CN106041074A - Preparation method for novel titanium alloy artificial bone implant - Google Patents
Preparation method for novel titanium alloy artificial bone implant Download PDFInfo
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- CN106041074A CN106041074A CN201610403344.6A CN201610403344A CN106041074A CN 106041074 A CN106041074 A CN 106041074A CN 201610403344 A CN201610403344 A CN 201610403344A CN 106041074 A CN106041074 A CN 106041074A
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
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- A—HUMAN NECESSITIES
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y30/00—Apparatus for additive manufacturing; Details thereof or accessories therefor
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention provides a preparation method for a novel titanium alloy artificial bone implant. The preparation method comprises the following steps that (1) metal powder is mixed to be titanium alloy powder which is composed of, by weight, 13%-16.5% of thallium, 1%-12% of zirconium and the balance titanium and inevitable impurities, and the sum of the components is 100%; (2) the titanium alloy powder is subjected to ball milling and material mixing treatment; (3) the titanium alloy powder subjected to ball milling and material mixing treatment is conveyed to selective laser melting quick forming equipment; and (4) formed titanium alloy is subjected to segmented cooling treatment. By means of the technical scheme, the minimum Young modulus of the titanium alloy artificial bone implant prepared through the method reaches 41 GPa and is very close to the Young modulus (30-40 GPa) of a human bone; and meanwhile, the titanium alloy artificial bone implant has good mechanical properties, accordingly, a bone stress-shielding effect cannot be caused, growing of bones can be facilitated, and implant infection cannot happen.
Description
Technical field
The present invention relates to biology medical material technical field, be specifically related to the system of a kind of new titanium alloy artificial bone implant
Preparation Method.
Background technology
Due to wound, the Cranial defect that the reason such as tumor and infection causes all is tormenting numerous patients every year, need into
Row bone grafting is transplanted.But, clinically pollution in wide area Cranial defect is treated use conventional bone-grafting material likely because of
Secondary infection and cause bone collection failure.Bone tissue engineer includes three key factors: signaling molecule (skeletal growth factor, self-bone grafting
The factor), timbering material and target cell.Wherein the selection of timbering material is the key problem of bone tissue engineer.Current support material
Material mainly has natural timbering material, the timbering material of synthetic and composite.The skeletal support frame material such as hone lamella, nail
Key technology be that it possesses good biocompatibility, certain porosity and hole traffic rate.Natural material has biofacies
Capacitive is good, cell recognition signal, beneficially cell adhesion propagation；Although artificial material lacks cell signal, but has natural material
Not enough can with large-scale production, can design and the advantage such as control structure, mechanical performance and degradation time.Along with skeleton damages
Continuing to bring out and trend that aged tendency of population is the most serious of wound, develop have satisfactory texture, biocompatibility bionical
Artificial bone repair materials is particularly important.Titanium alloy because of have specific strength height, corrosion resistance welding good, easy, low Young's modulus with
And the feature such as outstanding biocompatibility and be widely used in making the biomaterials such as prosthetic appliance, taken
Obtained good result.The Young's modulus of general titanium alloy is more much higher than the Young's modulus of skeleton, first practical titanium
Alloy is the Ti-6Al-4V alloy that the U.S. succeeds in developing, due to its thermostability, intensity, plasticity, toughness, formability, solderable
Property, corrosion resistance and biocompatibility all preferable, and become the trump alloy in titanium alloy industry, this alloy usage amount has accounted for all
The 75%～85% of titanium alloy.But the Young's modulus of Ti-6Al-4V alloy is 131.51GPa, this can cause skeleton stress to hide
Cover effect, cause bone gradually atrophy around, it was reported that the incidence rate that titanium alloy implant infects averagely up to 5.8%.Therefore,
Research and develop low Young's modulus, other titanium alloys corrosion resistant are significant.
The metal implant of traditional method manufacture is the overweight and excessive discomfort easily causing patient of rigidity because of self, and real
The structure of the heart causes between implant-host bone fixing without engaging each other, and easily causes and gets loose, causes implant to subtract service life
Few.Selective laser fusing (Selective Laser Melting, SLM) technology, Three-dimensional Gravity after scanning first with micro-CT
Build, its parameter of pore structure of MIMICS software measurement, and and the three-dimensional modeling data of its correspondence do statistics comparison.Its correspondence
Three-dimensional modeling data；The three-dimensional modeling data of early stage is modified and the removable free titanium alloy powder of post processing of material, improvement
The porosity characteristic of material, can prepare baroque artificial bone scaffold from there through SLM technology.But, how to select laser
The parameters of selective melting: melt temperature, slicing delamination, scanning speed etc., need according to different metal dusts and making
Requirement and designed, designed.
Therefore, for drawbacks described above present in currently available technology, it is necessary to study in fact, to provide a kind of scheme,
Solve defect present in prior art.
Summary of the invention
Too high in order to change the Young's modulus of titanium alloy artificial bone implant in prior art, the invention provides a kind of new
The preparation method of Type Titanium Alloy artificial bone implant, uses new titanium alloy formula, uses selective laser melting method simultaneously, if
Meter selects the parameters of selective laser fusing, makes good biocompatibility and the tool of the titanium alloy artificial bone implant of the present invention
There are certain porosity and hole traffic rate and there is certain mechanical strength to support the growth of defective bone.
For solving the problem that prior art exists, the technical scheme is that
The preparation method of a kind of new titanium alloy artificial bone implant, comprises the following steps:
(1) metal dust is mixed into titanium alloy powder, wherein, described titanium alloy powder by 13～16.5% (weight) thallium and
1～the zirconium of 12% (weight), remaining is made up of titanium and inevitable impurity, and above each component sum is 100%；
(2) titanium alloy powder in step (1) is carried out ball mill mixing process；Wherein, the parameter of ball-milling treatment is: ratio of grinding media to material 1:
2～1:4, rotating speed 90～105rpm, Ball-milling Time 3～4h, make titanium alloy powder spherical in shape, particle diameter is less than 25 μm；
(3) titanium alloy powder after ball mill mixing processes is transported to precinct laser fusion rapid molding equipment, according to importing
The CAD diagram molding artificial bone implant of described precinct laser fusion rapid molding equipment；In forming process, and simultaneously with every point
The flow input argon of clock 2～3.5 liters and the oxygen of 100～200ppm, be gradually heating to temperature 1090 that laser melts～
1180℃；
(4) titanium alloy of molding is carried out sub-sectional cooling process；
Wherein, sub-sectional cooling processes further comprising the steps of: the first stage, after precinct laser fusion soak terminates, with
90～105 DEG C are cooled to 1000 DEG C per hour, keep 2～3.5 hours；Second stage, arrives with per hour 80～95 DEG C of water coolings
500 DEG C, keep 3～4.5 hours；Phase III, with per hour 100～115 DEG C of air coolings to room temperature, prepare new titanium alloy
Artificial bone implant.
Preferably, in titanium alloy powder, wherein, the purity of Titanium powder is more than 99.9%, thallium powder
Purity is 99.9%, and the purity of metal zirconium powder is more than 99.9%.
Preferably, in described step (3), precinct laser fusion rapid molding equipment is SLM Solution ' s 500HL
(SLM Solutions Group AG, Germany).
Preferably, in described step (3), the parameter of precinct laser fusion rapid molding equipment is: output be 390～
420W, scanning speed is 200～215mm/s.
Preferably, the size of the artificial bone implant of molding is
Compared with prior art, beneficial effects of the present invention is as follows:
(1) Young's modulus of the titanium alloy artificial bone implant of the present invention is minimum up to 41GPa, with the Young's modulus (30-of people's bone
40GPa) closely, from without causing skeleton stress capture-effect, the growth of skeleton can be promoted, will not occur to plant body-sensing
Dye；
(2) the titanium alloy artificial bone implant of the present invention has good mechanical performance, ultimate tensile strength (Ultimate
Tensile strength), yield strength (Yield strength (YS)), the index such as elongation percentage (Elongation) relative to
Prior art is all significantly increased such that it is able to ensure that enough intensity is to support the growth of defective bone；
(3) simultaneously, the microcellular structure of the titanium alloy artificial bone implant of the present invention, there is certain porosity and hole traffic
Rate, beneficially bone cells stick propagation.
Accompanying drawing explanation
Fig. 1 is the SEM shape appearance figure of the stretching fracture of the embodiment of the present invention 1；
Fig. 2 is the SEM shape appearance figure of the stretching fracture of the embodiment of the present invention 2；
Fig. 3 is the SEM shape appearance figure of the stretching fracture of the embodiment of the present invention 3；
Fig. 4 is the SEM shape appearance figure of the stretching fracture of the embodiment of the present invention 4；
Fig. 5 is the Young's modulus comparison figure of the embodiment of the present invention；
Fig. 6 is four embodiment mechanical performance comparison figures of the present invention；
Fig. 7 is the XRD analysis figure of four embodiments of the present invention；
Fig. 8 is to use the artificial bone implant of embodiment 3 to carry out osteorrhaphy to be implanted in the tibia of rat, shows after 8 weeks
Micro-inspection bone growth figure.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and
It is not used in the restriction present invention.
On the contrary, the present invention contain any be defined by the claims the replacement done in the spirit and scope of the present invention, repair
Change, equivalent method and scheme.Further, in order to make the public that the present invention to be had a better understanding, thin to the present invention below
During joint describes, detailed describe some specific detail sections.There is no these detail sections for a person skilled in the art
Description can also understand the present invention completely.
The preparation method of a kind of new titanium alloy artificial bone implant, it is characterised in that comprise the following steps:
(1) metal dust is mixed into titanium alloy powder, wherein, described titanium alloy powder by 13～16.5% (weight) thallium and
1～the zirconium of 12% (weight), remaining is made up of titanium and inevitable impurity, and above each component sum is 100%；
(2) titanium alloy powder in step (1) is carried out ball mill mixing process；Wherein, the parameter of ball-milling treatment is: ratio of grinding media to material 1:
2～1:4, rotating speed 90～105rpm, Ball-milling Time 3～4h, make titanium alloy powder spherical in shape, particle diameter is less than 25 μm；
(3) titanium alloy powder after ball mill mixing processes is transported to precinct laser fusion rapid molding equipment, according to importing
The CAD diagram molding artificial bone implant of described precinct laser fusion rapid molding equipment；In forming process, simultaneously with per minute
The flow input argon and the oxygen of 100～200ppm of 2～3.5 liters, and be gradually heating to temperature 1090 that laser melts～
1180℃；Wherein argon is used as inertia protection gas, and for rinsing the titanium of fusing, thallium and zirconium metal to eliminate in molded samples
Unnecessary pore.The effect of oxygen is used for exothermic heat of reaction: the big calorimetric of releasing is conducive to titanium, thallium and zirconium metal under the effect of laser
Melt completely.
(4) titanium alloy of molding is carried out sub-sectional cooling process；The purpose using sub-sectional cooling method is conducive to titanium alloy microcosmic to tie
Being formed uniformly of structure, simultaneously for the consistency of new titanium alloy artificial bone implant, the strain cracking of prevention part, energy simultaneously
Obtain the strongest plasticity coupling.
Wherein, sub-sectional cooling processes further comprising the steps of: the first stage, terminate in precinct laser fusion soak
After, it is cooled to 1000 DEG C with per hour 90～105 DEG C, keeps 2～3.5 hours；Second stage, with per hour 80～95 DEG C of water-cooleds
But to 500 DEG C, keep 3～4.5 hours；Phase III, with per hour 100～115 DEG C of air coolings to room temperature, prepare Novel Titanium
Alloy artificial bone implant.
In the titanium alloy powder of step (1), wherein, the purity of Titanium powder is more than 99.9%, thallium powder
Purity be 99.9%, the purity of metal zirconium powder is more than 99.9%.
The composition of raw materials selected is based primarily upon following:
Titanium (Ti) is a kind of important structural metal grown up the 1950's, and titanium alloy is high, anti-corrosion because having intensity
Good, the thermostability high of property.
Thallium (Ta), a kind of silvery white heavy metal, matter is soft, nonelastic, easily melt.The titanium alloy made with thallium has raising alloy
Intensity, improve alloy rigidity, strengthen the multifrequency nature such as alloy corrosion performance.
Zirconium (Zr), is a kind of rare metal, has surprising corrosion resistance, high fusing point, the hardness of superelevation and intensity etc.
Characteristic, zirconium, be referred to as " vitamin " of metallurgical industry, play its strong deoxidation, denitrogenate, the effect of desulfuration.It is reported, steel
Add millesimal zirconium, hardness and intensity in as long as will shockingly improve, the titanium alloy containing zirconium, the lightest but also high temperature resistant, by force
Degree is the twice of ordinary magnesium alloy, in the manufacture available to jet engine component.Zirconium has excellent biocompatibility simultaneously,
Be conducive to stablizing β phase simultaneously, thus reduce Young's modulus.
The precinct laser fusion rapid molding equipment used in step (3) is SLM Solution ' s500HL (SLM
Solutions Group AG, Germany).Precinct laser fusion is that one utilizes high power laser light directly by metal powder sintered one-tenth
The quick molding method of 3D solid, through complex three-dimensional manufacture being converted into the superposition of two dimension manufacture, eliminates the sky of part
Between complexity.The artificial bone CAD diagram that will process is converted into stl file and is input in SLM, the Autofab software energy in SLM
Automatically process and detect inputted stl file can process.SLM can directly produce the functor of arbitrarily complicated shape.
Following parameter: output is 390～420W, scanning speed is 200～215mm/s.Metal dust paving powder
Thickness is 0.25～0.30mm.The slippage of moulding cylinder every layer is 30～40 μm, and inputs with the flow of 2～3.5 liters per minute
Argon and the oxygen of 100～200ppm.After molding a layer entity, workbench declines a thickness, and and then raw material is put down
Spread out new layer to be processed.Thus rapid shaping titanium alloy artificial bone implant.SLM Solution ' s 500HL is utilized to add
Work goes out the artificial bone implant of various sizes, and wherein, the preferably artificial bone implant of molding is
Embodiment 1
Titanium alloy powder, contains in terms of weight %: 13% thallium, 1% zirconium, and remaining is titanium and inevitable impurity composition.
The material powder of above-mentioned configuration is carried out ball mill mixing.The parameter of ball-milling treatment is: ratio of grinding media to material 1:2, rotating speed
90rpm, Ball-milling Time 3h, make titanium alloy powder spherical in shape, and particle diameter is less than 25 μm.
The SLM Solutions 500HL using Germany carries out precinct laser fusion rapid molding, and precinct laser fusion is fast
The parameter of speed former is: output is 390W, and scanning speed is 200mm/s, and accessory size isInput argon and the oxygen of 100ppm with the flow of 2 liters per minute simultaneously；The temperature that laser melts
It it is 1090 DEG C.
Again titanium alloy being carried out sub-sectional cooling, the parameter of sub-sectional cooling is: the first stage, at precinct laser fusion high temperature dwell
After temperature terminates, it is cooled to 1000 DEG C with per hour 90 DEG C, keeps 2 hours；Second stage, with per hour 80 DEG C of water coolings to 500
DEG C, keep 3 hours；Phase III, with per hour 100 DEG C of air coolings to room temperature.
Use JEOL JSM-6460 to carry out SEM detection, observe the microstructure of alloy, referring specifically to shown in Fig. 1.
Using PANalyticX'Pert PRO to carry out XRD detection, the phase composition of detection alloy, referring specifically to shown in Fig. 7.
Use the Young's modulus of resonance method test titanium alloy, referring specifically to shown in Fig. 5.
Embodiment 2
Titanium alloy powder, contains in terms of weight %: 14.2% thallium, 4.7% zirconium, and remaining is titanium and inevitable impurity group
Become.
The material powder of above-mentioned configuration is carried out ball mill mixing.The parameter of ball-milling treatment is: ratio of grinding media to material 1:3, rotating speed
95rpm, Ball-milling Time 3.5h, make titanium alloy powder spherical in shape, and particle diameter is less than 25 μm.
The SLM Solutions 500HL using Germany carries out precinct laser fusion rapid molding, and precinct laser fusion is fast
The parameter of speed former is: output is 400W, and scanning speed is 205mm/s, and accessory size isInput argon and the oxygen of 150ppm with the flow of 2.5 liters per minute simultaneously；The temperature that laser melts
Degree is 1100 DEG C.
Again titanium alloy being carried out sub-sectional cooling, the parameter of sub-sectional cooling is: the first stage, at precinct laser fusion high temperature dwell
After temperature terminates, it is cooled to 1000 DEG C with per hour 95 DEG C, keeps 2.5 hours；Second stage, arrives with per hour 85 DEG C of water coolings
500 DEG C, keep 3.5 hours；Phase III, with per hour 105 DEG C of air coolings to room temperature.
Use JEOL JSM-6460 to carry out SEM detection, observe the microstructure of alloy, referring specifically to shown in Fig. 2.
PANalyticX'Pert PRO is used to carry out XRD detection, referring specifically to shown in Fig. 7.
Use the Young's modulus of resonance method test titanium alloy, referring specifically to shown in Fig. 5.
Embodiment 3
Titanium alloy powder, contains in terms of weight %: 15.2% thallium, 9.6% zirconium, and remaining is titanium and inevitable impurity group
Become.
The material powder of above-mentioned configuration is carried out ball mill mixing.The parameter of ball-milling treatment is: ratio of grinding media to material 1:3, rotating speed
100rpm, Ball-milling Time 3.5h, make titanium alloy powder spherical in shape, and particle diameter is less than 25 μm.
The SLM Solutions 500HL using Germany carries out precinct laser fusion rapid molding, and precinct laser fusion is fast
The parameter of speed former is: output is 410W, and scanning speed is 210mm/s, and accessory size isInput argon and the oxygen of 200ppm with the flow of 3 liters per minute simultaneously；The temperature that laser melts
It it is 1150 DEG C.
Again titanium alloy being carried out sub-sectional cooling, the parameter of sub-sectional cooling is: the first stage, at precinct laser fusion high temperature dwell
After temperature terminates, it is cooled to 1000 DEG C with per hour 100 DEG C, keeps 3 hours；Second stage, with per hour 90 DEG C of water coolings to 500
DEG C, keep 4 hours；Phase III, with per hour 110 DEG C of air coolings to room temperature.
Use JEOL JSM-6460 to carry out SEM detection, observe the microstructure of alloy, referring specifically to shown in Fig. 3.
PANalyticX'Pert PRO is used to carry out XRD detection, referring specifically to shown in Fig. 7.
Using the Young's modulus of resonance method test titanium alloy, test result is referring specifically to shown in Fig. 5.
Titanium alloy is cut into the height fritter for 3.75mm, fritter is put in ethanol and clean 2.5 hours, pass through afterwards
Osteorrhaphy is implanted in the tibia of rat, carries out micrography after 8 weeks.
Embodiment 4
Titanium alloy powder, contains in terms of weight %: 16.5% thallium, 12% zirconium, and remaining is titanium and inevitable impurity group
Become.
The material powder of above-mentioned configuration is carried out ball mill mixing.The parameter of ball-milling treatment is: ratio of grinding media to material 1:4, rotating speed
105rpm, Ball-milling Time 4h, make titanium alloy powder spherical in shape, and particle diameter is less than 25 μm.
The SLM Solutions 500HL using Germany carries out precinct laser fusion rapid molding, and precinct laser fusion is fast
The parameter of speed former is: output is 420W, and scanning speed is 215mm/s, and accessory size isInput argon and the oxygen of 180ppm with the flow of 3.5 liters per minute simultaneously；The temperature that laser melts
Degree is 1180 DEG C.
Again titanium alloy being carried out sub-sectional cooling, the parameter of sub-sectional cooling is: the first stage, at precinct laser fusion high temperature dwell
After temperature terminates, it is cooled to 1000 DEG C with per hour 105 DEG C, keeps 3.5 hours；Second stage, arrives with per hour 95 DEG C of water coolings
500 DEG C, keep 4.5 hours；Phase III, with per hour 115 DEG C of air coolings to room temperature.
Use JEOL JSM-6460 to carry out SEM detection, observe the microstructure of alloy, referring specifically to shown in Fig. 4.
PANalyticX'Pert PRO is used to carry out XRD detection, referring specifically to shown in Fig. 7.
Use the Young's modulus of resonance method test titanium alloy, referring specifically to shown in Fig. 5.
The titanium alloy artificial bone implant prepared by above-described embodiment, and by professional equipment, it is carried out test analysis,
See Fig. 1 to Fig. 4, the SEM image of the shown SEM pattern alloy being respectively four embodiment stretching fractures of the present invention, can see
Go out the microcellular structure of the titanium alloy of the present invention, there is certain porosity and hole traffic rate, be beneficial to bone cells and stick increasing
Grow.
See Fig. 5, show the Young's modulus of titanium alloy artificial bone implant of the present invention and the Ti-6Al-4V of prior art
Performance comparision, it can be seen that Young's modulus 131.51GPa of Ti-6Al-4V, the titanium alloy Young mould of present invention design
Measure minimum up to 41GPa, with the Young's modulus (30-40GPa) of people's bone closely.Seeing Fig. 8, showing employing and have
Titanium alloy artificial bone implant in the embodiment 3 of low Young's modulus, is implanted in the tibia of rat by osteorrhaphy, 8 weeks
After carry out micrography bone growth figure, inspection after postoperative eight weeks display is without infecting phenomenon, and bone molding is all right.Do not go out
Existing periosteum necrosis or osteoporosis.Thus prove that the titanium alloy of the present invention will not cause skeleton stress capture-effect, can promote
Enter the growth of skeleton, implantation body will not be occurred to infect.
Seeing Fig. 6, the mechanical performance showing titanium alloy artificial bone implant of the present invention and Ti-Ta alloy compares, four
The ultimate tensile strength (Ultimate tensile strength) that embodiment sample measurement obtains be respectively 1078,831,
911,723Mpa, is higher than ultimate tensile strength 594Mpa of Ti-Ta；Yield strength Yield of four embodiment samples
Strength (YS) be respectively 1051,793,864,619Mpa, be all higher than yield strength 5699Mpa of Ti-Ta；Four embodiments
The elongation percentage Elongation of sample is respectively 22.9%, 20.8%, 18.9%, 13.5%, is all higher than the elongation percentage of Ti-Ta
5.9%.Therefore, the titanium alloy artificial bone implant of the present invention has good mechanical performance, and good mechanical performance ensures foot
Enough intensity is to support the growth of defective bone.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (5)
1. the preparation method of a new titanium alloy artificial bone implant, it is characterised in that comprise the following steps:
(1) metal dust is mixed into titanium alloy powder, wherein, described titanium alloy powder by 13～16.5% (weight) thallium and
1～the zirconium of 12% (weight), remaining is made up of titanium and inevitable impurity, and above each component sum is 100%；
(2) titanium alloy powder in step (1) is carried out ball mill mixing process；Wherein, the parameter of ball-milling treatment is: ratio of grinding media to material 1:
2～1:4, rotating speed 90～105rpm, Ball-milling Time 3～4h, make titanium alloy powder spherical in shape, particle diameter is less than 25 μm；
(3) titanium alloy powder after ball mill mixing processes is transported to precinct laser fusion rapid molding equipment, according to importing
The CAD diagram molding artificial bone implant of described precinct laser fusion rapid molding equipment；In forming process, and simultaneously with every point
The flow input argon of clock 2～3.5 liters and the oxygen of 100～200ppm, be gradually heating to temperature 1090 that laser melts～
1180℃；
(4) titanium alloy of molding is carried out sub-sectional cooling process；
Wherein, sub-sectional cooling processes further comprising the steps of: the first stage, after precinct laser fusion soak terminates, with
90～105 DEG C are cooled to 1000 DEG C per hour, keep 2～3.5 hours；Second stage, arrives with per hour 80～95 DEG C of water coolings
500 DEG C, keep 3～4.5 hours；Phase III, with per hour 100～115 DEG C of air coolings to room temperature, prepare new titanium alloy
Artificial bone implant.
The preparation method of new titanium alloy artificial bone implant the most according to claim 1, it is characterised in that at titanium alloy
In powder, wherein, the purity of Titanium powder is more than 99.9%, and the purity of thallium powder is 99.9%, metal zirconium powder
Purity be more than 99.9%.
The preparation method of new titanium alloy artificial bone implant the most according to claim 1, it is characterised in that described step
(3) in, precinct laser fusion rapid molding equipment is SLM Solution ' s 500HL (SLM Solutions Group AG, moral
State).
The preparation method of new titanium alloy artificial bone implant the most according to claim 3, it is characterised in that described step
(3) in, the parameter of precinct laser fusion rapid molding equipment is: output is 390～420W, scanning speed be 200～
215mm/s。
The preparation method of new titanium alloy artificial bone implant the most according to claim 1, it is characterised in that the people of molding
The size of work bone implant is
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| CN106822994A (en) * | 2016-12-30 | 2017-06-13 | 浙江工业大学 | A kind of stainless steel is implanted into composite material and its preparation and application |
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| CN108159488A (en) * | 2018-01-12 | 2018-06-15 | 杭州电子科技大学 | A kind of porous titanium magnesium alloy artificial bone that can promote bone growth and preparation method thereof |
| CN110066928A (en) * | 2019-06-03 | 2019-07-30 | 南通晶朋新材料科技有限公司 | A kind of artificial bone preparation method |
| CN110575289A (en) * | 2019-09-20 | 2019-12-17 | 重庆新索医药科技有限公司 | 3D printing method for bone defect prosthesis |
| CN111299585A (en) * | 2020-03-20 | 2020-06-19 | 武汉市第一医院 | Preparation method of artificial bone |
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| CN106822994A (en) * | 2016-12-30 | 2017-06-13 | 浙江工业大学 | A kind of stainless steel is implanted into composite material and its preparation and application |
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| CN108159488B (en) * | 2018-01-12 | 2020-08-07 | 杭州电子科技大学 | Porous titanium-magnesium alloy artificial bone capable of promoting bone growth and preparation method thereof |
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| CN110575289A (en) * | 2019-09-20 | 2019-12-17 | 重庆新索医药科技有限公司 | 3D printing method for bone defect prosthesis |
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