Zirconia modification solution and use thereof

By controlling the color shading and color component content in the zirconia modification liquid, the problem of difficult to take into account both the color shading effect and aesthetics in the prior art is solved, and a dental restoration modification liquid with efficient color shading and aesthetics is achieved.

WO2025092650A1PCT designated stage expired Publication Date: 2025-05-08AIDITE (QINHUANGDAO) TECH CO LTD
View PDF 9 Cites 0 Cited by

Patent Information

Application Number
PCT/CN2024/127719
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2023-10-30
Filing Date
2024-10-28
Publication Date
2025-05-08

AI Technical Summary

Technical Problem

When the existing zirconia modification liquid achieves color shading effect, it is difficult to maintain the aesthetics of the dental restoration, and it is complex in operation and high in cost.

Method used

By controlling the content of color shading components and color components, a zirconia modification liquid is prepared so that its permeability is ≤20%, and the light transmittance is reduced by ≥20%, so that the color shading effect is achieved while maintaining aesthetics.

Benefits of technology

Effectively cover dark abutments, discolored teeth or metal abutments to avoid color exposure, improve repair effect and aesthetics, while simplifying operation and reducing costs.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN2024127719_08052025_PF_FP_ABST
    Figure CN2024127719_08052025_PF_FP_ABST
Patent Text Reader

Abstract

Disclosed are a zirconia modification solution and use thereof. On a weight basis, the zirconia modification solution comprises: 30-80 wt% of a color-masking component, and the balance of a colored component. The zirconia modification solution exhibits an infiltration rate of ≤20% into dental restorations, and a reduction in the light transmittance of the dental restorations by ≥20%. The zirconia modification solution achieves a color-masking effect without compromising the aesthetic appearance of the dental restorations. By controlling the content of the color-masking component and the colored component, the color-masking layer can shield dark abutment teeth, discolored teeth, or metal abutments, and is prevented from being viewed through the surface of the zirconia dental restorations to maintain the restoration effect, thereby achieving a color-masking effect without compromising the aesthetic appearance of the dental restorations.
Need to check novelty before this filing date? Find Prior Art

Description

Zirconia modification liquid and its application

[0001] This application claims priority to the Chinese patent application filed with the China Patent Office on October 30, 2023, with application number CN202311420248.9 and invention name “A Zirconia Modification Liquid and Its Application”, the entire contents of which are incorporated by reference into this application. Technical Field

[0002] The present application relates to the technical field of dental materials, and in particular to a zirconium oxide modification liquid and its application. Background Art

[0003] With the improvement of living standards, people's demand for denture restoration is not only to restore the chewing function of dentures, but also to focus on the aesthetics of dentures after restoration. The development of zirconia ceramic preparation technology has led to more and more aesthetic ceramics being used for denture restoration. The aesthetics of dentures requires that the color and transparency of the restoration materials should be similar and coordinated with natural teeth. However, due to their good permeability, aesthetic ceramics have the disadvantage of insufficient color-masking ability when used in scenarios such as small thickness, dark abutment color, and upper implant restoration. This causes the color of the abutment or metal base to show through from the inside to the outside, thus affecting the overall aesthetics of the restoration.

[0004] Currently, commercially available zirconia finishing fluids are generally divided into coating type and penetrating type. Among them, coating type finishing fluid products improve the color-shielding performance by coating the inner surface of the crown after final firing. However, this type of coating process is complex, the operation is cumbersome, and the cost is high; penetrating type finishing fluid products are applied before the final firing of the restoration. However, the use of penetrating finishing fluid products in the existing technology has the defect of high penetration depth, resulting in an unnatural chalky color after final firing and showing through the crown, which seriously affects the overall restoration effect, especially when used on ultra-thin restorations such as clinical veneers, and cannot achieve an aesthetic effect.

[0005] CN 108703890A discloses a color-blocking zirconia restoration, which is formed by applying one or more layers of a dyed color-blocking layer, a coated color-blocking layer, and a color adhesive layer to the tooth-wearing surface of the zirconia restoration. However, this color-blocking zirconia restoration requires a multi-layer composite color-blocking method to achieve the color-blocking effect. The process is cumbersome and highly dependent on the operator's skill level. Furthermore, excessive color-blocking layers may result in a large amount of clinical tooth preparation, hindering clinical application and promotion.

[0006] CN 110314001A discloses an opacity-imparting liquid, a liquid material applied to a portion of a high-transparency zirconia crown, that does not impart color, but rather adjusts its transparency. The opacity-imparting liquid, used in dental restorations made from zirconia, comprises: (a) 10-39 wt% of a water-soluble aluminum compound and / or a water-soluble lanthanum compound; (b) 60-89 wt% of water; and (c) 1-20 wt% of an organic solvent. However, the overall transparency and exterior transparency of high-transparency zirconia crowns are high, and the opaque layer formed on the inside of the crown after treatment easily penetrates through the outside of the crown, affecting the transparency and color harmony of the entire restoration, reducing the quality of the restorative material itself and the clinical effectiveness of the restoration.

[0007] CN 109608233A discloses a technology for improving the transparency of dental zirconium dioxide ceramics. Specifically, it involves a masking fluid formulated with potassium nitrate, yttrium chloride, praseodymium nitrate, alcohol, citric acid, gluconic acid, and water. Before the final sintering of the zirconium dioxide ceramic, the masking fluid is applied to the surface of the zirconium dioxide ceramic, followed by the final sintering. However, the masking fluid has a transparency-enhancing effect and cannot achieve optimal masking effects on darker abutments, discolored teeth, and metal abutments. This results in the base color showing through the crown, seriously affecting the aesthetics of the restoration.

[0008] Therefore, in view of the shortcomings of the existing technology, there is an urgent need to provide a zirconium oxide modifying liquid that can achieve a color-shielding effect without affecting the overall aesthetics of the dental restoration.

[0009] Summary of the Invention

[0010] The purpose of the present application is to provide a zirconium oxide modifying liquid and its application, which controls the content of the masking component and the color component so that the masking layer can cover dark abutment teeth, discolored teeth or metal abutments, thereby achieving the masking effect without affecting the aesthetics of the dental restoration.

[0011] To achieve the purpose of this application, this application adopts the following technical solutions:

[0012] In a first aspect, the present application provides a zirconium oxide modification liquid, which comprises, based on a total mass percentage of 100 wt%, 30-80 wt% of an opaque component and the remainder being a color component;

[0013] The zirconia modifying liquid has a permeability of ≤20% on the dental restoration, and the reduction in light transmittance of the dental restoration is ≥20%. The zirconia modifying liquid achieves a color-shading effect while not affecting the aesthetics of the dental restoration. In this application, the reduction in light transmittance of the dental restoration refers to the light transmittance of the dental zirconia restoration obtained after color-shading the dental restoration using the zirconia modifying liquid of this application, relative to the light transmittance of the dental restoration before color-shading. The color-shading method is described below in the application of the zirconia modifying liquid.

[0014] The zirconia modifying liquid provided in the present application controls the content of the masking component and the color component so that the masking layer can cover dark abutment teeth, discolored teeth or metal abutments, preventing them from showing through the surface of the dental zirconia restoration and thus reducing the restoration effect. While using the zirconia modifying liquid to achieve the masking effect, it does not affect the aesthetics of the dental restoration. At the same time, by adjusting the color of the masking layer, it is avoided that the zirconia transmittance is too high, which causes the color of the masking layer to show through and affect the aesthetic effect.

[0015] The mass percentage of the opaque component in the zirconium oxide modifying liquid is 30-80wt%, for example, it can be 30wt%, 40wt%, 50wt%, 60wt%, 70wt% or 80wt%, but is not limited to the listed values. Other values ​​not listed within the numerical range are also applicable.

[0016] If the content of the masking component in the zirconium oxide modifying liquid is too low, dark abutment teeth, discolored teeth or metal abutments may easily show through the surface of the dental zirconium oxide restoration, thereby reducing the restoration effect. If the content is too high, the color of the masking layer may show through, thereby affecting the aesthetics of the dental restoration.

[0017] The permeability of the zirconium oxide modification liquid to the dental restoration is ≤20%, for example, it can be 20%, 18%, 15%, 12% or 10%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0018] The light transmittance reduction of the dental restoration is ≥ 20%, for example, it can be 20%, 22%, 25%, 28% or 30%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0019] Preferably, the opacifying component comprises an amphiphilic compound containing silicon.

[0020] Preferably, the opacifying component includes any one of KH550, KH560, KH570, KH792 or DL602, or a combination of at least two of them. Typical but non-limiting combinations include a combination of KH550 and KH560, a combination of KH570, KH792 and DL602, or a combination of KH550, KH560, KH570, KH792 and DL602.

[0021] The masking component used in this application works synergistically with the color component to form a complex phase layer after high-temperature calcination. This composite material has extremely low transparency, which can achieve the masking effect, so that the use process of the dental zirconia restoration meets the aesthetic requirements; at the same time, this masking layer has a low penetration depth and will not penetrate into the outer surface of the zirconia restoration to affect its aesthetic effect; the masking layer also has adjustable colors, thereby simulating the color of normal dentin and achieving a more bionic aesthetic effect.

[0022] Preferably, the color component comprises a soluble metal salt, a stabilizer and a solvent.

[0023] Preferably, based on 100 wt% of the color component, the mass percentage of the soluble metal salt in the color component is 0.5-58.18 wt%, the mass percentage of the stabilizer is 0.13-16 wt%, and the balance is the solvent.

[0024] The mass percentage of the soluble metal salt is 0.5-58.18wt%, for example, it can be 0.5wt%, 1wt%, 7wt%, 14wt%, 20wt%, 28wt%, 50wt% or 58.18wt%, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0025] The mass percentage of the stabilizer is 0.13-16wt%, for example, it can be 0.13wt%, 0.5wt%, 1.6wt%, 3.2wt%, 8.18wt%, 12wt% or 16wt%, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0026] Preferably, the cations in the soluble metal salt include Fe 3+ 、Ce 3+ 、Er 3+ 、Nd 3+ Cr 3+ 、Mn 2+ 、Co 2+ or Gd 3+ Any one or a combination of at least two of, a typical but non-limiting combination includes Fe 3+ With Ce 3+ The combination of Er3+ 、Nd 3+ With Cr 3+ Combination of Nd 3+ Cr 3+ 、Mn 2+ 、Co 2+ With Gd 3+ A combination of, or Fe 3+ 、Ce 3+ 、Er 3+ 、Nd 3+ Cr 3+ 、Mn 2+ 、Co 2+ With Gd 3+ combination.

[0027] Preferably, the anion in the soluble metal salt includes NO3 - 、CH3COO - 、Cl - 、C5H7O5COO - or SO4 2- Any one or a combination of at least two of the following, a typical but non-limiting combination includes NO3 - With CH3COO - The combination of Cl - 、C5H7O5COO - With SO4 2- A combination of NO3 - 、CH3COO - 、Cl - 、C5H7O5COO - With SO4 2- combination.

[0028] Preferably, the stabilizer comprises any one of citric acid, tartaric acid, lactic acid, oxalic acid, malic acid, ascorbic acid or polydextrose, or a combination of at least two thereof. Typical but non-limiting combinations include a combination of citric acid and tartaric acid, a combination of lactic acid, oxalic acid, malic acid and ascorbic acid, or a combination of citric acid, tartaric acid, lactic acid, oxalic acid, malic acid, ascorbic acid and polydextrose.

[0029] Preferably, the solvent comprises any one or a combination of at least two of deionized water, pentaerythritol, ethylene glycol, 1,2-propylene glycol, 1,3-butanediol, 1,4-butanediol, polyethylene glycol, 1,6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol (I), trimethylolpropane or glycerol. Typical but non-limiting combinations include a combination of deionized water and pentaerythritol, ethylene glycol, 1,2-propylene glycol, 1,3-butanediol, , a combination of 1,4-butanediol, polyethylene glycol and 1,6-hexanediol, a combination of 1,6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol, trimethylolpropane and glycerol, or a combination of deionized water, pentaerythritol, ethylene glycol, 1,2-propylene glycol, 1,3-butanediol, 1,4-butanediol, polyethylene glycol, 1,6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol (I), trimethylolpropane and glycerol.

[0030] In a second aspect, the present application provides a use of the zirconium oxide modifying liquid as described in the first aspect, wherein the zirconium oxide modifying liquid is used for color shading of dental restorations; and a method for color shading of dental restorations using the zirconium oxide modifying liquid comprises the following steps:

[0031] The zirconium oxide modifying liquid is brushed and / or impregnated onto the inner surface of the dental restoration, and then sintered.

[0032] The zirconium oxide modifying liquid provided in the present application is applied to dental restorations, which can effectively reduce the transparency of the interior of the dental restoration, cover dark abutment teeth, discolored teeth, and metal bases. Since it has a base color that is coordinated with the color of the restoration, it avoids the problem of poor restoration effect caused by the color showing through the surface of the dental restoration. At the same time, by adjusting the color of the masking layer formed by the zirconium oxide modifying liquid, it can be avoided that when the modifying liquid is used with high-transmittance zirconium oxide, the zirconium oxide transparency is too high, causing the color of the masking layer to show through and affect the aesthetic effect.

[0033] Preferably, the sintering temperature is 1450-1570°C, for example, 1450°C, 1480°C, 1500°C, 1530°C or 1570°C, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0034] Preferably, the sintering treatment time is 10-150 min, for example, 10 min, 50 min, 100 min, 120 min or 150 min, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0035] Compared with the prior art, this application has the following beneficial effects:

[0036] The zirconia modifying liquid provided in the present application controls the content of the masking component and the color component so that the masking layer can cover dark abutment teeth, discolored teeth or metal abutments, preventing them from showing through the surface of the dental zirconia restoration and thus reducing the restoration effect. While using the zirconia modifying liquid to achieve the masking effect, it does not affect the aesthetics of the dental restoration. At the same time, by adjusting the color of the masking layer, it is avoided that the zirconia transmittance is too high, which causes the color of the masking layer to show through and affect the aesthetic effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] FIG1 is an optical image of a dental zirconia restoration provided in Test Example 3 of the present application;

[0038] FIG2 is an optical image of a dental restoration provided in Test Example 3 of the present application;

[0039] FIG3 is an optical image of a dental zirconia restoration filled with dark gray plasticine provided in Test Example 3 of the present application;

[0040] FIG4 is an optical image of a dental restoration filled with dark grey plasticine provided in Test Example 3 of the present application. DETAILED DESCRIPTION

[0041] The technical solution of the present application is further described below through specific implementation methods. Those skilled in the art should understand that the embodiments are only used to help understand the present application and should not be regarded as specific limitations of the present application.

[0042] Example 1

[0043] This embodiment provides a zirconium oxide finishing liquid, which, based on a total mass percentage of 100wt%, includes: 50wt% of a color-shielding component and the remainder being a color component; the color-shielding component is KH550; based on a mass percentage of 100wt%, the color component includes: 14wt% of Fe(NO3)3, 3.2wt% of citric acid, and the remainder being deionized water.

[0044] Example 2

[0045] This embodiment provides a zirconium oxide finishing liquid, which, based on a total mass percentage of 100 wt%, includes: 60 wt% of a color-shielding component, and the balance is a color component; the color-shielding component is KH560; based on a mass percentage of 100 wt%, the color component includes: 0.5 wt% of Fe(NO3)3, 0.13 wt% of oxalic acid, and the balance is ethylene glycol.

[0046] Example 3

[0047] This embodiment provides a zirconium oxide finishing liquid, which, based on a total mass percentage of 100 wt%, includes: 45 wt% of a color-shielding component, and the balance is a color component; the color-shielding component is KH570; and, based on a total mass percentage of 100 wt%, the color component includes: 58.18 wt% of FeCl3, 8.18 wt% of lactic acid, and the balance is glycerol.

[0048] Example 4

[0049] This embodiment provides a zirconium oxide modifying liquid, which is different from the embodiment 1 in that the mass percentage of the opaque component is adjusted to 30 wt % and the balance is the color component, and the rest is the same as the embodiment 1.

[0050] Example 5

[0051] This embodiment provides a zirconium oxide modifying solution, which is different from the embodiment 1 in that the mass percentage of the opaque component is adjusted to 80 wt %, with the remainder being the color component, and the rest is the same as the embodiment 1.

[0052] Example 6

[0053] This embodiment provides a zirconium oxide modification liquid, which differs from Example 1 in that, except for adjusting the mass percentage of Fe(NO3)3 in the color component to 28wt%, the mass percentage of citric acid to 0.08wt%, and the balance being deionized water, the rest is the same as Example 1.

[0054] Example 7

[0055] This embodiment provides a zirconium oxide modification liquid, which differs from Example 1 in that, except for adjusting the mass percentage of Fe(NO3)3 in the color component to 70wt%, the mass percentage of citric acid to 20wt%, and the balance being deionized water, the rest is the same as Example 1.

[0056] Example 8

[0057] This embodiment provides a zirconium oxide modification solution, which differs from Example 1 in that citric acid is not added to the color component, the mass percentage of the Fe(NO3)3 is adaptively adjusted to 50wt%, and the rest is the same as Example 1.

[0058] Example 9

[0059] This embodiment provides a zirconium oxide finishing liquid. Based on a total weight percentage of 100 wt%, the zirconium oxide finishing liquid comprises: 40 wt% of a color-shielding component and the remainder of color components. The color-shielding component is KH570. Based on a total weight percentage of 100 wt%, the color components comprise: 16 wt% of FeCl3, 4.5 wt% of lactic acid, 67 wt% of ethylene glycol, 6 wt% of 1,2-propylene glycol, 3 wt% of 1,3-butanediol, 3 wt% of 1,4-butanediol, 0.3 wt% of polyethylene glycol, and 0.2 wt% of 1,6-hexanediol.

[0060] Example 10

[0061] This embodiment provides a zirconium oxide finishing liquid. Based on a total weight percentage of 100 wt%, the zirconium oxide finishing liquid comprises: 30 wt% of an opaque component, and the remainder is a color component. Based on a total weight percentage of 100 wt%, the opaque component comprises: 50 wt% of KH550 and 50 wt% of KH560. Based on a total weight percentage of 100 wt%, the color component comprises: 14 wt% of Fe(NO3)3, 32 wt% of Ce(CH3COO), 2.2 wt% of citric acid, 1 wt% of tartaric acid, 40.8 wt% of deionized water, and 40 wt% of pentaerythritol.

[0062] Example 11

[0063] This embodiment provides a zirconium oxide finishing liquid. Based on a total weight percentage of 100 wt%, the zirconium oxide finishing liquid includes: 80 wt% of an opaque component, and the remainder is a color component. Based on a total weight percentage of 100 wt%, the opaque component includes: 40 wt% of DL602, 30 wt% of KH570, and 30 wt% of KH792. Based on a total weight percentage of 100 wt%, the color component includes: 35 wt% of Cr2(SO4), 8 wt% of ErCl3, 31 wt% of Nd(C5H7O5COO), 2.2 wt% of lactic acid, 0.5 wt% of oxalic acid, 0.5 wt% of malic acid, 40 wt% of 1,2-propylene glycol, 22.8 wt% of 1,3-butanediol, and 20 wt% of 1,4-butanediol.

[0064] Example 12

[0065] This embodiment provides a zirconium oxide finishing liquid. Based on a total weight percentage of 100 wt%, the zirconium oxide finishing liquid includes: 50 wt% of an opaque component, and the remainder is a color component. Based on a total weight percentage of 100 wt%, the opaque component includes: 50 wt% of KH550, 25 wt% of KH570, 15 wt% of KH792, and 10 wt% of DL602. Based on a total weight percentage of 100 wt%, the color component includes: 35 wt% of Cr2(SO4), 25 wt% of Mn(CH3COO), 38 wt% of Co(NO3), 38 wt% of NdCl, 32 wt% of Gd(C5H7O5COO), 0.04 wt% of malic acid, 0.04 wt% of ascorbic acid, 30 wt% of 1,6-hexanediol, 20 wt% of neopentyl glycol, 10 wt% of diethylene glycol, 10 wt% of dipropylene glycol, 1 wt% of trimethylolpropane, and 0.92 wt% of glycerol.

[0066] Example 13

[0067] This embodiment provides a zirconium oxide finishing liquid, which, based on the total mass percentage of 100wt%, includes: 50wt% of a color-shielding component and the remainder of a color component; based on the mass percentage of 100wt%, the color-shielding component includes: 70wt% of KH550, 10wt% of KH560, 10wt% of KH570, 25wt% of KH79, and 25wt% of DL60; based on the mass percentage of 100wt%, the color component includes: 35wt% of Fe(NO3), 35wt% of Cr(NO3), 25wt% of Mn(NO3), 38wt% of Er(NO3), and 38wt% of Co(NO3). %, Nd(NO3)36wt%, Ce(NO3)31wt%, Gd(NO3)32wt%, lactic acid 10wt%, malic acid 5wt%, oxalic acid 3wt%, ascorbic acid 2wt%, deionized water 8wt%, pentaerythritol 0.5wt%, ethylene glycol 0.5wt%, 1,2-propylene glycol 0.1wt%, 1,3-butanediol 0.1wt%, 1,4-butanediol 0.1wt%, polyethylene glycol 0.1wt%, 1,6-hexanediol 0.1wt%, neopentyl glycol 0.1wt%, diethylene glycol 0.1wt%, dipropylene glycol 0.1wt%, trimethylolpropane 0.1wt%, glycerol 0.1wt%.

[0068] Comparative Example 1

[0069] This comparative example provides a zirconium oxide modifying liquid, which is the same as Example 1 except that the mass percentage of the opaque component is adjusted to 20 wt % and the balance is the color component.

[0070] Comparative Example 2

[0071] This comparative example provides a zirconium oxide modifying liquid, which is the same as Example 1 except that the mass percentage of the opaque component is adjusted to 90 wt %, with the remainder being the color component.

[0072] Comparative Example 3

[0073] This comparative example provides a dental restoration, which is obtained by sintering at 1480° C. for only 100 minutes.

[0074] Test Example 1

[0075] Permeability test: A 15 mm × 10 mm × 8 mm dental restoration was infiltrated with the zirconium oxide modification liquid provided in Examples 1-13 and Comparative Examples 1 and 2. The dental restoration was taken out after 1 second, the excess liquid on the surface was wiped off, and the restoration was dried at room temperature for 10 minutes. The restoration was then dried at 120°C for 30 minutes and taken out. The dental restoration was then cut in half along the long side with a grinding needle, and the cut surface was polished with 800 mesh and 2000 mesh sandpaper in sequence until it was flat. The polished dental restoration was then sintered at 1480°C for 100 minutes with the cut surface facing down to obtain a dental zirconia restoration. A high-definition microscope was used to observe the penetration and calculate the permeability. The results are shown in Table 1.

[0076] Test Example 2

[0077] Transmittance test: The zirconia modification liquid provided in Examples 1-13 and Comparative Examples 1 and 2 was used to brush one side of a 15 mm × 10 mm × 8 mm dental restoration, and the mixture was dried at room temperature for 10 minutes. The mixture was then turned over after being dried in an oven at 120°C for 5 minutes, and then turned over again after being dried for 5 minutes. The mixture was then taken out after being dried at 180°C for 10 minutes. The mixture was sintered at 1480°C for 100 minutes to obtain a dental zirconia restoration, and the transmittance was measured using a haze meter. Comparative Example 3 was used as a control and was not coated with the zirconia modification liquid. The transmittance was measured using a haze meter. The decrease in transmittance of the dental zirconia restorations obtained in Examples 1-12 and Comparative Examples 1 and 2 relative to the dental restoration in Comparative Example 3 was calculated, and the results are shown in Table 1.

[0078] Test Example 3

[0079] Color opacity, restoration aesthetics, and solution stability testing: The zirconia finishing solutions provided in Examples 1-13 and Comparative Examples 1 and 2 were evenly applied to the inner surface of a 1.2 mm thick anterior tooth restoration. The solution was air-dried at room temperature for 10 minutes, then oven-dried at 120°C for 10 minutes, and sintered at 1480°C for 100 minutes to produce dental zirconia restorations. Compared to the dental restoration in Comparative Example 3, when the restoration was filled with dark gray plasticine (simulating a dark abutment or metal abutment), the color of the dark abutment within the restoration did not clearly show through the outer surface of the restoration, indicating good color opacity; otherwise, poor color opacity. Compared to the dental restoration in Comparative Example 3, when the color of the opacifying layer on the inner surface of the restoration did not clearly show through the outer surface of the restoration, the restoration aesthetics was considered good; otherwise, poor aesthetics was considered. If the zirconia finishing solution flocculated or precipitated after being sealed for more than 10 minutes, the solution was considered unstable; otherwise, it was considered stable. The results are shown in Table 1.

[0080] The optical image of the dental zirconia restoration obtained in Example 1 is shown in Figure 1, and the optical image of the dental restoration obtained in Comparative Example 3 is shown in Figure 2. The inner surface of the dental zirconia restoration coated with zirconia modifying liquid can form a masking layer with a certain color effect, and the color of the masking layer will not be obviously visible through the outer surface of the restoration. The color of the outer surface of the restoration is basically unaffected, and the restoration has better aesthetics; while the optical properties of the inner and outer surfaces of the dental restoration not coated with zirconia modifying liquid have no obvious difference, and the dental restoration has better aesthetics but cannot achieve the masking effect.

[0081] An optical image of the dental zirconia restoration obtained in Example 1, with its interior filled with dark gray plasticine, is shown in Figure 3. The color of the dark abutment teeth within the restoration does not clearly show through to the outer surface of the restoration, demonstrating good color concealment. An optical image of the dental restoration obtained in Comparative Example 3, with its interior filled with dark gray plasticine, is shown in Figure 4. The color of the dark abutment teeth within the restoration clearly shows through to the outer surface of the restoration, demonstrating poor color concealment.

[0082] Table 1

[0083] As can be seen from Table 1, the use of the zirconium oxide modifying liquid provided in this application for color masking of dental restorations avoids the problem of the color masking layer showing through the surface of the dental zirconium oxide restoration, resulting in poor restoration effect, while not affecting the aesthetic effect.

[0084] From the comparison of Examples 1-5, 10-11 and Comparative Examples 1 and 2, it can be seen that the content of the opaque component and the color component in the zirconia modification liquid should be limited to a reasonable range. If the content of the opaque component is too low or too high, it will result in poor opaque effect or the color of the opaque layer will show through (a permeability of more than 20% will cause the color of the opaque layer to show through), thereby affecting the aesthetic effect; from the comparison of Example 1 with Examples 6, 7, 12, and 13, it can be seen that the content of soluble metal salts and stabilizers in the color component also needs to be controlled within a reasonable range, otherwise the color of the opaque layer will be too white and will show through the restoration, causing the brightness of the restoration to increase, or the color of the opaque layer will show through the restoration, resulting in an unnatural color, thereby affecting the aesthetics of the dental zirconia restoration; from the comparison of Example 1 with Example 8, it can be seen that if no stabilizer is added to the color component, the cation will undergo a hydrolysis reaction, resulting in the appearance of flocculent precipitation in the solution, affecting the opaque effect and color uniformity;

[0085] From the comparison between Example 1 and Comparative Example 3, it can be seen that the color-shielding effect cannot be achieved without applying the zirconium oxide finishing liquid on the inner surface of the dental restoration.

[0086] In summary, the zirconia modifying liquid provided in the present application controls the content of the masking component and the color component so that the masking layer can cover the dark abutment teeth, discolored teeth or metal abutments, preventing them from showing through the surface of the dental zirconia restoration and thus reducing the restoration effect. While using the zirconia modifying liquid to achieve the masking effect, it does not affect the aesthetics of the dental restoration. At the same time, by adjusting the color of the masking layer, it is avoided that the zirconia transmittance is too high, which causes the color of the masking layer to show through and affect the aesthetic effect.

[0087] The above description is only a specific implementation method of the present application, but the protection scope of the present application is not limited thereto. Those skilled in the art should understand that any changes or replacements that can be easily thought of by those skilled in the art within the technical scope disclosed in the present application fall within the protection scope and disclosure scope of the present application.

Claims

1. A zirconium oxide modification solution, characterized in that: Based on the total mass percentage of 100wt%, the zirconium oxide modification liquid includes: 30-80wt% of the color-shielding component, and the remainder is the color component; The permeability of the zirconium oxide modification liquid to the dental restoration is ≤20%, and the light transmittance reduction of the dental restoration is ≥20%.

2. The zirconium oxide modification solution according to claim 1, characterized in that: The zirconium oxide modifying liquid achieves a color-shielding effect without affecting the aesthetics of the dental restoration.

3. The zirconium oxide modification solution according to claim 1 or 2, characterized in that: The opacifying component includes an amphiphilic compound containing silicon.

4. The zirconium oxide modification solution according to claim 1 or 2, characterized in that: The opaque component includes any one of KH550, KH560, KH570, KH792 and DL602, or a combination of at least two thereof.

5. The zirconium oxide modification solution according to claim 4, characterized in that: The opacifying component includes a combination of KH550 and KH560, a combination of KH570, KH792 and DL602, or a combination of KH550, KH560, KH570, KH792 and DL602.

6. The zirconium oxide modification solution according to claim 1 or 2, characterized in that: The color components include soluble metal salts, stabilizers and solvents.

7. The zirconium oxide modification solution according to claim 6, characterized in that: Taking the mass percentage of the color component as 100wt%, in the color component, the mass percentage of the soluble metal salt is 0.5-58.18wt%, the mass percentage of the stabilizer is 0.13-16wt%, and the remainder is the solvent.

8. The zirconium oxide modification solution according to claim 6, characterized in that: The cations in the soluble metal salt include Fe 3+ 、Ce 3+ , Er 3+ 、Nd 3+ Cr 3+ , Mn 2+ 、Co 2+ and Gd 3+ Any one or a combination of at least two of the following.

9. The zirconium oxide modification solution according to claim 8, characterized in that: The cations in the soluble metal salt include Fe 3+ With Ce 3+ The combination of Er 3+ 、Nd 3+ With Cr 3+ Combination of Nd 3+ Cr 3+ , Mn 2+ 、Co 2+ With Gd 3+ A combination of Fe 3+ 、Ce 3+ , Er 3+ 、Nd 3+ Cr 3+ , Mn 2+ 、Co 2+ With Gd 3+ combination of.

10. The zirconium oxide modification solution according to claim 6, characterized in that: The anions in the soluble metal salt include NO3 - 、CH3COO - , Cl - 、C5H7O5COO - and SO4 2- Any one or a combination of at least two of the following.

11. The zirconium oxide modification solution according to claim 10, characterized in that: The anions in the soluble metal salt include NO3 - With CH3COO - The combination of Cl - 、C5H7O5COO - With SO4 2- A combination of NO3 - 、CH3COO - , Cl - 、C5H7O5COO - With SO4 2- combination.

12. The zirconium oxide modification solution according to claim 7, characterized in that: The cations in the soluble metal salt include Fe 3+ 、Ce 3+ , Er 3+ 、Nd 3+ Cr 3+ , Mn 2+ 、Co 2+ and Gd 3+ Any one or a combination of at least two of the following.

13. The zirconium oxide modification solution according to claim 7, characterized in that: The anions in the soluble metal salt include NO3 - 、CH3COO - , Cl - 、C5H7O5COO - and SO4 2- Any one or a combination of at least two of the following.

14. The zirconium oxide modification solution according to claim 6, characterized in that: The stabilizer includes any one of citric acid, tartaric acid, lactic acid, oxalic acid, malic acid, ascorbic acid and polydextrose, or a combination of at least two thereof.

15. The zirconium oxide modification solution according to claim 14, characterized in that: The stabilizer includes a combination of citric acid and tartaric acid, a combination of lactic acid, oxalic acid, malic acid and ascorbic acid, or a combination of citric acid, tartaric acid, lactic acid, oxalic acid, malic acid, ascorbic acid and polydextrose.

16. The zirconium oxide modification solution according to claim 7, characterized in that: The stabilizer includes any one of citric acid, tartaric acid, lactic acid, oxalic acid, malic acid, ascorbic acid and polydextrose, or a combination of at least two thereof.

17. The zirconium oxide modification solution according to claim 6, characterized in that: The solvent includes any one or a combination of at least two of deionized water, pentaerythritol, ethylene glycol, 1,2-propylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, polyethylene glycol, 1,6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol, trimethylolpropane and glycerol.

18. The zirconium oxide modification solution according to claim 17, characterized in that: The solvent includes a combination of deionized water and pentaerythritol, a combination of ethylene glycol, 1,2-propylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, polyethylene glycol and 1,6-hexanediol, a combination of 1,6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol, trimethylolpropane and glycerol, or a combination of deionized water, pentaerythritol, ethylene glycol, 1,2-propylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, polyethylene glycol, 1,6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol, trimethylolpropane and glycerol.

19. The zirconium oxide modification solution according to claim 7, characterized in that: The solvent includes any one or a combination of at least two of deionized water, pentaerythritol, ethylene glycol, 1,2-propylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, polyethylene glycol, 1,6-hexanediol, neopentyl glycol, diethylene glycol, dipropylene glycol, trimethylolpropane and glycerol.

20. An application of the zirconium oxide modification solution according to any one of claims 1 to 19, characterized in that: The zirconium oxide modifying liquid is used for color shading of dental restorations; the method for color shading of dental restorations by using the zirconium oxide modifying liquid comprises the following steps: The zirconium oxide modifying liquid is brushed and / or impregnated onto the inner surface of the dental restoration, and then sintered.

21. The use according to claim 20, characterized in that The sintering temperature is 1450-1570°C.

22. The use according to claim 20 or 21, characterized in that The sintering time is 10-150 minutes.

23. A dental zirconium oxide restoration, characterized in that: It comprises a dental restoration and a masking layer located on the inner surface of the dental restoration; the masking layer is formed by sintering the zirconium oxide modifying liquid according to any one of claims 1 to 19.

Citation Information

Patent Citations

  • Masking zirconium oxide restoration

    CN108703890A

  • Technology for improving permeability of dental zirconium dioxide ceramic

    CN109608233A

  • Opaque imparting liquid for zirconia

    CN110314001A

  • Dyeing liquor used for dental zirconia ceramic and having color indication function

    CN105924227A

  • Masking liquid for dental zirconium oxide ceramic as well as preparation method and application thereof

    CN109095950A