An environment-friendly simple and elegant ceramic tile with oracle bone patterns and a preparation method thereof

Abstract

The application discloses a kind of environment-friendly simple and elegant ceramic tiles of oracle bone script patterns and a preparation method thereof, and belongs to the technical field of ceramic tile production.The application uses superfine matte dry particle powder as effect glaze layer.The application is inspired by the fact that cracks are generated in mud field due to drainage shrinkage caused by drought.By adjusting the glaze formula, the surface glaze layer generates "oracle bone script pattern" glaze cracks during the drying process.By increasing the high-temperature viscosity of the effect glaze layer, the glaze layer is prevented from melting and fusing the cracks in the glaze layer at high temperature.Due to the superfine matte dry particle, which is pre-fused and then crushed, the adhesion between particles is small, and the superfine powder has a small particle size, so it is easier to form cracks during the drying process.In addition, after high-temperature firing, the glaze surface of the superfine matte dry particle is further enhanced in terms of stain resistance and texture performance.Meanwhile, various design crack textures can be formed by using fine carving and digital functional ink, and the design textures and "oracle bone script pattern" cracks complement each other.

Description

Technical Field

[0001] This invention belongs to the field of ceramic tile production technology, specifically relating to an environmentally friendly, elegant ceramic tile with an oracle bone pattern and its preparation method. Background Technology

[0002] With a younger consumer base, people's demands for tile decoration are becoming increasingly personalized and diverse. Traditional flat tiles, due to their relatively monotonous visual effects and tactile feel, can no longer meet consumer needs. Developing and manufacturing visually striking tile products that catch the eye of consumers has become the goal of contemporary researchers.

[0003] Currently, ceramic tile products with three-dimensional decorative effects on the market are mainly formed through pressing with molds and digital functional ink engraving. Patent application number CN201810771219.X, entitled "A three-dimensional high-simulation ceramic tile with matte glaze and its preparation method," uses digital press molds to prepare the blank. However, this process has shortcomings such as limited texture and misalignment between patterns and textures. Furthermore, it suffers from long mold conversion and installation times and high production costs. Patent application number CN201910641835.8, entitled "A method for manufacturing ceramic thin plates with concave-convex mold effects on flat blanks," utilizes the corrosive effect of low-temperature functional ink on the glaze layer, creating a downward concave effect at the ink location. However, due to the damaging effect of the low-temperature functional ink on the glaze layer, the glaze surface is prone to dirt accumulation and difficult to clean. Patent application number CN202110047404.6, entitled "A method for preparing a matte, deeply sculpted ceramic tile and the ceramic tile itself," utilizes the principle of water-repellent glaze expulsion using digital mold ink, while simultaneously employing high-pressure spraying to further enhance the repulsion effect, thus creating a textured surface. While the resulting texture exhibits natural layers, it lacks detailed detail. Summary of the Invention

[0004] To address the shortcomings of existing technologies, the purpose of this invention is to provide an environmentally friendly, elegant ceramic tile with an oracle bone pattern and its preparation method. Inspired by the cracking caused by the shrinkage of muddy fields due to drought drainage, this invention adjusts the glaze formula to allow the surface glaze layer to drain during the drying process, resulting in "oracle bone" pattern-like glaze cracks. At the same time, by increasing the high-temperature viscosity of the effect glaze layer, it prevents the glaze layer from melting and fusing cracks at high temperatures.

[0005] The key to this invention is resolving the contradiction between the high-temperature viscosity and surface texture of the effect glaze. This invention uses ultrafine matte dry powder as the effect glaze layer. Because the ultrafine matte dry powder has undergone pre-melting and subsequent crushing, the particles have low inter-particle adhesion, and the ultrafine powder fineness makes it easier to form cracks during the drying process. Furthermore, after high-temperature firing, the anti-fouling and texture properties of the glaze are further enhanced. Simultaneously, various designed crack textures can be created using fine-carving and digital inks, complementing the "oracle bone" crack pattern.

[0006] To solve the above problems, the present invention is achieved through the following technical solution:

[0007] The first objective of this invention is:

[0008] A method for preparing an environmentally friendly, elegant ceramic tile with an oracle bone pattern is provided, comprising the following preparation steps:

[0009] S1. Prepare a blank and apply a base glaze to the blank to obtain brick body A;

[0010] S2. Maintain the temperature of the brick body A at 35-45°C, print digital engraving ink and design patterns to obtain brick body B;

[0011] The digital engraving ink is a glossy engraving ceramic ink;

[0012] The aforementioned glossy engraved ceramic ink is a mixture of fine engraving ink and glossy ink;

[0013] S3. Apply an ultrafine matte dry-granule glaze with a specific gravity of 1.2–1.4 g / cm³ to the brick body B. 3 Glazing amount is 300-500g / m² 2 Then it enters the glaze drying line to obtain brick body C;

[0014] S4. The brick C is fired at high temperature to obtain brick D with an elegant effect of oracle bone pattern;

[0015] S5. The brick body D is brushed, polished, and edged to obtain an environmentally friendly, elegant ceramic brick with a oracle bone pattern.

[0016] The base glaze includes the following preparation steps:

[0017] Composition of the base glaze: includes the following raw materials by weight percentage:

[0018] Potassium feldspar 45-60%, color-producing frit 6-10%, kaolin 5-10%, quartz 5-12%, alumina 8%-12%, zirconium silicate 6-10%, wollastonite 2-5%, the sum of all components is 100%;

[0019] The color-developing frit comprises the following raw materials by weight percentage:

[0020] Potassium feldspar 30-40%, sodium feldspar 20-35%, barium carbonate 8-15%, strontium carbonate 7-12%, zinc oxide 5%-8%, quartz 6-10%, wollastonite 2-5%, the sum of all components is 100%;

[0021] Preparation of the base glaze:

[0022] Select the appropriate proportion of raw materials according to the base glaze formula, add an appropriate amount of water, and ball mill them into a glaze slurry with a sieve residue of 0.1% to 0.2% and a water content of 28% to 32%. After the ball milling is qualified, the slurry is discharged, and after sieving, iron removal, homogenization and aging, the base glaze is obtained.

[0023] The ultrafine matte dry granule glaze comprises the following preparation steps:

[0024] Preparation of ultrafine matte dry granules:

[0025] Composition of ultrafine matte dry granules: includes the following raw materials by weight percentage:

[0026] Potassium feldspar 48-55%, alumina 8-15%, kaolin 3-5%, barium carbonate 7-10%, dolomite 8-12%, zinc oxide 5-8%, wollastonite 10-15%, the sum of all components is 100%;

[0027] Preparation of ultrafine matte dry granules:

[0028] Select the appropriate proportion of component raw materials according to the ultrafine matte dry granule formula, mix them evenly, put them into a frit furnace and melt them at a high temperature of 1700℃, and obtain frit after quenching; then crush the frit and control the particle size to 325-500 mesh to obtain ultrafine matte dry granules.

[0029] Preparation of ultrafine matte dry granule glaze:

[0030] The ultrafine matte dry granules are mixed evenly with the glue suspending agent, and the weight percentage of the ultrafine matte dry granules added is 25% to 50% to obtain ultrafine matte dry granule glaze.

[0031] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0032] The chemical composition of the base glaze by weight percentage is as follows:

[0033] Al₂O₃ 15–23%, SiO₂ 62–66%, Fe₂O₃ 0.1–0.6%, K₂O 3.5–4.6%, CaO 0.1–0.8%, MgO 0.1–1.1%, Na₂O 1.2–1.8%, TiO₂ 0–0.1%, ZrO₂ 5–8%, loss on ignition 0–0.8%, and the sum of all components is 100%.

[0034] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0035] The weight percentage chemical composition of the ultrafine matte dry granules is as follows:

[0036] The composition is as follows: SiO2 48-53%, Al2O3 18-25%, Fe2O3 0.1-3%, CaO 6-12%, MgO 1.5-2.3%, K2O 4.3-5.6%, Na2O 1.8-2.6%, TiO2 0-0.3%, BaO 4-6%, ZnO 5-6.2%, loss on ignition 0.2-0.6%, and the sum of all components is 100%.

[0037] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0038] The weight percentage chemical composition of the color-developing frit is as follows:

[0039] Al₂O₃ 8–13%, SiO₂ 55–64%, Fe₂O₃ 0.1–0.5%, K₂O 3.5–4.6%, CaO 0.1–0.8%, MgO 0.1–1.1%, Na₂O 3.2–3.8%, TiO₂ 0–0.1%, BaO 5–8%, SrO 5–8%, ZnO 5–8%, loss on ignition 0–0.8%, and the sum of all components is 100%.

[0040] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0041] The adhesive suspending agent is a viscous, dry granule-specific suspending agent prepared by mixing one or more of methyl ethylene glycol, sodium carboxymethyl cellulose, and polymethylsiloxane with one or more of sodium metaphosphate, sodium dodecylbenzene sulfonate, and dodecyltrimethylammonium bromide in water.

[0042] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0043] The adhesive suspending agent has the following weight composition:

[0044] 100 parts water, 5-10 parts methyl ethylene glycol, 1-2 parts sodium carboxymethyl cellulose, 0.5-1 part polymethylsiloxane, and 0.3-0.8 parts sodium dodecylbenzene sulfonate.

[0045] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0046] The prepared body includes the following steps:

[0047] Select conventional raw materials, add an appropriate amount of water, and ball mill them into a slurry with a particle size of 240-260 mesh. After iron removal, sieving, spray drying, and then pressing and molding, the green body is obtained after drying.

[0048] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0049] The drying temperature of the blank is 180-220℃, and the drying time is 65-80 minutes.

[0050] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0051] The specific gravity of the base glaze is 1.89–1.95 g / cm³. 3 The glaze application rate is 500-600 g / m². 2 .

[0052] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0053] The calcination temperature for high-temperature firing in step S4 is 1160–1190°C, and the calcination time is 60–70 min.

[0054] The preparation method of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention is further optimized as follows:

[0055] The ink volume of the digital engraving ink is 20-100 g / m³. 2 .

[0056] The second objective of this invention is:

[0057] An environmentally friendly, elegant ceramic tile with an oracle bone pattern is provided, which is prepared by the aforementioned method for preparing such an environmentally friendly, elegant ceramic tile with an oracle bone pattern.

[0058] Compared with the prior art, the present invention has at least the following beneficial effects:

[0059] This invention avoids the shortcomings of existing preparation processes by utilizing the glaze cracking that occurs during the drying and drainage of an ultrafine matte dry granule glaze layer. Simultaneously, by increasing the high-temperature viscosity of the ultrafine matte dry granule glaze layer, it prevents the glaze layer from melting and fusing together at high temperatures, thus preventing cracking. Compared to conventional glazes, the ultrafine matte dry granules are pre-melted, resulting in poorer interparticle adhesion. The ultrafine powder fineness makes it prone to cracking during the drying and drainage stage, forming "oracle bone" pattern cracks. Furthermore, functional inks such as those for engraving and digital printing can be used to create designed cracks that complement the "oracle bone" pattern cracks.

[0060] This invention effectively resolves the contradiction between a delicate glaze texture and high-temperature viscosity by employing ultra-fine matte dry granules. Unlike ordinary flat matte glazes and recessed line textures, to ensure that the "oracle bone pattern" cracks do not fuse, the base glaze must first have a high melting temperature to support the formed pattern texture. If the base glaze melting temperature is too low, it will melt at high temperatures, causing the surface cracks to sink into the base glaze layer. Similarly, the surface effect glaze layer also has high requirements. To perfectly showcase the texture details and glaze texture, the effect glaze layer requires a suitable melting temperature and high-temperature viscosity. High melting temperature and high viscosity result in a rough glaze surface and poor stain resistance. Conversely, low melting temperature and low high-temperature viscosity make the formed "oracle bone pattern" texture easily filled in, resulting in a poor three-dimensional effect.

[0061] In summary, the key to this invention is balancing the conflict between the desired glaze finish and the crackle effect. Ordinary effect glazes struggle to achieve both a delicate texture and clear lines. Therefore, this invention creatively employs ultrafine high-temperature matte dry granules to achieve this.

[0062] (I) Preparation of the base glaze:

[0063] In the preparation of glazed tiles, to avoid the influence of the body color on the product appearance, a common decorative process is to first apply a base glaze to the body surface, then inkjet print the design, and finally apply a top glaze. The main function of the base glaze is to cover the body color and enhance the color of the inkjet ink. Generally, the base glaze and effect glaze are used together, and their expansion coefficients must be compatible with those of the body and the effect glaze. Furthermore, to ensure that the dry-granule glaze maintains a good crack pattern and does not sink into the base glaze at high temperatures, the base glaze also requires a high melting temperature. Therefore, this invention optimizes the base glaze as follows:

[0064] 1. Increase the alumina content in the base glaze formula:

[0065] Increasing the alumina content in the base glaze formulation can significantly improve the glaze's initial melting temperature and final melting temperature. Alumina (Al2O3), as an intermediate in network formation, increases the hardness of the base glaze at high temperatures, thus supporting and maintaining the sculpted three-dimensional texture. Furthermore, increasing the initial melting temperature of the base glaze facilitates the smooth escape of gases before the glaze melts, reducing the formation of defects such as pinholes and bubbles.

[0066] Typically, Al2O3 in glaze formulations is introduced in the form of potassium feldspar, sodium feldspar, kaolin, and industrial alumina powder. However, the Al2O3 content in potassium and sodium feldspar is usually relatively low. Therefore, increasing the alumina content by introducing potassium and sodium feldspar would significantly increase the content of alkali metals such as potassium and sodium, lowering the melting temperature of the base glaze formulation. This would cause the effect glaze on the surface of the glaze layer to sink into the base glaze layer, resulting in an overly smooth glaze surface that lacks three-dimensionality. Increasing the alumina content by using kaolin would cause problems such as high glaze viscosity and thixotropy. Therefore, this invention increases the alumina content by adding industrial alumina micropowder. Experimental results show that when the amount of alumina micropowder added is between 8% and 12%, the melting temperature, high-temperature viscosity, color development performance, and other properties of the base glaze reach their optimal levels.

[0067] 2. Use potassium feldspar to increase the melting temperature of the base glaze:

[0068] Potassium feldspar is an alkali metal aluminosilicate and the most common feldspar in the feldspar group, serving as a primary flux. Potassium feldspar melts and decomposes at approximately 1130–1450℃ and has a relatively high viscosity. Since potassium feldspar ore is often associated with sodium feldspar, it contains varying amounts of sodium. Na₂O has a stronger fluxing effect than K₂O. Due to its superior fluxing effect, the fired glaze has good transparency, which can easily allow the base color of the body to show through, affecting the stability of the glaze color. Secondly, its narrow firing range is detrimental to production stability. Furthermore, Na₂O increases the coefficient of thermal expansion of the glaze, reducing its chemical and thermal stability. Through extensive experimentation, this invention has shown that the optimal glaze performance is achieved when the potassium feldspar content is between 45% and 60%.

[0069] 3. Introduce a color-developing frit to improve color development performance:

[0070] Because the base glaze formula contained excessive alumina, its color development was poor. To improve the color development performance of the base glaze, a color-developing frit was introduced into the formula. The addition of the color-developing frit effectively improved the color development performance of the top glaze, making the patterns and colors of the product more vibrant and colorful. Through extensive testing, this invention found that the optimal performance of the glaze was achieved when the amount of color-developing frit added was between 6% and 10%.

[0071] In addition, to enhance the hiding power of the glaze, zirconium silicate was added to the base glaze formula to enhance its opacifying effect. However, since zirconium silicate is radioactive, the less added, the better. Research in this invention shows that adding 6-10% results in better hiding power and is more environmentally friendly and human-friendly.

[0072] (II) Preparation of ultrafine dry granules:

[0073] To perfectly showcase the texture details and glaze finish, the effect glaze layer requires a suitable melting temperature and high-temperature viscosity. A high melting temperature and high viscosity result in a rough glaze surface and poor stain resistance; conversely, a low melting temperature and low high-temperature viscosity make the resulting "oracle bone texture" easily filled in, resulting in a poor three-dimensional effect.

[0074] In summary, the key to this invention lies in balancing the conflict between the surface effect and crackle effect of dry-granule glaze. Ordinary effect glazes struggle to achieve both a delicate texture and clear patterns. Therefore, this invention focuses on dry-granule glaze as a breakthrough point. Because the ultra-fine matte dry granules used in this invention are pre-melted, their anti-fouling properties are guaranteed to a certain extent. Simultaneously, to obtain a delicate glaze texture, the dry granules are crushed to a fineness of 325 mesh or higher.

[0075] This invention mainly adjusts and optimizes the dry granule formulation composition in the following aspects:

[0076] 1. Increase the K2O content in the dry granule formulation:

[0077] Potassium feldspar and sodium feldspar are both commonly used low-temperature fluxes in ceramic production. Compared with sodium feldspar, potassium feldspar has a higher initial melting point, which is beneficial for the expulsion of gas from the green body. In addition, potassium feldspar has a wider firing range than sodium feldspar. It begins to decompose and melt at a melting point of about 1130 to 1450℃. After melting, its high-temperature viscosity is also relatively high, which can prevent the low viscosity from melting and smoothing out crack textures.

[0078] 2. Increase the calcium oxide content in the dry granule formulation:

[0079] Calcium oxide (CaO) primarily functions as a flux in glazes, reducing their high-temperature viscosity and enhancing their chemical stability. Simultaneously, at high temperatures, the reaction of CaO with Al and Si to form microcrystals such as anorthite and wollastonite strengthens the glaze's hardness and corrosion resistance. These microcrystals also reduce the glaze's gloss. In the ultrafine matte dry granule formulation of this invention, CaO is mainly introduced through dolomite and wollastonite.

[0080] 3. Increase the alumina content in the dry pellet formulation:

[0081] Similarly, to improve the high-temperature viscosity of the dry granules, this invention introduces alumina micropowder into the formulation. Alumina (Al2O3), as an intermediate in forming the network, increases the Al2O3 content in the formulation, thereby increasing the viscosity of the dry granules at high temperatures and ensuring that the engraved texture pattern is not melted flat. Experimental results of this invention show that when the amount of alumina micropowder added is between 8% and 15%, the melting temperature, high-temperature viscosity, color development properties, and other properties of the dry granules are optimal.

[0082] 4. Introduce appropriate amounts of zinc oxide and barium carbonate:

[0083] Zinc oxide (ZnO) is a fluxing agent with significant fluxing and color-enhancing effects, especially for red glazes. Furthermore, zinc oxide can reduce the coefficient of thermal expansion of the glaze, prevent cracking, increase glaze elasticity, and broaden the firing temperature range of the glaze. However, due to its high price, it is only added at 5-8% in the formula of this invention for better color enhancement. Barium carbonate is a good fluxing agent in glazes, and unlike calcium carbonate and talc, it has a wider fluxing range. Simultaneously, barium carbonate helps in the color development of inkjet inks. When the amount of barium carbonate added to the formula reaches a certain range, barium feldspar crystals precipitate on the glaze surface, reducing the gloss and making the light more soft. Compared to high-temperature matte glazes, crystalline matte glazes have a more delicate and smooth feel.

[0084] 5. Optimal particle size selection for ultrafine matte dry granules:

[0085] To ensure the sculpted texture effect of the glaze, a higher proportion of alumina is added to the ultra-fine matte dry granule formula to maintain the high-temperature viscosity of the granules. To ensure a delicate glaze texture, the dry granules are crushed to a fineness of 325-500 mesh. Furthermore, because the ultra-fine matte dry granules undergo high-temperature calcination, their interparticle adhesion is poor. During the drying process, the dry granule layer cracks due to drainage, forming fine crack textures. These fine textures are random and natural, difficult to create with digital inks, and the crack textures are fine and subtle, possessing a unique decorative effect. Compared to the crackle glaze of ancient porcelain, its glaze layer is stable and does not exhibit later-stage glaze chipping.

[0086] Table 1. Effect of different dry particle fineness on glaze finish

[0087]

[0088] 6. Preparation of dry granular glaze slurry

[0089] Because ultrafine matte dry granules are pre-melted, their suspension effect is poor and they are prone to sedimentation. To solve the sedimentation problem of ultrafine matte dry granules, this invention uses an adhesive suspending agent to formulate a dry granule glaze slurry with ultrafine matte dry granules.

[0090] The adhesive suspending agent is a viscous dry particle suspending agent prepared by mixing one or more of methyl ethylene glycol, sodium carboxymethyl cellulose, and polymethylsiloxane with one or more of sodium metaphosphate, sodium dodecylbenzene sulfonate, and dodecyltrimethylammonium bromide and dissolving them in water. It can completely suspend and disperse ceramic dry particles in the suspending agent, and improve the overall suspension fluidity while ensuring the suspension and dispersion performance.

[0091] Table 2 shows the effect of the amount of ultrafine matte dry particles added on the glaze effect:

[0092] Table 2. Effect of the amount of ultrafine matte dry granules added on the glaze effect (weight percentage %)

[0093]

[0094] In summary, the preferred addition amount of ultrafine matte dry granules is 25% to 50%. Attached Figure Description

[0095] Figure 1 This is a flowchart illustrating the preparation process of the oracle bone pattern environmentally friendly and elegant ceramic tile of the present invention.

[0096] Figure 2 This is an overall rendering of the oracle bone pattern environmentally friendly and elegant ceramic tile product of the present invention.

[0097] Figure 3 This is a magnified view of a portion of the oracle bone pattern environmentally friendly and elegant ceramic tile product of the present invention. Detailed Implementation

[0098] To make the application, technical solution, and advantages of this invention clearer, the invention is described in detail with reference to specific embodiments. It should be understood that the embodiments are for illustrative purposes only and are not intended to limit the scope of protection of this invention. Any simple improvements to the preparation method of this invention based on the inventive concept fall within the scope of protection of this invention.

[0099] Example 1

[0100] A method for preparing an environmentally friendly, elegant ceramic tile with an oracle bone pattern, comprising the following preparation steps:

[0101] S1. Prepare the green body, dry the green body at 180℃ for 65 minutes, and apply a base glaze to the green body with a specific gravity of 1.89 g / cm³. 3 Glazing amount is 600g / m 2 We obtain brick A;

[0102] S2. Maintain the temperature of the brick body A at 42°C, print digital engraving ink and design patterns to obtain brick body B;

[0103] The digital engraving ink is a glossy engraving ceramic ink;

[0104] The aforementioned glossy engraved ceramic ink is a mixture of fine engraving ink and glossy ink;

[0105] The ink volume of the digital engraving ink is 40g / m³. 2 ;

[0106] S3. Apply an ultrafine matte dry granule glaze with a specific gravity of 1.28 g / cm³ to the brick body B. 3 Glazing amount is 420g / m 2 Then it enters the glaze drying line to obtain brick body C;

[0107] S4. The brick C is fired at a high temperature of 1170℃ for 65 minutes to obtain a brick D with an elegant effect of oracle bone pattern.

[0108] S5. The brick body D is brushed, polished, and edged to obtain an environmentally friendly, elegant ceramic brick with a oracle bone pattern.

[0109] The base glaze includes the following preparation steps:

[0110] Composition of the base glaze: includes the following raw materials by weight percentage:

[0111] Potassium feldspar 55%, color-forming frit 8%, kaolin 8%, quartz 8%, alumina 10%, zirconium silicate 7%, wollastonite 4%;

[0112] The color-developing frit comprises the following raw materials by weight percentage:

[0113] Potassium feldspar 35%, sodium feldspar 24%, barium carbonate 12%, strontium carbonate 10%, zinc oxide 7%, quartz 8%, wollastonite 4%, the sum of all components is 100%;

[0114] Preparation of the base glaze:

[0115] Select the appropriate proportion of raw materials according to the base glaze formula, add an appropriate amount of water, and ball mill them into a glaze slurry with a sieve residue of 0.3% to 0.5% and a water content of 28% to 32%. After the ball milling is qualified, the slurry is discharged, and after sieving, iron removal, homogenization and aging, the base glaze is obtained.

[0116] The ultrafine matte dry granule glaze comprises the following preparation steps:

[0117] Preparation of ultrafine matte dry granules:

[0118] Composition of ultrafine matte dry granules: includes the following raw materials by weight percentage:

[0119] Potassium feldspar 50%, alumina 10%, kaolin 3%, barium carbonate 9%, dolomite 10%, zinc oxide 6%, wollastonite 12%;

[0120] Preparation of ultrafine matte dry granules:

[0121] Select the appropriate proportion of component raw materials according to the ultrafine matte dry granule formula, mix them evenly, put them into a frit furnace and melt them at a high temperature of 1700℃, and obtain frit after quenching; then crush the frit and control the particle size to 325-500 mesh to obtain ultrafine matte dry granules.

[0122] Preparation of ultrafine matte dry granule glaze:

[0123] The ultrafine matte dry granules are mixed evenly with the glue suspending agent, and the weight percentage of the ultrafine matte dry granules added is 35%, to obtain the ultrafine matte dry granule glaze.

[0124] The adhesive suspending agent has the following weight composition:

[0125] 100 parts water, 8 parts methyl ethylene glycol, 1 part sodium carboxymethyl cellulose, 0.6 parts polymethylsiloxane, and 0.4 parts sodium dodecylbenzene sulfonate.

[0126] The prepared body includes the following steps:

[0127] Select conventional raw materials, add an appropriate amount of water, and ball mill them into a slurry with a particle size of 240-260 mesh. After iron removal, sieving, spray drying, and then pressing and molding, the green body is obtained after drying.

[0128] Example 2

[0129] A method for preparing an environmentally friendly, elegant ceramic tile with an oracle bone pattern, comprising the following preparation steps:

[0130] S1. Prepare the green body, dry the green body at 180℃ for 65 minutes, and apply a base glaze to the green body with a specific gravity of 1.89 g / cm³. 3 Glazing amount is 600g / m 2 We obtain brick A;

[0131] S2. Maintain the temperature of the brick body A at 42°C, print digital engraving ink and design patterns to obtain brick body B;

[0132] The digital engraving ink is a glossy engraving ceramic ink;

[0133] The aforementioned glossy engraved ceramic ink is a mixture of fine engraving ink and glossy ink;

[0134] The ink volume of the digital engraving ink is 100g / m³. 2 .

[0135] S3. Apply an ultra-fine matte dry-granule glaze with a specific gravity of 1.40 g / cm³ to the brick body B. 3 Glazing amount is 500g / m 2 Then it enters the glaze drying line to obtain brick body C;

[0136] S4. The brick C is fired at a high temperature of 1183℃ for 70 minutes to obtain a brick D with an elegant effect of oracle bone pattern.

[0137] S5. The brick body D is brushed, polished, and edged to obtain an environmentally friendly, elegant ceramic brick with a oracle bone pattern.

[0138] The base glaze includes the following preparation steps:

[0139] Composition of the base glaze: includes the following raw materials by weight percentage:

[0140] Potassium feldspar 46%, color-forming frit 10%, kaolin 8%, quartz 12%, alumina 12%, zirconium silicate 8%, wollastonite 4%;

[0141] The color-developing frit comprises the following raw materials by weight percentage:

[0142] Potassium feldspar 35%, sodium feldspar 24%, barium carbonate 12%, strontium carbonate 10%, zinc oxide 7%, quartz 8%, wollastonite 4%, the sum of all components is 100%;

[0143] Preparation of the base glaze:

[0144] Select the appropriate proportion of raw materials according to the base glaze formula, add an appropriate amount of water, and ball mill them into a glaze slurry with a sieve residue of 0.1% to 0.2% and a water content of 28% to 32%. After the ball milling is qualified, the slurry is discharged, and after sieving, iron removal, homogenization and aging, the base glaze is obtained.

[0145] The ultrafine matte dry granule glaze comprises the following preparation steps:

[0146] Preparation of ultrafine matte dry granules:

[0147] Composition of ultrafine matte dry granules: includes the following raw materials by weight percentage:

[0148] Potassium feldspar 50%, alumina 10%, kaolin 3%, barium carbonate 9%, dolomite 10%, zinc oxide 6%, wollastonite 12%;

[0149] Preparation of ultrafine matte dry granules:

[0150] Select the appropriate proportion of component raw materials according to the ultrafine matte dry granule formula, mix them evenly, put them into a frit furnace and melt them at a high temperature of 1700℃, and obtain frit after quenching; then crush the frit and control the particle size to 325-500 mesh to obtain ultrafine matte dry granules.

[0151] Preparation of ultrafine matte dry granule glaze:

[0152] The ultrafine matte dry granules are mixed evenly with the glue suspending agent, and the weight percentage of the ultrafine matte dry granules added is 40%, to obtain the ultrafine matte dry granule glaze.

[0153] The adhesive suspending agent has the following weight composition:

[0154] 100 parts water, 8 parts methyl ethylene glycol, 1 part sodium carboxymethyl cellulose, 0.6 parts polymethylsiloxane, and 0.4 parts sodium dodecylbenzene sulfonate.

[0155] The prepared body includes the following steps:

[0156] Select conventional raw materials, add an appropriate amount of water, and ball mill them into a slurry with a particle size of 240-260 mesh. After iron removal, sieving, spray drying, and then pressing and molding, the green body is obtained after drying.

[0157] Comparative Example 1

[0158] The difference between Comparative Example 1 and Example 1 is that a low-temperature base glaze is used instead of the base glaze (high-temperature base glaze) in Example 1.

[0159] Composition of low-temperature base glaze: includes the following raw materials by weight percentage:

[0160] Potassium feldspar 65%, color-forming frit 8%, kaolin 6%, quartz 8%, alumina 2%, zirconium silicate 7%, wollastonite 4%.

[0161] Comparative Example 2

[0162] The difference between Comparative Example 2 and Example 1 is that ordinary low-temperature dry granules replace the ultrafine matte dry granules in Example 1; ordinary low-temperature dry granules have a low melting temperature and low viscosity.

[0163] Composition of ordinary low-temperature matte dry granules: includes the following raw materials by weight percentage:

[0164] Potassium feldspar 56%, alumina 2%, kaolin 3%, barium carbonate 9%, dolomite 10%, zinc oxide 8%, wollastonite 12%.

[0165] Table 3 Comparison of glaze effects between the examples and the comparative examples

[0166] project Base glaze dry grains Glazed effect Example 1 high temperature base glaze Ultrafine matte dry granules The glaze is delicate, with cracks resembling oracle bone patterns. Example 2 high temperature base glaze Ultrafine matte dry granules The glaze is delicate, with cracks resembling oracle bone patterns. Comparative Example 1 Low temperature base glaze Ultrafine matte dry granules The glaze is delicate, and the cracks in the oracle bone pattern are not obvious. Comparative Example 2 high temperature base glaze Ordinary low-temperature matte dry granules The glaze is relatively smooth, with no cracks resembling oracle bone patterns.

[0167] For a detailed rendering of the environmentally friendly, elegant ceramic tile with oracle bone pattern prepared in Example 1, please refer to the image below. Figure 2 and Figure 3 .

[0168] As shown in Table 3, the formulations and preparation methods of Examples 1 and 2 can produce environmentally friendly, elegant ceramic tiles with a fine glaze and oracle bone-patterned crackles. However, the comparative examples could not produce products with the same effect as the examples.

[0169] Inspired by the cracking caused by drainage shrinkage in muddy fields during drought, this invention creates "oracle bone" pattern glaze cracks during the drying process of the surface dry granule layer. Simultaneously, by increasing the high-temperature viscosity of the glaze layer, it prevents the glaze layer from melting and fusing together at high temperatures. While the comparative example also forms "oracle bone" pattern glaze cracks during drying, the cracks melt and flatten during high-temperature firing because the melting temperature of the base glaze or surface dry granules is too low, resulting in low high-temperature viscosity. Furthermore, this invention resolves the contradiction between high-temperature drying and glaze texture (the higher the temperature of the dry granules, the rougher the glaze surface) by using ultrafine matte dry granules.

[0170] In summary, the above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any changes, modifications, and evolutions made by those skilled in the art without departing from the scope of the present invention based on the disclosed technical content shall be considered equivalent embodiments of the present invention. Furthermore, any changes, modifications, and evolutions made to the above embodiments based on the essential technology of the present invention shall still fall within the protection scope of the present invention.

[0171] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0172] Experimental methods not specified in this invention are generally performed under conventional conditions or as recommended by the manufacturer.

[0173] Unless otherwise stated, the various optimized technical solutions in this invention can be combined with each other.

[0174] Unless otherwise stated, percentages and parts are weight percentages and weight parts.

[0175] Experimental methods not specified in the instructions and examples are generally performed under standard conditions or as recommended by the manufacturer.

[0176] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as are familiar to those skilled in the art. Furthermore, any methods and materials similar to or equivalent to those described herein may be used in the methods of this invention.

Claims

1. A method for preparing an environmentally friendly, elegant ceramic tile with an oracle bone pattern, characterized in that: It includes the following preparation steps: S1. Prepare a blank and apply a base glaze to the blank to obtain brick body A; S2. Maintain the temperature of the brick body A at 35-45°C, print digital engraving ink and design patterns to obtain brick body B; The digital engraving ink is a glossy engraving ceramic ink; The aforementioned glossy engraved ceramic ink is a mixture of fine engraving ink and glossy ink; S3. Apply an ultrafine matte dry-granule glaze with a specific gravity of 1.2–1.4 g / cm³ to the brick body B. 3 Glazing amount is 300-500g / m² 2 Then it enters the glaze drying line to obtain brick body C; S4. The brick C is fired at high temperature to obtain brick D with an elegant effect of oracle bone pattern; S5. The brick body D is brushed, polished, and edged to obtain an environmentally friendly, elegant ceramic brick with a oracle bone pattern. The base glaze includes the following preparation steps: Composition of the base glaze: includes the following raw materials by weight percentage: Potassium feldspar 45-60%, color-producing frit 6-10%, kaolin 5-10%, quartz 5-12%, alumina 8%-12%, zirconium silicate 6-10%, wollastonite 2-5%, the sum of all components is 100%; The color-developing frit comprises the following raw materials by weight percentage: Potassium feldspar 30-40%, sodium feldspar 20-35%, barium carbonate 8-15%, strontium carbonate 7-12%, zinc oxide 5%-8%, quartz 6-10%, wollastonite 2-5%, the sum of all components is 100%; Preparation of the base glaze: Select the appropriate proportion of raw materials according to the base glaze formula, add an appropriate amount of water, and ball mill them into a glaze slurry with a sieve residue of 0.1% to 0.2% and a water content of 28% to 32%. After the ball milling is qualified, the slurry is discharged, and after sieving, iron removal, homogenization and aging, the base glaze is obtained. The ultrafine matte dry granule glaze comprises the following preparation steps: Preparation of ultrafine matte dry granules: Composition of ultrafine matte dry granules: includes the following raw materials by weight percentage: Potassium feldspar 48-55%, alumina 8-15%, kaolin 3-5%, barium carbonate 7-10%, dolomite 8-12%, zinc oxide 5-8%, wollastonite 10-15%, the sum of all components is 100%; Preparation of ultrafine matte dry granules: Select the appropriate proportion of component raw materials according to the ultrafine matte dry granule formula, mix them evenly, put them into a frit furnace and melt them at a high temperature of 1700℃, and obtain frit after quenching; then crush the frit and control the particle size to 325-500 mesh to obtain ultrafine matte dry granules. Preparation of ultrafine matte dry granule glaze: The ultrafine matte dry granules are mixed evenly with the glue suspending agent, and the weight percentage of the ultrafine matte dry granules added is 25% to 50% to obtain ultrafine matte dry granule glaze.

2. The method for preparing the oracle bone pattern environmentally friendly and elegant ceramic tile according to claim 1, characterized in that: It includes one or a combination of the following technical features: The chemical composition of the base glaze by weight percentage is as follows: Al2O3 15-23%, SiO2 62-66%, Fe2O3 0.1-0.6%, K2O 3.5-4.6%, CaO 0.1-0.8%, MgO 0.1-1.1%, Na2O 1.2-1.8%, TiO2 0-0.1%, ZrO2 5-8%, loss on ignition 0-0.8%, the sum of all components is 100%; The weight percentage chemical composition of the ultrafine matte dry granules is as follows: SiO2 48-53%, Al2O3 18-25%, Fe2O3 0.1-3%, CaO 6-12%, MgO 1.5-2.3%, K2O 4.3-5.6%, Na2O 1.8-2.6%, TiO2 0-0.3%, BaO 4-6%, ZnO 5-6.2%, loss on ignition 0.2-0.6%, the sum of all components is 100%; The weight percentage chemical composition of the color-developing frit is as follows: Al₂O₃ 8–13%, SiO₂ 55–64%, Fe₂O₃ 0.1–0.5%, K₂O 3.5–4.6%, CaO 0.1–0.8%, MgO 0.1–1.1%, Na₂O 3.2–3.8%, TiO₂ 0–0.1%, BaO 5–8%, SrO 5–8%, ZnO 5–8%, loss on ignition 0–0.8%, and the sum of all components is 100%.

3. The method for preparing the environmentally friendly, elegant ceramic tile with oracle bone pattern according to claim 1, characterized in that: The adhesive suspending agent is a viscous, dry granule-specific suspending agent prepared by mixing one or more of methyl ethylene glycol, sodium carboxymethyl cellulose, and polymethylsiloxane with one or more of sodium metaphosphate, sodium dodecylbenzene sulfonate, and dodecyltrimethylammonium bromide in water.

4. The method for preparing the oracle bone pattern environmentally friendly and elegant ceramic tile according to claim 3, characterized in that: The adhesive suspending agent has the following weight composition: 100 parts water, 5-10 parts methyl ethylene glycol, 1-2 parts sodium carboxymethyl cellulose, 0.5-1 part polymethylsiloxane, and 0.3-0.8 parts sodium dodecylbenzene sulfonate.

5. The method for preparing the oracle bone pattern environmentally friendly and elegant ceramic tile according to claim 1, characterized in that: The prepared body includes the following steps: Select conventional raw materials, add an appropriate amount of water, and ball mill them into a slurry with a particle size of 240-260 mesh. After iron removal, sieving, spray drying, and then pressing and molding, the green body is obtained after drying.

6. The method for preparing the oracle bone pattern environmentally friendly and elegant ceramic tile according to claim 5, characterized in that: The drying temperature of the blank is 180-220℃, and the drying time is 65-80 minutes.

7. The method for preparing the oracle bone pattern environmentally friendly and elegant ceramic tile according to claim 1, characterized in that: The specific gravity of the base glaze is 1.89–1.95 g / cm³. 3 The glaze application rate is 500-600 g / m². 2 .

8. The method for preparing the oracle bone pattern environmentally friendly and elegant ceramic tile according to claim 1, characterized in that: The calcination temperature for high-temperature firing in step S4 is 1160–1190°C, and the calcination time is 60–70 min.

9. The method for preparing the oracle bone pattern environmentally friendly and elegant ceramic tile according to claim 1, characterized in that: The ink volume of the digital engraving ink is 20-100 g / m³. 2 .

10. An environmentally friendly, elegant ceramic tile with an oracle bone pattern, characterized in that: It is prepared by the method of preparing oracle bone pattern environmentally friendly and elegant ceramic tiles according to any one of claims 1 to 9.

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