Porcelain paste for dentistry, porcelain kit for dentistry, and method for manufacturing porcelain patch for dentistry

By using dental porcelain paste containing glass powder, organic solvents and decolorizing agents, the problems of uneven coating and leakage in the prior art are solved, and high recognition and efficient coating operations are achieved, and the aesthetics and production efficiency of dental porcelain are improved.

CN119816284APending Publication Date: 2025-04-11KURARAY NORITAKE DENTAL
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Patent Information

Application Number
CN202380062729.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2022-09-02
Filing Date
2023-09-01
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

The existing dental porcelain paste is difficult to identify the coated and uncoated parts in the coating operation, resulting in uneven coating and leakage of porcelain materials, affecting aesthetics and production efficiency.

Method used

Dental porcelain paste containing glass powder, organic solvent and colorants that abrogate during calcination is used. By adjusting the composition and treatment conditions, specific color difference and brightness conditions are met to improve the recognition of the paste.

Benefits of technology

It significantly improves the recognition in the coating operation before calcination, avoids coating unevenness and leakage, shortens production time, and improves aesthetics and matching.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to a dental ceramic paste, a dental ceramic kit, and a method for producing a dental patch, the dental ceramic paste satisfying at least one condition selected from the following conditions: (A) a glass powder, (B) an organic solvent, and (C) a colorant that discolors during calcination, and the dental ceramic paste containing (A) a glass powder, (B) an organic solvent, and (C) a colorant that discolors during calcination, and the dental ceramic paste containing (A) a glass powder, (B) an organic solvent, and (C) a colorant that discolors during calcination. Condition (1): The color difference [Delta] E * calculated from the color tone obtained by measuring the color of a dental ceramic paste having a thickness of 0.5 mm before calcination in an L * a * b * color space and the color tone obtained by measuring the color of a calcined body having a thickness of 0.5 mm obtained by vacuum calcination of the dental ceramic paste at 740 DEG C in the L * a * b * color space is 8.5 or more. Condition (2): The brightness difference [Delta] L * calculated from the brightness obtained by color measurement of the dental ceramic paste having a thickness of 0.5 mm before calcination using an L * a * b * color space and the brightness obtained by color measurement of a calcined body having a thickness of 0.5 mm obtained by vacuum calcination of the dental ceramic paste at 740 DEG C using an L * a * b * color space is 6.5 or more.
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Description

Technical Field

[0001] The present invention relates to a dental porcelain paste, a dental porcelain kit containing the dental porcelain paste, and a method for producing a dental porcelain prosthesis using the dental porcelain paste. Background Art

[0002] Ceramics have a transparency and color similar to natural teeth, making them an indispensable material for the production of crowns that require aesthetics.

[0003] Generally speaking, a tooth crown is made by repeatedly filling and calcining a frame (e.g., a metal frame, a ceramic frame) covering a bridge abutment tooth using a dental mixing solution formed by a porcelain material and one or more selected from water and an organic solvent, or a porcelain material obtained by pre-mixing one or more selected from water and an organic solvent with ceramics and making it into a paste.

[0004] Powdered porcelain materials are complicated because they need to be mixed with a solvent each time they are processed, and require skill to adjust the mixing ratio and viscosity according to the desired color tone. However, porcelain materials in paste form are mixed with a solvent in advance to a viscosity that allows dental technicians to work with good workability, so the time required for dental technicians to work can be shortened.

[0005] For example, Patent Document 1 discloses a dental porcelain paste comprising a colorant (A) that discolors during firing, an organic solvent (B), and a porcelain powder (C), wherein the porcelain powder (C) contains an inorganic pigment.

[0006] In addition, as the base material of dental prostheses made of ceramic materials, zirconia (zirconium oxide), alumina (aluminum oxide), feldspar glass, disilicate glass, etc. are used. Recently, the opportunities for processing these raw materials using dental CAD / CAM systems and using them as dental prostheses are also increasing.

[0007] Representative examples of dental prostheses made of the aforementioned ceramic materials include: porcelain fused to metal (PFM), full zirconia (PFZ), full contour zirconia (FCZ), and lithium pyrophosphate (LDS) dental prostheses.

[0008] Dental porcelain materials such as dyed porcelain materials and glazed porcelain materials are used for finishing of these dental prostheses.

[0009] For example, Patent Document 2 discloses a coloring composition for ceramic crown porcelain, which is characterized by comprising a colorant and two or more types of aluminosilicate glasses, wherein the two or more types of aluminosilicate glasses respectively satisfy specific conditions.

[0010] Prior art literature

[0011] Patent Literature

[0012] Patent Document 1: Japanese Patent Application Publication No. 2017-193492

[0013] Patent Document 2: Japanese Patent Application Publication No. 2009-207743 Summary of the invention

[0014] Problems to be solved by the invention

[0015] However, in general, glazed porcelain is mainly used for the purpose of polishing dental prostheses, and it is required that the color difference between it and the base material (hereinafter also referred to as "base") after calcination is small. Therefore, the porcelain paste used as glazed porcelain is a transparent or translucent material with almost no color before calcination. However, if such a porcelain paste is used, it is difficult to distinguish the parts coated with glazed porcelain from the parts not coated, and to confirm the coating thickness during the coating operation. As a result, the coating leakage and uneven coating of the porcelain are likely to occur. If the coating leakage and uneven coating of the porcelain occur, the following disadvantages will occur: poor aesthetics, time-consuming matching and contact adjustment of adjacent surfaces, and an increase in the coating operation and the number of calcinations to make up for the uncoated parts of the porcelain and the parts with insufficient coating.

[0016] Therefore, in order to enable the dental porcelain paste to be used also as a glaze porcelain, it is required that when the dental porcelain paste before calcination is applied to the substrate, the property of being able to visually identify the area coated with the dental porcelain paste (hereinafter also abbreviated as "identifiability") is further improved.

[0017] Here, Patent Document 1 mentions the color difference of the paste before and after calcination. However, it mainly mentions that: in the case of coloring with dyed porcelain, the color tone of the porcelain is not the same before and after calcination. Therefore, it requires skilled technology to predict the color tone after calcination and adjust the color tone when the porcelain is filled. To address this problem, the color difference of the paste-like dental porcelain before and after calcination should be suppressed. Therefore, the paste-like dental porcelain disclosed in the embodiments of Patent Document 1 mainly involves examples of dyed porcelain, and glazed porcelain is not disclosed. When the paste-like dental porcelain disclosed in Patent Document 1 is used as glazed porcelain, further improvement is required for the aforementioned recognition. In addition, as mentioned above, in the case of glazed porcelain, polishing is the main purpose, and therefore, it is expected that the color difference between the calcined body obtained by calcining the dental porcelain paste and the substrate is small.

[0018] Furthermore, Patent Document 2 does not mention the aforementioned problems associated with the use of glaze ceramics.

[0019] Therefore, in particular, when the dental porcelain paste is also used as a glaze porcelain, further improvement in visibility is required.

[0020] Therefore, an object of the present invention is to provide a dental porcelain paste having excellent visibility during the coating operation before firing.

[0021] Means used to solve problems

[0022] The present inventors have conducted intensive studies and have found that the above-mentioned problems can be solved by using a dental porcelain paste containing glass powder (A), an organic solvent (B) and a colorant (C) that loses color during firing and that satisfies specific conditions, thereby completing the present invention.

[0023] That is, the present invention includes the following technical solutions.

[0024] [1] A dental porcelain paste comprising glass powder (A), an organic solvent (B), and a colorant (C) that loses color when fired, wherein the dental porcelain paste satisfies at least one of the following conditions (1) and (2).

[0025] Condition (1): The color difference ΔE calculated from the color tone of the dental porcelain paste with a thickness of 0.5 mm before calcination measured using the L*a*b* color space and the color tone of the calcined body with a thickness of 0.5 mm obtained by vacuum calcining the dental porcelain paste at 740°C using the L*a*b* color space * 8.5 or above;

[0026] Condition (2): The lightness difference ΔL calculated from the lightness obtained by colorimetrically measuring the 0.5 mm thick dental porcelain paste before calcination using the L*a*b* color space and the lightness obtained by colorimetrically measuring the 0.5 mm thick calcined body obtained by vacuum calcining the dental porcelain paste at 740°C using the L*a*b* color space * It is above 6.5.

[0027] [2] The dental porcelain paste according to [1], wherein the color difference ΔE1 is calculated based on the color tone of the substrate measured using the L*a*b* color space and the color tone of the dental porcelain paste applied to the substrate at a thickness of 0.5 mm measured using the L*a*b* color space. * It is above 11.0.

[0028] [3] The dental porcelain paste according to [1] or [2], wherein the color tone of the base material is measured using the L*a*b* color space and the color tone of the base material is measured using the L*a*b* color space. * a * b * The color difference ΔE2 calculated by measuring the color tone of the calcined body in the color space * The calcined body is obtained by applying the dental porcelain paste on the substrate so that the thickness after calcination is 65 μm, and calcining the dental porcelain paste at 740° C. in a vacuum.

[0029] [4] The dental porcelain paste according to any one of [1] to [3] above, wherein the content of component (C) is 0.001 parts by mass or more and less than 0.60 parts by mass relative to 100 parts by mass of the total of components (A) and (B).

[0030] [5] The dental porcelain paste according to any one of [1] to [4] above, wherein the component (C) contains an organic pigment dissolved in the component (B).

[0031] [6] The dental porcelain paste according to [5] above, wherein the organic pigment is an aromatic organic pigment.

[0032] [7] The dental porcelain paste according to [5] or [6], wherein the organic pigment is at least one selected from anthraquinone compounds, azo compounds, xanthene compounds, porphyrin compounds, phthalocyanine compounds and triarylmethane compounds.

[0033] [8] The dental porcelain paste according to any one of [1] to [7] above, comprising a fluorescent agent.

[0034] [9] The dental porcelain paste according to [8] above, wherein the content of the fluorescent agent is 0.001 to 0.50 parts by mass based on 100 parts by mass of the total of components (A) and (B).

[0035]

[10] The dental porcelain paste according to any one of [1] to [9] above, comprising an inorganic pigment.

[0036]

[11] A dental porcelain kit comprising the dental porcelain paste according to any one of [1] to

[10] and a color sample for matching the coating thickness of the dental porcelain paste.

[0037]

[12] A method for producing a dental prosthesis, comprising: a step (I) of applying the dental porcelain paste described in any one of [1] to

[10] to a substrate; and a step (II) of calcining the dental porcelain paste applied to the substrate.

[0038]

[13] The method for producing a dental prosthesis according to

[12] above, wherein the calcination temperature in the step (II) is 700° C. or higher.

[0039]

[14] The method for producing a dental prosthesis according to

[12] or

[13] , wherein the step (I) includes using a color sample for matching the coating thickness of the dental porcelain paste.

[0040] Effects of the Invention

[0041] According to the present invention, a dental ceramic paste having excellent visibility in the coating operation before firing can be provided. DETAILED DESCRIPTION

[0042] Hereinafter, the present invention will be described in detail using embodiments.

[0043] In the present specification, the upper limit and the lower limit of the numerical range (the content of each component, the value calculated from each component, each physical property, etc.) can be combined as appropriate.

[0044] That is, in this specification, the lower limit and upper limit described in stages for the numerical range can be independently combined. For example, based on the description of "preferably 10 to 90, more preferably 30 to 60" for the same item, "preferably the lower limit (10)" and "more preferably the upper limit (60)" can also be combined to "10 to 60".

[0045] In addition, with respect to the numerical range, for example, according to the statement “preferably 10 to 90, more preferably 30 to 60”, the upper limit value may not be particularly limited, and only the lower limit value side may be specified as “above 10” or “above 30”. Similarly, the lower limit value may not be particularly specified, and only the upper limit value side may be specified as “below 90” or “below 60”.

[0046] In addition, unless otherwise specified, when a numerical range is abbreviated as "10 to 90", it means a range of 10 or more and 90 or less.

[0047] Similarly to the above, for example, based on the description of "preferably 10 or more, more preferably 30 or more" and the description of "preferably 90 or less, more preferably 60 or less" for the same item, the "preferable lower limit (10)" and the "more preferably upper limit (60)" may be combined to be "10 or more and 60 or less". Also, similarly to the above, only the lower limit side may be specified as "10 or more" or "30 or more", and similarly, only the upper limit side may be specified as "90 or less" or "60 or less". When the upper end of the above numerical range is "less than", the same applies when the lower limit is "more than".

[0048] In addition, in this specification, unless otherwise specified, the term "identifiability" refers to the property that, when a dental porcelain paste before firing is applied to a substrate, a portion to which the dental porcelain paste is applied and a portion not applied can be visually distinguished. Specifically, it refers to a property evaluated by the method described in the Examples.

[0049] In addition, in this specification, unless otherwise specified, when abbreviated as "calcined body", the "calcined body" means a calcined body obtained by calcining the dental porcelain paste.

[0050] [Dental porcelain paste]

[0051] One embodiment of the present invention, namely, a dental porcelain paste (hereinafter also referred to as "porcelain paste") contains a glass powder (A) (hereinafter also referred to as "component (A)"), an organic solvent (B) (hereinafter also referred to as "component (B)"), and a colorant (C) that loses color during calcination (hereinafter also referred to as "component (C)"), and satisfies at least one of the following conditions (1) and (2).

[0052] Condition (1): The color difference ΔE calculated from the color tone of the dental porcelain paste with a thickness of 0.5 mm before calcination measured using the L*a*b* color space and the color tone of the calcined body with a thickness of 0.5 mm obtained by vacuum calcining the dental porcelain paste at 740°C using the L*a*b* color space * 8.5 or above;

[0053] Condition (2): The lightness difference ΔL calculated from the lightness obtained by colorimetrically measuring the 0.5 mm thick dental porcelain paste before calcination using the L*a*b* color space and the lightness obtained by colorimetrically measuring the 0.5 mm thick calcined body obtained by vacuum calcining the dental porcelain paste at 740°C using the L*a*b* color space * It is above 6.5.

[0054] Furthermore, the dental porcelain paste can satisfy at least one of the conditions (1) and (2) by containing a coloring agent (C) that loses color during firing.

[0055] <Condition (1)>

[0056] If the color difference ΔE described in the above condition (1) * If ΔE is 8.5 or more, the difference between the color tone of the ceramic paste before firing and the color tone of the fired body obtained by firing the ceramic paste becomes larger. Therefore, for example, when the color tone of the base forming the fired body is similar to the color tone of the fired body, if ΔE * When the value of is 8.5 or more, when the ceramic paste before firing is applied to a base, the portion to which the ceramic paste is applied can be easily and clearly identified, and the recognition of the ceramic paste is improved.

[0057] From the viewpoint of further improving the visibility of the ceramic paste, the color difference ΔE * It is preferably 11.0 or more, more preferably 15.0 or more, further preferably 20.0 or more, further preferably 30.0 or more, further preferably 40.0 or more.

[0058] In addition, the color difference ΔE * There is no particular upper limit on the color difference ΔE. * It is preferably 95.0 or less, more preferably 90.0 or less, further preferably 85.0 or less, and further preferably 80.0 or less.

[0059] As described above, the lower limit and upper limit values ​​described in these stages can be independently combined. For example, in one embodiment of the present invention, the color difference ΔE * It is 8.5 to 95.0, preferably 11.0 to 95.0, more preferably 15.0 to 90.0, further preferably 20.0 to 85.0, further preferably 30.0 to 80.0, further preferably 40.0 to 80.0.

[0060] Specifically, the color difference ΔE described in the above condition (1) * The calculation was performed by the method described in the Examples.

[0061] <Condition (2)>

[0062] In addition, by making the brightness difference ΔL described in the above condition (2) * When the ratio is 6.5 or more, for the same reason as described above for condition (1), when the pre-fired ceramic paste is applied to a base, the portion to which the ceramic paste is applied can be easily and clearly identified, thereby improving the recognizability of the ceramic paste.

[0063] From the viewpoint of further improving the visibility of the ceramic paste, the brightness difference ΔL * It is preferably 11.0 or more, more preferably 15.0 or more, further preferably 18.0 or more, further preferably 20.0 or more, further preferably 25.0 or more.

[0064] In addition, the brightness difference ΔL * There is no particular upper limit on the color difference ΔL. * It is preferably 100.0 or less, more preferably 80.0 or less, and further preferably 60.0 or less.

[0065] As described above, the lower limit and upper limit values ​​described in these stages can be independently combined. For example, in one embodiment of the present invention, the brightness difference ΔL * It is 6.5 to 100.0, preferably 11.0 to 100.0, more preferably 15.0 to 80.0, further preferably 18.0 to 80.0, further preferably 20.0 to 60.0, further preferably 25.0 to 60.0.

[0066] Specifically, the color difference ΔL described in the above condition (2) * The calculation was performed by the method described in the Examples.

[0067] In addition, from the viewpoint of further improving the recognition of the dental porcelain paste, the color difference ΔE1 calculated from the color tone of the dental porcelain paste obtained by colorimetric measurement of the substrate using the L*a*b* color space and the color tone of the dental porcelain paste applied to the substrate at a thickness of 0.5 mm using the L*a*b* color space is * It is preferably 11.0 or more, more preferably 15.0 or more, further preferably 20.0 or more, further preferably 30.0 or more, further preferably 40.0 or more.

[0068] In addition, the color difference ΔE1 * There is no particular upper limit on the color difference ΔE1. * It is preferably 95.0 or less, more preferably 90.0 or less, further preferably 85.0 or less, and further preferably 80.0 or less.

[0069] As described above, the lower limit and upper limit values ​​described in these stages can be independently combined. For example, in one embodiment of the present invention, the color difference ΔE1 * It is preferably 11.0 to 95.0, more preferably 15.0 to 90.0, further preferably 20.0 to 85.0, further preferably 30.0 to 80.0, further preferably 40.0 to 80.0.

[0070] Specifically, the color difference ΔE1 * The color difference ΔE1 is calculated by the method described in the examples. * The aforementioned "substrate" used in the calculation of the color difference ΔE1 is used to calculate * The substrate specifically refers to a specific substrate described in the embodiments described later. Therefore, the type of the "substrate" to which the ceramic paste is applied is not limited, and similarly, the type of the "substrate" to which the ceramic paste is applied in the step (I) described later is not limited.

[0071] In addition, for example, from the viewpoint of further reducing the influence of the calcined body on the base color tone, the color tone of the dental porcelain paste obtained by colorimetric measurement of the base material using the L*a*b* color space and the color tone obtained by colorimetric measurement of the base material using the L*a*b* color space are * a * b * The color difference ΔE2 calculated by measuring the color tone of the calcined body in the color space * Preferably it is 3.0 or less, more preferably 2.5 or less, further preferably 2.0 or less, further preferably 1.5 or less, further preferably 1.2 or less, and the calcined body is obtained by applying the dental porcelain paste on the substrate in a manner such that the thickness after calcination becomes 65 μm, and vacuum calcining at 740°C.

[0072] In addition, the color difference ΔE2 * There is no particular lower limit for the color difference ΔE2. * It is preferably 0.0 or more.

[0073] As described above, the lower limit and upper limit values ​​described in these stages can be independently combined. For example, in one embodiment of the present invention, the color difference ΔE2 * It is preferably 0.0 to 3.0, more preferably 0.0 to 2.5, further preferably 0.0 to 2.0, further preferably 0.0 to 1.5, further preferably 0.0 to 1.2.

[0074] Specifically, the color difference ΔE2 * The color difference ΔE2 is calculated by the method described in the examples. * The "substrate" used in the calculation of refers to the substrate described in the examples described later.

[0075] Hereinafter, each component contained in the dental porcelain paste which is one embodiment of the present invention will be described in order.

[0076] <Glass powder (A)>

[0077] The glass powder (A) is not particularly limited, but is preferably a material that can be used for dental applications, and may contain crystals.

[0078] Examples of the material of component (A) include SiO 2 Glass or crystallized glass as the main component (the component with the largest content in glass). This glass contains SiO 2 In addition, Al 2 O 3 , B 2 O 3 , ZnO, K 2 O、Na 2 O. Li 2 O, ZrO 2 、CaO、MgO、Sb 2 O 3 、CeO 2 、BaO、SnO 2 etc., and it is possible to suitably use, for example, potassium aluminosilicate glass (4SiO 2 ·Al 2 O 3 ·K 2 O), potassium aluminum silicate glass of leucite crystal type, fluoroapatite glass and lithium silicate glass. Among them, amorphous potassium aluminum silicate glass is more preferred. In addition, examples of the aforementioned crystals include leucite, potassium feldspar, fluorphlogopite, diopside, mica, β-spodumene (LiAlSi 2 O 6 ), β-calcium metaphosphate, apatite, magnesium titanate, β-eucryptite, alumina, etc.

[0079] In addition, depending on the application of the porcelain paste, the component (A) may be used alone or in appropriate combination of two or more.

[0080] In addition, as the raw material of the glass used as the material of component (A), a wide range of commonly used ceramic raw materials can be used, and SiO 2 、Al 2 O 3 , B 2 O 3 , ZnO, K 2 O、Na 2 O. Li 2 O, ZrO 2 、CaO、MgO、Sb 2 O 3 、CeO 2 、BaO、SnO 2 Various oxides such as SiO2 can be formed when heated in the atmosphere.2 、Al 2 O 3 , B 2 O 3 , ZnO, K 2 O、Na 2 O. Li 2 O, ZrO 2 、CaO、MgO、Sb 2 O 3 、CeO 2 、BaO、SnO 2 or a mixture of the aforementioned oxides and the aforementioned substances that can form the aforementioned oxides when heated in the atmosphere. In this case, the composition of the obtained glass is calculated in advance, and the ratio of each raw material is determined and mixed. The method of mixing the raw materials is not particularly limited, but it is preferably uniformly dispersed.

[0081] The mixed raw materials are heated at about 700° C. or higher. The heating method is not particularly limited as long as all the raw materials are dissolved to form a uniform melt. The method for cooling the melt is also not particularly limited, and air cooling or the like can be used.

[0082] The glass block obtained by the above operation is crushed and classified to prepare a component (A) with an adjusted particle size. The method of crushing and classifying the glass block is not particularly limited. As a crushing device, compression crushers such as jaw crushers and cone crushers can be listed; ball mills such as vibrating ball mills and planetary mills; medium stirring crushers such as tower crushers, stirring trough crushers, and ring crushers; high-speed rotary impact crushers such as pin mills and disc mills; other roller mills; jet crushers; autogenous crushers, etc. As a classification device, screening classifiers such as vibrating screens and sifters can be listed; centrifugal classifiers such as cyclone separators; wet classifiers such as sedimentation classifiers, etc. It should be noted that for these crushing devices or classification devices, in order to avoid the mixing of metal impurities, it is preferred to use a device coated with resin or glass.

[0083] The average particle size of component (A) is preferably 1 to 30 μm, more preferably 2 to 20 μm, and still more preferably 3 to 9 μm. If the average particle size is 1 μm or more, it is easy to suppress the reduction of the transparency of the patch, so it is preferred. In addition, if the average particle size is 30 μm or less, it is preferred from the viewpoint of facilitating the coating operation of the porcelain paste.

[0084] The average particle size of the component (A) refers to a volume-based average particle size (D50) that can be determined by measurement using a laser diffraction scattering method, and can be measured, for example, by the method described in Examples.

[0085] From the viewpoint of being able to calcine at a lower temperature and shortening the calcination time, the glass transition temperature of component (A) is preferably 400-600°C, more preferably 420-580°C, and further preferably 450-550°C. In addition, from the same viewpoint, the softening point of component (A) is preferably 500-680°C, more preferably 520-650°C, and further preferably 550-630°C. In the case where the glass transition temperature is 400°C or above or the softening point is 500°C or above, it is preferred because the component (A) can be prevented from dripping during calcination. In addition, in the case where the glass transition temperature is 600°C or below or the softening point is 680°C or below, calcination can be performed at a low temperature, and therefore, deformation of the ceramic frame made of lithium disilicate glass ceramics or the like due to high temperature calcination can be avoided, so it is preferred.

[0086] The linear thermal expansion coefficient (50 to 500° C.) of component (A) can be appropriately selected according to the material of the substrate to which the ceramic paste is applied, and is not particularly limited, but can be 4.0×10 -6 ~6.0×10 -6 / ℃, for example, it can be 6.1×10 -6 ~13.5×10 -6 / ℃, which can be 6.3×10 -6 ~12.5×10 -6 For example, when a ceramic paste is used in a substrate containing zirconium oxide as a main component, the linear thermal expansion coefficient of the component (A) is preferably 9.0×10 -6 ~11.0×10 -6 For example, when a ceramic paste is used in a substrate having aluminum oxide as a main component, the linear thermal expansion coefficient of the component (A) is preferably 6.1×10 -6 ~8.8×10 -6 / °C. The linear thermal expansion coefficient can be measured by, for example, heating a sample from room temperature (25°C) to 500°C using a thermal analyzer TMA120 (manufactured by Seiko Instruments, with a heating rate of 5°C / min). The linear thermal expansion coefficient can be adjusted using a known method, for example, according to K 2 O content to adjust.

[0087] In the dental porcelain paste, the content of component (A) is preferably 40 to 80 parts by mass, more preferably 45 to 75 parts by mass, and even more preferably 50 to 70 parts by mass based on 100 parts by mass of the total of component (A) and component (B).

[0088] <Organic Solvent (B)>

[0089] Examples of the organic solvent (B) include esters such as dimethyl phthalate, diethyl phthalate, and dibutyl phthalate;

[0090] Monohydric alcohols such as methanol, ethanol, 1-propanol, 2-propanol, isopropanol, 1-butanol, 2-butanol, 1-heptanol, 2-heptanol, 3-heptanol, 1-hexanol, 2-hexanol, 3-hexanol, 2-methyl-1-pentanol, 3-methyl-1-pentanol, 4-methyl-1-pentanol, 2-methyl-2-pentanol, 2-methyl-3-pentanol, 2,2-dimethyl-1-butanol, and 2-ethyl-1-butanol;

[0091] 1,2-Ethanediol, 1,2-Propanediol, 1,3-Propanediol, 1,2-Butanediol, 1,3-Butanediol, 1,4-Butanediol, 2,3-Butanediol, 1,2-Pentanediol, 1,5-Pentanediol, 2,4-Pentanediol, 1,2-Hexanediol, 2,5-Hexanediol, 1-Methyl-1,3-Propanediol, 2-Methyl-1,3-Propanediol, 2-Methyl-1,4-Butanediol, 3-Methyl-1,3-Butanediol (also known as isoprene glycol), 2- Methyl-2,4-pentanediol, 3-methyl-1,5-pentanediol, 2,4-diethyl-1,5-pentanediol, 2-ethyl-1,3-hexanediol, 3-benzyloxy-1,2-propylene glycol, 4-benzyloxy-1,2-butanediol, ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, polyethylene glycol (molecular weight: 200-600), propylene glycol, dipropylene glycol, polypropylene glycol, glycerol, 1,2,3-butanetriol, 1,2,6-hexanetriol and other polyols;

[0092] Aromatic alcohols such as 2-phenoxyethanol and benzyl alcohol;

[0093] Ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, propylene glycol monopropyl ether, dipropylene glycol monoethyl ether, tripropylene glycol monomethyl ether, diethylene glycol monobutyl ether, triethylene glycol monomethyl ether and other polyol monoethers;

[0094] (Meth)acrylic acid-based polymerizable monomers such as 2-hydroxyethyl (meth)acrylate, and the like.

[0095] The component (B) can be used alone or in appropriate combination of two or more.

[0096] The component (B) is preferably at least one selected from a polyhydric alcohol, an aromatic alcohol, and a polyhydric alcohol monoether, and more preferably at least one selected from a polyhydric alcohol and an aromatic alcohol.

[0097] In addition, as component (B), among the above compounds, at least one selected from 1,2-propylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, 3-methyl-1,3-butylene glycol (also known as isopentylene glycol), 3-methyl-1,5-pentanediol, 2-ethyl-1,3-hexanediol and 2-phenoxyethanol is more preferred.

[0098] In addition, as component (B), alcohols that are liquid at 20°C are preferred.

[0099] Moreover, the boiling point of component (B) is preferably 100 to 300°C, more preferably 100 to 280°C, and even more preferably 100 to 250°C.

[0100] In the dental porcelain paste, the content of component (B) is not particularly limited, and is preferably 20 to 60 parts by mass, more preferably 25 to 55 parts by mass, and further preferably 30 to 50 parts by mass, relative to 100 parts by mass of the total of component (A) and component (B). If the content of component (B) is 20 parts by mass or more, the kneading properties of component (A) and component (B) are improved, and it is easy to paste, so it is preferred. In addition, if the content of component (B) is 60 parts by mass or less, it is easy to ensure the amount of glass components in the porcelain paste, and it is easy to carry out the coating operation of the porcelain paste, so it is preferred.

[0101] <Coloring agent (C) that loses color during calcination>

[0102] The colorant (C) that loses color during calcination loses color during calcination. Therefore, when the porcelain paste before calcination is applied to the base, it is easy to clearly identify the area where the porcelain paste is applied. On the other hand, the calcined body obtained by calcining the porcelain paste loses color due to the coloring originating from component (C), which can further reduce the influence of the calcined body on the base color tone.

[0103] Here, in this specification, the term "the color of component (C) fades during firing" means that the color of the colorant itself disappears during firing, and also includes the color of component (C) in the ceramic paste fades during firing. That is, it is considered that the reason why the coloring caused by component (C) fades is also due to the burning out of component (C) during firing.

[0104] As described above, by using the component (C), the dental porcelain paste can satisfy at least one condition selected from the above conditions (1) and (2).

[0105] In the present specification, "decolorization" of component (C) means that when a ceramic paste (I) comprising glass powder (A) and an organic solvent (B) and not containing a colorant (C) that decolorizes upon firing, and a ceramic paste (II) obtained by further adding a colorant (C) that decolorizes upon firing to the ceramic paste (I), are fired at 700° C. or higher, the color difference ΔE between the fired body of the ceramic paste (I) and the fired body of the ceramic paste (II) is obtained. * ab is preferably less than 0.50, more preferably less than 0.30, and further preferably less than 0.20. Calcination conditions other than calcination temperature and color difference ΔE * The method for measuring ab is as described in the examples below.

[0106] Component (C) preferably contains an organic dye dissolved in the above-mentioned component (B). Here, "dissolved in component (B)" means that when 1 g of the organic dye is added to 10 mL of component (B) at 25°C, no white turbidity is observed visually.

[0107] The content of the organic pigment in 100 mass % of component (C) is preferably 60 mass % or more, more preferably 80 mass % or more, further preferably 90 mass % or more, further preferably 98 mass % or more, and is 100 mass % or less.

[0108] As mentioned above, the lower limit and the upper limit of these stage-by-stage records can be combined independently of each other.For example, in one mode of the present invention, the content of aforementioned organic pigment is preferably 60~100 mass %, more preferably 80~100 mass %, further preferably 90~100 mass %, more preferably 98~100 mass % in component (C) 100 mass %.

[0109] Furthermore, the organic dye is preferably an aromatic organic dye.

[0110] The aromatic organic dye is an organic dye containing one or more optionally substituted aromatic groups, and is preferably an aromatic organic dye having an auxiliary color group in addition to a chromogenic group.

[0111] As the aforementioned chromogenic group, there is no particular limitation as long as it is an atomic group that is bonded to an aromatic ring and becomes the cause of color development. As the aforementioned atomic group, nitro, azo, acyl ketimino (>C=N-), carbonyl, carbon-carbon double bond, carbon-carbon triple bond, carbon-nitrogen heavy bond, thiocarbonyl, nitroso, oxidized azo etc. can be listed. The aforementioned aromatic organic pigment can contain one or more of these atomic groups individually or in appropriate combination.

[0112] Examples of the auxochrome group include a hydroxyl group, an amino group, a carboxyl group, a sulfone group, a halogen atom, etc. The aromatic organic dye may contain one type of these auxochrome groups alone or in appropriate combination of two or more types.

[0113] In addition, the organic pigment is preferably selected from at least one of anthraquinone compounds, azo compounds, xanthene compounds, porphyrin compounds, phthalocyanine compounds and triarylmethane compounds, more preferably selected from at least one of anthraquinone compounds, azo compounds, xanthene compounds and phthalocyanine compounds, and further preferably selected from at least one of azo compounds and phthalocyanine compounds. These compounds have good color development properties, and therefore, the content of component (C) in the aforementioned porcelain paste can be reduced. As mentioned above, it is also preferred from the viewpoint of being able to reduce the combustion residue of component (C) during calcination, being able to further inhibit bubbles and carbonization in the obtained calcined body.

[0114] In addition, specific examples of these organic dyes are not limited as long as the effects of the present invention are exhibited, and examples thereof include the following organic dyes.

[0115] In the following description, for example, the description "CI Direct Blue (25, 86, 90, 108)" means "CI Direct Blue 25, CI Direct Blue 86, CI Direct Blue 90, CI Direct Blue 108".

[0116] CI Direct Blue (25, 86, 90, 108)

[0117] CI Solvent Blue (11, 14, 18, 25, 37, 44, 45, 49, 58, 59, 68, 78, 94)

[0118] CI Acid Blue (1, 3, 7, 9, 15, 83, 90, 103, 104, 158, 161, 249)

[0119] CI basic blue (1, 3, 7, 9, 25, 105)

[0120] ·CI Disperse Blue (198)

[0121] CI Medium Blue (1)

[0122] CI Solvent Red (25, 27, 30, 35, 49, 83, 89, 100, 122, 138, 149, 150, 160, 179, 218, 230)

[0123] CI Acid Red (6, 8, 9, 13, 14, 18, 26, 27, 51, 52, 87, 88, 89, 92, 94, 97, 111, 114, 115, 134, 145, 151, 154, 180, 183, 184, 186, 198)

[0124] CI direct red (20, 37, 39, 44)

[0125] ·CI Basic Red (12, 13)

[0126] CI Disperse Red (5, 7, 13, 17, 58)

[0127] CI solvent black (3, 5, 7, 27, 28, 29, 35, 45, 46)

[0128] CI Solvent Yellow (2, 5, 14, 15, 16, 19, 21, 33, 56, 62, 77, 83, 93, 162)

[0129] CI Disperse Yellow (3, 4, 7, 31, 54, 61, 201)

[0130] CI Direct Yellow (1, 11, 12, 28)

[0131] CI Acid Yellow (1, 3, 11, 17, 23, 38, 40, 42, 76, 98)

[0132] ·CI Basic Yellow (1)

[0133] CI Solvent Violet (13, 33, 45, 46)

[0134] CI Disperse Violet (22, 24, 26, 28, 31)

[0135] ·CI Acid Violet (49)

[0136] ·CI Basic Violet (2, 7, 10)

[0137] CI Solvent Orange (1, 2, 5, 6, 37, 45, 62, 99)

[0138] CI Acid Orange (1, 7, 8, 10, 20, 24, 28, 33, 56, 74)

[0139] ·CI Direct Orange (1)

[0140] ·CI Disperse Orange (5)

[0141] CI direct brown (6, 58, 95, 101, 173)

[0142] ·CI Acid Brown (14)

[0143] The component (C) can be used alone or in appropriate combination of two or more.

[0144] In the dental porcelain paste, the content of the component (C) is not particularly limited. For example, it is easy to adjust the ΔE * , ΔL * , ΔE1 * From the viewpoint of setting the value of to a larger value, it is preferably 0.001 parts by mass or more, more preferably 0.002 parts by mass or more, further preferably 0.004 parts by mass or more, and further preferably 0.010 parts by mass or more, relative to 100 parts by mass of the total of component (A) and component (B). In addition, for example, from the viewpoint of suppressing the occurrence of bubbles and carbonization of the calcined body, it is preferably less than 0.60 parts by mass, more preferably 0.50 parts by mass or less, further preferably 0.40 parts by mass or less, and further preferably 0.30 parts by mass or less, relative to 100 parts by mass of the total of component (A) and component (B).

[0145] As described above, the lower limit and upper limit values ​​described in these stages can be independently combined. For example, in one embodiment of the present invention, in the dental porcelain paste, the content of the component (C) is preferably 0.001 parts by mass or more and less than 0.60 parts by mass, more preferably 0.002 to 0.50 parts by mass, further preferably 0.004 to 0.40 parts by mass, and further preferably 0.010 to 0.30 parts by mass, relative to 100 parts by mass of the total of the components (A) and (B).

[0146] In addition, from the viewpoint of more easily exerting the effects of the present invention, in the dental porcelain paste, the total content of component (A), component (B) and component (C) is preferably 90% by mass or more, more preferably 95% by mass or more, further preferably 98% by mass or more, further preferably 99% by mass or more, further preferably 99.5% by mass or more, and is 100% by mass or less, based on 100% by mass of the dental porcelain paste.

[0147] As described above, the lower limit and upper limit values ​​described in these stages can be independently combined. For example, in one embodiment of the present invention, in the dental porcelain paste, the total content of component (A), component (B) and component (C) is preferably 90 to 100% by mass, more preferably 95 to 100% by mass, further preferably 98 to 100% by mass, and further preferably 99.5 to 100% by mass in 100% by mass of the dental porcelain paste.

[0148] (Fluorescent agent)

[0149] From the viewpoint of reproducing the fluorescence of natural teeth, the porcelain paste preferably further contains a fluorescent agent.

[0150] The type of the fluorescent agent is not limited as long as it can exert the effect of the present invention, and examples thereof include Y 2 SiO 5 :Ce, Y 2 SiO 5 :Tb、(Y,Gd,Eu)BO 3 , Y 2 O 3 :Eu、YAG:Ce、ZnGa 2 O 4 :Zn、BaMgAl 10 O 17 :Eu et al.

[0151] These fluorescent agents can be used alone or in appropriate combination of two or more.

[0152] When the aforementioned porcelain paste contains a fluorescent agent, the content of the fluorescent agent is not particularly limited as long as the effect of the present invention is exerted. For example, from the viewpoint of easily expressing the fluorescence of natural teeth, the content is preferably 0.001 mass part or more, more preferably 0.010 mass part or more, further preferably 0.050 mass part or more, and further preferably 0.10 mass part or more, and is preferably 0.50 mass part or less, more preferably 0.45 mass part or less, further preferably 0.40 mass part or less, and further preferably 0.35 mass part or less, from the viewpoint of easily expressing the fluorescence of natural teeth.

[0153] As described above, the lower limit and upper limit values ​​described in these stages can be independently combined. For example, in one embodiment of the present invention, in the dental porcelain paste, the content of the fluorescent agent is preferably 0.001 to 0.50 parts by mass, more preferably 0.010 to 0.45 parts by mass, further preferably 0.050 to 0.40 parts by mass, and further preferably 0.10 to 0.35 parts by mass, relative to 100 parts by mass of the total of component (A) and component (B).

[0154] (Inorganic Pigments)

[0155] In addition, the ceramic paste may further contain an inorganic pigment.

[0156] The inorganic pigments are not limited in type as long as they can exert the effects of the present invention, and examples thereof include praseodymium oxide, vanadium oxide, iron oxide, nickel oxide, chromium oxide, manganese oxide, cerium oxide, tin oxide compounds (e.g., composite oxides containing tin (II) oxide and tin (IV) oxide as components (e.g., vanadium tin yellow, chrome tin red, etc.)), bismuth vanadium yellow, vanadium zirconium yellow, praseodymium yellow, cobalt blue, manganese red, chrome aluminum red, chrome iron zinc, titanium oxide (TiO 2 ), zirconium oxide (ZrO 2 ), zirconium silicate (ZrSiO 4 )wait.

[0157] These inorganic pigments can be used alone or in appropriate combinations of two or more.

[0158] When the ceramic paste contains an inorganic pigment, the content of the inorganic pigment is not particularly limited as long as the effect of the present invention is exerted. For example, the content is preferably 0.001 parts by mass or more, more preferably 0.010 parts by mass or more, further preferably 0.050 parts by mass or more, and further preferably 0.10 parts by mass or more, and is preferably 0.50 parts by mass or less, more preferably 0.45 parts by mass or less, further preferably 0.40 parts by mass or less, and further preferably 0.30 parts by mass or less, relative to 100 parts by mass of the total of component (A) and component (B).

[0159] As described above, the lower limit and upper limit values ​​described in these stages can be independently combined. For example, in one embodiment of the present invention, in the dental porcelain paste, the content of the inorganic pigment is preferably 0.001 to 0.50 parts by mass, more preferably 0.010 to 0.45 parts by mass, further preferably 0.050 to 0.40 parts by mass, and further preferably 0.10 to 0.30 parts by mass, relative to 100 parts by mass of the total of component (A) and component (B).

[0160] <Other ingredients>

[0161] The ceramic paste may contain other components as required, in addition to the components (A) to (C) and the fluorescent agent and inorganic pigment, as long as they do not hinder the effect of the present invention. Examples of such other components include water, colorants other than component (C), opacifying materials, pH adjusters, polymerization accelerators, polymerization initiators, and the like.

[0162] Here, for example, water is sometimes mixed into the dental porcelain paste as a rule when it is used. However, as long as the composition of the dental porcelain paste is satisfied and the effect of the present invention is exerted, the water mixed into the dental porcelain as a rule when it is used is not regarded as a component of the dental porcelain paste as a rule of the present invention. That is, the water mixed into the dental porcelain paste as a rule when it is used is not subjectively different from the water in the other components.

[0163] As one embodiment of the present invention, i.e., a method for producing a dental porcelain paste, for example, a method for producing a dental porcelain paste having at least the step of mixing the aforementioned component (A), component (B) and component (C), and one or more of the aforementioned fluorescent agent, inorganic pigment and other components optionally added as needed. The mixing conditions are not particularly limited, and the contained components can be added together or in batches. A conventional mixing machine can be used as the mixing machine. For example, a mortar, a twin-screw mixing machine (Twinmix), a triple-screw mixing machine (Trimix), a kneader, a planetary mixer, etc. can be listed. Among these, a mortar and a planetary mixer are preferably used.

[0164] [Applications of dental porcelain paste, etc.]

[0165] The porcelain paste can be used to make dental restorations such as ceramic inlays, onlays, veneers and crowns.

[0166] The use of the porcelain paste is not particularly limited, and the porcelain paste can be used as, for example, body porcelain (dentine-colored porcelain), neck porcelain, incisal porcelain (enamel-colored porcelain), translucent porcelain, opaque porcelain, dyed porcelain, glazed porcelain, etc.

[0167] In addition, since the dental porcelain paste of one embodiment of the present invention has a large color difference between the material used for the dental porcelain that becomes the base before firing, the applied portion and the unapplied portion of the porcelain paste applied on the base can be easily distinguished visually.

[0168] In addition, in one embodiment of the present invention, namely the dental porcelain paste, after firing, the coloring originating from the component (C) fades and there is almost no color difference with the base, so there is almost no influence on the color tone of the base, and it also has the effect of suppressing the occurrence of bubbles and black spots.

[0169] Therefore, the dental porcelain paste, which is one embodiment of the present invention, is suitable for applications requiring better identification in the coating work before firing.

[0170] Therefore, as described above, the porcelain paste is preferably used mainly as a dyeing porcelain or a glazing porcelain used for finishing a ceramic prosthesis, and is more preferably used as a glazing porcelain.

[0171] For example, when the porcelain paste is used as a glaze porcelain, it is preferably used for finishing of a dental prosthesis formed of the ceramic material. As described above, as a dental prosthesis formed of the ceramic material, PFM type, PFZ type, FCZ type, LDS type, etc. are known as representative examples.

[0172] Among these, the surface of the FCZ type is also zirconium oxide, so it is impossible to obtain a polishing effect by the self-glazing effect, so it is necessary to apply the porcelain paste in a predetermined thickness (for example, 20 μm or more) for polishing. As described above, the porcelain paste has excellent recognition ability and is easy to adjust the coating thickness. Therefore, among the various types of dental prostheses described above, the porcelain paste can be suitably used for the FCZ type dental prostheses.

[0173] As another embodiment of the present invention, the use of the dental porcelain paste for treating teeth (for example, aesthetic dental treatment, treatment of defective teeth, prosthetic and repair treatment of artificial teeth, treatment of caries, etc.) can be cited.

[0174] The above-mentioned porcelain paste may be used alone or in appropriate combination of two or more kinds as long as the effects of the present invention are exhibited.

[0175] [Dental porcelain kit]

[0176] A dental porcelain kit according to one embodiment of the present invention includes the dental porcelain paste according to one embodiment of the present invention and a color sample for matching the coating thickness of the dental porcelain paste.

[0177] The dental porcelain paste included in the dental porcelain kit is the same as the paste described in the dental porcelain paste section, and its applicable aspects are also the same.

[0178] The color sample for matching the coating thickness of the dental porcelain paste is used to judge the coating thickness of the porcelain paste based on the color tone of a coating film when the dental porcelain paste before firing is applied to a specific base.

[0179] As an example of the color sample, there is no particular limitation as long as the user can visually confirm the color tone when the ceramic paste is applied to a specific substrate such as a zirconia substrate at a specific thickness. For example, in order to enable the user of the ceramic paste to visually confirm, the color tone when the ceramic paste is applied to a specific substrate at a specific thickness may be reproduced and colored on a paper surface, a plastic plate, a metal plate, a ceramic plate, etc., or in fact, it may be a photograph or a physical sample of the ceramic paste at each coating thickness.

[0180] As one form of the aforementioned color sample, for example, in the case of applying the aforementioned ceramic paste to a substrate in a range of 20 to 40 μm, a color sample can be listed in which, within this range, a user can visually confirm the color tone of the ceramic paste applied at each specified thickness interval (e.g., the color tone when the thickness is 20 μm, the color tone when the thickness is 25 μm) or within a specified thickness range (e.g., the color tone when the thickness is 20 to 25 μm, the color tone when the thickness is 25 to 30 μm).

[0181] In addition, the base used for preparing the color sample is not particularly limited. For example, when a base made of zirconium oxide is used as the base, the color sample can be prepared as a color sample that can confirm the color tone of the coating surface formed by applying the ceramic paste to the zirconium oxide base with a specific thickness.

[0182] [Method for producing dental prosthesis]

[0183] One aspect of the present invention, that is, a method for producing a dental prosthesis, comprises: a step (I) of applying the dental porcelain paste according to one aspect of the present invention to a substrate; and a step (II) of calcining the dental porcelain paste applied to the substrate.

[0184] <Step (I)>

[0185] In the step (I), the dental porcelain paste is applied to a substrate.

[0186] The dental porcelain paste used in step (I) is the same as the paste described in the above section of the dental porcelain paste, and its suitable mode is also the same.

[0187] In step (I), the "substrate" (base) to which the ceramic paste is applied is not particularly limited and can be appropriately selected depending on the application of the ceramic paste.

[0188] For example, when the porcelain paste is used as a glaze porcelain, it is preferably used for finishing the dental prosthesis of the ceramic material. Examples of the base material in the dental prosthesis of these ceramic materials include zirconia (zirconium oxide), aluminum oxide (aluminum oxide), feldspar-based glass, lithium disilicate glass, and the like.

[0189] As described above, among these, since zirconium oxide cannot obtain a glazing effect through an automatic glazing effect, it is necessary to apply a ceramic paste with a predetermined thickness (for example, 20 μm or more) for glazing. As described above, the ceramic paste has excellent recognition ability and is easy to adjust the coating thickness. Therefore, the ceramic paste can be suitably used for a substrate formed of zirconium oxide.

[0190] In addition, there is no particular limitation on the shape of the substrate. For example, when the porcelain paste is used as a glazing porcelain, as described above, it is preferably used for finishing a dental prosthesis made of a ceramic material. Therefore, the shape of the substrate is preferably processed into the shape of a dental prosthesis.

[0191] In step (I), as a method for applying (attaching) the aforementioned porcelain paste to the substrate, it can be carried out using, for example, a pen or a brush. In addition, it can also be carried out using a spray depending on the type of the aforementioned porcelain paste. Furthermore, it can also be carried out by immersing the substrate in a container filled with the aforementioned porcelain paste. At this time, in order to prevent the coating agent from flowing into the inner surface of the substrate, it is preferably sealed in advance.

[0192] The thickness of the coating film formed by applying the ceramic paste can be appropriately set according to the application. For example, when the ceramic paste is used as a glazing ceramic, the obtained calcined body has a predetermined thickness, which facilitates glazing. Therefore, the thickness is preferably 10 μm or more, more preferably 15 μm or more, and further preferably 20 μm or more. In addition, from the viewpoint of preventing the inclusion of bubbles due to the excessive thickness of the ceramic paste and reducing the influence of the thickness of the obtained calcined body on the occlusal surface, occlusal diameter, and contact between the prostheses, the thickness is preferably 50 μm or less, more preferably 45 μm or less, and further preferably 40 μm or less.

[0193] In addition, in step (I), it is preferred to use the sample for matching the coating thickness of the dental ceramic paste described in the column of the dental ceramic kit. That is, in step (I), it is preferred to use one embodiment of the present invention, that is, the dental ceramic kit.

[0194] As described above, by using the coating thickness matching sample, it is easy to adjust the coating thickness to a predetermined thickness even when the coating operation is performed visually or manually.

[0195] The sample for matching the coating thickness of the dental porcelain paste preferably used in step (I) is the same as the sample described in the section of the dental porcelain kit, and the suitable mode thereof is also the same.

[0196] <Step (II)>

[0197] In step (II), the dental porcelain paste applied to the substrate is fired.

[0198] The calcination temperature (maximum calcination temperature) when calcining the above-mentioned porcelain paste can be appropriately set according to the type of porcelain, usage form, type of substrate, etc., and is not particularly limited as long as it is a temperature that causes component (C) to decolorize by calcination. It is preferably above 700°C, more preferably above 720°C, and further preferably above 730°C, and is preferably below 1050°C, more preferably below 1000°C, and further preferably below 980°C.

[0199] As described above, the lower limit and upper limit described in these stages can be independently combined. For example, in one embodiment of the present invention, in the step (II), the calcination temperature is preferably 700 to 1050°C, more preferably 720 to 1000°C, and even more preferably 730 to 980°C.

[0200] The heating temperature during calcination to the maximum calcination temperature can be appropriately changed according to the type of porcelain material and is not particularly limited, but is preferably 10 to 70°C / min, more preferably 15 to 60°C / min, and further preferably 20 to 50°C / min.

[0201] In addition, before calcining, the aforementioned porcelain paste may be dried, and the drying conditions are not particularly limited. Furthermore, from the viewpoint of significantly reducing the bubbles present inside the glass powder (A), the transparency of the obtained dental prosthesis is better, and a better aesthetics can be obtained, the aforementioned calcination may be performed as vacuum calcination under vacuum. The degree of vacuum in vacuum calcination is not particularly limited, for example, it may be less than 750 mmHg, or less than 730 mmHg. The temperature for starting vacuuming is not particularly limited, for example, it may be 550 to 700°C. In addition, in the case of vacuum calcination, heating may be performed under vacuum conditions when the temperature is raised, and when the maximum calcination temperature is reached, it may be opened to atmospheric pressure and retained under atmospheric pressure conditions.

[0202] The present invention includes various combinations of the above-described configurations within the scope of the technical concept of the present invention as long as the effects of the present invention are exhibited.

[0203] Example

[0204] Next, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to these Examples at all.

[0205] <Production of glass powder>

[0206] SiO 2 、Al 2 O 3 , ZnO, K 2 O、Na 2 O. Li 2O, CaO, MgO, Sb 2 O 3 、CeO 2 The amorphous potassium aluminum silicate glass frit formed with BaO was pulverized with a planetary mill to produce powders with average particle sizes as shown in Tables 1 and 2 below. The average particle size was measured by a laser diffraction / scattering method for the average particle size (D50) based on volume. The measuring device used was "Microtrac (registered trademark) MT3300II" (manufactured by Microtrac Bel Co.), and water was used as a dispersion medium for the measurement.

[0207] [Examples 1 to 14 and Comparative Example 1]

[0208] The components described in the following Tables 1 and 2 were mixed in a mortar at room temperature (25° C.) at the contents (parts by mass) described in Tables 1 and 2 for about 10 minutes to prepare a dental porcelain paste.

[0209] [Evaluation of dental porcelain paste]

[0210] The properties of each of the ceramic pastes prepared in each of the Examples and Comparative Examples were measured by the following methods. The obtained evaluation results are shown in Tables 1 and 2 below.

[0211] <Evaluation of color tone of dental porcelain paste before firing>

[0212] Each ceramic paste was put into a stainless steel ring (inner diameter 15 mm, thickness 0.5 mm), and pressed from the top and bottom using two slides ("ASLAB (registered trademark) slide" manufactured by ASONE, width 25 mm, length 75 mm, thickness 1 mm), and measured using a spectrophotometer ("CM-3610A": manufactured by KONICAMINOLTA, D65 light source, geometric conditions c (di: 8°, de: 8°), diffuse illumination: 8° light reception, measurement mode SCI, ), measured against a white background * a * b * Value (JIS Z 8781-4: 2013 Color Measurement-Part 4: CIE1976 L * a * b * The result is set as the color tone L1 of the dental porcelain paste before calcination. * 、a1 * 、b1 * (n=3).

[0213] <Evaluation of color tone of fired body after firing of ceramic paste>

[0214] Each porcelain paste was vacuum calcined at a maximum calcination temperature of 740°C, and ground with #1500 grinding paper to obtain a calcined body with an inner diameter of 15 mm and a thickness of 0.5 mm. The calcination conditions other than the aforementioned maximum calcination temperature were carried out under the following conditions: the drying time before calcination was 6 minutes; the calcination start temperature was 400°C; the heating rate was 45°C / minute; the vacuum start temperature was 650°C; the vacuum degree was 720 mmHg, and when it reached 740°C, it was opened (vacuum released) to atmospheric pressure and retained for 1 minute; after retention, it was rapidly cooled to room temperature (25°C).

[0215] Each calcined body was pressed from the top and bottom by two slides ("ASLAB (registered trademark) slides" manufactured by AS ONE, width 25 mm, length 75 mm, thickness 1 mm) and measured using a spectrophotometer ("CM-3610A": manufactured by KONICAMINOLTA, D65 light source, geometric conditions c (di: 8°, de: 8°), diffuse illumination: 8° light reception, measurement mode SCI, ), measured against a white background * a * b * Value (JIS Z 8781-4: 2013 Color Measurement-Part 4: CIE1976 L * a * b * The result is set as the color tone L2 of the calcined body. * 、a2 * 、b2 * (n=3).

[0216] <Calculation of color tone difference before and after calcination>

[0217] Based on the color tone of the porcelain paste before firing and the color tone of the fired body obtained by firing the porcelain paste, the color tone change (color tone difference) of the porcelain paste before and after firing was calculated using the following calculation formula.

[0218] ΔE * ={(L2 * -L1 * ) 2 +(a2 * -a1 * ) 2 +(b2 * -b1 * ) 2} 1 / 2

[0219] ΔL * =|L2 * -L1 * |

[0220] The above ΔE * is the color difference ΔE involved in the above condition (1) * In addition, the above ΔL * is the brightness ΔL involved in the above condition (2) * .

[0221] <Preparation of base material>

[0222] A substrate used in the evaluation described later was produced.

[0223] First, as a sample, a disk having a diameter of 19 mm and a thickness of 1.6 mm was cut from dental zirconium oxide (trade name "KATANA (registered trademark) Ziroconia STMLA3", thickness 14 mm, manufactured by Kuraray Noritake Dental Co., Ltd.) using a dental cutting machine DWX-51D (manufactured by Roland DG) to produce a molded product.

[0224] Next, the molded product was calcined in the atmosphere from room temperature (25°C) using a calcination furnace manufactured by SK Medical Electronics (trade name "Noritake Katana (registered trademark) F-1N"), the temperature was raised to 1550°C at a heating rate of 10°C / min, and the molded product was calcined at 1550°C (atmospheric calcination) for 2 hours. The product was then ground using #1500 grinding paper to produce a substrate consisting of a disc-shaped zirconia sintered body having a diameter of 14 mm and a thickness of 1.2 mm.

[0225] <Evaluation of the Identification of Porcelain Paste>

[0226] Each of the prepared ceramic pastes was applied to the substrate produced above, and the visibility of the applied portion was evaluated according to the following criteria (n=3).

[0227] "A": The applied portion of the paste can be clearly identified visually.

[0228] "F": The color difference between the base material and the ceramic paste is unclear, and it is difficult to visually identify the application site.

[0229] <Color difference between the porcelain paste and the substrate before firing ΔE1 * Calculation>

[0230] First, the substrate prepared above was measured using a spectrophotometer ("CM-3610A": manufactured by Konica Minolta, D65 light source, geometric conditions c (di: 8°, de: 8°), diffuse illumination: 8° light reception, measurement mode SCI, ), measured against a white background * a * b *Value (JIS Z 8781-4: 2013 Color Measurement-Part 4: CIE1976 L * a * b * The result is set as the hue L3 of the substrate * 、a3 * 、b3 * (n=3) The color tone of the aforementioned substrate is L3 * =73.4, a3 * =4.0, b3 * =27.4.

[0231] Next, a stainless steel ring (15 mm in inner diameter, 0.5 mm in thickness) was placed on the substrate, and each of the prepared ceramic pastes was placed in the ring. Thereafter, a carrier sheet (AS ONE's "ASLAB (registered trademark) carrier sheet", 25 mm in width, 75 mm in length, 1 mm in thickness) was used for crimping from above, and a spectrophotometer (KONICA MINOLTA's "CM-3610A") was used to measure the color under the same conditions as above (L * a * b * The result is set as the color tone L4 after the paste is applied. * 、a4 * 、b4 * (n=3).

[0232] The color difference ΔE1 between the dental porcelain paste and the substrate before calcination is calculated according to the following formula: * .

[0233] ΔE1 * ={(L4 * -L3 * ) 2 +(a4 * -a3 * ) 2 +(b4 * -b3 * ) 2} 1 / 2

[0234] <Evaluation of bubbles and carbonization after calcination>

[0235] Each of the prepared ceramic pastes was applied onto the substrate prepared above and then vacuum fired at 740°C to obtain a fired body. The fired bodies were observed at 100 times magnification using an optical microscope ("DIGITAL MICROSCOP EKH-7700" manufactured by HIROX Corporation) to evaluate the presence of bubbles and carbides.

[0236] As an evaluation standard, a conventional dental porcelain material ("CERBIAN (registered trademark) ZR FC paste-dyed Clear Glaze", manufactured by Kuraray Noritake Dental Co., Ltd.) was used and vacuum calcined at a calcination temperature of 750°C. The calcined body obtained was observed using the same optical microscope as above and the same operation was performed. The results were compared and evaluated as follows (n=3).

[0237] "A": Compared with conventional dental porcelain, bubbles and black spots are not observed to the same extent.

[0238] "B": Compared with conventional dental porcelain, it has more bubbles, but it is not a problem in terms of practicality, and no black spots are observed.

[0239] "F": Compared with conventional dental porcelain, there are significantly more bubbles, black spots are observed, or both problems exist.

[0240] <Color difference between calcined body and substrate ΔE2 * Calculation>

[0241] First, the substrate prepared above was measured using a spectrophotometer ("CM-3610A": manufactured by Konica Minolta, D65 light source, geometric conditions c (di: 8°, de: 8°), diffuse illumination: 8° light reception, measurement mode SCI, ), measured against a white background * a * b * Value (JIS Z 8781-4: 2013 Color Measurement-Part 4: CIE1976 L * a * b * The result is set as the hue L3 of the substrate * 、a3 * 、b3 * (n=3) The color tone of the aforementioned substrate is L3 * =73.4, a3 * =4.0, b3 * =27.4.

[0242] Next, each of the prepared ceramic pastes was applied to the substrate so that the thickness of the calcined body after calcination was 65 μm, and then vacuum calcined at a maximum calcination temperature of 740°C to obtain a calcined body. The calcination conditions other than the maximum calcination temperature were as follows: the drying time before calcination was 6 minutes; the calcination start temperature was 400°C; the heating rate was 45°C / min; the vacuum start temperature was 650°C; the vacuum degree was 720 mmHg; when the temperature reached 740°C, the vacuum was released to atmospheric pressure and retained for 1 minute; after the retention, the calcined body was rapidly cooled to room temperature (25°C).

[0243] The color of each calcined body obtained was measured using a spectrophotometer ("CM-3610A" manufactured by Konica Minolta) under the same conditions as above (L * a * b * The result is set as the color tone L5 of the calcined body. * 、a5 * 、b5 * The color difference ΔE2 between the calcined body obtained after calcining the porcelain paste and the substrate is calculated according to the following formula: * (n=3).

[0244] ΔE2 * ={(L5 * -L3 * ) 2 +(a5 * -a3 * ) 2 +(b5 * -b3 * ) 2} 1 / 2

[0245] [Table 1]

[0246] Table 1

[0247]

[0248] (※1): Color tone of the porcelain paste (thickness 0.5 mm) before firing (※2): Color tone of the fired body (thickness 0.5 mm) obtained by firing the porcelain paste

[0249] [Table 2]

[0250] Table 2

[0251]

[0252] (※1): Color tone of the porcelain paste (thickness 0.5mm) before firing

[0253] (※2): Color tone of the fired body (thickness 0.5 mm) obtained by firing the porcelain paste

[0254] The results in Tables 1 and 2 show that, for the ceramic pastes of Examples 1 to 14 containing components (A) to (C) and satisfying at least one of the conditions (1) and (2), the color difference ΔE1 between the ceramic paste before firing and the substrate coated with the paste is * Large, excellent identification in the coating work before calcination.

[0255] In addition, it can be seen that after the ceramic pastes of Examples 1 to 14 are fired, the color difference ΔE2 between the fired body obtained by firing the ceramic paste and the substrate is * The color tone of the base material is almost not affected. Furthermore, the porcelain pastes of Examples 1 to 13 have the same level of bubbles generated in the calcined body as compared with conventional dental porcelain, and no black spots are observed. In addition, the porcelain paste of Example 14 has more bubbles generated in the calcined body than conventional dental porcelain, but it is not a problem in terms of practicality, and no black spots are observed.

[0256] Therefore, it is understood that the dental porcelain paste, which is one aspect of the present invention, is suitable for applications requiring further identification in the coating work before firing.

[0257] Industrial Applicability

[0258] As described above, the dental porcelain paste of one embodiment of the present invention has a large color difference with the base material that becomes the base before firing, so that the applied part and the unapplied part of the porcelain paste can be easily distinguished even by visual observation. Therefore, the dental porcelain paste of one embodiment of the present invention can avoid the occurrence of coating leakage of the porcelain paste and can also easily adjust the coating thickness, so it is excellent in recognition during the coating operation before firing.

[0259] In addition, one embodiment of the present invention, namely the dental porcelain paste, changes its color tone after firing, and has almost no color difference from the base, so it has almost no effect on the base color tone, and also has the effect of suppressing the occurrence of bubbles and black spots.

[0260] Therefore, the dental porcelain paste which is one embodiment of the present invention can also be suitably used as, for example, a glazing porcelain.

[0261] In recent years, the demand for ceramic prostheses has been increasing, and as personal aesthetics improve, the frequency of use of dental ceramics is expected to increase. Therefore, from this viewpoint, one embodiment of the present invention, that is, a dental ceramic paste, is also useful.

Claims

1. A dental porcelain paste comprising a glass powder (A), an organic solvent (B), and a colorant (C) that loses color when fired, wherein the dental porcelain paste satisfies at least one of the following conditions (1) and (2). Condition (1): Based on the use of L * a * b * Color space The color tone of the dental porcelain paste with a thickness of 0.5 mm before calcination and the color space of the dental porcelain paste with a thickness of 0.5 mm before calcination were measured ... * a * b * Color space The color difference ΔE calculated from the color tone of the calcined body with a thickness of 0.5 mm obtained by vacuum calcining the dental porcelain paste at 740°C * 8.5 or above; Condition (2): Based on the use of L * a * b * Color space The lightness of the dental porcelain paste with a thickness of 0.5 mm before calcination and the lightness obtained by L * a * b * Color space The lightness difference ΔL is calculated by measuring the lightness of a calcined body having a thickness of 0.5 mm obtained by vacuum calcining the dental porcelain paste at 740°C. * It is above 6.

5.

2. The dental porcelain paste according to claim 1, wherein: According to the use of L * a * b * The hue obtained by measuring the color of the substrate in color space and the color tone obtained by using L * a * b * Color space: Color difference ΔE1 calculated from the color tone obtained by colorimetric measurement of the dental porcelain paste applied on the substrate at a thickness of 0.5 mm * It is above 11.

0.

3. The dental porcelain paste according to claim 1 or 2, wherein: According to the use of L * a * b * The hue obtained by measuring the color of the substrate in color space and the color tone obtained by using L * a * b * The color difference ΔE2 calculated by measuring the color tone of the calcined body in the color space * The calcined body is obtained by applying the dental porcelain paste on the substrate so that the thickness after calcination is 65 μm, and calcining the dental porcelain paste at 740° C. in a vacuum.

4. The dental porcelain paste according to any one of claims 1 to 3, wherein The content of the component (C) is 0.001 parts by mass or more and less than 0.60 parts by mass based on 100 parts by mass of the total of the components (A) and (B).

5. The dental porcelain paste according to any one of claims 1 to 4, wherein The component (C) contains an organic pigment dissolved in the component (B).

6. The dental porcelain paste according to claim 5, wherein: The organic pigment is an aromatic organic pigment.

7. The dental porcelain paste according to claim 5 or 6, wherein: The organic pigment is at least one selected from anthraquinone compounds, azo compounds, xanthene compounds, porphyrin compounds, phthalocyanine compounds and triarylmethane compounds. 8 . The dental porcelain paste according to claim 1 , comprising a fluorescent agent.

9. The dental porcelain paste according to claim 8, wherein: The content of the fluorescent agent is 0.001 to 0.50 parts by mass based on 100 parts by mass of the total of components (A) and (B). 10 . The dental porcelain paste according to claim 1 , comprising an inorganic pigment. 11 . A dental porcelain kit comprising the dental porcelain paste according to claim 1 and a color sample for matching the coating thickness of the dental porcelain paste.

12. A method for producing a dental prosthesis, comprising: A step (I) of applying the dental porcelain paste according to any one of claims 1 to 10 to a substrate; and a step (II) of firing the dental porcelain paste applied to the substrate.

13. The method for manufacturing a dental prosthesis according to claim 12, wherein: The calcination temperature in the step (II) is 700° C. or higher.

14. The method for producing a dental prosthesis according to claim 12 or 13, wherein: The step (I) includes an operation of matching the coating thickness of the dental porcelain paste with a color sample.

Citation Information

Patent Citations

  • Aluminosilicate glass and color tone adjustment composition for ceramics based dental crown porcelain

    JP2009207743A

  • Pasty dental porcelain

    JP2017193492A