Ice needle dry granule, ceramic tile with ice needle effect and preparation method thereof

Abstract

The present application belongs to the field of building ceramics, and particularly relates to an ice needle dry particle, a ceramic tile with ice needle effect and a preparation method thereof. Mineral composition of the ice needle dry particle comprises, in weight parts, 20-35 parts of sodium feldspar, 6-12 parts of kaolin, 8-12 parts of zoisite, 15-25 parts of wollastonite, 10-15 parts of dolomite, 10-18 parts of quartz, 8-15 parts of zirconium powder and 1-5 parts of zinc oxide. The obtained ceramic tile glaze has a visual effect of ice needle-like texture highly simulating ice needles in nature by using the specially designed ice needle dry particle, and the glaze has excellent texture and good touch and transparency.

Description

Technical Field

[0001] This invention belongs to the field of building ceramics, specifically relating to a dry granule of ice needles, a ceramic brick with an ice needle effect, and its preparation method. Background Technology

[0002] With the rapid development of the building ceramics industry, ceramic tiles have become widely used in the field of building decoration materials due to their unique texture and physical properties. However, traditional ceramic tiles lack innovation and artistry, making it difficult to meet the diversified needs of modern decorative design. In recent years, the rise of young consumers has led to a continuous improvement in their aesthetic standards and increasingly higher demands for building decoration materials. Currently, young consumers tend to choose ceramic tile products that can showcase individuality, possess artistic flair, and offer novel visual effects.

[0003] Currently, granular frit powder is widely used in the market as the main material to enhance the surface texture of ceramic tiles, aiming to more accurately mimic the natural texture and feel of natural stone. Its particle size is typically controlled between 100 and 250 mesh to achieve an ideal balance between visual effect and physical properties. However, with consumers' increasing pursuit of aesthetics and the diversification of decorative styles, traditional granular frit powder can no longer meet all market demands. To drive the ceramic industry to a higher level of development, the industry has begun to actively explore frit powder materials with different forms (such as flakes, needles, flocs, and strips).

[0004] Chinese patent CN 114014698 A discloses a sheet-like silver-luster ceramic slab and its preparation method. The method involves preparing high-refractive-index zirconium oxide with a specific phase composition into zirconium sheets and spreading them on the surface of the brick blank. The refractive index difference between the zirconium sheets and the glass phase formed after firing the transparent glaze promotes a reflective effect on the glaze surface of the zirconium sheet decoration area.

[0005] Chinese patent CN 118388138 B discloses a needle-like crystal particle and its application. The raw material is melted at high temperature to form a liquid state, then cooled and crystallized. After rapid cooling, it breaks down into incomplete small crystal pieces, and various needle-like textures are naturally formed in the crystals. Summary of the Invention

[0006] To address the aforementioned problems, the present invention aims to provide a ceramic tile with ice needle-like texture and a method for its preparation. By using specially designed ice needle-like dry granules, the ceramic tile glaze of the invention exhibits a visual effect that highly simulates the ice needle-like texture found in nature, and the glaze also possesses excellent texture, good tactile feel, and translucency.

[0007] In a first aspect, the present invention provides dried ice needle granules. The mineral composition of the dried ice needle granules includes, by weight, 20-35 parts of albite, 6-12 parts of kaolinite, 8-12 parts of cordierite, 15-25 parts of wollastonite, 10-15 parts of dolomite, 10-18 parts of quartz, 8-15 parts of zircon powder, and 1-5 parts of zinc oxide.

[0008] Preferably, the chemical composition of the dried ice needle granules includes, by mass percentage: SiO2: 55%–59%; Al2O3: 17%–19%; Fe2O3: 0.1%–0.3%; TiO2: 0.1%–0.3%; CaO: 7%–10%; MgO: 0.8%–1.2%; K2O: 0.7%–1.3%; Na2O: 4%–4.8%; ZrO2: 6.4%–9%; ZnO: 1.9%–4.9%.

[0009] Preferably, the dry ice needle particles have a mesh size of 30 to 40 mesh.

[0010] Preferably, the visible light transmittance of the calcined ice needle dry particles is 15% to 20%.

[0011] Secondly, the present invention provides a method for preparing ceramic tiles with an ice needle effect. The preparation method includes the following steps:

[0012] Apply a base glaze to the surface of the blank;

[0013] Decorative patterns are printed by inkjet printing on the surface of the blank after the base glaze is applied.

[0014] After inkjet printing the decorative pattern, apply an ice needle dry particle glaze containing the ice needle dry particles to the surface of the blank.

[0015] A matte covering glaze is applied to the surface of the body after the application of ice needle dry granule glaze.

[0016] The ceramic tile with an ice needle effect is obtained by firing the body after applying a matte glaze.

[0017] Preferably, the ice needle dry granule glaze is applied by pouring glaze; more preferably, the specific gravity of the ice needle dry granule glaze is 1.18±0.1 g / cm³. 3 The glaze application amount is 160-220 g / m². 2 .

[0018] Preferably, the mineral composition of the matte coating glaze includes, by weight, 10-20 parts of matte frit, 10-15 parts of potassium feldspar, 25-35 parts of sodium feldspar, 10-18 parts of dolomite, 6-12 parts of washed clay, 5-10 parts of calcined kaolin, 5-10 parts of strontium carbonate, 4-10 parts of wollastonite, 1-6 parts of alumina, and 1-6 parts of zinc oxide.

[0019] Preferably, the chemical composition of the matte frit comprises, by mass percentage: SiO2: 51%–54%; Al2O3: 17%–19%; Fe2O3: 0.1%–0.2%; TiO2: 0.2%–0.5%; CaO: 7.2%–9%; MgO: 2.5%–3.2%; K2O: 2.6%–3.6%; Na2O: 3.8%–4.6%; BaO: 4%–4.9%; SrO: 3.6%–5%.

[0020] Preferably, the mineral composition of the matte frit includes, by weight, 5-15 parts kaolin, 20-30 parts potassium feldspar, 15-25 parts sodium feldspar, 5-15 parts limestone, 5-11 parts barium carbonate, 3-8 parts alumina, 5-12 parts talc, and 4-7 parts strontium carbonate.

[0021] Preferably, the chemical composition of the matte coating glaze comprises, by mass percentage: SiO2: 44%–49%; Al2O3: 14%–17%; Fe2O3: 0.1%–0.2%; TiO2: 0.2%–0.5%; CaO: 6.5%–7.3%; MgO: 1.7%–2.1%; K2O: 1.9%–2.7%; Na2O: 3.6%–4.3%; ZnO: 1%–5.6%; BaO: 1.2%–1.9%; SrO: 4%–4.6%; and loss on ignition: 9%–12%.

[0022] Preferably, the matte overglaze is applied by pouring an glaze; more preferably, the specific gravity of the matte overglaze is 1.89 ± 0.1 g / cm³. 3 The glaze application rate is 400-450 g / m². 2 .

[0023] Preferably, the chemical composition of the base glaze includes, by mass percentage: SiO2: 56%–60%; Al2O3: 26%–29%; Fe2O3: 0.1%–0.3%; TiO2: 0.2%–0.5%; CaO: 0.5%–0.8%; MgO: 0.1%–0.3%; K2O: 3.5%–4.7%; Na2O: 3.2%–4.3%; ZrO2: 4%–4.9%; and loss on ignition: 1%–3%.

[0024] Preferably, the mineral composition of the base glaze includes, by weight, 30-45 parts potassium feldspar, 5-12 parts sodium feldspar, 18-28 parts nepheline, 6-12 parts kaolinite, 10-16 parts ultra-white alumina, 5-12 parts quartz, and 6-8 parts zirconium silicate.

[0025] Preferably, the base glaze is applied by pouring; more preferably, the specific gravity of the base glaze is 1.89 ± 0.1 g / cm³. 3The glaze application amount is 480-520 g / m². 2 .

[0026] Preferably, the maximum firing temperature is 1198–1205℃, and the firing cycle is 45–55 minutes.

[0027] Thirdly, the present invention provides a ceramic tile with an ice needle effect. The ceramic tile with the ice needle effect is obtained according to the preparation method described above.

[0028] Beneficial effects

[0029] This invention uses specially designed ice needle dry granules to create ceramic tile glazes that highly simulate the visual effect of ice needle-like textures found in nature, and the glazes also have excellent texture, good tactile feel, and translucency. Attached Figure Description

[0030] Figure 1 The image shows the surface effect of the ice needle effect ceramic tile prepared in Example 1.

[0031] Figure 2 The image shows the surface effect of the ceramic tile with the ice needle effect obtained in Example 2.

[0032] Figure 3 This is a picture of the surface effect of the ceramic tile prepared in Comparative Example 1. Detailed Implementation

[0033] The present invention will be further described below with reference to the accompanying drawings through the following embodiments. It should be understood that the following embodiments are for illustrative purposes only and are not intended to limit the present invention. The following exemplarily illustrates the method for preparing ceramic tiles with an ice needle effect according to the present invention.

[0034] Green bodies are prepared by pressing and molding green body powder. The chemical composition of the green body powder is not limited, and commonly used green body powders in this field can be used. The green body raw material is ball-milled and spray-granulated to obtain the green body powder.

[0035] The forming methods include, but are not limited to, dry pressing. The raw material powder is fed into a press mold and pressed to obtain a ceramic blank. For example, a brick blank is obtained by pressing under a pressure of 320 bar. The size of the blank can be varied as needed. A blank with a diameter of 800mm x 800mm can be used.

[0036] Dry the billet. Drying can be done in a drying kiln. The drying temperature can be adjusted as needed. For example, the drying cycle can be 55 minutes. The moisture content of the dried billet should be controlled within 0.2wt% to 0.5wt%.

[0037] A base glaze is applied to the surface of the brick blank. The purpose of the base glaze is to cover defects in the blank and to assist in the color development of inkjet printing inks. For example, the chemical composition of the base glaze includes, by mass percentage: SiO2: 56%–60%; Al2O3: 26%–29%; Fe2O3: 0.1%–0.3%; TiO2: 0.2%–0.5%; CaO: 0.5%–0.8%; MgO: 0.1%–0.3%; K2O: 3.5%–4.7%; Na2O: 3.2%–4.3%; ZrO2: 4%–4.9%; Loss on ignition: 1%–3%.

[0038] In some embodiments, the mineral composition of the base glaze includes, by weight, 30-45 parts potassium feldspar, 5-12 parts sodium feldspar, 18-28 parts nepheline, 6-12 parts kaolinite, 10-16 parts ultra-white alumina, 5-12 parts quartz, and 6-8 parts zirconium silicate.

[0039] Raw materials (considered dry material) are weighed according to the mineral composition of the base glaze, and then ball-milled with water and additives. The mass ratio of dry material to water can be 100:(10-60). For example, the mass ratio of dry material to water can be 100:40. Additives include, but are not limited to, sodium carboxymethyl cellulose and sodium tripolyphosphate. Sodium carboxymethyl cellulose can account for 0.1wt% to 0.4wt% of the base glaze mineral composition, and sodium tripolyphosphate can account for 0.1wt% to 0.4wt% of the base glaze mineral composition. For example, sodium carboxymethyl cellulose can account for 0.15wt% of the base glaze mineral composition, and sodium tripolyphosphate can account for 0.35wt% of the base glaze mineral composition. The ball-milled slurry is then subjected to iron removal, sieving, aging, and homogenization to obtain the base glaze slurry. The residue on a 325-mesh sieve of the base glaze slurry can be 0.6±0.1wt%. In some embodiments, the viscosity of the base glaze slurry is 220±20 Pa·s. When using a base glaze, water can be added to the glaze slurry to adjust the final glaze slurry specific gravity to the desired level. The flow rate of the base glaze slurry on the brick surface can be 27s / 50ml.

[0040] A base glaze can be applied using a glazing process. In some embodiments, the specific gravity of the base glaze is 1.89 ± 0.1 g / cm³. 3 The glaze application amount is 480-520 g / m². 2 If the amount of base glaze is too small, it will be difficult to cover the color of the body and weaken the ability of ink to develop color; if the amount of base glaze is too large, it will increase production costs and hinder the air release of the body, resulting in more air holes on the brick surface.

[0041] In some embodiments, the coefficient of thermal expansion of the base glaze at 600°C is 8.8 × 10⁻⁶. -6 / K~9.0×10 -6 / K. For example, the coefficient of thermal expansion of the base glaze at 600°C is 8.9012 × 10⁻⁶. -6 / K.

[0042] Decorative patterns are printed using inkjet printing on the surface of the ceramic body after the base glaze has been applied. The inkjet printing pattern can be selected based on the layout design. The texture and color of the inkjet-printed pattern can be adapted to the layout design.

[0043] After inkjet printing the decorative pattern, an ice needle dry particle glaze containing ice needle dry particles is applied to the surface of the ceramic tile. The purpose of the ice needle dry particles is to enhance the decorative texture of the ceramic tile surface and improve the product's grade.

[0044] In some embodiments, the mineral composition of the dried ice needle particles includes, by weight, 20-35 parts of albite, 6-12 parts of kaolinite, 8-12 parts of cordierite, 15-25 parts of wollastonite, 10-15 parts of dolomite, 10-18 parts of quartz, 8-15 parts of zircon powder, and 1-5 parts of zinc oxide.

[0045] Sodium feldspar can accelerate the melting rate of minerals such as quartz, zircon powder, and clay; wollastonite, dolomite, and zinc oxide provide divalent oxide fluxes such as calcium oxide, magnesium oxide, and zinc oxide, which form composite fluxes with monovalent oxide fluxes. At high temperatures, these fluxes not only promote the chemical reaction between raw materials but also help form more complex and ordered crystal structures. These structures are composed of various forms and types of crystals interwoven, giving ice needle dry granules unique physical and chemical properties; cordierite will be converted into a large amount of α-cordierite crystal phase during high-temperature firing. The excellent thermal stability and extremely low coefficient of thermal expansion of this crystal phase can effectively prevent material deformation or cracking caused by temperature changes, thereby improving the thermal stability of ice needle dry granules. Zircon powder possesses a unique tetragonal crystal structure. While it may retain its original tetragonal phase after high-temperature firing, some zircon elements react with other minerals to form new compounds or crystal phases. These not only affect the crystal structure and microstructure of the ice needle granules but also potentially influence the ice needle effect by altering light scattering and reflection. Furthermore, as a key opacifier in ice needle granules, the crystal phase formed during firing often exhibits an opaque state. This opacity effectively scatters light, causing diffuse reflection as it passes through the ice needle granules, thus reducing visible light transmittance. By precisely controlling the proportion of zircon powder added or adjusting its crystallization degree, the visible light transmittance of the ice needle granules can be flexibly adjusted. Zinc oxide can further enhance the opacification effect of ice needle granules and promote crystallization. The reaction of zinc oxide with aluminum forms zinc-aluminum spinel, a crystal phase that also possesses excellent scattering properties, further enhancing light scattering within the ice needle granules. Wollastonite, dolomite, and quartz can also be used to adjust gloss and hardness. The phase composition of the dried ice needle granules after firing includes potassium-sodium feldspar crystal phases, calcium feldspar crystal phases, zircon crystal phases, and zinc-aluminum spinel crystal phases.

[0046] Ice needle granules are prepared according to the following steps: Mineral raw materials for ice needle granules are mixed in a specific ratio and placed in a crucible, tank furnace, or rotary furnace. The mixture is melted at a high temperature of 1450–1600°C to obtain molten glass. The molten glass is then poured into cold water for quenching, causing it to become a brittle block. This block is then dried to obtain a fused mass. The resulting fused mass can be crushed and sieved to obtain ice needle granules of the desired particle size. The mesh size of the ice needle granules can be 30–40 mesh. The shape of the ice needle granules can be flake-like. For example, the fused mass can be dried and then conveyed to a machine for flake removal to obtain flake-like ice needle granules. In some embodiments, the thickness of the ice needle granules is 0.2–0.5 mm; the diagonal length is 2–6 mm. After firing, the visible light transmittance of the ice needle granules is 15%–20%.

[0047] In some embodiments, the coefficient of thermal expansion of the dried ice needle granules at 600°C is 4.1 × 10⁻⁶. -6 / K~4.3×10 -6 / K. For example, the coefficient of thermal expansion of the dry ice needle granules at 600℃ is 4.236×10. -6 / K.

[0048] A dry-granule glaze slurry for ice needles is prepared. The slurry is composed of dry-granule ice needles and a suspending agent. The suspending agent can be a mixture of sodium methylcellulose, ethylene glycol, bentonite, and water. Bentonite improves the suspension and adhesion properties of the suspending agent. The raw materials for the suspending agent are weighed according to their composition and stirred evenly to prepare the suspending agent. In some technical solutions, the mass ratio of sodium methylcellulose:ethylene glycol:bentonite:water is 1–5:40–60:2–8:40–50. For example, the mass ratio of sodium methylcellulose:ethylene glycol:bentonite:water is 3:50:5:42. The amounts of dry-granule ice needles and the suspending agent can be adjusted as needed. For example, the mass ratio of suspending agent to dry-granule ice needles can be 100–120:5–10.

[0049] In some technical solutions, the chemical composition of the dried ice needle granules includes, by mass percentage: SiO2: 55%–59%; Al2O3: 17%–19%; Fe2O3: 0.1%–0.3%; TiO2: 0.1%–0.3%; CaO: 7%–10%; MgO: 0.8%–1.2%; K2O: 0.7%–1.3%; Na2O: 4%–4.8%; ZrO2: 6.4%–9%; ZnO: 1.9%–4.9%.

[0050] The ice-needle dry granule glaze can be applied using a glazing process. In some embodiments, the specific gravity of the ice-needle dry granule glaze is 1.18 ± 0.1 g / cm³. 3 Glazing amount: 160-220g / m 2 .

[0051] A matte overglaze is applied to the surface of the ceramic tile after the application of the ice needle dry granule glaze. The matte overglaze gives the ceramic tile a soft and delicate feel, while also resisting wear and tear during daily use and extending the lifespan of the ceramic tile.

[0052] In some embodiments, the mineral composition of the matte coating glaze includes, by weight: 10-20 parts matte frit, 10-15 parts potassium feldspar, 25-35 parts sodium feldspar, 10-18 parts dolomite, 6-12 parts washed clay, 5-10 parts calcined kaolin, 5-10 parts strontium carbonate, 4-10 parts wollastonite, 1-6 parts alumina, and 1-6 parts zinc oxide.

[0053] In some technical solutions, the chemical composition of the matte frit includes, by mass percentage: SiO2: 51%–54%; Al2O3: 17%–19%; Fe2O3: 0.1%–0.2%; TiO2: 0.2%–0.5%; CaO: 7.2%–9%; MgO: 2.5%–3.2%; K2O: 2.6%–3.6%; Na2O: 3.8%–4.6%; BaO: 4%–4.9%; SrO: 3.6%–5%.

[0054] In some embodiments, the mineral composition of the matte frit includes, by weight: 5-15 parts kaolin, 20-30 parts potassium feldspar, 15-25 parts sodium feldspar, 5-15 parts limestone, 5-11 parts barium carbonate, 3-8 parts alumina, 5-12 parts talc, and 4-7 parts strontium carbonate. Pre-forming the raw materials into frits can improve the stability of the glaze and reduce the generation of defects.

[0055] After weighing the materials according to the mineral composition of the matte frit, it is melted in a frit furnace at a high temperature of 1400℃~1500℃ (e.g., 1450℃) to obtain molten glass. The molten glass is then poured into cold water for quenching, and the molten glass forms a frit upon cooling. The frit is then crushed and sieved to obtain dry granular powder. The mesh size of the matte frit can be 150~200 mesh.

[0056] In some technical solutions, the chemical composition of the matte coating glaze includes, by mass percentage: SiO2: 44%–49%; Al2O3: 14%–17%; Fe2O3: 0.1%–0.2%; TiO2: 0.2%–0.5%; CaO: 6.5%–7.3%; MgO: 1.7%–2.1%; K2O: 1.9%–2.7%; Na2O: 3.6%–4.3%; ZnO: 1%–5.6%; BaO: 1.2%–1.9%; SrO: 4%–4.6%; Loss on ignition: 9%–12%.

[0057] The raw materials (considered dry materials) are weighed according to the mineral composition of the matte overglaze glaze, and then ball-milled with water and additives. The mass ratio of dry material to water can be 100:10 to 60. For example, the mass ratio of dry material to water can be 100:40. Additives include, but are not limited to, sodium carboxymethyl cellulose and sodium tripolyphosphate. Sodium carboxymethyl cellulose can account for 0.1wt% to 0.4wt% of the mineral composition of the matte overglaze glaze, and sodium tripolyphosphate can account for 0.1wt% to 0.4wt% of the mineral composition of the matte overglaze glaze. For example, sodium carboxymethyl cellulose can account for 0.15wt% of the mineral composition of the matte overglaze glaze, and sodium tripolyphosphate can account for 0.3wt% of the mineral composition of the matte overglaze glaze. The ball-milled slurry is then subjected to iron removal, sieving, aging, and homogenization to obtain the matte overglaze glaze slurry. The residue on a 325-mesh sieve of the matte overglaze glaze slurry can be 0.4±0.1wt%. When using the matte overglaze glaze, water can be added to the matte overglaze glaze slurry to adjust to the desired final slurry specific gravity. The flow rate of the matte glaze on the surface of the brick blank can be 28s / 50ml.

[0058] A matte overglaze can be applied using a glazing process. In some embodiments, the specific gravity of the matte overglaze is 1.89 ± 0.1 g / cm³. 3 The glaze application rate is 400-450 g / m². 2 If too much glaze is applied to a matte finish, the color rendering of the design will be reduced, and the glaze surface will become opaque.

[0059] In some embodiments, the matte overglaze has a coefficient of thermal expansion of 7.9 × 10⁻⁶ at 600°C. -6 / K~8.1×10 -6 / K. For example, the coefficient of thermal expansion of the matte overglaze at 600°C is 8.0111 × 10⁻⁶. -6 / K.

[0060] The body is then fired after being coated with a matte glaze. Firing can be done in a kiln. For example, the maximum firing temperature is 1198–1205℃, and the firing cycle is 45–55 minutes. Under this firing regime, the dry ice needle particles exhibit good chemical stability and a stable opacifying effect, avoiding adverse physical and chemical changes.

[0061] In summary, the present invention uses dry ice needle particles with a low coefficient of thermal expansion, good thermal stability, and a visible light transmittance of 15% to 20% after firing. During the high-temperature firing process, these particles will not produce adverse physical and chemical reactions with the matte covering glaze. They have a texture, feel, and visual effect that highly simulates the ice needles in nature. Moreover, under the covering effect of the matte covering glaze, the dry ice needle particles still retain their characteristics, and the glaze surface has a good tactile and translucent feel.

[0062] The following examples further illustrate the present invention in detail. It should also be understood that the following examples are only for further explanation of the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention are within the scope of protection of the present invention. The specific process parameters, etc., in the following examples are merely examples within a suitable range; that is, those skilled in the art can make appropriate selections within the range based on the description herein, and are not intended to be limited to the specific values ​​in the examples below. It should be noted that the description of these examples is for the purpose of helping to understand the present invention, but does not constitute a limitation on the present invention.

[0063] Example 1

[0064] This embodiment prepares ceramic bricks with an ice needle effect according to the following steps:

[0065] S1, Pressing the blank.

[0066] S2. Apply a base glaze to the body. The mineral composition of the base glaze includes, by weight, 34 parts potassium feldspar, 5 parts sodium feldspar, 23 parts nepheline, 10 parts kaolin, 14 parts ultra-white alumina, 7 parts quartz, and 7 parts zirconium silicate. The chemical composition of the base glaze includes, by mass percentage, SiO2: 57.45%; Al2O3: 27.48%; Fe2O3: 0.21%; TiO2: 0.26%; CaO: 0.54%; MgO: 0.15%; K2O: 3.88%; Na2O: 3.71%; ZrO2: 4.42%; loss on ignition: 1.9%. The base glaze is applied using a pouring glaze process. The specific gravity of the base glaze is 1.89 g / cm³. 3 Glazing amount is 500g / m 2 .

[0067] S3. Inkjet print decorative patterns on the glazed body.

[0068] S4. Apply ice needle dry granule glaze to the blank after inkjet printing the decorative pattern. The mineral composition of the ice needle dry granules includes, by weight: 28 parts albite, 7 parts kaolinite, 9 parts cordierite, 18 parts wollastonite, 10 parts dolomite, 13 parts quartz, 12 parts zircon powder, and 3 parts zinc oxide. Weigh and mix the mineral raw materials according to the proportions of the ice needle dry granules, place them in a crucible, and melt them at a high temperature of 1450℃ to obtain glass melt. Pour the molten glass into cold water for quenching, and rapidly cool it to make it into brittle blocks. Dry the blocks and convey them to a machine for peeling to obtain ice needle dry granules. The chemical composition of the ice needle granules includes, by mass percentage: SiO2: 56.81%; Al2O3: 17.88%; Fe2O3: 0.14%; TiO2: 0.16%; CaO: 8.46%; MgO: 0.84%; K2O: 0.89%; Na2O: 4.37%; ZrO2: 7.56%; ZnO: 2.89%. The visible light transmittance of the ice needle granules after firing is 16%, as measured by an instrument. A suspending agent is prepared by weighing and stirring the materials according to a mass ratio of sodium methylcellulose: ethylene glycol: bentonite: water = 3:50:5:42. The ice needle granule glaze is obtained by weighing and stirring the materials according to a mass ratio of suspending agent: ice needle granules = 100:6. The ice needle granule glaze is applied using a glazing process. The specific gravity of the ice needle granule glaze is 1.18 g / cm³. 3 Glazing amount is 200g / m 2 .

[0069] S5. Apply a matte covering glaze to the body after applying the ice needle dry granule glaze. The mineral composition of the matte covering glaze includes, by weight: 12 parts matte frit, 11 parts potassium feldspar, 28 parts sodium feldspar, 14 parts dolomite, 11 parts washed clay, 6 parts calcined kaolin, 6 parts strontium carbonate, 8 parts wollastonite, 2 parts alumina, and 2 parts zinc oxide. The mineral composition of the matte frit includes, by weight: 12 parts kaolin, 26 parts potassium feldspar, 22 parts sodium feldspar, 14 parts limestone, 9 parts barium carbonate, 4 parts alumina, 8 parts talc, and 5 parts strontium carbonate. The chemical composition of the matte coating glaze includes, by mass percentage: SiO2: 48.53%; Al2O3: 15.92%; Fe2O3: 0.13%; TiO2: 0.29%; CaO: 6.95%; MgO: 1.91%; K2O: 2.44%; Na2O: 4.11%; ZnO: 1.97%; BaO: 1.46%; SrO: 4.51%; Loss on ignition: 11.78%. The matte coating glaze is applied using a pour-over process. The specific gravity of the matte coating glaze is 1.89 g / cm³. 3 The glaze application amount is 420g / m². 2 .

[0070] S6. The unglazed ceramic body with a matte finish is transferred to the kiln for high-temperature firing. After edge grinding and sorting, a finished ceramic tile with an ice needle effect is obtained. The maximum firing temperature is 1202℃, and the firing cycle is 47 minutes.

[0071] Figure 1 The image shows the surface effect of the ice needle effect ceramic tile prepared in Example 1. It can be seen that the glaze of the ceramic tile highly simulates the texture, feel, and visual effect of ice needles in nature.

[0072] Example 2

[0073] This embodiment follows the preparation process of Example 1, but differs in that the mineral composition of the dried ice needle granules includes, by weight, 28 parts albite, 7 parts kaolinite, 12 parts cordierite, 18 parts wollastonite, 11 parts dolomite, 13 parts quartz, 10 parts zircon powder, and 3 parts zinc oxide. The chemical composition of the dried ice needle granules includes, by mass percentage, 57.18% SiO2; 18.01% Al2O3; 0.17% Fe2O3; 0.17% TiO2; 8.58% CaO; 1.07% MgO; 0.92% K2O; 4.45% Na2O; 6.53% ZrO2; and 2.92% ZnO. After firing, the visible light transmittance of the dried ice needle granules was measured to be 20%. Weigh and mix the mineral raw materials according to the proportions for making ice needle dry granules, place them in a crucible, and melt them at a high temperature of 1600℃ to obtain glass melt. Pour the molten glass into cold water to quench it, and make it into a brittle block by rapid cooling. Dry the block and convey it to a machine for peeling to obtain ice needle dry granules.

[0074] Figure 2 This image shows the surface effect of the ceramic tile with the ice needle effect obtained in Example 2. This example also exhibits the desired ice needle effect.

[0075] Example 3

[0076] This embodiment follows the preparation process of Example 1, but differs in that: the materials are weighed and stirred evenly according to a mass ratio of suspending agent to dried ice needle granules of 100:10 to obtain the dried ice needle granule glaze. The specific gravity of the dried ice needle granule glaze is 1.19 g / cm³. 3 Glazing amount is 160g / m 2 Furthermore, the specific gravity of the matte coating glaze is 1.89 g / cm³. 3 Glazing amount is 450g / m 2 .

[0077] The ice needle effect and tactile feel of the ceramic tile surface in this embodiment are basically the same as those in Embodiment 1.

[0078] Example 4

[0079] This embodiment follows the preparation process of Example 1, but differs from Example 1 in that: the mineral composition of the matte coating glaze includes, by weight, 15 parts matte frit, 11 parts potassium feldspar, 28 parts sodium feldspar, 14 parts dolomite, 11 parts washed clay, 5 parts calcined kaolin, 6 parts strontium carbonate, 8 parts wollastonite, 3 parts alumina, and 2 parts zinc oxide. The chemical composition of the matte coating glaze includes, by mass percentage, SiO2: 48.37%; Al2O3: 16.19%; Fe2O3: 0.11%; TiO2: 0.22%; CaO: 7.11%; MgO: 1.96%; K2O: 2.37%; Na2O: 4.26%; ZnO: 1.94%; BaO: 1.51%; SrO: 4.58%; loss on ignition: 11.38%.

[0080] In this embodiment, the glaze transparency is enhanced, the ice needle effect becomes more obvious, and the brick surface has a softer and more delicate tactile feel.

[0081] Comparative Example 1

[0082] This comparative example follows the preparation process of Example 1, but differs from Example 1 in that: the mineral composition of the dried ice needle granules includes, by weight, 28 parts of albite, 7 parts of kaolinite, 9 parts of cordierite, 18 parts of wollastonite, 10 parts of dolomite, 13 parts of quartz, and 3 parts of zinc oxide. The chemical composition of the dried ice needle granules includes, by mass percentage, SiO2: 61.55%; Al2O3: 18.13%; Fe2O3: 0.17%; TiO2: 0.19%; CaO: 9.35%; MgO: 1.04%; K2O: 0.98%; Na2O: 4.87%; ZnO: 3.72%.

[0083] Figure 3 This is a picture of the ceramic tile surface effect obtained in Comparative Example 1. The mineral composition of the ice needle dry granules in this comparative example does not contain zircon powder, and the prepared dry granules are transparent. When applied to the surface of the tile, they cannot produce the ice needle texture.

[0084] Comparative Example 2

[0085] This comparative example uses the same raw materials and preparation process as Example 1. The difference between this example and Example 1 is that the application amount of the ice needle dry granule glaze is 300g / m³. 2 The results showed that the needle-like dry particles on the brick surface were densely distributed, affecting the visual effect.

[0086] Comparative Example 3

[0087] This comparative example follows the preparation process of Example 1, but differs from Example 1 in that the amount of matte overglaze applied is 600 g / m². 2 The results showed that the glaze surface was white, which affected the color of the designed pattern.

[0088] Comparative Example 4

[0089] This comparative example follows the preparation process of Example 1, but differs from Example 1 in that: the mineral composition of the matte coating glaze includes, by weight, 12 parts matte frit, 11 parts potassium feldspar, 28 parts sodium feldspar, 14 parts dolomite, 11 parts washed clay, 6 parts calcined kaolin, 6 parts strontium carbonate, 8 parts wollastonite, 8 parts alumina, and 2 parts zinc oxide. The chemical composition of the matte coating glaze includes, by mass percentage, SiO2: 47.42%; Al2O3: 20.61%; Fe2O3: 0.12%; TiO2: 0.21%; CaO: 6.47%; MgO: 1.73%; K2O: 2.22%; Na2O: 3.83%; ZnO: 1.79%; BaO: 1.34%; SrO: 4.27%; and loss on ignition: 9.99%.

[0090] The results showed that the increased alumina content in the control ratio resulted in an underfired and whitish glaze with a rough texture, and the design patterns and ice needle particles were obscured, failing to achieve the desired effect.

[0091] Comparative Example 5

[0092] This comparative example follows the preparation process of Example 1, but differs from Example 1 in that step S4 (applying the ice needle dry granule glaze layer) is omitted. Instead, in step S5, the ice needle dry granules are directly incorporated into the matte covering glaze. The mass ratio of the ice needle dry granules to the matte covering glaze is 5:100, and the combined amount of the mixed ice needle dry granules and matte covering glaze is 420 g / m³. 2 .

[0093] The results showed that although the comparative sample exhibited the ice needle effect, it also had numerous defects on the brick surface, such as glaze defects, glaze marks, and depressions, making stable production difficult. This is because the dry ice needle granules are a ridge-like material with irregular, elongated shapes. When directly added to the covering glaze slurry, the poor bonding between the two affects the flowability of the glaze slurry during the glazing process, causing significant problems for production stability.

[0094] Comparative Example 6

[0095] This comparative example follows the preparation process of Example 1, but differs from Example 1 in that: the mineral composition of the dried ice needle particles includes, by weight, 28 parts of albite, 7 parts of kaolinite, 18 parts of wollastonite, 10 parts of dolomite, 13 parts of quartz, 12 parts of zircon powder, and 3 parts of zinc oxide. The chemical composition of the dried ice needle particles includes, by mass percentage, SiO2: 57.57%; Al2O3: 16.63%; Fe2O3: 0.11%; TiO2: 0.17%; CaO: 8.94%; MgO: 0.49%; K2O: 0.86%; Na2O: 4.37%; ZrO2: 7.33%; ZnO: 3.53%.

[0096] The results showed that the thermal stability of the ice needle dry granules deteriorated. When applied to the glaze layer and fired at high temperature, the ice needle dry granules cracked. At the same time, the glaze layer in the affected area bulged, and the brick surface effect did not meet the production requirements.

[0097] The above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A type of dried ice needle granules, characterized in that, The mineral composition of the ice needle dry granules includes, by weight, 20-35 parts of albite, 6-12 parts of kaolinite, 8-12 parts of cordierite, 15-25 parts of wollastonite, 10-15 parts of dolomite, 10-18 parts of quartz, 8-15 parts of zircon powder, and 1-5 parts of zinc oxide; the visible light transmittance of the ice needle dry granules after firing is 15%-20%.

2. The dried ice needle granules according to claim 1, characterized in that, The chemical composition of the dried ice needle granules includes, by mass percentage: SiO2: 55%~59%; Al2O3: 17%~19%; Fe2O3: 0.1%~0.3%; TiO2: 0.1%~0.3%; CaO: 7%~10%; MgO: 0.8%~1.2%; K2O: 0.7%~1.3%; Na2O: 4%~4.8%; ZrO2: 6.4%~9%; ZnO: 1.9%~4.9%.

3. The dried ice needle granules according to claim 1, characterized in that, The dry ice needle particles have a mesh size of 30-40 mesh.

4. A method for preparing ceramic tiles with an ice needle effect, characterized in that, The preparation method includes the following steps: Apply a base glaze to the surface of the blank; Decorative patterns are printed by inkjet printing on the surface of the blank after the base glaze is applied. After inkjet printing a decorative pattern, an ice needle dry particle glaze containing ice needle dry particles according to any one of claims 1 to 3 is applied to the surface of the body; a matte covering glaze is applied to the surface of the body after the ice needle dry particle glaze is applied; and the body after the matte covering glaze is applied is fired to obtain a ceramic tile with an ice needle effect.

5. The preparation method according to claim 4, characterized in that, The ice needle dry granular glaze is applied by glazing; the specific gravity of the ice needle dry granular glaze is 1.18 ± 0.1 g / cm 3 , and the glazing amount is 160~220 g / m 2 .

6. The preparation method according to claim 4, characterized in that, The mineral composition of the matte coating glaze includes, by weight: 10-20 parts matte frit, 10-15 parts potassium feldspar, 25-35 parts sodium feldspar, 10-18 parts dolomite, 6-12 parts washed clay, 5-10 parts calcined kaolin, 5-10 parts strontium carbonate, 4-10 parts wollastonite, 1-6 parts alumina, and 1-6 parts zinc oxide.

7. The preparation method according to claim 6, characterized in that, The chemical composition of the matte frit includes, by mass percentage: SiO2: 51%~54%; Al2O3: 17%~19%; Fe2O3: 0.1%~0.2%; TiO2: 0.2%~0.5%; CaO: 7.2%~9%; MgO: 2.5%~3.2%; K2O: 2.6%~3.6%; Na2O: 3.8%~4.6%; BaO: 4%~4.9%; SrO: 3.6%~5%.

8. The preparation method according to claim 6, characterized in that, The mineral composition of the matte frit includes, by weight, 5-15 parts kaolin, 20-30 parts potassium feldspar, 15-25 parts sodium feldspar, 5-15 parts limestone, 5-11 parts barium carbonate, 3-8 parts alumina, 5-12 parts talc, and 4-7 parts strontium carbonate.

9. The preparation method according to claim 4, characterized in that, The chemical composition of the matte coating glaze includes, by mass percentage: SiO2: 44%~49%; Al2O3: 14%~17%; Fe2O3: 0.1%~0.2%; TiO2: 0.2%~0.5%; CaO: 6.5%~7.3%; MgO: 1.7%~2.1%; K2O: 1.9%~2.7%; Na2O: 3.6%~4.3%; ZnO: 1%~5.6%; BaO: 1.2%~1.9%; SrO: 4%~4.6%; Loss on ignition: 9%~12%.

10. The preparation method according to claim 4, characterized in that, The matte coating glaze is applied by pouring; the specific gravity of the matte coating glaze is 1.89 ± 0.1 g / cm³. 3 The glaze application rate is 400~450 g / m². 2 .

11. The preparation method according to claim 4, characterized in that, The chemical composition of the base glaze includes, by mass percentage: SiO2: 56%~60%; Al2O3: 26%~29%; Fe2O3: 0.1%~0.3%; TiO2: 0.2%~0.5%; CaO: 0.5%~0.8%; MgO: 0.1%~0.3%; K2O: 3.5%~4.7%; Na2O: 3.2%~4.3%; ZrO2: 4%~4.9%; Loss on ignition: 1%~3%.

12. The preparation method according to claim 4, characterized in that, The mineral composition of the base glaze includes, by weight, 30-45 parts potassium feldspar, 5-12 parts sodium feldspar, 18-28 parts nepheline, 6-12 parts kaolinite, 10-16 parts ultra-white alumina, 5-12 parts quartz, and 6-8 parts zirconium silicate.

13. The preparation method according to claim 4, characterized in that, The base glaze is applied by pouring; the specific gravity of the base glaze is 1.89 ± 0.1 g / cm³. 3 The glaze application rate is 480~520g / m². 2 .

14. The preparation method according to claim 4, characterized in that, The maximum firing temperature is 1198~1205℃, and the firing cycle is 45~55 minutes.

15. A ceramic tile with an ice needle effect, characterized in that, The ceramic tile with the ice needle effect is obtained by the preparation method according to any one of claims 4 to 14.

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