KR20190018579A - High translucency silicate glass for enamel layer of natural tooth - Google Patents

High translucency silicate glass for enamel layer of natural tooth Download PDF

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KR20190018579A
KR20190018579A KR1020170102957A KR20170102957A KR20190018579A KR 20190018579 A KR20190018579 A KR 20190018579A KR 1020170102957 A KR1020170102957 A KR 1020170102957A KR 20170102957 A KR20170102957 A KR 20170102957A KR 20190018579 A KR20190018579 A KR 20190018579A
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weight
silicate glass
present
glass
zirconia
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KR1020170102957A
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KR102037401B1 (en
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임형봉
김성민
김준형
오경식
홍영표
전현준
김용수
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주식회사 하스
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    • A61K6/0088
    • A61K6/024

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Abstract

The present invention relates to a silicate glass which is an artificial tooth material for repairing a damaged tooth, and more particularly to a highly transparent silicate glass similar in enamel to translucency and mechanical properties similar to enamel of a natural tooth having a high visible light transmittance.
To this end, an artificial tooth material with a struggling light component proposed by the present invention, the ZrO2 to improve the wettability for the bonding to the zirconia 3-5 wt%, SiO 2 69 ~ 79% by weight of the structural role of the glass, Li 2 O (M = Ca, Zn, Mg) in an amount of 0.1 to 3% by weight, 10 to 13% by weight of P 2 O 5, 3 to 7% by weight of P 2 O 5 , 1 to 4% by weight of Al 2 O 3 and 1.0 to 2.5% And a colorant in an amount of 0.5 to 2.0% by weight.
In addition, the blank (ingot) prepared from the glass composition proposed in the present invention is heat-treated at a temperature of 300 ° C to 600 ° C for 1 minute to 2 hours, particularly at a temperature of 300 ° C to 400 ° C for 1 minute to 2 hours. Having a light transmittance of 50% or more and having a very high translucency.

Description

TECHNICAL FIELD [0001] The present invention relates to a high-transmittance silicate glass for enamel layer of natural tooth,

The present invention relates to a silicate glass which is an artificial tooth material for repairing a damaged tooth, and more particularly to a highly transparent silicate glass similar to enamel with translucency and mechanical properties similar to enamel of a natural tooth having a high visible light transmittance.

Although many artificial tooth replacement materials have been developed and used so far, there have been no artificial tooth materials that are compatible with the light transmittance and physical properties of enamel among the inherent characteristics of natural teeth. The enamel does not have a very high light transmittance as glass, but it does not have as low a light transmittance as zirconia or ceramics. At present, artificial teeth require appropriate light transmittance (visible light transmittance: 40 to 60%), and aesthetic characteristics such as fluorescence are also important. As far as the artificial tooth materials developed so far are concerned, lithium disilicate or lucite crystallized glass exhibits a visible light transmittance of 25 to 40% lower than enamel. In the case of zirconia, the visible light transmittance has recently been increased, but it is still lower than that of the crystallized glass, and the porcelain has lower mechanical properties than the enamel transmittance.

1. Korean Patent Publication No. 2017-0008746 2. Korean Patent Publication No. 2014-0064736

An object of the present invention is to provide an artificial tooth material showing a light transmittance at enamel level of a natural tooth.

Another object of the present invention is to provide a natural-friendly artificial tooth material having properties similar to those of a natural tooth enamel.

Another object of the present invention is to provide an artificial tooth material in which the color of zirconia can be transmitted to the outside.

Artificial tooth material having a high tugwangyul proposed by the present invention for this purpose is the ZrO2 to improve the wettability for the bonding to the zirconia 3-5 wt%, SiO 2 69 ~ 79% by weight of the structural role of the glass, Li 2 O (M = Ca, Zn, Mg) in an amount of 0.1 to 3% by weight, 10 to 13% by weight of P 2 O 5, 3 to 7% by weight of P 2 O 5 , 1 to 4% by weight of Al 2 O 3 and 1.0 to 2.5% And a colorant in an amount of 0.5 to 2.0% by weight.

In addition, the blank (ingot) prepared from the glass composition proposed in the present invention is heat-treated at a temperature of 300 ° C to 600 ° C for 1 minute to 2 hours, particularly at a temperature of 300 ° C to 400 ° C for 1 minute to 2 hours. It has a very high light transmittance with a light transmittance of 50% or more and can be used to obtain a highly transparent translucent prosthesis.

The glass composition, which is an artificial tooth material proposed in the present invention, can be replaced when the enamel located in the outermost layer of the tooth structure is damaged due to the blending ratio of the composition and the heat treatment process, the visible light average transmittance of 40 to 70% . In particular, the artificial tooth material of the present invention exhibited a visible light transmittance of 50% or more when the ingot heat-treated at 300 ° C to 400 ° C was hot-pressed. As described above, since the artificial tooth material proposed in the present invention has a high light transmittance, it is possible to realize esthetics, which is an important requirement of the tooth material, when the external coating is applied to the outside of zirconia.

In addition, since the conventional veneer materials for pressing zirconia have a low light transmittance of 25 to 40%, the color of the veneer itself determines the color of the prosthesis in a state in which the coating layer is thickly raised, and the amount of cutting zirconia And the mechanical stability of the prosthesis is lowered.

On the other hand, the artificial teeth suggested in the present invention can maintain the mechanical structural stability by thinly bonding the zirconia prosthesis to the surface thereof without cutting the zirconia prosthesis, and the zirconia is transmitted through the thin coating layer, By obtaining color, it is possible to obtain optical characteristics similar to natural teeth. Therefore, it can be said that the utility value is high by suggesting a method of overcoming the low esthetics which is the biggest disadvantage of the existing zirconia prosthesis.

Since the hot pressing process is performed in a high temperature and high pressure environment, the mechanical properties of the prosthesis can be enhanced because the internal porosity is lower than the conventional method of raising the veneer at the normal pressure and the low temperature (porcelain forming) The silicate glass changes into the crystallized glass of the lithium disilicate microcrystals while increasing the strength.

Figure 1 shows a conventional microstructure of a zirconia prosthesis cut surface.
FIG. 2 illustrates the interface of a silicate crystallized glass thermally bonded to zirconia according to an embodiment of the present invention.
FIG. 3 shows the result of the crystal phase analysis after the final hot junction according to an embodiment of the present invention.
FIG. 4 illustrates the visible light transmittance of a silicate crystallized glass that has been subjected to a final heat treatment of a silicate glass according to an embodiment of the present invention and a conventional veneer material.
FIG. 5 shows the interface tensile bond strengths when the silicate glass according to an embodiment of the present invention is subjected to the final hot junction heat treatment with zirconia and when the existing zirconia-based veneer material is laminated on zirconia.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, it will be understood by those skilled in the art that the following embodiments are provided so that those skilled in the art will be able to fully understand the present invention, and that various changes and modifications may be made without departing from the scope of the present invention. It is not.

The present invention proposes a crystallized glass material that exhibits light (visible light) translucency and physical properties similar to enamel, and the crystallized glass material of the present invention can replace the enamel of a damaged tooth. When used with zirconia, the low light transmittance of zirconia Can be made with prosthetic material. In addition, the crystallized glass material of the present invention can be applied to part or all of teeth, and can be applied in various forms such as a bridge shape.

Hereinafter, a silicate glass and a manufacturing method thereof will be described with reference to FIGS. 1 to 5, and then a method for manufacturing a final prosthesis using the lithium disilicate crystallized glass produced by the final pressing heat treatment will be described .

Fig. 1 is a photograph of a cut surface of a prosthesis made by a conventional method. In the past, a crown was made by forming a ceramic material (veneer material) on zirconia. Also, as shown in Fig. 1, the porcelain contains porosity, which remains after the heat treatment, thereby affecting the property deterioration. Since the silicate glass according to an embodiment of the present invention is bonded to zirconia through hot bonding (or hot pressing), and the hot bonding is performed at a higher heat treatment temperature and vacuum than in ceramics, There is an advantage that it can be easily removed.

FIG. 3 is a lithium disilicate crystal phase when a silicate glass according to an embodiment of the present invention is subjected to a final hot junction heat treatment. The silicate glass is transformed into a crystallized glass by a hot junction heat treatment, and the crystalline phase produced at this time is a lithium disilicate crystalline phase. In addition, the transmittance of the crystallized glass is very high, which is called incisal translucency (IT), and it is divided into three products such as IT 0, 1 and 2 according to the degree of translucency. As a result of the analysis, a lithium disilicate crystal phase is likewise formed.

FIG. 4 shows the visible light transmittance of a conventional ceramic-based ceramics and a silicate crystallized glass obtained by final heat-treating the silicate glass of the present invention. The ceramics crystallized glass of the present invention exhibits a visible light transmittance of 55%, and particularly exhibits a visible light transmittance of up to 70% depending on the heat treatment temperature, while the ceramics ceramics of the present invention exhibits a visible light transmittance of 35% .

Fig. 5 shows the tensile bond strength in the case where the ceramics based ceramics according to the present invention is laminated on the zirconia and the tensile bond strength after the thermal bonding of the zirconia with the silicate crystallized glass according to the present invention. Conventional ceramics based ceramics show a tensile bond strength of 25 MPa, whereas the silicate crystallized glass of the present invention shows a tensile bond strength of 40 MPa, so that the tensile bond strength of the silicate crystallized glasses proposed in the present invention .

As described above, the present invention proposes an artificial tooth material having high transparency through a glass composition and a heat treatment process. The glass composition comprises 3 to 5% by weight of ZrO 2 improving the wettability for bonding with zirconia, 69 to 79% by weight of SiO 2 serving as a glass structure, Li 2 10 to 13% by weight of Al 2 O 3 , 3 to 7% by weight of P 2 O 5 serving as a nucleating agent for crystal formation, 1 to 4% by weight of Al 2 O 3 controlling the crystal formation rate through controlling the viscosity of the glass, 1.0 to 2.5% by weight of K 2 O, 0.1 to 3% by weight of MO (M = Ca, Zn, Mg) and 0.5 to 2.0% by weight of a coloring agent for controlling the viscosity and wettability of the pigment.

The core composition is ZrO 2 and has the greatest influence on the wettability of zirconia. Particularly, when it is less than 3% by weight, local zirconia bonding failure occurs. When it exceeds 5% by weight, the thermal expansion coefficient is increased, There is a problem that it is difficult. In addition, ZrO 2 is fine, but also affects toning characteristics and serves as a color of reddish ivory series.

The blank (ingot) produced through the above-described glass composition is heat treated at 300 to 600 ° C for 1 minute to 2 hours, and particularly when heat treatment is performed at 300 ° C to 400 ° C for 1 minute to 2 hours, It is possible to obtain a prosthesis exhibiting an extremely high light transmission rate of 50% or more.

If the blank heat treatment temperature is less than 300 ° C, nucleation of the glass is difficult, and at 600 ° C or higher, crystal formation is excessive and a high transmittance can not be obtained after the final pressing. If the time is less than 1 minute, the nucleation time is insufficient, and if it exceeds 2 hours, crystals are excessively generated.

In addition, the silicate glass according to a preferred embodiment of the present invention may further include 0.001 to 3% by weight of MgO for enhancing durability against thermal denaturation.

Further, in the silicate glass is a product state according to an embodiment of the present invention shows a glass phase of the semi-transparent, there is a lithium die silicate crystal phase formed after the final pressing thermal treatment wherein MnO 2 0.001 ~ to lower the formation temperature of the crystal phase formed 3% by weight As shown in FIG.

In addition, the high-strength crystallized glass for artificial teeth according to a preferred embodiment of the present invention may further include 0.5 to 2% by weight of a coloring agent to impart the same or similar color to teeth. The coloring agent is for imparting the same or similar color and fluorescence as that of a tooth. The coloring agent is titanium oxide (TiO 2 ), red iron oxide (Fe 2 O 3 ), white cerium (CeO 2 ) Vanadium pentoxide (V 2 O 5 ), black vanadium trioxide (V 2 O 3 ), Er 2 O 3 , La 2 O 3 , Tb 2 O 3 , Pr 2 O 3 , Y 2 O 3 , TaO 2 , MnO 2, or a mixture thereof. For example, red iron oxide (Fe 2 O 3 ), ceria (CeO 2 ), or vanadium pentoxide (V 2 O 5 ) is added together with the starting material and melted to give a yellow color similar to the color of teeth, Titanium oxide (TiO 2 ) is white and gives a color very similar to the color of teeth.

Li 2 CO 3 may be added in place of Li 2 O, and carbon dioxide (CO 2 ), which is a carbon (C) component of Li 2 CO 3 , may be added to the glass as a gas And discharged. Further, K 2 CO 3 and Na 2 CO 3 may be added instead of K 2 O and Na 2 O in the alkali oxide, and carbon dioxide (CO 2 ) of K 2 CO 3 and Na 2 CO 3 , ) Is discharged into the gas in the melting process of the glass and then escapes.

The mixing may be performed using a dry mixing process, and a ball milling process may be used as a dry mixing process. Specifically, the starting material is charged into a ball milling machine, and the ball milling machine is rotated at a constant speed to mechanically pulverize the starting material and mix it uniformly. The ball used in the ball miller may be a ball made of ceramics such as zirconia or alumina, and the balls may have the same size or at least two or more sizes. Considering the size of the target particle, adjust the size of the ball, the milling time, and the rotation speed per minute of the ball miller. For example, the size of the balls may be set in the range of about 1 mm to 30 mm in consideration of the size of the particles, and the rotation speed of the ball miller may be set in the range of about 50 to 500 rpm. The ball milling is preferably carried out for 1 to 48 hours in consideration of the size of the target particle and the like. By ball milling, the starting material is pulverized into fine sized particles, having a uniform particle size and being uniformly mixed at the same time.

The mixed starting material is placed in a melting furnace, and the starting material is melted by heating the melting furnace containing the starting material. Here, melting means that the starting material is changed into a liquid state viscous material state, not a solid state. The melting furnace is preferably made of a material having a low contact angle in order to suppress the phenomenon that the melt has a high melting point and a high degree of sticking of the melt. For this purpose, platinum (Pt), diamond-like carbon (DLC), chamotte Or a surface-coated melting furnace made of a material such as platinum (Pt) or diamond-like-carbon (DLC).

The melting is preferably performed at 1400 ° C to 2000 ° C at normal pressure for 1 hour to 12 hours. When the melting temperature is less than 1400 ° C, the starting material may not melt. If the melting temperature exceeds 2000 ° C, excessive energy is consumed and it is not economical. Therefore, it is preferable to melt at a temperature within the above range. If the melting time is too short, the starting material may not be sufficiently melted, and if the melting time is too long, excessive energy is consumed and it is not economical. If the heating rate of the melting furnace is too slow, it takes a long time to lower the productivity. If the rate of temperature rise of the melting furnace is too fast, the temperature of the melting furnace is increased by a rapid temperature rise. The volatilization amount becomes large and the physical properties of the crystallized glass may be poor. Therefore, it is preferable to raise the temperature of the melting furnace at the temperature raising rate within the above-mentioned range. The melting is preferably carried out in an oxidizing atmosphere such as oxygen (O 2 ) and air.

The melt is cast into a defined mold to obtain crystallized glass for a tooth of the desired shape and size. The mold is preferably made of a material having a low contact angle in order to suppress the phenomenon that the glass melt has a high melting point and a high melting point, and the mold is made of a material such as graphite or carbon, It is preferable to preheat the molten material to 200 to 300 DEG C and pour the molten material into the forming mold. If necessary, the molten material may be poured into the forming mold immediately without preheating.

When the melt contained in the molding mold is cooled to 60 ° C to 100 ° C, a heat treatment process is performed. The heat treatment is preferably carried out at 300 ° C to 600 ° C at normal pressure for 1 minute to 2 hours. Crystallization is hardly achieved after the heat treatment, and a lithium disilicate crystal phase is generated after the final hot pressing according to the heat treatment temperature, and the light transmittance can be adjusted within the range of 40% to 70%. The lower the heat treatment temperature is, the more advantageous it is to obtain a pressing object having a high light transmittance. In particular, a pressing material having a high transmittance can be obtained at 300 ° C to 400 ° C for 1 minute to 2 hours. In the context of the present invention, the hot pressing is carried out at a temperature of 900 to 950 DEG C and 4 bar. The hot pressing process is divided into a hot junction for joining the silicate glass proposed in the present invention to the outer side of zirconia at a high temperature and a high pressure, and a hot press for processing the silicate glass at a high temperature and a high pressure.

  The artificial tooth material according to the present invention can improve the optical transparency inherent in zirconia by making a hot joint with the outer surface of the zirconia when preparing the prosthesis (single piece or bristle tooth) using the high strength zirconia material, Can be implemented.

Claims (5)

3 to 5 wt% of ZrO 2 improving wettability for bonding with zirconia, 69 to 79 wt% of SiO 2 serving as a structure of glass, 10 to 13 wt% of Li 2 O, 3 to 7 wt% of P 2 O 5 SiO 2 containing 0.1 to 3% by weight of MO (M = Ca, Zn, Mg) and 0.5 to 2.0% by weight of a colorant in 1 to 4% by weight of Al 2 O 3 , 1.0 to 2.5% by weight of K 2 O, Based silicate glass.
The method of claim 1 wherein the silicate glass in the range 300 ℃ ~ 600 ℃, 1 ~ 2 sigan bun during the heat treatment, and a silicate glass that is based on SiO 2 using the visible light transmittance of 40 to 70% by said heat treatment.
The method of claim 1, wherein in the silicate glass region to 300 ℃ ~ 400 ℃, 1 bun ~ 2 sigan heat-treated for, and silicate glass that by the heat treatment Visible light transmittance based on SiO 2 of 50% to 70%.
An artificial tooth wherein the silicate glass based on SiO 2 according to claim 2 or 3 is hot-pressed on the outer surface of zirconia and the lithium disilicate crystal phase is formed by the hot pressing.
A single-piece or a bristle made by the hot pressing process of claim 4.
KR1020170102957A 2017-08-14 2017-08-14 High translucency silicate glass for enamel layer of natural tooth KR102037401B1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20230042681A (en) * 2021-06-15 2023-03-29 주식회사 하스 Dental bulk blocks and manufacturing method of the same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140064736A1 (en) 2012-09-05 2014-03-06 Sony Corporation Information processing apparatus, information processing system, information processing method, and program therefor
US20170008746A1 (en) 2015-07-10 2017-01-12 E.& J. Gallo Winery System and Method for Dispensing a Beverage
KR20170026697A (en) * 2015-08-26 2017-03-09 주식회사 하스 Dental glass-ceramics block bonded Abutment and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140064736A1 (en) 2012-09-05 2014-03-06 Sony Corporation Information processing apparatus, information processing system, information processing method, and program therefor
US20170008746A1 (en) 2015-07-10 2017-01-12 E.& J. Gallo Winery System and Method for Dispensing a Beverage
KR20170026697A (en) * 2015-08-26 2017-03-09 주식회사 하스 Dental glass-ceramics block bonded Abutment and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20230042681A (en) * 2021-06-15 2023-03-29 주식회사 하스 Dental bulk blocks and manufacturing method of the same

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