Strong-stability staining solution suitable for wide temperature window

Abstract

The invention relates to the technical field of dental restoration materials, in particular to a high-stability staining solution suitable for a wide temperature window. According to the specific technical scheme, the high-stability staining solution suitable for the wide temperature window comprises, by weight, 20-200 parts of a coloring agent, 50-200 parts of a stabilizer, 15-25 parts of preservatives and 1000 parts of water, the stabilizer is PEG600, and the preservatives are gluconic acid and citric acid. The staining solution disclosed by the invention can keep color stability in a wide temperature window (+ / -30 DEG C), and meanwhile, by optimizing a formula and a process of the staining solution, the staining time is shortened to 10-20 seconds, and the staining efficiency and the color consistency after sintering are remarkably improved.

Description

Technical Field

[0001] This invention relates to the field of dental restorative materials technology, and specifically to a highly stable staining solution suitable for a wide temperature window. Background Technology

[0002] Narrow sintering temperature window: Existing staining solutions are extremely sensitive to temperature fluctuations during high-temperature sintering. Typically, when the temperature deviation exceeds ±10℃, the color deviation ΔE > 2.0, failing to meet clinical requirements for color consistency. Taking the most commonly used ST ceramic blocks and the most commonly used color A3 from different brands of staining solutions as examples, samples were sintered at 1520℃ for 2 hours as a control curve. Then, the furnace temperature was adjusted by increasing or decreasing, and the LAB value and ΔE value were observed, where ΔE = (ΔL...). 2 +ΔA 2 +ΔB 2 ) 0.5 The results showed that the actual sintering temperature fluctuated by more than ±30℃ due to factors such as different brands of sintering furnaces and seasonal temperature and humidity changes, which further aggravated the color distortion problem.

[0003] Dyeing solution processing time: Existing dyeing solutions on the market typically require 60 seconds or more for penetration and color development, which is insufficient for high-efficiency production, especially in automated production lines where dyeing time directly impacts production efficiency. Furthermore, prolonged dyeing time can lead to uneven penetration of the dyeing solution onto the zirconium oxide surface, affecting the uniformity and consistency of the final color.

[0004] Insufficient stability of staining solutions: Existing staining solutions are prone to component decomposition or destruction of color core structure during high-temperature sintering, resulting in unstable staining effects. Moreover, insufficient penetration depth (<1.0mm) limits the application of multi-layer staining processes, affecting the aesthetics and functionality of dentures. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a highly stable dyeing solution suitable for a wide temperature window, which can maintain color stability within a wide temperature window (±30℃). At the same time, by optimizing the dyeing solution formula and process, the dyeing time is shortened to 10-20 seconds, significantly improving dyeing efficiency and color consistency after sintering.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] This invention discloses a highly stable staining solution suitable for a wide temperature window, comprising, by weight, 20-200 parts of colorant, 50-200 parts of stabilizer, 15-25 parts of preservative, and 1000 parts of water, wherein the stabilizer is PEG600 and the preservative is gluconic acid and citric acid.

[0008] Preferably, the mass ratio of gluconic acid to citric acid is 2:1.

[0009] Preferably, the colorant comprises Er(NO3)3 and Pr(NO3)3·6H2O, and in the dyeing solution, by weight, Pr(NO3)3·6H2O is 3-20 parts and Er(NO3)3 is 12-80 parts.

[0010] Preferably, the mass ratio of Pr(NO3)3·6H2O to Er(NO3)3 is 0.5-3:4.

[0011] Preferably, the colorant further includes one or both of FeCl3 and Mn(NO3)2.

[0012] Accordingly, a method for using the highly stable staining solution suitable for a wide temperature window involves placing a zirconia denture in the staining solution and performing ultrasonic treatment at a frequency of 40kHz and a power of 200W. The zirconia denture is stained within 10-20 seconds, and the penetration depth is ≥1.5mm.

[0013] The present invention has the following beneficial effects:

[0014] This invention utilizes ultrasonic-assisted penetration (frequency 40kHz, power 200W) impregnation technology to significantly improve the penetration rate of staining solution on the surface of zirconia dentures, shortening the staining time to 10-20s. The zirconia dentures rapidly and uniformly absorb the staining solution to reach saturation. The surface tension of the staining solution is 30-40mN / m, ensuring that the staining solution completes uniform penetration to a depth of ≥1.5mm within 10-20 seconds.

[0015] This invention uses Er 3+ / Pr 3+ The 1-3:4 dual rare earth co-doping technology utilizes the df electron transition characteristics to offset the effects of temperature fluctuations. Tested according to ISO 17304:2020 standards, the color deviation ΔE after sintering the dye solution within the range of 1520℃±30℃ is ≤1.5, meeting the precise matching requirements of the Vita 16-26 color series. It is compatible with mainstream sintering furnace brands (such as Sirona, VITA, Bessma, and LONAI), and stable color development can be achieved without extremely strict temperature calibration. Attached Figure Description

[0016] Figure 1 The flowchart shows the process of coloring ST zirconia ceramic blocks with dye solution A3. Detailed Implementation

[0017] The technical solutions of 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.

[0018] Unless otherwise specified, the technical means used in the implementation examples are conventional means well known to those skilled in the art.

[0019] This invention discloses a highly stable staining solution suitable for a wide temperature window, comprising, by weight, 20-200 parts of colorant, 50-200 parts of stabilizer, 15-25 parts of preservative, and 1000 parts of water. The stabilizer is PEG600, which maintains solution stability and increases the penetration rate. The preservative is gluconic acid and citric acid, which effectively prevent the staining solution from spoiling. The mass ratio of gluconic acid to citric acid is 2:1.

[0020] The colorant comprises Er(NO3)3 and Pr(NO3)3·6H2O, in which, by weight, Pr(NO3)3·6H2O comprises 3-20 parts and Er(NO3)3 comprises 12-80 parts in the entire dyeing solution. Preferably, the mass ratio of Pr(NO3)3·6H2O to Er(NO3)3 is 0.5-3:4. The colorant also includes one or both of FeCl3 and Mn(NO3)2.

[0021] In this invention, zirconium oxide is stained using the above-mentioned dyeing solution and then calcined at high temperature. At high temperature, the Pr in the dyeing solution... 3+ and Er 3+ The combination with the zirconium oxide lattice produces a stable color that remains stable despite temperature fluctuations. Mn can be used during the dyeing process. 2+ and Fe 3+ Color correction, specifically: Fe 3+ Can be used for Pr 3+ The yellow color was corrected, while Mn 2+ The main adjustment is to the brightness of the colors.

[0022] This invention also discloses a method for using a highly stable staining solution suitable for a wide temperature window. The method involves pre-firing a zirconia block, then using CAD / CAM to mill the tooth body to create a zirconia denture. The zirconia denture is then placed in the staining solution and subjected to ultrasonic impregnation at a frequency of 40kHz and a power of 200W, allowing the zirconia denture to complete staining within 10-20 seconds. The zirconia denture rapidly and uniformly absorbs the staining solution to reach saturation. The surface tension of the staining solution is 30-40 mN / m, ensuring uniform penetration to a depth of ≥1.5 mm within 10-20 seconds.

[0023] The present invention will be further described below with reference to specific embodiments.

[0024] Example

[0025] 1. In this invention, the proportions of different staining solutions are shown in Table 1 below.

[0026] Table 1. Proportions of different staining solutions (parts by weight)

[0027]

[0028] 2. Zirconia dentures (material selected: ST zirconia ceramic blocks) were ultrasonically impregnated and stained using the method disclosed in this invention. The ultrasonic soaking lasted for 20 seconds, and the staining was followed by high-temperature sintering. The ΔE values ​​after holding at different furnace temperatures (1520±30℃) for 2 hours are shown in Table 2 below. The results show that the color deviation of the staining solution after sintering at different furnace temperatures is ≤1.5, and the color consistency is high in the range of 1490-1550℃.

[0029] Table 2 ΔE values ​​at different furnace temperatures

[0030]

[0031]

[0032] 3. Twelve sets of ST zirconia dentures were ultrasonically impregnated and stained using the staining solution of color A3 in Table 1. The staining time was 20 seconds. After staining, the dentures were sintered at 1530℃. The staining process is as follows: Figure 1 As shown, the staining depth was approximately 2.3 mm, indicating thorough staining. The teeth obtained after sintering at 1530℃ had a normal color. Simultaneously, a comparative test was conducted on the three-point flexural strength of the zirconia dentures before and after staining, and the results are shown in Table 3 below. The results show that there was no statistically significant difference in the strength of the zirconia dentures, high color consistency at 1530℃, and minimal impact on strength testing before and after staining.

[0033] Table 3. Three-point flexural strength of zirconia dentures before and after staining.

[0034] Test number Before dyeing / MPa After staining / MPa 1 1262 1279 2 854 1089 3 1213 1338 4 1378 1193 5 1317 1287 6 1037 1013 7 1166 992 8 1192 1169 9 1186 1217 10 1250 1020 11 1140 1182 12 1204 1287 average value 1183.25 1172.17

[0035] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims

1. A highly stable staining solution suitable for a wide temperature window, characterized in that: The product comprises, by weight, 20-200 parts colorant, 50-200 parts stabilizer, 15-25 parts preservative, and 1000 parts water, wherein the stabilizer is PEG600 and the preservative is gluconic acid and citric acid.

2. The highly stable staining solution suitable for a wide temperature window according to claim 1, characterized in that: The mass ratio of gluconic acid to citric acid is 2:

1.

3. The highly stable staining solution suitable for a wide temperature window according to claim 1, characterized in that: The coloring agents include Er(NO3)3 and Pr(NO3)3·6H2O. By weight, in the dyeing solution, Pr(NO3)3·6H2O is 3-20 parts and Er(NO3)3 is 12-80 parts.

4. The highly stable staining solution suitable for a wide temperature window according to claim 3, characterized in that: The mass ratio of Pr(NO3)3·6H2O to Er(NO3)3 is 0.5-3:

4.

5. A highly stable staining solution suitable for a wide temperature window according to claim 3 or 4, characterized in that: The colorant also includes one or both of FeCl3 and Mn(NO3)2.

6. A method of using the highly stable staining solution suitable for a wide temperature window as described in any one of claims 1-5, characterized in that: The zirconia denture was placed in the staining solution and ultrasonically treated at a frequency of 40kHz and a power of 200W. The zirconia denture was stained within 10-20 seconds, and the penetration depth was ≥1.5mm.

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