Inkjet crystal flower ice crack ceramic and preparation method thereof

By introducing the base glaze between the low-aluminum blank body and the high-expansion crack glaze layer, the difference in thermal expansion coefficient is controlled, and inkjet printing technology is used to prepare inkjet crystal flower ice crack ceramics at low temperatures, which solves the defects in the preparation process in the existing technology, and realizes low-cost batch production and colorful ice crack ceramics with ice crack ceramics with rich and colorful patterns.

CN120349176APending Publication Date: 2025-07-22GAOAN MONALISA NEW MATERIAL CO LTD +1
View PDF 0 Cites 0 Cited by

Patent Information

Application Number
CN202510487280.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-18
Publication Date
2025-07-22

AI Technical Summary

Technical Problem

During the preparation process, existing ice-crack ceramic products are prone to defects such as large cracks, glazed peeling and brick-shaped turtle. High temperature firing leads to high energy consumption, making it difficult to achieve low-cost mass production.

Method used

The base glaze is introduced between the low-aluminum body and the high-expansion crack glaze layer. By controlling the difference in thermal expansion coefficient, inkjet printing technology is used to prepare inkjet crystal flower ice crack ceramics at low temperatures, using specific composition base glaze and high-expansion crack glaze materials.

Benefits of technology

Under the low-temperature fast firing system, ice crack ceramics with rich and colorful patterns were steadily prepared, avoiding defects such as large cracks, glazed peeling and brick-shaped turtle-shaped, and achieving low-cost mass production.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN120349176A_ABST
    Figure CN120349176A_ABST
Patent Text Reader

Abstract

The invention relates to inkjet crystal flower ice crack ceramic and a preparation method thereof, and belongs to the technical field of ceramic production and manufacturing. The preparation method comprises the following steps: applying ground glaze on the surface of a low-aluminum green body; carrying out ink-jet printing on the surface of the low-aluminum green body after the ground glaze is applied with a decorative pattern; applying high-expansion cracked glaze on the surface of the green body subjected to inkjet printing of the decorative pattern; and firing the green body applied with the high-expansion crack glaze to obtain the inkjet crystal flower ice crack ceramic. According to the invention, the ground glaze is introduced between the low-aluminum green body layer and the high-expansion cracked glaze layer, so that the defects of large cracks, glaze stripping, tile shape deviation and the like on the glaze surface can be avoided, and stable, low-cost and batch preparation of the inkjet crystal flower ice crack ceramic under a low-temperature fast firing system of building ceramic is realized.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to an inkjet crystal flower ice crack ceramic and a preparation method thereof, belonging to the technical field of ceramic production and manufacturing. Background Art

[0002] Cracking is a common phenomenon in architectural ceramics. During molding, the clay extends in a certain direction, affecting the molecular arrangement, or the different expansion coefficients of the clay and glaze lead to a large shrinkage rate of the glaze layer during cooling after firing, which may cause cracks in the ceramic glaze.

[0003] Ice crack glazed tiles have a three-dimensional effect and high ornamental value because their patterns are like cracked ice, and the visual effect is like crystal flowers stacked in the glaze layer. The current ice crack ceramic products have the following characteristics: more oblique cracks, circular closed cracks, overlapping cracks; the cracks are located in the body and are inclined; the glaze surface has dense microbubbles with a diameter of about 0.05 to 0.1 mm; due to the influence of oblique cracks and microbubbles on light scattering, the cracks on the glaze surface are white.

[0004] The preparation of ice crack glazed tiles has high requirements for the body and glaze, and the firing temperature and firing atmosphere need to be strictly controlled in order to stably produce ice crack ceramics in batches. Otherwise, defects such as large cracks, glaze peeling, and delamination are likely to occur. In addition, the firing temperature of ice crack glazed tiles is relatively high, basically above 1250℃, which consumes a lot of energy. Summary of the invention

[0005] In view of the above problems, the present invention provides an inkjet crystal flower ice crack ceramic and a preparation method thereof. By introducing a bottom glaze between the low-aluminum body layer and the high-expansion crack glaze layer, defects such as large cracks, glaze peeling, and brick-shaped turtles on the glaze surface can be avoided, and the inkjet crystal flower ice crack ceramic can be prepared stably, at low cost, and in batches under the low-temperature fast-firing system of building ceramics.

[0006] In a first aspect, the present invention provides a method for preparing inkjet crystal flower ice crack ceramics. The preparation method comprises the following steps: applying a base glaze on the surface of a low-aluminum blank; inkjet printing a decorative pattern on the surface of the blank after the base glaze is applied; applying a high expansion crack glaze on the surface of the blank after the decorative pattern is inkjet printed; and sintering the blank after the high expansion crack glaze is applied to obtain the inkjet crystal flower ice crack ceramics.

[0007] Preferably, the aluminum mass content of the low-aluminum billet is 12% to 18%; preferably, the chemical composition of the low-aluminum billet includes, in mass percentage, IL: 1% to 3%, SiO2: 65% to 75%, Al2O3: 12% to 18%, Fe2O3: 0.5% to 1.5%, TiO2: 0.1% to 0.2%, CaO: 0.2% to 0.5%, MgO: 0.1% to 0.5%, K2O: 2% to 6%, Na2O: 1% to 5%.

[0008] Preferably, the mineral composition of the low-aluminum green body includes: by mass percentage, clay: 15% - 25%, potassium / sodium feldspar: 35% - 60%, potassium sand: 10% - 30%, calcined talc: 0.5% - 5%, talc: 1% - 5%.

[0009] Preferably, the mineral composition of the base glaze includes: by mass percentage, high-aluminum ball clay: 75% - 85%, α-aluminum oxide: 5% - 15%, calcined talc: 1% - 10%, potassium / sodium feldspar: 1% - 10%; preferably, the chemical composition of the base glaze includes: by mass percentage, IL: 5% - 13%, SiO2: 45% - 55%, Al2O3: 25% - 35%, Fe2O3: 0.5% - 1.5%, TiO2: 0.1% - 0.2%, CaO: 0.2% - 0.5%, MgO: 0.1% - 5%, K2O: 0.5% - 2%, Na2O: 0.2% - 2.5%.

[0010] Preferably, the application method of the base glaze is spraying; preferably, the specific gravity of the base glaze is 1.44 - 1.46 g / cm 3 , and the glaze application amount is 500 - 700 g / m 2 .

[0011] Preferably, the mineral composition of the high-expansion crack glaze includes: by mass percentage, clay: 3% - 15%, high-expansion frit: 40% - 50%, high-sodium frit: 10% - 20%, high-calcium frit: 5% - 15%, high-boron frit: 1% - 10%, lead frit: 1% - 5%; preferably, the chemical composition of the high-expansion crack glaze includes: by mass percentage, IL: 0.1% - 0.5%, SiO2: 55% - 65%, Al2O3: 5% - 15%, Fe2O3: 0.1% - 0.5%, TiO2: 0.1% - 0.2%, CaO: 5% - 15%, MgO: 0.1% - 0.5%, K2O: 0.5% - 2%, Na2O: 15% - 25%, PbO: 1% - 5%, B2O3: 1% - 5%.

[0012] Preferably, the chemical composition of the high-expansion frit includes: by mass percentage, SiO2: 55% - 70%, Al2O3: 5% - 15%, Fe2O3: 0.1% - 0.5%, TiO2: 0.1% - 0.2%, CaO: 5% - 15%, MgO: 0.1% - 0.5%, K2O: 0.5% - 2%, Na2O: 10% - 20%; preferably, the mineral composition of the high-expansion frit includes: by mass percentage, clay: 3% - 15%, albite: 50% - 70%, nepheline: 5% - 15%, calcite: 15% - 35%, talc: 1% - 6%.

[0013] Preferably, the chemical composition of the high-sodium frit includes: by mass percentage, SiO2: 55% - 65%, Al2O3: 10% - 15%, Fe2O3: 0.3% - 1.5%, TiO2: 0.2% - 0.5%, CaO: 5% - 15%, MgO: 0.5% - 3%, K2O: 1% - 5%, Na2O: 15% - 25%; Preferably, the mineral composition of the high-sodium frit includes: by mass percentage, clay: 5% - 10%, potassium / sodium feldspar: 55% - 75%, nepheline: 3% - 10%, limestone: 15% - 25%, talc: 0.5% - 3%.

[0014] Preferably, the chemical composition of the high-calcium frit includes: by mass percentage, SiO2: 65% - 75%, Al2O3: 5% - 15%, Fe2O3: 0.1% - 0.5%, TiO2: 0.1% - 0.3%, CaO: 15% - 20%, MgO: 0.5% - 5%, K2O: 1% - 5%, Na2O: 3% - 10%; Preferably, the mineral composition of the high-calcium frit includes: by mass percentage, clay: 5% - 15%, potassium / sodium feldspar: 10% - 30%, nepheline: 5% - 15%, limestone: 35% - 45%, calcite: 30% - 40%, talc: 0.5% - 5%.

[0015] Preferably, the chemical composition of the high-boron frit includes: by mass percentage, SiO2: 40% - 50%, Al2O3: 1% - 5%, Fe2O3: 0.1% - 1%, TiO2: 0.01% - 1%, CaO: 10% - 20%, MgO: 0.1% - 1%, K2O: 0.1% - 1%, Na2O: 5% - 15%, B2O3: 10% - 30%; Preferably, the mineral composition of the high-boron frit includes: by mass percentage, borax: 50% - 70%, quartz sand: 15% - 25%, limestone: 20% - 30%, albite: 5% - 10%.

[0016] Preferably, the chemical composition of the lead frit includes: by mass percentage, SiO2: 35% - 45%, Al2O3: 3% - 8%, Fe2O3: 0.1% - 1%, TiO2: 0.01% - 0.1%, CaO: 0.1% - 2.5%, MgO: 0.1% - 0.5%, K2O: 1% - 5%, Na2O: 2% - 10%, PbO: 25% - 35%, B2O3: 5% - 15%; Preferably, the mineral composition of the lead frit includes: by mass percentage, cerussite: 20% - 40%, albite: 10% - 20%, quartz sand: 35% - 45%, borax: 25% - 35%.

[0017] Preferably, the high-expansion crack glaze is applied by spraying; preferably, the specific gravity of the high-expansion crack glaze is 1.65-1.67 g / cm 3 , and the glaze application amount is 2000-2500 g / m 2 .

[0018] Preferably, the maximum firing temperature is 1140-1180 °C, and the firing cycle is 40-50 minutes.

[0019] In a second aspect, the present invention provides an inkjet crystal flower crack ceramic. The inkjet crystal flower crack is obtained according to the preparation method described in any one of the above. Description of the Drawings

[0020] Figure 1 It is the brick surface effect diagram of Example 1. Detailed Embodiments

[0021] The present invention is further illustrated by the following embodiments. It should be understood that the following embodiments are only used to illustrate the present invention, rather than limiting the present invention. In the case where the present invention does not make specific descriptions, the percentage contents refer to mass percentage contents. The preparation method of the inkjet crystal flower crack ceramic described in the present invention is exemplarily described below.

[0022] Prepare a low-aluminum green body. The aluminum mass content of the low-aluminum green body can be 12%-18%. In some embodiments, the chemical composition of the low-aluminum green body includes: by mass percentage, IL: 1%-3%, SiO2: 65%-75%, Al2O3: 12%-18%, Fe2O3: 0.5%-1.5%, TiO2: 0.1%-0.2%, CaO: 0.2%-0.5%, MgO: 0.1%-0.5%, K2O: 2%-6%, Na2O: 1%-5%. By reducing the aluminum content of the green body, rapid firing can be promoted, which is suitable for controlling the difference in thermal expansion coefficients between the bottom glaze and the high-expansion crack glaze, and is conducive to presenting the crack effect.

[0023] It should be understood that any mineral formula that can obtain the above chemical composition of the low-aluminum green body is applicable to the present invention. For example, the mineral composition of the low-aluminum green body includes: by mass percentage, clay: 15%-25%, potassium / sodium feldspar: 35%-60%, potassium sand: 10%-30%, calcined talc: 0.5%-5%, talc: 1%-5%. As a preference, the mineral composition of the green body includes: by mass percentage, clay: 15%-25%, potassium / sodium feldspar: 40%-60%, potassium sand: 20%-30%, calcined talc: 0.5%-5%, (raw ore) talc: 1%-5%.

[0024] Clays (such as kaolin), potassium / sodium feldspar, calcined talc, talc, and nepheline, calcite, limestone, potassium sand, borax, quartz sand, etc. used hereinafter are all common raw materials in the field of building ceramics and can be obtained through commercial channels.

[0025] Including but not limited to, the chemical composition of the potassium / sodium feldspar includes: by mass percentage, IL: 0% - 3%, SiO2: 65% - 75%, Al2O3: 12% - 18%, Fe2O3: 0.5% - 1.5%, TiO2: 0.1% - 0.2%, CaO: 0.2% - 0.5%, MgO: 0.1% - 0.5%, K2O: 2% - 6%, Na2O: 1% - 5%. For example, the fineness of the potassium / sodium feldspar is less than 250 mesh.

[0026] Weigh each raw material according to the mineral composition of the low-aluminum green body, add water to the raw materials for ball milling to obtain the green body slurry. The fineness of the slurry can be controlled such that the residue on a 250-mesh sieve is within 0.8 - 1.0 wt%. The ball milling speed and time can be selected as needed. For example, the ball milling time can be 10 - 15 h. Screen and remove iron from the ball-milled slurry, and then spray granulate to obtain the green body powder.

[0027] Press the green body powder into shape to obtain a low-aluminum green body. The forming method includes but is not limited to dry pressing. The expansion coefficient of the low-aluminum green body at 20°C - 600°C can be 8.5×10 -6 / °C - 9.5×10 -6 / °C.

[0028] Dry the low-aluminum green body. Drying can be carried out in a drying kiln. The drying process is a conventional process in the field of building ceramics.

[0029] Apply a base glaze on the surface of the dried green body. The mineral composition of the base glaze includes: by mass percentage, high-aluminum ball clay: 75% - 85%, α-aluminum oxide: 5% - 15%, calcined talc: 1% - 10%, potassium / sodium feldspar: 1% - 10%. By adding a base glaze as a buffer layer between the low-aluminum green body and the high-expansion crack glaze layer, the matching problem between the low-aluminum green body and the high-expansion crack glaze can be solved.

[0030] Use high-aluminum ball clay commonly used in the art. For example, the chemical composition of the high-aluminum ball clay includes: by mass percentage, IL: 5% - 13%, SiO2: 45% - 55%, Al2O3: 25% - 35%, Fe2O3: 0.5% - 1.5%, TiO2: 0.1% - 0.2%, CaO: 0.2% - 0.5%, MgO: 0.1% - 0.5%, K2O: 0.5% - 2%, Na2O: 0.2% - 0.5%. The fineness of the high-aluminum ball clay can be less than 250 mesh.

[0031] Weigh each raw material according to the mineral composition of the base glaze, add water and additives to the raw materials, ball mill them, and remove iron by sieving to obtain the base glaze slurry. The ball mill speed and ball mill time can be selected as needed. For example, the ball mill time can be 5 to 10 hours. The additives include, but are not limited to, sodium carboxymethylcellulose and / or sodium tripolyphosphate. The dosage of the additives can be 0.1% to 0.6% of the total mass of the base glaze mineral composition. The fineness of the slurry can be controlled such that the residue on a 250-mesh sieve is within 0.4 to 0.6 wt%. When in use, water can be added to the base glaze slurry to adjust to obtain the desired glaze slurry specific gravity.

[0032] In some embodiments, the chemical composition of the base glaze includes: by mass percentage, IL: 5% to 13%, SiO2: 45% to 55%, Al2O3: 25% to 35%, Fe2O3: 0.5% to 1.5%, TiO2: 0.1% to 0.2%, CaO: 0.2% to 0.5%, MgO: 0.1% to 5%, K2O: 0.5% to 2%, Na2O: 0.2% to 2.5%.

[0033] The thermal expansion coefficient of the base glaze at 20°C to 600°C can be 4.5×10 -6 / °C to 5.5×10 -6 / °C.

[0034] The application method of the base glaze can be spraying glaze. For example, the specific gravity of the base glaze is 1.44 to 1.46 g / cm 3 , and the glaze application amount is 500 to 700 g / m 2 . Controlling the specific gravity and glaze application amount of the base glaze within the above ranges is conducive to forming the ice crack crystal flower effect. If the specific gravity and glaze application amount of the base glaze are too low, it will result in a weak sense of hierarchy of the ice cracks and the brick shape being warped. If the specific gravity and glaze application amount of the base glaze are too high, it will cause the brick shape to be tortoise-shaped and even the glaze layer to fall off later.

[0035] Dry the green body after applying the base glaze. For example, it can be dried in a drying kiln.

[0036] Inkjet print an ink pattern on the surface of the dried green body after applying the base glaze. The texture and color of the inkjet printed ink pattern can be adaptively changed as needed. Through the inkjet process, an ice crack crystal flower effect with rich and colorful patterns can be obtained.

[0037] Apply a high-expansion crack glaze on the surface of the green body after inkjet printing the pattern. The mineral composition of the high-expansion crack glaze includes: by mass percentage, clay: 3% - 15%, high-expansion frit: 40% - 50%, high-sodium frit: 10% - 20%, high-calcium frit: 5% - 15%, high-boron frit: 1% - 10%, lead frit: 1% - 5%. The high-expansion crack glaze uses high-expansion frit, high-sodium frit, and high-calcium frit to increase the expansion coefficient, and uses high-boron frit and lead frit as composite fluxes, achieving the effect of crystal flower ice cracks even with a low-aluminum green body under a low-cost and fast-firing system.

[0038] The chemical composition of the high-expansion frit may include: by mass percentage, SiO2: 55% - 70%, Al2O3: 5% - 15%, Fe2O3: 0.1% - 0.5%, TiO2: 0.1% - 0.2%, CaO: 5% - 15%, MgO: 0.1% - 0.5%, K2O: 0.5% - 2%, Na2O: 10% - 20%. The thermal expansion coefficient of the high-expansion frit at 20°C - 800°C may be 10.5×10 -6 / °C - 12.5×10 -6 / °C.

[0039] It should be understood that any mineral formula that makes the chemical composition of the high-expansion frit fall within the above range is applicable to the present invention. For example, the mineral composition of the high-expansion frit includes: by mass percentage, clay: 3% - 15%, albite: 50% - 70%, nepheline: 5% - 15%, calcite: 15% - 35%, talc: 1% - 6%. Weigh each raw material according to the mineral composition of the high-expansion frit, mix the raw materials evenly, melt them at 1250°C - 1350°C for 5 - 12 hours to obtain a melt, and then water-quench and crush the melt to obtain the high-expansion frit. The fineness of the high-expansion frit may be below 4 mesh.

[0040] The chemical composition of the high-sodium frit may include: by mass percentage, SiO2: 55% - 65%, Al2O3: 10% - 15%, Fe2O3: 0.3% - 1.5%, TiO2: 0.2% - 0.5%, CaO: 5% - 15%, MgO: 0.5% - 3%, K2O: 1% - 5%, Na2O: 15% - 25%.

[0041] It should be understood that any mineral formula that makes the chemical composition of the high-sodium frit fall within the above range is applicable to the present invention. For example, the mineral composition of the high-sodium frit includes: by mass percentage, clay: 5% - 10%, potassium / sodium feldspar: 55% - 75%, nepheline: 3% - 10%, limestone: 15% - 25%, talc: 0.5% - 3%. Weigh each raw material according to the mineral composition of the high-sodium frit, mix the raw materials evenly, and then melt them at 1250°C - 1350°C for 5 - 12 hours to obtain a melt. Quench the melt with water and then crush it to obtain the high-sodium frit.

[0042] The chemical composition of the high-calcium frit may include: by mass percentage, SiO2: 65% - 75%, Al2O3: 5% - 15%, Fe2O3: 0.1% - 0.5%, TiO2: 0.1% - 0.3%, CaO: 15% - 20%, MgO: 0.5% - 5%, K2O: 1% - 5%, Na2O: 3% - 10%.

[0043] It should be understood that any mineral formula that makes the chemical composition of the high-calcium frit fall within the above range is applicable to the present invention. For example, the mineral composition of the high-calcium frit includes: by mass percentage, clay: 5% - 15%, potassium / sodium feldspar: 10% - 30%, nepheline: 5% - 15%, limestone: 35% - 45%, calcite: 30% - 40%, talc: 0.5% - 5%. Weigh each raw material according to the mineral composition of the high-calcium frit, mix the raw materials evenly, and then melt them at 1200°C - 1300°C for 5 - 12 hours to obtain a melt. Quench the melt with water and then crush it to obtain the high-calcium frit.

[0044] The chemical composition of the high-boron frit may include: by mass percentage, SiO2: 40% - 50%, Al2O3: 1% - 5%, Fe2O3: 0.1% - 1%, TiO2: 0.01% - 1%, CaO: 10% - 20%, MgO: 0.1% - 1%, K2O: 0.1% - 1%, Na2O: 5% - 15%, B2O3: 10% - 30%.

[0045] It should be understood that any mineral formula that makes the chemical composition of the high-boron frit fall within the above range is applicable to the present invention. The mineral composition of the high-boron frit includes: by mass percentage, borax: 50% - 70%, quartz sand: 15% - 25%, limestone: 20% - 30%, albite: 5% - 10%. Weigh each raw material according to the mineral composition of the high-boron frit, mix the raw materials evenly, and then melt them at 1150°C - 1250°C for 5 - 12 hours to obtain a melt. Quench the melt with water and then crush it to obtain the high-boron frit.

[0046] The chemical composition of the lead frit may include: by mass percentage, SiO2: 35% - 45%, Al2O3: 3% - 8%, Fe2O3: 0.1% - 1%, TiO2: 0.01% - 0.1%, CaO: 0.1% - 2.5%, MgO: 0.1% - 0.5%, K2O: 1% - 5%, Na2O: 2% - 10%, PbO: 25% - 35%, B2O3: 5% - 15%.

[0047] It should be understood that any mineral formula that makes the chemical composition of the lead frit fall within the above range is applicable to the present invention. For example, the mineral composition of the lead frit includes: by mass percentage, cerussite: 20% - 40%, albite: 10% - 20%, quartz sand: 35% - 45%, borax: 25% - 35%. Weigh each raw material according to the mineral composition of the lead frit, mix the raw materials evenly, and then melt them at 1150°C - 1250°C for 5 - 12 hours to obtain a melt. Quench the melt with water and then crush it to obtain the lead frit.

[0048] Weigh each raw material according to the mineral composition of the high-expansion crack glaze, add water and additives to the raw materials for ball milling, and remove iron by sieving to obtain the high-expansion crack glaze slurry. The ball milling speed and time can be selected as needed. For example, the ball milling time can be 4 - 6h. The additives include but are not limited to sodium carboxymethylcellulose and / or sodium tripolyphosphate. The usage amount of the additives can be 0.1% - 0.6% of the total mass of the mineral composition of the high-expansion crack glaze. The fineness of the slurry can be controlled such that the residue on a 250-mesh sieve is within 3.8 - 4.0 wt%. When in use, water can be added to the glaze slurry of the high-expansion crack glaze to adjust the specific gravity of the required glaze slurry.

[0049] In some embodiments, the chemical composition of the high-expansion crack glaze includes: by mass percentage, IL: 0.1% - 0.5%, SiO2: 55% - 65%, Al2O3: 5% - 15%, Fe2O3: 0.1% - 0.5%, TiO2: 0.1% - 0.2%, CaO: 5% - 15%, MgO: 0.1% - 0.5%, K2O: 0.5% - 2%, Na2O: 15% - 25%, PbO: 1% - 5%, B2O3: 1% - 5%. The high-expansion crack glaze adopts a Pb-B-Na-Ca-Si-Al composite flux system to achieve low-temperature and rapid firing.

[0050] The thermal expansion coefficient of the high-expansion crack glaze at 20°C - 600°C is 13×10 -6 / °C - 14×10 -6 / °C.

[0051] The application method of the high-expansion crack glaze can be spraying. For example, the specific gravity of the high-expansion crack glaze is 1.65 - 1.67 g / cm 3, the glaze application amount is 2000 - 2500 g / m 2 . By controlling the specific gravity and glaze application amount of the high-expansion crack glaze within the above ranges, the ice crack crystal flower effect can be achieved. If the specific gravity and glaze application amount of the high-expansion crack glaze are too low, the ice crack layering will not be strong enough. If the specific gravity and glaze application amount of the high-expansion crack glaze are too high, glaze bleeding will occur at the brick edges.

[0052] Fire the green body after applying the high-expansion crack glaze. Firing can be carried out in a roller hearth kiln. For example, the maximum firing temperature is 1140 - 1180 °C, and the firing cycle is 40 - 50 min.

[0053] Sort and pack.

[0054] In summary, different from the prior art that uses high-aluminum green bodies to increase the difference in thermal expansion coefficients between the green body and the high-expansion crack glaze to form ice cracks, the present invention introduces an underglaze with a specific composition between the low-aluminum green body and the high-expansion crack glaze, and the ice crack effect can be achieved without using high-aluminum green bodies. Defects such as large cracks, glaze peeling, and uneven brick shape can be avoided, and low-cost inkjet crystal flower ice crack ceramic products with rich and colorful patterns can be obtained under the conditions of low aluminum content in the green body and rapid firing.

[0055] The following further lists embodiments to illustrate the present invention in detail. It should also be understood that the following embodiments are only used to further illustrate the present invention and cannot be construed as limiting the protection scope of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the above content of the present invention all fall within the protection scope of the present invention. The specific process parameters and the like in the following examples are also only an example within a suitable range, that is, those skilled in the art can make selections within a suitable range through the description in this article, rather than being limited to the specific values in the following examples.

[0056] Example 1

[0057] The preparation method of the inkjet crystal flower ice crack ceramic includes the following steps:

[0058] Step 1. Prepare a low-aluminum green body. The mineral composition of the low-aluminum green body includes: by mass percentage, clay: 20%, potassium feldspar: 30%, albite: 20%, potassium sand: 26%, calcined talc: 2%, talc: 2%. The chemical composition of the low-aluminum green body includes: by mass percentage, IL: 2.5%, SiO2: 73%, Al2O3: 14.5%, Fe2O3: 0.8%, TiO2: 0.15%, CaO: 0.4%, MgO: 0.35%, K2O: 5.1%, Na2O: 3.2%.

[0059] Step 2. Dry the low-aluminum green body.

[0060] Step 3. Apply a base glaze on the surface of the dried low-aluminum green body. The mineral composition of the base glaze includes: by mass percentage, high-aluminum ball clay: 80%, α-aluminum oxide: 10%, calcined talc: 5%, potassium feldspar: 5%. The chemical composition of the base glaze includes: by mass percentage, IL: 11.5%, SiO2: 48.85%, Al2O3: 34.5%, Fe2O3: 0.6%, TiO2: 0.15%, CaO: 0.5%, MgO: 1.5%, K2O: 1.5%, Na2O: 0.9%. The thermal expansion coefficient of the base glaze at 20°C to 600°C is 4.8×10 -6 / °C. The application method of the base glaze is spraying. The specific gravity of the base glaze is 1.45 g / cm 3 , and the glaze application amount is 600 g / m 2 .

[0061] Step 4. Dry the green body after applying the base glaze.

[0062] Step 5. Inkjet print a common ink pattern on the surface of the dried green body after applying the base glaze.

[0063] Step 6. Apply a high-expansion crack glaze on the surface of the green body after inkjet printing the ordinary ink pattern. The mineral composition of the high-expansion crack glaze includes: by mass percentage, clay: 10%, high-expansion frit: 48%, high-sodium frit: 18%, high-calcium frit: 13%, high-boron frit: 8%, lead frit: 3%. The chemical composition of the high-expansion frit includes: by mass percentage, SiO2: 64.55%, Al2O3: 7.76%, Fe2O3: 0.1%, TiO2: 0.1%, CaO: 8.54%, MgO: 0.1%, K2O: 2%, Na2O: 16.85%. The chemical composition of the high-sodium frit includes: by mass percentage, SiO2: 59.03%, Al2O3: 12.32%, Fe2O3: 0.3%, TiO2: 0.3%, CaO: 6.19%, MgO: 0.58%, K2O: 2.61%, Na2O: 18.67%. The chemical composition of the high-calcium frit includes: by mass percentage, SiO2: 68%, Al2O3: 8%, Fe2O3: 0.2%, TiO2: 0.3%, CaO: 15%, MgO: 1.5%, K2O: 2%, Na2O: 5%. The chemical composition of the high-boron frit includes: by mass percentage, SiO2: 44.57%, Al2O3: 2.27%, Fe2O3: 0.52%, TiO2: 0.01%, CaO: 16.96%, MgO: 0.1%, K2O: 0.16%, Na2O: 10.97%, B2O3: 24.44%. The chemical composition of the lead frit includes: by mass percentage, SiO2: 41.49%, Al2O3: 7.04%, Fe2O3: 0.15%, TiO2: 0.03%, CaO: 0.9%, MgO: 0.11%, K2O: 1.74%, Na2O: 6.47%, PbO: 31.25%, B2O3: 10.82%. The chemical composition of the high-expansion crack glaze includes: by mass percentage, IL: 0.4%, SiO2: 55.9%, Al2O3: 10.6%, Fe2O3: 0.5%, TiO2: 0.2%, CaO: 6%, MgO: 0.4%, K2O: 2%, Na2O: 17%, PbO: 4%, B2O3: 3%. The coefficient of thermal expansion of the high-expansion crack glaze at 20 °C to 600 °C is 13.0×10 -6 / °C. The application method of the high-expansion crack glaze is spraying. The specific gravity of the high-expansion crack glaze is 1.66 g / cm 3 , and the glaze application amount is 2500 g / m 2 .

[0064] Step 7. Put the green body applied with the high-expansion crack glaze into a roller hearth kiln for firing. The highest firing temperature is 1180 °C, and the firing cycle is 42 min.

[0065] Figure 1 It is the brick surface effect diagram of Example 1. It can be seen that the brick surface has an excellent ice crack crystal flower effect.

[0066] The inkjet crystal flower ice crack ceramics were subjected to thermal cycling tests according to GB / T3298-2008. The samples had no defects such as cracks and breakages.

[0067] Comparative Example 1

[0068] The preparation method of the inkjet crystal flower ice crack ceramics comprises the following steps:

[0069] Step 1. Prepare a high-aluminum green body. The chemical composition of the high-aluminum green body includes: by mass percentage, IL: 5%, SiO2: 60%, Al2O3: 30%, Fe2O3: 0.5%, TiO2: 0.1%, CaO: 0.4%, MgO: 2%, K2O: 1%, Na2O: 1%. The thermal expansion coefficient of the high-aluminum green body at 20°C to 600°C is 6×10 -6 / °C.

[0070] Step 2. Dry the high-aluminum green body.

[0071] Step 3. Inkjet print a common ink pattern on the surface of the dried green body.

[0072] Step 4. Apply a high-expansion crack glaze on the surface of the green body after inkjet printing the common ink pattern. The composition and glazing parameters of the high-expansion crack glaze are the same as those in Example 1.

[0073] Step 5. Fire the green body applied with the high-expansion crack glaze in a roller hearth kiln. The highest firing temperature is 1250°C and the firing cycle is 60 min.

[0074] This comparative example uses a high-aluminum green body, which can reduce the thermal expansion coefficient of the green body, thereby increasing the difference in the expansion coefficients of the body and glaze and achieving the ice crack effect. However, this will increase the firing temperature, which is not conducive to the rapid firing of building ceramics, resulting in an increase in production costs and making it difficult to achieve mass production.

[0075] Comparative Example 2

[0076] It is the same as Example 1, except that: only Step 3 is omitted.

[0077] Only ordinary cracks appear on the brick surface of this comparative example, and the stacked ice crack effect cannot be formed.

[0078] Comparative Example 3

[0079] It is basically the same as Example 1, except that:

[0080] The mineral composition of the base glaze includes: in terms of mass percentage, high-aluminum ball clay: 40%, potassium feldspar: 25%, calcined talc: 5%, albite: 20%, quartz: 10%. The chemical composition of the base glaze includes: in terms of mass percentage, IL: 8.6%, SiO2: 65.1%, Al2O3: 19.45%, Fe2O3: 0.6%, TiO2: 0.15%, CaO: 0.5%, MgO: 1.6%, K2O: 2.5%, Na2O: 1.5%. The thermal expansion coefficient of the base glaze at 20°C to 600°C is 7.4×10 -6 / °C. The application method of the base glaze is spraying. The specific gravity of the base glaze is 1.45 g / cm 3 , and the glaze application amount is 600 g / m 2 .

[0081] Large cracks appeared on the brick surface of this comparative example, and the effect of ice crack crystal flowers could not be achieved.

[0082] Comparative Example 4

[0083] It is basically the same as Example 1, with the only difference being that: the specific gravity of the base glaze is 1.45 g / cm 3 , and the glaze application amount is 800 g / m 2 .

[0084] The brick shape of this comparative example is biased towards a turtle shape, and even glaze layer peeling occurs.

Claims

1. A preparation method of an inkjet crystal flower crackle ceramic, characterized in that, The preparation method comprises the following steps: Applying a base glaze on the surface of the low-aluminum green body; Inkjet printing a decorative pattern on the surface of the low-aluminum green body after applying the base glaze; Applying a high-expansion crack glaze on the surface of the green body after inkjet printing the decorative pattern; Firing the green body after applying the high-expansion crack glaze to obtain an inkjet crystal flower crack ceramic.

2. The preparation method according to claim 1, characterized in that, The aluminum mass content of the low-aluminum green body is 12% to 18%; preferably, the chemical composition of the low-aluminum green body comprises: by mass percentage, IL: 1% to 3%, SiO2: 65% to 75%, Al2O3: 12% to 18%, Fe2O3: 0.5% to 1.5%, TiO2: 0.1% to 0.2%, CaO: 0.2% to 0.5%, MgO: 0.1% to 0.5%, K2O: 2% to 6%, Na2O: 1% to 5%.

3. The preparation method according to claim 1 or 2, characterized in that, The mineral composition of the low-aluminum green body comprises: by mass percentage, clay: 15% to 25%, potassium / sodium feldspar: 35% to 60%, potassium sand: 10% to 30%, calcined talc: 0.5% to 5%, talc: 1% to 5%.

4. The preparation method according to any one of claims 1 to 3, characterized in that, The mineral composition of the base glaze comprises: by mass percentage, high-aluminum ball clay: 75% to 85%, α-aluminum oxide: 5% to 15%, calcined talc: 1% to 10%, potassium / sodium feldspar: 1% to 10%; preferably, the chemical composition of the base glaze comprises: by mass percentage, IL: 5% to 13%, SiO2: 45% to 55%, Al2O3: 25% to 35%, Fe2O3: 0.5% to 1.5%, TiO2: 0.1% to 0.2%, CaO: 0.2% to 0.5%, MgO: 0.1% to 5%, K2O: 0.5% to 2%, Na2O: 0.2% to 2.5%.

5. The preparation method according to any one of claims 1 to 4, characterized in that, The application method of the underglaze is spraying; preferably, the specific gravity of the underglaze is 1.44-1.46 g / cm 3 , and the glaze application amount is 500-700 g / m 2 .

6. The preparation method according to any one of claims 1 to 5, characterized in that, The mineral composition of the high-expansion crack glaze comprises: by mass percentage, clay: 3% to 15%, high-expansion frit: 40% to 50%, high-sodium frit: 10% to 20%, high-calcium frit: 5% to 15%, high-boron frit: 1% to 10%, lead frit: 1% to 5%; preferably, the chemical composition of the high-expansion crack glaze comprises: by mass percentage, IL: 0.1% to 0.5%, SiO2: 55% to 65%, Al2O3: 5% to 15%, Fe2O3: 0.1% to 0.5%, TiO2: 0.1% to 0.2%, CaO: 5% to 15%, MgO: 0.1% to 0.5%, K2O: 0.5% to 2%, Na2O: 15% to 25%, PbO: 1% to 5%, B2O3: 1% to 5%.

7. The preparation method according to claim 6, characterized in that, The chemical composition of the high-expansion frit includes: by mass percentage, SiO2: 55% - 70%, Al2O3: 5% - 15%, Fe2O3: 0.1% - 0.5%, TiO2: 0.1% - 0.2%, CaO: 5% - 15%, MgO: 0.1% - 0.5%, K2O: 0.5% - 2%, Na2O: 10% - 20%; Preferably, the mineral composition of the high-expansion frit includes: by mass percentage, clay: 3% - 15%, albite: 50% - 70%, nepheline: 5% - 15%, calcite: 15% - 35%, talc: 1% - 6%.

8. The preparation method according to claim 6 or 7, characterized in that, The chemical composition of the high-sodium frit includes: by mass percentage, SiO2: 55% - 65%, Al2O3: 10% - 15%, Fe2O3: 0.3% - 1.5%, TiO2: 0.2% - 0.5%, CaO: 5% - 15%, MgO: 0.5% - 3%, K2O: 1% - 5%, Na2O: 15% - 25%; Preferably, the mineral composition of the high-sodium frit includes: by mass percentage, clay: 5% - 10%, potassium / sodium feldspar: 55% - 75%, nepheline: 3% - 10%, limestone: 15% - 25%, talc: 0.5% - 3%.

9. The preparation method according to any one of claims 6 to 8, characterized in that, The chemical composition of the high-calcium frit includes: by mass percentage, SiO2: 65% - 75%, Al2O3: 5% - 15%, Fe2O3: 0.1% - 0.5%, TiO2: 0.1% - 0.3%, CaO: 15% - 20%, MgO: 0.5% - 5%, K2O: 1% - 5%, Na2O: 3% - 10%; Preferably, the mineral composition of the high-calcium frit includes: by mass percentage, clay: 5% - 15%, potassium / sodium feldspar: 10% - 30%, nepheline: 5% - 15%, limestone: 35% - 45%, calcite: 30% - 40%, talc: 0.5% - 5%.

10. The preparation method according to any one of claims 6 to 9, characterized in that, The chemical composition of the high-boron frit includes: by mass percentage, SiO2: 40% - 50%, Al2O3: 1% - 5%, Fe2O3: 0.1% - 1%, TiO2: 0.01% - 1%, CaO: 10% - 20%, MgO: 0.1% - 1%, K2O: 0.1% - 1%, Na2O: 5% - 15%, B2O3: 10% - 30%; Preferably, the mineral composition of the high-boron frit includes: by mass percentage, borax: 50% - 70%, quartz sand: 15% - 25%, limestone: 20% - 30%, albite: 5% - 10%.

11. The preparation method according to any one of claims 6 to 10, characterized in that, The chemical composition of the lead frit includes: by mass percentage, SiO2: 35% - 45%, Al2O3: 3% - 8%, Fe2O3: 0.1% - 1%, TiO2: 0.01% - 0.1%, CaO: 0.1% - 2.5%, MgO: 0.1% - 0.5%, K2O: 1% - 5%, Na2O: 2% - 10%, PbO: 25% - 35%, B2O3: 5% - 15%; preferably, the mineral composition of the lead frit includes: by mass percentage, cerussite: 20% - 40%, albite: 10% - 20%, quartz sand: 35% - 45%, borax: 25% - 35%.

12. The preparation method according to any one of claims 6 to 11, characterized in that, The application method of the high-expansion crack glaze is spraying; preferably, the specific gravity of the high-expansion crack glaze is 1.65 to 1.67 g / cm 3 , and the glaze application amount is 2000 to 2500 g / m 2 .

13. The preparation method according to any one of claims 1 to 12, characterized in that, The maximum firing temperature is 1140 - 1180 °C, and the firing cycle is 40 - 50 minutes.

14. Inkjet crystal flower crackle ceramics, characterized in that, The inkjet crystal flower crack ceramic is obtained by the preparation method according to any one of claims 1 to 13.