CN109574657A - A method of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology - Google Patents
A method of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology Download PDFInfo
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Abstract
The present invention relates to a kind of methods for preparing dental zirconium oxide prosthesis based on Stereo Lithography Apparatus Rapid Prototyping technology, it include: that zirconia ceramics powder, dispersing agent are added in light-cured resin premixed liquid by (1), photoinitiator ball milling again is added after abundant ball milling, obtains ceramic slurry；(2) ceramic slurry is placed in vacuum desiccator and vacuumizes exclusion bubble, then carry out 3D printing；By the cleaning of obtained dental zirconium oxide prosthesis, dry, then progress degreasing, sintering, finally dyeing, glazing.Present invention process is simple, quick and convenient, high production efficiency, while solving the problems, such as that traditional machining production technology waste of raw materials is serious；The dental zirconium oxide prosthesis density being prepared is high, and high mechanical strength meets the clinical requirement of oral restoration, has a good application prospect.
Description
Technical field
The invention belongs to dental restorative areas, in particular to a kind of to prepare dentistry based on Stereo Lithography Apparatus Rapid Prototyping technology
The method of zirconium oxide prosthesis.
Background technique
Dental zirconium oxide all-ceramic prosthesis intensity height, color and stereovision are good, and biocompatibility is splendid, represents no metal
Change the main trend repaired, is the development trend of 21 century dental prosthetic.Cooperate the CAD/CAM technology to reach its maturity at present, it is right
In advance at zirconium oxide porcelain block carry out numerical control cutting molding, obtain designed dummy (corona, bridge).Over 20 years, this skill
Art continues to develop, and reaches its maturity, has clinically obtained extensive and good application, has very vast market prospect.
However for zirconium oxide all-ceramic prosthesis Digital manufacturing, there was only a kind of forming method of numerical control cutting at present,
Although there is also some drawbacks using very successful.For example, due to being subtraction manufacture, therefore the serious (utilization rate of waste of raw materials
Less than 20%), that cutting may cause material internal micro-crack, the abrasion of cutter, processing efficiency is not high, in the process of processing and manufacturing
It will cause a large amount of dust to cause environmental pollution and cause damages to human health.
The third time industrial revolution just occurring with we, with the rapid development of 3D printing technique, to medical instrument system
The influence made is more and more big, especially the Digital manufacturing of mouth mending material.It is complex-shaped due to mouth mending material, it is typical
Personalized customization product, be particularly suitable for the 3D printing straight forming based on increasing material manufacturing method.By it is this with the addition method at
The Digital manufacturing that the three-dimensional printing technology of type is applied to dental zirconium oxide all-ceramic prosthesis ceramic member is also increasingly subject to both at home and abroad
The concern of scholar, has been increasingly becoming research hotspot.Compared to Computerized Numerical Control processing technology, it has high stock utilization, environmental protection, processing effect
The features such as rate is high has good feasibility and application prospect.
From it is existing research from the point of view of, be mainly the following three-dimensional printing technology be attempted it is complete applied to dental zirconium oxide
The Digital manufacturing of Porcelain veneer.1. traditional 3 D-printing (3DP) is to spread one layer of ceramic powders on the table, then count again
Under the control of calculation machine instruction, binder is selectively ejected into ceramic powders surface, this layer of powder bonding aftertable is downward
The mobile and new powder of layer overlay repeats appeal step and finally obtains expected stereoscopic member, and the advantage of this technology is
Ceramic component can be mass produced, cost is relatively low, but since strength of parts is limited, it is difficult to meet clinical requirement.2. selection
Property laser sintered (SLS) principle it is similar to 3 D-printing, binder is only changed into high-intensitive laser, is set along computer
The path point by point scanning powder surface of meter, scanning area ceramic particle melts and mutually melting generates good bonding, by layer
Layer superposition obtains final component, and the part not being sintered becomes the support construction of sintering part, because being supported without designing,
But since the sintering temperature of ceramic powder itself is higher, it is difficult to the melting connection immediately under the laser scanning of short time, therefore
Need to promote by addition low melting point binder the effect of laser melting, ceramic powders need pre- hot and cold in print procedure
But, molding cycle is long, and subsequent treatment process is complicated and is unable to get highdensity ceramic product.3. direct inkjet printing (DIP)
It is that ceramic powders and various organic matters and additive are first prepared by mixing into ceramic slurry, is ejected on carrier point by point by spray head
Ceramic raw embryo is formed, the moulding mechanism of this technology is simple, and the cost of printing device is relatively low, but the size of shower nozzle caliber limits
The precision of printing is made, and since ceramic slurry viscosity is larger, has been easy blocking spray head.4. micro- extruding rapid shaping (SME) is
Configured ceramic slurry is passed through into syringe needle direct extrusion molding, then its mechanical strength, this technology are improved by drying and sintering
There is unique advantage in terms of printing microcellular structure, and be not suitable for the printing of highdensity zirconium oxide prosthesis.
Stereo Lithography Apparatus Rapid Prototyping (SLA) is that ceramic powders are mixed into liquid photosensitive resin and are formed to have certain fluidity
Ceramic slurry, selectively solidified by ultraviolet laser, the ceramic green printed obtains final pottery by degreasing sintered
Porcelain component, this technology formed precision is high, the ceramic component of high compaction can be obtained after sintering, especially suitable for zirconium oxide reparation
The production of body.Currently, the Stereo Lithography Apparatus Rapid Prototyping technology of ceramic material has had in fields such as aviation, industry, art
More mature application still since dental zirconium oxide Ceramic restorations have higher requirement to its intensity and precision, is such as made
The base ceramic for making four units and the above dummy of four units needs to reach 800Mpa, hat marginal no more than 120um,
The technology can be used for mouth mending material production also in the Primary Study stage.
Summary of the invention
Technical problem to be solved by the invention is to provide one kind to prepare dentistry based on Stereo Lithography Apparatus Rapid Prototyping technology
It is raw both to have solved traditional machining for the method for zirconium oxide prosthesis, this method simple process, quick and convenient, high production efficiency
The serious problem of production. art waste of raw materials, and it is able to satisfy clinical requirement.
The present invention provides a kind of method for preparing dental zirconium oxide prosthesis based on Stereo Lithography Apparatus Rapid Prototyping technology,
Include:
(1) zirconia ceramics powder, dispersing agent are added in light-cured resin premixed liquid, light is added after abundant ball milling and draws
Agent ball milling again is sent out, ceramic slurry is obtained；Wherein, percent by volume of the zirconia ceramics powder in light-cured resin premixed liquid
Be 40~55%, light-cured resin premixed liquid by 70~85:10 of mass ratio~20:5~10 photosensitive resin, reactive diluent and
Plasticizer composition；
(2) ceramic slurry is placed in vacuum desiccator and vacuumizes exclusion bubble, then carry out 3D printing；The tooth that will be obtained
The cleaning of section's zirconium oxide prosthesis green compact, dry, then progress degreasing, sintering, finally dyeing, glazing.
Zirconia ceramics in the step (1) is tetragonal phase zirconium oxide ceramics, infiltration glass Zirconia reinforced alumina
One or more of ceramics, partial stabilization zirconium oxide ceramic, nano zircite, zirconium oxide/alumina composite ceramic.
Photosensitive resin in the step (1) is (methyl) acrylate, polyester acrylate, polyether acrylate, gathers
One or more of urethane acrylate, Epoxy Resin Acrylate, acrylamide, vinyl ethers.
Reactive diluent in the step (1) is butyl acrylate, Isooctyl acrylate monomer, hydroxy-ethyl acrylate, propylene
One or more of sour hydroxypropyl acrylate, phenoxyethyl acrylate.
Plasticizer in the step (1) be one of acrylamide, polyethylene glycol, glycerol, hydroxymethyl cellulose or
It is several.
Dispersing agent in the step (1) is polyacrylamide, polyacrylic acid, Sodium Polyacrylate, hydroxymethyl cellulose, gathers
One or more of vinyl alcohol, additional amount are the 0.5~3% of zirconia ceramics powder quality.
Photoinitiator in the step (1) is benzyl dimethyl ketal, 1- hydroxycyclohexyl phenyl ketone, 2,4,6- tri-
One of methyl benzoyl diphenyl phosphine oxide, 2- benzyl -2- dimethylamino -1- (4- morpholinyl phenyl) butanone are several
Kind, additional amount is the 0.5~3% of photosensitive resin quality.
The preparation of light-cured resin premixed liquid: by photosensitive resin, reactive diluent and plasticizer in mass ratio in ball mill
Middle ball milling to get arrive light-cured resin premixed liquid.Wherein, ball milling speed be 150~350r/min, Ball-milling Time be 30~
60min.。
Ball milling speed in the step (1) is 150~350r/min, and Ball-milling Time is 12~36h (ball milling condition twice
It is identical).
Vaporization temperature in the step (2) is room temperature, and the pumpdown time is 30~60min.
The 3D printer that 3D printing uses in the step (2) is Stereo Lithography 3D ceramic printer.
Specific step is as follows for 3D printing: obtaining abutment three-dimensional data by optical scanner, is repaired using CAD design personalization
Complex, it is contemplated that the initial three-dimensional data of dummy need to suitably be amplified, amplified threedimensional model is input to by sintering shrinkage
3D printer terminal uses above-mentioned ceramic slurry printing shaping.
95~99% alcohol washes are used in the step (2)；Drying temperature is room temperature, drying time is 12~for 24 hours.
Skimming temp in the step (2) is 500~600 DEG C, 2~3h of soaking time, 0.3~0.5 DEG C of heating rate/
min；1350~1550 DEG C of sintering temperature, 2~3h of soaking time, 5~10 DEG C/min of heating rate.
The coloring agent and porcelain powder that dyeing, glazing in the step (2) use are matched for the common zirconium oxide of dental laboratory
Cotton up to powder, such as VITA, adopted Huojia County, loose wind brand.
Beneficial effect
Present invention process is simple, quick and convenient, high production efficiency, while solving traditional machining production technology former material
Material wastes serious problem；The dental zirconium oxide prosthesis density being prepared is high, and high mechanical strength meets facing for oral restoration
Bed requires, and has a good application prospect.
Detailed description of the invention
Fig. 1 is the three-point bending resistance intensity for the ceramic test piece that different print conditions obtain in embodiment 1；
Fig. 2 is the three-point bending resistance intensity of the ceramic test piece obtained under optimal print conditions in embodiment 1；
Fig. 3 is the zirconium oxide all-ceramic crown photo that embodiment 2 prints；
Fig. 4 is the gap replicated between hat inner surface and abutment obtained by embodiment 2 using silicon rubber.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) preparation of light-cured resin premixed liquid: by 1,6 hexanediol diacrylate, butyl acrylate and polyethylene glycol
Ball milling, revolving speed 300r/min, time are 30min to get pre- to light-cured resin to 70:20:10 in mass ratio in the ball mill
Mixed liquid；
(2) preparation of ceramic slurry: tetragonal phase zirconium oxide ceramic powder, polyacrylamide are added in step (1)
In light-cured resin premixed liquid, percent by volume of the zirconia ceramics powder in light-cured resin premixed liquid is 49%, poly- third
The additional amount of acrylamide is the 0.5% of powder quality, and benzyl dimethyl ketal ball milling again, photoinitiator are added after abundant ball milling
Additional amount be the 0.5% of acrylate quality, obtain that quality is uniform, the moderate ceramic slurry of mobility；Wherein, ball milling twice
Rate is 200r/min, and Ball-milling Time is 12h；
(3) degasification: the ceramic slurry in step (2) is placed in vacuum desiccator and vacuumizes exclusion bubble at room temperature
30min；
(4) it prints: using CAD design 30mm × 5mm × 1.7mm bar shaped test specimen, threedimensional model is input to 3D printer
Terminal, using above-mentioned ceramic slurry according to following table technological parameter printing shaping；
(5) it is cleaned and dried: printed dummy green compact is taken out, dried at room temperature for 24 hours with 95% alcohol washes；
(6) degreasing sintered: dry dummy green compact being put into sintering furnace and carry out degreasing sintered, skimming temp 500
DEG C, soaking time 2h, 0.3 DEG C/min of heating rate, 1350 DEG C of sintering temperature, soaking time 2h, 5 DEG C/min of heating rate obtain
To the ceramic test piece sintered；
(7) performance detection: the three-point bending resistance intensity of ceramic test piece is detected, as a result as shown in Figure 1.
(8) each each horizontal signal-to-noise ratio of parameter is calculated, optimal procedure parameters group is obtained and is combined into laser power 0.45W, is scanned
Speed 750mm/s, sweep span 25um.
(9) using optimal procedure parameters combination printing ceramic test piece obtained by step (8), after cleaning, dry, sintering, test
Its 3 bending strengths are 978.05Mpa, reach national peak demand standard, as a result as shown in Figure 2.Shrinking percentage has been measured simultaneously
Be it is long by 17.70%, wide by 18.83%, high by 23.22%, density is up to 98.42%.
Embodiment 2
(1) preparation of light-cured resin premixed liquid: by 1,6 hexanediol diacrylate, butyl acrylate and polyethylene glycol
Ball milling, revolving speed 300r/min, time are 30min to get pre- to light-cured resin to 70:20:10 in mass ratio in the ball mill
Mixed liquid；
(2) preparation of ceramic slurry: tetragonal phase zirconium oxide ceramic powder, polyacrylamide are added in step (1)
In light-cured resin premixed liquid, percent by volume of the zirconia ceramics powder in light-cured resin premixed liquid is 49%, poly- third
The additional amount of acrylamide is the 0.5% of powder quality, and benzyl dimethyl ketal ball milling again, photoinitiator are added after abundant ball milling
Additional amount be the 0.5% of acrylate quality, obtain that quality is uniform, the moderate ceramic slurry of mobility；Wherein, ball milling twice
Rate is 200r/min, and Ball-milling Time is 12h；
(3) degasification: the ceramic slurry in step (2) is placed in vacuum desiccator and vacuumizes exclusion bubble at room temperature
30min；
(4) it prints: abutment three-dimensional data being obtained by optical scanner, using CAD design individualized therapy body, length is put
1.21 times big, width amplifies 1.22 times, and highly enlarged 1.27 times, amplified threedimensional model is input to 3D printer terminal,
Use above-mentioned ceramic slurry printing shaping；
(5) it is cleaned and dried: printed dummy green compact is taken out, dried at room temperature for 24 hours with 95% alcohol washes；
(6) degreasing sintered: dry dummy green compact being put into sintering furnace and carry out degreasing sintered, skimming temp 500
DEG C, soaking time 2h, 0.3 DEG C/min of heating rate, 1350 DEG C of sintering temperature, soaking time 2h, 5 DEG C/min of heating rate obtain
To the dental polishing dummy sintered；
(7) it dyes glazing: putting and dry under heat lamps after selecting corresponding staining reagent according to patient's colorimetric, then
Glazing is carried out with porcelain powder, is sintered in porcelain furnace, finally obtains high performance dental zirconium oxide Ceramic restorations, as shown in Figure 3.
(8) as shown in figure 4, being using the marginal of silicon rubber gap replica method detection zirconia ceramics dummy
109.33um meeting clinical requirement.
Claims (9)
1. a kind of method for preparing dental zirconium oxide prosthesis based on Stereo Lithography Apparatus Rapid Prototyping technology, comprising:
(1) zirconia ceramics powder, dispersing agent are added in light-cured resin premixed liquid, photoinitiator is added after abundant ball milling
Ball milling again obtains ceramic slurry；Wherein, percent by volume of the zirconia ceramics powder in light-cured resin premixed liquid is 40
~55%, light-cured resin premixed liquid is by 70~85:10 of mass ratio~20:5~10 photosensitive resin, reactive diluent and plasticising
Agent composition；
(2) ceramic slurry is placed in vacuum desiccator and vacuumizes exclusion bubble, then carry out 3D printing；The dentistry oxygen that will be obtained
Change the cleaning of zirconium dummy green compact, dry, then progress degreasing, sintering, finally dyeing, glazing.
A kind of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology 2. according to claim 1
Method, it is characterised in that: the zirconia ceramics in the step (1) is tetragonal phase zirconium oxide ceramics, the increasing of infiltration glass zirconium oxide
One of tough aluminium oxide ceramics, partial stabilization zirconium oxide ceramic, nano zircite, zirconium oxide/alumina composite ceramic are several
Kind.
A kind of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology 3. according to claim 1
Method, it is characterised in that: photosensitive resin in the step (1) be acrylate, polyester acrylate, polyether acrylate,
One or more of urethane acrylate, Epoxy Resin Acrylate, acrylamide, vinyl ethers；Reactive diluent is
One of butyl acrylate, Isooctyl acrylate monomer, hydroxy-ethyl acrylate, hydroxypropyl acrylate, phenoxyethyl acrylate or
It is several；Plasticizer is one or more of acrylamide, polyethylene glycol, glycerol, hydroxymethyl cellulose.
A kind of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology 4. according to claim 1
Method, it is characterised in that: the dispersing agent in the step (1) is polyacrylamide, polyacrylic acid, Sodium Polyacrylate, methylol
One or more of cellulose, polyvinyl alcohol, additional amount are the 0.5~3% of zirconia ceramics powder quality.
A kind of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology 5. according to claim 1
Method, it is characterised in that: photoinitiator in the step (1) be benzyl dimethyl ketal, 1- hydroxycyclohexyl phenyl ketone,
One in 2,4,6- trimethyl benzoyl diphenyl base phosphine oxide, 2- benzyl -2- dimethylamino -1- (4- morpholinyl phenyl) butanone
Kind is several, and additional amount is the 0.5~3% of photosensitive resin quality.
A kind of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology 6. according to claim 1
Method, it is characterised in that: the ball milling speed in the step (1) is 150~350r/min, and Ball-milling Time is 12~36h.
A kind of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology 7. according to claim 1
Method, it is characterised in that: the vaporization temperature in the step (2) is room temperature, and the pumpdown time is 30~60min.
A kind of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology 8. according to claim 1
Method, it is characterised in that: 95~99% alcohol washes are used in the step (2)；Drying temperature is room temperature, and drying time is
12~for 24 hours.
A kind of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology 9. according to claim 1
Method, it is characterised in that: the skimming temp in the step (2) is 500~600 DEG C, 2~3h of soaking time, heating rate 0.3
~0.5 DEG C/min；1350~1550 DEG C of sintering temperature, 2~3h of soaking time, 5~10 DEG C/min of heating rate.
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