Ceramic tile with iridescent structural color and preparation method thereof

By applying a variety of feather -like structures formed by a variety of rare earth elements on the surface of the tiles, combined with the silk mesh method and spraying technology, it solves the problem of complexity and defects in the development of crystal glaze application. Improve physical properties.

CN119350063AActive Publication Date: 2025-01-24QINGYUAN GANI CERAMICS CO LTD +2

Patent Information

Application Number
CN202411309570.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-19
Publication Date
2025-01-24
Estimated Expiration
2044-09-19

AI Technical Summary

Technical Problem

In the prior art, the application development of crystalline glaze is limited by the complex process conditions and the many defects in the finished glaze surface, which limits its commercial production.

Method used

By adding niobium pentoxide, zirconium silicate, yttrium oxide, cerium oxide, scandium oxide and other rare earth elements, a well-proportioned and interlocking feather-like microstructure is formed, bionicly simulating the microscopic morphology of natural kingfisher feathers, using wire mesh Dry and spray techniques apply a crystallized glaze layer and protective layer to the tile surface.

Benefits of technology

It achieves the special visual effect of iridescent structural color on the surface of ceramic tiles, improves the artistic effect and physical properties of ceramic tiles, and solves the problems of complex and defective traditional crystallized glaze processes.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of ceramic tiles, in particular to a ceramic tile with an iridescent structural color and a preparation method of the ceramic tile. The invention discloses a ceramic tile with an iridescent structural color. The ceramic tile comprises a green body, a cover glaze layer is arranged on the green body, a pattern layer is arranged on the cover glaze layer, a crystal glaze layer is arranged on the pattern layer, and a protective layer is arranged on the crystal glaze layer. The crystal glaze layer comprises the following raw materials in parts by weight: 30-50 parts of feldspar, 5-20 parts of quartz, 5-15 parts of dolomite, 5-10 parts of talc, 1-5 parts of kaolin, 2-7 parts of niobium pentoxide, 3-5 parts of zirconium silicate, 1-3 parts of yttrium oxide, 1-3 parts of cerium oxide and 0.5-2 parts of scandium oxide. According to the ceramic tile, various rare earth elements are added, mixed material dry particles of the crystal glaze layer form well-proportioned and staggered occlusion feather-shaped microstructures on the microscopic level, the micromorphology similar to natural turnip feathers is simulated in a bionic mode, and the special visual effect of iridescent structural color is shown.
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Description

Technical Field

[0001] The invention relates to the technical field of ceramic tiles, and in particular to a ceramic tile with iridescent structural color and a preparation method thereof. Background Art

[0002] Crystalline glaze refers to a glaze that introduces one or more crystallizing agents into the basic ceramic glaze, so that it is supersaturated during the melting process of the glaze and precipitates during the cooling process, thus forming crystal flowers. Crystalline glaze is an artificial crystal flower glaze developed on the basis of ancient colored glaze in my country. The ancients used the crystallization properties of inorganic compounds to prepare the world-famous microcrystalline iron-based crystal glaze: Tianmu glaze. Tea leaves, rabbit hair, oil drops, Tianmu, etc. in the Song Dynasty in my country are all precious varieties of crystallized glaze.

[0003] The composition of crystalline glaze mainly includes three parts: crystallizing agent, basic glaze and colorant.

[0004] Among the basic glazes, the concentration of silica and other crystalline substances has the greatest impact, that is, the so-called supersaturation. It is a key factor affecting the composition of crystalline glazes. If the supersaturation is low, the crystals are difficult to grow; if the supersaturation is too high, the crystal nuclei will accumulate, the crystal flowers will be too small or the crystallization will be rough.

[0005] Crystallization agent is mainly used to adjust the firing temperature, viscosity and thermal expansion coefficient of crystalline glaze. The content of alkali metal oxide cannot be too much, otherwise the crystallization effect will be weakened, while alkaline earth metal oxide will promote crystallization.

[0006] In addition to the crystalline components, the main function of the colorant is to give the glaze and crystal flowers a specific color tone. Generally, the amount used is small and the impact is small. Rare earth elements have the function of inducing structural colors in different crystalline glazes. For example, CeO2 in willemite crystalline glaze makes the crystal flowers appear blue, while in pyroxene crystalline glaze, the crystal flowers appear pink.

[0007] However, the application and development of crystalline glaze in the ceramic industry is still relatively small. The main reason is that the traditional crystalline glaze has complex process conditions and many defects on the glaze surface of the finished product, which limits its commercial production.

[0008] To this end, the present application provides a ceramic tile with iridescent structural color and a method for preparing the same. Summary of the invention

[0009] The present application provides a ceramic tile with iridescent structural color and a preparation method thereof. The ceramic tile is formed with a staggered and interlocking feather-like microstructure at the microscopic level by adding a plurality of rare earth elements such as niobium pentoxide, zirconium silicate, yttrium oxide, cerium oxide, and scandium oxide. The mixed dry particles of the crystalline glaze layer form a microscopically staggered and interlocking feather-like microstructure, biomimetically simulating a microscopic morphology similar to that of natural kingfisher feathers, and showing a special visual effect of iridescent structural color.

[0010] The technical solution adopted by this application to solve its technical problem is:

[0011] The first object of the present application is to provide a ceramic tile with iridescent structural color, comprising a body, a surface glaze layer is arranged on the body, a pattern layer is arranged on the surface glaze layer, a crystalline glaze layer is arranged on the pattern layer, and a protective layer is arranged on the crystalline glaze layer;

[0012] The crystalline glaze layer comprises the following raw materials in parts by weight:

[0013] 30-50 parts of feldspar, 5-20 parts of quartz, 5-15 parts of dolomite, 5-10 parts of talc, 1-5 parts of kaolin, 2-7 parts of niobium pentoxide, 3-5 parts of zirconium silicate, 1-3 parts of yttrium oxide, 1-3 parts of cerium oxide, and 0.5-2 parts of scandium oxide.

[0014] The preparation process of the mixture of the crystalline glaze layer comprises the following steps:

[0015] According to the weight composition of the raw materials of the crystalline glaze layer, weigh the corresponding raw materials;

[0016] The raw materials are mixed and put into a high-temperature melting furnace. After the addition is completed, the temperature is raised to 1580°C and kept warm for 5 hours. After the insulation is completed, the molten liquid is water quenched and cooled to room temperature to form a mixture of a crystalline glaze layer.

[0017] In some embodiments, the protective layer comprises the following raw materials in parts by weight:

[0018] 34-40 parts of albite, 3.5-7.5 parts of kaolin, 3-6 parts of alumina, 18.5-22.5 parts of calcite, 0.5-1.5 parts of dolomite, 2.5-4.5 parts of zinc oxide, and 6-10 parts of zircon powder.

[0019] The preparation process of the mixture of the protective layer comprises the following steps:

[0020] According to the weight composition of the raw materials of the protective layer, the corresponding raw materials are weighed; the raw materials are mixed to obtain a primary mixture, the primary mixture is calcined and melted at 1130-1160° C. to a dry particle slurry, the dry particle slurry is water quenched, and cooled to room temperature; the mixture is crushed and passed through a 60-120 mesh sieve to obtain a protective layer mixture.

[0021] In some embodiments, the thickness of the crystalline glaze layer is 0.5-2 mm.

[0022] In some embodiments, the protective layer has a thickness of 0.5-2 mm.

[0023] The second object of the present application is to provide a method for preparing the above-mentioned ceramic tile, comprising the following steps:

[0024] S1. Applying glaze on the surface of the body to obtain a body containing a glaze layer;

[0025] S2. On the surface of the glaze layer, inkjet printing a design pattern to obtain a body containing a pattern layer;

[0026] S3. preparing a mixture of a crystalline glaze layer;

[0027] S4. Preparing a mixture for a protective layer;

[0028] S5. On the surface of the pattern layer, applying the mixture of the crystalline glaze layer obtained in step S3 by a screen dry method, and spraying the mixture of the protective layer on the crystalline glaze layer;

[0029] S6. The green body of the mixture sprayed with the spray protective layer is fired and polished to obtain a tile with iridescent structural color.

[0030] In some embodiments, in step S5, the mesh size of the wire mesh in the wire mesh dry method is 40 meshes.

[0031] In some embodiments, in step S6, the sintering temperature is 1130-1160°C.

[0032] The beneficial effects of this application are:

[0033] 1. The preparation method described in the present application uses a screen dry method to accurately position dry particles with different refractive ratios on the plate surface, thereby forming a decorative effect with iridescent structural color on the local ceramic glaze layer.

[0034] 2. The ceramic tile described in the present application, through the addition of multiple rare earth elements such as niobium pentoxide, zirconium silicate, yttrium oxide, cerium oxide, and scandium oxide, the mixed material dry particles of the crystalline glaze layer form a staggered and interlocking feather-like microstructure at the microscopic level, bionic simulation of the microscopic morphology similar to natural kingfisher feathers, showing the special visual effect of iridescent structural color. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] The present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0036] Figure 1 This is a process flow chart of a method for preparing a ceramic tile with iridescent structural color described in this application.

[0037] Figure 2 This is a product appearance diagram of a ceramic tile with iridescent structural color according to Example 1 described in the present application. DETAILED DESCRIPTION

[0038] In order to facilitate the understanding of those skilled in the art, the present invention is further described below in conjunction with embodiments, and the contents mentioned in the implementation modes are not intended to limit the present invention.

[0039] As used herein, "and / or" includes the term of any and all combinations of one or more associated listed items. The terms used herein are only used to describe specific embodiments and are not intended to limit the present invention. As used herein, the singular forms "a", "an", "an" and "the" are also intended to include the plural forms, unless the context clearly indicates otherwise. It is further understood that "including", when used in this specification, specifies the stated features, integers, steps, operations, elements and / or compositions, but does not exclude the existence or addition of one or more other features, integers, steps, operations, elements, compositions and / or combinations thereof.

[0040] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention belongs. It is further understood that terms, such as defined in commonly used dictionaries, are interpreted in accordance with their meanings in the context of the relevant art and are not in an idealized or overly formal sense unless explicitly so defined herein.

[0041] The exemplary invention described herein may appropriately lack any one or more element limitations that are not specifically disclosed herein. Therefore, the terms "comprise", "include", "contain", etc. should be understood broadly and non-restrictively. In addition, the terminology used herein is used as a description, not a limitation, and it is unintentional to use these terminology expressions that do not include any equivalent characteristics, but only describe some of their characteristics, but various modifications are possible within the scope of the present invention according to the rights. Therefore, although the present invention has been specifically disclosed by preferred embodiments and optional features, the modifications disclosed herein to embody the changes of the present invention may be recorded by those skilled in the art, and such modifications and changes will be considered to be within the scope of the present invention.

[0042] Terminology explanation:

[0043] The green body, as the main structure of the tile, is the basis of tile manufacturing. It is a semi-finished product with a certain strength and shape made from ceramic raw materials through processes such as molding, drying, and firing. The main function of the green body is to support the overall structure of the tile, withstand external pressure and load, and provide a stable base for subsequent glaze layers, pattern layers, and crystallized glaze layers. The green body can be made using conventional, existing processes.

[0044] The glaze layer, as a decorative layer on the surface of the tile, mainly plays the role of beautifying the tile and improving the texture of the tile. It covers the surface of the body, which can not only protect the body from external erosion, but also make the tile present a rich and diverse appearance through different colors and texture designs; in this application, the glaze layer can be made by conventional and existing processes.

[0045] A ceramic tile with iridescent structural color, comprising a body, a surface glaze layer is arranged on the body, a pattern layer is arranged on the surface glaze layer, a crystal glaze layer is arranged on the pattern layer, and a protective layer is arranged on the crystal glaze layer;

[0046] The crystalline glaze layer comprises the following raw materials in parts by weight:

[0047] 30-50 parts of feldspar, 5-20 parts of quartz, 5-15 parts of dolomite, 5-10 parts of talc, 1-5 parts of kaolin, 2-7 parts of niobium pentoxide, 3-5 parts of zirconium silicate, 1-3 parts of yttrium oxide, 1-3 parts of cerium oxide, and 0.5-2 parts of scandium oxide.

[0048] Specifically, in crystalline glazes, niobium pentoxide is a key component. It forms an [NbO6] octahedral structure and connects with oxygen atoms as an external body in the network in the form of non-bridging oxygen, effectively reducing the high-temperature viscosity of the glaze melt. This characteristic change promotes the growth of phase separation droplets in the glaze, which in turn affects the mechanism of structural color generation in the glaze layer, making the color richer and more diverse.

[0049] It is understandable that the addition of Nb2O5 provides the basic conditions for the formation of structural colors by changing the high-temperature fluidity and phase separation behavior of the glaze. At the same time, the structural characteristics of [NbO] octahedron optimize the scattering effect of light in the glaze layer, thus producing a more obvious iridescence effect.

[0050] Specifically, in crystalline glazes, zirconium silicate usually exists as a reinforcing agent and stabilizer. It not only improves the hardness and wear resistance of the glaze layer, but also optimizes the crystal structure and distribution through synergistic effects with other rare earth elements, further enhancing the artistic effect and physical properties of the glaze layer.

[0051] It is understandable that the addition of zirconium silicate makes it easier for the glaze layer to form stable and fine grains during the firing process. These grains provide the glaze layer with unique optical properties through light scattering and interference. At the same time, the interaction between zirconium silicate and other rare earth elements also promotes the formation of a more complex crystal structure, improving the overall quality of the glaze layer.

[0052] Specifically, in crystalline glazes, yttrium oxide is mainly used as a crystallization promoter. It can effectively reduce the formation temperature of certain crystal phases, promote the crystallization process, and improve the purity and crystallinity of the crystals. This allows the glaze layer to obtain a good crystallization effect at a lower firing temperature, reducing energy consumption and improving production efficiency.

[0053] It is understandable that the ionic radius of Y2O3 is similar to that of other metal cations in the glaze, so it can easily enter the lattice position in the glaze and form a stable solid solution or composite crystal with other components. This structural optimization makes it easier for crystals to form and grow, thereby improving the crystallization effect and performance of the glaze layer.

[0054] Specifically, in crystalline glazes, cerium oxide has a significant color-enhancing and color-adjusting effect. It can change the optical properties of certain crystal phases in the glaze layer by cooperating with other metal cations, thereby producing different color effects. In addition, CeO2 can also enhance the weather resistance and UV resistance of the glaze layer, making ceramic tiles more durable.

[0055] It is understandable that the valence change of CeO2 and the chemical reaction with other components in the glaze are the main reasons for its color-enhancing and color-adjusting effects. In different crystal structures, the valence state of CeO2 can change, which in turn affects the light absorption and reflection properties of the crystal. At the same time, the interaction between CeO2 and other metal cations in the glaze also promotes the formation of more complex crystal structures, making the color of the glaze layer richer and more varied.

[0056] Specifically, in crystalline glaze, scandium oxide mainly plays the role of increasing crystallinity and increasing grain size. It can promote the formation of large-grained crystals by optimizing the growth conditions of crystals, and increase the density and hardness of the glaze layer. This makes the ceramic tile have a more beautiful appearance while also having higher physical strength and wear resistance.

[0057] It is understandable that the addition of Sc2O3 can reduce the nucleation barrier of the glaze and promote the formation and growth of crystal nuclei. At the same time, it can also synergize with other rare earth elements to further optimize the growth environment and structure of the crystal. This optimized crystal growth condition enables the glaze layer to form a more complete and dense crystal structure during the firing process, thereby improving the overall performance of the glaze layer.

[0058] Therefore, through the addition of multiple rare earth elements such as niobium pentoxide, zirconium silicate, yttrium oxide, cerium oxide and scandium oxide, the mixed dry particles of the crystalline glaze layer form a staggered and interlocking feather-like microstructure at the microscopic level, bionically simulating the microscopic morphology similar to natural kingfisher feathers, showing the special visual effect of iridescent structural color.

[0059] In some embodiments, the preparation process of the mixture of the crystalline glaze layer comprises the following steps:

[0060] According to the weight composition of the raw materials of the crystalline glaze layer, weigh the corresponding raw materials;

[0061] The raw materials are mixed and put into a high-temperature melting furnace. After the addition is completed, the temperature is raised to 1580°C and kept warm for 5 hours. After the insulation is completed, the molten liquid is water quenched and cooled to room temperature to form a mixture of a crystalline glaze layer.

[0062] Specifically, the raw materials are mixed and placed in a silicon-molybdenum rod high-temperature melting furnace, and multiple feeding methods are used to prevent overflow due to the volume expansion of the batch materials during the melting process. The batch materials are added at 1450°C, and after the feeding is completed, the temperature is raised to 1580°C and kept for 5 hours, and stirred twice to promote homogenization and eliminate bubbles. The molten liquid is placed in a water quenching basin, and after cooling to room temperature, the desired dry particles are formed, which are crushed and passed through a 60-120 mesh sieve to obtain a mixture of a crystalline glaze layer.

[0063] In some embodiments, the protective layer comprises the following raw materials in parts by weight:

[0064] 34-40 parts of albite, 3.5-7.5 parts of kaolin, 3-6 parts of alumina, 18.5-22.5 parts of calcite, 0.5-1.5 parts of dolomite, 2.5-4.5 parts of zinc oxide, and 6-10 parts of zircon powder.

[0065] Specifically, in protective glaze, zircon powder is mainly used as a reinforcing agent and opacifier. Zircon powder can improve the hardness and wear resistance of the glaze layer, making the surface of the ceramic tile more scratch-resistant and corrosion-resistant. At the same time, the opacifying effect of zircon powder can also cover up the defects and color differences in the glaze layer, making the surface of the ceramic tile smoother and more beautiful.

[0066] In some embodiments, the preparation process of the mixture of the protective layer comprises the following steps:

[0067] According to the weight composition of the raw materials of the protective layer, the corresponding raw materials are weighed; the raw materials are mixed to obtain a primary mixture, the primary mixture is calcined and melted at 1130-1160° C. to a dry particle slurry, the dry particle slurry is water quenched, and cooled to room temperature; the mixture is crushed and passed through a 60-120 mesh sieve to obtain a protective layer mixture.

[0068] In some embodiments, the thickness of the crystalline glaze layer is 0.5-2 mm.

[0069] In some embodiments, the protective layer has a thickness of 0.5-2 mm.

[0070] In a second aspect, the present application provides a method for preparing the above-mentioned ceramic tile, comprising the following steps:

[0071] S1. Applying glaze on the surface of the body to obtain a body containing a glaze layer;

[0072] S2. On the surface of the glaze layer, inkjet printing a design pattern to obtain a body containing a pattern layer;

[0073] S3. preparing a mixture of a crystalline glaze layer;

[0074] S4. Preparing a mixture for a protective layer;

[0075] S5. On the surface of the pattern layer, 60-130 mesh crystalline glaze dry particles are scraped onto the surface of the body of S2 using a 40 mesh screen with a pattern through a screen printing machine. The amount of dry particles per square meter is between 20-50g depending on the pattern effect. Then, the mixture of the crystalline glaze layer prepared in step S3 is applied on the surface through a dry particle spreading machine. The amount of the spreading is 730-780g per square meter.

[0076] S6. The green body of the mixture sprayed with the spray protective layer is fired and polished to obtain a tile with iridescent structural color.

[0077] In some embodiments, in step S5, the mesh size of the wire mesh in the wire mesh dry method is 40 meshes.

[0078] In some embodiments, in step S6, the sintering temperature is 1130-1160°C.

[0079] Example 1

[0080] A method for preparing a ceramic tile with iridescent structural color comprises the following steps:

[0081] S1. Applying glaze on the surface of the body to obtain a body containing a glaze layer;

[0082] S2. On the surface of the glaze layer, inkjet printing a design pattern to obtain a body containing a pattern layer;

[0083] S3. preparing a mixture of a crystalline glaze layer;

[0084] According to the raw material composition of the crystalline glaze layer by weight, 30 parts of feldspar, 5 parts of quartz, 5 parts of dolomite, 5 parts of talc, 1 part of kaolin, 2 parts of niobium pentoxide, 3 parts of zirconium silicate, 1 part of yttrium oxide, 1 part of cerium oxide, and 0.5 parts of scandium oxide are weighed;

[0085] Mix all the raw materials and put them into the silicon-molybdenum rod high-temperature melting furnace. Use multiple feeding methods to prevent overflow due to the volume expansion of the batch materials during the melting process. Add them at 1450℃. After the feeding is completed, raise the temperature to 1580℃ and keep it for 5 hours. Stir twice to promote homogenization and eliminate bubbles. Put the molten liquid into a water quenching basin, and after cooling to room temperature, form the required dry particles, crush them and pass through a 60-120 mesh sieve to obtain a mixture for the crystallized glaze layer.

[0086] S4. Preparing a mixture for a protective layer;

[0087] According to the raw material composition of the protective layer in parts by weight, 34 parts of albite, 3.5 parts of kaolin, 3 parts of alumina, 18.5 parts of calcite, 0.5 parts of dolomite, 2.5 parts of zinc oxide and 6 parts of zircon powder are weighed; the raw materials are mixed to obtain a primary mixture, the primary mixture is calcined and melted at 1130-1160°C to a dry particle slurry, the dry particle slurry is water quenched, and cooled to room temperature; the mixture is crushed and passed through a 60-120 mesh sieve to obtain a mixture for the protective layer.

[0088] S5. On the surface of the pattern layer, the mixture of the crystalline glaze layer obtained in step S3 is dry-applied through a 40-mesh screen, and the mixture of the spray protective layer on the crystalline glaze layer;

[0089] S6. The green body of the mixture sprayed with the spray protective layer is fired and polished to obtain a tile with iridescent structural color.

[0090] Example 2

[0091] A method for preparing a ceramic tile with iridescent structural color comprises the following steps:

[0092] S1. Applying glaze on the surface of the body to obtain a body containing a glaze layer;

[0093] S2. On the surface of the glaze layer, inkjet printing a design pattern to obtain a body containing a pattern layer;

[0094] S3. preparing a mixture of a crystalline glaze layer;

[0095] According to the raw material composition of the crystalline glaze layer by weight, 50 parts of feldspar, 20 parts of quartz, 15 parts of dolomite, 10 parts of talc, 5 parts of kaolin, 7 parts of niobium pentoxide, 5 parts of zirconium silicate, 3 parts of yttrium oxide, 3 parts of cerium oxide, and 2 parts of scandium oxide are weighed;

[0096] Mix all the raw materials and put them into the silicon-molybdenum rod high-temperature melting furnace. Use multiple feeding methods to prevent overflow due to the volume expansion of the batch materials during the melting process. Add them at 1450℃. After the feeding is completed, raise the temperature to 1580℃ and keep it for 5 hours. Stir twice to promote homogenization and eliminate bubbles. Put the molten liquid into a water quenching basin, and after cooling to room temperature, form the required dry particles, crush them and pass through a 60-120 mesh sieve to obtain a mixture for the crystallized glaze layer.

[0097] S4. Preparing a mixture for a protective layer;

[0098] According to the raw material composition of the protective layer in parts by weight, 40 parts of albite, 7.5 parts of kaolin, 6 parts of aluminum oxide, 22.5 parts of calcite, 1.5 parts of dolomite, 4.5 parts of zinc oxide and 10 parts of zircon powder are weighed; the raw materials are mixed to obtain a primary mixture, the primary mixture is calcined and melted at 1130-1160°C to a dry particle slurry, the dry particle slurry is water quenched, and cooled to room temperature; the mixture is crushed and passed through a 60-120 mesh sieve to obtain a mixture for the protective layer.

[0099] S5. On the surface of the pattern layer, the mixture of the crystalline glaze layer obtained in step S3 is dry-applied through a 40-mesh screen, and the mixture of the spray protective layer on the crystalline glaze layer;

[0100] S6. The green body of the mixture sprayed with the spray protective layer is fired and polished to obtain a tile with iridescent structural color.

[0101] Example 3

[0102] A method for preparing a ceramic tile with iridescent structural color comprises the following steps:

[0103] S1. Applying glaze on the surface of the body to obtain a body containing a glaze layer;

[0104] S2. On the surface of the glaze layer, inkjet printing a design pattern to obtain a body containing a pattern layer;

[0105] S3. preparing a mixture of a crystalline glaze layer;

[0106] According to the raw material composition of the crystalline glaze layer by weight, 40 parts of feldspar, 15 parts of quartz, 10 parts of dolomite, 8 parts of talc, 3 parts of kaolin, 4 parts of niobium pentoxide, 4 parts of zirconium silicate, 2 parts of yttrium oxide, 2 parts of cerium oxide, and 1 part of scandium oxide are weighed;

[0107] Mix all the raw materials and put them into the silicon-molybdenum rod high-temperature melting furnace. Use multiple feeding methods to prevent overflow due to the volume expansion of the batch materials during the melting process. Add them at 1450℃. After the feeding is completed, raise the temperature to 1580℃ and keep it for 5 hours. Stir twice to promote homogenization and eliminate bubbles. Put the molten liquid into a water quenching basin, and after cooling to room temperature, form the required dry particles, crush them and pass through a 60-120 mesh sieve to obtain a mixture for the crystallized glaze layer.

[0108] S4. Preparing a mixture for a protective layer;

[0109] According to the raw material composition of the protective layer in parts by weight, 38 parts of albite, 5 parts of kaolin, 4 parts of aluminum oxide, 20 parts of calcite, 1 part of dolomite, 3 parts of zinc oxide and 8 parts of zircon powder are weighed; the raw materials are mixed to obtain a primary mixture, the primary mixture is calcined and melted at 1130-1160°C to a dry particle slurry, the dry particle slurry is water quenched, and cooled to room temperature; the mixture is crushed and passed through a 60-120 mesh sieve to obtain a mixture for the protective layer.

[0110] S5. On the surface of the pattern layer, the mixture of the crystalline glaze layer obtained in step S3 is dry-applied through a 40-mesh screen, and the mixture of the spray protective layer on the crystalline glaze layer;

[0111] S6. The green body of the mixture sprayed with the spray protective layer is fired and polished to obtain a tile with iridescent structural color.

[0112] Example 4

[0113] A method for preparing a ceramic tile with iridescent structural color comprises the following steps:

[0114] S1. Applying glaze on the surface of the body to obtain a body containing a glaze layer;

[0115] S2. On the surface of the glaze layer, inkjet printing a design pattern to obtain a body containing a pattern layer;

[0116] S3. preparing a mixture of a crystalline glaze layer;

[0117] According to the raw material composition of the crystalline glaze layer by weight, 30 parts of feldspar, 20 parts of quartz, 5 parts of dolomite, 10 parts of talc, 1 part of kaolin, 7 parts of niobium pentoxide, 3 parts of zirconium silicate, 1 part of yttrium oxide, 3 parts of cerium oxide, and 0.5 parts of scandium oxide are weighed;

[0118] Mix all the raw materials and put them into the silicon-molybdenum rod high-temperature melting furnace. Use multiple feeding methods to prevent overflow due to the volume expansion of the batch materials during the melting process. Add them at 1450℃. After the feeding is completed, raise the temperature to 1580℃ and keep it for 5 hours. Stir twice to promote homogenization and eliminate bubbles. Put the molten liquid into a water quenching basin, and after cooling to room temperature, form the required dry particles, crush them and pass through a 60-120 mesh sieve to obtain a mixture for the crystallized glaze layer.

[0119] S4. Preparing a mixture for a protective layer;

[0120] According to the raw material composition of the protective layer in parts by weight, 34 parts of albite, 3.5 parts of kaolin, 3 parts of alumina, 22.5 parts of calcite, 0.5 parts of dolomite, 4.5 parts of zinc oxide and 6 parts of zircon powder are weighed; the raw materials are mixed to obtain a primary mixture, the primary mixture is calcined and melted at 1130-1160°C to a dry particle slurry, the dry particle slurry is water quenched, and cooled to room temperature; the mixture is crushed and passed through a 60-120 mesh sieve to obtain a mixture for the protective layer.

[0121] S5. On the surface of the pattern layer, the mixture of the crystalline glaze layer obtained in step S3 is dry-applied through a 40-mesh screen, and the mixture of the spray protective layer on the crystalline glaze layer;

[0122] S6. The green body of the mixture sprayed with the spray protective layer is fired and polished to obtain a tile with iridescent structural color.

[0123] Example 5

[0124] A method for preparing a ceramic tile with iridescent structural color comprises the following steps:

[0125] S1. Applying glaze on the surface of the body to obtain a body containing a glaze layer;

[0126] S2. On the surface of the glaze layer, inkjet printing a design pattern to obtain a body containing a pattern layer;

[0127] S3. preparing a mixture of a crystalline glaze layer;

[0128] According to the raw material composition of the crystalline glaze layer by weight, 35 parts of feldspar, 8 parts of quartz, 7 parts of dolomite, 6 parts of talc, 2 parts of kaolin, 3 parts of niobium pentoxide, 3 parts of zirconium silicate, 3 parts of yttrium oxide, 1 part of cerium oxide, and 1 part of scandium oxide are weighed;

[0129] Mix all the raw materials and put them into the silicon-molybdenum rod high-temperature melting furnace. Use multiple feeding methods to prevent overflow due to the volume expansion of the batch materials during the melting process. Add them at 1450℃. After the feeding is completed, raise the temperature to 1580℃ and keep it for 5 hours. Stir twice to promote homogenization and eliminate bubbles. Put the molten liquid into a water quenching basin, and after cooling to room temperature, form the required dry particles, crush them and pass through a 60-120 mesh sieve to obtain a mixture for the crystallized glaze layer.

[0130] S4. Preparing a mixture for a protective layer;

[0131] According to the raw material composition of the protective layer in parts by weight, 34 parts of albite, 4 parts of kaolin, 4 parts of alumina, 19 parts of calcite, 0.6 parts of dolomite, 3 parts of zinc oxide and 7 parts of zircon powder are weighed; the raw materials are mixed to obtain a primary mixture, the primary mixture is calcined and melted at 1130-1160°C to a dry particle slurry, the dry particle slurry is water quenched, and cooled to room temperature; the mixture is crushed and passed through a 60-120 mesh sieve to obtain a mixture for the protective layer.

[0132] S5. On the surface of the pattern layer, the mixture of the crystalline glaze layer obtained in step S3 is dry-applied through a 40-mesh screen, and the mixture of the spray protective layer on the crystalline glaze layer;

[0133] S6. The green body of the mixture sprayed with the spray protective layer is fired and polished to obtain a tile with iridescent structural color.

[0134] Comparative Example 1

[0135] A method for preparing a tile comprises the following steps:

[0136] In the mixed material for preparing the crystalline glaze layer in step S3, niobium pentoxide, zirconium silicate, yttrium oxide, cerium oxide and scandium oxide are not added;

[0137] The remaining conditions are the same as those in Example 1.

[0138] Comparative Example 2

[0139] A method for preparing a tile comprises the following steps:

[0140] The step S4 of preparing the mixture for the protective layer is not performed; and in the step S5, the mixture for the crystalline glaze layer prepared in the step S3 is dry-applied on the surface of the pattern layer through a 40-mesh screen; and in the step S6, the body to which the mixture for the crystalline glaze layer is applied is fired and polished to obtain a tile with iridescent structural color.

[0141] The remaining conditions are the same as those in Example 1.

[0142] In the mixed material for preparing the crystalline glaze layer in step S3, niobium pentoxide, zirconium silicate, yttrium oxide, cerium oxide and scandium oxide are not added;

[0143] The remaining conditions are the same as those in Example 1.

[0144] Comparative Example 3

[0145] A method for preparing a tile comprises the following steps:

[0146] In the step S4 of preparing the mixture for the protective layer, no zircon powder is added;

[0147] The remaining conditions are the same as those in Example 1.

[0148] The ceramic tiles prepared in Examples 1-5 and Comparative Examples 1-3 were subjected to the following performance tests, and the test results are summarized in Table 1:

[0149] (1) Wear resistance: GB / T3810.7-2016 test method is used.

[0150] (2) Vickers hardness, tested using a Vickers hardness tester;

[0151] Wear resistance Vickers hardness Example 1 Level 3 1500 rpm 7.5 Example 2 Level 3 1500 rpm 7.5 Example 3 Level 3 1500 rpm 7 Example 4 Level 3 1500 rpm 7 Example 5 Level 3 1500 rpm 7.4 Comparative Example 1 Level 3 750 rpm 7 Comparative Example 2 Second level 600 rpm 5 Comparative Example 3 Level 3 750 rpm 6

[0152] The raw materials or reagents used in the examples and comparative examples of the present invention are all purchased from mainstream manufacturers in the market. Those without indicating the manufacturer or concentration are all analytically pure raw materials or reagents that can be routinely obtained. As long as they can play the expected role, there is no special limitation.

[0153] The instruments and equipment used in this embodiment are all purchased from major manufacturers in the market, and there is no particular limitation as long as they can play the expected role. In this embodiment, if no specific technology or conditions are specified, the technology or conditions described in the literature in this field or the product instructions are used. The above embodiments are preferred implementation schemes of the present invention. In addition, the present invention can also be implemented in other ways. Any obvious replacement without departing from the concept of the present invention is within the protection scope of the present invention.

Claims

1. A ceramic tile with iridescent structural color, comprising a body, a glaze layer is arranged on the body, and a pattern layer is arranged on the glaze layer, characterized in that: A crystallized glaze layer is disposed on the patterned part, and a protective layer is disposed on the crystallized glaze layer; The crystalline glaze layer comprises the following raw materials in parts by weight: 30-50 parts of feldspar, 5-20 parts of quartz, 5-15 parts of dolomite, 5-10 parts of talc, 1-5 parts of kaolin, 2-7 parts of niobium pentoxide, 3-5 parts of zirconium silicate, 1-3 parts of yttrium oxide, 1-3 parts of cerium oxide, and 0.5-2 parts of scandium oxide.

2. The ceramic tile according to claim 1, characterized in that: The protective layer comprises the following raw materials in parts by weight: 34-40 parts of albite, 3.5-7.5 parts of kaolin, 3-6 parts of alumina, 18.5-22.5 parts of calcite, 0.5-1.5 parts of dolomite, 2.5-4.5 parts of zinc oxide, and 6-10 parts of zircon powder.

3. The tile according to claim 1, characterized in that: The crystalline glaze layer comprises the following raw materials in parts by weight: 40 parts of feldspar, 15 parts of quartz, 10 parts of dolomite, 8 parts of talc, 3 parts of kaolin, 4 parts of niobium pentoxide, 4 parts of zirconium silicate, 2 parts of yttrium oxide, 2 parts of cerium oxide, and 1 part of scandium oxide.

4. The ceramic tile according to claim 1, characterized in that: The preparation process of the mixture of the crystalline glaze layer comprises the following steps: According to the weight composition of the raw materials of the crystalline glaze layer, weigh the corresponding raw materials; The raw materials are mixed and put into a high-temperature melting furnace. After the addition is completed, the temperature is raised to 1580°C and kept warm for 5 hours. After the insulation is completed, the molten liquid is water quenched and cooled to room temperature to form a mixture of a crystalline glaze layer.

5. The ceramic tile according to claim 1, characterized in that: The preparation process of the mixture of the protective layer comprises the following steps: According to the weight composition of the raw materials of the protective layer, the corresponding raw materials are weighed; the raw materials are mixed to obtain a primary mixture, the primary mixture is calcined and melted at 1130-1160° C. to a dry particle slurry, the dry particle slurry is water quenched, and cooled to room temperature; the mixture is crushed and passed through a 60-120 mesh sieve to obtain a protective layer mixture.

6. The ceramic tile according to claim 1, characterized in that: The thickness of the crystalline glaze layer is 0.5-2 mm.

7. The tile according to claim 1, characterized in that: The thickness of the protective layer is 0.5-2 mm.

8. The method for preparing a ceramic tile according to any one of claims 1 to 7, characterized in that: The following steps are involved: S1. Applying glaze on the surface of the body to obtain a body containing a glaze layer; S2. On the surface of the glaze layer, inkjet printing a design pattern to obtain a body containing a pattern layer; S3. preparing a mixture of a crystalline glaze layer; S4. Preparing a mixture for a protective layer; S5. On the surface of the pattern layer, applying the mixture of the crystalline glaze layer obtained in step S3 by a screen dry method, and spraying the mixture of the protective layer on the crystalline glaze layer; S6. The green body of the mixture sprayed with the spray protective layer is fired and polished to obtain a tile with iridescent structural color. 9 . The preparation method according to claim 8 , wherein in step S5 , the mesh size of the screen in the screen dry method is 40 meshes.

10. The preparation method according to claim 8, wherein in step S6, the sintering temperature is 1130-1160°C.

Citation Information

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