KR101873570B1 - Dental prosthetic restorative material manufacturing method - Google Patents

Abstract

The present invention relates to a manufacturing method of a dental prosthetic and restorative material. The purpose of the technical realization is to provide a manufacturing method of a dental prosthetic and restorative material which can greatly improve handling and use functionality by making a polymerizable monomer stably passed through and combined to the inside of a ceramic block body, increasing density of a ceramic block body which is an inorganic filler, and making excellent aesthetic and high mechanical strength such as bending strength, tensile strength, or the like improved in comparison with a conventional dental composite resin accordingly. Therefore, a specific means of the present invention for achieving the purpose performs: a ceramic shaped object pretreatment process which is composed of a ceramic coating step and a ceramic block body shaping step; a monomer mixture creating process which is composed of a resin mixture forming step and a polymerization initiator mixing step; a monomer passing through and combining process which is composed of a monomer natural absorption step and a monomer absorption accelerating step; and a monomer polymerization and hardening process which is composed of a photopolymerization reaction step and a thermal polymerization step.

Description

TECHNICAL FIELD The present invention relates to a dental prosthetic restorative material manufacturing method,

The present invention relates to a dental prosthesis restorative material for use in a dental CAD / CAM system, and more particularly to a prosthodontic restoration material made of a ceramic formed body, To a dental prosthesis repair material, and to a method for manufacturing a dental prosthesis repair material.

Prosthetic treatment is needed to restore teeth that have been lost or damaged when teeth are lost due to gum disease or tooth decay, or when teeth and surrounding tissues are damaged by an external impact caused by an accident or the like.

The dental prosthetic restorative biomaterial is usually used for dental prosthesis restoration. Here, the term biomaterial for restoration of dental prosthesis refers to a restoration of the dental caries or the esthetics and functions of damaged or missing teeth It refers to dental prosthetic & restorative materials that are biocompatible.

Regarding the prosthetic restorative materials, natural materials such as animal bones or woods have been mainly used before the development of the conventional science and technology. However, today, as science and technology have developed, materials such as metals, ceramics, polymers, It is developed and used.

In choosing prosthetic restorative materials, the most important considerations are: first, there should be no risk to the human body; second, to endure repetitive workloads in the mouth; and third, to be able to reproduce the color of natural teeth That is, biocompatibility, functionality, and aesthetics are required to be very high.

However, all of the above biocompatibility, functionality, and aesthetic properties can not be satisfied with any one material. Therefore, it is possible to combine materials each having a unique type characteristic to satisfy such an expectation.

As an example of a prosthetic restorative material made of a composite material, a dental composite resin for direct restoration is usually made of an acrylic or methacrylic system having a high molecular weight multi-functional group, various kinds of inorganic filler, a radiation- And a composite resin polymer composed of a polymerization promoter, an additive such as a UV stabilizer, an antioxidant, a pigment, and a fluorescent agent.

Since the mechanical properties and biocompatibility of the composite resin polymers are greatly influenced by the polymerization conversion of the monomers, the composition of the photoinitiator and the polymerization accelerator used in the photopolymerizable resin by UV light This is very important.

Examples of the photoinitiator include diketone, coumarin, acylphosphine oxide, and the like. The photoinitiators include diketone camphorquinone (CQ) and acylphosphine oxide Ethyl (2,4,6-trimethylbenzoyl) phenylphosphinate (Ethyl (2,4,6-tribenzoylphopshinate) is mainly used. As a polymerization accelerator for efficiently performing photopolymerization in a short time, aldehyde (2H-Benzotriazol-2-yl) 4,6-dihydroxybenzoate (EDMAB) as a UV stabilizer, and a tertiary amine system such as ethyl 4-dimethylaminophenoxide -ditertpentylphenol is mainly used, and barium, strontium, lanthanum, titanium, zirconium and the like are used as the radiopaque metal component.

However, as the inorganic filler which occupies 40 to 85 wt% of the total amount and the filling ratio of the inorganic filler, the filler used for the composite resin has the largest influence on the mechanical properties such as the flexural strength and tensile strength of the composite resin polymer, (MAFC), fine particle type (MIFC), ultra fine particle type (NFC) and hybrid type (HFC) depending on the size of the composite resin. The mechanical properties of the composite resin are different depending on the particle size of the filler used in the composite resin. .

The macromolecular composite resin having a relatively large average particle size of 10 to 100 탆 of filler has excellent mechanical properties, but has a disadvantage in that the surface roughness and surface roughness are increased during the final treatment, resulting in deterioration of the aesthetic effect.

The ultrafine particle type composite resin using a fine silica-based filler having an average particle size of about 0.04 μm has a smooth surface of the prosthesis restoration material, a small surface roughness, less contamination due to stains, plaque, etc., The surface area of the inorganic filler is very large and the viscosity is increased, so that the filler content is limited and the mechanical properties such as bending strength and weather resistance are deteriorated. In order to simultaneously exhibit the two advantages of large particle type (MAFC) and ultrafine particle type (NFC), it is possible to consider a prosthetic restorative of mixed particle (HFC)

Meanwhile, in recent years, in addition to the above-described prosthetic restorative materials, a technique for machining the prosthesis according to the development of a device for processing the prosthesis restorative material, that is, introduction of a CAD / CAM system for dental use, It is a fact that repeatedly.

For example, in recent years, there has been an increase in the use of digital impression methods using an intraoral camera in the treatment of prosthesis, and the use of wax, composite resin, polymethyl methacrylate (PMMA) (CAD / CAM) system by changing it according to the characteristics of the dental CAD / CAM system.

Currently, the ceramic material, which is mainly processed and manufactured as a prosthesis by a CAD / CAM system for dental use, is zirconia. Such zirconia has high mechanical strength of a flexural strength of 1000 MPa or more, There is a problem that the stability of the material is deteriorated due to a phenomenon such as shrinkage which occurs during high-temperature sintering.

In addition, in the case of an all-ceramic tube made of zirconia ceramics, there is a limitation in application of the anterior portion of the oral cavity due to low transparency. In addition to the risk of fracture due to the brittleness of the ceramic itself, .

Alternatively, the sintered zirconia may be sintered at a high temperature for a long period of time in order to remove the incorporated chemical components and to crystallize the sintered zirconia in a zirconia block, There is an inefficient and uneconomical problem that unnecessary facility investment costs, waste of energy resources due to the use of the equipment, and excessive manufacturing time of the prosthesis are required.

On the other hand, as a material partially complementary to the disadvantages of the above-mentioned zirconia ceramics, a polymer composite resin which uniformly mixes polymers and ceramics and cures by photopolymerization in a patient's mouth is used in clinical practice.

However, since polymer composite resins have a low elastic modulus, they are easy to process and unlike zirconia ceramics, sintering is not required, so that the manufacturing process of the prosthesis can be simplified. On the other hand, compared with the zirconia ceramics, , There is a problem that unexpected physical occlusion such as color change and strength deterioration is caused due to leakage of monomer that has been polymerized due to aging caused by wet oral environment.

Therefore, taking into consideration the advantages of ceramic and composite resin, it is possible to facilitate fabrication in dental CAD / CAM system, as well as to improve the physical properties such as the aesthetic superiority of the composite resin and the mechanical strength of the ceramic The development of dental prosthetic restorative materials made of hybrid ceramics, for example, is left as an urgent challenge.

Accordingly, the present invention has been made to solve the general problems of a conventional prosthetic restoration material manufacturing method that is processed by a CAD / CAM system for dentistry.

An object of the present invention is to stably penetrate and bond a mixture containing a polymerizable monomer in a ceramic block body to increase the content of the inorganic filler to increase the density of the ceramic block body, And a method for manufacturing a dental prosthesis restoration material by which the esthetics and the high mechanical strength, for example, the flexural strength, the tensile strength and the like are increased, thereby greatly improving handling and usability.

The object of the present invention is to prevent the discoloration and mechanical strength deterioration caused by the conventional composite resin through the introduction of a minimal amount of monomer and to offset the brittle defects of the prosthesis during oral chewing, And a method for manufacturing a dental prosthesis restoration material that can extend the service life of the prosthesis extremely.

It is also an object of the present invention to provide a dental CAD / CAM system for preventing fracture, chipping, cracking, and the like during cutting and molding of a prosthetic material (prosthetic restoration material) using a dental CAD / CAM system, Thereby minimizing the thickness of the machinable prosthesis, thereby greatly improving the machinability of the dental prosthesis restoration.

In order to achieve the above object, according to the present invention, there is provided a method of manufacturing a dental prosthesis repair material,

In order to achieve the above object, according to the present invention, there is provided a method of manufacturing a dental prosthesis repair material,

A ceramic coating step comprising a ceramic coating step and a ceramic block body forming step;

A resin mixture forming step, and a polymerization initiator mixing step;

A monomer permeation bonding step comprising a monomer natural absorption step and a monomer absorption promotion step;

Then, a monomer polymerization curing step consisting of a photopolymerization reaction step and a thermal polymerization reaction step is carried out.

As described above, the method for manufacturing a dental prosthesis restoration material according to the present invention stably penetrates and binds a mixture containing a polymerizable monomer in a ceramic block body using capillary phenomenon, thereby increasing the density of the ceramic block body, As well as the mechanical strength, thereby providing an effect of greatly improving the handling property and the use function.

In addition, the method of manufacturing a dental prosthesis restoration material according to the present invention prevents discoloration or deterioration of mechanical strength through the application of a minimum amount of applicable monomers, and also eliminates brittle defects of the prosthesis during oral chewing, The durability of the dental patient is improved, and the service life of the dental prosthesis is also prolonged.

Alternatively, the method of manufacturing a dental prosthesis restoration material according to the present invention prevents fracture, chipping and cracking of the prosthesis material (prosthetic restorative material) using a dental CAD / CAM system due to its improved mechanical strength So that the thickness of the machinable prosthesis can be minimized, thereby greatly improving the workability. This provides a very useful anticipatory effect.

1 is a flowchart of an integrated process of a method for manufacturing a dental prosthesis restoration material according to the present invention

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of a dental prosthetic restoration material manufacturing method according to the present invention will be described in detail with reference to the accompanying drawings.

With reference to the accompanying drawings, a schematic configuration of a method of manufacturing a dental prosthetic restoration according to the present invention will be described.

This is composed of a preforming step (S1) of a ceramic formed body, a monomer mixture producing step (S2), a monomer permeation bonding step (S3), and a monomer polymerization curing step (S4).

In the method construction of the present invention, the first ceramic formed body preprocessing step (S1) includes a step of preparing a material serving as a foundation of the dental prosthesis restoration material according to the present invention, For example, in the process of forming a ceramic formed body, the preforming process S1 of the ceramic formed body may include a ceramic coating step S1-1, a ceramic block forming step S1-2, As shown in FIG.

At this time, in the above-described preform processing step (S1) of the ceramic formed body, the ceramic coating step (S1-1) is a step of coating a ceramic powder having an average particle size of 0.2 to 5 탆, An inorganic pigment and a fluorescent agent may be further mixed so that the ceramic of the powder having the nano particle size is mixed at a ratio of 1: 1 and the aesthetic property is similar to the natural value according to the purpose of use. And a silane coupling agent, for example, a kind of a crosslinking agent component serving as an intermediate contact for bonding two or more different materials is added to the mixed powdery ceramic to coat the surface of the powdery ceramic Process.

The powder ceramic having an average particle diameter of 0.2 to 5 탆 according to the present invention may be a barium boroaluminosilicate glass, a strontium boroaluminosilicate glass, a fluoroaluminium silicate glass, Among various inorganic particles such as a fluoroaluminosilicate glass, a glass including zirconia, a glass including a stone lentium, a Lanthanum glass and the like, a barium boroalumino silicate glass, Nano powder ceramics using inorganic particles of a strontium boroaluminosilicate glass component and having a particle size of 100 nm or less can be produced by spray pyrolysis of fumed alumina or fumed silica Fumed silica, or its composite oxides, And silane coupling agents are prepared by reacting a silane coupling agent of a methacryloxypropyl trimethoxysilane component having a methacryloxy functional group among silane coupling agents of various components coupling agents are preferably used.

Alternatively, the above-described ceramic coating step (S1-1) may be carried out by two optional coating methods, for example, in the case of coating the mixed ceramic with different particle diameters in the form of an average particle size and a nano particle size , A mixture of distilled water 5% and ethanol 95% was adjusted to pH 4.5 to 5 with acetic acid, ceramic was added to disperse the dispersion, silane coupling agents were added in an amount of 2% , Followed by rinsing with ethanol twice or more, and then drying the mixture at a temperature of 90 to 110 캜 for 5 to 60 minutes by vacuum distillation.

1% of water was added to the ceramic particles to be used as an inorganic filler, and the mixture was allowed to stand in a sealed container at a temperature of 50 to 70 ° C for 8 hours, and then put into an industrial mixer (not shown) to rotate at a high speed. And a dry coating method in which silane coupling agents are spray-applied to perform a coating treatment.

In the ceramic molded body preprocessing step S1 described above, the ceramic block body forming step S1-2 is a step of forming the ceramic formed through the ceramic coating step S1-1 into a mold having a predetermined size and capacity , And then pressing the ceramic block body by a compression press (not shown) to mold the ceramic block body.

At this time, the pressing of the ceramic block body by the compression press is performed by press-molding the ceramic block at a temperature of 30 to 90 MPa for 1 to 30 minutes by using a uniaxial press-forming press (not shown) And then the primary press-molded ceramic block body is secondarily press-molded at a pressure of 100 to 300 MPa for 1 to 60 minutes by using a cold isostatic press (not shown) to form a ceramic block body.

Meanwhile, in the method construction of the present invention, the second monomer mixture producing step (S2) is a step of preparing a mixture containing a polymerizable monomer for charging into a ceramic formed body, (S2) is preferably composed of a resin mixture forming step (S2-1) and a polymerization initiator mixing step (S2-2), as shown in Fig.

At this time, in the monomer mixture producing step (S2), the resin mixture forming step (S2-1) may include a diluent such as triethylene glycol dimethacylate, an antioxidant, And the mixture is stirred until the components are completely dissolved and mixed. Then, the dissolved mixture is mixed with bisphenol A glycidyl methacrylate or urethane dimethacrylate used for the dental composite resin, Acrylate (urethane dimethacrylate), and stirring the mixture for 1 to 12 hours to form a resin mixture.

Further, in the above monomer mixture producing step (S2), the polymerization initiator mixing step (S2-2) is a step of mixing the resin mixture formed through the resin mixture forming step (S2-1) with the acylphosphine used in the dental composite resin A photopolymerization initiator such as acylphosphine oxide or diketone and a thermal polymerization initiator such as an organic peroxide or an azo compound are further added thereto and stirred for 1 to 24 hours by an industrial mixer (not shown) . At this time, a photopolymerization accelerator such as tertiary amine may be added for efficient photopolymerization in a short time.

At this time, in the monomer mixture producing step (S2) described above, the polymerization initiator mixing step (S2-2) is a step of mixing the thermal polymerization initiator and the photopolymerization initiator into the resin mixture and mixing the resin mixture with an industrial vacuum mixer And the bubbles are prevented from being generated by stirring the photopolymerization initiator and the photopolymerization initiator in such a state that the vacuum is maintained by the industrial vacuum mixer.

In the method construction of the present invention, the third monomer permeation bonding step (S3) is a step of mixing the ceramic formed body prepared through the above-mentioned preform processing step (S1) It is preferable that the monomer permeation bonding step (S3) includes a monomer natural absorption step (S3-1) and a monomer absorption promotion step (S3-2).

At this time, in the monomer permeation bonding step (S3), the monomer natural absorption step (S3-1) is carried out by immersing the monomer block in the monomer mixture produced through the mixture preparation step (S2) The ceramic block body immersed in the mixture is kept at room temperature for 3 to 10 days in an industrial vacuum chamber reactor (not shown), and the monomer mixture is introduced into the inside of the ceramic block body (fine pores inside the block body) So as to be absorbed.

In the above-described monomer permeation bonding step (S3), the monomer absorption promotion step (S3-2) is preferably a step (S3-1) of neutralizing the inside of the vacuum dark room reactor, And the monomer mixture is absorbed by vacuum evaporation. The ceramic block body having the monomer mixture absorbed therein is vacuum-packed, and then the mixture is vacuum-packed with a pressure of 100 to 300 MPa for 1 to 30 minutes And a pressure is applied to accelerate the absorption of the monomer.

 Finally, the aforementioned monomer polymerization curing step (S4) is a step of forming a single ceramic formed body, that is, a prosthetic restoration material, completed by a stepwise polymerization reaction. Such a monomer polymerization curing step (S4) (S4-1) and a thermal polymerization reaction step (S4-2).

At this time, in the above monomer polymerization curing step (S4), the photopolymerization reaction step (S4-1) is a step of reacting the polymerizable monomer produced through the monomer permeation bonding step (S3), for example, A UV light source of 370 nm to 420 nm is irradiated from the photopolymerization reactor under the state of being put in an industrial photopolymerization reactor (not shown), and the ceramic molded body is exposed to the irradiated UV light source in the range of 1 to 30 minutes, Followed by polymerization.

In the above monomer polymerization curing step (S4), the thermal polymerization reaction step (S4-2) is a step in which the ceramic molded body subjected to the photopolymerization reaction step (S4-1) is again placed in an industrial thermal polymerization reactor (Not shown), thermally curing the mixture by heating at a temperature ranging from 60 to 250 ° C. for 1 to 24 hours, and then thermally treating the cured ceramic molded body at a temperature of 90 to 160 ° C. for 1 to 3 hours, And a post-treatment process to alleviate the stress.

Therefore, as described above, a series of step-by-step processes, that is, a ceramic molded body pre-processing step (S1) The method for producing a dental prosthesis restoration material according to the present invention is implemented by proceeding to a sequential flow process (S2), a monomer permeation bonding step (S3), and a monomer polymerization curing step (S4).

S1: Pretreatment process of ceramic compact
S1-1: Ceramic coating step
S1-2: Ceramic block body molding step
S2: Monomer mixture production process
S2-1: resin mixture forming step
S2-2: polymerization initiator mixing step
S3: Monomer penetration bonding process
S3-1: Monomer natural absorption step
S3-2: Monomer absorption promotion step
S4: Monomer polymerization curing process
S4-1: photopolymerization reaction step
S4-2: Thermal polymerization step

Claims (5)

A powder ceramic having an average particle diameter of 0.2 to 5 mu m and a ceramic having a nanoparticle diameter of 100 nm or less were mixed and silane coupling agents were added to the mixed ceramic with different particle diameters to prepare a ceramic surface (S1-1);
A ceramic block preforming step (S1) comprising a ceramic block body forming step (S1-3) of charging the ceramic into a mold and pressurizing it with a compression press to form a ceramic block body;
A diluent, an antioxidant and an ultraviolet light stabilizer are mixed and dissolved in a solvent to form a solution of bisphenol A glycidyl methacrylate and urethane dimethacrylate A resin mixture forming step (S2-1) of adding a raw material and stirring and mixing for 1 to 12 hours;
A monomer mixture producing step (S2) of further adding a thermopolymerization initiator and a photopolymerization initiator to the resin mixture thus formed and stirring the mixture for 1 to 24 hours by an industrial mixer (S2-2);
The ceramic block body immersed in the monomer mixture is immersed in the monomer mixture produced in the monomer mixture production step (S2). The ceramic block body immersed in the monomer mixture is kept in a vacuum dark room reactor at room temperature for 3 to 10 days, A monomer natural absorption step (S3-1) for causing the monomer to be naturally absorbed into the ceramic block body;
In the monomer natural absorption step (S3-1), a monomer absorption promoting step (S3-2) for promoting the absorption of the monomer mixture by repeatedly changing the internal space environment of the dark room vacuum reactor to atmospheric pressure and vacuum twice or more A monomer permeation bonding step (S3);
A photopolymerization reaction step (S4-1) of putting the ceramic formed body infiltrated with the monomer mixture into a photopolymerization reactor to cause the cause of cracks in the ceramic formed body to be canceled by exposure to a UV light source;
The ceramic molded body subjected to the photopolymerization reaction step is placed in a thermal polymerization reactor and thermally cured at a temperature of 60 ° C to 250 ° C for 1 to 20 hours to thermally polymerize the thermally polymerized ceramic molded body for 1 to 3 hours at 90 to 160 ° C And a monomer polymerization curing step (S4) comprising a thermal polymerization reaction step (S4-2) of heat-treating the dental prosthesis.
The method of claim 1, further comprising:
In the ceramics coating step (S1-1), a mixed solution of 5% of distilled water and 95% of ethanol is adjusted to pH 4.5 to 5 with acetic acid, and the mixture is added to and dispersed in ceramic. Silane coupling agents are further added thereto in an amount of 2% or more and stirred for 1 to 3 hours, followed by rinsing with ethanol twice or more. The mixture is distilled under reduced pressure, Lt; RTI ID = 0.0 > g / min < / RTI >
1% water was added to ceramic particles to be used as an inorganic filler, and the mixture was allowed to stand in a sealed container at a temperature of 50 to 70 ° C for 8 hours. Then, the mixture was put into an industrial mixer, rotated at a high speed, and a silane coupling agent wherein the coating layer is formed by spraying a coating agent onto a surface of the dental prosthesis.
The method of claim 1, further comprising:
In the ceramic block body preprocessing step (S1), the ceramics block body forming step (S1-3) is a step of charging ceramics into a mold and pressing the ceramic block at a temperature of 30 to 90 MPa for 1 to 30 minutes for 1 to 30 minutes using a uniaxial press- Car press forming;
Further comprising the step of subjecting the first press-molded ceramic to a secondary press forming at a pressure of 100 to 300 MPa for 1 to 60 minutes using a cold isostatic pressing.
The method of claim 1, further comprising:
In the monomer mixture producing step (S2), the polymerization initiator mixing step (S2-1) is a step of mixing the thermoplastic polymerization initiator and the photopolymerization initiator into the resin mixture by using an industrial vacuum mixer, So that air bubbles are not generated. The method for manufacturing a dental prosthesis restoration material according to claim 1,
The method of claim 1, further comprising:
In the monomer polymerization curing step (S4), the photopolymerization reaction step (S4-1) is a step of irradiating a UV light source of 370 to 420 nm from the photopolymerization reactor, irradiating the irradiated UV light source with the ceramic molded body for 1 to 30 minutes Wherein the dental prosthesis is made to be exposed to the dental prosthesis.

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