Transparent ceramic frit and preparation method thereof

By using raw materials such as quartz sand and other raw materials combined with the segmented temperature-controlled sintering method, the problem of insufficient transparency and elastic modulus of transparent ceramic frit was solved, and the preparation of ceramic frit with high transparency and elastic modulus was achieved, avoiding the health risks of lead precipitation.

CN120441199BActive Publication Date: 2025-09-02ZIBO JINDING GLAZE CO LTD
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202510953696.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-07-11
Publication Date
2025-09-02
Estimated Expiration
2045-07-11

AI Technical Summary

Technical Problem

The existing transparent ceramic frits have problems such as poor transparency and insufficient elastic modulus in the production of ceramic wall and floor tiles, and lead-free frit glaze has problems such as health precipitation during use.

Method used

Quartz sand is used as the main raw material, combined with calcined kaolin, waltite and strontium zirconate to improve mechanical properties, zinc stannate, niobium pentoxide and lithosparapara to improve transparency, topaz and antimony oxide are added to reduce high-temperature melt viscosity, and transparent ceramic fuses are prepared by segmented temperature-controlled sintering and step-by-step cooling.

Benefits of technology

The prepared transparent ceramic frit has excellent transparency and elastic modulus, ensuring the performance stability and safety of the ceramic frit and avoiding the health hazards of lead precipitation.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure SMS_1
    Figure SMS_1
Patent Text Reader

Abstract

The present invention belongs to the technical field of ceramic frit preparation, and specifically relates to a transparent ceramic frit and a preparation method thereof. The transparent ceramic frit described in the present invention is composed of the following raw materials: quartz sand, calcined kaolin, pyrophyllite, strontium zirconate, zinc stannate, niobium pentoxide, boracite, petalite, calcium silicate, topaz, and antimony oxide. The transparent ceramic frit described in the present invention uses quartz sand as the main raw material to provide a base network, adds calcined kaolin, pyrophyllite and strontium zirconate to improve the mechanical properties of the prepared transparent ceramic frit, adds zinc stannate, boracite, niobium pentoxide, petalite and calcium silicate to improve the transparency of the prepared transparent ceramic frit, adds topaz and antimony oxide to reduce the high-temperature melt viscosity and improve the smoothness of the prepared transparent ceramic frit, thereby synergistically acting between the raw materials to ensure that the prepared transparent ceramic frit has excellent transparency and elastic modulus.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention belongs to the technical field of ceramic frit preparation, and particularly relates to a transparent ceramic frit and a preparation method thereof. Background Art

[0002] Frit is a type of glass, made from a specific set of raw materials, melted at high temperatures and then quenched. It exhibits insolubility and stability. After grinding, it is applied to various vessels and blanks, forming a thin layer of glassy texture after firing. Frit glazes are categorized by their properties as transparent, opalescent, leaded, and lead-free. During the melting process, the appearance can vary from granular to flaky, depending on the manufacturing method. Because frit glaze is insoluble, it is highly safe and can be used alone or added to regular raw glazes as a solvent.

[0003] Transparent ceramic frits are widely used in the production of ceramic wall and floor tiles. However, varying degrees of devitrification can occur during production. This is often related to the formulation and its fluctuations, in addition to process control. Ceramic frits primarily composed of lead offer advantages such as excellent melting properties, a high refractive index, a glossy glaze, and a wide firing temperature range. However, lead-glazed products are susceptible to lead precipitation during use, posing a health risk to users. Currently, lead-free ceramic frit glazes are increasingly widely used, but they suffer from several drawbacks: poor transparency; and insufficient high-temperature fluidity of ceramic frit glazes, which can easily lead to various defects during firing, resulting in an insufficient elastic modulus in the final ceramic frit.

[0004] Therefore, it is necessary to explore a new method for preparing ceramic frit. Summary of the Invention

[0005] The purpose of the present invention is to provide a transparent ceramic frit having excellent transparency and elastic modulus, and also to provide a preparation method thereof.

[0006] The transparent ceramic frit of the present invention is composed of the following raw materials, in parts by weight: 50 parts of quartz sand, 11-13 parts of calcined kaolin, 7-9 parts of pyrophyllite, 2.8-3.5 parts of strontium zirconate, 5.5-6.0 parts of zinc stannate, 1.1-1.3 parts of niobium pentoxide, 9.8-10.8 parts of borate, 4.6-5.0 parts of petalite, 2.7-3.3 parts of calcium silicate, 3.0-3.2 parts of topaz, and 0.6-0.64 parts of antimony oxide.

[0007] in:

[0008] The petalite has the following chemical composition, calculated by mass percentage: SiO2 75.98%, Al2O3 17.02%, CaO 0.13%, MgO 0.04%, K2O 0.15%, Na2O 0.27%, LiO2 5.11%, and loss on ignition 1.30%.

[0009] The chemical composition of the boracic acid is as follows: MgO 32.68%, B2O3 33.85%, Cl 5.23%, Fe2O3 1.00%, SiO2 12.45%, Al2O3 2.01%, CaO3.02%, and loss on ignition 9.76%.

[0010] The chemical composition of the topaz, calculated by mass percentage, is as follows: Al2O3 52.29%, SiO2 34.25%, MgO 0.01%, CaO 0.23%, Fe2O3 0.29%, TiO2 0.04%, K2O 0.03%, Na2O 0.01%, F 11.73%, and loss on ignition 1.12%.

[0011] Preferably, the transparent ceramic frit described in the present invention is composed of the following raw materials, in parts by mass: 50 parts of quartz sand, 12 parts of calcined kaolin, 8 parts of pyrophyllite, 3.2 parts of strontium zirconate, 5.7 parts of zinc stannate, 1.2 parts of niobium pentoxide, 10.3 parts of borate, 4.8 parts of petalite, 3.0 parts of calcium silicate, 3.1 parts of topaz, and 0.62 parts of antimony oxide.

[0012] The transparent ceramic frit described herein uses quartz sand as its primary raw material to provide silicon dioxide, forming a continuous network of [SiO4] tetrahedra, providing a hardness foundation for the prepared transparent ceramic frit. The interaction between calcined kaolin, pyrophyllite, and strontium zirconate improves the mechanical properties of the prepared transparent ceramic frit. Calcined kaolin and pyrophyllite decompose into a mullite phase at high temperatures, providing dispersion strengthening. Strontium zirconate decomposes at high temperatures to produce zirconium oxide and strontium oxide. Zirconium oxide anchors mullite grain boundaries, increasing crack propagation resistance. Strontium oxide also reacts with aluminum oxide and silicon dioxide to form strontium feldspar, reducing the coefficient of thermal expansion. Thus, the synergistic effect between calcined kaolin, pyrophyllite, and strontium zirconate ensures the mechanical properties of the prepared transparent ceramic frit.

[0013] The transparent ceramic frit of the present invention is added with zinc stannate, borate, niobium pentoxide, petalite and calcium silicate to improve the transparency of the prepared transparent ceramic frit. Zinc stannate decomposes at high temperature to form zinc oxide and tin dioxide, and the oxygen vacancies on the surface of SnO2 adsorb Zn 2+, forming Zn-O-Sn bonds, inhibiting agglomeration, and interacting with niobium pentoxide to form a solid solution, eliminating the ZnO / SnO2 phase boundary, reducing scattering centers, and Sn 4+ With Nb 5+ Covalent bonding reduces the absorption of light by free electrons and increases visible light transmittance. Petalite has a strong fluxing and crystallization reducing effect. Calcium silicate increases hardness while increasing light transmittance. 2+ Fill the network, with Sr 2+ Forming an ion size gradient. The B2O3 produced by the decomposition of boracic acid is a strong glass former, forming a uniform network structure with SiO2, inhibiting phase separation and crystallization, reducing light scattering centers, and improving light transmittance. At the same time, it can form a low-temperature eutectic with petalite, shortening the melting time. In addition, the magnesium oxide produced by the high-temperature decomposition of boracic acid acts as an external oxide in the network to increase the hardness. The addition of petalite can inhibit the phase change of cristobalite, eliminate microcrack scattering, and has a strong fluxing and viscosity-reducing effect, reducing bubble scattering. At the same time, it reacts with silicon dioxide to form a β-spodumene solid solution, reducing grain boundary scattering, playing a role in regulating the gradient of the refractive index, and reducing interface reflection. Ca2+, which is dissociated from calcium silicate at high temperature, 2+ Adsorbed on the surface of crystal nuclei, it increases the activation energy of crystallization and inhibits crystal growth. 2+ Embedding silicon-oxygen network holes improves the density of the glass frit, thereby improving the light transmittance of the glass frit.

[0014] The transparent ceramic frit described in the present invention also contains additional topaz and antimony oxide. The fluoride ions generated by the high-temperature decomposition of topaz break the Si-O-Si bonds, significantly reducing the melt viscosity. At the same time, the fluoride ions volatilize at high temperatures, promoting the merging and floating of microbubbles. The antimony oxide eliminates microbubbles and improves the smoothness of the prepared transparent ceramic frit.

[0015] The method for preparing the transparent ceramic frit of the present invention comprises the following steps:

[0016] (1) Quartz sand, calcined kaolin, pyrophyllite, strontium zirconate, zinc stannate, niobium pentoxide, borate, petalite, calcium silicate, topaz and antimony oxide are mixed in a certain weight ratio and added into a ball mill for grinding, and the ground material is dried and sieved;

[0017] (2) cold isostatic pressing the sieved material to obtain a ceramic frit body, and placing the ceramic frit body into a high-temperature furnace for sintering;

[0018] (3) The sintered product was first cooled to 840-850°C at a rate of 10°C / min, then cooled to 590-600°C at a rate of 1°C / min, placed in 5°C cold water for cooling, and then kept at 510-520°C for 1 hour. Finally, it was naturally cooled to room temperature to prepare a transparent ceramic frit.

[0019] in:

[0020] In step (1), water is used as a dispersant, zirconia balls are used as a grinding medium, the ball milling time is 40-45 min, the ball milling speed is 450 r / min, and the mass ratio of balls, materials, and water during ball milling is 2.7:1:0.7.

[0021] The drying in step (1) is to dry at 120°C to constant weight and pass through an 80-mesh sieve.

[0022] In step (2), the molding pressure is 110 MPa and the molding time is 3 min.

[0023] The sintering in step (2) is to heat the temperature to 590-600°C at a heating rate of 2°C / min and keep it warm for 1 hour, heat the temperature to 1040-1050°C at a heating rate of 5°C / min and keep it warm for 2.2 hours, heat the temperature to 1390-1400°C at a heating rate of 2°C / min and keep it warm for 1.5 hours, and heat the temperature to 1520-1530°C at a heating rate of 3°C / min and keep it warm for 2 hours.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] (1) The transparent ceramic frit described in the present invention uses quartz sand as the main raw material to provide a base network, adds calcined kaolin, pyrophyllite and strontium zirconate to improve the mechanical properties of the prepared transparent ceramic frit, adds zinc stannate, borate, niobium pentoxide, petalite and calcium silicate to improve the transparency of the prepared transparent ceramic frit, and adds topaz and antimony oxide to reduce the high-temperature melt viscosity and improve the smoothness of the prepared transparent ceramic frit. The synergistic effect between the raw materials ensures that the prepared transparent ceramic frit has excellent transparency and elastic modulus.

[0026] (2) The method for preparing the transparent ceramic frit of the present invention, through segmented temperature-controlled sintering and step-by-step cooling, ensures the high-temperature fluidity of the ceramic frit while reducing defects during the firing process, thereby ensuring that the performance of the prepared ceramic frit is stable. DETAILED DESCRIPTION

[0027] Example 1

[0028] The transparent ceramic frit described in Example 1 is composed of the following raw materials, in parts by weight: 50 parts of quartz sand, 12 parts of calcined kaolin, 8 parts of pyrophyllite, 3.2 parts of strontium zirconate, 5.7 parts of zinc stannate, 1.2 parts of niobium pentoxide, 10.3 parts of borate, 4.8 parts of petalite, 3.0 parts of calcium silicate, 3.1 parts of topaz, and 0.62 parts of antimony oxide.

[0029] in:

[0030] The petalite has the following chemical composition, calculated by mass percentage: SiO2 75.98%, Al2O3 17.02%, CaO 0.13%, MgO 0.04%, K2O 0.15%, Na2O 0.27%, LiO2 5.11%, and loss on ignition 1.30%.

[0031] The chemical composition of the boracic acid is as follows: MgO 32.68%, B2O3 33.85%, Cl 5.23%, Fe2O3 1.00%, SiO2 12.45%, Al2O3 2.01%, CaO3.02%, and loss on ignition 9.76%.

[0032] The chemical composition of the topaz, calculated by mass percentage, is as follows: Al2O3 52.29%, SiO2 34.25%, MgO 0.01%, CaO 0.23%, Fe2O3 0.29%, TiO2 0.04%, K2O 0.03%, Na2O 0.01%, F 11.73%, and loss on ignition 1.12%.

[0033] The method for preparing the transparent ceramic frit described in Example 1 comprises the following steps:

[0034] (1) Quartz sand, calcined kaolin, pyrophyllite, strontium zirconate, zinc stannate, niobium pentoxide, borate, petalite, calcium silicate, topaz and antimony oxide are mixed in a certain weight ratio and added into a ball mill for grinding, and the ground material is dried and sieved;

[0035] (2) cold isostatic pressing the sieved material to obtain a ceramic frit body, and placing the ceramic frit body into a high-temperature furnace for sintering;

[0036] (3) The sintered product was first cooled to 845°C at a rate of 10°C / min, then cooled to 595°C at a rate of 1°C / min, placed in 5°C cold water for cooling, and then kept at 515°C for 1 hour. Finally, it was naturally cooled to room temperature to prepare a transparent ceramic frit.

[0037] in:

[0038] In step (1), water is used as a dispersant, zirconia balls are used as a grinding medium, the ball milling time is 43 min, the ball milling speed is 450 r / min, and the mass ratio of balls, materials, and water during ball milling is 2.7:1:0.7.

[0039] The drying in step (1) is to dry at 120°C to constant weight and pass through an 80-mesh sieve.

[0040] In step (2), the molding pressure is 110 MPa and the molding time is 3 min.

[0041] The sintering in step (2) is to heat up to 595°C at a heating rate of 2°C / min and keep warm for 1 hour, heat up to 1045°C at a heating rate of 5°C / min and keep warm for 2.2 hours, heat up to 1395°C at a heating rate of 2°C / min and keep warm for 1.5 hours, and heat up to 1525°C at a heating rate of 3°C / min and keep warm for 2 hours.

[0042] Example 2

[0043] The transparent ceramic frit described in Example 2 is composed of the following raw materials, in parts by weight: 50 parts of quartz sand, 11 parts of calcined kaolin, 9 parts of pyrophyllite, 2.8 parts of strontium zirconate, 6.0 parts of zinc stannate, 1.3 parts of niobium pentoxide, 9.8 parts of borate, 5.0 parts of petalite, 3.3 parts of calcium silicate, 3.0 parts of topaz, and 0.64 parts of antimony oxide.

[0044] in:

[0045] The petalite has the following chemical composition, calculated by mass percentage: SiO2 75.98%, Al2O3 17.02%, CaO 0.13%, MgO 0.04%, K2O 0.15%, Na2O 0.27%, LiO2 5.11%, and loss on ignition 1.30%.

[0046] The chemical composition of the boracic acid is as follows: MgO 32.68%, B2O3 33.85%, Cl 5.23%, Fe2O3 1.00%, SiO2 12.45%, Al2O3 2.01%, CaO3.02%, and loss on ignition 9.76%.

[0047] The chemical composition of the topaz, calculated by mass percentage, is as follows: Al2O3 52.29%, SiO2 34.25%, MgO 0.01%, CaO 0.23%, Fe2O3 0.29%, TiO2 0.04%, K2O 0.03%, Na2O 0.01%, F 11.73%, and loss on ignition 1.12%.

[0048] The method for preparing the transparent ceramic frit described in Example 2 comprises the following steps:

[0049] (1) Quartz sand, calcined kaolin, pyrophyllite, strontium zirconate, zinc stannate, niobium pentoxide, borate, petalite, calcium silicate, topaz and antimony oxide are mixed in a certain weight ratio and added into a ball mill for grinding, and the ground material is dried and sieved;

[0050] (2) cold isostatic pressing the sieved material to obtain a ceramic frit body, and placing the ceramic frit body into a high-temperature furnace for sintering;

[0051] (3) The sintered product was first cooled to 840°C at a rate of 10°C / min, then cooled to 590°C at a rate of 1°C / min, placed in 5°C cold water for cooling, and then kept at 520°C for 1 hour. Finally, it was naturally cooled to room temperature to prepare a transparent ceramic frit.

[0052] in:

[0053] In step (1), water is used as a dispersant, zirconia balls are used as a grinding medium, the ball milling time is 40 min, the ball milling speed is 450 r / min, and the mass ratio of balls, materials, and water during ball milling is 2.7:1:0.7.

[0054] The drying in step (1) is to dry at 120°C to constant weight and pass through an 80-mesh sieve.

[0055] In step (2), the molding pressure is 110 MPa and the molding time is 3 min.

[0056] The sintering in step (2) is to heat up to 590°C at a heating rate of 2°C / min and keep warm for 1 hour, heat up to 1040°C at a heating rate of 5°C / min and keep warm for 2.2 hours, heat up to 1390°C at a heating rate of 2°C / min and keep warm for 1.5 hours, and heat up to 1520°C at a heating rate of 3°C / min and keep warm for 2 hours.

[0057] Example 3

[0058] The transparent ceramic frit described in Example 3 is composed of the following raw materials, in parts by weight: 50 parts of quartz sand, 13 parts of calcined kaolin, 7 parts of pyrophyllite, 3.5 parts of strontium zirconate, 5.5 parts of zinc stannate, 1.1 parts of niobium pentoxide, 10.8 parts of borate, 4.6 parts of petalite, 2.7 parts of calcium silicate, 3.2 parts of topaz, and 0.6 part of antimony oxide.

[0059] in:

[0060] The petalite has the following chemical composition, calculated by mass percentage: SiO2 75.98%, Al2O3 17.02%, CaO 0.13%, MgO 0.04%, K2O 0.15%, Na2O 0.27%, LiO2 5.11%, and loss on ignition 1.30%.

[0061] The chemical composition of the boracic acid is as follows: MgO 32.68%, B2O3 33.85%, Cl 5.23%, Fe2O3 1.00%, SiO2 12.45%, Al2O3 2.01%, CaO3.02%, and loss on ignition 9.76%.

[0062] The chemical composition of the topaz, calculated by mass percentage, is as follows: Al2O3 52.29%, SiO2 34.25%, MgO 0.01%, CaO 0.23%, Fe2O3 0.29%, TiO2 0.04%, K2O 0.03%, Na2O 0.01%, F 11.73%, and loss on ignition 1.12%.

[0063] The method for preparing the transparent ceramic frit described in Example 3 comprises the following steps:

[0064] (1) Quartz sand, calcined kaolin, pyrophyllite, strontium zirconate, zinc stannate, niobium pentoxide, borate, petalite, calcium silicate, topaz and antimony oxide are mixed in a certain weight ratio and added into a ball mill for grinding, and the ground material is dried and sieved;

[0065] (2) cold isostatic pressing the sieved material to obtain a ceramic frit body, and placing the ceramic frit body into a high-temperature furnace for sintering;

[0066] (3) The sintered product was first cooled to 850°C at a rate of 10°C / min, then cooled to 600°C at a rate of 1°C / min, placed in 5°C cold water for cooling, and then kept at 520°C for 1 hour. Finally, it was naturally cooled to room temperature to prepare a transparent ceramic frit.

[0067] in:

[0068] In step (1), water is used as a dispersant, zirconia balls are used as a grinding medium, the ball milling time is 45 min, the ball milling speed is 450 r / min, and the mass ratio of balls, materials, and water during ball milling is 2.7:1:0.7.

[0069] The drying in step (1) is to dry at 120°C to constant weight and pass through an 80-mesh sieve.

[0070] In step (2), the molding pressure is 110 MPa and the molding time is 3 min.

[0071] The sintering in step (2) is to heat the sample to 600°C at a heating rate of 2°C / min and keep the temperature for 1 hour, heat the sample to 1050°C at a heating rate of 5°C / min and keep the temperature for 2.2 hours, heat the sample to 1400°C at a heating rate of 2°C / min and keep the temperature for 1.5 hours, and heat the sample to 1530°C at a heating rate of 3°C / min and keep the temperature for 2 hours.

[0072] Comparative Example 1

[0073] The transparent ceramic frit described in Comparative Example 1 was prepared in the same manner as in Example 1, differing only in the raw material composition. The transparent ceramic frit described in Comparative Example 1 was composed, by weight, of the following raw materials: 50 parts quartz sand, 5.7 parts zinc stannate, 1.2 parts niobium pentoxide, 10.3 parts borate, 4.8 parts petalite, 3.0 parts calcium silicate, 3.1 parts topaz, and 0.62 parts antimony oxide.

[0074] Comparative Example 2

[0075] The transparent ceramic frit described in Comparative Example 2 was prepared in the same manner as in Example 1, differing only in the raw material composition. The transparent ceramic frit described in Comparative Example 2 was composed, by weight, of the following raw materials: 50 parts quartz sand, 12 parts calcined kaolin, 8 parts pyrophyllite, 3.2 parts strontium zirconate, 10.3 parts borate, 4.8 parts petalite, 3.0 parts calcium silicate, 3.1 parts topaz, and 0.62 parts antimony oxide.

[0076] Comparative Example 3

[0077] The transparent ceramic frit described in Comparative Example 3 was prepared in the same manner as in Example 1, differing only in the raw material composition. The transparent ceramic frit described in Comparative Example 3 was composed, by weight, of the following raw materials: 50 parts quartz sand, 12 parts calcined kaolin, 8 parts pyrophyllite, 3.2 parts strontium zirconate, 5.7 parts zinc stannate, 1.2 parts niobium pentoxide, 3.1 parts topaz, and 0.62 parts antimony oxide.

[0078] The transparent ceramic frits prepared in Examples 1-3 and Comparative Examples 1-3 were subjected to performance tests. The transmittance was measured in accordance with GB / T3296-2021, and the elastic modulus was measured using a dynamic elastic modulus meter. The results are shown in Table 1 below:

[0079] Table 1 Performance test results of transparent ceramic frits prepared in Examples 1-3 and Comparative Examples 1-2

[0080]

[0081] As shown in Table 1, the elastic modulus and transparency of the transparent ceramic frits prepared in Examples 1-3 are much higher than those in Comparative Examples 1-3. The elastic modulus measures the strength of the bonds between atoms, molecules, or ions within a material, as well as the rigidity of its structure. A high elastic modulus indicates a very rigid material, making it difficult to elastically stretch or compress even under significant stress. It also means that the transparent ceramic frit has a denser, more rigid glass network structure. Compared with Example 1, Comparative Example 1 has a significantly decreased elastic modulus of the prepared transparent ceramic frit due to the absence of calcined kaolin, pyrophyllite, and strontium zirconate, and its transparency is also affected to a certain extent. Compared with Example 1, Comparative Example 2 has an increased number of scattering centers due to the absence of zinc stannate and niobium pentoxide, which greatly decreases the transparency of the prepared transparent ceramic frit and also affects its elastic modulus to a certain extent. Compared with Example 1, Comparative Example 3 has a lack of crystallization-inhibiting substances due to the absence of boracite, petalite, and calcium silicate, which decreases the transparency of the prepared transparent ceramic frit and also affects its elastic modulus to a certain extent. Therefore, the raw materials described in this application cooperate with each other to ensure the excellent performance of the prepared transparent ceramic frit.

Claims

1. A transparent ceramic frit, characterized in that: The invention is composed of the following raw materials in parts by weight: 50 parts of quartz sand, 11-13 parts of calcined kaolin, 7-9 parts of pyrophyllite, 2.8-3.5 parts of strontium zirconate, 5.5-6.0 parts of zinc stannate, 1.1-1.3 parts of niobium pentoxide, 9.8-10.8 parts of borate, 4.6-5.0 parts of petalite, 2.7-3.3 parts of calcium silicate, 3.0-3.2 parts of topaz, and 0.6-0.64 parts of antimony oxide.

2. The transparent ceramic frit according to claim 1, characterized in that: The petalite has the following chemical composition, calculated by mass percentage: SiO2 75.98%, Al2O3 17.02%, CaO 0.13%, MgO 0.04%, K2O 0.15%, Na2O 0.27%, LiO2 5.11%, and loss on ignition 1.30%.

3. The transparent ceramic frit according to claim 1, wherein: The chemical composition of the boracic acid is as follows: MgO 32.68%, B2O3 33.85%, Cl 5.23%, Fe2O3 1.00%, SiO2 12.45%, Al2O3 2.01%, CaO 3.02%, and loss on ignition 9.76%.

4. The transparent ceramic frit according to claim 1, wherein: The chemical composition of the topaz, calculated by mass percentage, is as follows: Al2O3 52.29%, SiO2 34.25%, MgO 0.01%, CaO 0.23%, Fe2O3 0.29%, TiO2 0.04%, K2O 0.03%, Na2O 0.01%, F 11.73%, and loss on ignition 1.12%.

5. The transparent ceramic frit according to claim 1, wherein: The invention is composed of the following raw materials in parts by mass: 50 parts of quartz sand, 12 parts of calcined kaolin, 8 parts of pyrophyllite, 3.2 parts of strontium zirconate, 5.7 parts of zinc stannate, 1.2 parts of niobium pentoxide, 10.3 parts of borate, 4.8 parts of petalite, 3.0 parts of calcium silicate, 3.1 parts of topaz, and 0.62 parts of antimony oxide.

6. A method for preparing the transparent ceramic frit according to claim 1, characterized in that: It consists of the following steps: (1) Quartz sand, calcined kaolin, pyrophyllite, strontium zirconate, zinc stannate, niobium pentoxide, borate, petalite, calcium silicate, topaz and antimony oxide are mixed in a certain weight ratio and added into a ball mill for grinding, and the ground material is dried and sieved; (2) cold isostatic pressing the sieved material to obtain a ceramic frit body, and placing the ceramic frit body into a high-temperature furnace for sintering; (3) The sintered product was first cooled to 840-850°C at a rate of 10°C / min, then cooled to 590-600°C at a rate of 1°C / min, placed in 5°C cold water for cooling, and then kept at 510-520°C for 1 hour. Finally, it was naturally cooled to room temperature to prepare a transparent ceramic frit.

7. The method for preparing a transparent ceramic frit according to claim 6, wherein: In step (1), water is used as a dispersant, zirconia balls are used as a grinding medium, the ball milling time is 40-45 min, the ball milling speed is 450 r / min, and the mass ratio of balls, materials, and water during ball milling is 2.7:1:0.

7.

8. The method for preparing a transparent ceramic frit according to claim 6, wherein: The drying in step (1) is to dry at 120°C to constant weight and pass through an 80-mesh sieve.

9. The method for preparing a transparent ceramic frit according to claim 6, wherein: In step (2), the molding pressure is 110 MPa and the molding time is 3 min.

10. The method for preparing a transparent ceramic frit according to claim 6, wherein: The sintering in step (2) is to heat the temperature to 590-600°C at a heating rate of 2°C / min and keep it warm for 1 hour, heat the temperature to 1040-1050°C at a heating rate of 5°C / min and keep it warm for 2.2 hours, heat the temperature to 1390-1400°C at a heating rate of 2°C / min and keep it warm for 1.5 hours, and heat the temperature to 1520-1530°C at a heating rate of 3°C / min and keep it warm for 2 hours.

Citation Information

Patent Citations

  • Yellow high-gloss glaze material for ceramics and preparation method thereof

    CN102491793A

  • 12-degree soft-light porcelain glaze facing bricks

    CN107540344A