CN106747430A - A kind of resin penetration 3Y TZP composites and preparation method thereof - Google Patents
A kind of resin penetration 3Y TZP composites and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of the resin penetration 3Y TZP composites for gear division reparation, comprise the following steps：(1) according to relative mass ratio, 3Y TZP and ErO are weighed2And carry out being mixed to get mixed material；(2) mixed material is ground and obtains precursor powder；(3) precursor powder is pressed into biscuit of ceramics through tablet press machine；(4) biscuit of ceramics through isostatic cool pressing suppress obtaining ceramic body；(5) ceramic body is put into sintering furnace the ceramic body for being sintered and obtaining pre-sintering；(6) according to relative mass ratio, bisphenol-A glycerine dimethacrylate and three (ethylene glycol) dimethylacrylates are weighed and carries out being mixed to get mixed solution；(7) a certain amount of benzoyl peroxide addition mixed solution is carried out being mixed to get hybrid resin；(8) in the pre-sintered ceramic body immersion hybrid resin, will be put into vacuum environment and permeate, obtain the ceramics of infiltration resin；(9) ceramics of the infiltration resin are put into baking oven and are solidified, obtain resin penetration ceramic composite.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of resin penetration 3Y-TZP for gear division reparation is answered
Condensation material and preparation method thereof.
Background technology
Oral health is closely bound up with national life quality.According to World Health Organization's recent statistics, mouth disease is arranged
It is the third-largest disease after cancer and cranial vascular disease.Research display, the illness rate of the various stomatopathys of China is up to
97.6%, it is concentrated mainly on the stomatopathys such as carious tooth and periodontitis.According to Third National oral health epidemiological investigation result,
China human mortality caries incidence is 40%, and each patient is averagely related to 2-3 tooth.As population structure aging and people are to life
The raising of quality requirement, the demand of oral restoration treatment and the just rapid expansion of research.It is presently used for the composite of gear division reparation
Research formd a direction with important research and Practical significance, while developing advanced composite material (ACM) and technique is closed
It is also current materials of bone tissue research emphasis into optimization.
Ceramic material and composite combination CAD/CAM technologies are being widely used in gear division reparation field in recent years.It is main at present
There is ceramic material of two classes for gear division reparation, be respectively：Glass ceramics and polycrystalline ceramics.(Li R.W.K..,et.al,
J.Prosthodont.Res., 2014,58,208-216) glass ceramics, such as Lithium silicate glass ceramics, although with excellent
Biocompatibility and aesthetic properties, but fragility is big, mechanical property is poor.And the polycrystalline with higher intensity and toughness is made pottery
Porcelain, such as alumina-based ceramic or 3Y-TZP bases ceramics, with the defect that opaque, hardness and modulus are too high.Repaiied for gear division
Multiple material, it is opaque, mean that aesthetic properties are poor, in order to make up this defect, would generally be outside ceramics during reparation
Layer is plus decorations porcelain.But decorations porcelain poor mechanical property and poor with the binding ability of dummy, finally easily cause and entirely repair
The failure of body.The hardness of polycrystalline ceramics is typically 2-4 times of enamel, and the repair materials of too high hardness will wear and tear surrounding
Natural tooth, damages to natural tooth.Secondly, the Young's modulus of dentine is 20-25GPa in human teeth, much low
In 3Y-TZP (200GPa) and the Young's modulus of aluminum oxide (340-390GPa).This significant difference will repair material to power
Transmission in material and natural tooth adversely affects (Ziskind D., et.al, J.Struct.Biol., 2011,174,23-
30；White S.N.,et.al,J.Prosthet.Dent.,2005,94,125-131；Mangalaraja R.V.,et.al,
Mater.Sci.Eng.A,2003,343,71-73)。
In order to mechanical property is preferably combined together with aesthetic properties, composite is introduced into gear division and repaiies in 1960s
Multiple field, and afterwards people be devoted to improving always they performance (Ferracane J.L., et.al,
Dent.Mater.,2005,21,36-42).However, be far smaller than the intermolecular bond distance between monomer due to the bond distance of covalent bond,
Inorganic particle toughened resin based composites have significant shrinkage after hardening.This distinctive shrinkage is compound
Residual stress can be introduced in material repair process, so as to cause repair materials to depart from dummy, resin base is seriously limited and is combined
The extensive use (Ferracane J.L., et.al, Dent.Mater., 2011,27,29-38) of material.
Resin two-phase of the resin penetration ceramic composite by porous ceramic network structure and infiltration wherein is constituted, this
Plant the shrinkage that structure overcomes conventional particles toughened resin based composites.And can make such composite has ceramics
High intensity, high tenacity and resin material attractive in appearance, low modulus advantage.
The content of the invention
It is an object of the invention to provide a kind of resin penetration 3Y-TZP (Tetragonal for gear division reparation
Zirconia Polycrystals stabilized with 3mol%Y2O3) composite and preparation method thereof.
A kind of preparation method of resin penetration 3Y-TZP composites for gear division reparation provided by the present invention, including
Following steps：
(1) according to relative mass ratio, 3Y-TZP and ErO is weighed2And carry out being mixed to get mixed material；
(2) mixed material is ground and obtains precursor powder；
(3) precursor powder is pressed into biscuit of ceramics through tablet press machine；
(4) biscuit of ceramics through isostatic cool pressing suppress obtaining ceramic body；
(5) ceramic body is put into sintering furnace the ceramic body for being sintered and obtaining pre-sintering；
(6) according to relative mass ratio, bisphenol-A glycerine dimethacrylate and three (ethylene glycol) dimethyl allenes are weighed
Acid esters simultaneously carries out being mixed to get mixed solution；
(7) a certain amount of benzoyl peroxide addition mixed solution is carried out being mixed to get hybrid resin；
(8) in the pre-sintered ceramic body immersion hybrid resin, will be put into vacuum environment and permeate, obtain infiltration tree
The ceramics of fat；
(9) ceramics of the infiltration resin are put into baking oven and are solidified, obtain resin penetration ceramic composite.
In above-mentioned preparation method, the ErO2Mass fraction be 0.1~0.4wt%.
In above-mentioned preparation method, the wet-milling being ground to alcohol as abrasive media, the rotating speed of grinding can be
250rpm~500rpm, the time of the wet-milling can be 2h~24h.
In above-mentioned preparation method, be dried for the precursor powder after being additionally included in step (2) by methods described
The step of.
In above-mentioned preparation method, the dry temperature is 50 DEG C~80 DEG C, and drying time is 2h~24h.
In above-mentioned preparation method, the pressure of described tablet press machine compacting biscuit can be 2MPa~10MPa.
In above-mentioned preparation method, the pressure of described isostatic cool pressing can be 150MPa~220MPa.
In above-mentioned preparation method, the pre-sintering temperature is 1000 DEG C~1150 DEG C, and the time is 2h~4h.
In above-mentioned preparation method, bisphenol-A glycerine dimethacrylate described in step (6) and three (ethylene glycol) diformazans
The mass ratio of base acrylate is 1:1.
In above-mentioned preparation method, mass fraction of the benzoyl peroxide in mixed solution is described in step (7)
0.5wt.%~2wt.%.
In above-mentioned preparation method, time of penetration described in step (8) is 2h~24h.
In above-mentioned preparation method, solidification temperature described in step (9) be 50 DEG C~100 DEG C, hardening time be 2h~
24h。
The present invention still further provides the resin penetration 3Y-TZP for gear division reparation prepared by the above method and be combined
Material；By compound 3Y-TZP ceramics and resin material, gained composite is existing compared with high bending strength, fracture toughness, while
Remain to maintain relatively low consistency and elasticity modulus, be new gear division repair composite material that a class has broad prospect of application.
The invention has the advantages that：Compared with conventional particles toughened resin composite, harmful consolidating is overcome
Change shrinkage, with high bending strength, high-fracture toughness, relatively low hardness and relatively low elastic modelling quantity, mechanical property with from
Right tooth is close.
Brief description of the drawings
Fig. 1 is the resin penetration 3Y-TZP/ErO that embodiment of the present invention 1-5 is sequentially prepared2Composite photo.
Fig. 2 is the resin penetration 3Y-TZP/ErO that embodiment of the present invention 1-5 is sequentially prepared2Composite materials property figure.
Specific embodiment
Below in conjunction with the accompanying drawings, the present invention is described in more detail.
Experimental technique used in following embodiments is conventional method unless otherwise specified.
Material used, reagent etc. in following embodiments, unless otherwise specified, commercially obtain.Embodiment
1st, resin penetration 3Y-TZP composites are prepared
A certain amount of 3Y-TZP is weighed, powder is inserted in ball grinder, add absolute ethyl alcohol to carry out ball as ball-milling medium
Mill, rotational speed of ball-mill is 250rpm, and the time is 10h, obtains precursor powder；The precursor powder is dried into 24h in 70 DEG C；With pressure
Precursor powder is compressed to biscuit by piece machine, and pressure is 4MPa, and the dwell time is 3min；Made pottery using isostatic cool pressing compacting 3Y-TZP
Porcelain biscuit, pressure is 220MPa, and the dwell time is 1min；Ceramic body is carried out into pre-sintering, sintering temperature in air atmosphere
It it is 1150 DEG C, soaking time is 2h.It is 1 by mass ratio:1 bisphenol-A glycerine dimethacrylate and three (ethylene glycol) two
Methacrylate is mixed, and 2h is stirred using magnetic agitation；Curing agent benzoyl peroxide 0.5wt% is added above-mentioned mixed
Continue to stir 2h in resin；By in pre-sintered ceramics immersion resin solution, it is placed in vacuum environment, permeates 4h；Will infiltration
The material of resin solidifies in being placed on vacuum drying oven, and solidification temperature is 70 DEG C, and hardening time is 2h, obtains resin penetration 3Y-TZP and answers
Condensation material.
As shown in embodiment 1 in Fig. 1, its color is chalk color to the photo of sample prepared by the embodiment as known in the figure,
Differed farther out with natural color of teeth.
The mechanical property of sample prepared by the embodiment is as shown in embodiment 1 in Fig. 2.At 1150 DEG C, without doping ErO2
Under, up to 240.3 ± 17.4MPa, hardness is 3.1 ± 0.2GPa to its bending strength, and elastic modelling quantity is 58.8 ± 2.0GPa.
Embodiment 2, prepare resin penetration 3Y-TZP composites
Weigh a certain amount of 3Y-TZP, ErO2, the ErO2Content 0.1wt.%, powder is inserted in ball grinder, adds nothing
Water-ethanol carries out ball milling as ball-milling medium, and rotational speed of ball-mill is 250rpm, and the time is 10h, obtains precursor powder；By the forerunner
Body powder dries 24h in 70 DEG C；Precursor powder is compressed to biscuit with tablet press machine, pressure is 4MPa, and the dwell time is 3min；
3Y-TZP biscuit of ceramics is suppressed using isostatic cool pressing, pressure is 220MPa, and the dwell time is 1min；By ceramic body in air gas
Pre-sintering is carried out under atmosphere, sintering temperature is 1150 DEG C, and soaking time is 2h.It is 1 by mass ratio:1 bisphenol-A glycerine dimethyl
Acrylate and three (ethylene glycol) dimethylacrylates are mixed, and 2h is stirred using magnetic agitation；By curing agent peroxidating
Benzoyl 2wt% continues to stir 2h in adding above-mentioned hybrid resin；By in pre-sintered ceramics immersion resin solution, vacuum is placed in
In environment, 4h is permeated；The material of infiltration resin is placed in vacuum drying oven and is solidified, solidification temperature is 70 DEG C, and hardening time is 2h,
Obtain resin penetration 3Y-TZP composites.
The embodiment prepare sample photo as shown in embodiment 2 in Fig. 1, as known in the figure its color be it is faint yellow,
It is close with natural color of teeth.
The mechanical property of sample prepared by the embodiment is as shown in embodiment 2 in Fig. 2.At 1150 DEG C, adulterate 0.1wt.%
ErO2Under, up to 213 ± 13.1MPa, hardness is 3.38 ± 0.9GPa to its bending strength, and elastic modelling quantity is 60.9 ± 9.8GPa.
Embodiment 3, prepare resin penetration 3Y-TZP composites
Weigh a certain amount of 3Y-TZP, ErO2, ErO2Content 0.2wt.%, powder is inserted in ball grinder, adds anhydrous second
Alcohol carries out ball milling as ball-milling medium, and rotational speed of ball-mill is 250rpm, and the time is 10h, obtains precursor powder；By the precursor
End dries 24h in 70 DEG C；Precursor powder is compressed to biscuit with tablet press machine, pressure is 4MPa, and the dwell time is 3min；Utilize
Isostatic cool pressing suppresses 3Y-TZP biscuit of ceramics, and pressure is 220MPa, and the dwell time is 1min；By ceramic body in air atmosphere
Pre-sintering is carried out, sintering temperature is 1150 DEG C, and soaking time is 2h.It is 1 by mass ratio:1 bisphenol-A glycerine dimethyl allene
Acid esters and three (ethylene glycol) dimethylacrylates are mixed, and 2h is stirred using magnetic agitation；By curing agent benzoyl peroxide first
Acyl 1wt% continues to stir 2h in adding above-mentioned hybrid resin；By in pre-sintered ceramics immersion resin solution, vacuum environment is placed in
In, permeate 4h；The material of infiltration resin is placed in vacuum drying oven and is solidified, solidification temperature is 70 DEG C, and hardening time is 2h, is obtained
Resin penetration 3Y-TZP composites.
The embodiment prepare sample photo as shown in embodiment 3 in Fig. 1, as known in the figure its color be it is faint yellow,
It is close with natural color of teeth.
The mechanical property of sample prepared by the embodiment is as shown in embodiment 3 in Fig. 2.At 1150 DEG C, adulterate 0.1wt.%
ErO2Under, up to 200 ± 20.4MPa, hardness is 2.4 ± 0.7GPa to its bending strength, and elastic modelling quantity is 42.3 ± 3.7GPa.
Embodiment 4, prepare resin penetration 3Y-TZP composites
Weigh a certain amount of 3Y-TZP, ErO2, ErO2Content 0.3wt%, powder is inserted in ball grinder, adds anhydrous second
Alcohol carries out ball milling as ball-milling medium, and rotational speed of ball-mill is 250rpm, and the time is 10h, obtains precursor powder；By the precursor
End dries 24h in 70 DEG C；Precursor powder is compressed to biscuit with tablet press machine, pressure is 4MPa, and the dwell time is 3min；Utilize
Isostatic cool pressing suppresses 3Y-TZP biscuit of ceramics, and pressure is 220MPa, and the dwell time is 1min；By ceramic body in air atmosphere
Pre-sintering is carried out, sintering temperature is 1150 DEG C, and soaking time is 2h.It is 1 by mass ratio:1 bisphenol-A glycerine dimethyl allene
Acid esters and three (ethylene glycol) dimethylacrylates are mixed, and 2h is stirred using magnetic agitation；By curing agent benzoyl peroxide first
Acyl 1.5wt% continues to stir 2h in adding above-mentioned hybrid resin；By in pre-sintered ceramics immersion resin solution, vacuum ring is placed in
In border, 4h is permeated；The material of infiltration resin is placed in vacuum drying oven and is solidified, solidification temperature is 70 DEG C, and hardening time is 2h, is obtained
To resin penetration 3Y-TZP composites.
The embodiment prepare sample photo as shown in embodiment 4 in Fig. 1, as known in the figure its color be it is faint yellow,
It is close with natural color of teeth.
The mechanical property of sample prepared by the embodiment is as shown in embodiment 4 in Fig. 2.At 1150 DEG C, adulterate 0.3wt.%
ErO2Under, up to 178 ± 25MPa, hardness is 5.3 ± 0.3GPa to its bending strength, and elastic modelling quantity is 87 ± 4.5GPa.
Embodiment 5, prepare resin penetration 3Y-TZP composites
Weigh a certain amount of 3Y-TZP, ErO2, ErO2Content 0.4wt%, powder is inserted in ball grinder, adds anhydrous second
Alcohol carries out ball milling as ball-milling medium, and rotational speed of ball-mill is 250rpm, and the time is 10h, obtains precursor powder；By the precursor
End dries 24h in 70 DEG C；Precursor powder is compressed to biscuit with tablet press machine, pressure is 4MPa, and the dwell time is 3min；Utilize
Isostatic cool pressing suppresses 3Y-TZP biscuit of ceramics, and pressure is 220MPa, and the dwell time is 1min；By ceramic body in air atmosphere
Pre-sintering is carried out, sintering temperature is 1150 DEG C, and soaking time is 2h.It is 1 by mass ratio:1 bisphenol-A glycerine dimethyl allene
Acid esters and three (ethylene glycol) dimethylacrylates are mixed, and 2h is stirred using magnetic agitation；By curing agent benzoyl peroxide first
Acyl 0.8wt% continues to stir 2h in adding above-mentioned hybrid resin；By in pre-sintered ceramics immersion resin solution, vacuum ring is placed in
In border, 4h is permeated；The material of infiltration resin is placed in vacuum drying oven and is solidified, solidification temperature is 70 DEG C, and hardening time is 2h, is obtained
To resin penetration 3Y-TZP composites.
The embodiment prepare sample photo as shown in embodiment 5 in Fig. 1, as known in the figure its color be it is faint yellow,
It is close with natural color of teeth.
The mechanical property of sample prepared by the embodiment is as shown in embodiment 5 in Fig. 2.At 1150 DEG C, adulterate 0.4wt.%
ErO2Under, up to 153 ± 21MPa, hardness is 2.3 ± 0.3GPa to its bending strength, and elastic modelling quantity is 38 ± 3.5GPa.
Above-described embodiment has been described in detail to technical scheme.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiment in the present invention, those skilled in the art can also accordingly make various changes, but appoint
What is equal to the present invention or similar change belongs to the scope of protection of the invention.
Claims (10)
1. the preparation method of a kind of resin penetration 3Y-TZP composites for gear division reparation, it is characterised in that including as follows
Step：
(1) according to relative molar proportions, 3Y-TZP and ErO is weighed2And carry out being mixed to get mixed material；
(2) mixed material is ground and obtains precursor powder；
(3) precursor powder is pressed into biscuit of ceramics through tablet press machine；
(4) biscuit of ceramics through isostatic cool pressing suppress obtaining ceramic body；
(5) ceramic body is put into sintering furnace the ceramic body for being sintered and obtaining pre-sintering；
(6) according to relative mass ratio, bisphenol-A glycerine dimethacrylate and three (ethylene glycol) dimethylacrylates are weighed
And carry out being mixed to get mixed solution；
(7) a certain amount of benzoyl peroxide addition mixed solution is carried out being mixed to get hybrid resin；
(8) in the pre-sintered ceramic body immersion hybrid resin, will be put into vacuum environment and permeate, obtain infiltration resin
Ceramics；
(9) ceramics of the infiltration resin are put into baking oven and are solidified, obtain resin penetration ceramic composite.
2. preparation method according to claim 1, it is characterised in that ErO described in step (1)2Mass fraction be 0.1
~0.4wt%.
3. preparation method according to claim 1, it is characterised in that it is grinding to be ground to described in step (2) with alcohol
The wet-milling of medium, the rotating speed of grinding is 250rpm~500rpm, and the wet-milling time is 2h~24h.
4. preparation method according to claim 1, it is characterised in that methods described is additionally included in institute after step (2)
The step of stating precursor powder and be dried, the dry temperature is 50 DEG C~80 DEG C, and drying time is 2h~24h.
5. preparation method according to claim 1, it is characterised in that：Tablet press machine described in step (3) suppresses the pressure of biscuit
Power is 2MPa~10MPa.
6. preparation method according to claim 1, it is characterised in that：The pressure of isostatic cool pressing is described in step (4)
150MPa~220MPa.
7. preparation method according to claim 1, it is characterised in that：Pre-sintering temperature described in step (5) is 1000 DEG C
~1150 DEG C, the time is 2h~4h.
8. preparation method according to claim 1, it is characterised in that：Bisphenol-A glycerine dimethyl allene described in step (6)
The mass ratio of acid esters and three (ethylene glycol) dimethylacrylates is 1:1；Benzoyl peroxide described in step (7) is in mixing
Mass fraction in solution is 0.5wt%~2wt%.
9. preparation method according to claim 1, it is characterised in that：Time of penetration described in step (8) is 2h~24h,
Solidification temperature described in step (9) is 50 DEG C~100 DEG C, and hardening time is 2h~24h.
10. the resin penetration 3Y-TZP composites for gear division reparation that in claim 1-9 prepared by any methods described.
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