Glazed tile with mottled metallic three-dimensional texture and preparation process

Abstract

The application discloses a glazed tile with colorful metal stereoscopic texture and a preparation process thereof, and relates to the technical field of ceramic tiles. The A dry particle slurry with high silicon content and containing part of heavy metal salt is sprayed to obtain an A dry particle slurry spraying area, and a stereoscopic effect is formed in the spraying area. In a slightly acidic condition, the phosphate in B ink reacts with C protective glaze to generate iron phosphate phase separation, different degrees of saturation of simulated silver metal luster are formed according to the content of the generated iron phosphate, and the heavy metal salt in the A dry particle slurry forms new colors under high-temperature oxidation conditions. Part of the color areas and the simulated silver metal color are combined to form the colorful metal luster.

Description

Technical Field

[0001] This invention relates to the field of ceramic tile technology, and in particular to a glazed tile with a mottled metallic three-dimensional texture and its preparation process. Background Technology

[0002] Marble-look ceramic tiles in the industry mainly use scanned patterns of marble to imitate them. However, the imitation of surface effects such as concave and convex surfaces, sandblasted surfaces, flamed surfaces, and metallic surfaces is low. The concave and convex effects are not very realistic, and it is especially difficult to imitate the randomly distributed metallic texture of some high-end natural stones after polishing.

[0003] Current technologies typically employ powder pressing to create flat or molded blanks. To achieve a three-dimensional effect on the flat blank, dry granules or positioning adhesive granules are often used to create subtle textures. However, this usually only produces a three-dimensional effect without any additional metallic texture layering. Meanwhile, metallic ceramic tiles in the industry currently use conventional single-metal glazes. Single-metal glazes have relatively limited color options and lack a vibrant metallic texture effect. Summary of the Invention

[0004] The main objective of this invention is to propose a preparation process for glazed tiles with a colorful metallic three-dimensional texture, overcoming the technical problem that existing glazed tiles cannot simultaneously achieve a three-dimensional effect and a colorful metallic surface decoration effect. The secondary objective of this invention is to propose a glazed tile that is prepared using the aforementioned preparation process for a colorful metallic three-dimensional texture.

[0005] To achieve the above objectives, this invention proposes a preparation process for glazed tiles with a mottled metallic three-dimensional texture, comprising the following preparation steps:

[0006] S1. The blank is obtained by pressing;

[0007] S2. Spray A dry granule slurry to obtain the A dry granule slurry spraying area. The dry material composition of A dry granule slurry, by mass parts, includes: 50-60 parts of A dry granules and 1-3.5 parts of heavy metal salts. The raw material composition of A dry granules, by weight parts, includes: 60-76 parts of quartz powder, 10-17 parts of wollastonite, 5-8 parts of calcined kaolin, 3-5 parts of limestone, 3-7 parts of alumina powder and 4-10 parts of zirconium silicate. The above raw materials are melted at high temperature, cooled, crushed and then screened to obtain A dry granules.

[0008] S3. Apply ink B to obtain a functional ink layer. The raw material composition of ink B, by weight, includes: 8-18 parts of phosphate, 1-5.5 parts of dispersant and 70-80 parts of solvent. After mixing the above raw materials evenly, adjust the pH to 6-7 to obtain ink B.

[0009] S4. Apply C protective glaze to the outermost layer. The raw materials of C protective glaze, by weight, include: 15-25 parts of soluble trivalent iron salt, 7-12 parts of potassium feldspar, 8-13 parts of sodium feldspar, 1-2 parts of calcined alumina powder, 7-10 parts of calcined kaolin, 10-17 parts of calcined talc powder, 4-8 parts of calcined zinc oxide, 5-8 parts of barium carbonate, and 5-12 parts of quartz powder. Ball mill, mix, and sieve the above raw materials to obtain C protective glaze.

[0010] S5. Glazed tiles are obtained after firing.

[0011] Specifically, the pressed blank can be a planar blank or a mold blank. Even when applied to a planar blank, this invention can achieve a three-dimensional tactile effect.

[0012] Specifically, the soluble ferric salts are one or more of ferric chloride, ferric sulfate, ferric bromide, ferric iodide, or ferric nitrate, and will not be listed exhaustively here. Those skilled in the art can select the soluble ferric salt with the best performance by considering factors such as cost, metallic luster, and the generation of impurities.

[0013] Preferably, the preparation steps also include a polishing process. The metallic luster in this solution is easily removed by conventional polishing processes to maintain the surface decorative effect. For example, the polishing process can use a 240-mesh abrasive brush for light sweeping polishing to avoid cutting away the metallic luster. Those skilled in the art should understand that a shallow or gentle polishing process suitable for the preparation process of this invention can be obtained through limited experimentation to avoid cutting away the metallic luster effect on the surface.

[0014] Preferably, after step S1, a surface decoration step is also included, in which a decorative pattern layer is obtained on the blank or the area where the A dry granule paste is sprayed or on the functional ink layer by known printing methods such as inkjet penetration process, inkjet printing, roller printing, screen printing, etc.

[0015] This invention achieves the sprayed area of ​​dry granule slurry A by spraying it. Dry granule A has a semi-emulsified effect, with a high silicon content in its main raw materials and high viscosity at high temperatures, creating a three-dimensional effect in the sprayed area. Under slightly acidic conditions, the phosphates in ink B react with protective glaze C to generate iron phosphate phase separation. Depending on the different amounts of iron phosphate produced, different saturations of imitation silver metallic luster are formed. Simultaneously, the heavy metal salts in dry granule A form new metallic colors under high-temperature oxidation conditions. Some colored areas overlap and combine with the imitation silver metallic colors, creating a colorful metallic luster.

[0016] Preferably, the particle size distribution of the powder in dry granules A is as follows:

[0017] ≥20 mesh 63~70%,

[0018] 20 mesh-40 mesh (<20 mesh, ≥40 mesh) 15-20%,

[0019] 40 mesh-60 mesh (<40 mesh, ≥60 mesh) 15-20%.

[0020] Powder with a mesh size smaller than 60 is not used because fine powder cannot effectively form a three-dimensional effect after sintering. The composition of A dry granule raw material, combined with this particle size distribution, forms a more significant three-dimensional effect in the A dry granule slurry spraying area.

[0021] Further preferred, the highest firing temperature in the firing process is 1170-1225℃.

[0022] This maximum firing temperature range allows A dry particles to be fired well in the system.

[0023] Further preferably, the nozzle diameter for spraying the A dry granule slurry is 1.5mm-2.3mm, and the raw material for the C protective glaze is ball-milled and sieved to a fineness of 0.5-1.0% residue on a 325-mesh sieve to obtain the C protective glaze. This nozzle size prevents the A dry granules from clogging the nozzle during spraying.

[0024] Preferably, the soluble ferric salt is composed of 5-10 parts ferric chloride and 10-15 parts ferric bromide by mass.

[0025] Preferably, the heavy metal salt contains at least one of copper, zinc, iron, nickel, manganese and cobalt; the phosphate contains at least one of sodium phosphate Na3PO4 and calcium phosphate Ca3(PO4)2.

[0026] Preferably, ink B further comprises, by weight, 2-10 parts of a pH adjuster and 0.5-1.5 parts of a defoamer. For demonstration purposes, but not limited to, the pH adjuster is DeuAdd MA-95 aqueous pH adjuster; the dispersant is ammonium polyacrylate; the solvent is diethylene glycol butyl ether; and the defoamer is a fatty acid polymer. Those skilled in the art can confirm through limited experimentation that other pH adjusters, defoamers, dispersants, and solvents are applicable to this invention, and it may also contain other additives that do not affect the surface decoration effect of this invention.

[0027] Preferably, the functional ink layer occupies 35-50% of the surface area of ​​the green body, and the A dry granule slurry spraying area occupies 50-70% of the surface area of ​​the green body. More preferably, the functional ink layer and the A dry granule slurry spraying area do not completely overlap.

[0028] By controlling the area ratio between the functional ink layer and the A dry granule slurry spraying area, after the overall C protective glaze is sprayed, the overlapping part of the functional ink layer and the A dry granule slurry spraying area presents a colorful metallic luster decorative effect, while the non-overlapping part of the functional ink layer and the A dry granule slurry spraying area presents a silver-like metallic luster.

[0029] Preferably, in step S2, the specific gravity of the dry granule slurry A is 1.55-1.65 g / ml, and the glazing amount is 500-650 g / m².

[0030] In step S3, the grayscale value of ink B is 10-100%, and the ink volume of ink B is 150-200 grams per square meter.

[0031] In step S4, the amount of C protective glaze applied is 600-800 g / m², and the specific gravity is 1.55-1.60 g / ml.

[0032] By controlling the specific gravity and glaze application amount of dry granules A, the grayscale value and ink volume of ink B, and the glaze application amount and specific gravity of protective glaze C, the reaction between the metal salts in dry granules A and ink B and protective glaze C is effectively ensured. Grayscale uses black tones to represent objects, with each grayscale object having a brightness value from 0% (white) to 100% (black). By setting different printing grayscale values, the phosphate content in ink B is controlled. After fully reacting with protective glaze C to form iron phosphate, different shades of metallic luster can be achieved.

[0033] This invention also proposes a glazed tile, characterized in that it is prepared by the glazed tile preparation process with a mottled metallic three-dimensional texture according to any of the above-mentioned schemes. Therefore, it possesses all the corresponding beneficial effects of the aforementioned schemes, which will not be elaborated upon here.

[0034] Compared with existing technologies, this invention provides a preparation process for glazed tiles with a colorful metallic three-dimensional texture. The process involves spraying an A dry granule slurry with a high silicon content and containing some heavy metal salts to create an A dry granule slurry spraying area. The sprayed area forms a three-dimensional effect. Under slightly acidic conditions, B ink reacts with C protective glaze to generate iron phosphate phase separation. Depending on the different iron phosphate content produced by the reaction, different saturations of imitation silver metallic luster are formed. At the same time, the heavy metal salts in the A dry granule slurry form new colors under high-temperature oxidation conditions. Some colored areas overlap and combine with the imitation silver metallic luster to form a colorful metallic luster. Attached Figure Description

[0035] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0036] Figure 1 This is a schematic diagram of the glaze effect of the glazed tile with a colorful metallic three-dimensional texture in this invention.

[0037] The realization of the purpose, functional features and advantages of this application will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0038] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. In addition, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed by the present invention.

[0039] To address the technical problem that existing metallic glazes offer limited color expression and cannot create a three-dimensional, textured effect, this application provides a preparation process for glazed tiles with a vibrant, three-dimensional metallic texture, comprising the following preparation steps:

[0040] S1. The blank is obtained by pressing;

[0041] S2. Spray A dry granule slurry to obtain the A dry granule slurry spraying area. The dry material composition of A dry granule slurry, by mass parts, includes: 50-60 parts of A dry granules and 1-3.5 parts of heavy metal salts. The raw material composition of A dry granules, by weight parts, includes: 60-76 parts of quartz powder, 10-17 parts of wollastonite, 5-8 parts of calcined kaolin, 3-5 parts of limestone, 3-7 parts of alumina powder and 4-10 parts of zirconium silicate. The above raw materials are melted at high temperature, cooled, crushed and then screened to obtain A dry granules.

[0042] S3. Apply ink B to obtain a functional ink layer. The raw material composition of ink B, by weight, includes: 8-18 parts of phosphate, 1-5.5 parts of dispersant and 70-80 parts of solvent. After mixing the above raw materials evenly, adjust the pH to 6-7 to obtain ink B.

[0043] S4. Apply C protective glaze to the outermost layer. The raw materials of C protective glaze, by weight, include: 15-25 parts of soluble trivalent iron salt, 7-12 parts of potassium feldspar, 8-13 parts of sodium feldspar, 1-2 parts of calcined alumina powder, 7-10 parts of calcined kaolin, 10-17 parts of calcined talc powder, 4-8 parts of calcined zinc oxide, 5-8 parts of barium carbonate, and 5-12 parts of quartz powder. Ball mill, mix, and sieve the above raw materials to obtain C protective glaze.

[0044] S5. Glazed tiles are obtained after firing.

[0045] In some specific embodiments, the pressed blank is a planar blank or a mold blank. Even when applied to a planar blank, this application can achieve a three-dimensional tactile effect.

[0046] In some specific embodiments, the preparation steps also include a polishing process. The metallic luster in this application is easily removed by conventional polishing processes to maintain the surface decorative effect. In one specific embodiment, the polishing process can use a 240-mesh abrasive brush for light sweeping polishing to avoid cutting away the metallic luster. Those skilled in the art should understand that a shallow or gentle polishing process suitable for the preparation process of this invention can be obtained through limited experimentation to avoid cutting away the metallic luster effect on the surface.

[0047] In some preferred embodiments, after step S1, a surface decoration step is also included, in which a decorative pattern layer is obtained on the blank or the area where the A dry granule paste is sprayed or on the functional ink layer by known printing methods such as inkjet penetration process, inkjet printing, roller printing, screen printing, etc.

[0048] In some specific embodiments, the slurry composition of the A dry granule slurry, by weight percentage, includes: 50-60 parts of A dry granules, 1-3.5 parts of heavy metal salts, and 40-50 parts of suspension. The suspension consists of 2.5-3.5 parts of sodium carboxymethyl cellulose and 100 parts of water. The two are thoroughly mixed and stirred evenly, and the residue is 0% after passing through a 325-mesh sieve.

[0049] In some specific embodiments, the soluble ferric salt is composed of 5-10 parts ferric chloride and 10-15 parts ferric bromide by mass.

[0050] In some preferred embodiments, the particle size distribution of the powder in dry granules A is as follows:

[0051] ≥20 mesh 63~70%,

[0052] 20 mesh-40 mesh (<20 mesh, ≥40 mesh) 15-20%,

[0053] 40 mesh-60 mesh (<40 mesh, ≥60 mesh) 15-20%.

[0054] Powder with a mesh size smaller than 60 is not used because fine powder cannot effectively form a three-dimensional effect after sintering. The composition of dry granules A, combined with this particle size distribution, further enhances the three-dimensional effect of the sprayed area.

[0055] Further preferred, the highest firing temperature in the firing process is 1170-1225℃.

[0056] This maximum firing temperature range allows A dry granules to be fired well in the system.

[0057] Further preferably, the nozzle diameter of the spraying dry granule slurry A is 1.5mm-2.3mm. With this nozzle size, the clogging of the nozzle by the dry granule A can be prevented when spraying dry granule A.

[0058] In some preferred embodiments, the heavy metal salt contains at least one of copper, zinc, iron, nickel, manganese, and cobalt; the phosphate contains at least one of sodium phosphate (Na3PO4) and calcium phosphate (Ca3(PO4)2).

[0059] In some preferred embodiments, ink B further comprises, by weight, 2 to 10 parts of pH adjuster and 0.5 to 1.5 parts of defoamer.

[0060] In some specific embodiments, the pH adjuster is DeuAdd MA-95 aqueous acid-base pH adjuster; the dispersant is ammonium polyacrylate; the solvent is diethylene glycol butyl ether solvent; and the defoamer is a fatty acid polymer substance.

[0061] In some preferred embodiments, the functional ink layer occupies 35-50% of the surface area of ​​the green body, the A dry granule slurry spraying area occupies 50-70% of the surface area of ​​the green body, and the functional ink layer and the A dry granule slurry spraying area do not completely overlap.

[0062] In some preferred embodiments, in step S2, the specific gravity of A dry granule slurry is 1.55-1.65 g / ml, and the glazing amount is 500-650 g / m².

[0063] In step S3, the grayscale value of ink B is 10-100%, and the ink volume of ink B is 150-200 grams per square meter.

[0064] In step S4, the amount of C protective glaze applied is 600-800 g / m², and the specific gravity is 1.55-1.60 g / ml.

[0065] This application also proposes a glazed tile, which is prepared by the glazed tile preparation process with a colorful metallic three-dimensional texture in any of the above embodiments.

[0066] The technical solution of the present invention will be further described in detail below with reference to specific embodiments. It should be understood that the following embodiments are only used to explain the present invention and are not intended to limit the present invention.

[0067] Example 1-1

[0068] A glazed tile is provided, comprising the following preparation steps:

[0069] S1. The mold blank is obtained by pressing. Here is a specific composition of the blank as an example: the raw material composition of the blank, by mass parts, includes: 12.5 parts raw ore, 3.7 parts bentonite, 9.6 parts kaolin, 11.1 parts washed mud, 29.5 parts stone powder, 29.3 parts potassium sand, 4 parts talc, and 0.3 parts blank reinforcing agent. The above raw materials are ball-milled, mixed, sieved, and pressed to obtain the mold blank.

[0070] S2. Spray A dry granule slurry to obtain the A dry granule slurry spraying area.

[0071] In this embodiment, a slurry composition of A dry granule slurry is provided, which, by mass parts, includes: 59.5 parts of A dry granules, 3.5 parts of heavy metal salt, and 38 parts of suspension. The raw material composition of the suspension, by mass parts, includes: 3 parts of sodium carboxymethyl cellulose and 100 parts of water. The suspension is obtained by uniformly mixing the raw materials and passing it through a 325-mesh sieve with 0% residue.

[0072] The raw material composition of A dry granules, by weight, includes: 66 parts quartz powder, 13 parts wollastonite, 6 parts calcined kaolin, 4 parts limestone, 5 parts alumina powder, and 6 parts zirconium silicate. The above raw materials are melted at high temperature, cooled, crushed, and then screened to obtain A dry granules.

[0073] The particle size distribution of the powder in dry granules A is as follows: ≥20 mesh 39%, 20-40 mesh (<20 mesh, ≥40 mesh) 20%, 40-60 mesh (<40 mesh, ≥60 mesh) 23%, <60 mesh 18%.

[0074] S3. Apply ink B to obtain a functional ink layer. Specifically, in this embodiment, ink B and ordinary ink are used, and a decorative pattern layer incorporating the functional ink layer is obtained by screen printing. In the embodiments or comparative examples, the ordinary inks mentioned are CIK-NE6118 ink produced by Foshan Yidajia Precision Ceramics Technology Co., Ltd., E3566 ink produced by Foshan Sanshui Kanglitai Inorganic Synthetic Materials Co., Ltd., and NGY-62016 and NGY-62012 inks produced by Foshan NGY Yangtze Pigment Co., Ltd.

[0075] The raw material composition of ink B, by weight, includes: 18 parts phosphate, 1 part dispersant, 76 parts solvent, and 5 parts pH adjuster. After the above raw materials are mixed evenly, the pH is adjusted to 6-7 to obtain ink B.

[0076] The heavy metal salt is copper chloride, the phosphate is Na3PO4, the dispersant is ammonium polyacrylate, the solvent is diethylene glycol butyl ether, and the pH adjuster is DeuAdd MA-95 aqueous acid-base pH adjuster.

[0077] S4. Apply C protective glaze to the outermost layer. The raw materials of C protective glaze, by weight, include: 15 parts soluble iron salt, 12 parts potassium feldspar, 13 parts sodium feldspar, 1 part calcined alumina powder, 10 parts calcined kaolin, 17 parts calcined talc powder, 8 parts calcined zinc oxide, 5 parts barium carbonate, and 12 parts quartz powder. Ball mill, mix, and sieve the above raw materials to obtain C protective glaze.

[0078] The soluble iron salt consists of 15 parts of ferric chloride. The raw materials for the C protective glaze are ball-milled and sieved until the fineness is 0.5% on a 325-mesh sieve, thus obtaining the C protective glaze.

[0079] S5. Glazed tiles are obtained after firing.

[0080] The highest firing temperature in the firing process is 1170℃.

[0081] In this embodiment, the functional ink layer occupies 40% of the surface area of ​​the green body, and the A dry granule slurry spraying area occupies 40% of the surface area of ​​the green body. The functional ink layer and the A dry granule slurry spraying area completely overlap.

[0082] In step S2, the specific gravity of A dry granule slurry is 1.40 g / ml, and the glaze application amount is 450 g / m²; in step S3, the gray value of B ink is 10-100%, and the ink amount of B ink is 100 g / m²; in step S4, the glaze application amount of C protective glaze is 500 g / m², and the specific gravity is 1.50 g / ml.

[0083] Examples 1-2

[0084] A glazed tile is provided, comprising the following preparation steps:

[0085] S1. A flat blank is obtained by pressing;

[0086] The raw materials used are as described in Example 1-1; the raw materials are ball-milled, mixed, sieved, and pressed to obtain a planar blank.

[0087] S2. Spray A dry granule slurry to obtain the A dry granule slurry spraying area. In this embodiment, a slurry composition of A dry granule slurry is provided, which includes, by mass parts: 50 parts of A dry granules, 1 part of heavy metal salt and 49 parts of suspension. The raw material composition and preparation method of the suspension are as described in Example 1-1.

[0088] The raw material composition of A dry granules, by weight, includes: 60 parts quartz powder, 17 parts wollastonite, 5 parts calcined kaolin, 5 parts limestone, 3 parts alumina powder, and 10 parts zirconium silicate. The above raw materials are melted at high temperature, cooled, crushed, and then screened to obtain A dry granules.

[0089] The particle size distribution of the powder in dry granules A is: ≥20 mesh 70%, 20-40 mesh (<20 mesh, ≥40 mesh) 15%, 40-60 mesh (<40 mesh, ≥60 mesh) 15%.

[0090] S3. Apply ink B to obtain a functional ink layer. Specifically, in this embodiment, ink B and ordinary ink are loaded into different channels and sprayed by inkjet printing to obtain a decorative pattern layer that incorporates the functional ink layer.

[0091] The raw material composition of ink B, by weight, includes: 8 parts phosphate, 5.5 parts dispersant, 1.5 parts defoamer, 80 parts solvent, and 5 parts pH adjuster. After mixing the above raw materials evenly, the pH is adjusted to 6-7 to obtain ink B.

[0092] The heavy metal salts are nickel sulfate and manganese sulfate, the phosphates are Na3PO4 and Ca3(PO4)2 in a 1:1 (weight ratio), the dispersant is ammonium polyacrylate, the solvent is diethylene glycol butyl ether, and the pH adjuster is DeuAdd MA-95 aqueous acid-base pH adjuster.

[0093] S4. Apply C protective glaze to the outermost layer. The raw materials of C protective glaze, by weight, include: 25 parts soluble iron salt, 8 parts potassium feldspar, 13 parts sodium feldspar, 2 parts calcined alumina powder, 10 parts calcined kaolin, 17 parts calcined talc powder, 8 parts calcined zinc oxide, 7 parts barium carbonate, and 10 parts quartz powder. Ball mill, mix, and sieve the above raw materials to obtain C protective glaze.

[0094] The soluble iron salt consists of 15 parts ferric chloride and 10 parts ferric bromide. The raw materials for the C protective glaze are ball-milled and sieved until the fineness is 0.5% on a 325-mesh sieve, thus obtaining the C protective glaze.

[0095] S5. Glazed tiles are obtained through firing and polishing processes.

[0096] In the firing process, the highest firing temperature is 1200℃, and the polishing process involves lightly sweeping with a 240-mesh grinding brush.

[0097] In this embodiment, the functional ink layer occupies 50% of the surface area of ​​the green body, and the A dry granule slurry spraying area occupies 50% of the surface area of ​​the green body. The functional ink layer and the A dry granule slurry spraying area do not completely overlap.

[0098] In step S2, the specific gravity of A dry granule slurry is 1.55 g / ml, and the glaze application amount is 500 g / m²; in step S3, the gray value of B ink is 10-100%, and the ink amount of B ink is 150 g / m²; in step S4, the glaze application amount of C protective glaze is 600 g / m², and the specific gravity is 1.55 g / ml.

[0099] Examples 1-3

[0100] A glazed tile is provided, comprising the following preparation steps:

[0101] S1. A flat blank is obtained by pressing;

[0102] The raw materials used are as described in Example 1-1; the raw materials are ball-milled, mixed, sieved, and pressed to obtain a planar blank.

[0103] S2. Spray A dry granule slurry to obtain the A dry granule slurry spraying area.

[0104] In this embodiment, a slurry composition of A dry granule slurry is provided, which, by mass parts, includes: 51.5 parts of A dry granules, 3.5 parts of heavy metal salts, and 45 parts of suspension. The raw material composition and preparation method of the suspension are as described in Example 1-1.

[0105] The raw material composition of A dry granules, by weight, includes: 70 parts quartz powder, 10 parts wollastonite, 7 parts calcined kaolin, 3 parts limestone, 6 parts alumina powder, and 4 parts zirconium silicate. The above raw materials are melted at high temperature, cooled, crushed, and then screened to obtain A dry granules.

[0106] The particle size distribution of the powder in dry granules A is as follows: ≥20 mesh 63%, 20-40 mesh (<20 mesh, ≥40 mesh) 17%, 40-60 mesh (<40 mesh, ≥60 mesh) 20%.

[0107] S3. Apply ink B to obtain a functional ink layer. Specifically, in this embodiment, ink B and ordinary ink are loaded into different channels and sprayed by inkjet printing to obtain a decorative pattern layer that incorporates the functional ink layer.

[0108] The raw material composition of ink B, by weight, includes: 15 parts phosphate, 4.5 parts dispersant, 0.5 parts defoamer, 70 parts solvent, and 10 parts pH adjuster.

[0109] After mixing the above raw materials evenly, adjust the pH to 6-7 to obtain ink B.

[0110] The heavy metal salts are nickel sulfate, manganese sulfate and cobalt chloride, the phosphate is Ca3(PO4)2, the dispersant is ammonium polyacrylate, the solvent is diethylene glycol butyl ether, and the pH adjuster is DeuAdd MA-95 aqueous acid-base pH adjuster.

[0111] S4. Apply C protective glaze to the outermost layer. The raw materials of C protective glaze, by weight, include: 25 parts soluble iron salt, 11 parts potassium feldspar, 11 parts sodium feldspar, 1.5 parts calcined alumina powder, 8 parts calcined kaolin, 16 parts calcined talc powder, 7.5 parts calcined zinc oxide, 7 parts barium carbonate, and 6 parts quartz powder. Ball mill, mix, and sieve the above raw materials to obtain C protective glaze.

[0112] The soluble iron salt consists of 10 parts ferric chloride and 15 parts ferric bromide. The raw materials for the C protective glaze are ball-milled and sieved until the fineness is 1.0% residue on a 325-mesh sieve, thus obtaining the C protective glaze.

[0113] S5. Glazed tiles are obtained through firing and polishing processes.

[0114] The highest firing temperature in the firing process is 1225℃. The polishing process involves lightly brushing with a 240-mesh abrasive brush.

[0115] In this embodiment, the functional ink layer occupies 35% of the surface area of ​​the green body, and the A dry granule slurry spraying area occupies 70% of the surface area of ​​the green body. The functional ink layer and the A dry granule slurry spraying area do not completely overlap.

[0116] In step S2, the specific gravity of A dry granule slurry is 1.65 g / ml, and the glaze application amount is 650 g / m²; in step S3, the gray value of B ink is 10-100%, and the ink amount of B ink is 200 g / m²; in step S4, the glaze application amount of C protective glaze is 800 g / m², and the specific gravity is 1.60 g / ml.

[0117] Random samples were taken from the overlapping areas of the glazed tiles prepared in the above embodiments to test the color development, gloss, and unevenness. The results are as follows:

[0118]

[0119]

[0120] Note: In glazed tiles, C is the outermost protective glaze. The ABC overlapping area refers to the area where the functional ink layer overlaps with the A dry granule slurry spraying area. The AC overlapping area refers to the area where the A dry granule slurry spraying area does not overlap with the functional ink layer. The BC overlapping area refers to the area where the functional ink layer does not overlap with the A dry granule slurry spraying area. Randomly select 3 sampling areas with an area of ​​2mm*2mm from each overlapping area.

[0121] As can be seen from the above data, in Example 1-1, due to the non-optimal range of particle size of A dry granule powder, grayness of B ink, ink volume, glaze application amount and specific gravity of A dry granule paste and C protective glaze, the reaction was not sufficient. The color tone generated in the ABC overlapping area was lighter, and its three-dimensional effect was generally inferior to that of Examples 1-2 and 1-3. Furthermore, since the functional ink layer completely overlapped with the A dry granule paste spraying area, it did not produce the different decorative effects of the AC or BC overlapping areas as in Examples 1-2 and 1-3. However, since Example 1-1 was within the optimal raw material composition ratio range of A dry granule paste, B ink and C protective glaze in this scheme, it still formed a colorful metallic luster in the ABC overlapping area. Among them, Example 1-2 is the best embodiment, with the most prominent three-dimensional effect, colorful and deep and elegant tone, and the luster of the three different overlapping areas is layered and not abrupt, with the most comfortable overall light feeling.

[0122] Comparative Example 1

[0123] The difference from Examples 1-2 is that after pressing the flat body in step S1, a conventional metal glaze is applied to the surface of the body. In this comparative example, the DS08500 metal glaze produced by Guangdong Daoshi Technology Co., Ltd. is used, and the metal glaze tile of the prior art is obtained by firing.

[0124] Comparative Example 2

[0125] The difference from Examples 1-2 is that only ordinary ink is used in step S3. (The ink does not contain phosphoric acid.)

[0126] Comparative Example 3

[0127] The difference from Examples 1-2 is that the raw material composition of A dry granule slurry in step S2 does not contain heavy metal salts.

[0128] Random samples were taken from the overlapping areas of the glazed tiles prepared in the above comparative examples to test their color development, gloss, and unevenness. The results were compared with those of Examples 1-2, and the data are as follows:

[0129]

[0130]

[0131] Comparing the effects of the conventional metallic glaze in Comparative Example 1 with those in Examples 1-2, it can be seen that the conventional metallic glaze has a single metallic color and no three-dimensional effect; Comparative Example 2 uses ordinary ink instead of ink B, which cannot react with dry granule slurry A or protective glaze C, so it does not form a colorful metallic luster, and the color in the randomly sampled area is single; In Comparative Example 3, the raw material composition of dry granule slurry A does not contain heavy metal salts, and the ceramic tile produced only has a single metallic luster generated by the reaction of the functional ink layer and protective glaze C, which also cannot form a colorful metallic luster effect.

[0132] The above description is merely a preferred embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made using the contents of the present invention under the inventive concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.

Claims

1. A preparation process for glazed tiles with a mottled metallic three-dimensional texture, characterized in that, The preparation steps include the following: S1. The blank is obtained by pressing; S2. Spray A dry granule slurry to obtain the A dry granule slurry spraying area. The dry material composition of the A dry granule slurry, by weight, includes: 50-60 parts of A dry granules and 1-3.5 parts of heavy metal salts. The raw material composition of the A dry granules, by weight, includes: 60-76 parts of quartz powder, 10-17 parts of wollastonite, 5-8 parts of calcined kaolin, 3-5 parts of limestone, 3-7 parts of alumina powder and 4-10 parts of zirconium silicate. The above raw materials are melted at high temperature, cooled, crushed and then screened to obtain the A dry granules. S3. Apply ink B to obtain a functional ink layer. The raw material composition of ink B, by weight, includes: 8-18 parts of phosphate, 1-5.5 parts of dispersant and 70-80 parts of solvent. After mixing the above raw materials evenly, adjust the pH to 6-7 to obtain ink B. S4. Apply C protective glaze to the outermost layer. The raw materials of the C protective glaze, by weight, include: 15-25 parts of soluble trivalent iron salt, 7-12 parts of potassium feldspar, 8-13 parts of sodium feldspar, 1-2 parts of calcined alumina powder, 7-10 parts of calcined kaolin, 10-17 parts of calcined talc powder, 4-8 parts of calcined zinc oxide, 5-8 parts of barium carbonate, and 5-12 parts of quartz powder. Ball mill, mix, and sieve the above raw materials to obtain the C protective glaze. S5. Glazed tiles are obtained after firing.

2. The preparation process of glazed tiles with a mottled metallic three-dimensional texture as described in claim 1, characterized in that, Following step S1, a surface decoration step is also included, in which a decorative pattern layer is obtained on the blank or the A dry granule spraying area or the functional ink layer by a known printing method.

3. The preparation process of glazed tiles with a mottled metallic three-dimensional texture as described in claim 1, characterized in that, The particle size distribution of the powder in the A dry granules is as follows: ≥20 mesh 63~70%, 20 mesh-40 mesh (<20 mesh, ≥40 mesh) 15-20%, 40 mesh-60 mesh (<40 mesh, ≥60 mesh) 15-20%.

4. The preparation process of glazed tiles with a mottled metallic three-dimensional texture as described in claim 1, characterized in that, In the firing process, the highest firing temperature is 1170-1225℃.

5. The preparation process of glazed tiles with a mottled metallic three-dimensional texture as described in claim 1, characterized in that, The nozzle diameter for spraying the dry granules A is 1.5mm-2.3mm.

6. The preparation process of glazed tiles with a mottled metallic three-dimensional texture as described in claim 1, characterized in that, The heavy metal salt contains at least one of copper, zinc, iron, nickel, manganese, and cobalt; the phosphate contains at least one of sodium phosphate (Na3PO4) and calcium phosphate (Ca3(PO4)2).

7. The preparation process of glazed tiles with a mottled metallic three-dimensional texture as described in claim 1, characterized in that, The composition of ink B further includes 2-10 parts by weight of pH adjuster and 0.5-1.5 parts by weight of defoamer. The pH adjuster is DeuAdd MA-95 water-based acid-base pH adjuster; the dispersant is ammonium polyacrylate; the solvent is diethylene glycol butyl ether; and the defoamer is a fatty acid polymer.

8. The preparation process of glazed tiles with a mottled metallic three-dimensional texture as described in claim 1, characterized in that, The functional ink layer occupies 35-50% of the surface area of ​​the green body, and the A dry granule slurry spraying area occupies 50-70% of the surface area of ​​the green body. The functional ink layer and the A dry granule slurry spraying area do not completely overlap.

9. The preparation process of glazed tiles with a mottled metallic three-dimensional texture as described in claim 1, characterized in that, In step S2, the specific gravity of the A dry granule slurry is 1.55-1.65 g / ml, and the glaze application amount is 500-650 g / m²; in step S3, the gray value of the B ink is 10-100%, and the ink amount of the B ink is 150-200 g / m²; in step S4, the glaze application amount of the C protective glaze is 600-800 g / m², and the specific gravity is 1.55-1.60 g / ml.

10. A glazed tile, characterized in that, The glazed tile with a three-dimensional metallic texture as described in any one of claims 1 to 9 is prepared.

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