CN115124338B - Color coating slurry, color zirconia ceramic and preparation method thereof - Google Patents
Color coating slurry, color zirconia ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses color coating slurry, color zirconia ceramic and a preparation method thereof, and relates to the technical field of ceramic materials. The color coating slurry comprises the following components in parts by weight: 5 to 25 portions of colorant, 0.1 to 3 portions of gallium oxide, 10 to 40 portions of binder, 0.5 to 2 portions of curing agent and 50 to 80 portions of organic solvent. The color zirconia ceramics prepared by the color coating slurry has the advantages of uniform color appearance, good permeability of the colorant and high color saturation.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to color coating slurry, color zirconia ceramic and a preparation method thereof.
Background
The zirconia ceramic is a novel ceramic material and has a plurality of excellent characteristics of wear resistance, corrosion resistance, high strength, high toughness, good thermal stability and the like. The zirconia powder is white powder, the prepared ceramic is white naturally, and the colored zirconia ceramic is usually realized by adding rare earth colorants such as praseodymium oxide, erbium oxide, cobalt oxide and the like into the raw materials. However, this method can only color the zirconia ceramic body, and it is difficult to develop a surface effect such as a pattern on the ceramic surface.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides color coating slurry, color zirconia ceramics and a preparation method thereof. The color coating slurry can be used for well coloring a zirconia ceramic matrix, and the prepared color zirconia ceramic has uniform color, high color saturation and higher strength.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the color coating slurry comprises the following components in parts by weight: 5 to 25 portions of colorant and gallium oxide (Ga) 2 O 3 ) 0.1 to 3 portions of adhesive, 10 to 40 portions of binder and 0.5 to 2 portions of curing agentAnd 50-80 parts of organic solvent.
According to the invention, a certain amount of gallium oxide is added into the color coating slurry, and in the sintering process, the gallium oxide can be preferentially infiltrated into the zirconia ceramic matrix to activate the crystal boundary, so that coloring ions are promoted to be further diffused into the zirconia ceramic matrix through the crystal boundary, and finally, a coloring layer with uniform color and a certain penetration depth is obtained. On the other hand, when gallium oxide is not added or the amount of the additive is too small, the diffusion driving force of coloring ions is small, the required penetration coloring time is long, the color is not uniform, and the penetration depth is limited. When the content of gallium oxide is too high, the secondary sintering of zirconia grains is abnormally increased, and the strength of the matrix is reduced. If the amount of the colorant is too low, the coloring is lighter, and the effect is not obvious; if the amount of the colorant is too large, the coloring oxide is likely to be deposited on the surface, and cannot completely permeate into the zirconia, resulting in poor coloring effect. The usage of the binder, the curing agent and the organic solvent is easier to form only by controlling the usage within the range, and the binder, the curing agent and the organic solvent are also easy to remove in the glue discharging process, so that the performance of the ceramic is not influenced.
Preferably, the color coating paste comprises the following components in parts by weight: 10 to 20 portions of colorant, 0.25 to 1.5 portions of gallium oxide, 10 to 20 portions of binder, 0.5 to 1 portion of curing agent and 60 to 80 portions of organic solvent.
By further optimizing the dosage of each component in the color coating slurry, the ceramic prepared by the color coating slurry can be ensured to have bright appearance and higher strength.
Preferably, the colorant is at least one of transition metal oxide and rare earth metal oxide, such as iron oxide and cobalt oxide (Co) 3 O 4 ) Nickel oxide, copper oxide (CuO), chromium oxide, manganese oxide (MnO), vanadium oxide (V) 2 O 5 ) Praseodymium oxide, and the like. The binder comprises at least one of epoxy resin, methyl silicone resin and phenolic resin; the curing agent comprises at least one of an epoxy resin curing agent, an acrylate curing agent and a polyurethane curing agent; the organic solvent comprises at least one of ethanol, ethylene glycol, isopropanol and ethyl acetate. The adhesive, the epoxy resin and the organic solvent are all in the fieldThe domain is a common material.
Meanwhile, the invention also discloses a preparation method of the colored zirconia ceramic, which comprises the following steps:
(1) Preparing a zirconia ceramic matrix;
(2) Spraying, brushing or printing the color coating slurry on the surface of the zirconia ceramic matrix;
(3) Removing the glue, and removing organic substances in the color coating slurry;
(4) And sintering to obtain the colored zirconia ceramic.
Preferably, in the step (1), the zirconia ceramic matrix is yttria-stabilized zirconia, and the molar percentage of yttria in the yttria-stabilized zirconia is 2 to 4mol%; the preparation method of the zirconia ceramic matrix comprises the following steps: weighing zirconia and yttria in proportion, adding a binder, dry pressing, tape casting or injection molding, removing glue, sintering at 1350-1450 ℃, and then polishing to obtain the zirconia ceramic matrix.
If the molar percentage of the yttrium oxide is too low, the zirconium oxide ceramic is prone to phase change and cracking, and if the molar percentage of the yttrium oxide is too high, the strength of the ceramic is low, preferably, the molar percentage of the yttrium oxide is 3mol%, and under the condition, the mechanical property of the prepared zirconium oxide ceramic matrix is optimal. The sintering temperature can also directly influence the comprehensive performance of the zirconia ceramic matrix, and experiments show that when the sintering temperature falls in the range of 1350-1450 ℃, the mechanical property of the zirconia ceramic matrix is better, and the zirconia ceramic matrix can still maintain higher strength after a subsequent color coating is prepared.
Preferably, in the step (3), the rubber discharging conditions are as follows: heating to 400-600 ℃ at the heating rate of 1-3 ℃/min, and keeping the temperature for 1-3 h; in the step (4), the sintering temperature is 1100-1400 ℃. In the process of preparing the coating, the ceramic matrix is subjected to secondary sintering, the colorant is decomposed at a high temperature, and coloring ions attached to the surface of the ceramic blank enter the zirconia matrix through ion diffusion to develop color. When the secondary sintering temperature is lower than 1100 ℃, the colorant can not be decomposed into the zirconia matrix, and when the secondary sintering temperature is higher than 1400 ℃, the zirconia crystal grains grow abnormally, and the matrix strength is greatly attenuated.
In addition, the invention also discloses the colored zirconia ceramic prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
1) The color coating slurry has simple components and low cost, can be applied to a substrate by methods of spraying, brushing or printing, and the like, and can be used for coloring the surface and drawing patterns of the zirconia ceramic by high-temperature sintering.
2) According to the invention, gallium oxide is added into the color coating slurry as a diffusion aid, so that the permeation of coloring particles in a coloring agent in a zirconium oxide matrix can be promoted, the coloring capability is enhanced, and the prepared ceramic has a color development layer with a certain depth, and is uniform in color and bright in color.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Examples 1 to 19 and comparative examples 1 to 4
Examples 1 to 19 are examples of the color coating paste according to the present invention, comparative examples 1 to 4 are color coating pastes, and the formulations of examples 1 to 19 and comparative examples 1 to 4 are shown in table 1.
TABLE 1 (parts by weight)
Application examples 1 to 19 and application comparative examples 1 to 4
Colored zirconia ceramics were prepared by spraying the colored coating slurries described in examples 1 to 19 and comparative examples 1 to 4 onto zirconia ceramic substrates, respectively, as application examples 1 to 19 and application comparative examples 1 to 4, respectively, and were prepared as follows:
(1) Mixing yttria-stabilized zirconia powder with 3mol percent of yttria with a binder polyvinyl alcohol (PVA), dry-pressing for molding, heating to 500 ℃ at a speed of 2 ℃/min, preserving heat for 2 hours for binder removal, then placing the binder-removed green body in an oxygen atmosphere for sintering at a sintering temperature of 1400 ℃ for 25 hours to obtain a ceramic sintered blank, and then polishing to obtain a zirconia ceramic matrix; the mass of the PVA is 10% of that of the yttria-stabilized zirconia powder.
(2) Spraying the color coating slurry on the surface of the zirconia ceramic matrix;
(3) Carrying out glue discharging on the sprayed zirconia ceramic, wherein the glue discharging condition is as follows: heating to 500 ℃ at the heating rate of 2 ℃/min and preserving the heat for 2h;
(4) And after the binder removal, sintering the zirconia ceramics for 2 hours in an air atmosphere at 1300 ℃ to obtain the colored zirconia ceramics.
The production conditions of application examples 1 to 19 and application comparative examples 1 to 4 were completely the same.
Comparative application example 5
A colored zirconia ceramic which differs from application example 1 only in that the sintering temperature when preparing the zirconia ceramic substrate was 1300 ℃.
Comparative application example 6
A colored zirconia ceramic which differs from application example 1 only in that the sintering temperature at the time of preparing the zirconia ceramic substrate was 1500 ℃.
Application comparative example 7
A colored zirconia ceramic which differs from application example 1 only in that in the step (4), the sintering temperature is 950 ℃.
Comparative application example 8
A colored zirconia ceramic which differs from application example 1 only in that, in the step (4), the sintering temperature was 1450 ℃.
Comparative application 9
A colored zirconia ceramic which differs from application example 1 only in that the zirconia ceramic substrate was prepared without sintering after binder removal. The properties of application examples 1 to 19 and application comparative examples 1 to 9 were tested
1) 4PB testing
Testing equipment: universal material testing machine, model INSTRON5965;
the test method comprises the following steps:
a. the sample requirements are as follows: (45 ± 0.05) mm (30 ± 0.05) mm (0.45 ± 0.05) mm, chamfered (0.1 ± 0.05) × 45 ° or rounded R0.15 ± 0.05mm;
b. polishing and grinding the front surface and the back surface of the sample, removing grinding traces, deep scratches, indentations and the like of a grinding wheel on the surface, wherein the surface roughness Ra is required to be less than or equal to 0.02 mu m, and grinding and chamfering other surfaces by using a 1200-mesh grinding wheel;
c. an upper wheel base: 18mm, lower wheelbase 36mm, loading bar diameter: 6mm, speed: 10mm/min;
d. the upper and lower roller rods are clean, and the surfaces are not seriously scratched;
e. the same size samples were cut from the finished product and tested as above with the results shown in table 2.
2) Color test
Testing equipment: a colorimeter;
the test method comprises the following steps: the stains on the sample surface were removed, the spot was taken for testing, the colorimetric values were recorded, and the colorimetric values were recorded in table 2.
TABLE 2
As is clear from Table 2, application examples 1 to 19 have both good mechanical properties and good coloring effects. Comparing the test results of application example 9 and application comparative example 1, it can be found that when the proportion of gallium oxide is too high, the strength of the colored zirconia ceramic is obviously attenuated, the strength of the colored gallium oxide ceramic is lower than 900MPa, and the mechanical properties are too poor, which results in a great reduction of the application range. This is caused by the fact that gallium ions are incorporated into the crystal lattice of zirconia excessively, so that the crystal grains of zirconia ceramics grow abnormally and the strength of the ceramics is lowered. The formulations and test results of application examples 1 to 9 show that the coloring effect is optimal and the mechanical properties are good when the content of gallium oxide is 1.2%.
Comparing the formulations of application examples 10 to 13 with the formulations of application comparative examples 2 to 3 and the test results, it can be seen that when the content of the colorant is too low, the color saturation value of the colored zirconia ceramic is significantly reduced, and when the content of the colorant is too high, since coloring ions permeate into the colored zirconia ceramic to be saturated, unreacted colorant remains on the surface of the colored zirconia ceramic, and the coloring effect is deteriorated.
Comparing the formulations of application examples 1 to 19 with application comparative example 4 and the test results, it can be found that the diffusion driving force of the coloring ions becomes significantly small when no gallium oxide is added, the color of the colored zirconia ceramic is not uniform, the penetration depth is limited, and the saturation of the color is low.
The test results of the application example 1 and the application comparative examples 5 to 6 are compared, and it can be found that when the zirconia ceramic matrix is prepared, the sintering temperature has a crucial effect on the performance of the colored zirconia ceramic, and the mechanical properties are greatly attenuated when the temperature is too high or too low.
Comparing the test results of application example 1 and application comparative examples 7 to 8, it can be found that the sintering temperature during the preparation of the color coating layer also has great influence on the performance, and the temperature is too low, the color saturation is low, the temperature is too high, and the mechanical properties are deteriorated.
Comparing the test results of application example 1 and application comparative example 9, it can be found that the mechanical properties of the prepared colored zirconia ceramics are sharply reduced without sintering the zirconia ceramic matrix.
From the formulations and test results of application examples 14 to 19, it is found that the addition of gallium oxide can promote the diffusibility of various colored ions in ceramics, and can be widely applied to the preparation of colored ceramics.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The preparation method of the colored zirconia ceramic is characterized by comprising the following steps:
(1) Preparing a zirconia ceramic matrix;
(2) Spraying, brushing or printing the color coating slurry on the surface of the zirconia ceramic matrix;
(3) Removing the glue, and removing organic substances in the color coating slurry;
(4) Sintering to obtain the colored zirconia ceramics;
the color coating slurry comprises the following components in parts by weight: 5 to 25 parts of colorant, 0.1 to 3 parts of gallium oxide, 10 to 40 parts of binder, 0.5 to 2 parts of curing agent and 50 to 80 parts of organic solvent.
2. The method of claim 1, wherein the color coating paste comprises the following components in parts by weight: 10-20 parts of a colorant, 0.25-1.5 parts of gallium oxide, 10-20 parts of a binder, 0.5-1 part of a curing agent and 60-80 parts of an organic solvent.
3. The method of claim 1, wherein the colorant is at least one of a transition metal oxide and a rare earth metal oxide.
4. The method of claim 1, wherein the binder comprises at least one of an epoxy resin, a methyl silicone resin, and a phenolic resin; the curing agent comprises at least one of an epoxy resin curing agent, an acrylate curing agent and a polyurethane curing agent; the organic solvent comprises at least one of ethanol, ethylene glycol, isopropanol and ethyl acetate.
5. The preparation method according to claim 1, wherein in the step (1), the zirconia ceramic matrix is yttria-stabilized zirconia, and the molar percentage of yttria in the yttria-stabilized zirconia is 2 to 4mol%; the preparation method of the zirconia ceramic matrix comprises the following steps: weighing zirconia and yttria according to a proportion, adding a binder, performing dry pressing, tape casting or injection molding, discharging glue, sintering at 1350-1450 ℃, and processing to a polished state to obtain the zirconia ceramic matrix.
6. The preparation method according to claim 1, wherein in the step (3), the conditions for removing the gel are as follows: heating to 400-600 ℃ at the heating rate of 1-3 ℃/min, and keeping the temperature for 1-3 h.
7. The production method according to claim 1, wherein in the step (4), the sintering temperature is 1100 to 1400 ℃.
8. A colored zirconia ceramic produced by the method according to any one of claims 1 to 7.
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| CA2538964A1 (en) * | 1999-08-16 | 2001-02-22 | 3M Espe Ag | Blank for producing a dental prosthesis |
| CN102674888A (en) * | 2012-05-15 | 2012-09-19 | 深圳市爱尔创科技有限公司 | Coloring solution for dental zirconia ceramic product and using method of coloring solution |
| CN104918900A (en) * | 2012-09-20 | 2015-09-16 | 3M创新有限公司 | Coloring of zirconia ceramics |
| CN108585845A (en) * | 2018-06-14 | 2018-09-28 | 长沙鹏登生物陶瓷有限公司 | A kind of preparation method of color and permeability gradual change zirconium oxide artificial tooth ceramic body |
| CN109734444A (en) * | 2019-03-07 | 2019-05-10 | 珠海新茂义齿科技有限公司 | A kind of zirconium oxide immersion coloration and dyeing method |
| CN111205094A (en) * | 2020-01-14 | 2020-05-29 | 伯恩光学(惠州)有限公司 | Preparation method of 3D color ceramic backboard |
| CN112694327A (en) * | 2020-12-30 | 2021-04-23 | 潮州三环（集团）股份有限公司 | White zirconia ceramic |
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