KR20230163627A - Method for manufacturing a non-metallic root canal post for dental use - Google Patents

Abstract

The present invention relates to a method of manufacturing a dental non-metallic root canal post, and more specifically, the method comprising: providing a glass fiber strand; washing and drying the glass fiber strands; Plasma treatment on the surface of the dried glass fiber strands; Treating the surface of the plasma-treated glass fiber strand with a silane coupling agent, which is an interfacial binder; Gathering a plurality of glass fiber strands that have been treated with the silane coupling agent and assembling them with light-polymerization resin in a vacuum; curing the assembled glass fiber strands into a post-shaped mold by irradiating light using a UV curing machine; It includes: marking a point to be used as a cutting point on the outer surface of the post on which the hardening has been completed.

Description

Method for manufacturing a non-metallic root canal post for dental use}

The present invention relates to a method of manufacturing a dental non-metallic root canal post, and more specifically, to a dental non-metallic post that has elasticity similar to the dentin of natural teeth, radiopacity, excellent light transparency, strong bending strength, and excellent biocompatibility. It relates to a root canal post manufacturing method.

The world is aging rapidly. The 100-year-old society has arrived, and with the rapid increase in the elderly population and improved living standards, interest in health such as U-health, health functional foods, medical tourism, and medical devices is increasing. Accordingly, the importance of dental treatment continues to increase. Treatment for tooth damage such as fractured teeth, damaged hemorrhoids, and dental caries is largely divided into implant treatment, which is an alternative method, and root canal treatment, which is a conservative method.

In the case of implants, it is a treatment method that places a great burden on patients due to the long procedure period, possible side effects after the procedure, and high costs. A root canal post is a dental medical device used after root canal treatment. Root canal treatment using a root canal post is a tooth-preserving method and has the advantage of being simpler and cheaper than implants. Compared to amalgam and core resin, it can be applied even when there are insufficient remaining teeth, and is available in a variety of materials, making it aesthetically pleasing. You can ease the burden.

Important physical properties that a root canal post must possess include an appropriate level of strength and elastic modulus to withstand stress applied to the crown of the tooth and prevent fracture of the tooth. In the case of non-metallic root canal posts, a radiopacity test is required to confirm the procedure. If a tooth fracture occurs after the procedure, corrosion caused by body fluids is a problem for metal root canal posts, so a corrosion test or cytotoxicity test is recommended.

In addition, if there is a safety problem due to an unsuitable root canal post or inappropriate procedure, a biological evaluation recommended by ISO 7405, a common standard for biological safety of medical devices or a characteristic evaluation method for dental materials, is required for the medical device or medical device material. need. Accordingly, the establishment of an evaluation method and evaluation technology that can more scientifically and objectively evaluate the physical properties and biological safety of root canal post materials is required.

The purpose of the present invention is to have strong bending strength, no corrosion, excellent biocompatibility and stability, and excellent radiation immunity in terms of the physical properties that a root canal post must have, such as root fracture, radiopacity, and biocompatibility. The purpose is to provide a dental non-metallic root canal post having transparency and light transparency.

More specifically, glass fiber is used as the main material of the non-metallic root canal post of the present invention, the composition and value of the components of the light-polymerized resin that gathers the glass fiber are limited, and the strength and wettability are improved through surface modification of the glass fiber. The purpose is to provide a dental non-metallic root canal post that improves the radiopacity, bending strength, and biostability of existing root canal posts by improving the interfacial bonding force.

The method of manufacturing a dental non-metallic root canal post of the present invention includes the steps of providing glass fiber strands; washing and drying the glass fiber strands; Plasma treatment on the surface of the dried glass fiber strands; Treating the surface of the plasma-treated glass fiber strand with a silane coupling agent, which is an interfacial binder; Gathering a plurality of glass fiber strands that have been treated with the silane coupling agent and assembling them with light-polymerization resin in a vacuum; curing the assembled glass fiber strands into a post-shaped mold by irradiating light using a UV curing machine; It includes: marking a point to be used as a cutting point on the outer surface of the post on which the hardening has been completed.

The photopolymerization resin is characterized in that it contains 15 to 30 parts by weight of monomer, 5 to 15 parts by weight of additive, 5 to 10 parts by weight of curing agent, and 5 to 9 parts by weight of inorganic filler, based on 20 to 50 parts by weight of oligomer.

The silane coupling agent is any one of 3-Methacryloxypropyltrimethoxysilane, 3-Methacryloxypropyltriethoxysilane, 3-Methacryloxypropylmethyldimethoxysilane, 3-(Acryloyloxy)propyltrimethoxysilane, 3-Aminopropyltriethoxysilane, N-2-(Aminoethyl)-3-aminopropyltrimethoxysilane, and Triethoxy(octyl)silane. More than that It is characterized by its use including.

The oligomers include Bisphenol A diglycidyl ether (BFDGE), Bisphenol A glycerolate dimethacrylate (Bis-GMA), Bisphenol A dimethacrylate (Bis-MA), Bisphenol A ethoxylated dimethacrylate (Bis-EMA), Diurethane dimethacrylate (UDMA), Diglycidyl ether of bisphenol It is characterized by containing at least one or more of A (DGEBA).

The monomer is characterized in that it contains at least one of Ethylene glycol dimethacrylate ( EGDMA ), Trimethylpropane triacrylate (TMPTA), Tetrahydrofurfuryl methacrylate (THFMA), and Glycidyl acrylate.

The curing agent is Diethylenetriamine (DETA), Triethylenetetramine (TETA), N-aminoethylpiperazine (N-AEP), m-phenylenediamine (m-PDA), 4-4'-diaminodiphenylmethane (DDM), 4-4'-diaminodiphenylsulfone (DDS) It is characterized by comprising at least one or more of the following.

The inorganic filler contains Ytterbium trifluoride and is used to improve radiopacity.

The photopolymerization resin for improving the interfacial bond with the glass fiber includes the oligomers Bisphenol A diglycidyl ether (BFDGE), Bisphenol A glycerolate dimethacrylate (Bis-GMA), Bisphenol A dimethacrylate (Bis-MA), and Bisphenol A ethoxylated dimethacrylate (Bis). -EMA), diglycidyl ether of bisphenol A (DGEBA), the additive includes dopamine, and the curing agent includes Diethylenetriamine (DETA), Triethylenetetramine (TETA), N-aminoethylpiperazine (N-AEP) , m-phenylenediamine (m-PDA), 4-4'-diaminodiphenylmethane (DDM), and 4-4'-diaminodiphenylsulfone (DDS).

In the photopolymerization resin for improving the interfacial bond with the glass fiber, the oligomer includes at least one of Propylene glycol, Ethylene glycol, Diethylene glycol, 1,4-Butadiol, Poly tetra hydrofuran, and Polypropylene glycol, and the monomer is Contains at least one of Styrene, Methyl methacrlate, Vinyl toluene, Vinyl acetate, and Ethylene glycol diacrylate, and the additives include Dibutyltin dilaurate (DBTDL), Maleic anhydride, Methacylic acid, Acrylic acid, Fumaric anhydride, 1,1,1- It contains at least one of tris(hydroxymethyl) propane, hexamethylene diisosyanate, Acetone, and dibutyltindilaurate, the curing agent contains a polyisocyanate prepolymer, and the inorganic material contains at least one of CaCO₃, zinc stearate, and magnesium oxide. Do it as

The silane coupling agent treatment involves preparing a co-solvent by diluting 85 to 95 parts by weight of N-butanol with 5 to 15 parts by weight of distilled water, and then adding 0.1 to 0.5 parts by weight of silane to prepare an aqueous silanol solution to form the glass fiber strands. It is characterized by immersion.

According to the present invention as described above, a dental non-metallic root canal post has strong bending strength, is corrosion-free, biocompatibility and stability are guaranteed, and has excellent radiopacity and light transparency. can do.

In addition, it can protect teeth by preventing root canal fracture compared to metal posts due to its elasticity similar to that of regular dentin, and has a tapered form that is easy to use in root canals, providing an aesthetically excellent dental non-metallic root canal post.

More specifically, the generation of air bubbles is reduced by plasma treatment and silane coupling treatment on the surface of the post, and the wettability of the glass fiber is improved through surface modification, increasing the interfacial bonding force between the glass fiber and the resin, thereby improving the strength of the root canal post. A non-metallic root canal post can be provided.

1 is a photograph of a dental non-metallic root canal post manufactured by the manufacturing method of the present invention.
Figure 2 is an x-ray photograph showing the radiopacity of the non-metallic dental root canal post of the present invention.
Figure 3 is a photograph showing the light transmittance of the dental non-metallic root canal post of the present invention.

The present invention relates to a method of manufacturing a non-metallic dental root canal post.

Root canal treatment or root canal treatment refers to a procedure that removes the nerve tissue of a tooth and its roots. It involves opening the occlusal area of the teeth and removing any remaining pulp. At this time, a chemical to sterilize the inside of the tooth is used to prevent infection. The inside of a root canal exposed to the outside must be filled, and a periodontal (post) may be inserted into the root canal to restore the tooth. This is a method of preserving teeth so that they can function in place.

The root canal post is a dental material that maintains and stabilizes the core by connecting the tooth root and the crown restoration after root canal treatment, buffers stress applied to the crown part, and supports the connection between the tooth root and the crown part. If caries occurs in a tooth or fracture occurs due to external shock, root canal treatment is followed as a conservative treatment method for the vital tooth. Materials used to remove the pulp of a fractured tooth and fill the expanded root canal include core resin and root canal post. Root canal post has the advantage of being applicable even when the amount of remaining tooth is not large compared to core resin. there is.

Types of root canal posts are largely divided into cast posts and prefabricated posts. Pre-formed posts can be broadly classified into metal root canal posts and non-metal root canal posts according to their components. Metal root canal post products include gold, palladium, stainless steel, and titanium. Non-metallic root canal posts include fiber-reinforced composite root canal post products reinforced with ceramic materials such as zirconia and alumina, or carbon fiber, glass fiber, and quartz fiber.

The glass fiber is hard and strong, has good deformability, does not break, and has a low density. Fiber is the main component of fiber-reinforced composite materials and occupies a large volume of the composite material. In addition, the orientation, type, amount, and size of the fiber are very important because they affect the properties of the composite material, such as specific gravity, tensile strength, elastic modulus, compressive strength, elastic modulus, fatigue strength, fatigue failure mechanism, electrical and thermal conductivity, and cost. do.

Since glass has the property of allowing light to pass through, the polymerization efficiency by light irradiation can be increased when manufacturing a root canal post, and when the post is restored to a tooth, light irradiation can be carried even to the inside. Glass is hard and brittle, made by solidifying an inorganic molten body into a solid state without crystallization upon cooling. Glass fiber is manufactured by melting and spinning such glass in a heated state.

The method of manufacturing a dental non-metallic root canal post of the present invention includes the steps of providing glass fiber strands; washing and drying the glass fiber strands; Plasma treatment on the surface of the dried glass fiber strands; Treating the surface of the plasma-treated glass fiber strand with a silane coupling agent, which is an interfacial binder; Gathering a plurality of glass fiber strands that have been treated with the silane coupling agent and assembling them with light-polymerization resin in a vacuum; curing the assembled glass fiber strands into a post-shaped mold by irradiating light using a UV curing machine; It includes: marking a point to be used as a cutting point on the outer surface of the post on which the hardening has been completed.

Steps to provide glass fiber

The diameter of the single fiber is 5㎛ to 15㎛, and each strand is provided with a plurality of glass fiber strands consisting of about 3,000 to 4,000 single fibers.

The short fibers are odorless solid fibers that do not have a specific shape or shape and have a color ranging from white to gray. It is preferable to use single fibers having a specific gravity between 2.5 and 2.55.

Washing and drying steps

To remove impurities present on the surface of the glass fiber strands, they are washed by soaking them in acetone or phosphoric acid for 20 to 40 minutes, dried at a temperature of 60°C to 80°C for 6 to 12 hours, and then left at room temperature for a day. Dry for a while.

Plasma surface treatment step

Plasma treatment is performed on the surface of the dried glass fiber strand. When the surface of a glass fiber strand is treated using plasma, active species such as radicals, ultraviolet rays, and colliding electrons in the plasma form polarity and fine irregularities on the surface of the glass fiber strand. As a result, an electrostatic charging effect occurs, improving the wettability of the glass fiber strands. If the wettability of the glass fiber strands is improved, the contact angle between the glass fiber strands with improved wettability and the resin in the bonding step is reduced, thereby improving the interfacial adhesion, thereby providing a root canal post with excellent strength.

Through the plasma surface treatment step, contaminated organic substances can be removed from the surface, and a large amount of radicals in the plasma collide with the surface of the glass fiber, causing hydrophilization. As the radicals formed on the surface are hydrophilic and contain oxygen, the wettability is improved, the surface activation energy increases, and the interfacial bond between the glass fiber strands and the resin increases.

The dried glass fiber strands are placed in a plasma reaction tank and a plasma discharge is generated. At this time, it is desirable to set the vacuum level to 0.1 to 0.5 Torr and perform plasma treatment for 1 to 10 minutes using a 7 to 14 Mhz plasma generator.

Silane coupling agent processing step

There are various methods for treating the surface of glass fiber to improve the mechanical properties of the root canal post. Silane coupling agent treatment reduces surface bubbles and improves the strength of the root canal post through chemical bonding between glass fiber strands and resin. It has an effect. The use of organic silane creates a coupling effect between organic polymers and inorganic materials, improving the interfacial adhesion of different materials.

The silane coupling agent causes hydrolysis and condensation reactions in the solvent. Generally, it has the structure of R-Si-(OR μ)n. The organofunctional group (R) reacts with organic materials to create a chemical bond, and the hydrolyzable group (OR μ) is hydrolyzed by water to produce silanol (Si). -OH) is formed to form an R-Si-(OH)n structure, and a bond is formed through a dehydration reaction with -OH of the inorganic material.

A co-solvent can be prepared and used for the silane coupling agent treatment.

A co-solvent is prepared by diluting 85 to 95 parts by weight of N-butanol with 5 to 15 parts by weight of distilled water, and then 0.1 to 0.5 parts by weight of silane is added to it, which is hydrolyzed in an acidic environment of pH 3.0 to 4.0 to form an aqueous silanol solution. It is manufactured. The most preferred method is to immerse the glass fiber strands in the silanol aqueous solution prepared in this way for 1 to 5 minutes.

The silane coupling agent is any one of 3-Methacryloxypropyltrimethoxysilane, 3-Methacryloxypropyltriethoxysilane, 3-Methacryloxypropylmethyldimethoxysilane, 3-(Acryloyloxy)propyltrimethoxysilane, 3-Aminopropyltriethoxysilane, N-2-(Aminoethyl)-3-aminopropyltrimethoxysilane, and Triethoxy(octyl)silane. Includes more than It is desirable to do so.

Light-polymerized resin assembly stage

A plurality of glass fiber strands that have been treated with the silane coupling agent are prepared and assembled with light-polymerized resin in a vacuum.

The photopolymerization resin serves to bind the glass fiber strands together, transmits external stress to the fiber, and prevents the surface of the glass fiber from being damaged by friction and abrasion. In addition, it protects against chemical reactions and separates fibers from each other to prevent cracks from propagating along the fibers.

The photopolymerization resin includes 15 to 30 parts by weight of monomer, 5 to 15 parts by weight of additive, 5 to 10 parts by weight of curing agent, and 5 to 9 parts by weight of inorganic filler, based on 20 to 50 parts by weight of oligomer.

The oligomers include Bisphenol A diglycidyl ether (BFDGE), Bisphenol A glycerolate dimethacrylate (Bis-GMA), Bisphenol A dimethacrylate (Bis-MA), Bisphenol A ethoxylated dimethacrylate (Bis-EMA), Diurethane dimethacrylate (UDMA), Diglycidyl ether of bisphenol It is preferred that it contains at least one of A (DGEBA).

The Bispenol A diglycidyl ether (BFDGE) exists as a liquid with a specific gravity of 1.16 at 20°C, has a molecular weight of 340.42, and has no odor. The flash point is 79℃, the melting point is 8℃ to 12℃, the vapor pressure is very low at 0.000000108mmHg at room temperature of 25℃, and the vapor density is preferably 11.7.

The monomer preferably includes at least one of Ethylene glycol dimethacrylate ( EGDMA ), Trimethylpropane triacrylate (TMPTA), Tetrahydrofurfuryl methacrylate (THFMA), and Glycidyl acrylate.

The additive preferably includes at least one of Triethylene glycol dimethacrylate (TEGDMA), Phenol-formaldehyde polymer glycidyl ether, and dopamine.

Triethylene glycol dimethacrylate (TEGDMA) is preferably used as a viscosity regulator.

The phenol-formaldehyde polymer glycidyl ether is a yellow liquid component with a sweet odor, has a specific gravity of 1.22, which is higher than water, has a flash point of 218°C, a boiling point of 245°C or more, and a vapor pressure of 200 mmHg or less at 20°C. desirable.

The curing agent is Diethylenetriamine (DETA), Triethylenetetramine (TETA), N-aminoethylpiperazine (N-AEP), m-phenylenediamine (m-PDA), 4-4'-diaminodiphenylmethane (DDM), 4-4'-diaminodiphenylsulfone (DDS) It is preferable to include at least one of the following.

Since root canal posts are restored directly within the tooth, they must exhibit high radiopacity to be distinguishable from the surrounding anatomical structures on radiographs. Accordingly, the inorganic filler is used to satisfy radiopacity, and preferably contains Ytterbium trifluoride.

The Ytterbium trifluoride is a white solid powder crystal with a molecular weight of 230.04 and a specific gravity of 8.2 at 20°C. In addition, the boiling point is 2227°C, the melting point is 1163.85 to 1179.85°C, and the vapor pressure is preferably 0.00000000459mmHg at 25°C.

Here, the photopolymerization resin for improving interfacial bonding with glass fiber may be configured as follows.

The oligomer is at least one of Bisphenol A diglycidyl ether (BFDGE), Bisphenol A glycerolate dimethacrylate (Bis-GMA), Bisphenol A dimethacrylate (Bis-MA), Bisphenol A ethoxylated dimethacrylate (Bis-EMA), and diglycidyl ether of bisphenol A (DGEBA). The additives include dopamine, and the hardeners include Diethylenetriamine (DETA), Triethylenetetramine (TETA), N-aminoethylpiperazine (N-AEP), m-phenylenediamine (m-PDA), and 4-4'-diaminodiphenylmethane (DDM). ), 4-4'-diaminodiphenylsulfone (DDS) may be included to form a light-polymerized resin.

It is preferable to use 4-(2-Aminoethyl)benzene-1,2-diol as the dopamine.

The dopamine is an eco-friendly additive that improves interfacial adhesion, and serves to improve the interfacial adhesion between the oligomer and glass fiber. By inducing hydrogen bonding between the hydroxyl group of dopamine and the hydroxyl group of glass fiber, the mechanical strength of the root canal post manufactured with excellent interfacial adhesion can be improved.

Additionally, the photopolymerization resin for improving interfacial bonding with glass fiber may be configured as follows.

The oligomer includes at least one of Propylene glycol, Ethylene glycol, Diethylene glycol, 1,4-Butadiol, Poly tetra hydrofuran, and Polypropylene glycol, and the monomer includes at least one of Styrene, Methyl methacrlate, Vinyl toluene, Vinyl acetate, and Ethylene glycol diacrylate. Contains one or more of the additives Dibutyltin dilaurate (DBTDL), Maleic anhydride, Methacylic acid, Acrylic acid, Fumaric anhydride, 1,1,1-tris(hydroxymethyl) propane, hexamethylene diisosyanate, Acetone, and dibutyltindilaurate. The curing agent may include a polyisocyanate prepolymer, and the inorganic material may include at least one of CaCO₃, zinc stearate, and magnesium oxide to form a photopolymerization resin.

The additive is unsaturated by polycondensation reaction of glycol with any one or more of Maleic anhydride, Methacylic acid, Acrylic acid, Fumaric anhydride, and one or more of the oligomers Propylene glycol, Ethylene glycol, Diethylene glycol, and 1,4-Butadiol. Polyester can be produced.

The produced unsaturated polyester reacts with one or more of the monomers Styrene, Methyl methacrlate, Vinyl toluene, Vinyl acetate, and Ethylene glycol diacrylate to produce a polymerization reaction using Dibutyltin dilaurate (DBTDL) as a catalyst to produce an unsaturated polyester resin. can be created.

At least one of the oligomers Poly tetra hydrofuran and polypropylene glycol and the 1,1,1-tris(hydroxymethyl)propane are placed in a reactor and mixed under vacuum, and then the hexamethylene diisosyanate and Acetone: dibutyltindilaurate, which acts as a catalyst, are added to the reactor. Polyurethane can be obtained by mixing at a weight ratio of 200 to 300:1 and reacting for 30 minutes to 1 hour.

The polyurethane may be added to the unsaturated polyester, and at least one of the inorganic substances CaCO₃, zinc stearate, and magnesium oxide may be added to form a photopolymerization resin.

When the light-polymerized resin and glass fiber produced in this way are combined, the unsaturated polyester is light and has excellent physical properties, but is weak to impact, so the disadvantage can be overcome by adding polyurethane to it to give flexibility, and the combination of the glass fiber and the light-polymerized resin can be achieved. By improving the interfacial bonding force, the mechanical properties of the root canal post manufactured can be improved.

The reason for performing this step in a vacuum is to improve processability by removing air bubbles in the glass fiber and light-polymerized resin.

In addition, double-cured resin (dual resin cement) can be used as the light-cured resin.

The polymerization rate of the double-polymerized resin is determined by self-polymerization after light-polymerization, and polymerization occurs twice to ensure transparency and increase light transparency of the root canal post.

Figure 3 is a diagram showing the light transmittance of a dental non-metallic root canal post manufactured by the manufacturing method of the present invention using the above photopolymerized resin.

Hardening stage

The assembled glass fibers are cured by irradiating light using a UV curing machine into a curing mold to have a post shape. At this time, the UV curing machine light wavelength has an output of 320 nm to 600 nm, and it is desirable to carry out curing in a dark room where all surrounding light is blocked.

The hardening mold is characterized in that one end has a tapered shape that is relatively sharper than the other end. The tapered shape has the advantage of being easy to use in root canals as it is similar to the shape of a root canal.

Point display stage

A groove is made on the outer surface of the hardened post to be used as a cutting point and a point is marked. This is to prevent nerve damage by inserting the post at an appropriate length. Before inserting the root canal post, cut it to the appropriate length using a diamond disk or diamond bur.

1 is a photograph of a dental non-metallic root canal post manufactured by the manufacturing method of the present invention.

Through the following manufacturing examples, a non-metallic root canal post was manufactured according to the manufacturing method of a dental non-metallic root canal post of the present invention, and its excellence was confirmed through experiments.

It will be said that the present invention is not limited to these manufacturing examples and experimental examples.

<Manufacturing Example 1> Manufacturing of non-metallic root canal post

Each strand consists of 4,000 single fibers, and six strands of glass fiber with a diameter of 13㎛ are prepared, washed by soaking in acetone for 30 minutes, and then dried at a temperature of 80°C for 12 hours. The dried glass fiber is placed in a plasma reaction tank and a vacuum of 0.1 Torr and plasma of 13Mhz are generated for 3 minutes.

Next, the glass fiber is immersed in a silane solution of 3-methacryloxypropyltrimethoxysilane for 3 minutes and treated with a silane coupling agent. The six strands of glass fiber that have been treated with the silane coupling agent are bundled together and assembled with light-polymerized resin in a vacuum.

At this time, the photopolymerization resin contains 40 parts by weight of oligomer Bispenol A diglycidyl ether (BFDGE), 5 parts by weight of additive Triethylene glycol dimethacrylate (TEGDMA), 10 parts by weight of additive Phenol-formaldehyde polymer glycidyl ether, and mineral based on 100 parts by weight of the glass fiber. 9 parts by weight of filler ytterbium trifluoride, 5 parts by weight of dopamine (4-(2-Aminoethyl)benzene-1,2-diol), and 7 parts by weight of hardener Diethylenetriamine (DETA) were all mixed and used.

Afterwards, it was placed in a tapered curing mold in a dark room not exposed to any light, cured by irradiating light for 10 minutes using a UV curing machine at a wavelength of 360 nm, and then a groove was made to mark the cutting point as in Manufacturing Example 1. Root canal posts were prepared.

<Experimental Example 1> Measurement of radiopacity

In the case of a root canal post, it is necessary to be able to distinguish the radiopacity of the root canal post compared to the dentin when taking an

The root canal post manufactured according to Manufacturing Example 1 was prepared, and its opacity was measured using dental X-rays.

The aluminum step wedge has a length of 50 mm and a width of 50 mm that satisfies the standards of ISO 4049, and is made of aluminum with a purity of 98% or more and containing up to 0.1% copper and up to 1% iron. At this time, the thickness ranges from 0.5mm to 5.0mm with the width at equal intervals of 0.1mm.

The experimental method is to place the X-ray sensor on a lead plate with a thickness of 2 mm or more, and place the manufactured root canal post and aluminum step wedge close to the center of the sensor. The root canal post and aluminum step wedge are exposed to X-rays at 65 KV and 10 mA for 0.8 seconds, with the distance between the cathode and the root canal post being 300 mm to 400 mm. After this, the gray value of the aluminum step wedge is measured.

As a result, the opacity of the root canal post has a value corresponding to that of an aluminum step wedge of approximately 3.3 mm. This was found to be equivalent to the opacity of the aluminum step wedge, and was found to be suitable for the radiation opacity value of at least 3.0 mmAl, which is the standard presented in ISO 6876. In FIG. 2, the opacity of the present invention manufactured according to Production Example 1 is shown in FIG. Radiopacity of dental non-metallic root canal posts was shown.

<Experimental Example 2> Flexural strength measurement

Flexural strength refers to the deformation resistance of a material to a bending load, and since root canal posts are manufactured in various shapes, it is difficult to measure it using standardized specimens. Accordingly, five specimens were manufactured and the resistance to bending was measured by applying the average value.

The experimental method is to fix the root canal post manufactured according to Manufacturing Example 1 in a groove on one side of a square-shaped stainless steel fixing jig measuring 50 mm in width, 50 mm in length, and 50 mm in height, and the center of the groove and the bottom of the fixing jig are tilted at 45°. Set it to have. At this time, the base for fixing the root canal post to the jig is manufactured using PMMA and attached to the jig with adhesive. Afterwards, the maximum load until fracture of the root canal post specimen was measured at a speed of 1 mm/1 min.

The bending strength is calculated using the diameter of the root canal post and the distance between the fixation point at the end of the base and the load point. Flexural strength (S) can be obtained by the following equation.

<Calculation 1>

S: Flexural strength (MPa), F: Maximum load (N), : Distance between fixed point and load point (mm), b: Width of specimen (mm), h: Thickness of specimen (mm)

As a result of calculating the bending strength according to Equation 1 above, a value of 1600 MPa was obtained. It was found to have a strong flexural strength compared to the average value of 1200 to 1300 MPa from other conventional manufacturers.

<Experimental Example 3> Cytotoxicity measurement

Root canal posts are inserted into the root canal and used in direct contact with dentin. Therefore, infection of living organisms may occur due to cytotoxicity, and therefore a cytotoxicity experiment using the direct contact method was conducted.

배양기에서 성장상 로그 곡선의 마지막에 도달할 때까지 배양하였다. 두개의 배양용기의 면적의 80%이상이 될 때까지 배양한 후 배양 용기로부터 배양액을 각각 제거하고 신선한 배양액을 배양용기에 재 분주한다. 이 후, 두 개의 배양용기 중 하나의 세포층 중앙에는 제조 예 1에 의해 제조된 근관 포스트를 올려놓고, 나머지 하나의 세포층 중앙에는 시중에 판매하는 메탈 근관 포스트를 올려놓고 5% CO2, 97%의 습도 조건을 갖추어 37

배양기에서 다시 24시간동안 배양한 후 결과를 관찰하였다.As an in vitro cytotoxicity test method, the eluate was brought into contact with the root canal post specimen prepared according to Preparation Example 1 and the cells were cultured through diffusion. Cell culture was performed using Fibroblasts (NCTC clone 929 cells) at 37 °C with 5% CO2 and 97% humidity conditions.

The cells were cultured in the incubator until the end of the logarithmic growth curve was reached. After culturing until more than 80% of the area of the two culture vessels is reached, the culture medium is removed from each culture vessel and fresh culture medium is redistributed into the culture vessels. Afterwards, the root canal post prepared according to Manufacturing Example 1 was placed in the center of the cell layer of one of the two culture vessels, and a commercially available metal root canal post was placed in the center of the cell layer of the other one, and placed in 5% CO2 and 97% humidity. meet the conditions 37

After culturing in the incubator for another 24 hours, the results were observed.

For the reaction of cultured cells, observe the culture vessel against a white background and check for red-stained cells around the sample. As a result, compared to the metal root canal post, the extent of cells with reduced staining in the root canal post prepared according to Preparation Example 1 of the present invention was significantly smaller, which shows that the non-metallic root canal post of the present invention has low cytotoxicity and is excellent in biocompatibility. there was.

Therefore, the dental non-metallic root canal post manufactured according to the present invention was found to have strong bending strength, no corrosion, guaranteed biocompatibility and stability, and excellent radiopacity.

Those skilled in the art to which the present invention pertains will understand that the present invention can be implemented in other specific forms without changing its technical idea or essential features. Therefore, the embodiments described above should be understood in all respects as illustrative and not restrictive. The scope of the present invention is indicated by the scope of the claims described below rather than the detailed description above, and all changes or modified forms derived from the meaning and scope of the claims and their equivalent concepts are included in the scope of the present invention. must be interpreted.

Claims (10)

In the method of manufacturing a dental non-metallic root canal post,
providing glass fiber strands;
washing and drying the glass fiber strands;
Plasma treatment on the surface of the dried glass fiber strands;
Treating the surface of the plasma-treated glass fiber strand with a silane coupling agent, which is an interfacial binder;
Gathering a plurality of glass fiber strands that have been treated with the silane coupling agent and assembling them with light-polymerization resin in a vacuum;
curing the assembled glass fiber strands into a post-shaped mold by irradiating light using a UV curing machine;
A method of manufacturing a dental non-metallic root canal post, comprising: marking a point to be used as a cutting point on the outer surface of the hardened post. According to clause 1,
The silane coupling agent is at least any of 3-Methacryloxypropyltrimethoxysilane, 3-Methacryloxypropyltriethoxysilane, 3-Methacryloxypropylmethyldimethoxysilane, 3-(Acryloyloxy)propyltrimethoxysilane, 3-Aminopropyltriethoxysilane, N-2-(Aminoethyl)-3-aminopropyltrimethoxysilane, and Triethoxy(octyl)silane. more than one A method of manufacturing a dental non-metallic root canal post comprising: According to clause 1,
The photopolymerized resin is a dental treatment comprising 15 to 30 parts by weight of monomer, 5 to 15 parts by weight of additive, 5 to 10 parts by weight of hardener, and 5 to 9 parts by weight of inorganic filler, based on 20 to 50 parts by weight of oligomer. Method for manufacturing non-metallic root canal posts. According to clause 3,
The oligomers include Bisphenol A diglycidyl ether (BFDGE), Bisphenol A glycerolate dimethacrylate (Bis-GMA), Bisphenol A dimethacrylate (Bis-MA), Bisphenol A ethoxylated dimethacrylate (Bis-EMA), Diurethane dimethacrylate (UDMA), Diglycidyl ether of bisphenol A method of manufacturing a dental non-metallic root canal post comprising at least one of A (DGEBA). According to clause 3,
A method of manufacturing a dental non-metallic root canal post, wherein the monomer includes at least one of Ethylene glycol dimethacrylate ( EGDMA ), Trimethylpropane triacrylate (TMPTA), Tetrahydrofurfuryl methacrylate (THFMA), and Glycidyl acrylate. According to clause 3,
The curing agent is Diethylenetriamine (DETA), Triethylenetetramine (TETA), N-aminoethylpiperazine (N-AEP), m-phenylenediamine (m-PDA), 4-4'-diaminodiphenylmethane (DDM), 4-4'-diaminodiphenylsulfone (DDS) A method of manufacturing a dental non-metallic root canal post comprising at least one of the following. According to clause 3,
A method of manufacturing a dental non-metallic root canal post, wherein the inorganic filler contains Ytterbium trifluoride and is used to improve radiopacity. According to clause 3,
The light-polymerized resin is,
The oligomer is at least Bisphenol A diglycidyl ether (BFDGE), Bisphenol A glycerolate dimethacrylate (Bis-GMA), Bisphenol A dimethacrylate (Bis-MA), Bisphenol A ethoxylated dimethacrylate (Bis-EMA), and Diglycidyl ether of bisphenol A (DGEBA). Contains one or more,
The additive includes dopamine,
The curing agent is Diethylenetriamine (DETA), Triethylenetetramine (TETA), N-aminoethylpiperazine (N-AEP), m-phenylenediamine (m-PDA), 4-4'-diaminodiphenylmethane (DDM), 4-4'-diaminodiphenylsulfone (DDS) Contains at least one or more of
A method of manufacturing a dental non-metallic root canal post characterized by improving the interfacial bond with glass fiber. According to clause 3,
The light-polymerized resin is,
The oligomer includes at least one of propylene glycol, ethylene glycol, diethylene glycol, 1,4-butadiol, poly tetra hydrofuran, and polypropylene glycol,
The monomer includes at least one of Styrene, Methyl methacrlate, Vinyl toluene, Vinyl acetate, and Ethylene glycol diacrylate,
The additive includes at least one of Dibutyltin dilaurate (DBTDL), Maleic anhydride, Methacylic acid, Acrylic acid, Fumaric anhydride, 1,1,1-tris(hydroxymethyl) propane, hexamethylene diisosyanate, Acetone, and dibutyltindilaurate,
The curing agent includes a polyisocyanate prepolymer,
The inorganic material includes at least one of CaCO₃, zinc stearate, and magnesium oxide,
A method of manufacturing a dental non-metallic root canal post characterized by improving the interfacial bond with glass fiber. According to clause 1,
The silane coupling agent treatment involves preparing a co-solvent by diluting 85 to 95 parts by weight of N-butanol with 5 to 15 parts by weight of distilled water, and then adding 0.1 to 0.5 parts by weight of silane to prepare an aqueous silanol solution to form the glass fiber strands. A method of manufacturing a dental non-metallic root canal post, characterized in that immersion.