Ice crack porcelain tile and preparation method thereof

Abstract

The invention belongs to the field of architectural ceramics, and relates to an ice crack porcelain tile and a preparation method thereof. The preparation method of the ice crack porcelain tile comprises the following steps: carrying out first firing on a green body to obtain a biscuit firing green body; applying cover glaze on the biscuit firing blank; carrying out ink-jet printing on an ink pattern on the biscuit firing blank subjected to overglaze application; applying ice crack glaze on the biscuit firing blank after ink-jet printing of the ink pattern; and performing secondary firing on the biscuit firing blank applied with the ice crack glaze to obtain the ice crack porcelain tile. According to the ice crack porcelain tile obtained through the preparation method, the artistic aesthetic feeling of ice cracks such as ice cracking and crack stacking is completely copied, the firing time is short, the production cost is greatly reduced, the large-specification porcelain tile can be prepared, technical breakthrough is achieved, and the market blank is filled.

Description

Technical Field

[0001] This invention belongs to the field of building ceramics and relates to ice-crack pattern porcelain tiles and their preparation methods. Background Technology

[0002] With the development of the building ceramics market, the variety of building decoration materials is increasing, and consumers are placing higher demands on the material, pattern layering, color, and decorative effect of tiles. Artistic glazes in daily-use ceramics are highly favored by consumers due to their unique artistic style, while ice crackle patterns, also known as crackle patterns, are named for their layered, three-dimensional appearance resembling cracked ice. The production process of ice crackle patterns is exceptionally complex. Currently, ice crackle patterns can only be applied to the high-temperature, slow-firing process of daily-use ceramics, while the low-temperature, fast-firing technology for ice crackle patterns has not yet been fully mastered in the building ceramics industry.

[0003] Chinese patent CN201910425351.X discloses a crackle glaze for glass mosaics and a preparation process for glass mosaics. First, a mosaic blank is prepared and then bisque-fired at 650–700℃ for 80–100 minutes. A crackle glaze is applied to the surface of the bisque-fired mosaic blank, and the glazed blank is then sintered in a roller kiln with a glaze application rate of 0.6–1.0 kg / m³. 2 The sintering temperature is 780–820℃, and the time is 80–100 min. This preparation method has a long firing time and cannot produce large-format ceramic tiles. Summary of the Invention

[0004] To address the aforementioned problems, this invention provides an ice-crack pattern porcelain tile and its preparation method. The surface cracks resemble ice cracks, with overlapping cracks that completely replicate the artistic beauty of ice cracks. Furthermore, this preparation method has a short firing time and significantly reduces production costs, enabling the production of large-format porcelain tiles. This represents a technological breakthrough and fills a market gap.

[0005] In a first aspect, the present invention provides an ice-crack pattern porcelain tile and a method for preparing the same. The preparation method includes the following steps: The blank is fired in the first firing to obtain a bisque blank; Apply a surface glaze to the bisque-fired clay; Ink patterns are printed on the bisque after the surface glaze has been applied; Apply ice-crack glaze to the bisque fired with inkjet-printed ink patterns; The unglazed body with ice-crack glaze is fired a second time to obtain ice-crack porcelain tiles.

[0006] Preferably, the water absorption rate of the bisque is 8% to 16%.

[0007] Preferably, the mineral composition of the glaze includes, by mass percentage: 20%–40% potassium feldspar, 20%–35% spodumene, 8%–12% washed kaolin, 10%–20% quartz, 10%–15% calcined alumina, 8%–12% zirconium silicate, 2%–10% calcite, and 1.5%–3% zinc oxide.

[0008] Preferably, the chemical composition of the surface glaze includes, by mass percentage: loss on ignition: 1.2%–2.8%; Al2O3: 23.2%–28.5%; SiO2: 58.5%–62.3%; Fe2O3: 0.3%–0.6%; CaO: 1.5%–2.8%; ZnO: 1.2%–2.5%; K2O: 2.2%–3.4%; Li2O: 1.8%–3.0%; TiO2: 0.1%–0.3%; ZrO2: 4.2%–6.3%.

[0009] Preferably, the coefficient of thermal expansion of the glaze at 20–600°C is controlled at 3.2 × 10⁻⁶. -6 / ℃~4.6×10 -6 / ℃. If the coefficient of thermal expansion of the surface glaze is too large, the difference between the surface glaze and the ice-crack glaze will be too small, and the cracks will not be obvious or will not open. If the coefficient of thermal expansion of the surface glaze is too small, the difference between the surface glaze and the ice-crack glaze will be too large, resulting in cracks that are too large and dense, and may even cause the glaze layer to peel off.

[0010] Preferably, the glaze is applied by pouring; more preferably, the specific gravity of the glaze is 1.82–1.86 g / cm³. 3 The glaze application rate is 660–720 g / m². 2 .

[0011] Preferably, the mineral composition of the ice-crack glaze includes, by mass percentage: 5%–10% kaolin, 80%–90% high-expansion calcium-magnesium frit, 3%–6% calcined zinc oxide, 2%–8% barium carbonate, and 1%–5% strontium carbonate.

[0012] Preferably, the chemical composition of the high-expansion calcium-magnesium frit includes, by mass percentage: SiO2: 52%–64%, Al2O3: 12%–20%, CaO: 18%–35%, MgO: 2.5%–6.4%, K2O: 1.2%–3%, Na2O: 3.2%–8.6%, Fe2O3: 0.1%–0.3%, TiO2: 0.1%–0.3%.

[0013] Preferably, the chemical composition of the ice-crack glaze includes, by mass percentage: loss on ignition: 2.2%–3.8%; SiO2: 50.8%–60.4%; Al2O3: 10.2%–14.6%; CaO: 14.8%–18.5%; MgO: 1.5%–2.8%; K2O: 0.8%–2.2%; Na2O: 2.1%–3.9%; BaO: 1.5%–2.7%; SrO: 0.8%–1.6%; ZnO: 2.8%–5.2%.

[0014] Preferably, the coefficient of thermal expansion of the crackle glaze is controlled at 9.2 × 10⁻⁶ at 20–600 °C. -6 / ℃~10.8×10 -6 / ℃. If the coefficient of expansion of the crackle glaze is too large, the difference between the surface glaze and the crackle glaze will be too great, resulting in excessively large and dense cracks, or even causing the glaze layer to peel off; if the coefficient of expansion of the crackle glaze is too small, the difference between the surface glaze and the crackle glaze will be too small, and the cracks will not be obvious or will not crack at all.

[0015] Preferably, the ice-crack glaze is applied by pouring glaze; more preferably, the specific gravity of the ice-crack glaze is 1.82–1.86 g / cm³. 3 The glaze application rate is 1030–1260 g / m². 2 .

[0016] Preferably, the firing temperature for the second firing is 1180–1250°C, and the firing time is 40–50 minutes.

[0017] Preferably, the firing temperature for the first firing is 1020–1080°C, and the firing time is 30–35 minutes.

[0018] Preferably, the chemical composition of the brick blank includes, by mass percentage: loss on ignition: 3.5%–6.8%; SiO2: 63.8%–73.3%; Al2O3: 15.2%–20.5%; CaO: 0.2%–2.5%; MgO: 0.4%–1.8%; K2O: 2.2%–4.4%; Na2O: 2.8%–5.2%; Fe2O3: 0.2%–0.6%; TiO2: 0.1%–0.3%.

[0019] Secondly, the present invention provides an ice-crack pattern porcelain tile, which is obtained according to the preparation method described above. Attached Figure Description

[0020] Figure 1 This is a rendering of the surface of the ice-crack pattern porcelain tile from Example 1. Figure 2 This is a rendering of the surface of the ice-crack pattern porcelain tile from Example 2; Figure 3 This is a brick surface rendering at scale 7; Figure 4 This is a scaled-down rendering of the brick surface. Detailed Implementation

[0021] The present invention is further illustrated by 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. Unless otherwise specified, all percentage contents refer to mass percentage contents. The following exemplarily illustrates the preparation method of the ice-crack pattern porcelain tile according to the present invention.

[0022] The brick blank is obtained by pressing the powdered material into shape. It should be understood that any blank in the field of architectural ceramics is applicable to this invention. In an optional embodiment, the chemical composition of the brick blank includes, by mass percentage: loss on ignition: 3.5%–6.8%; SiO2: 63.8%–73.3%; Al2O3: 15.2%–20.5%; CaO: 0.2%–2.5%; MgO: 0.4%–1.8%; K2O: 2.2%–4.4%; Na2O: 2.8%–5.2%; Fe2O3: 0.2%–0.6%; TiO2: 0.1%–0.3%. For example, the chemical composition of the brick blank includes, by mass percentage: loss on ignition: 4.5%–6.8%; SiO2: 66.1%–70.5%; Al2O3: 18.2%–20.5%; CaO: 0.2%–0.5%; MgO: 0.4%–0.8%; K2O: 2.2%–4.4%; Na2O: 2.8%–5.2%; Fe2O3: 0.2%–0.6%; TiO2: 0.1%–0.3%.

[0023] Any mineral composition that causes the chemical composition of the brick blank to fall within the stated range is applicable to this invention. For example, the mineral composition of the brick blank includes, by mass percentage: 12%–16% selected white sand, 10%–16% medium-temperature sand, 1%–4% white talc powder, 5%–9% Zhou water-milled powder, 4%–6% strong plastic clay, 0%–3% raw ore sand, 6%–12% Liu water-milled powder, 8%–16% Fengsheng sodium carbonate powder, 8%–12% high-whiteness ball clay, 2%–6% Wuhua stone particles, 4%–9% Jinxin sand, 1%–3% Zhongying black clay, 0%–2% high-whiteness bentonite, and 6%–12% ball clay.

[0024] As an example, the mineral composition of the brick blank includes, by mass percentage: 15% selected white sand, 14.7% medium-temperature sand, 2.3% white talc powder, 7% Zhou water-milled powder, 6% strong plastic clay, 1% original ore sand, 9% Liu water-milled powder, 12% Fengsheng sodium quartz powder, 10.5% high-whiteness ball clay, 4.5% Wuhua stone particles, 6.5% Jinxin sand, 1.5% Zhongying black clay, 1% high-whiteness bentonite, and 9% ball clay.

[0025] Brick blanks are obtained by ball milling, spray granulation, and pressing of the brick blank minerals. The blank powder can be applied into the press mold cavity for pressing. As an example, the particle size distribution of the blank powder includes, by mass percentage: <2% residue on a 20-mesh sieve, 30%–40% residue on a 40-mesh sieve, 75%–85% residue on a 60-mesh sieve, and >92% residue on a 100-mesh sieve; the residue values ​​for each mesh size are cumulative. The moisture content of the blank powder should preferably be controlled between 7.0% and 7.6% by mass.

[0026] Dry the brick blanks. Drying can be carried out in a drying kiln. The moisture content of the dried brick blanks should be controlled within 0.2% to 0.3% by mass.

[0027] The dried brick blanks are then bisque-fired to obtain bisque-fired bricks. For example, the maximum bisque-firing temperature is 1020–1080℃, and the firing time is 30–35 minutes. The whiteness of the bisque-fired bricks can be 50–54. The coefficient of thermal expansion of the bisque-fired bricks at 20–600℃ is 8.2 × 10⁻⁶. -6 / ℃~8.9×10 -6 / ℃.

[0028] The water absorption rate of the bisque-fired body is preferably 8% to 16%. If the water absorption rate of the bisque-fired body is too high, such as when using raw body directly, the water absorption rate of the raw body is very high and uneven. When the glaze slurry is applied, the body will absorb water violently like a sponge, causing the water in the glaze slurry to be quickly absorbed into the body. Glaze particles will then quickly accumulate on the surface, resulting in uneven glaze thickness, with some areas having thick glaze and others thin, leading to a chaotic and disordered ice crack effect after firing. If the water absorption rate of the bisque-fired body is too low, such as an over-sintered low-water-absorption body, its strength and rigidity are very high. Its coefficient of thermal expansion may also change due to over-sintering (usually becoming lower), leading to stress mismatch. While the coefficient of thermal expansion of the glaze is fixed, the body becomes denser due to over-firing, reducing its coefficient of thermal expansion. This results in an excessively large stress difference (Δα) between the body and the glaze, potentially causing excessively severe and coarse cracks, or even destructive cracking instead of a beautiful network pattern, reducing the product's strength.

[0029] A surface glaze is applied to the surface of the bisque-fired body. As an example, the mineral composition of the surface glaze includes, by mass percentage: 20%–40% potassium feldspar, 20%–35% spodumene, 8%–12% washed kaolin, 10%–20% quartz, 10%–15% calcined alumina, 8%–12% zirconium silicate, 2%–10% calcite, and 1.5%–3% zinc oxide.

[0030] The surface glaze reduces its coefficient of thermal expansion by introducing spodumene and zirconium silicate. In an optional embodiment, the coefficient of thermal expansion of the surface glaze at 20–600°C is 3.2 × 10⁻⁶. -6 / ℃~4.6×10 -6 / ℃. Preferably, the coefficient of thermal expansion of the glaze at 20–600℃ is 3.2 × 10⁻⁶. -6 / ℃~4.2×10 -6 / ℃. In an optional embodiment, the chemical composition of the surface glaze includes, by mass percentage, loss on ignition: 1.2%–2.8%; Al2O3: 23.2%–28.5%; SiO2: 58.5%–62.3%; Fe2O3: 0.3%–0.6%; CaO: 1.5%–2.8%; ZnO: 1.2%–2.5%; K2O: 2.2%–3.4%; Li2O: 1.8%–3.0%; TiO2: 0.1%–0.3%; Zr2O: 4.2%–6.3%.

[0031] Water and auxiliary materials can be added to the mineral composition of the glaze to adjust it to the desired specific gravity. The auxiliary materials include sodium tripolyphosphate and sodium carboxymethyl cellulose. The sodium carboxymethyl cellulose content in the mineral composition of the glaze can be 0.1%–0.4% by mass, and the sodium tripolyphosphate content can be 0.1%–0.4% by mass. In actual production, water can be added to the glaze slurry to adjust the glaze specific gravity to the desired level.

[0032] The surface glaze can be applied by pouring glaze. Preferably, the specific gravity of the surface glaze is 1.82–1.86 g / cm³. 3 The glaze application rate is 660–720 g / m². 2 By controlling the glazing parameters within this range, the surface blemishes of the brick can be covered, and the shape of the brick can also be controlled.

[0033] Dry the bisque-fired body with the glaze applied. This helps to remove as much moisture as possible from the glaze layer. Electric kiln drying is suitable. For example, the drying temperature is 250–280℃, and the drying time is 120–240 seconds.

[0034] Ink patterns are printed onto the bisque surface after glazing. Multi-channel inkjet printing can be used to create multi-color patterns. Ink colors include blue, reddish-brown, orange, golden yellow, lemon yellow, black, and red. The decorative patterns, textures, and color effects of the inkjet prints are determined according to the design requirements.

[0035] Apply a crackle glaze to the surface of the bisque after inkjet printing the ink pattern. As an example, the mineral composition of the crackle glaze includes, by mass percentage: 5%–10% kaolin, 80%–90% high-expansion calcium-magnesium frit, 3%–6% calcined zinc oxide, 2%–8% barium carbonate, and 1%–5% strontium carbonate.

[0036] In an optional embodiment, the chemical composition of the high-expansion calcium-magnesium frit includes, by mass percentage: SiO2: 52%–64%; Al2O3: 12%–20%; CaO: 18%–35%; MgO: 2.5%–6.4%; K2O: 1.2%–3%; Na2O: 3.2%–8.6%; Fe2O3: 0.1%–0.3%; TiO2: 0.1%–0.3%. In an optional embodiment, the coefficient of thermal expansion of the high-expansion calcium-magnesium frit is 13 × 10⁻⁶ at 20–600°C. -6 / ℃~14×10 -6 / ℃.

[0037] Ice-crack glaze increases the coefficient of thermal expansion by introducing high-expansion calcium-magnesium frit, while reducing the content of alumina and silica (making the glaze softer and increasing the difference in expansion). The introduction of alkaline earth metal oxides such as barium and strontium carbonate (e.g., barium carbonate and strontium carbonate) can be used to fine-tune the shape and size of the cracks. Zinc oxide is a highly effective flux that significantly lowers the melting temperature of the glaze, resulting in a smoother, more even surface with higher gloss. It also imparts a unique, soft, milky or opaque effect (not completely opaque), making the glaze appear warmer and richer, reducing harsh glassy shine, and widening the firing range, allowing the glaze to remain stable over a wider temperature range and reducing firing defects (such as pinholes and glaze shrinkage).

[0038] The coefficient of thermal expansion of the crackle glaze is controlled at 9.2 × 10⁻⁶ at 20–600℃. -6 / ℃~10.8×10 -6 / ℃. If the coefficient of expansion of the crackle glaze is too large, the difference between the surface glaze and the crackle glaze will be too great, resulting in excessively large and dense cracks, or even causing the glaze layer to peel off; if the coefficient of expansion of the crackle glaze is too small, the difference between the surface glaze and the crackle glaze will be too small, and the cracks will not be obvious or will not crack at all.

[0039] For example, the chemical composition of the ice-crack glaze includes, by mass percentage: loss on ignition: 2.2%–3.8%; SiO2: 50.8%–60.4%; Al2O3: 10.2%–14.6%; CaO: 14.8%–18.5%; MgO: 1.5%–2.8%; K2O: 0.8%–2.2%; Na2O: 2.1%–3.9%; BaO: 1.5%–2.7%; SrO: 0.8%–1.6%; ZnO: 2.8%–5.2%.

[0040] Water and auxiliary materials can be added to the mineral composition of the crackle glaze to adjust it to the desired specific gravity. The auxiliary materials include sodium tripolyphosphate and sodium carboxymethyl cellulose. The sodium carboxymethyl cellulose content in the crackle glaze mineral composition can be 0.1%–2% by mass, and the sodium tripolyphosphate content can be 0.3%–5% by mass. In actual production, water can be added to the crackle glaze slurry to adjust it to the desired specific gravity.

[0041] The ice-crack glaze can be applied by pouring glaze. Preferably, the specific gravity of the ice-crack glaze is 1.82–1.86 g / cm³. 3 The glaze application rate is 1030–1260 g / m². 2 The specific gravity of the glaze within this range is beneficial for the uniformity of glazing. If the glaze layer is too thin, the internal stress of the glaze surface is insufficient, making it impossible to form continuous and clear crackles; only scattered small cracks will appear, or even no cracks at all. If the glaze layer is thick enough, sufficient stress accumulation can form a clear and beautiful network of crackles that runs through the glaze layer. A thick glaze layer also makes the crackles more three-dimensional, and the texture will be more prominent and beautiful.

[0042] Firing. The glaze is fired in a kiln. The maximum firing temperature for glaze is 1180–1250℃, and the firing time is 40–50 minutes. If the firing temperature is insufficient, the glaze will not fully melt, resulting in a rough, dull surface with poor or no cracking. If the firing temperature is too high, the glaze will melt excessively, becoming too fluid, leading to glaze runny, dry glaze, or deformation. Excessively high temperatures may even cause cracks that have already begun to form to re-melt.

[0043] Edge grinding, grading, and packaging.

[0044] The method for preparing ice-crack pattern porcelain tiles described in this invention produces a clear and beautiful network of ice-crack textures that penetrates the glaze layer after firing. The cracks resemble cracked ice, with overlapping layers creating a strong three-dimensional effect. This method has a short firing time and can produce tiles of any size. The surface cracks resemble cracked ice, with overlapping layers, completely replicating the artistic beauty of ice-crack patterns. Furthermore, this method significantly reduces production costs, achieving a technological breakthrough and filling a market gap.

[0045] 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 appropriate range based on the description herein, and are not intended to be limited to the specific values ​​in the examples below.

[0046] Example 1

[0047] The preparation method of ice-crack pattern porcelain tiles includes the following steps: Step 1. Press the raw material powder into brick blanks, and then fire them to obtain bisque-fired brick blanks. The chemical composition of the brick blanks includes, by mass percentage: Loss on ignition: 3.78%; SiO2: 70.45%; Al2O3: 17.08%; CaO: 1.5%; MgO: 1.35%; K2O: 2.3%; Na2O: 3.13%; Fe2O3: 0.25%; TiO2: 0.16%. The bisque-firing temperature is 1050℃, and the firing time is 32 minutes. The water absorption rate of the bisque-fired brick blanks is 13.2%, and the whiteness is 52.

[0048] Step 2. Apply a top glaze to the surface of the bisque-fired body. The mineral composition of the top glaze includes, by mass percentage: 28% potassium feldspar, 22% spodumene, 8% washed kaolin, 13% quartz, 15% calcined alumina, 8% zirconium silicate, 4% calcite, and 2% zinc oxide. The chemical composition of the top glaze includes, by mass percentage: loss on ignition: 1.8%; Al₂O₃: 24.3%; SiO₂: 59.2%; Fe₂O₃: 0.45%; CaO: 1.8%; ZnO: 1.6%; K₂O: 2.8%; Li₂O: 2.2%; TiO₂: 0.25%; ZrO₂: 5.6%. The coefficient of thermal expansion of the top glaze at 20~600℃ is 4.5×10⁻⁶. -6 / ℃. The glaze is applied by pouring. The specific gravity of the glaze is 1.85 g / cm³. 3 The glaze application rate is 680 g / m². 2 .

[0049] Step 3. Inkjet print an ink pattern onto the surface of the bisque after the surface glaze has been applied.

[0050] Step 4. Apply a crackle glaze to the bisque surface after inkjet printing the ink pattern. The mineral composition of the crackle glaze includes, by mass percentage: 8% kaolin, 82% high-expansion calcium-magnesium frit, 4% calcined zinc oxide, 4% barium carbonate, and 2% strontium carbonate. The chemical composition of the high-expansion calcium-magnesium frit includes, by mass percentage: 55.05% SiO2; 12.8% Al2O3; 23.2% CaO; 2.8% MgO; 2.1% K2O; 3.5% Na2O; 0.23% Fe2O3; and 0.32% TiO2. The coefficient of thermal expansion of the high-expansion calcium-magnesium frit is 13.8 × 10⁻⁶ at 20–600°C. -6 / ℃. The chemical composition of the ice-crack glaze includes, by mass percentage: loss on ignition: 2.4%; SiO2: 56.4%; Al2O3: 12.6%; CaO: 16.1%; MgO: 1.8%; K2O: 1.6%; Na2O: 2.8%; BaO: 1.8%; SrO: 0.8%; ZnO: 3.7%. The coefficient of thermal expansion of the ice-crack glaze in the range of 20~600℃ is 10.2×10⁻¹⁰. -6 / ℃. The ice-crack glaze is applied by pouring. The specific gravity of the ice-crack glaze is 1.84 g / cm³. 3 The glaze application rate is 1180 g / m². 2 .

[0051] Step 5. Place the bisque glaze-coated with the crackle glaze into the kiln for firing. The maximum firing temperature is 1195℃, and the firing time is 50 minutes.

[0052] Step 6. Edge grinding, grading and packaging.

[0053] Figure 1 This is a rendering of the surface of the porcelain tile from Example 1. From... Figure 1 It can be seen that the surface texture of the porcelain tile sample resembles ice cracks, with the cracks layered on top of each other, completely replicating the artistic beauty of ice crack patterns.

[0054] Example 2

[0055] The preparation method of ice-crack pattern porcelain tiles includes the following steps: Step 1. Press the raw material powder into brick blanks, and then fire them to obtain bisque-fired brick blanks. The chemical composition of the brick blanks includes, by mass percentage: Loss on ignition: 3.82%; SiO2: 70.45%; Al2O3: 17.08%; CaO: 1.5%; MgO: 1.35%; K2O: 2.3%; Na2O: 3.13%; Fe2O3: 0.21%; TiO2: 0.16%. The bisque-firing temperature is 1080℃, and the firing time is 30 minutes. The water absorption rate of the bisque-fired brick blanks is 10.5%, and the whiteness is 51.

[0056] Step 2. Apply a top glaze to the surface of the bisque-fired body. The mineral composition of the top glaze includes, by mass percentage: 24% potassium feldspar, 26% spodumene, 8% washed kaolin, 13% quartz, 15% calcined alumina, 8% zirconium silicate, 4% calcite, and 2% zinc oxide. The chemical composition of the top glaze includes, by mass percentage: loss on ignition: 2.3%; Al₂O₃: 24.2%; SiO₂: 59%; Fe₂O₃: 0.52%; CaO: 1.8%; ZnO: 1.6%; K₂O: 2.3%; Li₂O: 2.5%; TiO₂: 0.28%; ZrO₂: 5.5%. The coefficient of thermal expansion of the top glaze at 20~600℃ is 3.8×10⁻⁶. -6 / ℃. The glaze is applied by pouring. The specific gravity of the glaze is 1.86 g / cm³. 3 The glaze application rate is 670 g / m². 2 .

[0057] Step 3. Inkjet print an ink pattern onto the surface of the bisque after the surface glaze has been applied.

[0058] Step 4. Apply a crackle glaze to the bisque surface after inkjet printing the ink pattern. The mineral composition of the crackle glaze includes, by mass percentage: 8% kaolin, 80% high-expansion calcium-magnesium frit, 5% calcined zinc oxide, 4% barium carbonate, and 3% strontium carbonate. The chemical composition of the high-expansion calcium-magnesium frit includes, by mass percentage: 56.15% SiO2; 13.8% Al2O3; 21.2% CaO; 2.7% MgO; 2.2% K2O; 3.4% Na2O; 0.28% Fe2O3; and 0.27% TiO2. The coefficient of thermal expansion of the high-expansion calcium-magnesium frit is 13.2 × 10⁻⁶ at 20–600°C. -6 / ℃. The chemical composition of the ice-crack glaze includes, by mass percentage: loss on ignition: 2.4%; SiO2: 55.8%; Al2O3: 12.5%; CaO: 15.8%; MgO: 1.8%; K2O: 1.6%; Na2O: 2.8%; BaO: 1.8%; SrO: 1.1%; ZnO: 4.4%. The coefficient of thermal expansion of the ice-crack glaze at 20~600℃ is 9.8×10⁻⁶. -6 / ℃. The ice-crack glaze is applied by pouring. The specific gravity of the ice-crack glaze is 1.84 g / cm³. 3 The glaze application rate is 1080 g / m². 2 .

[0059] Step 5. Place the brick blanks, after applying the crackle glaze, into the kiln for firing. The maximum firing temperature is 1225℃, and the firing time is 40 minutes.

[0060] Step 6. Edge grinding, grading and packaging.

[0061] Figure 2 This is a rendering of the ceramic tile surface from Example 2. From... Figure 2 It can be seen that the surface texture of the porcelain tile sample resembles ice cracks, with the cracks layered on top of each other, completely replicating the artistic beauty of ice crack patterns.

[0062] Comparative Example 1 The process is essentially the same as in Example 1, with the main difference being that the surface glaze is replaced with a high coefficient of thermal expansion glaze in step 2. The mineral composition of the high coefficient of thermal expansion glaze includes, by mass percentage: 17% potassium feldspar, 23% sodium feldspar, 12% nepheline, 8% washed kaolin, 13% quartz, 15% calcined alumina, 8% zirconium silicate, and 4% calcite. The chemical composition of the high coefficient of thermal expansion glaze includes, by mass percentage: loss on ignition: 1.8%; SiO2: 55.9%; Al2O3: 25.7%; K2O: 3.5%; Na2O: 5.8%; CaO: 1.8%; ZrO2: 5.5%. The coefficient of thermal expansion of the high coefficient of thermal expansion glaze is 7.5 × 10⁻⁶ at 20–600°C. -6 / ℃. The high expansion coefficient glaze is applied by pouring. The specific gravity of the high expansion coefficient glaze is 1.84 g / cm³. 3 The glaze application rate is 670 g / m². 2 .

[0063] The high expansion coefficient of the surface glaze in this comparison is close to that of the ice crack glaze, so it cannot produce ice cracks through shrinkage.

[0064] Comparative Example 2 The composition is basically the same as in Example 1, with the main difference being that the mineral composition of the ice-crack glaze includes, by mass percentage: 15% potassium feldspar, 30% sodium feldspar, 8% washed kaolin, 6% quartz, 5% calcined alumina, 10% calcite, 12% barium carbonate, 4% strontium carbonate, 5% calcined talc, and 5% zinc oxide. The chemical composition of the ice-crack glaze includes, by mass percentage: loss on ignition: 5.7%; SiO2: 51.8%; Al2O3: 14.8%; CaO: 6.5%; MgO: 2.8%; K2O: 2.6%; Na2O: 3.8%; BaO: 5.8%; SrO: 2.1%; ZnO: 4.1%. The coefficient of thermal expansion of the ice-crack glaze at 20~600℃ is 6.5×10⁻⁶. -6 / ℃. The ice-crack glaze is applied by pouring. The specific gravity of the ice-crack glaze is 1.84 g / cm³. 3 The glaze application rate is 1080 g / m². 2 .

[0065] The coefficient of thermal expansion of the ice-crack glaze in this comparison is too small, and the difference between it and the surface glaze is small, so it cannot produce ice cracks through shrinkage.

[0066] Comparative Example 3 The results are basically the same as in Example 1, except that the specific gravity of the crackle glaze is 1.83 g / cm³. 3 Glazing amount is 600 g / m 2 .

[0067] The proportion of crackle glaze applied is too little, the glaze layer is too thin, and the internal stress of the glaze surface is insufficient, so it cannot form a continuous and clear crackle, and only sporadic small cracks appear, or even no cracks at all.

[0068] Comparative Example 4 It is basically the same as Example 1, except that the water absorption rate of the bisque is 2.5%.

[0069] The bisque fired in this proportion has too low a water absorption rate, making it difficult for the glaze to be absorbed and resulting in a glaze layer that is too thin. As a result, the glaze surface is dry and dull after firing, and it is impossible to form a full and lustrous ice crack effect. In some cases, the bisque may even have exposed clay.

[0070] Comparative Example 5 It is basically the same as Example 1, except that the second firing temperature is 1120°C.

[0071] The second firing temperature of this comparative example is too low, which can easily lead to the glaze not melting completely, and the glaze surface cannot form a clear and continuous network crack pattern.

[0072] Comparative Example 6 It is basically the same as Example 1, except that the second firing temperature is 1280°C.

[0073] The second firing temperature of this comparative example was too high, resulting in no ice crackle effect on the glaze.

[0074] Comparative Example 7 It is basically the same as Example 1, except that the surface glaze is applied directly to the surface of the brick blank.

[0075] The blank in this comparative example was not bisque fired, resulting in an uneven glaze after firing, with the effect as follows: Figure 3 As shown.

[0076] Comparative Example 8 The composition is basically the same as in Example 1, with the main difference being that the mineral composition of the ice-crack glaze includes, by mass percentage: 10% potassium feldspar, 26% sodium feldspar, 8% washed kaolin, 6% quartz, 15% corundum, 16% calcite, 5% barium carbonate, 4% strontium carbonate, 5% calcined talc, and 5% zinc oxide. The chemical composition of the ice-crack glaze includes, by mass percentage: Loss on ignition: 4.7%; SiO2: 48.8%; Al2O3: 19.8%; CaO: 6.5%; MgO: 2.8%; K2O: 1.8%; Na2O: 3.3%; BaO: 5.8%; SrO: 2.1%; ZnO: 4.4%. The coefficient of thermal expansion of the ice-crack glaze at 20~600℃ is 8.5×10⁻⁶. -6 / ℃.

[0077] Although the crackle glaze in this comparison has a large coefficient of thermal expansion, it also has high viscosity and surface tension at high temperatures. After firing, the cracks bulge upwards, creating an effect similar to... Figure 4 As shown.

Claims

1. A method for preparing ice-crack pattern porcelain tiles, characterized in that, The preparation method includes the following steps: The blank is fired in the first firing to obtain a bisque blank; Apply a surface glaze to the bisque-fired clay; Ink patterns are printed on the bisque after the surface glaze has been applied; Apply ice-crack glaze to the bisque after inkjet printing the ink pattern; The unglazed body with the ice-crack glaze is then fired a second time to obtain ice-crack porcelain tiles.

2. The preparation method according to claim 1, characterized in that, The water absorption rate of the bisque-fired blank is 8% to 16%.

3. The preparation method according to claim 1 or 2, characterized in that, The mineral composition of the glaze includes, by mass percentage: 20%–40% potassium feldspar, 20%–35% spodumene, 8%–12% washed kaolin, 10%–20% quartz, 10%–15% calcined alumina, 8%–12% zirconium silicate, 2%–10% calcite, and 1.5%–3% zinc oxide. Preferably, the chemical composition of the glaze includes, by mass percentage: loss on ignition: 1.2%–2.8%; Al₂O₃: 23.2%–28.5%; SiO₂: 58.5%–62.3%; Fe₂O₃: 0.3%–0.6%; CaO: 1.5%–2.8%; ZnO: 1.2%–2.5%; K₂O: 2.2%–3.4%; Li₂O: 1.8%–3.0%; TiO₂: 0.1%–0.3%; ZrO₂: 4.2%–6.3%.

4. The preparation method according to any one of claims 1 to 3, characterized in that, The coefficient of thermal expansion of the glaze is controlled at 3.2 × 10⁻⁶ at 20–600 °C. -6 / ℃~4.6×10 -6 / ℃.

5. The preparation method according to any one of claims 1 to 4, characterized in that, The surface glaze is applied by pouring glaze; preferably, the specific gravity of the surface glaze is 1.82–1.86 g / cm³. 3 The glaze application rate is 660–720 g / m². 2 .

6. The preparation method according to any one of claims 1 to 5, characterized in that, The mineral composition of the ice-crack glaze includes, by mass percentage: 5%–10% kaolin, 80%–90% high-expansion calcium-magnesium frit, 3%–6% calcined zinc oxide, 2%–8% barium carbonate, and 1%–5% strontium carbonate; wherein, the chemical composition of the high-expansion calcium-magnesium frit includes, by mass percentage: SiO2: 52%–64%; Al2O3: 12%–20%; CaO: 18%–35%; MgO: 2.5%–6.4%; K2O: 1.2%–3%; Na2O: 3.2%–8.6%; Fe2O3: 0.1%–0.3%; TiO2: 0.1%–0.3%.

7. The preparation method according to any one of claims 1 to 6, characterized in that, The chemical composition of the ice-crack glaze includes, by mass percentage: loss on ignition: 2.2%–3.8%; SiO2: 50.8%–60.4%; Al2O3: 10.2%–14.6%; CaO: 14.8%–18.5%; MgO: 1.5%–2.8%; K2O: 0.8%–2.2%; Na2O: 2.1%–3.9%; BaO: 1.5%–2.7%; SrO: 0.8%–1.6%; ZnO: 2.8%–5.2%.

8. The preparation method according to any one of claims 1 to 7, characterized in that, The coefficient of thermal expansion of the crackle glaze is controlled at 9.2 × 10⁻⁶ at 20–600℃. -6 / ℃~10.8 ×10 -6 / ℃.

9. The preparation method according to any one of claims 1 to 8, characterized in that, The ice-crack glaze is applied by pouring glaze; preferably, the specific gravity of the ice-crack glaze is 1.82–1.86 g / cm³. 3 The glaze application rate is 1030–1260 g / m². 2 .

10. The preparation method according to any one of claims 1 to 9, characterized in that, The second firing temperature is 1180–1250℃, and the firing time is 40–50 minutes.

11. The preparation method according to any one of claims 1 to 10, characterized in that, The firing temperature for the first firing is 1020–1080℃, and the firing time is 30–35 minutes.

12. The preparation method according to any one of claims 1 to 11, characterized in that, The chemical composition of the brick blank includes, by mass percentage: loss on ignition: 3.5%–6.8%; SiO2: 63.8%–73.3%; Al2O3: 15.2%–20.5%; CaO: 0.2%–2.5%; MgO: 0.4%–1.8%; K2O: 2.2%–4.4%; Na2O: 2.8%–5.2%; Fe2O3: 0.2%–0.6%; TiO2: 0.1%–0.3%.

13. A type of ice-crack pattern porcelain tile, characterized in that, The ice-crack pattern porcelain tile is obtained by the preparation method according to any one of claims 1 to 12.

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