CN107158474A - Photocuring 3D printing dentistry implant slurry and its preparation method and application - Google Patents
Photocuring 3D printing dentistry implant slurry and its preparation method and application Download PDFInfo
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- CN107158474A CN107158474A CN201710383565.6A CN201710383565A CN107158474A CN 107158474 A CN107158474 A CN 107158474A CN 201710383565 A CN201710383565 A CN 201710383565A CN 107158474 A CN107158474 A CN 107158474A
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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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- 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
- A61L27/02—Inorganic materials
- A61L27/10—Ceramics or glasses
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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
- A61L27/14—Macromolecular materials
- A61L27/16—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- A61L27/14—Macromolecular materials
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
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Abstract
The invention discloses a kind of photocuring 3D printing dentistry implant slurry and its preparation method and application, material composition is:Silicon nitride ceramic, photosensitive resin, light trigger, reactive diluent, dispersant and auxiliary agent, wherein:The volume ratio of the photosensitive resin and the silicon nitride ceramic is 3:7~1:9, the adding proportion of the light trigger is 0.1~1.5wt% of photosensitive resin, the adding proportion of the reactive diluent is 15~30wt% of photosensitive resin, and the dispersant adding proportion is 1~5wt% of silicon nitride ceramic weight, and the auxiliary agent adding proportion accounts for the 0.1~1% of gross mass.The dentistry implant that the slurry of the present invention is prepared has outside good biocompatibility, and its intensity, fracture toughness and wearability are respectively provided with larger raising.
Description
Technical field
The present invention relates to the composition of medical silicon nitride, manufacture, application, and in particular to a kind of photocuring 3D printing dentistry plantation
Body slurry and its preparation method and application.
Background technology
With the development of human society, the increase of aging population ratio, and war, traffic accident, athletic competition etc. are living
Unexpected injury caused by dynamic is also more and more, and which results in people's implants in vivo (artificial, elbow, knee joint, artificial femur
Head, utilization of cervical implants, Invasive lumbar fusion device, intervention support, pacemaker, artificial auditory ossicle, fracture of lumbar vertebra steel plate, screw fixture, tooth
Section's planting body etc.) demand increase.According to statistics, the annual whole world there are about 800,000 people and do joint prosthesis operation;Tooth-implanting is produced
Industry is also increased on world market with annual 20% speed.The wide application prospect of visible human body implant.
Conventional people's implants in vivo material has several major classes such as metal material, high-molecular organic material and ceramic material.
Titanium and its alloy because its good corrosion resistance, outstanding biocompatibility, low modulus of elasticity and excellent fatigue resistance into
For most widely used metal material in people's implants in vivo, but titanium alloy coefficient of friction is high, wears no resistance and often limits it
Application.Comparatively ideal high-molecular organic material is the superelevation average molecular weight northylen (UHMWPE) of excellent in abrasion resistance, relatively
Molecular mass about 3,000,000, its Volume erosion rate is only the 1/5~1/10 of high density polyethylene (HDPE) and nylon, and coefficient of friction is much small
In stainless steel.But its wear particle easily brings bone dissolution at a specified future date, and there are some researches show:When with gamma-rays to polyethylene
When transplant carries out disinfection, the polymer chain in radial energy cut-out ultra-high molecular weight polyethylene makes its wearability degradation.Phosphorus
Sour DFP ceramics, hydroxylapatite ceramic and calcium phosphate cement and bone, the inorganic composition of tooth are close, and its basis is hydroxyl
Apatite, belongs to biomaterial category.Research shows that the material has good compatibility and bone guided effect, but biomaterial
Deficiency is all there is in terms of intensity, toughness, plasticity.Played an important role for a long time in people's implants in vivo material
Aluminium oxide ceramics stable chemical performance, good biocompatibility, in biologically inert, its hardness is high, and anti-wear performance is good.But aluminum oxide
Ceramics category fragile material, its bending strength is only 380MPa, and fracture toughness only has 3.5MPam1/2, can go out in use
Existing brittle break and bone injury.And the fracture toughness of zirconium oxide is good, 15~30MPam is reached as high as1/2, but its Vickers hardness is only
There is 13Gpa, wearability is poor.
Silicon nitride ceramics due to high intensity, high rigidity, high abrasion resistance and good biological tolerance make its
Application in terms of the implantation in human body orthopaedics and joint receives much concern.Single silicon nitride ceramics under certain conditions by break-in,
Silicon nitride ceramics surface of friction pair can reach the clean degree of ultraphotic, and its friction factor and wear rate in water can become very little.From
From the point of view of tribology angle, under certain condition, its friction and wear behavior is quite outstanding for single silicon nitride ceramics.But single nitridation
Silicon ceramic sintering temperature is high, not easy-sintering and to there is aquation dangerous, and its performance must be generally improved by doping vario-property.
Silicon nitride is prepared into people's implants in vivo with other composition doping although having at present, is all to be confined to bone
On bone or articular prosthesis, silicon nitride is mixed with which composition can just overcome single silicon nitride ceramics as the scarce of people's implants in vivo
The correlative study that point can be suitable as dentistry implant again has no report.
The forming method of traditional silicon nitride ceramic material has dry-pressing formed, isostatic pressing, note solidification forming, is injected into
Type, these methods are required to preparation, sinter molding and the machinery in later stage of the mold design, silicon nitride powder or slurry of early stage
Processing, surface polishing.It can be prepared completely using conventional method for the simple people's implants in vivo of shape matching,
And for the preparation of the extremely complex people's implants in vivo of those shapes, particularly dentistry implant, using needed for conventional method
The early stage mold design and the machining operation in later stage wanted often lead to the extension of manufacturing cycle and the raising of production cost, very
Cause conventional method can not realize the manufacture of the product to due to unconventional complicated shape.
The content of the invention
An object of the present invention is to provide a kind of photocuring 3D printing dentistry implant slurry.
To achieve these goals, the present invention is achieved through the following technical solutions:
A kind of photocuring 3D printing dentistry implant slurry, material composition is:Silicon nitride ceramic, photosensitive resin, light
Initiator, reactive diluent, dispersant and auxiliary agent, wherein:The volume ratio of the photosensitive resin and the silicon nitride ceramic is
3:7~1:9, the adding proportion of the light trigger is 0.1~1.5wt% of photosensitive resin, the addition of the reactive diluent
Ratio is 15~30wt% of photosensitive resin, and the dispersant adding proportion is 1~5wt% of silicon nitride ceramic weight, institute
State auxiliary agent adding proportion accounts for gross mass 0.1~1%.
It is preferred that:The silicon nitride ceramic, including following component:α-Si3N4Powder 60~90wt%, β-Si3N4Powder 30~
0wt%, surplus is that additive is (preferred:10wt% additive), the additive is Al2O3、Y2O3、La2O3、TiO2、
One or more of magnesium aluminate spinel.
It is preferred that:The photosensitive resin is the mixing of urethane acrylate, epoxy acrylate or both.
It is preferred that:The light trigger is 1173 (2- hydroxy-2-methyl -1- phenyl -1- acetone), TPO (2,4,6 (front threes
Base benzoyl) diphenyl phosphine oxide), one or more of 819 (phenyl double (2,4,6- trimethylbenzoyls) phosphine oxides).
It is preferred that:The reactive diluent is:HEMA (hydroxyethyl methacrylate), TPGDA (tripropylene glycol dipropyls
Olefin(e) acid ester), HDDA (1,6- hexylene glycol double methacrylate), one or more of TMPTA (trimethylolpropane trimethacrylate).
It is preferred that:The dispersant is the mixture of polyamide and polyester, low molecule amount unsaturated carboxylic acid polymer, containing acid
Silane alcohol base ammonium salt, the high score with ceramic powder affinity groups of the copolymer of property group, the block interpolymers with acidic-group
One or more of son amount block copolymerization liquid solution.
It is preferred that:The auxiliary agent be cross linking polysiloxane acrylate, cross-linked silicone polyether acrylate, be crosslinked it is organic
One or more of silicon polyether acrylate.
The second object of the present invention is to provide the preparation method of above-mentioned slurry, first by photosensitive resin, light trigger, activity
Diluent is mixed (preferably:Mixed by way of magnetic agitation) obtain photopolymer system, then by silicon nitride ceramic,
Dispersant, auxiliary agent are (in batches, preferably:2-3 times) add in above-mentioned photopolymer system, then carry out disperseing (preferably:Carry out
Ball milling disperses), obtain slurry (preferably:Viscosity is 2000~5000mPas).
The third object of the present invention, which is to provide above-mentioned slurry, is used for the forming method of 3D printing:Slurry addition light is consolidated
In the hopper for changing 3D printer, suitable exposure parameter is adjusted (preferably:10~30ms of time for exposure, sweep speed 1000~
4000mm/s) the required dentistry implant CAD model printed is opened, in shaping software:Cura、Repetier Host、
The lower printing for completing dentistry implant biscuit of the control such as 3DBuilder, biscuit is dried, degreasing, obtained after high temperature sintering
Dentistry implant.
Compared with prior art, the invention has the advantages that:
(1) present invention is to single silicon nitride powder doping vario-property, and the formula powder of formation overcomes single silicon nitride powder
Performance shortcomings, and this formula powder need not move through traditional mist projection granulating, compacting, sintering, machining.Formula slurry is matched somebody with somebody
Closing light solidification 3D printing shaping, the dentistry implant of preparation realizes quick manufacture while proof strength, toughness, wearability.
(2) present invention is more than 700MPa using the silicon nitride dentistry implant bending strength of photocuring 3D shapings, is broken tough
Property be more than 6MPam1/2, Volume erosion rate is less than 1mm3/ 1,000 ten thousand cycles, with presently commercially available metal material dentistry implant
Compared to higher reliability, and photocuring 3D printing shaping can realize the quick, demand of personalized customization.
(3) in stereolithographic process, the determination of special exposure parameter needs to consider silicon nitride ceramics powder particles to light
The scattering process in source, calculates critical phototonus energy, adjusts suitable curing depth, it is ensured that the Stereolithography of dentistry implant;
The viscosity of ceramic slurry be then ensure ceramic powder high solids content and ceramic slurry good fluidity it is dual under the premise of determine,
High solid loading ensure that the intensity of dentistry implant, the good fluidity of slurry ensure that Stereolithography effect.
Embodiment
In order to be better understood by technical scheme, the present invention is made furtherly with reference to specific embodiment
It is bright.
Embodiment 1
Step 1:Carry out the preparation of silicon nitride ceramic:Proportionally, α-siliconnitride, beta-silicon nitride, addition are weighed respectively
Agent, 4 hours are stirred to well mixed standby by ball mill;
Step 2:A certain amount of photosensitive resin, light trigger, reactive diluent are weighed according to proportioning, is added by 60 DEG C of water-baths
The mode of heat+magnetic agitation mixes 5 minutes and obtains photopolymer system;
Step 3:Silicon nitride ceramic, dispersant, 2 batches of other auxiliary agents point are added in above-mentioned photopolymer system, entered
Row ball milling disperses, and obtains the ceramic slurry that viscosity is 3500mPas.
Step 4:In the hopper that ceramic slurry is added to photocuring 3D printer, exposure parameter is adjusted:Time for exposure 20ms,
Sweep speed 2500mm/s, opens the dentistry implant CAD model Jing Guo slicing treatment, and dentistry is completed under shaping software control
The printing of planting body biscuit.
Step 5:Biscuit is dried, degreasing, dentistry implant is obtained after high temperature sintering.
The consumption of each raw material:Silicon nitride ceramic 72g, photosensitive resin 10ml, light trigger 0.1g, reactive diluent 2g,
Dispersant 2.16g, auxiliary agent 0.43g.
Used photosensitive resin is urethane acrylate, and the light trigger is 1173, and the reactive diluent is
HEMA, the dispersant is the modest-DP983 of moral, and the auxiliary agent is Rad 2100.
Embodiment 2
Step 1:Carry out the preparation of silicon nitride ceramic:Proportionally, α-siliconnitride, beta-silicon nitride, addition are weighed respectively
Agent, 3 hours are stirred to well mixed standby by ball mill;
Step 2:A certain amount of photosensitive resin, light trigger, reactive diluent are weighed according to proportioning, is added by 60 DEG C of water-baths
The mode of heat+magnetic agitation mixes 7 minutes and obtains photopolymer system;
Step 3:Silicon nitride ceramic, dispersant, 3 batches of other auxiliary agents point are added in above-mentioned photopolymer system, entered
Row ball milling disperses, and obtains the ceramic slurry that viscosity is 2000mPas.
Step 4:In the hopper that ceramic slurry is added to photocuring 3D printer, exposure parameter is adjusted:Time for exposure 10ms,
Sweep speed 4000mm/s, opens the dentistry implant CAD model Jing Guo slicing treatment, and dentistry is completed under shaping software control
The printing of planting body biscuit.
Step 5:Biscuit is dried, degreasing, dentistry implant is obtained after high temperature sintering.
The consumption of each raw material:Silicon nitride ceramic 168g, photosensitive resin 30ml, light trigger 0.45g, reactive diluent
9g, dispersant 8.4g, auxiliary agent 2.16g.
Used photosensitive resin is epoxy acrylate, and the light trigger is TPO, and the reactive diluent is
TPGDA or/and HDDA, the dispersant is Bi Ke-BYKP-105 or/and Disperbyk-180, and the auxiliary agent is Rad
2200。
Embodiment 3
Step 1:Carry out the preparation of silicon nitride ceramic:Proportionally, α-siliconnitride, beta-silicon nitride, addition are weighed respectively
Agent, 5 hours are stirred to well mixed standby by ball mill;
Step 2:A certain amount of photosensitive resin, light trigger, reactive diluent are weighed according to proportioning, is added by 55 DEG C of water-baths
The mode of heat+magnetic agitation mixes 8 minutes and obtains photopolymer system;
Step 3:Silicon nitride ceramic, dispersant, 3 batches of other auxiliary agents point are added in above-mentioned photopolymer system, entered
Row ball milling disperses, and obtains the ceramic slurry that viscosity is 5000mPas.
Step 4:In the hopper that ceramic slurry is added to photocuring 3D printer, exposure parameter is adjusted:Time for exposure 30ms,
Sweep speed 1000mm/s, opens the dentistry implant CAD model Jing Guo slicing treatment, and dentistry is completed under shaping software control
The printing of planting body biscuit.
Step 5:Biscuit is dried, degreasing, dentistry implant is obtained after high temperature sintering.
The consumption of each raw material:Silicon nitride ceramic 216g, photosensitive resin 10ml, light trigger 0.15g, reactive diluent
3g, dispersant 10.8g, auxiliary agent 2.4g.
Used photosensitive resin is the mixing of urethane acrylate and epoxy acrylate, and the light trigger is
819, the reactive diluent is TMPTA, and the dispersant is Disperbyk-111 or/and Disperbyk-168, described to help
Agent is Rad 2250.
Comparative example
The performance comparision such as table 1 below of the products such as the performance and titanium alloy of dentistry implant prepared by the present invention.
Table 1
As can be seen from Table 1, the dentistry implant that the present invention is prepared has outside good biocompatibility, its intensity,
Fracture toughness and wearability are above the product that other compositions are prepared.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art
Member should be appreciated that invention scope involved in the application, however it is not limited to the technology of the particular combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, is carried out by above-mentioned technical characteristic or its equivalent feature
Other technical schemes formed by any combination.Such as features described above has similar work(with (but not limited to) disclosed herein
The technical characteristic of energy carries out technical scheme formed by replacement mutually.
Claims (10)
1. a kind of photocuring 3D printing dentistry implant slurry, it is characterized in that:Material composition is:It is silicon nitride ceramic, photosensitive
Resin, light trigger, reactive diluent, dispersant and auxiliary agent, wherein:The body of the photosensitive resin and the silicon nitride ceramic
Product is than being 3:7~1:9, the adding proportion of the light trigger is 0.1~1.5wt% of photosensitive resin, the reactive diluent
Adding proportion be photosensitive resin 15~30wt%, the dispersant adding proportion for silicon nitride ceramic weight 1~
5wt%, the auxiliary agent adding proportion accounts for the 0.1~1% of gross mass.
2. slurry as claimed in claim 1, it is characterized in that:The silicon nitride ceramic, including following component:α-Si3N4Powder 60
~90wt%, β-Si3N430~0wt% of powder, surplus is additive.
3. slurry as claimed in claim 2, it is characterized in that:The additive is Al2O3、Y2O3、La2O3、TiO2, magnalium point it is brilliant
One or more of stone.
4. slurry as claimed in claim 1, it is characterized in that:The photosensitive resin is urethane acrylate, epoxy acrylic
The mixing of ester or both.
5. slurry as claimed in claim 1, it is characterized in that:The light trigger is 2- hydroxy-2-methyl -1- phenyl -1- third
One in double (2,4,6- trimethylbenzoyls) phosphine oxides of ketone, 2,4,6 (trimethylbenzoyl) diphenyl phosphine oxides, phenyl
More than kind.
6. slurry as claimed in claim 1, it is characterized in that:The reactive diluent is:Hydroxyethyl methacrylate, two contractings three
One or more of propylene glycol diacrylate, 1,6- hexylene glycols double methacrylate, trimethylolpropane trimethacrylate.
7. slurry as claimed in claim 1, it is characterized in that:The dispersant is mixture, the low molecule of polyamide and polyester
Measure unsaturated carboxylic acid polymer, the copolymer containing acidic-group, the silane alcohol base ammonium salt of block interpolymers with acidic-group, tool
There is one or more of HMW block copolymerization liquid solution of ceramic powder affinity groups.
8. slurry as claimed in claim 1, it is characterized in that:The auxiliary agent is cross linking polysiloxane acrylate, crosslinking is organic
One or more of silicon polyether acrylate, cross-linked silicone polyether acrylate.
9. the preparation method of any described slurries of claim 1-8, it is characterized in that:First by photosensitive resin, light trigger, work
Property diluent be mixed to get photopolymer system, silicon nitride ceramic, dispersant, auxiliary agent are then added into above-mentioned photosensitive resin body
In system, then disperseed, obtain slurry.
10. the photocuring 3D printing forming method of any described slurries of claim 1-8, it is characterized in that:The slurry is added
In the hopper for entering photocuring 3D printer, suitable exposure parameter is adjusted, the dentistry implant CAD model of printing needed for opening,
The printing of dentistry implant biscuit is completed under shaping software control, biscuit is dried, degreasing, tooth is obtained after high temperature sintering
Section's planting body.
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