CN109701085A - A kind of porous titanium framework strontium doping hydroxyapatite bioactive coating preparation method of 3D printing - Google Patents
A kind of porous titanium framework strontium doping hydroxyapatite bioactive coating preparation method of 3D printing Download PDFInfo
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Abstract
The invention discloses a kind of porous titanium framework strontium doping hydroxyapatite bioactive coating preparation methods of 3D printing comprising: (1) porous titanium framework is prepared by 3D printing technique；(2) surface preparation is carried out to metal implant by sandblasting, annealing, forms the configuration of surface of relative smooth in POROUS TITANIUM rack surface；(3) it immerses in sodium hydroxide solution and is shaken；(4) it is rinsed with water multipass, is successively impregnated in distilled water, dilute hydrochloric acid solution respectively, then dries, heat up, after held for some time, room temperature is cold with furnace；(5) simulated body fluid is configured, strontium chloride is added in simulated body fluid, porous titanium framework is immersed in isothermal vibration in the simulated body fluid containing strontium ion, obtains the hydroxyapatite bioactive coating of strontium doping in POROUS TITANIUM rack surface.The present invention is remarkably improved the Integrated implant, osteoacusis and osteoinductive energy of porous titanium framework；The strontium ion adulterated in coating is remarkably improved in POROUS TITANIUM new Bone Ingrowth speed.
Description
Technical field
The present invention relates to biomedical materials field, specially a kind of porous titanium framework strontium doping hydroxyapatite of 3D printing
Bioactivity coatings preparation method.
Background technique
Bone defect is a kind of clinically common orthopaedic disease, is derived mainly from wound, ablation of tumors and congenital malformation
Deng, small size bone defect can self-heal, and larger-size bone defect is generally difficult to heal automatically, needs to pass through bone collection
Or Method of Tissue Engineering is treated.Wherein Method of Tissue Engineering is considered as treating the most promising research of bone defect
Direction, tissue engineering technique are made of timbering material, growth factor and cell three elements.Timbering material mainly includes metal material
Material, inorganic non-metallic material, high molecular material and its composite material, wherein metal material is due to having higher strength and toughness
Receive extensive research.Metal material, in use, usually with porous structure, meets the need of new Bone Ingrowth as timbering material
It asks.
Traditional porous metals processing technology is difficult to meet the porous structure and implant site being connected to inside orthopaedics implant
Anatomical structure such as matches at the technical needs, and 3D printing technique can then cater to different patients, different implant sites for planting completely
Enter the demand of object personalized customization, it is considered to be orthopaedics implant future most promising research direction.In various metals
In material, POROUS TITANIUM has that intensity is high, density is low and the advantage of good biocompatibility etc., therefore is considered as most having hair
The orthopaedics implant material of exhibition prospect is expected to be applied to the treatment of bone defect as timbering material.
Porous titanium is a kind of bio-inert material, and Integrated implant and osteoinductive can be poor, and new Bone Ingrowth is slow in bracket,
Bracket is difficult to quickly be combined with bone tissue length.For this problem, this patent proposes a kind of novel strontium doping
Hydroxyapatite bioactive coating technology of preparing.Wherein hydroxyapatite has the chemical group similar with bone tissue inorganic constituents
At, the bioactivity with good osseointegration character and osteoacusis and self-bone grafting, while strontium element is needed by human micro
One of element plays a significant role during the growth and development of bone tissue, and hydroxyapatite can degrade in human body, drop
In solution preocess, the strontium element adulterated in hydroxyapatite achievees the purpose that slow release, further increases porous titanium framework
Osteoinductive energy.
Summary of the invention
In order to overcome the above problem, it is living that the present invention provides a kind of porous titanium framework strontium doping hydroxylapatite biology of 3D printing
Property coating production.
The technical solution of the present invention is to provide a kind of porous titanium framework strontium doping hydroxyapatite bioactives of 3D printing to apply
Layer preparation method comprising, it is characterised in that:
(1) porous titanium framework is prepared by 3D printing technique；
(2) surface preparation is carried out to metal implant by sandblasting, annealing, forms relative smooth in POROUS TITANIUM rack surface
Configuration of surface；
(3) it will immerse in sodium hydroxide solution and shake through step (2) treated POROUS TITANIUM；
(4) it uses deionized water or distilled water as multipass is rinsed, is then successively impregnated in distilled water, dilute hydrochloric acid solution respectively
23-25h, is dried in an oven after immersion by 36-45 DEG C of soaking temperature, and 38-43 DEG C of drying temperature, drying time is 23-26 h,
Then sample is warming up to 580-630 DEG C with the rate of 5 DEG C/min, after held for some time, room temperature is cold with furnace；
(5) simulated body fluid is configured, strontium chloride is added in simulated body fluid, will be impregnated by the porous titanium framework of step (4) processing
The isothermal vibration in the simulated body fluid containing strontium ion, it is living in the hydroxylapatite biology that POROUS TITANIUM rack surface obtains strontium doping
Property coating.
Further, in the step (3), the concentration of the sodium hydroxide solution is 4.6-5.8M.
Further, in the step (3), the sodium hydroxide solution is temperature constant state at 54-66 DEG C, the POROUS TITANIUM
Bracket shakes 23-26h in sodium hydroxide solution.
Further, in the step (4), after sample is heated up, 50-75min is kept the temperature.
Further, in the step (4), using the dilute hydrochloric acid solution of 0.4-0.65mM.
Further, in the step (5), strontium ion concentration is 0.1mM-1.0mM.
Further, in the step (5), the porous titanium framework is immersed in simulated body fluid to be shaken with 33-37 DEG C of constant temperature
Swing 67-75h.
The beneficial effects of the present invention are: a kind of porous titanium framework strontium doping hydroxylapatite biology of 3D printing of the invention is living
Property coating production devise the hydroxyapatite bioactive coating of novel strontium doping a kind of, wherein hydroxyapatite coat
Layer is remarkably improved the Integrated implant, osteoacusis and osteoinductive energy of porous titanium framework；The strontium ion adulterated in coating can be significant
Improve new Bone Ingrowth speed in POROUS TITANIUM.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
A kind of porous titanium framework strontium doping hydroxyapatite bioactive coating preparation method of 3D printing of the invention includes
Following examples:
Embodiment 1:
It is described porous by the porous titanium framework of 3D printing processing and fabricating using the other Ti6Al4V metal powder of medical grade as substrate
In structure in being interconnected inside titanium framework, porosity 75%, pore-size is 500 μm, and the size of beam is 200 μm, resistance to compression
120 MPa of intensity, 3.5 GPa of elasticity modulus.
Raw material be the other Ti6Al4V spherical powder of medical grade, purity >=99.99 wt%, 15 μm -45 μm of partial size.
The preparation method of above-mentioned porous titanium framework, comprising the following steps:
(1) the .stl formatted file of the 3-D geometric model of porous titanium framework is obtained using graphics software design；
(2) the 3D printing work process of porous titanium framework are as follows: the interface Building Processing by titanium parameter packet with
.stl file mergences obtains POROUS TITANIUM identifiable .mtt formatted file in 3D printer equipment, by the .mtt formatted file
It is input to 3D printing equipment, is printed under argon atmosphere protection.The wherein parameter in POROUS TITANIUM print procedure are as follows: powdering with a thickness of
30 μm, laser power be 120 W, 70 μ s of time for exposure, 60 μm of laser scanning point spacing, 60 μm of line spacing；Porous titanium framework exists
It is printed under protective atmosphere, protective gas is high-purity argon gas (purity >=99.99%), is printed in engineering, the intracorporal oxygen of working chamber contains
Amount is less than 1000 ppm；
(3) printout is placed in blasting treatment in sand-blasting machine, removes the extra metal powder of surfaces stick；Wherein used in sandblasting
Abrasive material is white fused alumina, and white fused alumina partial size is 50 μm -150 μm, and sandblasting processing active force is 0.3 MPa, 60 s of blast time；
(4) printout successively uses acetone, alcohol, and distilled water is cleaned by ultrasonic 15 minutes respectively, 40 DEG C of vacuum drying；
(5) printout after cleaning is eliminated into the residual stress generated in process by high-temperature heat treatment, and makes bone plate
Smooth surface, heat treatment temperature are 750 DEG C, and heating rate is 5 DEG C/min, keep the temperature 1h, cold with furnace；
(6) it will be immersed through step (5) treated POROUS TITANIUM in the sodium hydroxide solution of 5 M, isothermal vibration is for 24 hours at 60 DEG C；
(7) it uses deionized water or distilled water as rinsing 3 times, then successively soaks in the dilute hydrochloric acid solution of distilled water, 0.5mM respectively
Bubble for 24 hours, 40 DEG C of soaking temperature, is dried, 40 DEG C of drying temperature in an oven after immersion, and drying time is 24 h, then sample
600 DEG C are warming up to the rate of 5 DEG C/min, keeps the temperature 1h, room temperature is cold with furnace；
(8) simulated body fluid is configured, strontium chloride is added in simulated body fluid, strontium ion concentration is 0.1 mM, will be by step (7)
The porous titanium framework of reason is immersed in the simulated body fluid containing strontium ion, isothermal vibration 3 days at 37 DEG C, in porous titanium framework table
Face obtains the hydroxyapatite bioactive coating of doping strontium ion, and content of the strontium element in hydroxyapatite coating layer is 0.9
wt%。
Embodiment 2:
It is described porous by the porous titanium framework of 3D printing processing and fabricating using the other Ti6Al4V metal powder of medical grade as substrate
In structure in being interconnected inside titanium framework, porosity 75%, pore-size is 500 μm, and the size of beam is 200 μm, resistance to compression
120 MPa of intensity, 3.5 GPa of elasticity modulus.
Raw material be the other Ti6Al4V spherical powder of medical grade, purity >=99.99 wt%, 15 μm -45 μm of partial size.
The preparation method of above-mentioned porous titanium framework, comprising the following steps:
(1) the .stl formatted file of the 3-D geometric model of porous titanium framework is obtained using graphics software design.
(2) the 3D printing work process of porous titanium framework are as follows: at the interface Building Processing by titanium parameter packet
With .stl file mergences, POROUS TITANIUM identifiable .mtt formatted file in 3D printer equipment is obtained, by the .mtt format text
Part is input to 3D printing equipment, prints under argon atmosphere protection.The wherein parameter in POROUS TITANIUM print procedure are as follows: powdering thickness
Be 30 μm, laser power be 120 W, 70 μ s of time for exposure, 60 μm of laser scanning point spacing, 60 μm of line spacing；Porous titanium framework
It is printed under protective atmosphere, protective gas is high-purity argon gas (purity >=99.99%), is printed in engineering, the intracorporal oxygen of working chamber
Content is less than 1000 ppm；
(3) printout is placed in blasting treatment in sand-blasting machine, removes the extra metal powder of surfaces stick；Wherein used in sandblasting
Abrasive material is white fused alumina, and white fused alumina partial size is 50 μm -150 μm, and sandblasting processing active force is 0.3 MPa, 60 s of blast time；
(4) printout successively uses acetone, alcohol, and distilled water is cleaned by ultrasonic 15 minutes respectively, 40 DEG C of vacuum drying；
(5) printout after cleaning is eliminated into the residual stress generated in process by high-temperature heat treatment, and makes bone plate
Smooth surface, heat treatment temperature are 750 DEG C, and heating rate is 5 DEG C/min, keep the temperature 1h, cold with furnace；
(6) it will be immersed through step (5) treated POROUS TITANIUM in the sodium hydroxide solution of 5 M, isothermal vibration is for 24 hours at 60 DEG C；
(7) it uses deionized water or distilled water as rinsing 3 times, then successively soaks in the dilute hydrochloric acid solution of distilled water, 0.5mM respectively
Bubble for 24 hours, 40 DEG C of soaking temperature, is dried, 40 DEG C of drying temperature in an oven after immersion, and drying time is 24 h, then sample
600 DEG C are warming up to the rate of 5 DEG C/min, keeps the temperature 1h, room temperature is cold with furnace；
(8) simulated body fluid is configured, strontium chloride is added in simulated body fluid, strontium ion concentration is 0.5 mM, will be by step (7)
The porous titanium framework of reason is immersed in the simulated body fluid containing strontium ion, isothermal vibration 3 days at 37 DEG C, in porous titanium framework table
Face obtains the hydroxyapatite bioactive coating of doping strontium ion, and content of the strontium element in hydroxyapatite coating layer is 1.6
wt%。
Embodiment 3:
It is described porous by the porous titanium framework of 3D printing processing and fabricating using the other Ti6Al4V metal powder of medical grade as substrate
In structure in being interconnected inside titanium framework, porosity 75%, pore-size is 500 μm, and the size of beam is 200 μm, resistance to compression
120 MPa of intensity, 3.5 GPa of elasticity modulus.
Raw material be the other Ti6Al4V spherical powder of medical grade, purity >=99.99 wt%, 15 μm -45 μm of partial size.
The preparation method of above-mentioned porous titanium framework, comprising the following steps:
(1) the .stl formatted file of the 3-D geometric model of porous titanium framework is obtained using graphics software design；
(2) the 3D printing work process of porous titanium framework are as follows: the interface Building Processing by titanium parameter packet with
.stl file mergences obtains POROUS TITANIUM identifiable .mtt formatted file in 3D printer equipment, by the .mtt formatted file
It is input to 3D printing equipment, is printed under argon atmosphere protection.The wherein parameter in POROUS TITANIUM print procedure are as follows: powdering with a thickness of
30 μm, laser power 120W, 70 μ s of time for exposure, 60 μm of laser scanning point spacing, 60 μm of line spacing；Porous titanium framework exists
It is printed under protective atmosphere, protective gas is high-purity argon gas (purity >=99.99%), is printed in engineering, the intracorporal oxygen of working chamber contains
Amount is less than 1000 ppm；
(3) printout is placed in blasting treatment in sand-blasting machine, removes the extra metal powder of surfaces stick；Wherein used in sandblasting
Abrasive material is white fused alumina, and white fused alumina partial size is 50 μm -150 μm, and sandblasting processing active force is 0.3 MPa, blast time 60s；
(4) printout successively uses acetone, alcohol, and distilled water is cleaned by ultrasonic 15 minutes respectively, 40 DEG C of vacuum drying；
(5) printout after cleaning is eliminated into the residual stress generated in process by high-temperature heat treatment, and makes bone plate
Smooth surface, heat treatment temperature are 750 DEG C, and heating rate is 5 DEG C/min, keep the temperature 1h, cold with furnace；
(6) it will be immersed through step (5) treated POROUS TITANIUM in the sodium hydroxide solution of 5 M, isothermal vibration is for 24 hours at 60 DEG C；
(7) it uses deionized water or distilled water as rinsing 3 times, then successively soaks in the dilute hydrochloric acid solution of distilled water, 0.5mM respectively
Bubble for 24 hours, 40 DEG C of soaking temperature, is dried, 40 DEG C of drying temperature in an oven after immersion, and drying time is 24 h, then sample
600 DEG C are warming up to the rate of 5 DEG C/min, keeps the temperature 1h, room temperature is cold with furnace；
(8) simulated body fluid is configured, strontium chloride is added in simulated body fluid, strontium ion concentration is 1.0 mM, will be by step (7)
The porous titanium framework of reason is immersed in the simulated body fluid containing strontium ion, isothermal vibration 3 days at 37 DEG C, in porous titanium framework table
Face obtains the hydroxyapatite bioactive coating of doping strontium ion, and content of the strontium element in hydroxyapatite coating layer is 2.0
wt%。
Above embodiments are only the one such embodiment of the present invention, and the description thereof is more specific and detailed, but can not
Therefore limitations on the scope of the patent of the present invention are interpreted as.It should be pointed out that for those of ordinary skill in the art,
Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection model of the invention
It encloses.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (7)
1. a kind of porous titanium framework strontium doping hydroxyapatite bioactive coating preparation method of 3D printing comprising following step
It is rapid:
(1) porous titanium framework is prepared by 3D printing technique；
(2) surface preparation is carried out to metal implant by sandblasting, annealing, forms relative smooth in POROUS TITANIUM rack surface
Configuration of surface；
It (3) will treated that porous titanium framework immerses in sodium hydroxide solution shakes through step (2)；
(4) it uses deionized water or distilled water as multipass is rinsed, is then successively impregnated in distilled water, dilute hydrochloric acid solution respectively
23-25h, is dried in an oven after immersion by 36-45 DEG C of soaking temperature, and 38-43 DEG C of drying temperature, drying time is 23-26 h,
Then sample is warming up to 580-630 DEG C with the rate of 5 DEG C/min, after held for some time, room temperature is cold with furnace；
(5) simulated body fluid is configured, strontium chloride is added in simulated body fluid, will be impregnated by the porous titanium framework of step (4) processing
The isothermal vibration in the simulated body fluid containing strontium ion, it is living in the hydroxylapatite biology that POROUS TITANIUM rack surface obtains strontium doping
Property coating.
2. the porous titanium framework strontium doping hydroxyapatite bioactive coating preparation of a kind of 3D printing according to claim 1
Method, it is characterised in that: in the step (3), the concentration of the sodium hydroxide solution is 4.6-5.8M.
3. the porous titanium framework strontium doping hydroxyapatite bioactive coating preparation of a kind of 3D printing according to claim 1
Method, it is characterised in that: in the step (3), the sodium hydroxide solution is temperature constant state at 54-66 DEG C, the POROUS TITANIUM
Bracket shakes 23-26h in sodium hydroxide solution.
4. the porous titanium framework strontium doping hydroxyapatite bioactive coating preparation of a kind of 3D printing according to claim 1
Method, it is characterised in that: in the step (4), after sample is heated up, keep the temperature 50-75min.
5. the porous titanium framework strontium doping hydroxyapatite bioactive coating preparation of a kind of 3D printing according to claim 1
Method, it is characterised in that: in the step (4), using the dilute hydrochloric acid solution of 0.4-0.65mM.
6. the porous titanium framework strontium doping hydroxyapatite bioactive coating preparation of a kind of 3D printing according to claim 1
Method, it is characterised in that: in the step (5), strontium ion concentration is 0.1mM-1.0mM.
7. the porous titanium framework strontium doping hydroxyapatite bioactive coating preparation of a kind of 3D printing according to claim 1
Method, it is characterised in that: in the step (5), the porous titanium framework is immersed in simulated body fluid with 33-37 DEG C of isothermal vibration
67-75h。
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Application publication date: 20190503 |