A special neutral water-based dyeing solution for full-ceramic denture zirconia and a preparation method and application thereof

By adopting a neutral water-based staining solution system, the stability and corrosiveness issues of acidic staining solutions during transportation, storage, and use have been resolved, enabling safe and stable staining of zirconia in all-ceramic dentures and improving their mechanical and aesthetic properties.

CN121342549BActive Publication Date: 2026-03-31HUNAN ZEERDUN NEW MATERIALS CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-12-17
Publication Date
2026-03-31

AI Technical Summary

Technical Problem

Existing acidic dyeing solutions have problems such as strong corrosivity, limited transportation conditions, poor solution stability, and the impact of dyeing on the mechanical properties of zirconia during transportation, storage, and use.

Method used

Using a water-based system with a near-neutral pH, the staining solution components are scientifically compounded, including the coloring component, the modification component, and the pH adjustment component, to form a clear, precipitate-free, neutral water-based staining solution for staining zirconia in all-ceramic dentures.

Benefits of technology

It improves the safety and stability of the dyeing solution, solves the problems of precipitation and stratification during transportation, enhances the mechanical and aesthetic properties of zirconium oxide, and ensures the consistency of dyeing effect and light transmittance.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application belongs to the technical field of denture materials, and particularly relates to a special neutral water-based dyeing solution for full-porcelain dentures, a preparation method and application thereof. The dyeing solution is formed by scientifically compounding a coloring part, a surface modification part and a pH adjusting part, and is a stable, neutral and non-corrosive water-based solution. The technical scheme effectively solves the hidden safety hazards existing in the transportation, storage and use of traditional acid dyeing solution, and effectively reduces the potential influence of the acid dyeing solution on the surface structure and mechanical properties of the full-porcelain denture zirconia restoration. After the full-porcelain denture zirconia restoration is treated by the neutral water-based dyeing solution, excellent coloring effect and high tooth color simulation can be achieved through subsequent sintering, and the color simulation degree and clinical application value of the full-porcelain denture product are significantly improved.
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Description

Technical Field

[0001] This invention relates to the field of dental materials technology, specifically to a neutral water-based staining solution for zirconia in all-ceramic dentures, its preparation method, and its application. Background Technology

[0002] Zirconia for all-ceramic dentures is made from nano-grade high-purity zirconia (ZrO2) ceramic powder through pressing, bisque firing, and machining processes. It is an important material for load-bearing areas in current dental restorations. To meet the needs of different patients, manufacturers of zirconia for all-ceramic dentures have designed various models, specifications, and color series. To meet the process requirements of different denture manufacturing plants, there are many methods for coloring zirconia for all-ceramic dentures. For example, before pre-sintering, the colorant can be left on the surface of the zirconia block by soaking or brushing; after sintering, it can be colored by surface porcelain finishing or external staining; it can even be pre-colored by directly adding the colorant to the powder raw material to form a pre-colored block. Among these methods, soaking staining is the simplest, most efficient, and lowest-cost, making it favored by most denture manufacturers.

[0003] Currently, the pH values ​​of staining solutions for zirconia used in all-ceramic dentures on the domestic and international markets are mostly between 1 and 3. These acidic staining solutions present several drawbacks during transportation and use: First, they may face additional procedures related to hazardous materials transportation restrictions, environmental protection, and corrosive containers and equipment. Second, during transportation, the acidic staining solution may experience color changes and sedimentation due to fluctuations in ambient temperature, vibration, and pressure, affecting the final staining effect of the zirconia used in all-ceramic dentures. Furthermore, during use, the acidic staining solution corrodes the microstructure of the zirconia used in all-ceramic dentures when soaking them, affecting the strength, translucency, and color of the dentures. Additionally, the gases produced by the volatilization of the raw materials used in the acidic staining solution during sintering can corrode the heating rods and thermocouples of the sintering furnace, thus affecting the accuracy of the sintering temperature and ultimately impacting the strength, color, and translucency of the zirconia used in all-ceramic dentures. Based on these findings, this invention proposes a neutral water-based staining solution specifically for zirconia used in all-ceramic dentures, its preparation method, and its application. Summary of the Invention

[0004] The purpose of this invention is to provide a neutral water-based staining solution for zirconia in all-ceramic dentures, its preparation method, and its application. This invention aims to solve the technical problems of existing acidic staining solutions, such as strong corrosivity, limited transportation conditions, poor solution stability, and the impact of staining on the mechanical properties of zirconia, during transportation, storage, and use.

[0005] This invention employs a near-neutral pH water-based system and scientifically formulates the staining solution components. This achieves a staining solution that minimizes the impact on the microstructure and mechanical properties of zirconia restorations while ensuring staining accuracy and penetration depth, thereby improving product safety and processing consistency. Through this staining solution system, the invention also solves the problems of precipitation, stratification, and solute adhesion that easily occur with acidic staining solutions during transportation, storage, and use. This system achieves "overall stability and safe storage" of the staining solution, significantly improving product applicability, industrial operability, and clinical application stability while meeting the demands of high-end all-ceramic dentures for simultaneous improvement in mechanical and aesthetic performance.

[0006] The objective of this invention can be achieved through the following technical solutions:

[0007] A neutral water-based staining solution for zirconia in all-ceramic dentures comprises the following three components: staining solution G1: 23.38%–41.56%, modification solution G2: 9.96%–30.24%, and pH adjustment solution G3: 45.00%–89.84%.

[0008] More preferably, the coloring partial solution G1 includes solvent 1, complexing agent and soluble metal salt; wherein the soluble metal salt is selected from one or more of soluble iron salt, soluble titanium salt, soluble cerium salt, soluble erbium salt, soluble neodymium salt, soluble cobalt salt, soluble manganese salt and soluble chromium salt.

[0009] More preferably, solvent 1 is deionized water, and based on the mass fraction of the colored solution G1 being 100%, solvent 1 accounts for 63.63%-98.00%, complexing agent accounts for 0.35%-7.62%, and soluble metal salt accounts for 0-36.96% and is not zero.

[0010] More preferably, the complexing agent is one or more of the following: sodium tripolyphosphate, sodium pyrophosphate, sodium hexametaphosphate, monoethanolamine, diethanolamine, triethanolamine, ethylenediaminetetraacetic acid, hydroxyethylethylenediaminetriacetic acid, sodium aminotriacetate, ethylenediaminetetraacetic acid salt, trisodium hydroxyethylethylenediaminetriacetate, diethylenetriaminepentacarboxylate, tartaric acid, citric acid, citrate, heptaphosphate, sodium gluconate, sodium alginate, sodium ethylenediaminetetramethylene phosphate, diethylenetriaminepentamethylene phosphonate, and aminetrimethylene phosphate.

[0011] More preferably, the modified partial solution G2 includes a surfactant, a wetting agent, and a dispersant; based on the total mass of the modified partial solution G2 as 100%, the surfactant accounts for 0-1.17% and is not 0, the wetting agent accounts for 11.67%-46.78%, and the dispersant accounts for 56.22%-85.33%.

[0012] More preferably, the surfactant is one or more of stearic acid, lecithin, polysorbate, alkylphenol polyoxyethylene ether quaternary ammonium potassium, alkyl glycoside, polyether-modified heptamethyltrisiloxane, fatty alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether-7, nonylphenol polyoxyethylene ether-10, and nonylphenol polyoxyethylene ether-8.

[0013] More preferably, the wetting agent is one or more of the following: sodium alkylnaphthalene sulfonate, sodium dioctyl sulfosuccinate, acetylenic diols, 1,2-propanediol, 1,3-propanediol, 1,3-butanediol, 2,3-butanediol, 1,2-hexanediol, glycerol, trimethylolethane, trimethylolpropane, 1,2,4-butanetriol, and fatty alcohol polyoxyethylene ether.

[0014] More preferably, the dispersant is one or more of polyethylene glycol, ammonium polyacrylate, polyacrylamide, sodium polyacrylate, sodium hexametaphosphate, sodium carboxymethyl cellulose, sodium lignosulfonate, sodium silicate, sodium pyrophosphate, and sodium dodecyl sulfate.

[0015] More preferably, the pH-adjusting solution G3 includes solvent 2 and pH adjuster; based on the total mass of pH-adjusting solution G3 as 100%, solvent 2 accounts for 78.10%-97.00%, and pH adjuster accounts for 3.00%-18.90%.

[0016] More preferably, solvent 2 is one or more of deionized water, methanol, ethanol, isopropanol, and lauryl alcohol, and the pH adjuster is one or more of citric acid, lactic acid, sodium bicarbonate, ammonia, phosphate, or sodium citrate.

[0017] More preferably, when using a 1 cm optical path cuvette, the absorbance of the neutral water-based staining solution measured at the maximum absorption wavelength of 490-500 nm should not be less than 2.0. The neutral water-based staining solution is a clear, homogeneous solution, and its visual color, when compared with a colorimetric card, is the RAL Classic color card standard color number RAL 3007.

[0018] A method for preparing a neutral water-based staining solution for zirconia in all-ceramic dentures includes the following steps:

[0019] S1. Prepare coloring solution G1, modification solution G2, and pH adjustment solution G3 respectively;

[0020] S2. Mix G1, G2, and G3 thoroughly to obtain the neutral water-based staining solution for zirconia in the all-ceramic denture.

[0021] The application of a neutral water-based staining solution specifically for zirconia in all-ceramic dentures includes the following steps:

[0022] (1) Immerse the zirconia restoration in the neutral aqueous staining solution for 5 to 70 seconds;

[0023] (2) After removing, dry at 50-100℃ for 10-60 minutes;

[0024] (3) Sinter at 1430-1630℃ and hold for 60-200 minutes to obtain the target color restoration body.

[0025] More preferably, the staining solution is used to improve the surface density and color uniformity of the zirconia restoration, thereby improving its flexural strength and visual simulation effect.

[0026] Compared with the prior art, the beneficial effects of the present invention are:

[0027] This invention provides a neutral water-based staining solution for zirconia in all-ceramic dentures, its preparation method, and its application. By scientifically controlling the types and proportions of components in the staining, modification, and pH adjustment components, and after thorough mixing, a clear, sediment-free neutral water-based staining solution with a visual color consistent with RAL 3007 in the RAL Classic color chart is obtained. This neutral water-based staining solution not only solves the problem of acidic staining solutions corroding zirconia in all-ceramic dentures, thus reducing their mechanical properties, but also makes the transportation, storage, and use of the neutral water-based staining solution safer and more convenient. Furthermore, it optimizes the problems of precipitation, stratification, and solute adhesion that occur with acidic staining solutions during transportation. After comprehensive extreme testing (extreme temperature thermal cycling test, high-frequency vibration test, and pressure change test), the neutral water-based staining solution maintains stable appearance (color, transmittance, clarity), pH value, and staining ability (color accuracy, penetration depth, staining effect, transmittance).

[0028] While solving the above-mentioned problems, this invention also provides an extreme working condition test scheme for the neutral water-based dyeing solution, including four aspects of testing: extreme temperature thermal cycling test, high frequency vibration test, pressure change test, and comprehensive extreme test. The neutral water-based dyeing solution remains stable in key indicators such as pH value, appearance clarity, color stability, dyeing depth, and light transmittance through the above-mentioned extreme test scheme, indicating that the dyeing solution prepared by this invention has excellent storage and transportation stability and adaptability. Attached Figure Description

[0029] Figure 1 This is a schematic diagram of the preparation process of the present invention. Detailed Implementation

[0030] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0031] A neutral water-based staining solution for zirconia in all-ceramic dentures comprises the following three components: staining solution G1: 23.38%–41.56%, modification solution G2: 9.96%–30.24%, and pH adjustment solution G3: 45.00%–89.84%.

[0032] More preferably, the coloring partial solution G1 includes solvent 1, complexing agent and soluble metal salt; wherein the soluble metal salt is selected from one or more of soluble iron salt, soluble titanium salt, soluble cerium salt, soluble erbium salt, soluble neodymium salt, soluble cobalt salt, soluble manganese salt and soluble chromium salt.

[0033] More preferably, solvent 1 is deionized water, and based on the mass fraction of the colored solution G1 being 100%, solvent 1 accounts for 63.63%-98.00%, complexing agent accounts for 0.35%-7.62%, and soluble metal salt accounts for 0-36.96% and is not zero.

[0034] More preferably, the complexing agent is one or more of the following: sodium tripolyphosphate, sodium pyrophosphate, sodium hexametaphosphate, monoethanolamine, diethanolamine, triethanolamine, ethylenediaminetetraacetic acid, hydroxyethylethylenediaminetriacetic acid, sodium aminotriacetate, ethylenediaminetetraacetic acid salt, trisodium hydroxyethylethylenediaminetriacetate, diethylenetriaminepentacarboxylate, tartaric acid, citric acid, citrate, heptaphosphate, sodium gluconate, sodium alginate, sodium ethylenediaminetetramethylene phosphate, diethylenetriaminepentamethylene phosphonate, and aminetrimethylene phosphate.

[0035] More preferably, the modified partial solution G2 includes a surfactant, a wetting agent, and a dispersant; based on the total mass of the modified partial solution G2 as 100%, the surfactant accounts for 0-1.17% and is not 0, the wetting agent accounts for 11.67%-46.78%, and the dispersant accounts for 56.22%-85.33%.

[0036] More preferably, the surfactant is one or more of stearic acid, lecithin, polysorbate, alkylphenol polyoxyethylene ether quaternary ammonium potassium, alkyl glycoside, polyether-modified heptamethyltrisiloxane, fatty alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether-7, nonylphenol polyoxyethylene ether-10, and nonylphenol polyoxyethylene ether-8.

[0037] More preferably, the wetting agent is one or more of the following: sodium alkylnaphthalene sulfonate, sodium dioctyl sulfosuccinate, acetylenic diols, 1,2-propanediol, 1,3-propanediol, 1,3-butanediol, 2,3-butanediol, 1,2-hexanediol, glycerol, trimethylolethane, trimethylolpropane, 1,2,4-butanetriol, and fatty alcohol polyoxyethylene ether.

[0038] More preferably, the dispersant is one or more of polyethylene glycol, ammonium polyacrylate, polyacrylamide, sodium polyacrylate, sodium hexametaphosphate, sodium carboxymethyl cellulose, sodium lignosulfonate, sodium silicate, sodium pyrophosphate, and sodium dodecyl sulfate.

[0039] More preferably, the pH-adjusting solution G3 includes solvent 2 and pH adjuster; based on the total mass of pH-adjusting solution G3 as 100%, solvent 2 accounts for 78.10%-97.00%, and pH adjuster accounts for 3.00%-18.90%.

[0040] More preferably, solvent 2 is one or more of deionized water, methanol, ethanol, isopropanol, and lauryl alcohol, and the pH adjuster is one or more of citric acid, lactic acid, sodium bicarbonate, ammonia, phosphate, or sodium citrate.

[0041] More preferably, when using a 1 cm optical path cuvette, the absorbance of the neutral water-based staining solution measured at the maximum absorption wavelength of 490-500 nm should not be less than 2.0. The neutral water-based staining solution is a clear, homogeneous solution, and its visual color, when compared with a colorimetric card, is the RAL Classic color card standard color number RAL 3007.

[0042] A method for preparing a neutral water-based staining solution for zirconia in all-ceramic dentures includes the following steps:

[0043] S1. Prepare coloring solution G1, modification solution G2, and pH adjustment solution G3 respectively;

[0044] S2. Mix G1, G2, and G3 thoroughly to obtain the neutral water-based staining solution for zirconia in the all-ceramic denture.

[0045] The application of a neutral water-based staining solution specifically for zirconia in all-ceramic dentures includes the following steps:

[0046] (1) Immerse the zirconia restoration in the neutral water-based staining solution for 5 to 70 seconds;

[0047] (2) After removing, dry at 50-100℃ for 10-60 minutes;

[0048] (3) Sinter at 1430-1630℃ and hold for 60-200 minutes to obtain the target color restoration body.

[0049] More preferably, the staining solution is used to improve the surface density and color uniformity of the zirconia restoration, thereby improving its flexural strength and visual simulation effect.

[0050] Comparative Example 1

[0051] This comparative example provides an acidic staining solution, which, based on a mass fraction of 100%, comprises 65% coloring component and 35% modification component; the modification component is polyethylene glycol (molecular weight 600); based on a mass fraction of 100% coloring component, the coloring component comprises 10% ferric sulfate, 10% erbium sulfate, and the remainder is deionized water.

[0052] After mixing the above parts evenly, immerse the all-ceramic denture zirconia restoration for 30 seconds, remove it, dry it at 80°C for 30 minutes, and then sinter it at 1530°C for 120 minutes.

[0053] Comparative Example 2

[0054] This comparative example provides an acidic staining solution, which, based on a mass fraction of 100%, comprises 80% coloring component and 20% modification component; the modification component is polyethylene glycol (molecular weight 40); based on a mass fraction of 100%, the coloring component comprises 20% titanium chloride, 5% cobalt chloride, and the remainder is deionized water.

[0055] After mixing the above parts evenly, immerse the all-ceramic denture zirconia restoration for 30 seconds, remove it, dry it at 80°C for 30 minutes, and then sinter it at 1530°C for 120 minutes.

[0056] Example 1

[0057] This embodiment provides a neutral water-based staining solution, which, based on a 100% mass fraction, comprises 25% coloring component, 10% modification component, and 65% pH adjustment component. The coloring component, also based on a 100% mass fraction, comprises 15% ferric sulfate and 15% erbium sulfate, with the remainder being deionized water. The modification component, also based on a 100% mass fraction, comprises 1% stearic acid, 15% sodium alkyl naphthalene sulfonate, and 84% polyethylene glycol (molecular weight 600). The pH adjustment component, also based on a 100% mass fraction, comprises 85% deionized water and 15% sodium citrate.

[0058] After mixing the above parts evenly, immerse the all-ceramic denture zirconia restoration for 30 seconds, remove it, dry it at 80°C for 30 minutes, and then sinter it at 1530°C for 120 minutes.

[0059] Example 2

[0060] This embodiment provides a neutral water-based staining solution, which, based on a 100% mass fraction, comprises a 40% coloring component, a 10% modification component, and a 50% pH adjustment component. The coloring component, also based on a 100% mass fraction, comprises 25% titanium chloride, 2.5% cobalt chloride, and the remainder is deionized water. The modification component, also based on a 100% mass fraction, comprises 1% polyether-modified heptamethyltrisiloxane, 15% propylene glycol, and 84% sodium carboxymethyl cellulose. The pH adjustment component, also based on a 100% mass fraction, comprises 85% deionized water and 15% ammonia.

[0061] After mixing the above parts evenly, immerse the all-ceramic denture zirconia restoration for 30 seconds, remove it, dry it at 80°C for 30 minutes, and then sinter it at 1530°C for 120 minutes.

[0062] Example 3

[0063] This embodiment provides a neutral water-based staining solution, which, based on a 100% mass fraction, comprises a 30% coloring component, a 20% modification component, and a 50% pH adjustment component. The coloring component, also based on a 100% mass fraction, comprises 30% cerium citrate, 5% manganese citrate, and the remainder is deionized water. The modification component, also based on a 100% mass fraction, comprises 0.5% nonylphenol polyoxyethylene ether, 14.5% 1,3-butanediol, and 85% sodium dodecyl sulfate. The pH adjustment component, also based on a 100% mass fraction, comprises 85% deionized water and 15% sodium bicarbonate.

[0064] After mixing the above parts evenly, immerse the all-ceramic denture zirconia restoration for 30 seconds, remove it, dry it at 80°C for 30 minutes, and then sinter it at 1530°C for 120 minutes.

[0065] Example 4

[0066] This embodiment provides a neutral water-based staining solution, which, based on a 100% mass fraction, comprises 35% coloring component, 25% modification component, and 40% pH adjustment component. The coloring component, also based on a 100% mass fraction, comprises 34% ferric nitrate, 1% chromium nitrate, and the remainder is deionized water. The modification component, also based on a 100% mass fraction, comprises 0.8% polysorbate, 15.2% trimethylolethane, and 84% polyacrylamide. The pH adjustment component, also based on a 100% mass fraction, comprises 85% deionized water and 15% dilute potassium hydroxide.

[0067] After mixing the above parts evenly, immerse the all-ceramic denture zirconia restoration for 30 seconds, remove it, dry it at 80°C for 30 minutes, and then sinter it at 1530°C for 120 minutes.

[0068] Example 5

[0069] This embodiment provides a neutral water-based staining solution, which, based on a 100% mass fraction, comprises 20% coloring component, 5% modification component, and 75% pH adjustment component. The coloring component, also based on a 100% mass fraction, comprises 25% titanium acetate, 10% neodymium acetate, and the remainder is deionized water. The modification component, also based on a 100% mass fraction, comprises 1% lecithin, 15% fatty alcohol polyoxyethylene ether, and 84% polyethylene glycol (molecular weight 200). The pH adjustment component, also based on a 100% mass fraction, comprises 80% deionized water, 15% lactic acid, and 5% methanol.

[0070] After mixing the above parts evenly, immerse the all-ceramic denture zirconia restoration for 30 seconds, remove it, dry it at 80°C for 30 minutes, and then sinter it at 1530°C for 120 minutes.

[0071] Example 6

[0072] This embodiment provides a neutral water-based staining solution, which, based on a 100% mass fraction, comprises a 40% coloring component, a 20% modification component, and a 40% pH adjustment component. The coloring component, also based on a 100% mass fraction, comprises 20% ferric ammonium citrate, 10% erbium ammonium citrate, and the remainder being deionized water. The modification component, also based on a 100% mass fraction, comprises 1% alkyl glycoside, 19% sodium dioctyl sulfosuccinate, and 80% sodium silicate. The pH adjustment component, also based on a 100% mass fraction, comprises 80% deionized water, 15% acetic acid, and 5% lauryl alcohol.

[0073] After mixing the above parts evenly, immerse the all-ceramic denture zirconia restoration for 30 seconds, remove it, dry it at 80°C for 30 minutes, and then sinter it at 1530°C for 120 minutes.

[0074] Performance testing

[0075] 1. Mechanical property testing

[0076] The present invention sets up experimental group 1, the purpose of which is to verify the effect of neutral water-based staining solution on improving the mechanical properties of zirconia restorations for all-ceramic dentures through comparative examples 1 and 2 and examples 1 and 2.

[0077] Experimental Group 1: Zirconia restoration samples soaked in different staining solutions and sintered were used. The transmittance was measured using a UV-Vis spectrophotometer; the flexural strength was measured using a universal tensile testing machine; and the hardness was measured using a Vickers microhardness tester. The results are shown in Table 1 below.

[0078] Table 1. Mechanical properties of zirconia restorations after treatment with different staining solutions

[0079]

[0080] Table 1 shows that different staining solutions applied to zirconia used in all-ceramic dentures resulted in different staining methods. Acidic staining solutions colored the zirconia surface by corroding it, while neutral water-based staining solutions altered the staining process, employing a "strong adhesion + rapid penetration" method. Without compromising the translucency of zirconia, these solutions increased the flexural strength of zirconia used in all-ceramic dentures by 16.31% and the hardness by 17.12%. This verifies the effectiveness of neutral water-based staining solutions in addressing the problem of "general staining solutions (acidic) corroding the surface of zirconia used in all-ceramic dentures, thus reducing its mechanical properties."

[0081] 2. Storage and transportation stability verification

[0082] Experimental group 2 was set up in this invention to verify the stability of the neutral water-based staining solution under storage, transportation and use conditions through comparative examples 1 and 2 and examples 1-6.

[0083] Experimental Group 2: The appearance, pH value and staining ability of the staining solution were evaluated through extreme temperature thermal cycling test, high frequency vibration test and pressure change test.

[0084] The test conditions are as follows:

[0085] Extreme hot and cold temperature cycling: alternating between -18 ℃ and 60 ℃, maintained for 24 h / cycle, 8 to 10 cycles;

[0086] High-frequency vibration test: frequency 5-60 Hz, vibration in three mutually perpendicular directions, 2 hours in each direction, for a total of 6 hours;

[0087] Pressure change test: The pressure range was 11.6-57 kPa, and the low pressure was maintained for 4 h at room temperature (25 ℃).

[0088] Transmittance was measured using a UV-Vis spectrophotometer, and pH value was measured using pH test strips. Table 2 shows the data records for different staining solutions before the comprehensive limit test, and Table 3 shows the data records for different staining solutions after the comprehensive limit test.

[0089] Table 2. Data Recording Table Before the Comprehensive Limit Test of Different Staining Solutions

[0090]

[0091] Table 3. Data Recording Table After Comprehensive Limit Test of Different Staining Solutions

[0092]

[0093] As shown in Tables 2 and 3, the comparison results of different types of staining solutions before and after comprehensive extreme tests (extreme temperature thermal cycling test, high frequency vibration test, and pressure change test) show that the acidic staining solution sample exhibits obvious darkening of appearance, precipitation, decrease in pH value, and reduced staining uniformity after the extreme tests, indicating poor system stability. In contrast, the neutral water-based staining solution provided by this invention, under the same test conditions, is clear and free of precipitation, maintains a pH value of 7-8, and exhibits transmittance and staining depth changes of no more than 5%, indicating stable physicochemical properties.

[0094] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit the scope of protection of the invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on these embodiments, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can still combine, add, delete, or otherwise adjust the features of the various embodiments of the present invention according to the circumstances without conflict or creative effort, thereby obtaining different technical solutions that do not fundamentally depart from the concept of the present invention. These technical solutions also fall within the scope of protection of the present invention.

Claims

1. A special-purpose neutral water-based dyeing solution for all-ceramic dentures of zirconium oxide, characterized in that it contains: The coloring part solution G1, the modification part solution G2 and the pH adjusting part solution G3 are added together to form a neutral water-based dyeing solution. The solvent 1 accounts for 63.63%-98.00%, the complexing agent accounts for 0.35%-7.62%, and the soluble metal salt accounts for 0-36.96% and is not 0, all based on 100% of the coloring part solution G1. The modification part solution G2 includes a surfactant, a wetting agent and a dispersant; the surfactant accounts for 0-1.17% and is not 0, the wetting agent accounts for 11.67%-46.78%, and the dispersant accounts for 56.22%-85.33%, all based on 100% of the total mass of the modification part solution G2. The pH adjusting part solution G3 includes a solvent 2 and a pH adjusting agent; the solvent 2 accounts for 78.10%-97.00%, and the pH adjusting agent accounts for 3.00%-18.90%, all based on 100% of the total mass of the pH adjusting part solution G3. The solvent 2 is one or more of deionized water, methanol, ethanol, isopropyl alcohol and lauryl alcohol, and the pH adjusting agent is one or more of citric acid, lactic acid, sodium bicarbonate, ammonia, phosphate or sodium citrate. The absorbance of the neutral water-based dyeing solution is not less than 2.0 at the maximum absorption wavelength of 490-500 nm when a 1 cm optical path cuvette is used, the neutral water-based dyeing solution is a clear and homogeneous solution, and the visual color is compared with a colorimetric card and is RAL 3007.

2. The neutral water-based dyeing solution for zirconia of all-ceramic dentures according to claim 1, characterized in that, The coloring part solution G1 includes the solvent 1, the complexing agent and the soluble metal salt; the soluble metal salt is selected from one or more of soluble iron salt, soluble titanium salt, soluble cerium salt, soluble erbium salt, soluble neodymium salt, soluble cobalt salt, soluble manganese salt and soluble chromium salt.

3. The neutral water-based dyeing solution for zirconia of full porcelain denture according to claim 2, characterized in that, The complexing agent is one or more of sodium tripolyphosphate, sodium pyrophosphate, sodium hexametaphosphate, monoethanolamine, diethanolamine, triethanolamine, ethylenediaminetetraacetic acid, hydroxyethylethylenediaminetriacetic acid, sodium nitrilotriacetic acid, ethylenediaminetetraacetic acid salt, hydroxyethylenediaminetriacetic acid trisodium salt, diethylenetriamine pentaacetic acid salt, tartaric acid, citric acid, citrate, heptonic acid salt, sodium gluconate, sodium alginate, sodium ethylenediaminetetramethylene phosphonate, diethylenetriamine pentamethylene phosphonate and amine trimethylene phosphonate.

4. The neutral water-based dyeing solution for zirconia of full porcelain denture according to claim 1, characterized in that, The surfactant is one or more of stearic acid, lecithin, polysorbate, alkyl phenol polyoxyethylene ether quaternary potassium, alkyl glycoside, polyether modified heptamethyl trisiloxane and fatty alcohol polyoxyethylene ether.

5. The neutral water-based dyeing solution for zirconia of full porcelain denture according to claim 1, characterized in that, The wetting agent is one or more of sodium alkyl naphthalene sulfonate, sodium dioctyl sulfosuccinate, acetylenic diols, 1,2-propanediol, 1,3-propanediol, 1,3-butanediol, 2,3-butanediol, 1,2-hexanediol, glycerol, trimethylol ethane, trimethylol propane, 1,2,4-butanetriol, and fatty alcohol polyoxyethylene ether.

6. The neutral water-based dyeing solution for zirconia of all-ceramic dentures according to claim 1, characterized in that, The dispersing agent is one or more of polyethylene glycol, ammonium polyacrylate, polyacrylamide, sodium polyacrylate, sodium hexametaphosphate, sodium carboxymethyl cellulose, sodium lignosulfonate, sodium silicate, sodium pyrophosphate, and sodium dodecyl sulfate.

7. A method for preparing a full porcelain denture zirconia special-purpose neutral water-based staining solution according to claim 1, characterized in that, The method comprises the following steps: S1. separately preparing a coloring part solution G1, a modifying part solution G2, and a pH adjusting part solution G3; S2. mixing G1, G2, and G3 to obtain the full denture zirconia special neutral water-based dyeing solution.

8. Use of a special neutral water-based staining solution for zirconia of all-ceramic dentures according to any one of claims 1 to 6, characterized in that, The method comprises the following steps: (1) immersing the zirconia restoration in the neutral water-based dyeing solution for 5-70 seconds; (2) drying at 50-100 ℃ for 10-60 minutes after taking out; (3) sintering at 1430-1630 ℃ and holding for 60-200 minutes to obtain the target color restoration.

9. Use of a neutral water-based dyeing liquor according to claim 8, characterized in that, The dyeing solution is used to improve the surface density and color uniformity of the zirconia restoration, thereby improving the bending strength and visual simulation effect.

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