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CN118791325B - Low expansion, wear-resistant, high light transmittance, dense seam and continuous grain ceramic rock plate and preparation method thereof - Google Patents

Low expansion, wear-resistant, high light transmittance, dense seam and continuous grain ceramic rock plate and preparation method thereof Download PDF

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Publication number
CN118791325B
CN118791325B CN202411275155.6A CN202411275155A CN118791325B CN 118791325 B CN118791325 B CN 118791325B CN 202411275155 A CN202411275155 A CN 202411275155A CN 118791325 B CN118791325 B CN 118791325B
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light
transmitting
low
expansion
overglaze
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CN118791325A (en
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萧礼标
王愉康
杨元东
邓来福
时炯亮
汪陇军
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Monalisa Group Co Ltd
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Monalisa Group Co Ltd
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
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    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
    • C04B2235/3454—Calcium silicates, e.g. wollastonite
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    • C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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Abstract

The invention relates to a low-expansion wear-resistant high-light-transmittance tight-joint-line ceramic rock plate and a preparation method thereof, and belongs to the technical field of ceramic brick production and manufacturing. The preparation method comprises the steps of preparing light-transmitting powder into a light-transmitting green body, applying light-transmitting overglaze on the surface of the light-transmitting green body, carrying out ink-jet printing on the surface of the green body after the light-transmitting overglaze is applied, applying low-expansion protective glaze on the surface of the green body after the ink-jet printing on the design pattern, and burning and polishing the green body after the low-expansion protective glaze is applied to obtain the low-expansion wear-resistant high-light-transmitting closely-sewn-pattern ceramic rock plate. According to the invention, the specially developed light-transmitting green body, the light-transmitting overglaze and the low-expansion protective glaze are matched to obtain the low-expansion wear-resistant high-light-transmitting tight joint continuous ceramic rock plate on the premise of avoiding deformation and glaze defects.

Description

Low-expansion wear-resistant high-light-transmittance tight-joint-line ceramic rock plate and preparation method thereof
Technical Field
The invention relates to a low-expansion wear-resistant high-light-transmittance tight-joint-line ceramic rock plate and a preparation method thereof, and belongs to the technical field of ceramic brick production and manufacturing.
Background
Ceramic tiles are a traditional decorative product in the field of building ceramics, and are favored by consumers due to their excellent wear resistance, antifouling property and diversified decorative effects. With the development of economy, people have pursued higher quality of life, and ceramic tiles with aesthetic feeling and use value are favored by consumers. The high-light-transmission close-joint continuous-grain ceramic rock plate is elegant and elegant, can show pattern textures under the irradiation of light rays, further improves the overall decoration effect, and has a large application space in the field of building material decoration. However, the close-joint continuous grain ceramic product also has higher requirements on the preparation process. Among them, how to prevent deformation and glaze defect of the tight joint and line product is one of the important problems to be overcome.
The close-joint continuous-grain low-expansion-coefficient floor heating ceramic tile disclosed in the China patent CN 114988857A sequentially comprises a blank layer and a glaze layer from bottom to top, wherein the blank layer comprises, by mass, 20-25 parts of feldspar, 12-16 parts of quartz, 12-16 parts of clay, 12-16 parts of mineral salt, 6-8 parts of bauxite and 20-40 parts of lithium-containing ceramic powder, the glaze layer comprises, by mass, 25-43 parts of feldspar, 18-23 parts of quartz, 13-20 parts of clay, 7-11 parts of calcined alumina, 1-4 parts of nepheline, 3-5 parts of calcined talcum and 2-5 parts of frit, and the glaze layer mainly comprises, by mass, 28 parts of petalite, and 7-10 parts of petalite. It can be seen that CN 114988857a mainly adopts spodumene, lithium porcelain stone, etc. to reduce the thermal expansion coefficient of ceramic products. However, the lithium-containing mineral raw materials are high in price, so that the cost of the formula is greatly increased.
Disclosure of Invention
Aiming at the problems, the invention provides the low-expansion wear-resistant high-light-transmission tight-joint-and-line ceramic rock plate and the preparation method thereof.
In a first aspect, the invention provides a preparation method of a low-expansion wear-resistant high-light-transmittance tight-joint-and-line ceramic rock plate. The preparation method comprises the following steps:
Preparing light-transmitting powder into a light-transmitting blank;
applying a light-transmitting overglaze on the surface of the light-transmitting green body;
ink-jet printing a design pattern on the surface of the blank body after the light-transmitting overglaze is applied;
Applying a low-expansion protective glaze on the surface of the green body after the design pattern is printed by the ink jet;
And (3) sintering and polishing the blank body after the low-expansion protective glaze is applied to obtain the low-expansion wear-resistant high-light-transmission tight joint pattern ceramic rock plate.
Preferably, the mineral composition of the light-transmitting overglaze comprises, by mass, 40-60% of water-washed kaolin, 20-30% of potassium feldspar, 5-15% of high-aluminum high-calcium frit, 5-15% of barium carbonate and 1-10% of wollastonite, wherein the chemical composition of the high-aluminum high-calcium frit comprises, by mass ,IL：1~10%、SiO2：35~65%、Al2O3：20~30%、Fe2O3：0.02~0.10%、TiO2：0.01~0.05%、CaO：10~23%、MgO：0.5~3%、K2O：1~8%、Na2O：1~10%、BaO：0.1~3%.
Preferably, the chemical composition of the light-transmitting overglaze comprises the following components in percentage by mass ,IL：4~6%、SiO2：55~65%、Al2O3：19~22%、Fe2O3：0.01~0.1%、TiO2：0.01~0.1%、CaO：3~5%、MgO：0.1~0.5%、K2O：2~3%、Na2O：1~3%、BaO：7~9%.
Preferably, the thermal expansion coefficient of the light-transmitting overglaze is 6.5X10 -6/K ~6.8×10-6/K at 40-600 ℃.
Preferably, the mineral composition of the low-expansion protective glaze comprises, by mass, 8-12% of kaolin, 10-18% of calcined talc, 45-55% of low-expansion frit, 5-20% of barium carbonate, 10-18% of wollastonite and 1-3% of calcined zinc oxide, wherein the chemical composition of the low-expansion frit comprises, by mass ,IL：0.1~0.5%、SiO2：47~54%、Al2O3：10~16%、Fe2O3：0.01~0.05%、TiO2：0.01~0.05%、CaO：5~10%、MgO：1~3%、K2O+Na2O：3~6%、BaO：8~12%、ZnO：10~15%.
Preferably, the chemical composition of the low-expansion protective glaze comprises the following components in percentage by mass ,IL：3~4%、SiO2：47~49%、Al2O3：11~13%、Fe2O3：0.01~0.2%、TiO2：0.01~0.05%、CaO：11~14%、MgO：4~6%、K2O：1~3%、Na2O：1~2%、BaO：8~10%、ZnO：4~6%.
Preferably, the thermal expansion coefficient of the low expansion protective glaze is 6.0X10 -6/K ~6.2×10-6/K at 40-600 ℃.
Preferably, the light-transmitting overglaze is sprayed in a mode of applying, the specific gravity of the light-transmitting overglaze is 1.4-1.5 g/cm 3, and the glazing amount is 540-700 g/m 2.
Preferably, the low-expansion protective glaze is sprayed in a mode of being applied, the specific gravity of the low-expansion protective glaze is 1.5-1.6 g/cm 3, and the glazing amount is 600-770g/m 2.
Preferably, the mineral composition of the light-transmitting powder comprises, by mass, 30-40% of water-washed kaolin, 15-25% of potassium feldspar, 25-35% of high-aluminum high-calcium frit and 10-25% of wollastonite, wherein the chemical composition of the high-aluminum high-calcium frit comprises, by mass ,IL：1~10%、SiO2：35~65%、Al2O3：20~30%、Fe2O3：0.02~0.10%、TiO2：0.01~0.05%、CaO：10~23%、MgO：0.5~3%、K2O：1~8%、Na2O：1~10%、BaO：0.1~3%.
Preferably, the firing temperature is 1190-1210 ℃ and the firing time is 60-80 minutes.
In a second aspect, the invention provides a low-expansion wear-resistant high-light-transmittance tight-joint-and-line ceramic rock plate. The low-expansion wear-resistant high-light-transmittance ceramic close-joint-and-line rock plate is obtained according to the preparation method.
Advantageous effects
According to the invention, the specially developed light-transmitting green body, the light-transmitting overglaze and the low-expansion protective glaze are matched, so that the low-expansion wear-resistant high-light-transmitting tight joint-line ceramic rock plate is obtained on the premise of avoiding deformation and glaze defects.
Drawings
FIG. 1 is a graph of the tile surface effect of example 1;
FIG. 2 is a graph comparing the light transmission effects of the light transmitting overglaze used in example 1 (left) and the conventional zirconium white overglaze used in comparative example 1 (right);
FIG. 3 is a graph comparing the tile surface effect of example 3 (left) and comparative example 2 (right);
FIG. 4 is a graph of the tile surface effect of comparative example 3;
FIG. 5 is a graph of the tile effect of comparative example 4.
Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof. The following illustrates the preparation method of the low-expansion wear-resistant high-light-transmittance tight-joint-line ceramic rock plate.
The tight joint of the tight joint and the line ceramic rock plate refers to the tight joint paving of ceramic tiles, and particularly refers to the control of gaps between the ceramic tiles within 0.5mm in the ceramic tile paving process, so that no obvious splicing boundary line exists between two ceramic tiles, and the two ceramic tiles are integrated. The good close joint paving is beneficial to realizing the tile connecting line effect. The flatness, expansion coefficient and water absorption of the ceramic tile are main factors affecting the effect of the close joint and the continuous line. The low expansion coefficient can effectively prevent the ceramic tile from deforming after being paved, so that the tight joint and the continuous line effect of the product is not influenced by changes of external temperature, humidity and the like.
Light-transmitting powder (light-transmitting blank) was prepared. In some embodiments, the mineral composition of the light-transmitting powder comprises, by mass, 30-40% of water-washed kaolin, 15-25% of potassium feldspar, 25-35% of high-aluminum high-calcium frit and 20-25% of wollastonite.
The high-aluminum high-calcium frit of the light-transmitting powder comprises the following chemical components in percentage by mass ,IL：1~10%、SiO2：35~65%、Al2O3：20~30%、Fe2O3：0.02~0.10%、TiO2：0.01~0.05%、CaO：10~23%、MgO：0.5~3%、K2O：1~8%、Na2O：1~10%、BaO：0.1~3%.
As an example, the chemical composition of the high-alumina high-calcium frit of the light-transmitting powder comprises the following components in percentage by mass ,IL：1~3%、SiO2：35~45%、Al2O3：25~30%、Fe2O3：0.02~0.10%、TiO2：0.01~0.05%、CaO：10~23%、MgO：1~3%、K2O：3~8%、Na2O：1~10%、BaO：1~3%.
In some embodiments, the mineral composition of the high-alumina high-calcium frit comprises, by mass, 25-31% of potassium feldspar, 34-42% of wollastonite, 4-10% of dolomite, 2-5% of barium carbonate and 20-24% of calcined alumina. Weighing raw materials according to the mineral composition of the high-aluminum high-calcium frit, uniformly mixing the raw materials, melting the raw materials at 1400-1500 ℃ for 1-2 hours to obtain glass liquid, quenching the glass liquid with water, and crushing the glass liquid to obtain the high-aluminum high-calcium frit.
The transparent powder material has the advantages that the content of calcium oxide and aluminum oxide in the transparent powder material is increased, a large amount of anorthite main crystal phases are generated in the blank body after high-temperature sintering, the refractive indexes of the anorthite and the glass are close, and the loss of light generated by scattering between the glass phase and the crystal phase can be reduced. The inventors have tried to use wollastonite and alumina directly in the formulation of light-transmitting green bodies, and found that less anorthite crystals are produced in the green bodies, and that the alumina does not participate effectively in the reaction to produce the anorthite, but is present as corundum, which increases the loss of light inside the green bodies. According to the invention, by adopting a mode of matching wollastonite with the special high-alumina high-calcium frit, the alumina content of the blank formula can be increased, the high-temperature viscosity is increased, the high-temperature deformation is reduced, and the production of the plase crystal phase with higher activity and higher content is facilitated, so that the light transmittance of the blank is improved.
Weighing raw materials according to the formula of the light-transmitting powder, adding water, ball milling, spray granulating, aging and the like to obtain the light-transmitting powder.
And forming the light-transmitting powder into a light-transmitting blank. The molding mode is not limited, and can be dry press molding. And drying the light-transmitting green body. For example, the drying temperature is 180-220 ℃ and the drying time is 40-60 minutes.
In some embodiments, the chemical composition of the light-transmitting blank comprises the following components in percentage by mass ,IL：3~5%、SiO2：52~57%、Al2O3：19~22%、Fe2O3：0.01~0.1%、TiO2：0.01~0.1%、CaO：11~15%、MgO：0.01~1.0%、K2O：1~5%、Na2O：1~4%、BaO：0.3~1.0%.
The thermal expansion coefficient of the light-transmitting green body at 40-600 ℃ is 6.1 multiplied by 10 -6/ K ~6.3×10-6/K.
According to the invention, the low-iron and low-titanium clay and flux raw materials are used in the light-transmitting blank formula, and the special high-aluminum high-calcium frit is added on the basis of wollastonite, so that the calcium oxide and aluminum oxide contents of the blank formula are improved, a large amount of radaite main crystal phases are generated in the blank after high-temperature sintering, and the light-transmitting performance of the blank is improved.
At the light-transmitting blank a light-transmitting overglaze is applied to the surface.
The mineral composition of the light-transmitting overglaze comprises, by mass, 40-60% of water-washed kaolin, 20-30% of potassium feldspar, 5-15% of high-aluminum high-calcium frit, 5-15% of barium carbonate and 1-10% of wollastonite.
The high-aluminum high-calcium frit of the light-transmitting overglaze comprises the following chemical compositions in percentage by mass ,IL：1~10%、SiO2：35~65%、Al2O3：20~30%、Fe2O3：0.02~0.10%、TiO2：0.01~0.05%、CaO：10~23%、MgO：0.5~3%、K2O：1~8%、Na2O：1~10%、BaO：0.1~3%.
For example, the chemical composition of the high aluminum high calcium frit of the light-transmitting overglaze comprises the following components in percentage by mass ,IL：1~10%、SiO2：35~65%、Al2O3：20~30%、Fe2O3：0.02~0.10%、TiO2：0.01~0.05%、CaO：10~23%、MgO：0.5~3%、K2O：1~5%、Na2O：1~3%、BaO：0.1~3%.
The barium carbonate is used in the light-transmitting overglaze formula, so that the formation of a celsian crystalline phase with the refractive index close to that of glass phase can be promoted, the color development performance of overglaze is improved on the premise of ensuring the light-transmitting performance of overglaze, and meanwhile, compared with the conventional potash sodium glass (8.5X10 -7/℃~10×10-7/° C), the expansion coefficient (3.0X10 -7/° C) of the celsian crystalline phase is smaller, the expansion coefficient of an overglaze layer is reduced, and the adaptability to overglaze blanks is improved.
In addition, the green body has poor color development for red ink and yellow ink due to the fact that the green body contains a large amount of calcium oxide in the formula. Meanwhile, the existence of a large amount of plagioclase crystal phases (expansion coefficient 4.8X10 -6/°C) in the blank body leads to lower expansion coefficient of the blank body. The invention creatively develops a surface glaze formula with low expansion coefficient, good light transmission performance and good color development, which is matched with a light-transmitting blank. Through generating the celsian crystal phase with the refractive index close to that of the glass phase in the overglaze formula, the light transmission performance and the color development performance of overglaze are improved, and meanwhile, the expansion coefficient of the celsian crystal phase is smaller than that of the conventional potash sodium glass, so that the expansion coefficient of a light transmission overglaze layer is reduced, and the adaptability to a blank body is improved.
In some embodiments, the chemical composition of the light-transmitting overglaze includes, in mass percent ,IL：4~6%、SiO2：55~65%、Al2O3：19~22%、Fe2O3：0.01~0.1%、TiO2：0.01~0.1%、CaO：3~5%、MgO：0.1~0.5%、K2O：2~3%、Na2O：1~3%、BaO：7~9%.
The thermal expansion coefficient of the light-transmitting overglaze is 6.5X10 -6/K~6.8×10-6/K at 40-600 ℃.
The manner of application of the light-transmitting overglaze is not limited. The light-transmitting overglaze may be applied by spraying. In some embodiments, the specific gravity of the light-transmitting overglaze is 1.4-1.5 g/cm 3, and the glazing amount is 540-700 g/m 2. The light-transmitting overglaze is too low in application amount, so that the light-transmitting green body cannot be uniformly covered, the ink-jet patterns at local positions are in direct contact with the green body, color development of the ink-jet patterns is not facilitated, the overglaze layer is thicker when the light-transmitting overglaze is too high in application amount, water discharge of the overglaze layer is not facilitated, sintering defects of products are easily increased, and meanwhile, too large overglaze application amount is not beneficial to improvement of effects, and production efficiency is reduced.
And (3) carrying out ink-jet printing on the surface of the blank body after the light-transmitting overglaze is applied. The digital ink jet machine is used for carrying out ink jet printing pattern decoration. The design and texture of the ink jet printed design may be adapted as desired.
A low expansion protective glaze is applied to the surface of the ink jet printed design.
The mineral composition of the low-expansion protective glaze comprises, by mass, 8-12% of kaolin, 10-18% of calcined talcum, 45-55% of low-expansion frit, 5-20% of barium carbonate, 10-18% of wollastonite and 1-3% of calcined zinc oxide.
The chemical composition of the low-expansion frit comprises, by mass, ,IL：0.1~0.5%、SiO2：47~54%、Al2O3：10~16%、Fe2O3：0.01~0.05%、TiO2：0.01~0.05%、CaO：5~10%、MgO：1~3%、K2O+Na2O（K2O and/or Na 2 O3-6%, baO 8-12% and ZnO 10-15%.
The mineral composition of the low-expansion frit comprises, by mass, 15-19% of quartz, 0-4% of kaolin (preferably 1-4%), 19-23% of potassium feldspar, 13-17% of albite, 12-16% of wollastonite, 2-6% of dolomite, 10-15% of zinc oxide, 10-15% of barium carbonate and 2-6% of aluminum oxide. Weighing raw materials according to the mineral composition of the low-expansion frit, uniformly mixing the raw materials, melting the raw materials at 1400-1500 ℃ for 1-2 hours to obtain glass liquid, quenching the glass liquid with water, and crushing the glass liquid to obtain the low-expansion frit. In some embodiments, the low expansion frit has a thermal expansion coefficient of 5.4X10 -6/K~5.6×10-6/K at 40-600 ℃.
Conventional protective glazes typically have a higher coefficient of expansion than the green body. If the conventional protective glaze is adopted, the glaze layer is tensioned to cause the glaze to crack due to mismatch of expansion coefficients of the blank glaze. The invention creatively develops a transparent protective glaze with low expansion coefficient, which is matched with a light-transmitting green body and a light-transmitting overglaze. The low-expansion protective glaze uses raw materials such as low-expansion frit, barium carbonate and the like to generate celsian and anorthite crystalline phases in the glaze layer, and finally reduces the expansion coefficient of the protective glaze due to the fact that glass deformation components such as potassium feldspar, albite and the like are not used, and meanwhile, the glaze surface has more crystalline phases after polishing due to the fact that the celsian and the celsian exist in the glaze layer, so that the wear resistance of the glaze surface is greatly improved.
In some embodiments, the chemical composition of the low expansion protective glaze comprises, in mass percent ,IL：3~4%、SiO2：47~49%、Al2O3：11~13%、Fe2O3：0.01~0.2%、TiO2：0.01~0.05%、CaO：11~14%、MgO：4~6%、K2O：1~3%、Na2O：1~2%、BaO：8~10%、ZnO：4~6%.
According to the invention, the specially developed low-expansion frit and barium carbonate are used in the low-expansion protective glaze formula, so that the low-expansion frit enters the glass phase to reduce the expansion coefficient of the protective glaze due to low self-expansion coefficient, and meanwhile, the barium carbonate is introduced to promote the generation of celsian and improve the wear resistance of the glaze by the synergistic effect of the barium carbonate and the labyr.
The thermal expansion coefficient of the low-expansion protective glaze is 6.0X10 -6/K~6.2×10-6/K at 40-600 ℃.
The manner of application of the low expansion protective glaze is not limited. For example, the low-expansion protective glaze is applied by spraying glaze. In some embodiments, the specific gravity of the low-expansion protective glaze is 1.5-1.6 g/cm 3, and the glazing amount is 600-770 g/m 2. The application amount of the protective glaze is too low, the later polishing difficulty is increased, the blank body is easy to polish, the blank body is exposed outside, the performance of the product is not up to the standard, the application amount of the protective glaze is too high, the improvement of the effect is not beneficial, the production efficiency is reduced, and air bubbles are difficult to eliminate and air hole defects are easy to form.
The inventors have attempted to ink jet print the design directly on the surface of the transparent blank and apply a low expansion protective glaze. Although the ceramic rock plate prepared at the moment has no glaze cracks, the yellow area and the red area of the ink-jet design pattern have color differences on the transparent blank body, and the decoration effect of the ink-jet design pattern is difficult to be displayed.
And (3) sintering the green bricks after the low-expansion protective glaze is applied at high temperature. For example, the firing temperature is 1190 to 1210 ℃ and the firing time is 60 to 80 minutes.
Polishing, grading, packaging and warehousing.
In conclusion, the specially developed light-transmitting green body, the light-transmitting overglaze and the low-expansion protective glaze are matched, so that the low-expansion wear-resistant high-light-transmitting closely-sewn-pattern ceramic rock plate is obtained on the premise of avoiding deformation and glaze defects. The invention uses clay with low iron and titanium and high aluminum and high calcium frit as raw materials, adopts a K-Na-Ca flux system, improves the content of calcium oxide and aluminum oxide in a blank formula, and generates a large amount of radalite main crystal phases in a transparent blank after high-temperature sintering. In addition, in order to improve the color development of the green body and the matching property with the green body, the invention also develops a light-transmitting overglaze formula matched with the light-transmitting green body, and on the premise of not reducing the light-transmitting property of the product, a celsian crystal phase is introduced into the light-transmitting overglaze component, and meanwhile, the purposes of improving the color development property, reducing the expansion coefficient of the light-transmitting overglaze and improving the adaptability with the green body are realized. In addition, the invention also develops the low-expansion protective glaze which uses the synergistic effect of celsian and aragonite, improves the wear resistance of the low-expansion protective glaze and reduces the thermal expansion coefficient. The low-expansion wear-resistant high-light-transmission tight-joint-line ceramic rock plate disclosed by the invention has excellent light transmission performance and good color development, and the later-stage moisture absorption expansion and brick deformation of a tight-joint-line product are greatly reduced. In some embodiments, the low expansion abrasion resistant high light transmission close-stitched ceramic rock plate has a visible light transmittance of 4.2% (5.5 mm) with reference to standard GB/T2680-2021.
The present invention will be described in more detail by way of examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1
The preparation method of the low-expansion wear-resistant high-light-transmittance tight-joint-and-line ceramic rock plate comprises the following steps:
And step 1, preparing light-transmitting powder into a light-transmitting blank. The mineral composition of the light-transmitting powder comprises, by mass, 36% of water-washed kaolin, 19% of potassium feldspar, 26% of high-aluminum high-calcium frit and 19% of wollastonite. The high-aluminum high-calcium frit comprises the following chemical components in percentage by mass ,IL：2.2%、SiO2：39.89%、Al2O3：27.4%、Fe2O3：0.09%、TiO2：0.02%、CaO：12%、MgO：1.7%、K2O：5.8%、Na2O：9.8%、BaO：1.1%. of the light-transmitting blank body ,IL：4.8%、SiO2：55.98%、Al2O3：20.3%、Fe2O3：0.1%、TiO2：0.02%、CaO：13.9%、MgO：0.9%、K2O：1.8%、Na2O：1.6%、BaO：0.6%.
And 2, applying a light-transmitting overglaze on the surface of the light-transmitting green body. The mineral composition of the light-transmitting overglaze comprises, by mass, 50% of water-washed kaolin, 25% of potassium feldspar, 10% of high-aluminum high-calcium frit, 10% of barium carbonate and 5% of wollastonite. The chemical composition of the high-aluminum high-calcium frit comprises ,IL：2.2%、SiO2：39.89%、Al2O3：27.4%、Fe2O3：0.09%、TiO2：0.02%、CaO：12%、MgO：1.7%、K2O：5.8%、Na2O：9.8%、BaO：1.1%. of the light-transmitting overglaze in percentage by mass and ,IL：5.7%、SiO2：57.58%、Al2O3：21%、Fe2O3：0.1%、TiO2：0.02%、CaO：3.7%、MgO：0.3%、K2O：2.1%、Na2O：1.8%、BaO：7.7%. of the light-transmitting overglaze in percentage by mass. The specific gravity of the light-transmitting overglaze is 1.4g/cm 3, and the glazing quantity is 620g/m 2.
And 3, carrying out ink-jet printing on the surface of the blank body after the light-transmitting overglaze is applied.
And 4, applying a low-expansion protective glaze on the surface of the ink-jet printing design pattern. The mineral composition of the low-expansion protective glaze comprises, by mass, 10% of kaolin, 15% of calcined talcum, 51% of low-expansion frit, 8% of barium carbonate, 15% of wollastonite and 1% of calcined zinc oxide. The chemical composition of the low-expansion frit comprises ,IL：0.2%、SiO2：50.75%、Al2O3：13%、Fe2O3：0.03%、TiO2：0.02%、CaO：8%、MgO：1%、K2O+Na2O：5%、BaO：10%;ZnO：12%. of the low-expansion protective glaze in percentage by mass and ,IL：3.4%、SiO2：48.5%、Al2O3：12.4%、Fe2O3：0.17%、TiO2：0.03%、CaO：12.4%、MgO：5.2%、K2O：1.9%、Na2O：1.2%、BaO：9.6%、ZnO：5.2%. of the low-expansion protective glaze in percentage by mass, wherein the low-expansion protective glaze is sprayed. The specific gravity of the low-expansion protective glaze is 1.5g/cm 3, and the glazing quantity is 680g/m 2.
And 5, sintering and polishing the blank body after the low-expansion protective glaze is applied to obtain the low-expansion wear-resistant high-light-transmission tight joint line ceramic rock plate. Firing temperature was 1190 ℃ and firing time was 60 minutes.
FIG. 1 is a graph of the tile effect of example 1. From the results, the product has excellent light transmission performance, the light is white after passing through, and the paving effect of the product reaches the closely-spaced paving requirement.
The water absorption, the wear resistance and the hardness are tested according to GB/T39156-2020 technical requirements for large-sized ceramic plates and test methods. According to the test result, the water absorption rate of the low-expansion wear-resistant high-light-transmittance tight joint line ceramic rock plate prepared in the example 1 is less than 0.1wt%, the wear-resistant revolution is 2100, and the hardness is 4.
Example 2
Substantially the same as in example 1, except that the chemical composition of the high alumina high calcium frit comprises, in mass percent ,IL：4.8%、SiO2：56.18%、Al2O3：20.3%、Fe2O3：0.1%、TiO2：0.02%、CaO：13.9%、MgO：0.9%、K2O：1.8%、Na2O：1.6%、BaO：0.4%.
Comparative example 1
Substantially the same as in example 1, except that the light-transmitting overglaze was replaced with a conventional zirconium white overglaze. The mineral composition of the conventional zirconium white overglaze comprises 30% of kaolin, 35% of potassium feldspar, 8% of albite, 3% of calcined alumina, 15% of calcined kaolin and 9% of zirconium silicate in percentage by mass. The chemical composition of the conventional zirconium white overglaze comprises the following components in percentage by mass ,IL：3.5%、SiO2：55.8%、Al2O3：27.5%、Fe2O3：0.4%、TiO2：0.2%、CaO：0.2%、MgO：0.1%、K2O：4.3%、Na2O：2.1%、ZrO2：5.9%.
FIG. 2 is a graph comparing the light transmission effects of the light transmitting overglaze used in example 1 (left) and the conventional zirconium white overglaze used in comparative example 1 (right). The light-transmitting overglaze of example 1 and the conventional zirconium overglaze of comparative example 1 were applied to the surface of a green body sample, respectively, and then fired to obtain a sample to be measured. From the above, it can be seen that the light transmittance of the conventional zirconium white overglaze is obviously reduced (the glaze surface is yellow), because the conventional zirconium white overglaze achieves the effects of covering the defects of the base color of the blank and improving the whiteness by adding a certain content of zirconium silicate, and the formed zircon has a larger refractive index, so that the overglaze layer has poor light transmittance and even is basically opaque. Furthermore, the ceramic rock plate prepared in comparative example 1 may exhibit a glaze cracking phenomenon.
Comparative example 2
Substantially the same as in example 1, except that a different ink-jet printed design was used and the low-expansion protective glaze was replaced with a common protective glaze. The mineral composition of the common protective glaze comprises, by mass, 10% of kaolin, 26% of potassium feldspar, 18% of albite, 13% of calcite, 15% of calcined talcum, 9% of barium carbonate, 6% of calcined kaolin and 3% of zinc oxide. The chemical composition of the common protective glaze comprises the following components in percentage by mass ,IL：8.7%、SiO2：48.8%、Al2O3：14.3%、Fe2O3：0.2%、TiO2：0.1%、CaO：7.5%、MgO：4.8%、K2O：2.9%、Na2O：2.9%、BaO：6.9%、ZnO：2.9%.
Example 3
Substantially the same as comparative example 2, except that the ordinary protective glaze was replaced with the low-expansion protective glaze of example 1.
FIG. 3 is a graph comparing the tile surface effect of example 3 (left) and comparative example 2 (right). It can be seen that the ceramic rock plate prepared in the comparative example 2 has a glaze cracking phenomenon, and the light transmittance is not obviously changed, because potassium feldspar and sodium feldspar are largely used in a common protective glaze formula, and because potassium and sodium are not glass forming body elements, the potassium feldspar and sodium are used for replacing Si-O bonds in the glaze formula, so that a glass network structure is damaged, the expansion coefficient of a glass phase is improved, the expansion coefficient of the protective glaze is larger and is far larger than that of a light-transmitting blank body, and the glaze layer is subjected to tensile stress, so that the glaze cracking phenomenon is generated.
The inventors have also found that when the light-transmitting overglaze is replaced by a conventional zirconium overglaze and the low-expansion protective glaze is replaced by a common protective glaze, the prepared ceramic rock plate shows a glaze cracking phenomenon, and the light transmittance is obviously reduced.
Comparative example 3
Substantially the same as in example 1 except that a different ink jet design was used and the low expansion frit was replaced with a boron frit. The mineral composition of the low-expansion protective glaze comprises, by mass, 10% of kaolin, 15% of calcined talcum, 51% of boron frit, 8% of barium carbonate, 15% of wollastonite and 1% of calcined zinc oxide. The chemical composition of the boron frit comprises ,SiO2：58.9%、Al2O3：12.1%、CaO：4%、MgO：1%、K2O+Na2O：8%、BaO：2%、ZnO：2%、B2O3：12%. mass percent of the low-expansion protective glaze ,IL：3.4%、SiO2：52.6%、Al2O3：9.6%、Fe2O3：0.2%、TiO2：0.1%、CaO：9.0%、MgO：5.2%、K2O：2.5%、Na2O：2.1%、BaO：7.2%、ZnO：2%、B2O3：6.1%.
FIG. 4 is a graph of the tile effect of comparative example 3. It can be seen that, although the expansion coefficient of the low expansion protective glaze using the boron frit is reduced, a large number of bubbles appear in the protective glaze layer due to the strong fluxing action of the boron frit, which also leads to the non-standard performance of the polished glaze surface of the product.
Comparative example 4
Substantially the same as in example 1, except that a different ink-jet printed design was used and the barium carbonate of the clear overglaze was replaced with wollastonite. The mineral composition of the light-transmitting overglaze comprises 50% of water-washed kaolin, 25% of potassium feldspar, 10% of high-aluminum high-calcium frit and 15% of wollastonite in percentage by mass. The chemical composition of the light-transmitting overglaze comprises the following components in percentage by mass ,IL：6.0%、SiO2：55.2%、Al2O3：22.9%、Fe2O3：0.2%、TiO2：0.1%、CaO：7.8%、MgO：0.4%、K2O：4.1%、Na2O：1.1%、ZnO：1.2%、BaO：1.0%.
FIG. 5 is a graph of the tile effect of comparative example 4. It can be seen that although the light-transmitting overglaze uses high alumina and high calcium frit, the overglaze formulation contains more calcium oxide, resulting in less excellent development of red and yellow inks on the overglaze.
Comparative example 5
Substantially the same as in example 1, except that the high alumina high calcium frit of the light transmitting powder was replaced with a high silicon frit. The mineral composition of the light-transmitting powder comprises, by mass, 30% of water-washed kaolin, 17% of potassium feldspar, 38% of high-silicon frit, 4% of calcined talcum and 11% of wollastonite. The chemical composition of the high-silicon frit comprises, by mass, 3% of SiO 2：91%、Al2O3：2%、CaO：2%、MgO：1%、K2O：1%、Na2 O. The chemical composition of the light-transmitting powder comprises the following components in percentage by mass ,IL：3.5%、SiO2：73.3%、Al2O3：12%、Fe2O3：0.1%、TiO2：0.1%、CaO：6.1%、MgO：1.9%、K2O：1.2%、Na2O：1.8%.
Although clinker is used in the light-transmitting green body formula, the expansion coefficient of the green body is larger (10.5 multiplied by 10 -6/K) because of the higher quartz content of the whole formula, which is far larger than that of the light-transmitting green body of the embodiment 1, and the requirement of a tight joint line product cannot be met.
The transmittance was measured with reference to the standard GB/T2680-2021 determination of visible transmittance, solar direct transmittance, solar total transmittance, ultraviolet transmittance and related glazing parameters for architectural glass. The expansion coefficient of the green body is tested by referring to the standard GB/T3810.8-2016 "determination of linear thermal expansion of ceramic tiles test method section 8". And judging whether the color generation condition is consistent with the design layout according to the display of the design pattern of the ink-jet printing on the surface of the ceramic rock plate. The antifouling property is tested by reference to the standard GB/T3810.14-2016 "determination of the antifouling property of the 14 th part of the ceramic tile test method". The product properties of each example and comparative example are summarized in Table 1.
TABLE 1
According to the table, the invention obtains the low-expansion wear-resistant high-light-transmission tight joint continuous-grain ceramic rock plate on the premise of avoiding deformation and glaze defects by matching the specially-developed light-transmission green body, the light-transmission overglaze and the low-expansion protective glaze.

Claims (8)

1. The preparation method of the low-expansion wear-resistant high-light-transmission tight-joint-connection-line ceramic rock plate is characterized by comprising the following steps of:
The light-transmitting powder is prepared into a light-transmitting green body, the mineral composition of the light-transmitting powder comprises, by mass, 30-40% of water-washed kaolin, 15-25% of potassium feldspar, 25-35% of high-alumina high-calcium frit and 10-25% of wollastonite, wherein the chemical composition of the high-alumina high-calcium frit comprises, by mass ,IL：1~10%、SiO2：35~65%、Al2O3：20~30%、Fe2O3：0.02~0.10%、TiO2：0.01~0.05%、CaO：10~23%、MgO：0.5~3%、K2O：1~8%、Na2O：1~10%、BaO：0.1~3%;
The surface of the light-transmitting green body is coated with a light-transmitting overglaze, wherein the mineral composition of the light-transmitting overglaze comprises, by mass, 40-60% of water-washed kaolin, 20-30% of potassium feldspar, 5-15% of high-aluminum high-calcium frit, 5-15% of barium carbonate and 1-10% of wollastonite, and the chemical composition of the high-aluminum high-calcium frit comprises, by mass, ,IL：1~10%、SiO2：35~65%、Al2O3：20~30%、Fe2O3：0.02~0.10%、TiO2：0.01~0.05%、CaO：10~23%、MgO：0.5~3%、K2O：1~8%、Na2O：1~10%、BaO：0.1~3%;, the specific gravity of the light-transmitting overglaze is 1.4-1.5 g/cm 3, and the glazing amount is 540-700 g/m 2;
ink-jet printing a design pattern on the surface of the blank body after the light-transmitting overglaze is applied;
the mineral composition of the low-expansion protective glaze comprises, by mass, 8-12% of kaolin, 10-18% of calcined talcum, 45-55% of low-expansion frit, 5-20% of barium carbonate, 10-18% of wollastonite and 1-3% of calcined zinc oxide, wherein the chemical composition of the low-expansion frit comprises, by mass, ,IL：0.1~0.5%、SiO2：47~54%、Al2O3：10~16%、Fe2O3：0.01~0.05%、TiO2：0.01~0.05%、CaO：5~10%、MgO：1~3%、K2O+Na2O：3~6%、BaO：8~12%、ZnO：10~15%;, 1.5-1.6 g/cm 3 of the low-expansion protective glaze, and the glazing amount is 600-770 g/m 2;
And (3) sintering and polishing the blank body after the low-expansion protective glaze is applied to obtain the low-expansion wear-resistant high-light-transmission tight joint pattern ceramic rock plate.
2. The method according to claim 1, wherein the light-transmitting overglaze has a thermal expansion coefficient of 6.5 x 10 -6/K ~6.8×10-6/K at 40-600 ℃.
3. The method according to claim 1, wherein the chemical composition of the low-expansion protective glaze comprises the following components in percentage by mass ,IL：3~4%、SiO2：47~49%、Al2O3：11~13%、Fe2O3：0.01~0.2%、TiO2：0.01~0.05%、CaO：11~14%、MgO：4~6%、K2O：1~3%、Na2O：1~2%、BaO：8~10%、ZnO：4~6%.
4. The method according to claim 1, wherein the low expansion protective glaze has a thermal expansion coefficient of 6.0 x 10 -6/K ~6.2×10-6/K at 40 to 600 ℃.
5. The method of claim 1, wherein the light-transmitting overglaze is applied by spraying.
6. The method of claim 1, wherein the low-expansion protective glaze is applied by spraying.
7. The method according to claim 1, wherein the firing temperature is 1190 to 1210 ℃ and the firing time is 60 to 80 minutes.
8. A low-expansion wear-resistant high-light-transmission close-joint-connected ceramic rock plate, characterized in that it is obtained according to the preparation method of any one of claims 1 to 7.
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