High-strength heap plastic glaze paste for false tooth repair and preparation method of high-strength heap plastic glaze paste

By preparing high-strength buildable glaze and combining it with zirconia whiskers for toughening, one-time low-temperature sintering is achieved, which solves the high time cost and cracking risk caused by multiple high-temperature sintering, simplifies the denture repair process, and improves the strength and toughness of the glaze.

CN120647154APending Publication Date: 2025-09-16CHENGDU BESMILE MEDICAL TECH CORP LTD
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Patent Information

Application Number
CN202510796066.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-16
Publication Date
2025-09-16

AI Technical Summary

Technical Problem

In the current denture aesthetic restoration process, multiple high-temperature sintering results in high time costs and increases the risk of cracking of the restoration. In addition, manual porcelain powder modeling requires high technical experience from the technician and is complex to operate.

Method used

A high-strength, buildable glaze paste is used, which contains glass powder and zirconia whiskers of different particle sizes and melting points, and a mixed blending liquid to achieve one-time low-temperature sintering to complete denture restoration. Combined with the toughening effect of zirconia whiskers, the sintering temperature is reduced to 780°C, reducing high-temperature operations.

Benefits of technology

It simplifies the denture restoration process, reduces the number of sintering times, and reduces the risk of cracking of the restoration. At the same time, it improves the strength and toughness of the glaze and reduces the complexity of the operation.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of false tooth repair materials, in particular to high-strength heap plastic glaze paste for false tooth repair and a preparation method of the high-strength heap plastic glaze paste. According to the specific technical scheme, the high-strength heap plastic glaze paste for false tooth repair comprises glass powder A, glass powder B and zirconium oxide whiskers. The dental plastifiable glaze paste is formed by preparing glass powder with different particle sizes and different melting points, adding zirconium oxide whiskers and mixing and adding the blending liquid, the form is repaired through the plastifiable glaze paste after glazing and polishing, glazing is carried out through common transparent glaze paste, sintering is completed at a time, the sintering frequency is small, time is shortened, and the production cost is reduced. And the cracking risk of the restoration body is also reduced.
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Description

Technical Field

[0001] The present invention relates to the technical field of denture restoration materials, and in particular to a high-strength buildable glaze paste for denture restoration and a preparation method thereof. Background Art

[0002] The application of dental porcelain powder in aesthetic denture restoration is a key technology for restoring the natural form, color, and function of teeth. Achieving the same aesthetic effect as natural teeth requires polishing, shaping, filling, and subsequent glazing, requiring at least three sintering cycles. Furthermore, the steps involved in aesthetic denture restoration are complex, and the manual application of porcelain powder requires a high level of technical experience and a long training cycle. Inexperienced technicians are prone to causing shrinkage and chipping during the application process.

[0003] Currently, most porcelain powders on the market are high-temperature ones. Trimming, polishing, and then re-sintering significantly increases time and costs. Multiple high-temperature sintering also increases the risk of cracking in restorations. The specific process is: porcelain application (sintering above 900°C) - trimming and polishing - porcelain shaping and sintering (sintering above 900°C) - glazing (sintering at 780°C). Summary of the Invention

[0004] In response to the deficiencies of the prior art, the present invention provides a high-strength buildable glaze paste for denture restoration and a preparation method thereof, which can simultaneously have the functions of shaping (generally only porcelain powder has the shaping function) and glazing.

[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions:

[0006] The invention discloses a high-strength buildable glaze for denture restoration, comprising glass powder A, glass powder B and zirconium oxide whiskers; the glass powder A comprises, by mass percentage, 50-60% SiO2, 10-20% B2O3, 1-5% CaO, 10-15% Al2O3, 5-10% Na2O, 5-15% K2O, 0-3% Li2O, 1-5% F - , 0-2% SnO2, 0-2% ZnO, 0-2% Y2O3, 0-2% CeO2, 1-8% ZrO2, 0-2% BaO, 0-2% MgO;

[0007] The glass powder B comprises 40-65% SiO2, 5-10% B2O3, 1-5% CaO, 10-15% Al2O3, 5-10% Na2O, 5-10% K2O, 0-1% Li2O, 0-1% F -, 0-2% SnO2, 1-2% ZnO, 0-2% Y2O3, 0-2% CeO2, 1-5% ZrO2, 1-2% BaO, 0-2% MgO.

[0008] Preferably, the particle size D50 of the glass powder A is controlled to be 10-50 μm.

[0009] Preferably, the particle size D50 of the glass powder B is controlled to be 10-50 μm.

[0010] Preferably, the zirconia whiskers have a particle size of 2-4 μm and a length of 20-300 μm.

[0011] Preferably, in terms of mass percentage, the amount of the glass powder A is 30-60wt%, the amount of the glass powder B is 40-70wt%, and the amount of the zirconia whisker added is 0.3-5wt% of the total amount of the glass powder A and the glass powder B.

[0012] Correspondingly, a method for preparing a high-strength buildable glaze for denture restoration comprises mixing glass powder A, glass powder B and zirconia whiskers, adding a blending liquid, and mixing to obtain a buildable glaze.

[0013] Preferably, the blending solution comprises 50%-60% 1-3 butanediol and 30%-60% diethanolamine in terms of mass percentage.

[0014] Preferably, after the components of glass powder A are mixed, they are sintered at 1500°C for 1 hour, and then water quenched, dried, crushed, and air flow milled in sequence to 10-50 μm to prepare glass powder A with a softening temperature of 650-800°C.

[0015] Preferably, the preparation process of the glass powder B is as follows: after mixing the components of the glass powder B, sintering at a high temperature of 1500°C for 1 hour, and then water quenching, drying, crushing, and air flow grinding in sequence, and grinding to 10-50μm to prepare glass powder B with a softening temperature of 350-500°C.

[0016] Preferably, during the process of repairing the denture, the denture after correction and polishing is filled with a buildable glaze, and ordinary transparent glaze is applied and then sintered at 780° C. in one go.

[0017] The present invention has the following beneficial effects:

[0018] 1. The present invention prepares glass powders of different particle sizes and melting points, adds zirconium oxide whiskers, and mixes and adds a blending liquid to form a dental buildable glaze (also known as a 3D glaze). After porcelain polishing, the 3D glaze is used to repair the shape, and ordinary glaze is used for glazing, and the sintering is completed in one step.

[0019] 2. Compared with the existing technology, the present invention can complete the aesthetic restoration of dentures through porcelain coating → sintering at above 900℃ → trimming and polishing → 3D glaze filling, and ordinary glaze coating → one-time sintering at 780℃. The whole restoration process has fewer sintering times, less time, and also reduces the risk of cracking of the restoration.

[0020] 3. The 3D glaze prepared by the present invention has the characteristics of low-temperature sintering (sintering at 780°C for 3 minutes). The low-temperature sintering can be used for appearance repair and ordinary glazing materials can be sintered at the same time, reducing the high-temperature porcelain repair (sintering at 900°C) operation, and avoiding the risk of cracks in the base material caused by high-temperature sintering.

[0021] 4. 3D glaze's plasticity: While similar to high-temperature porcelain powder in its plasticity, it differs from ordinary glazes in its fluidity, exhibiting thixotropy. The key characteristic of thixotropy is that it transforms from a gel to a sol state under external force, returning to the gel state upon removal of the external force. This characteristic allows 3D glazes to be used for plasticity. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The stackable glaze prepared by the present invention is in a static state (left picture) and in a static state after being shaped (right picture);

[0023] Figure 2 Schematic diagram of the shape of the buildable glaze before sintering (left) and after sintering (right). DETAILED DESCRIPTION

[0024] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0025] Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art.

[0026] The invention discloses a high-strength buildable glaze for denture restoration, comprising glass powder A, glass powder B and zirconium oxide whiskers; the glass powder A comprises, by mass percentage, 50-60% SiO2, 10-20% B2O3, 1-5% CaO, 10-15% Al2O3, 5-10% Na2O, 5-15% K2O, 0-3% Li2O, 1-5% F -, 0-2% SnO2, 0-2% ZnO, 0-2% Y2O3, 0-2% CeO2, 1-8% ZrO2, 0-2% BaO, 0-2% MgO;

[0027] The glass powder B comprises 40-65% SiO2, 5-10% B2O3, 1-5% CaO, 10-15% Al2O3, 5-10% Na2O, 5-10% K2O, 0-1% Li2O, 0-1% F - , 0-2% SnO2, 1-2% ZnO, 0-2% Y2O3, 0-2% CeO2, 1-5% ZrO2, 1-2% BaO, 0-2% MgO.

[0028] In the above ratio, for F - It can be introduced by adding raw materials such as CaF2, Na3AlF6, etc.

[0029] Furthermore, the particle size D50 of the glass powder A is controlled to be 10-50 μm. The particle size D50 of the glass powder B is controlled to be 10-50 μm. The particle size of the zirconia whisker is 2-4 μm, and the length is 20-300 μm.

[0030] Furthermore, in terms of mass percentage, the amount of the glass powder A is 30-60 wt %, the amount of the glass powder B is 40-70 wt %, and the amount of the zirconia whisker added is 0.3-5 wt % of the total amount of the glass powder A and the glass powder B.

[0031] The present invention discloses a method for preparing a high-strength, buildable glaze for denture restoration. The method comprises mixing glass powder A, glass powder B, and zirconium oxide whiskers according to the aforementioned proportions and components, adding a blending liquid at a solid-to-liquid ratio of 1:0.35, and mixing to obtain a buildable glaze (also known as a 3D glaze). The blending liquid comprises, by mass percentage, 50%-60% 1-3-butanediol and 30%-60% diethanolamine.

[0032] Furthermore, by preparing glass powder A with a high softening temperature (650-800°C) and controlling its particle size, it is used as a skeleton for the buildable glaze. The particle size D50 is controlled to 10-50 μm, accounting for 30-60% by weight. The preparation process of the glass powder A is as follows: according to the components of the glass powder A, mixing, sintering (1500°C, 1 hour), water quenching, drying (80°C), crushing, and air flow milling (10-50 μm), finally preparing glass powder A with a softening temperature of 650-800°C.

[0033] Furthermore, by preparing glass powder B with a low softening temperature (350-500°C) and controlling its particle size, the low-temperature fusible material serves as an infiltrant for the high-temperature glass, eliminating gaps between unmelted high-temperature glass particles. The low-temperature glass powder particle size D50 is controlled to be 10-50 μm, accounting for 40-70% by weight. The preparation process of the glass powder B is as follows: according to the components of the glass powder B, mixing, sintering (1500°C, 1 hour), water quenching, drying (80°C), crushing, and air flow milling (10-50 μm), finally preparing glass powder B with a softening temperature of 350-500°C.

[0034] In the present invention, the difference in softening temperature between glass frits A and B is determined by the differences in their components. Silicon dioxide is the primary constituent of the glass network; the higher its content, the higher the softening temperature. Borosilicate glass has a higher softening point due to the addition of B2O3. Alkaline oxides such as Na2O and K2O disrupt the silicon-oxygen network, lowering the softening point. CaO improves the high-temperature stability of the glass. By adjusting the content of different components, glasses with different softening temperatures can be obtained.

[0035] Furthermore, zirconium oxide whiskers with a particle size of 2-4 μm and a length of 20-300 μm can be added to the molding glaze. The strength and toughness of the glaze can be greatly improved by whisker toughening. The amount of zirconium oxide whiskers added accounts for 0.3-5 wt% of the total amount of glass powder A and glass powder B.

[0036] During the use of buildable glaze, the denture is polished and then restored with buildable glaze. A standard transparent glaze is then applied to simulate a natural tooth. This process is sintered in one go at 780°C for 3 minutes. The standard transparent glaze is commercially available. It's important to note that during the glazing process, a commercially available colored glaze can be selected based on the denture's color.

[0037] The present invention will be further described below with reference to specific embodiments.

[0038] Example 1

[0039] 1. The amounts of the components of glass powder A and glass powder B are shown in Table 1 below.

[0040] Table 1 Amount of each component of glass powder A and glass powder B

[0041]

[0042] 2. According to the components in Table 1, glass powder A with a softening temperature of 680°C and glass powder B with a softening temperature of 490°C were prepared by the preparation methods of glass powder A and glass powder B, respectively.

[0043] 3. Weigh 35wt% of the glass powder A, 65wt% of the glass powder B and 3wt% of the total amount of glass powder A and glass powder B, mix them, add the blending liquid, and mix well to obtain a compostable glaze paste. Figure 1 shown.

[0044] 4. After the denture is polished, the prepared compostable glaze is used to repair the shape of the denture, and ordinary transparent glaze and / or colored glaze are used to simulate the real tooth. The denture is sintered at 780℃ for 3 minutes. Figure 2 As shown, the flexural strength is 250 MPa.

[0045] Comparative strength data of zirconia whiskers before and after toughening.

[0046] As a Type I ceramic, ISO 6872:2015 requires that the flexural strength of the glaze be ≥50 MPa. The flexural strength of ordinary transparent glazes on the market is generally 50-100 MPa. The present invention strengthens the glass powder A and glass powder B by adding zirconium oxide whiskers, and the obtained enhanced glaze has a flexural strength of 200-250 MPa.

[0047] The embodiments described above are merely descriptions of preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by persons skilled in the art should fall within the scope of protection defined by the claims of the present invention.

Claims

1. A high-strength buildable glaze for denture restoration, characterized by: The invention comprises glass powder A, glass powder B and zirconium oxide whiskers; in terms of mass percentage, the glass powder A comprises 50-60% SiO2, 10-20% B2O3, 1-5% CaO, 10-15% Al2O3, 5-10% Na2O, 5-15% K2O, 0-3% Li2O, 1-5% F - , 0-2% SnO2, 0-2% ZnO, 0-2% Y2O3, 0-2% CeO2, 1-8% ZrO2, 0-2% BaO, 0-2% MgO; The glass powder B comprises 40-65% SiO2, 5-10% B2O3, 1-5% CaO, 10-15% Al2O3, 5-10% Na2O, 5-10% K2O, 0-1% Li2O, 0-1% F - , 0-2% SnO2, 1-2% ZnO, 0-2% Y2O3, 0-2% CeO2, 1-5% ZrO2, 1-2% BaO, 0-2% MgO.

2. The high-strength buildable glaze for denture restoration according to claim 1, characterized in that: The particle size D50 of the glass powder A is controlled to be 10-50 μm.

3. The high-strength buildable glaze for denture restoration according to claim 2, characterized in that: The particle size D50 of the glass powder B is controlled to be 10-50 μm.

4. The high-strength buildable glaze for denture restoration according to claim 1, characterized in that: The particle size of the zirconium oxide whisker is 2-4 μm, and the length is 20-300 μm.

5. The high-strength buildable glaze for denture restoration according to claim 3, characterized in that: In terms of mass percentage, the amount of the glass powder A is 30-60wt%, the amount of the glass powder B is 40-70wt%, and the amount of the zirconium oxide whisker added is 0.3-5wt% of the total amount of the glass powder A and the glass powder B.

6. A method for preparing the high-strength buildable glaze for denture restoration according to any one of claims 1 to 5, characterized in that: Glass powder A, glass powder B and zirconium oxide whiskers are mixed, and then a blending liquid is added and mixed to obtain a buildable glaze paste.

7. The preparation method according to claim 6, characterized in that: Calculated by mass percentage, the blending solution includes 50%-60% 1-3 butanediol and 30%-60% diethanolamine.

8. The preparation method according to claim 6, wherein: The preparation process of the glass powder A is as follows: after mixing the various components of the glass powder A, high-temperature sintering is performed at 1500°C for 1 hour, and then water quenching, drying, crushing, and air flow grinding are performed in sequence to grind to 10-50μm to prepare glass powder A with a softening temperature of 650-800°C.

9. The preparation method according to claim 6, characterized in that: The preparation process of the glass powder B is as follows: after mixing the components of the glass powder B, sintering at a high temperature of 1500°C for 1 hour, and then water quenching, drying, crushing, and air flow grinding in sequence to crush the powder to 10-50 μm to prepare glass powder B with a softening temperature of 350-500°C.

10. The preparation method according to claim 6, characterized in that: During the denture restoration process, a buildable glaze is used to fill the shape of the corrected and polished denture. Ordinary transparent glaze is applied and then sintered at 780°C in one go.