CN108578250B - Resin-permeable silicate composite material and preparation and application thereof - Google Patents
Resin-permeable silicate composite material and preparation and application thereof Download PDFInfo
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- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
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Abstract
The invention relates to a resin-impregnated silicate composite material, which is prepared by curing components comprising resin and glass phase silicate in the presence of a curing agent; wherein the resin comprises bisphenol A glycidyl dimethacrylate and tetraethylene glycol dimethacrylate. The invention also relates to a preparation method of the resin-impregnated silicate composite material, which prepares the porous ceramic block by controlling the sintering temperature and the heat preservation time, then the resin is permeated into the porous ceramic block body through vacuum capillary action, and then the porous ceramic block body is solidified to form the silicate/resin dual network structure. The resin-impregnated silicate composite material provided by the invention has high mechanical property and aesthetic property, and has great development potential and wide market prospect in the aspect of dental restoration application.
Description
Technical Field
The invention belongs to the technical field of composite materials for dental restoration, and particularly relates to a resin-permeable silicate composite material, and preparation and application thereof.
Background
Investigation data shows that the total population of caries patients in our country is about 6 hundred million, about 80% of teenagers suffer from various dental diseases, and an average of 2 to 3 teeth are involved in each patient. With the enhancement of the human's self-health consciousness, there is a growing trend in the need for dental restoration. In people not suffering from dental diseases, the need for restoration of teeth for aesthetic considerations (smile reconstruction) is also increasing with the day. With the improvement of the living standard of people, the requirements on the aesthetic properties of dental restoration materials are also increasing.
The main repair materials currently exist: metal alloys, all-ceramic, ceramic deposited metals and composite resins. Metals have high mechanical properties but poor aesthetic properties and biocompatibility. In recent years, some countries in europe have definitely banned silver amalgam and other materials for dental restoration. The all-ceramic repairing material has higher mechanical property and aesthetic property, but has poorer machinability, is more sensitive to cracks and has poor capability of bearing tensile stress, the defects easily cause early failure of all-ceramic repairing, and the original teeth are worn due to the excessively high hardness of ceramic. Ceramic deposited metal attempts to combine the advantages of metal and ceramic, but mismatch in thermal conductivity and modulus is a major cause of its early failure. In recent years, with the increasing demand for aesthetic properties, the enhancement of the consciousness of the original teeth, and the deep concept of minimally invasive restoration, composite resin restoration materials are becoming the main restoration materials. Reducing shrinkage stress, prolonging service life, improving mechanical properties and biocompatibility are major challenges of applying the composite resin to dental restorative materials.
The use of resin-based composites is a significant advancement in dental restorations. Bowen R L reported a combination of epoxy resin and silica particles as dental restorations (Bowen R L.use of epoxy resins in restorative materials J Dent Res,1956,35 (3): 360-369). In its subsequent work (US 3179623), an important monomer Bis-GMA was developed that became the backbone of the dental restoration composite, after which it was continuously used.
Dental repair materials are classified according to the repair mode, and can be classified into direct repair materials and indirect repair materials, and the classification standard mainly aims at resin matrix composite materials. Because of the low mechanical properties and polymeric shrinkage of direct restorative composites, indirect restorative composites have become the first choice for dentists and patients at present. With the development of computer aided design and computer aided manufacturing, indirect repair of composite materials has undergone tremendous revolution. Computer aided design and computer aided manufacturing are increasingly more tightly coupled with indirect repair composites, which are therefore also known as CAD/CAM blocks.
In terms of mechanical properties, the dental restoration material reaches the consensus that the dental restoration material industry is equivalent to dentin. Some mechanical properties of enamel and dentin are listed in table 1. Two commercially available dental restorative materials that are currently in very wide use are the Vita Enamic product of Vita corporation and the Lava Ultimate product of 3M ESPE corporation. The bending strength of Vita Enamic is 150-160 MPa, the difference between the bending strength and dentin is larger, and the bending strength of 3M ESPE is (204+ -19) MPa, and the bending strength is close to the lower limit of dentin bending strength, but has a certain difference. The elastic modulus of Vita Enamic is 30GPa, which is already greater than dentin; lava Ultimate has an elastic modulus of (12.77.+ -. 0.99) GPa, lower than dentin. The vickers hardness of Vita Enamic was 2.5GPa,3M ESPE Lava Ultimate and (1.15±0.13) GPa, both values were between dentin and enamel.
Table 1 some mechanical properties of dentin and enamel
In terms of aesthetic properties, achieving translucency or transparency of dental restoration composites is of paramount importance. On the one hand, the edge of the primary enamel presents a semitransparent state, and the semitransparent dental restoration composite material is closer to the enamel. Translucent dental restoration composites, on the other hand, facilitate staining according to the color of the native teeth of different people. The colors of Vita Enamic and Lava Ultimate are similar to those of the original teeth, but their transparency is to be improved.
Therefore, the problem at present is that research and development of a resin-permeable silicate composite material, a preparation method thereof and application thereof in dental restoration are urgently needed.
Disclosure of Invention
The invention aims to solve the technical problem of providing a resin-permeable silicate composite material, and a preparation method and application thereof. The inventor of the invention conducts extensive and intensive test research in the technical field of composite materials for dental restoration, and discovers that a partially sintered porous ceramic block is prepared by controlling sintering temperature and heat preservation time, resin is infiltrated into the partially sintered porous ceramic block through vacuum capillary action, and then a silicate/resin dual network structure is formed through curing reaction. The composite material prepared by the method effectively combines the advantages of resin and ceramic, and has higher mechanical property and aesthetic property.
To this end, a first aspect of the present invention provides a resin-infiltrated silicate composite material prepared by curing components comprising a resin and a glassy silicate in the presence of a curing agent; wherein the resin comprises bisphenol A glycidyl dimethacrylate (Bis-GMA) and tetraethylene glycol dimethacrylate (TEGDMA).
In some embodiments, the mass ratio of resin, glass phase silicate to curing agent is 1 (0.75-4.0): 0.005-0.02.
In some preferred embodiments, the mass ratio of bisphenol A diglycidyl dimethacrylate to tetraethyleneglycol dimethacrylate is (1-4): 1, more preferably (1-2): 1.
In some embodiments, the glass phase silicate is selected from one or more of fumed silica, aluminum silicate, sodium silicate, potassium silicate, magnesium silicate, calcium silicate, barium silicate, and zirconium silicate.
In other specific embodiments, the curing agent is selected from one or more of benzoyl peroxide, cumene peroxide, and methyl ethyl ketone peroxide.
In a second aspect, the present invention provides a method for preparing a composite material according to the first aspect of the present invention, comprising:
step A, performing ball milling and drying treatment on glass phase silicate, and performing molding and sintering treatment on the obtained powder to obtain porous ceramic blocks;
step B, penetrating resin containing curing agent into the porous ceramic block to obtain a block with sufficient resin penetration;
and step C, curing the block body with sufficient resin permeation to obtain the resin permeation silicate composite material.
In some specific embodiments, in step a, the ball-milled abrasive is zirconia balls; the ball milling treatment speed is 100-350r/min; the ball milling treatment time is 12-24 hours; the temperature of the drying treatment is 50-90 ℃.
According to some specific embodiments, in step a, the shaping treatment comprises compression molding and cold isostatic pressing.
According to some specific embodiments, the pressure of the compression molding is 2-4MPa and the dwell time is 1-3min.
According to other specific embodiments, the cold isostatic pressure is 150-220MPa and the dwell time is 1.5-2min.
In the present invention, the magnitude of the cold isostatic pressure will affect the hardness and modulus of the composite material. Controlling the pressure of the cold isostatic pressure may result in a final prepared composite material having a higher hardness and modulus.
According to some specific embodiments, in step a, the sintering process is performed at a gradually increasing temperature, the temperature increase rate of the sintering process being between 5 and 10 ℃/min; the heat preservation temperature of the sintering treatment is 550-850 ℃, and the heat preservation time of the sintering treatment is 1min-2h.
In the invention, the sintering temperature and the heat preservation time can influence the porosity and the pore structure, thereby finally influencing the mechanical property of the composite material. The porosity of the finally formed composite material is low by controlling the sintering and heat preservation time, the pore morphology tends to be round, and therefore the higher the elastic modulus and the hardness of the prepared composite material are.
According to some specific embodiments, in the step a, when the adhesion of the powder is poor, the step D is further included to mix the binder with the powder before the powder forming process.
In some preferred embodiments, the mass ratio of the binder to the powder is (0.01-0.1): 1.
In other preferred embodiments, the binder is present in a concentration of 0.5 to 10wt%.
In still other more preferred embodiments, the binder is selected from one or more of an aqueous polyvinyl alcohol solution, an aqueous starch solution, an aqueous dextrin solution, and an aqueous carboxymethyl cellulose solution.
According to some specific embodiments, in step B, the infiltration is performed under vacuum conditions at a pressure (-0.01) - (-0.1) MPa; the infiltration time is 1-48h.
According to some specific embodiments, in step C, the curing process is vacuum curing; the temperature of the vacuum solidification is 70-110 ℃; the time of vacuum curing is 8-16h.
In some preferred embodiments, in step C, the curing process is performed in two steps at different temperatures. For example, the curing treatment is first performed at a low temperature of 70 to 90 ℃ (inclusive of the case of 90 ℃ C.) and then at a high temperature of 90 (exclusive of the case of 90 ℃ C.) to 110 ℃ C. For a total time of 8 to 16 hours. The curing rate can be improved by adopting stepwise curing.
In some embodiments, the method of preparing the resin-infiltrated silicate composite material comprises the steps of:
(1) Mixing glass phase silicate and a solvent according to a mass ratio of 1:10 to prepare a solid-liquid mixture; preferably, the solvent is ethanol or deionized water;
(2) Injecting the solid-liquid mixture into a ball milling tank for ball milling treatment, wherein zirconia balls are adopted as abrasive materials, the ball milling speed is 100-350r/min, and the ball milling time is 12-24h, so as to prepare ball-milled powder;
(3) Drying the ball-milled powder at 50-90 ℃ for 24 hours to obtain dried powder;
(4) Mixing the dried powder with a binder to obtain a powder containing the binder; the mass ratio of the binder to the dried powder is (0.01-0.1): 1;
(5) Pressing the powder containing the binder into a blank by adopting a compression molding die, wherein the compression molding pressure is 2-4MPa, the pressure maintaining time is 1-3min, and then demolding to obtain the blank after compression molding;
(6) Placing the blank after compression molding in an oil pressure environment for cold isostatic pressing treatment, wherein the pressure of the cold isostatic pressing is 150-220MPa, and the pressure maintaining time is 1.5-2min, so as to prepare the blank after cold isostatic pressing;
(7) Sintering the blank subjected to cold isostatic pressing into a porous ceramic block at a gradually increased temperature, wherein the heating rate is 5-10 ℃/min, and the heat preservation time is 1-2 h; the heat preservation temperature is 550-850 ℃;
(8) Adding 0.5-2.0 wt% (based on the total mass of bisphenol A dimethacrylate and tetraglycol dimethacrylate) of a curing agent to a resin mixture of bisphenol A dimethacrylate and tetraglycol dimethacrylate in a mass ratio of (1-4) 1 to prepare a resin containing the curing agent;
(9) Penetrating resin containing curing agent into porous ceramic block body, and its method is: injecting a certain amount of resin into the mould in advance, preferably 1/3 of the height of the porous ceramic block, placing the porous ceramic block in the resin, and infiltrating under the vacuum environment with the infiltration pressure of (-0.01) - (-0.1) MPa for 1-48h until the resin is fully infiltrated, so as to obtain a block with fully infiltrated resin;
(10) And (3) placing the block body with sufficient resin permeation in a vacuum condition of 70-110 ℃ for curing for 8-16h, and obtaining the cured block body which is the resin permeation silicate composite material.
In a third aspect, the present invention provides the use of a resin-infiltrated silicate composite according to the first aspect of the invention or a resin-infiltrated silicate composite prepared according to the method of the second aspect of the invention in dental restorations.
When the resin-impregnated silicate composite material provided by the invention is used for dental restoration, the surface of the resin-impregnated silicate composite material is subjected to polishing treatment. For example, the resin-rich layer of the surface of the cured block (i.e., resin-infiltrated silicate composite) is sanded with 150 mesh coarse sandpaper, and then sanded with 2000 mesh fine sandpaper and polished to produce a resin-infiltrated silicate composite for dental restoration.
The materials and reagents used in the present invention are commercially available unless otherwise specified.
Unless otherwise indicated, all methods of experimentation used in the present invention are conventional in the art.
The term "heat-retaining temperature" as used herein refers to the sintering temperature and also refers to the temperature at which the temperature rises.
The term "soak time" as used herein refers to the holding time at the sintering temperature.
The resin-impregnated silicate composite material and the preparation method thereof provided by the invention have the following advantages:
(1) The preparation method of the resin-impregnated silicate composite material provided by the invention is simple, and the technological parameters are easy to control;
(2) The resin-impregnated silicate composite material provided by the invention has higher aesthetic property, the translucency of the resin-impregnated silicate composite material is more similar to that of the edge of enamel, the resin-impregnated silicate composite material is convenient to color according to the original tooth colors of different people, and the composite material can realize continuous controllable adjustment from super translucency to opalescence;
(3) The resin-impregnated silicate composite material provided by the invention has higher bending strength, fracture toughness, moderate hardness and modulus;
(4) The resin-impregnated silicate composite material provided by the invention has great development potential and wide market prospect in the aspect of dental restoration application.
Drawings
Fig. 1 is a secondary electron image of the polished surface of the resin-infiltrated silicate composite material prepared in example 1 of the present invention.
FIG. 2 is a secondary electron plot of a cross section of a resin-infiltrated silicate composite material prepared in example 1 of the present invention.
FIG. 3 is a back-scattered electron plot of the polished face of the resin-infiltrated silicate composite material prepared in example 1 of the present invention.
FIG. 4 is a back-scattered electron plot of a cross section of a resin-infiltrated silicate composite material prepared in example 1 of the present invention.
FIG. 5 is a sample graph of a resin-infiltrated silicate composite material prepared in example 4 of the present invention.
Detailed Description
In order that the invention may be more readily understood, the invention will be described in detail below with reference to the following examples and the accompanying drawings, which are given by way of illustration only and are not limiting the scope of application of the invention.
In the present invention, bending strength was measured by using an AGS-X instrument manufactured by Shimadzu corporation. The test conditions were: the three-point bending mode was adopted, the width X height X span was 2mm X10 mm, and the loading rate was 0.5mm/min. The elastic modulus and hardness were tested in the present invention using a nanoindentation apparatus (MTS, XP, USA) with an indentation depth of 1000nm for 4 seconds.
Examples
Example 1
Weighing 20g of sodium aluminum silicate, placing into a ball milling tank, adding alcohol and zirconia balls, and ball milling for 24 hours at the rotating speed of 250 r/min. Pouring the solid-liquid mixture after ball milling into a container, and placing the container in an environment of 70 ℃ for drying, and collecting the powder. And pressing the powder into a green body by using a molding press, wherein the pressure is 3MPa, the dwell time is 3min, and the green body is completely demolded. And (3) placing the pressed blank into a rubber film, pumping out air in the rubber film by using a vacuum pump, sealing, and treating the blank by using cold isostatic pressing with the pressure of 220MPa for 1.5min. Taking out the blank after cold isostatic pressing, sintering at 550 ℃, wherein the heating rate is 5 ℃/min, and the heat preservation time is 1min, so as to prepare the partially sintered porous ceramic block. Bisphenol A dimethacrylate and tetraethylene glycol dimethacrylate were mixed in a mass ratio of 1:1, stirred for 2 hours, 2wt% (based on the total mass of bisphenol A dimethacrylate and tetraethylene glycol dimethacrylate) benzoyl peroxide was added to the above mixed solution and stirring was continued for 2 hours. The resin mixture was injected into the mold, and the liquid level was 1/3 of the block height. The partially sintered sodium aluminum silicate block was placed therein, placed in a vacuum environment, infiltrated with resin using vacuum capillary action, and held for 24 hours until the porous ceramic block was fully infiltrated. And (3) placing the ceramic block body permeated with the resin in a vacuum oven with the pressure of-0.1 MPa for curing, wherein the curing temperature is 70 ℃, and the curing time is 16 hours, so as to obtain the resin permeated silicate composite material (the mass ratio of the resin, sodium aluminum silicate and benzoyl peroxide is 1:4.0:0.02, wherein the resin is the sum of bisphenol A dimethacrylate and tetraethylene glycol dimethacrylate). The surface resin-rich layer of the cured block was ground with 150 mesh coarse sand paper, then with 2000 mesh fine sand paper, and polished with diamond polishing powder, to finally form a resin-impregnated silicate composite material for dental restoration.
The secondary electron map of the polished surface, the secondary electron map of the cross section, the back-scattered electron map of the polished surface and the back-scattered electron map of the cross section of the composite material prepared in this example are shown in fig. 1 to 4, respectively. As can be seen from FIG. 1, the surface of the composite material is free from scratches, and has good polishing performance. As can be seen from fig. 2, the resin phase and the ceramic phase in the composite material form a good bond. As can be seen from fig. 3, the composite material has good polishing properties. As can be seen from fig. 4, the resin phase and the ceramic phase in the composite material can form a good bond.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 2
The preparation method of the resin-infiltrated silicate composite material was the same as in example 1, except that the sintering temperature was 600 ℃.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 3
The preparation method of the resin-infiltrated silicate composite material was the same as in example 1, except that the sintering temperature was 650 ℃.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 4
The preparation method of the resin-infiltrated silicate composite material was the same as in example 1, except that the sintering temperature was 700 ℃.
A sample plot of the composite material prepared in this example is shown in fig. 5. As can be seen in fig. 5, the composite material exhibits a milky white color with good aesthetic properties.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 5
The preparation of the resin-infiltrated silicate composite was the same as in example 1, except that the sintering temperature was 750 ℃.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 6
The preparation method of the resin-infiltrated silicate composite material was the same as in example 1, except that the sintering temperature was 800 ℃.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 7
The preparation method of the resin-infiltrated silicate composite material was the same as in example 1, except that the sintering temperature was 850 ℃.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 8
The preparation method of the resin-infiltrated silicate composite material is the same as in example 1, except that the curing method is as follows: first at 70℃for 8 hours and then at 110℃for 8 hours.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 9
The preparation method of the resin-infiltrated silicate composite material is the same as in example 2, except that the curing method is as follows: first at 70℃for 8 hours and then at 110℃for 8 hours.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 10
The preparation method of the resin-infiltrated silicate composite material is the same as in example 3, except that the curing method is as follows: first cured at 70℃for 8 hours and then at 110℃for 8 hours.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 11
The preparation method of the resin-infiltrated silicate composite material is the same as in example 4, except that the curing method is as follows: first at 70℃for 8 hours and then at 110℃for 8 hours.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 12
The preparation method of the resin-infiltrated silicate composite material is the same as in example 5, except that the curing method is as follows: first at 70℃for 8 hours and then at 110℃for 8 hours.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 13
The preparation method of the resin-infiltrated silicate composite material is the same as in example 6, except that the curing method is as follows: first at 70℃for 8 hours and then at 110℃for 8 hours.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 14
The preparation method of the resin-infiltrated silicate composite material is the same as in example 7, except that the curing method is as follows: first at 70℃for 8 hours and then at 110℃for 8 hours.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 15
The preparation method of the resin-impregnated silicate composite material was the same as in example 4, except that the heat-retaining time was 2 hours.
The mechanical property data of the composite material prepared in this example are shown in table 1.
Example 16
The preparation method of the resin-infiltrated silicate composite material is the same as in example 1, except that the mass ratio of bisphenol A dimethacrylate to tetraethylene glycol dimethacrylate is 2:1.
Example 17
The preparation method of the resin-infiltrated silicate composite material is the same as in example 1, except that the mass ratio of bisphenol A dimethacrylate to tetraethylene glycol dimethacrylate is 3:1.
TABLE 1 mechanical Properties of resin-infiltrated silicate composites
As can be seen from Table 1, the resin-infiltrated silicate composite material prepared by the resin system of the invention has good mechanical properties (particularly higher elastic modulus and hardness) and aesthetic properties, and achieves better effects.
It should be noted that the above-described embodiments are only for explaining the present invention and do not constitute any limitation of the present invention. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function.
Claims (12)
1. A resin-impregnated silicate composite material is prepared by curing components including resin and glass phase silicate in the presence of a curing agent; wherein the resin comprises bisphenol A glycidyl dimethacrylate and tetraethylene glycol dimethacrylate; the mass ratio of bisphenol A dimethacrylate to tetraethylene glycol dimethacrylate is 1:1 or 2:1, a step of;
a method of preparing a resin-infiltrated silicate composite comprising:
step A, performing ball milling and drying treatment on glass phase silicate, and performing molding and sintering treatment on the obtained powder to obtain porous ceramic blocks;
step B, penetrating resin containing curing agent into the porous ceramic block to obtain a block with sufficient resin penetration;
step C, curing the block body with sufficient resin permeation to prepare a resin permeation silicate composite material;
the temperature rising rate of the sintering treatment is 5-10 ℃/min; the heat preservation temperature of the sintering treatment is 550-600 ℃ or 700-850 ℃, and the heat preservation time of the sintering treatment is 1min;
the mass ratio of the resin, the glass phase silicate and the curing agent is 1:4.0:0.02.
2. the composite of claim 1, wherein the glass phase silicate is selected from one or more of fumed silica, aluminum silicate, sodium silicate, potassium silicate, magnesium silicate, calcium silicate, barium silicate, and zirconium silicate;
the curing agent is selected from one or more of benzoyl peroxide, cumene peroxide and methyl ethyl ketone peroxide.
3. A method of preparing a composite material according to any one of claims 1-2, comprising:
step A, performing ball milling and drying treatment on glass phase silicate, and performing molding and sintering treatment on the obtained powder to obtain porous ceramic blocks;
step B, penetrating resin containing curing agent into the porous ceramic block to obtain a block with sufficient resin penetration;
step C, curing the block body with sufficient resin permeation to prepare a resin permeation silicate composite material;
the temperature rising rate of the sintering treatment is 5-10 ℃/min; the heat preservation temperature of the sintering treatment is 550-600 ℃ or 700-850 ℃, and the heat preservation time of the sintering treatment is 1min.
4. The method according to claim 3, wherein in the step a, the ball-milled abrasive is zirconia balls; the ball milling treatment speed is 100-350r/min; the ball milling treatment time is 12-24 hours;
the temperature of the drying treatment is 50-90 ℃.
5. The method of claim 4, wherein in step a, the molding process comprises compression molding and cold isostatic pressing;
the pressure of compression molding is 2-4MPa, and the pressure maintaining time is 1-3min;
the pressure of the cold isostatic pressing is 150-220MPa, and the pressure maintaining time is 1.5-2.0min.
6. The method according to any one of claims 3 to 5, wherein in step a, the binder and the powder are mixed before the molding treatment.
7. The method according to claim 6, wherein the mass ratio of the binder to the powder is (0.01-0.1): 1.
8. The preparation method according to claim 7, wherein the mass concentration of the binder is 0.5-10wt%.
9. The method of claim 8, wherein the binder is selected from one or more of an aqueous polyvinyl alcohol solution, an aqueous starch solution, an aqueous dextrin solution, and an aqueous carboxymethyl cellulose solution.
10. The method according to any one of claims 3 to 5, wherein in step B, the infiltration is performed under vacuum conditions at a pressure (-0.01) - (-0.1) MPa; the infiltration time is 1-48h.
11. The method according to any one of claims 3 to 5, wherein in step C, the curing treatment is vacuum curing; the temperature of the vacuum solidification is 70-110 ℃; the time of vacuum curing is 8-16h.
12. Use of a resin-infiltrated silicate composite according to any one of claims 1-2 or prepared according to the method of any one of claims 3-11 in the preparation of a dental restoration material.
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| CN112295871A (en) * | 2019-07-31 | 2021-02-02 | 共享智能铸造产业创新中心有限公司 | Technology for pressurizing and permeating reinforcer on surface of mould and container |
| CN114732742A (en) * | 2022-03-14 | 2022-07-12 | 华南理工大学 | Efficient anti-deformation streptococcus aluminum sodium silicate/nano copper oxide composite ceramic and preparation and application thereof |
| CN114712250A (en) * | 2022-03-14 | 2022-07-08 | 华南理工大学 | Crown and bridge repairing ceramic with efficient anti-deformation streptococcus and preparation and application thereof |
| CN115894001B (en) * | 2023-03-10 | 2023-05-09 | 湖南康纳新材料有限公司 | High-hardness wear-resistant resin-infiltrated ceramic composite material and preparation method and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6159417A (en) * | 1994-09-19 | 2000-12-12 | Trustees Of Boston University | Method for fabricating ceramic network material |
| EP0803241B1 (en) * | 1996-04-27 | 2006-06-14 | GC Dental Products Corporation | Dental material |
| CN106007802B (en) * | 2016-05-24 | 2019-09-17 | 清华大学 | A kind of resin penetration ceramic composite and preparation method thereof |
-
2018
- 2018-05-07 CN CN201810426620.XA patent/CN108578250B/en active Active
Non-Patent Citations (3)
| Title |
|---|
| 张克立等编.精细陶瓷的烧结.《无机合成化学》.武汉大学出版社,2012,(第2版),273-276. * |
| 李世普编.生物无机复合材料的成型、制备技术.《生物医用材料导论》.武汉工业大学出版社,2000,(第1版),209-212. * |
| 李文虎等编.多孔陶瓷材料.《材料科学与工程专业实验教程》.北京邮电大学出版社,2015,(第1版),190. * |
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