2Mo alloy afterwards.Through analyzing, the porosity of Ti-2Mo alloy can reach 60%, pore size 50～200 μ m, and elastic modelling quantity is 3.25GPa, compressive yield strength is 78.84 MPa.
Claims (4)
1. method for preparing complicated shape bio-medical porous titanium molybdenum alloy implant; It is characterized in that: at first adopt Auto CAD, Pro/E mapping software; Maybe will datumize, design the threedimensional model of implant through the medical photography figure that CT scan, MRI technology obtain; Ti, Mo elemental metalpowder are carried out machinery with the organic polymer powder evenly mix, Mo content is 2～15wt% in the elemental metalpowder, and surplus is Ti, and organic macromolecule content accounts for the 3wt%-15wt% of metal dust total amount; Under argon shield, adopt CO
2Laser beam carries out selective laser sintering (SLS) with mixed-powder, obtains having the preform of the Ti-Mo alloy material implant of given shape; Under vacuum or argon shield, the shaping base is carried out hot degreasing and high temperature sintering, sintering temperature is 800～1500 ℃, promptly obtains bio-medical porous Ti-Mo alloy implant.
2. the method for preparing complicated shape bio-medical porous titanium molybdenum alloy implant according to claim 1 is characterized in that: concrete technological process and parameter are following:
(1) adopt ball-milling technology that material powder is carried out mechanical mixture, its technological parameter is: ratio of grinding media to material does
3:1～1:1, ball milling time 3～12h, rotating speed 30～100r/min;
(2) according to different patients' needs, adopt Pro E, CAD or CT scan, MRI technology, the threedimensional model of structure implant can carry out personalized threedimensional model design to the implant of any complicated shape;
(3) be under the protection of 99.0%～99.9% inert argon, in purity with CO
2Laser instrument is a thermal source, according to pre-designed processing route mixed-powder is carried out selective laser sintering (SLS), obtains the green part of required implant; The SLS technological parameter is: laser power: 10～40W, and sweep speed is 1500～2500mm/s, and sweep span is 0.08～0.25mm, and slice thickness is 0.08～0.25mm, and powder bed preheat temperature is 45～160 ℃;
(4) under vacuum or inert gas shielding, the implant green part is put into debinding furnace, directly carry out hot degreasing; The degreasing main technologic parameters is: skimming temp is 20～750 ℃, and temperature retention time is 0.5～3h, and removing speed is 1～5 ℃/min;
(5) under vacuum or inert gas shielding, implant degreasing part is put into sintering furnace, carry out high temperature sintering, finally obtain the titanium maxter alloy implant; The sintering main technologic parameters is: 800～1500 ℃ of sintering temperatures, temperature retention time are 0.5～3h, and heating rate is 1～5 ℃/min.
3. the method for preparing complicated shape bio-medical porous titanium molybdenum alloy implant according to claim 1 is characterized in that: the particle diameter of said raw material Ti powder, Mo powder and polymeric powder is respectively: 100～325 orders, 100～500 orders and 100～800 orders.
4. the method for preparing complicated shape bio-medical porous titanium molybdenum alloy implant according to claim 1 is characterized in that: said high-molecular organic material is thermoplastic resin and thermosetting resin; Thermoplastic resin comprises polyethylene, high density polyethylene (HDPE), polypropylene, polystyrene, polyamide, polymethyl methacrylate, Merlon or ethylene-vinyl acetate copolymer; Thermosetting resin comprises phenolic resins, melamine, amino resins or epoxy resin.
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