Zirconia ceramic slurry with good curing performance

Abstract

The invention discloses a preparation method of zirconia ceramic slurry with good curing performance, which comprises the following specific steps: 1) weighing a surface modifier, mixing and stirring with zirconia ceramic particles with different colors and particle sizes for 10-20 minutes, and then drying to obtain modified zirconia ceramic particles; 2) mixing the modified zirconia ceramic particles with a diluent, carrying out vacuum stirring and defoaming, and stirring to obtain a premixed solution; and 3) adding an initiator with the mass fraction of 1-10 wt.% into the premixed solution, and carrying out vacuum stirring for defoaming and stirring. The zirconia ceramic slurry with good curing performance is obtained through reasonable grading and matching of the color and particle size distribution of the ceramic powder.

Description

Technical Field

[0001] The invention relates to the technical field of light-cured zirconia ceramics, in particular to a zirconia ceramic slurry with good curing performance. Background Art

[0002] The absorption of ultraviolet light by ceramic particles can determine the photocuring performance of ceramic photocurable slurry. The color, particle size, and particle size distribution of ceramic powders will affect the absorption, refraction, and scattering of ultraviolet light by ceramic powders. Griffith et al. and Chartier et al. found that the curing depth of ceramic slurry is mainly affected by the square of the refractive index difference (Δn) between ceramic particles and the medium. The smaller Δn, the greater the curing thickness. Secondly, the second factor affecting the curing depth is the ratio Q of the particle spacing and the ultraviolet wavelength. The smaller the Q value, the greater the curing depth. Abouliatim et al. established the Kubelka-Munk model and studied the relationship between the extinction coefficient and transmission depth of Al2O3 and SiO2 ceramic particles of different particle sizes and ultraviolet light. It was found that as the particle size of ceramic particles increases, the diffuse reflectance and diffuse reflectance transmittance of ultraviolet light increase, the curing depth of the slurry decreases, and the curing width increases.

[0003] Jang et al. studied the effect of ZrO2 particle size distribution on the curing thickness and found that the narrower the powder particle size distribution, the greater the refraction of ultraviolet light and the smaller the curing depth. It should be pointed out that energy density, formulation system, and solid content also affect the curing thickness and curing depth of the slurry. Tomeckova et al. established the attenuation equation of ultraviolet light absorption and scattering when photocuring SiO2 ceramic slurry and found that the curing depth and curing width of the slurry are affected by critical energy. The greater the exposure energy, the greater the curing depth and the smaller the curing width. Li studied the rheological properties of Al2O3 slurries with different solid contents and found that with the increase of solid content, the wetting angle of the slurry increased, the curing thickness increased, and the width decreased.

[0004] It should be pointed out that since oxide ceramics such as Al2O3 and ZrO2 have relatively small light absorption, their photocuring slurry has good curing performance. Therefore, the photocuring mechanism and photocuring molding of oxide ceramics have been more widely studied. However, since nitride and carbide ceramics are usually off-white or dark in color, their ultraviolet light absorption rate is high and their curing performance is poor, which directly leads to their difficulty in curing molding. Ding et al. conducted ultraviolet light absorption on SiC ceramic powders of different colors and particle sizes and confirmed that darker SiC ceramics have stronger ultraviolet light absorption and their photocuring performance deteriorates. Summary of the invention

[0005] The technical problem to be solved by the present invention is to overcome the shortcomings of the above-mentioned prior art: to provide a method for preparing a zirconia ceramic slurry with good curing performance. The applicant has found that in addition to the high ultraviolet light absorption rate of the nitride itself, the color, particle size, particle size distribution, etc. of the ceramic powder can also affect the ceramic powder's absorption, refraction and scattering of ultraviolet light. The present invention realizes a zirconia ceramic slurry with good curing performance by reasonable grading and matching the color and particle size distribution of the ceramic powder.

[0006] The technical solution of the present invention is as follows: A method for preparing a zirconia ceramic slurry with good curing performance comprises the following specific steps:

[0007] 1) weighing a surface modifier and zirconia ceramic particles of different colors and different particle sizes, mixing and stirring for 10-20 minutes, and then drying to obtain modified zirconia ceramic particles;

[0008] 2) Mixing the modified zirconia ceramic particles and the diluent, stirring and removing bubbles under vacuum for 10-30 minutes to obtain a premixed solution, wherein the premixed solution comprises, by weight: 100 parts of the diluent and 1-30 parts of the modified zirconia ceramic particles;

[0009] 3) Add 1-10 wt.% of initiator to the premixed liquid and stir in vacuum to remove bubbles. Stirring time is 20-30 min to obtain zirconia ceramic slurry with good curing performance.

[0010] As an optimization, the surface modifier is one or more of KH550, KH560, and KH570.

[0011] As an optimization, in step 1), by weight: 10-15 parts of surface modifier, 30-40 parts of a mixture of zirconium oxide ceramic particles with a particle size range of 80nm-5μm and composed of three colors: white, off-white and dark gray.

[0012] As the most preferred, in step 1), by weight: 10-15 parts of surface modifier;

[0013] 5-6 parts of white zirconia ceramic particles (W-2.0) with a particle size of 2 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.;

[0014] 3-5 parts of white zirconia ceramic particles (W-1.5) with a particle size of 1.5 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.;

[0015] 9-10 parts of white zirconia ceramic particles (W-0.8) with a particle size of 0.8 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.;

[0016] 5-7 parts of off-white zirconium oxide ceramic particles (G-0.8) with a particle size of 0.8 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.;

[0017] Liaoning Desheng Special Ceramics Manufacturing Co., Ltd. produces and sells 9-10 parts of dark gray zirconia ceramic particles (D-0.8) with a particle size of 0.8μm.

[0018] Preferably, the diluent is one or more of HEA, HDDA, and TMPTA. Preferably, the initiator is one or more of TPO, 819, and 184.

[0019] The zirconia ceramic slurry prepared by the present invention is cured and formed on a 405nm optical machine to obtain a black zirconia ceramic body; the cured zirconia ceramic body is degreased; and the degreased zirconia body is placed in a gas pressure sintering furnace at a sintering temperature of 1500-1700°C.

[0020] The beneficial effect of the present invention is that the applicant has found that in addition to the high ultraviolet light absorption rate of the nitride itself, the color, particle size, particle size distribution, etc. of the ceramic powder can also affect the ultraviolet light absorption, refraction and scattering of the ceramic powder. The present invention prepares a zirconia ceramic slurry with good curing performance by reasonable grading and matching the color and particle size distribution of the ceramic powder. DETAILED DESCRIPTION

[0021] The present invention is further described in detail below with specific examples, but the present invention is not limited to the following specific examples.

[0022] Example

[0023] Zirconia ceramic slurry with good curing performance is prepared according to the following method, and the specific steps are as follows:

[0024] 1) Weigh the surface modifier KH550 and zirconia ceramic particles of different colors and different particle sizes, mix and stir for 20 minutes, and then dry to obtain modified zirconia ceramic particles; by weight: 15 parts of surface modifier;

[0025] 5 parts of white zirconia ceramic particles (W-2.0) with a particle size of 2 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.;

[0026] 5 parts of white zirconia ceramic particles (W-1.5) with a particle size of 1.5 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.;

[0027] 9 parts of white zirconia ceramic particles (W-0.8) with a particle size of 0.8 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.;

[0028] 7 parts of off-white zirconium oxide ceramic particles (G-0.8) with a particle size of 0.8 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.;

[0029] 10 portions of dark grey zirconia ceramic particles (D-0.8) with a particle size of 0.8 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.

[0030] 2) Mixing the modified zirconia ceramic particles and the diluent, stirring and removing bubbles under vacuum for 30 minutes to obtain a premixed solution, wherein the premixed solution comprises, by weight: 100 parts of the diluent HDDA and 30 parts of the modified zirconia ceramic particles;

[0031] 3) Add 10 wt.% of initiator TPO to the premixed liquid and perform vacuum stirring to remove bubbles. The stirring time is 30 minutes to obtain a zirconia ceramic slurry with good curing performance.

[0032] The zirconia ceramic slurry prepared in this embodiment was cured on a 405nm optical machine to obtain a black zirconia ceramic body; the cured zirconia ceramic body was degreased; and the degreased zirconia body was placed in a gas pressure sintering furnace at a sintering temperature of 1700-1800°C. The density, microhardness and fracture toughness of the prepared product were 3.12g / cm3, 14.11±0.1GPa and 7.63±0.5MPa·m1 / 2, respectively.

[0033] The above are only examples of the features of the present invention and do not constitute any limitation on the protection scope of the present invention. Any technical solution formed by equivalent exchange or equivalent replacement falls within the protection scope of the present invention.

Claims

1. A method for preparing a zirconia ceramic slurry with good curing performance, characterized in that: The specific steps include: 1) weighing a surface modifier and zirconia ceramic particles of different colors and different particle sizes, mixing and stirring for 10-20 minutes, and then drying to obtain modified zirconia ceramic particles; 2) Mixing the modified zirconia ceramic particles and the diluent, stirring and removing bubbles under vacuum for 10-30 minutes to obtain a premixed solution, wherein the premixed solution comprises, by weight: 100 parts of the diluent and 1-30 parts of the modified zirconia ceramic particles; 3) Add 1-10 wt.% of initiator to the premixed liquid and stir in vacuum to remove bubbles. Stirring time is 20-30 min to obtain zirconia ceramic slurry with good curing performance.

2. The method for preparing a zirconia ceramic slurry with good curing performance according to claim 1, characterized in that: The surface modifier is one or more of KH550, KH560 and KH570.

3. The method for preparing a zirconia ceramic slurry with good curing performance according to claim 1, characterized in that: In step 1), by weight: 10-15 parts of a surface modifier, 30-40 parts of a mixture of zirconium oxide ceramic particles having a particle size range of 80 nm-5 μm and consisting of three colors: white, off-white, and dark gray.

4. The method for preparing a zirconia ceramic slurry with good curing performance according to claim 3, characterized in that: 10-15 parts of surface modifier; 5-6 parts of white zirconia ceramic particles (W-2.0) with a particle size of 2 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.; 3-5 parts of white zirconia ceramic particles (W-1.5) with a particle size of 1.5 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.; 9-10 parts of white zirconia ceramic particles (W-0.8) with a particle size of 0.8 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.; 5-7 parts of off-white zirconium oxide ceramic particles (G-0.8) with a particle size of 0.8 μm produced and sold by Liaoning Desheng Special Ceramics Manufacturing Co., Ltd.; Liaoning Desheng Special Ceramics Manufacturing Co., Ltd. produces and sells 9-10 parts of dark gray zirconia ceramic particles (D-0.8) with a particle size of 0.8μm.

5. The method for preparing a zirconia ceramic slurry with good curing performance according to claim 1, characterized in that: The diluent is one or more of HEA, HDDA and TMPTA.

6. The method for preparing a zirconia ceramic slurry with good curing performance according to claim 1, characterized in that: The initiator is one or more of TPO, 819, and 184.