A ceramic tile with a gradient gloss effect and a three-dimensional texture and a preparation method thereof

Abstract

The present invention relates to the field of building ceramics, and discloses a ceramic tile with a gradient gloss effect and three-dimensional texture and a preparation method thereof, comprising the following steps: S1, pressing the green body powder material into shape to obtain a green body layer; S2, applying a base glaze on the surface of the green body layer to obtain a base glaze layer; S3, inkjet printing a texture on the surface of the base glaze layer to obtain a pattern layer; S4, printing a high-gloss glaze on the surface of the pattern layer to obtain a high-gloss glaze layer; S5, spraying a matte glaze on the surface of the high-gloss glaze layer to obtain a matte glaze layer; S6, performing laser engraving on the matte glaze layer to obtain a three-dimensional texture; S7, firing and shaping to obtain a ceramic tile with a gradient gloss effect and three-dimensional texture. By compounding a high-gloss glaze with a high refractive index and a matte glaze with a low refractive index, the present invention realizes differences in temperature, gloss, and degree of vitrification through local covering and differences in the melting degree during firing, so that after firing, the glaze surface presents an effect of gradient gloss and three-dimensional texture under the action of light reflection.

Description

Technical Field

[0001] The invention relates to the field of building ceramics, and in particular to a ceramic tile with a gradient gloss effect and a three-dimensional texture and a preparation method thereof. Background Art

[0002] Ceramic tiles are widely favored by consumers due to their excellent performance and decorative effects, and are widely used in the construction industry and people's daily life. Ceramic tiles on the market can be roughly divided into high-gloss glazed tiles and matte glazed tiles, and the glossiness is relatively single. In the prior art, the transition effect between gloss and matte is achieved by inkjet superposition of gloss and matte inks, but it has defects such as unnatural glaze light transition, high cost, poor pattern texture layering, and lack of three-dimensionality. Therefore, research and development of ceramic tiles that can make light present a gradient gloss effect and three-dimensional texture after reflection through the glaze has become a problem that needs to be solved urgently. Summary of the invention

[0003] The main purpose of the present invention is to provide a ceramic tile with a gradient gloss effect and a three-dimensional texture and a preparation method thereof, wherein the prepared ceramic tile glaze has a natural gradient gloss and a three-dimensional texture.

[0004] To achieve the above object, the present invention provides a method for preparing a tile with a gradient gloss effect and a three-dimensional texture, comprising the following steps:

[0005] S1, pressing the green body powder into a shape, and after drying, obtaining a green body layer;

[0006] S2, applying a base glaze on the surface of the green body layer to obtain a base glaze layer;

[0007] S3, inkjet printing a texture on the surface of the base glaze layer to obtain a pattern layer;

[0008] S4, screen printing a high-gloss glaze on the surface of the pattern layer to obtain a high-gloss glaze layer;

[0009] S5, spraying matte glaze on the surface of the high-gloss glaze layer using a high-pressure glaze spray cabinet to obtain a matte glaze layer;

[0010] S6, performing laser engraving on the surface of the matte glaze layer to obtain a three-dimensional texture;

[0011] S7, firing and molding, that is, obtaining the ceramic tile with a gradient gloss effect and a three-dimensional texture;

[0012] The raw materials for preparing the high gloss glaze in step S4 include, by weight: 28 to 40 parts of potassium feldspar, 17 to 25 parts of quartz, 8 to 15 parts of kaolin, 10 to 16 parts of high transparent frit, 2 to 4 parts of niobium pentoxide, 7 to 14 parts of dolomite, 1 to 4 parts of zirconium silicate, 1.5 to 4 parts of perlite and 2 to 4 parts of nanomaterials;

[0013] The raw materials for preparing the matte glaze in step S5, by weight, include: 30-45 parts of high-temperature dry particles, 8-12 parts of medium-temperature dry particles, 6-15 parts of opacifier, 20-35 parts of suspending agent, 11-23 parts of auxiliary agent, and 8-13 parts of water.

[0014] In the present invention, a high-gloss glaze with a high refractive index is compounded with a matte glaze with a low refractive index, and differences in temperature, gloss, and degree of vitrification are achieved through local covering and differences in the melting degree during firing, so that the fired glaze surface presents a gradually changing gloss effect under the action of light reflection.

[0015] Preferably, the nanomaterial is SiO2-coated TiO2 powder. Using SiO2-coated TiO2 powder can enhance the glaze surface performance and improve the glaze surface hardness and wear resistance.

[0016] Preferably, the chemical composition of the high-transparency frit, by mass percentage, includes:

[0017] SiO2 60%-75%;

[0018] Al2O3 5%-15%;

[0019] B2O3 5%-10%;

[0020] Na2O and / or K2O 10%-20%;

[0021] CaO and / or MgO 1%-5%;

[0022] ZnO 0%-5%;

[0023] The chemical composition of the high-temperature dry particles, by mass percentage, includes:

[0024] SiO2 50%-70%;

[0025] Al2O3 10%-25%;

[0026] B2O3 0%-8%;

[0027] ZnO 0%-5%;

[0028] ZrO2 0%-5%;

[0029] Alkali metal oxides 2%-10%;

[0030] Alkaline earth metal oxides 5%-15%;

[0031] The chemical composition of the medium-temperature dry particles, by mass percentage, includes:

[0032] SiO2 52%-66%;

[0033] Al2O3 10% - 12%;

[0034] Na2O and / or K2O 5% - 15%;

[0035] ZnO 5% - 7%;

[0036] SrO 2% - 3%;

[0037] Alkaline earth metal oxide 9% - 15.5%;

[0038] The alkali metal oxide is at least one of Na2O, K2O and Li2O; the alkaline earth metal oxide is at least one of CaO, MgO and BaO.

[0039] Preferably, the thickness of the high - gloss glaze layer is 180 - 360 μm, and the refractive index of the high - gloss glaze layer is 1.68 - 1.72; the thickness of the matte glaze layer is 90 - 180 μm, and the refractive index of the matte glaze layer is 1.45 - 1.55. By adjusting the refractive index between the high - gloss glaze layer and the matte glaze layer, and using the gloss difference formed by the different refractive indexes after firing of the two, a good gradient gloss effect of the glaze surface can be achieved.

[0040] Preferably, the opacifier includes one or both of zirconium silicate and calcium fluoride. Zirconium silicate can form microcrystals or incompletely melted particles to scatter light, reducing the glaze surface gloss and refractive index. Fluoride ions in calcium fluoride promote the formation of microporous structures on the glaze surface during firing, enhancing the matte effect.

[0041] Preferably, the auxiliary agent includes one or both of calcium phosphate and tetragonal alumina. Tetragonal alumina can improve the hardness and stability of the glaze layer, and calcium phosphate scatters light to reduce the glossiness and refractive index.

[0042] Preferably, in step S6, a three - dimensional texture with a depth of 10 - 50 μm is engraved on the surface of the matte glaze layer. The two - dimensional texture formed by the local misalignment and stacking of the high - refractive glaze layer and the low - refractive glaze layer, combined with the three - dimensional texture formed by laser engraving on the glaze surface, can enhance the three - dimensional effect of the tile surface pattern, making the texture more real and restored.

[0043] Preferably, the raw materials for preparing the green body layer, by weight, include: 10 - 15 parts of kaolin, 12 - 16 parts of potassium - sodium feldspar powder, 6 - 11 parts of high - alumina potassium sand, 10 - 13 parts of sodium feldspar powder, 9 - 14 parts of potassium sand, 14 - 19 parts of raw ore clay, 2 - 5 parts of black talc, 3 - 8 parts of polishing waste residue, 9 - 14 parts of washed sand, 5 - 9 parts of washed clay, and 0.8 - 1.5 parts of additive.

[0044] Preferably, in step S7, the firing temperature is 1180 - 1225 °C, and the firing time is 55 - 76 min.

[0045] The present invention also provides a ceramic tile with a gradient gloss effect and a three-dimensional texture, which is prepared by the above-mentioned preparation method. The prepared ceramic tile can present a natural gradient gloss effect while ensuring durability, and is more three-dimensional and vivid in combination with the three-dimensional texture, restoring real stone materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0046] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other relevant drawings can also be obtained based on these drawings.

[0047] Figure 1 Glaze effect of Example 1 Figure 1 ;

[0048] Figure 2 Glaze effect of Example 1 Figure 2 。

[0049] The realization of the purpose of the present application, functional features and advantages will be further described in combination with the embodiments with reference to the drawings. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0050] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some of the embodiments of the present invention, rather than all of them. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the protection scope of the present invention. It should be noted that, without conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. At the same time, for the raw materials not detailedly described below, they are all commercially available products; for the process steps or preparation methods not detailedly mentioned, they are all process steps or preparation methods known to those skilled in the art.

[0051] The present invention provides a preparation method for a ceramic tile with a gradient gloss effect and a three-dimensional texture, including the following steps:

[0052] S1. Pressing the green body powder into a shape and drying it to obtain a green body layer; preferably, the raw materials for preparing the green body layer, in parts by weight, include: 10-15 parts of kaolin, 12-16 parts of sodium potassium stone powder, 6-11 parts of high-aluminum potassium sand, 10-13 parts of sodium stone powder, 9-14 parts of potassium sand, 14-19 parts of raw ore mud, 2-5 parts of black talc, 3-8 parts of polishing waste residue, 9-14 parts of washed sand, 5-9 parts of washed mud and 0.8-1.5 parts of additives.

[0053] S2, applying a bottom glaze on the surface of the body layer, and drying it in a drying oven at a drying temperature of 80° C. for 30 seconds to obtain a bottom glaze layer;

[0054] S3, inkjet printing a texture on the surface of the base glaze layer to obtain a pattern layer;

[0055] S4. Screen-printed high-gloss glaze is applied on the surface of the pattern layer, and dried in a drying oven at a temperature of 120°C for 20 seconds to obtain a high-gloss glaze layer having a thickness of 180-360 μm and a refractive index of 1.68-1.72. Specifically, the raw materials for preparing the high-gloss glaze include, by weight: 28-40 parts of potassium feldspar, 17-25 parts of quartz, 8-15 parts of kaolin, 10-16 parts of high-transparent frit, 2-4 parts of niobium pentoxide, 7-14 parts of dolomite, 1-4 parts of zirconium silicate, 1.5-4 parts of perlite, and 2-4 parts of nanomaterials. The chemical composition of the high-transparency frit is calculated by mass percentage, including: SiO2: 60% to 75%, Al2O3: 5% to 15%, B2O3: 5% to 10%, Na2O and / or K2O: 10% to 20%, CaO and / or MgO: 1% to 5%, ZnO: 0% to 5%. It is understood that the chemical composition of the high-transparency frit includes at least one of Na2O and K2O, and the total amount accounts for 10% to 20%; similarly, the chemical composition of the high-transparency frit includes at least one of CaO and MgO, and the total amount accounts for 1% to 5%. Preferably, the nanomaterial is SiO2-coated TiO2 powder.

[0056] S5. Spray matte glaze on the surface of the high-gloss glaze layer using a high-pressure spraying cabinet, and dry it in a drying oven at a drying temperature of 150 °C for 1 minute to obtain a matte glaze layer with a thickness of 90 - 180 μm and a refractive index of 1.45 - 1.55. Specifically, the raw materials for preparing the matte glaze, in parts by weight, include: 30 - 45 parts of high-temperature dry particles, 8 - 12 parts of medium-temperature dry particles, 6 - 15 parts of opacifier, 20 - 35 parts of suspending agent, 11 - 23 parts of auxiliary agent, and 8 - 13 parts of water. Among them, the sintering temperature of the high-temperature dry particles is 30 - 40 °C higher than that of the medium-temperature dry particles. The chemical composition of the high-temperature dry particles, by mass percentage, includes: SiO2: 50% - 70%, Al2O3: 10% - 25%, B2O3: 0% - 8%, ZnO: 0% - 5%, ZrO2: 0% - 5%, alkali metal oxides: 2% - 10%, alkaline earth metal oxides: 5% - 15%; The chemical composition of the medium-temperature dry particles, by mass percentage, includes: SiO2: 52% - 66%, Al2O3: 10% - 12%, Na2O and / or K2O: 5% - 15%, ZnO: 5% - 7%, SrO: 2% - 3%, alkaline earth metal oxides: 9% - 15.5%. The alkali metal oxides are at least one of Na2O, K2O, and Li2O; the alkaline earth metal oxides are at least one of CaO, MgO, and BaO. It can be understood that the chemical composition of the high-temperature dry particles includes at least one of Na2O, K2O, and Li2O, and the total proportion is 2% - 10%; the chemical composition of the high-temperature dry particles also includes at least one of CaO, MgO, and BaO, and the total proportion is 5% - 15%; the chemical composition of the medium-temperature dry particles includes at least one of Na2O and K2O, and the total proportion is 5% - 15%; the chemical composition of the medium-temperature dry particles also includes at least one of CaO, MgO, and BaO, and the total proportion is 9% - 15.5%.

[0057] Preferably, the opacifier includes one or both of zirconium silicate and calcium fluoride; the auxiliary agent includes one or both of calcium phosphate and tetragonal alumina. The suspending agent can be a well-known organic suspending agent that can be used in glazes. The suspending agent used in the following examples of this application is a dry particle suspending agent, namely, the dry particle suspending agent 9022A purchased from Jiangxi Qiantao New Materials Co., Ltd.

[0058] S6. Engrave a three-dimensional texture with a depth of 10 - 50 μm on the surface of the matte glaze layer. Specifically, a laser etching machine can be used for bionic texture engraving.

[0059] S7. Fire and form at a firing temperature of 1180 - 1225 °C for 55 - 76 min to obtain the tile with a gradient gloss effect and three-dimensional texture.

[0060] The following are further examples to illustrate the present invention in detail. It should also be understood that the following examples are only used to further illustrate the present invention and should not be construed as limiting the protection scope of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the above content of the present invention all fall within the protection scope of the present invention. The specific process parameters in the following examples are only an example within a suitable range, that is, those skilled in the art can make selections within a suitable range through the description herein, rather than being limited to the specific values in the following examples. For those not specified in the examples, they are carried out under conventional conditions or conditions recommended by the manufacturer.

[0061] Exemplarily, the raw materials of the base glaze formulation in the following examples and comparative examples are in parts by mass and are as follows: 25 parts of potassium feldspar, 10 parts of sodium feldspar, 22 parts of quartz, 12 parts of kaolin, 8 parts of calcite, 5 parts of talc, 3 parts of zinc oxide, 3 parts of barium carbonate, 2 parts of bentonite, and 10 parts of zirconium silicate.

[0062] The additives used in the raw materials of the green body layer in the following examples are one or several of sodium tripolyphosphate, water glass, carboxymethyl cellulose (CMC), and green body plasticizer, all of which are commercially available products.

[0063] Example 1

[0064] A method for preparing a ceramic tile with a gradient gloss effect and three-dimensional texture, comprising the following steps:

[0065] S1. Press and mold the green body powder, and after drying, obtain the green body layer; the raw materials for preparing the green body layer, in parts by weight, include: 13 parts of kaolin, 12 parts of potassium-sodium stone powder, 8 parts of high-aluminum potassium sand, 11 parts of sodium stone powder, 10 parts of potassium sand, 16 parts of raw ore clay, 3 parts of black talc, 6 parts of polishing waste residue, 12 parts of washed sand, 8 parts of washed clay, and 1 part of sodium tripolyphosphate.

[0066] S2. Apply the base glaze on the surface of the green body layer, and dry it in a drying oven at a drying temperature of 80°C for 30 seconds to obtain the base glaze layer;

[0067] S3. Inkjet print the texture on the surface of the base glaze layer to obtain the pattern layer;

[0068] S4. Screen-print the high-gloss glaze on the surface of the pattern layer, and dry it in a drying oven at a drying temperature of 120°C for 20 seconds to obtain the high-gloss glaze layer, the thickness of the high-gloss glaze layer is 180 μm, and the refractive index is 1.72; the raw materials for preparing the high-gloss glaze, in parts by weight, include: 28 parts of potassium feldspar, 17 parts of quartz, 15 parts of kaolin, 16 parts of high-transparency frit, 4 parts of niobium pentoxide, 14 parts of dolomite, 1 part of zirconium silicate, 2 parts of perlite, and 2 parts of SiO2-coated TiO2 powder.

[0069] The chemical composition of the high-transparent frit is expressed in percentage by mass and includes: SiO2: 60%, Al2O3: 15%, B2O3: 10%, Na2O: 6%, K2O: 4%, MgO: 2%, and ZnO: 3%.

[0070] S5. Spray matte glaze on the surface of the high-gloss glaze layer using a high-pressure spray glaze cabinet, and dry it in a drying oven at a drying temperature of 150°C for 1 minute to obtain a matte glaze layer with a thickness of 90 μm and a refractive index of 1.55. The raw materials for preparing the matte glaze, in parts by weight, include: 30 parts of high-temperature dry particles, 12 parts of medium-temperature dry particles, 6 parts of zirconium silicate, 25 parts of 9022A, 19 parts of calcium phosphate, and 8 parts of water. Among them, the sintering temperature of the high-temperature dry particles is 40°C higher than that of the medium-temperature dry particles.

[0071] The chemical composition of the high temperature dry particles, in terms of mass percentage, includes: SiO2: 50%, Al2O3: 25%, B2O3: 5%, K2O: 2%, Li2O: 2%, CaO: 6%, BaO: 4%, ZnO: 3%, ZrO2: 3%;

[0072] The chemical composition of the medium-temperature dry particles, in terms of mass percentage, includes: SiO2: 52%, Al2O3: 10%, Na2O: 10%, K2O: 4%, MgO: 9%, BaO: 6%, ZnO: 7%, and SrO: 2%.

[0073] S6. A laser etching machine is used to carve a three-dimensional texture with a depth of 10 μm on the surface of the matte glaze layer.

[0074] S7, firing and molding, the firing temperature is 1180° C., and the firing time is 76 minutes, so as to obtain the ceramic tile with the gradient gloss effect.

[0075] Example 2

[0076] A method for preparing a tile with a gradient gloss effect and a three-dimensional texture comprises the following steps:

[0077] S1. Press the green body powder into shape, and after drying, obtain a green body layer; the raw materials for preparing the green body layer, in parts by weight, include: 10 parts of kaolin, 16 parts of potassium sodium stone powder, 11 parts of high-aluminum potassium sand, 10 parts of sodium stone powder, 9 parts of potassium sand, 19 parts of raw ore mud, 2 parts of black talc, 3 parts of polishing waste residue, 14 parts of washed sand, 5 parts of washed mud and 1 part of water glass.

[0078] S2, applying a bottom glaze on the surface of the body layer, and drying it in a drying oven at a drying temperature of 80° C. for 30 seconds to obtain a bottom glaze layer;

[0079] S3, inkjet printing a texture on the surface of the base glaze layer to obtain a pattern layer;

[0080] S4. Apply high-gloss glaze on the surface of the pattern layer and dry it in a drying oven at a drying temperature of 120 °C for 20 seconds to obtain a high-gloss glaze layer with a thickness of 360 μm and a refractive index of 1.68. The raw materials for preparing the high-gloss glaze, by weight, include: 32 parts of potassium feldspar, 17 parts of quartz, 11 parts of kaolin, 14 parts of high-transparency frit, 4 parts of niobium pentoxide, 14 parts of dolomite, 3 parts of zirconium silicate, 2 parts of perlite, and 2 parts of SiO2-coated TiO2 powder.

[0081] The chemical composition of the high-transparency frit, by mass percentage, includes: SiO2: 60%, Al2O3: 15%, B2O3: 10%, Na2O: 6%, K2O: 4%, MgO: 2%, ZnO: 3%.

[0082] S5. Spray matte glaze on the surface of the high-gloss glaze layer and dry it in a drying oven at a drying temperature of 150 °C for 1 minute to obtain a matte glaze layer with a thickness of 180 μm and a refractive index of 1.45. The raw materials for preparing the matte glaze, by weight, include: 45 parts of high-temperature dry particles, 8 parts of medium-temperature dry particles, 6 parts of calcium fluoride, 20 parts of 9022A, 11 parts of tetragonal alumina, and 10 parts of water. Among them, the sintering temperature of the high-temperature dry particles is 30 °C higher than that of the medium-temperature dry particles.

[0083] The chemical composition of the high-temperature dry particles, by mass percentage, includes: SiO2: 50%, Al2O3: 25%, B2O3: 5%, K2O: 2%, Li2O: 2%, CaO: 6%, BaO: 4%, ZnO: 3%, ZrO2: 3%;

[0084] The chemical composition of the medium-temperature dry particles, by mass percentage, includes: SiO2: 52%, Al2O3: 10%, Na2O: 10%, K2O: 4%, MgO: 9%, BaO: 6%, ZnO: 7%, SrO: 2%.

[0085] S6. Use a laser engraving machine to engrave a three-dimensional texture with a depth of 50 μm on the surface of the matte glaze layer.

[0086] S7. Fire and form at a firing temperature of 1225 °C for 55 min to obtain the tile with the gradient gloss effect.

[0087] Example 3

[0088] A method for preparing a tile with a gradient gloss effect and a three-dimensional texture, comprising the following steps:

[0089] S1. Press the green body powder into shape, and after drying, obtain a green body layer; the raw materials for preparing the green body layer, in parts by weight, include: 15 parts of kaolin, 12 parts of potassium sodium stone powder, 6 parts of high-aluminum potassium sand, 12 parts of sodium stone powder, 13 parts of potassium sand, 14 parts of raw ore mud, 5 parts of black talc, 8 parts of polishing waste residue, 9 parts of washed sand, 5 parts of washed mud and 1 part of CMC.

[0090] S2, applying a bottom glaze on the surface of the body layer, and drying it in a drying oven at a drying temperature of 80° C. for 30 seconds to obtain a bottom glaze layer;

[0091] S3, inkjet printing a texture on the surface of the base glaze layer to obtain a pattern layer;

[0092] S4. Screen-printed high-gloss glaze is applied on the surface of the pattern layer, and dried in a drying oven at a temperature of 120°C for 20 seconds to obtain a high-gloss glaze layer with a thickness of 270 μm and a refractive index of 1.70. The raw materials for preparing the high-gloss glaze include, by weight: 40 parts of potassium feldspar, 17 parts of quartz, 10 parts of kaolin, 13 parts of high-transparent frit, 2 parts of niobium pentoxide, 14 parts of dolomite, 1 part of zirconium silicate, 2 parts of perlite and 4 parts of SiO2-coated TiO2 powder.

[0093] The chemical composition of the high-transparent frit is expressed in percentage by mass and includes: SiO2: 60%, Al2O3: 15%, B2O3: 10%, Na2O: 6%, K2O: 4%, MgO: 2%, and ZnO: 3%.

[0094] S5. Spray matte glaze on the surface of the high-gloss glaze layer using a high-pressure spray glaze cabinet, dry it in a drying oven at a temperature of 150°C for 1 minute, and obtain a matte glaze layer with a thickness of 130 μm and a refractive index of 1.50; the raw materials for preparing the matte glaze, in parts by weight, include: 36 parts of high-temperature dry particles, 10 parts of medium-temperature dry particles, 5 parts of zirconium silicate, 5 parts of calcium fluoride, 20 parts of 9022A, 10 parts of calcium phosphate, 5 parts of tetragonal alumina, and 9 parts of water. Among them, the sintering temperature of the high-temperature dry particles is 30°C higher than that of the medium-temperature dry particles.

[0095] The chemical composition of the high temperature dry particles, in terms of mass percentage, includes: SiO2: 50%, Al2O3: 25%, B2O3: 5%, K2O: 2%, Li2O: 2%, CaO: 6%, BaO: 4%, ZnO: 3%, ZrO2: 3%;

[0096] The chemical composition of the medium-temperature dry particles, in terms of mass percentage, includes: SiO2: 52%, Al2O3: 10%, Na2O: 10%, K2O: 4%, MgO: 9%, BaO: 6%, ZnO: 7%, and SrO: 2%.

[0097] S6. Use a laser engraving machine to engrave a three-dimensional texture with a depth of 30 μm on the surface of the matte glaze layer.

[0098] S7. Fire and form, with a firing temperature of 1200 °C and a firing time of 65 min, thus obtaining the tile with a gradient gloss effect.

[0099] Comparative Example 1

[0100] This comparative example uses the same preparation process and parameters as Example 1, with the only difference being:

[0101] The raw materials for preparing the high-gloss glaze, by weight, include: 28 parts of potassium feldspar, 17 parts of quartz, 15 parts of kaolin, 16 parts of high-transparency frit, 4 parts of niobium pentoxide, 14 parts of dolomite, 1 part of zirconium silicate, and 2 parts of perlite.

[0102] Comparative Example 2

[0103] This comparative example uses the same preparation process and parameters as Example 1, with the only difference being:

[0104] The raw materials for preparing the matte glaze, by weight, include: 42 parts of high-temperature dry granules, 6 parts of zirconium silicate, 25 parts of 9022A, 19 parts of calcium phosphate, and 8 parts of water.

[0105] Comparative Example 3

[0106] This comparative example uses the same preparation process and parameters as Example 1, with the only difference being:

[0107] The raw materials for preparing the matte glaze, by weight, include: 42 parts of medium-temperature dry granules, 6 parts of zirconium silicate, 25 parts of 9022A, 19 parts of calcium phosphate, and 8 parts of water.

[0108] Comparative Example 4

[0109] This comparative example uses the same preparation process and parameters as Example 1, with the only difference being:

[0110] Adjust the application thickness of the high-gloss glaze layer to 150 μm.

[0111] Comparative Example 5

[0112] This comparative example uses the same preparation process and parameters as Example 1, with the only difference being:

[0113] Adjust the application thickness of the high-gloss glaze layer to 400 μm.

[0114] Comparative Example 6

[0115] This comparative example uses the same preparation process and parameters as Example 1, with the only difference being:

[0116] Adjust the glazing thickness of the matte glaze layer to 60 μm.

[0117] Comparative Example 7

[0118] This comparative example uses the same preparation process and parameters as Example 1, with the only difference being that:

[0119] Adjust the glazing thickness of the matte glaze layer to 200 μm.

[0120] Comparative Example 8

[0121] A method for preparing a ceramic tile with a gradient gloss effect and three-dimensional texture, comprising the following steps:

[0122] S1. Press and mold the green body powder, and after drying, obtain the green body layer; the raw materials for preparing the green body layer, in parts by weight, include: 13 parts of kaolin, 12 parts of potassium sodium feldspar powder, 8 parts of high-aluminum potassium sand, 11 parts of sodium feldspar powder, 10 parts of potassium sand, 16 parts of raw ore clay, 3 parts of black talc, 6 parts of polished waste residue, 12 parts of washed sand, 8 parts of washed clay, and 1 part of sodium tripolyphosphate.

[0123] S2. Apply a base glaze on the surface of the green body layer, and dry it in a drying oven at a drying temperature of 80 °C and a drying time of 30 seconds to obtain the base glaze layer;

[0124] S3. Inkjet print the texture on the surface of the base glaze layer to obtain the pattern layer;

[0125] S4. Spray the matte glaze on the surface of the pattern layer using a high-pressure glazing cabinet, and dry it in a drying oven at a drying temperature of 150 °C and a drying time of 1 minute to obtain the matte glaze layer. The thickness of the matte glaze layer is 90 μm, and the refractive index is 1.55; the raw materials for preparing the matte glaze, in parts by weight, include: 30 parts of high-temperature dry granules, 12 parts of medium-temperature dry granules, 6 parts of zirconium silicate, 25 parts of 9022A, 19 parts of calcium phosphate, and 8 parts of water. Among them, the sintering temperature of the high-temperature dry granules is 40 °C higher than that of the medium-temperature dry granules.

[0126] The chemical composition of the high-temperature dry granules, by mass percentage, includes: SiO2: 50%, Al2O3: 25%, B2O3: 5%, K2O: 2%, Li2O: 2%, CaO: 6%, BaO: 4%, ZnO: 3%, ZrO2: 3%;

[0127] The chemical composition of the medium-temperature dry granules, by mass percentage, includes: SiO2: 52%, Al2O3: 10%, Na2O: 10%, K2O: 4%, MgO: 9%, BaO: 6%, ZnO: 7%, SrO: 2%.

[0128] S5. Screen-print high-gloss glaze on the surface of the matte glaze layer, and dry it in a drying oven at a drying temperature of 120 °C for 20 seconds to obtain a high-gloss glaze layer with a thickness of 180 μm and a refractive index of 1.72. The raw materials for preparing the high-gloss glaze, by weight, include: 28 parts of potassium feldspar, 17 parts of quartz, 15 parts of kaolin, 16 parts of high-transparency frit, 4 parts of niobium pentoxide, 14 parts of dolomite, 1 part of zirconium silicate, 2 parts of perlite, and 2 parts of SiO₂-coated TiO₂ powder.

[0129] The chemical composition of the high-transparency frit, by mass percentage, includes: SiO₂: 60%, Al₂O₃: 15%, B₂O₃: 10%, Na₂O: 6%, K₂O: 4%, MgO: 2%, ZnO: 3%.

[0130] S6. Use a laser engraving machine to engrave a three-dimensional texture with a depth of 10 μm on the surface of the high-gloss glaze layer.

[0131] S7. Fire and form at a firing temperature of 1180 °C for 76 min to obtain the tile with the gradient gloss effect.

[0132] Comparative Example 9

[0133] A method for preparing a tile with a gradient gloss effect and three-dimensional texture includes the following steps:

[0134] S1. Press and form the green body powder, and after drying, obtain a green body layer. The raw materials for preparing the green body layer, by weight, include: 13 parts of kaolin, 12 parts of potassium-sodium feldspar powder, 8 parts of high-aluminum potassium sand, 11 parts of sodium feldspar powder, 10 parts of potassium sand, 16 parts of raw ore clay, 3 parts of black talc, 6 parts of polishing waste residue, 12 parts of washed sand, 8 parts of washed clay, and 1 part of sodium tripolyphosphate.

[0135] S2. Apply a base glaze on the surface of the green body layer, and dry it in a drying oven at a drying temperature of 80 °C for 30 seconds to obtain a base glaze layer.

[0136] S3. Inkjet print a texture on the surface of the base glaze layer to obtain a pattern layer.

[0137] S4. Screen-print high-gloss glaze on the surface of the pattern layer, and dry it in a drying oven at a drying temperature of 120 °C for 20 seconds to obtain a high-gloss glaze layer with a thickness of 180 μm and a refractive index of 1.72. The raw materials for preparing the high-gloss glaze, by weight, include: 28 parts of potassium feldspar, 17 parts of quartz, 15 parts of kaolin, 16 parts of high-transparency frit, 4 parts of niobium pentoxide, 14 parts of dolomite, 1 part of zirconium silicate, 2 parts of perlite, and 2 parts of SiO₂-coated TiO₂ powder.

[0138] The chemical composition of the high-transparent frit is expressed in percentage by mass and includes: SiO2: 60%, Al2O3: 15%, B2O3: 10%, Na2O: 6%, K2O: 4%, MgO: 2%, and ZnO: 3%.

[0139] S5. A laser etching machine is used to carve a three-dimensional texture with a depth of 10 μm on the surface of the high-gloss glaze layer.

[0140] S6, firing and forming, the firing temperature is 1180° C., and the firing time is 76 minutes, so as to obtain the ceramic tile with the gradient gloss effect.

[0141] Comparative Example 10

[0142] A method for preparing a tile with a gradient gloss effect and a three-dimensional texture comprises the following steps:

[0143] S1. Press the green body powder into shape, and after drying, obtain a green body layer; the raw materials for preparing the green body layer, in parts by weight, include: 13 parts of kaolin, 12 parts of potassium sodium stone powder, 8 parts of high-aluminum potassium sand, 11 parts of sodium stone powder, 10 parts of potassium sand, 16 parts of raw ore mud, 3 parts of black talc, 6 parts of polishing waste residue, 12 parts of washed sand, 8 parts of washed mud and 1 part of sodium tripolyphosphate.

[0144] S2, applying a bottom glaze on the surface of the body layer, and drying it in a drying oven at a drying temperature of 80° C. for 30 seconds to obtain a bottom glaze layer;

[0145] S3, inkjet printing a texture on the surface of the base glaze layer to obtain a pattern layer;

[0146] S4. Spray matte glaze on the surface of the pattern layer using a high-pressure spray glaze cabinet, dry it in a drying oven at a temperature of 150°C for 1 minute, and obtain a matte glaze layer with a thickness of 90 μm and a refractive index of 1.55; the raw materials for preparing the matte glaze, in parts by weight, include: 30 parts of high-temperature dry particles, 12 parts of medium-temperature dry particles, 6 parts of zirconium silicate, 25 parts of 9022A, 19 parts of calcium phosphate, and 8 parts of water. Among them, the sintering temperature of the high-temperature dry particles is 40°C higher than that of the medium-temperature dry particles.

[0147] The chemical composition of the high temperature dry particles, in terms of mass percentage, includes: SiO2: 50%, Al2O3: 25%, B2O3: 5%, K2O: 2%, Li2O: 2%, CaO: 6%, BaO: 4%, ZnO: 3%, ZrO2: 3%;

[0148] The chemical composition of the medium-temperature dry particles, in terms of mass percentage, includes: SiO2: 52%, Al2O3: 10%, Na2O: 10%, K2O: 4%, MgO: 9%, BaO: 6%, ZnO: 7%, and SrO: 2%.

[0149] S5. On the surface of the matte glaze layer, use a laser etching machine to engrave three-dimensional textures with a depth of 10 μm.

[0150] S6. Fire and form. The firing temperature is 1180 °C and the firing time is 76 min, thus obtaining the tile with the gradient gloss effect.

[0151] Perform performance tests on the tiles of Examples 1 to 3 and Comparative Examples 1 to 10. The test methods and standards are as follows:

[0152] 1. Abrasion resistance: Detect the abrasion resistance according to GB / T 3810.7-2016: Observe the wear condition of the brick surface after grinding at a specific number of grinding revolutions, which is divided into levels 0 to 5. Among them, visible wear after 100 revolutions is level 0, visible wear after 150 revolutions is level 1, visible wear after 600 revolutions is level 2, visible wear after 750 / 1500 revolutions is level 3, visible wear after 2100 / 6000 / 12000 revolutions is level 4, and greater than 12000 revolutions is level 5.

[0153] 2. Stain resistance: Detect the stain resistance with reference to the national standard GB / T 3810.14-2016: Conduct a stain resistance test on the brick surface treated with a surface treatment agent. The test principle is to make the pollutant agents (such as chrome green, iodine tincture, and olive oil) contact the front of the brick and act for a certain time, and then clean the brick surface according to the specified cleaning method, and observe the change of the brick surface to determine the stain resistance of the brick. The grades are divided into 1 to 5 levels, and level 5 has the best stain resistance performance.

[0154] 3. Glossiness: With reference to the GB / T4100-2015 standard, use a gloss meter to measure the glossiness of different positions on the brick surface, and the measurement angle is 60°.

[0155] 4. Surface texture three-dimensionality: Observe the brick surface at a distance of 0.5 m from the brick surface at an angle of 45° with the naked eye to check whether there is a three-dimensionality of height difference on the surface texture.

[0156] The test results of Examples 1 to 3 and Comparative Examples 1 to 10 are shown in Table 1.

[0157] Table 1

[0158]

[0159] As can be seen from Table 1, the glaze surfaces of the tiles in Examples 1 to 3 present a gradient gloss effect, with a wide gradient range of glossiness. The glossiness detected at an incident angle of 60° is 5 to 70 GU. As Figure 1 and Figure 2 shown, the three-dimensional texture of the glaze surface is combined with the gloss change, and the visual effect is more three-dimensional. Moreover, the physical properties of the glaze surface are good, the abrasion resistance can reach level 4, and the stain resistance can reach level 5.

[0160] The high-gloss glaze formula of Comparative Example 1 does not contain the nano-material SiO2-coated TiO2 powder, resulting in a decline in the physical properties of the glaze surface and a reduction in wear resistance to Grade 2.

[0161] The matte glaze formula of Comparative Example 2 does not include medium-temperature dry particles, leading to a high glaze surface temperature, porous surface, and a reduction in stain resistance to Grade 3.

[0162] The matte glaze formula of Comparative Example 3 does not include high-temperature dry particles, resulting in a low glaze surface temperature, a wear resistance of Grade 2 with a significant decline, and no obvious change in the light sense of the glaze surface.

[0163] In Comparative Examples 4 and 5, the high-gloss glaze layer is too thin or too thick, slightly weakening the glaze surface performance and reducing the light sense difference.

[0164] In Comparative Examples 6 and 7, the matte glaze layer is too thin or too thick, slightly weakening the glaze surface performance and reducing the light sense difference.

[0165] In Comparative Example 8, the matte glaze layer is applied first and then the high-gloss glaze layer, resulting in a reduction in the wear resistance of the glaze surface to Grade 2.

[0166] In Comparative Examples 9 and 10, no matte glaze layer or no high-gloss glaze layer is applied, without the superimposing effect of the two glaze layers, resulting in no light sense change on the glaze surface and poor surface three-dimensional sense.

[0167] The above are only the preferred embodiments of the present invention, and do not limit the patent scope of the present invention accordingly. Any equivalent structural transformation made using the content of the specification of the present invention under the inventive concept of the present invention, or any direct / indirect application in other related technical fields, is included in the patent protection scope of the present invention.

Claims

1. A method for preparing a tile with a gradient gloss effect and a three-dimensional texture, characterized in that: The following steps are involved: S1, pressing the green body powder into a shape, and after drying, obtaining a green body layer; S2, applying a base glaze on the surface of the green body layer to obtain a base glaze layer; S3, inkjet printing a texture on the surface of the base glaze layer to obtain a pattern layer; S4, screen printing a high-gloss glaze on the surface of the pattern layer to obtain a high-gloss glaze layer; S5, spraying matte glaze on the surface of the high-gloss glaze layer using a high-pressure glaze spray cabinet to obtain a matte glaze layer; S6, performing laser engraving on the surface of the matte glaze layer to obtain a three-dimensional texture; S7, firing and molding, that is, obtaining the ceramic tile with a gradient gloss effect and a three-dimensional texture; The raw materials for preparing the high gloss glaze in step S4 include, by weight: 28 to 40 parts of potassium feldspar, 17 to 25 parts of quartz, 8 to 15 parts of kaolin, 10 to 16 parts of high transparent frit, 2 to 4 parts of niobium pentoxide, 7 to 14 parts of dolomite, 1 to 4 parts of zirconium silicate, 1.5 to 4 parts of perlite and 2 to 4 parts of nanomaterials; The raw materials for preparing the matte glaze in step S5 include, by weight: 30-45 parts of high-temperature dry particles, 8-12 parts of medium-temperature dry particles, 6-15 parts of emulsifiers, 20-35 parts of suspending agents, 11-23 parts of auxiliary agents and 8-13 parts of water; The nano material is SiO2 coated TiO2 powder; The chemical composition of the highly transparent frit is expressed in mass percentage and includes: SiO2 60%~75%; Al2O35%~15%; B2O35%~10%; Na2O and / or K2O 10% to 20%; CaO and / or MgO 1% to 5%; ZnO 0%~5%; The chemical composition of the high-temperature dry particles, measured in mass percentage, includes: SiO250%~70%; Al2O310%~25%; B2O30%~8%; ZnO 0%~5%; ZrO20%~5%; Alkali metal oxides 2% to 10%; Alkaline earth metal oxides 5% to 15%; The chemical composition of the medium-temperature dry particles, measured in mass percentage, includes: SiO2 52%~66%; Al2O310%~12%; Na2O and / or K2O 5% to 15%; ZnO5%~7%; SrO2%~3%; Alkaline earth metal oxides 9% to 15.5%; The alkali metal oxide is at least one of Na2O, K2O and Li2O; the alkaline earth metal oxide is at least one of CaO, MgO and BaO; The opacifier includes one or both of zirconium silicate and calcium fluoride; The auxiliary agent includes one or both of calcium phosphate and tetragonal alumina.

2. The method for preparing a tile having a gradient gloss effect and a three-dimensional texture according to claim 1, characterized in that: The thickness of the high-gloss glaze layer is 180 to 360 μm, and the refractive index of the high-gloss glaze layer is 1.68 to 1.72; the thickness of the matte glaze layer is 90 to 180 μm, and the refractive index of the matte glaze layer is 1.45 to 1.

55.

3. The method for preparing a tile with a gradient gloss effect and a three-dimensional texture according to claim 1, characterized in that: In step S6, a three-dimensional texture with a depth of 10 to 50 μm is engraved on the surface of the matte glaze layer.

4. The method for preparing a tile with a gradient gloss effect and a three-dimensional texture according to claim 1, characterized in that: The raw materials for preparing the green body layer include, by weight, 10 to 15 parts of kaolin, 12 to 16 parts of sodium potassium stone powder, 6 to 11 parts of high-aluminum potassium sand, 10 to 13 parts of sodium stone powder, 9 to 14 parts of potassium sand, 14 to 19 parts of raw ore mud, 2 to 5 parts of black talc, 3 to 8 parts of polishing waste residue, 9 to 14 parts of washed sand, 5 to 9 parts of washed mud and 0.8 to 1.5 parts of additives.

5. The method for preparing a tile with a gradient gloss effect and a three-dimensional texture according to claim 1, characterized in that: In step S7, the firing temperature is 1180-1225° C., and the firing time is 55-76 minutes.

6. A tile with a gradient gloss effect and a three-dimensional texture, characterized in that: The product is prepared by the preparation method described in any one of claims 1 to 5.

Images