CN113548798A - Ultra-flat-bottom glaze and application thereof in ceramic tiles - Google Patents

Ultra-flat-bottom glaze and application thereof in ceramic tiles Download PDF

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Publication number
CN113548798A
CN113548798A CN202110738629.6A CN202110738629A CN113548798A CN 113548798 A CN113548798 A CN 113548798A CN 202110738629 A CN202110738629 A CN 202110738629A CN 113548798 A CN113548798 A CN 113548798A
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glaze
ultra
flat ground
percent
flat
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CN113548798B (en
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潘利敏
王贤超
庞伟科
邓来福
胡志敏
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Monalisa Group Co Ltd
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Monalisa Group Co Ltd
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    • 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
    • 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
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/10—Frit compositions, i.e. in a powdered or comminuted form containing lead
    • C03C8/12—Frit compositions, i.e. in a powdered or comminuted form containing lead containing titanium or zirconium
    • 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
    • C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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    • 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
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B41/45—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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/86—Glazes; Cold glazes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B41/80—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
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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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a super flat-bottom glaze and application thereof in ceramic tiles. The chemical composition of the ultra-flat ground glaze comprises: by mass percent, SiO2：58‑65%；Al2O3: 18 to 25 percent; alkaline earth metal oxide: 1 to 2 percent; alkali metal oxides: 2 to 4 percent; ZrO (ZrO)2: 5 to 6 percent. The ultra-flat ground coat and the green body have excellent blank glaze binding property, and the green body applied with the ultra-flat ground coat has high brick shape flatness after being fired, and the glaze surface has fine texture.

Description

Ultra-flat-bottom glaze and application thereof in ceramic tiles
Technical Field
The invention belongs to the field of ceramic building materials, and particularly relates to an ultra-flat-bottom glaze and application thereof in ceramic tiles.
Background
The water absorption requirement of the polished tiles in the market is lower and lower, which means that the requirements on the sintering degree and the vitrification degree of the polished tiles are increased. This results in a softer body for the ceramic tile in the firing area and a more difficult to control tile shape. For example, after conventional glazed tiles are sintered, serious S-shaped deformation (commonly known as raised grains or roller silver in the ceramic industry) is easily generated at the positions 5-20cm away from the front and rear sides of the green tiles in the kiln discharging direction, so that the paving and the attractiveness of the tiles are seriously influenced.
Disclosure of Invention
Aiming at the problems, the invention provides an ultra-flat bottom glaze and application thereof in ceramic tiles. The ultra-flat ground coat and the green body have excellent blank glaze binding property, and the green body applied with the ultra-flat ground coat has high brick shape flatness after being fired, and the glaze surface has fine texture.
In a first aspect, the present invention provides an ultra-flat ground glaze. The chemical composition of the ultra-flat ground glaze comprises: by mass percent, SiO2：58-65％；Al2O3: 18 to 25 percent; alkaline earth metal oxide: 1 to 2 percent; alkali metal oxides: 2 to 4 percent; ZrO (ZrO)2：5-6％。
Preferably, the content of sodium oxide in the alkali metal oxide of the ultra-flat ground coat is higher than that of potassium oxide. Preferably, the chemical composition of the ultra-flat bottom glaze is K in percentage by mass2O accounts for 1.0-1.3%, and Na2O accounts for 1.6 to 2.0 percent. The fluxing capacity of the sodium oxide is stronger than that of the potassium oxide, and the proper amount of the sodium oxide is more beneficial to the fusion reaction of all the components of the ultra-flat glaze, so that the glaze surface is smoother.
Preferably, the chemical composition of the ultra-flat ground coat comprises: by mass percent, IL: 2.5 to 3.5 percent; SiO 22：58-65％；Al2O3：18-25％；Fe2O3：0.3-0.5％；TiO2：0.05-0.3％；CaO：0.5-0.8％；MgO：0.7-1.2％；K2O：1.0-1.3％；Na2O：1.6-2.0％；ZrO2：5-6％。
Preferably, the expansion coefficient of the ultra-flat-bottom glaze is 7.7 multiplied by 10-6℃-1-7.9×10-6℃-1In the meantime.
Preferably, the expansion coefficient of the ultra-flat-bottom glaze is lower than that of the blank body positioned under the ultra-flat-bottom glaze layer. When the expansion coefficient of the ultra-flat ground coat is larger than that of the blank body, the contraction of the glaze layer is larger than that of the blank body in the blank glaze cooling process, the blank body is compressed by the glaze layer to generate compressive stress, the glaze is stretched by the blank body to generate tensile stress, and when the tensile stress exceeds the tensile strength of the glaze layer, the glaze surface is easy to crack. Preferably, the expansion coefficient of the blank is 8.0 x 10-6℃-1-8.3×10-6℃-1(ii) a More preferably, the difference of the expansion coefficients of the ultra-flat ground coat and the blank body is controlled to be 0.2 multiplied by 10-6℃-1-0.3×10-6℃-1In the meantime.
Preferably, the chemical composition of the blank comprises: by mass percent, SiO2：65-68％；Al2O3: 22 to 25 percent; alkaline earth metal oxide: 1 to 3 percent; alkali metal oxides: 2 to 3 percent.
Preferably, the ultra-flat ground coat and the green body react to generate a green glaze intermediate layer with anorthite and mullite crystals as main phases in the firing process.
Preferably, the maximum firing temperature is 1220-.
In a second aspect, the present invention provides the use of an ultra-flat ground glaze according to any one of the above in ceramic tiles. Applying the ultra-flat-bottom glaze on the blank body, and then sintering; the application mode of the ultra-flat ground coat is glaze spraying, and the specific gravity is 1.42-1.45g/cm3The glazing amount is 260-280g/m2。
Preferably, the glaze glossiness of the ultra-flat ground coat is 7-8 degrees, and the deviation of the flatness of the tile surface is +/-0.5 mm.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative of, and not restrictive on, the present invention. Unless otherwise specified, each percentage means a mass percentage.
The ultra-flat bottom glaze and its application in ceramic tiles of the present invention are exemplified below.
And distributing the blank powder and performing compression molding to obtain the blank. The chemical composition of the green body is not limited, and the green body commonly used in the field can be adopted. In some embodiments, the chemical composition of the body comprises: by mass percent, SiO2：65-68％；Al2O3: 22 to 25 percent; alkaline earth metal oxide: 1 to 3 percent; alkali metal oxides: 2 to 3 percent. For example, the chemical composition of the body includes: by mass percent, IL: 4.0 to 5.5 percent; SiO 22：65-68％；Al2O3：22-25％；Fe2O3：0.2-0.5％；TiO2：0.05-0.3％；CaO：0.3-0.5％；MgO：1.5-2.5％；K2O：1.6-2.1％；Na2O: 0.5 to 0.8 percent. Increasing K in the chemical composition of the body2O content to replace part of Na2And O, the sintering range of the green body can be widened, and the occurrence of high-temperature deformation of the green body is reduced. MgO and CaO are also introduced into the chemical composition of the green body as strong active assistants, so that the fluidity of the melt can be improved, the formation of a green glaze intermediate layer is promoted, the sintering of the green body is accelerated, the sintering temperature of the green body is reduced, and the cracking of the green body and the glaze is reduced.
The raw material composition of the green body can comprise: 8-10% of Qingqing potash sand, 8-11% of sodalite powder, 9-11% of terrazzo powder, 7-8% of Lihong potash sand, 8-10% of Nanfeng sand, 28-30% of Bongsha, 20-21% of ball clay, 7-9% of Dongji mud and 2-3% of black talc in percentage by mass. The formation of the intermediate layer of the green glaze can be promoted by the incorporation of black talc (mainly MgO) in the green body formulation.
The expansion coefficient of the blank is 8.0 x 10-6℃-1-8.3×10-6℃-1In the meantime.
Applying ultra-flat-bottom glaze ground coat on the surface of the blank body. The chemical composition of the ultra-flat ground glaze comprises: by mass percent, SiO2：58-65％；Al2O3: 18 to 25 percent; alkaline earth metal oxide: 1 to 2 percent; k2O：1.0-1.3％；Na2O：1.6-2.0％；ZrO2: 5 to 6 percent. In some embodiments, the chemical composition of the ultra-flat ground coat comprises: by mass percent, IL: 2.5 to 3.5 percent; SiO 22：58-65％；Al2O3：18-25％；Fe2O3：0.3-0.5％；TiO2：0.05-0.3％；CaO：0.5-0.8％；MgO：0.7-1.2％；K2O：1.0-1.3％；Na2O：1.6-2.0％；ZrO2：5-6％。
By using the (high-sodium low-potassium) ultra-flat ground coat system, the expansion coefficient of the ground coat can be controlled within a proper range, so that the sintering temperature and the brick shape can be controlled. The expansion coefficient of the ultra-flat ground coat is preferably 7.7 multiplied by 10-6℃-1-7.9×10-6℃-1In the meantime. More preferably, the difference of the expansion coefficients between the ground glaze and the green body is controlled to be 0.2 multiplied by 10-6℃-1-0.3×10-6℃-1In the meantime. The expansion coefficient of the ground glaze is slightly lower than that of the green body, and the difference of the expansion coefficients between the green body and the ultra-flat bottom glaze is moderate, so that the deformation of the brick surface can be controlled, and the glaze surface flatness of the ground glaze can be improved.
Although the common zirconium white base coat can also play a role in covering the base color and flaws of a blank, the common zirconium white base coat is generally a high-potassium low-sodium system, the glaze tends to be green-burned after being burned in a kiln, the texture of the glaze is rough, and ripples are easily generated, so that the mirror surface effect is not favorably presented.
The raw materials of the ultra-flat ground coat comprise: 30-35% of potassium feldspar, 8-10% of albite, 15-18% of nepheline, 25-30% of quartz, 0.5-1.0% of wollastonite, 0.8-1.2% of calcined talc, 8-10% of kaolin, 3-4% of calcined clay, 2.0-3.0% of superfine alumina and 5-6% of zirconium silicate by mass percentage. The ultra-flat bottom glaze increases the expansion coefficient of the ultra-flat bottom glaze through reasonable potassium-sodium feldspar matching (the content of an alumina component in a formula is increased), and wollastonite and ultrafine alumina are introduced to widen the sintering temperature range, so that more exquisite and smooth glaze texture is obtained on the basis of ensuring brick shapes, excellent thermal stability beneficial to the ultra-flat bottom glaze is formed, and the requirement of wide sintering range is met.
In some embodiments, the ultra-flat ground glaze has an onset temperature of 1085-1125 ℃.
The specific gravity of the ultra-flat ground coat is 1.42-1.45g/cm3The glazing amount is 260-280g/m2. The application amount of the ultra-flat ground coat is 40-50g/m higher than that of the common zirconium white ground coat2. Therefore, the glaze surface is difficult to sinter (green firing or under-glaze firing) due to excessive glazing amount of the ultra-flat glaze, so that the improvement of the flatness and the fineness of the glaze surface is not facilitated; and the phenomenon that the defects and the ground color of the blank cannot be covered due to too small glazing amount of the ultra-flat ground coat can also be avoided. In some embodiments, the ultra-flat glaze layer has a thickness of 2 to 3 mm.
The application mode of the ultra-flat ground coat can be glaze spraying. The requirement of glaze pouring on the fluidity of the glaze slip is high, and the specific gravity of the ultra-flat ground glaze is low, so that the glaze slip is easy to split when the ultra-flat ground glaze is applied by bell jar spraying, and the glaze pouring is uneven. The requirement of the ultra-flat ground coat on the fineness is that the screen residue of a 200-mesh screen is 0.3-0.6 wt%.
The glaze glossiness of the ultra-flat ground glaze is 7-8 degrees, and the glaze texture of the sintered ultra-flat ground glaze is good. If the glaze glossiness of the ultra-flat ground coat is lower than 7 degrees, the ground coat is seriously burnt, and a plurality of burrs which are not completely melted and leveled appear on the glaze; if the glaze glossiness of the ultra-flat ground glaze is higher than 8 degrees, under the condition that the ultra-flat ground glaze and the subsequent bright metal surface glaze begin to be fused to generate effects, the bright metal surface glaze has a local reaction devitrification phenomenon due to low initial melting point and low high-temperature viscosity.
It is stated herein that the chemical compositions between the body and the ultra-flat bottom glaze of the present invention are close and complementary to each other by interpenetration. The body and the ultra-flat bottom glaze interact at high temperature, so that components in the ultra-flat bottom glaze, particularly basic oxides, fully react with the body to permeate into the body, and simultaneously components in the body are promoted to enter a glaze layer to form crystals, and media between the body and the ultra-flat bottom glaze (also called as a body glaze combination body and a body glaze middle layer) are generated. Therefore, the invention controls the chemical compositions of the body and the ultra-flat ground coat (the body has higher acidity, namely SiO)2The mole ratio of RO is high, and the ground coatThe moderate acid system is used in the formula), so that a good chemical reaction is formed between the blank and the glaze in the sintering and forming process, thereby being beneficial to improving the binding property of the blank and the glaze. Specifically, the blank mainly absorbs alkaline substances from the ultra-flat ground coat, the ultra-flat ground coat mainly absorbs acidic substances from the blank, the expansion coefficient of the ultra-flat ground coat is properly reduced, the possibility of glaze cracking is eliminated, meanwhile, crystals with properties similar to those of the blank are generated in the middle layer, the glaze melts part of the surface of the blank and permeates into the blank, the contact area of the blank and the glaze is increased, and good reaction between the blank and the glaze is more favorable for balancing thermal stability and stabilizing brick shapes.
In some embodiments, the intermediate layer of the green glaze has a major phase of combined crystal of anorthite and mullite, and a minor amount of the rest is cristobalite and glass phase. The thickness of the intermediate layer of the green glaze is between about 3 and 5 mm.
In the experiment, the raw material composition of the ultra-flat ground coat is found to comprise: by mass percentage, 25-30% of albite, 25-30% of quartz, 25-30% of high-boron frit, 8-10% of kaolin and 5-6% of zirconium silicate. The expansion coefficient of the ultra-flat bottom glaze is large, the blank glaze has poor associativity, a blank glaze intermediate layer cannot be generated (the intermediate layer is formed to offset partial deviation caused by the blank glaze expansion coefficient), the glaze is cracked and falls off, the whole brick-shaped turtle glaze is burnt, and the glaze is rough. High boron frits are commercially available.
Before the surface of the blank body is coated with the ultra-flat ground coat, water can be sprayed on the surface of the blank body to wet the blank body, so that the bonding property between the blank body and the ground coat can be increased. The water spraying amount can be 10-30g/m2. Preferably, before the ultra-flat ground coat is applied on the green body, the green body is polished to be free of powder with visible impurities or particles with fluctuant height. This contributes to further increase the surface flatness of the ultra-flat ground coat. The blank can be polished by a blank polishing machine.
And firing the blank body applied with the ultra-flat ground coat in a kiln. Of course, the surface of the blank after the application of the ultra-flat ground coat may be decorated, for example, by glazing or printing, before firing. The maximum firing temperature is 1200-1225 ℃, and the firing period is 65-75 minutes.
In the firing process of the ultra-flat bottom glaze, the blank and the ultra-flat bottom glaze are subjected to good combination reaction, so that the fired brick is flat, the texture of the glaze surface is fine, and the deviation of the flatness of the brick surface is +/-0.5 mm, and even preferably +/-0.2 mm.
In some embodiments, a bright metal overglaze can be applied on the surface of the blank body after the ultra-flat overglaze is applied.
The chemical composition of the bright metal overglaze comprises: by mass percent, SiO2：38-41％；Al2O3：10-12％；TiO2：13-15％；CaO：16-18％；MgO：1.5-2.0％；K2O: 5.0 to 6.0 percent; CuO: 5 to 6 percent; ZnO: 8 to 10 percent; PbO: 0.5 to 0.8 percent. The bright metal overglaze can ensure the smoothness of the glaze surface and has a bright metal effect, wherein CaO has strong fluxing capacity, the high-temperature viscosity of the glaze can be reduced, the fluidity of the glaze and the glossiness of the glaze surface are improved, and the coloring capacity of CuO can be enhanced; in addition, the introduction of PbO can reduce the loss of the bright metal overglaze, reduce the viscosity of the glaze, ensure that the bright metal overglaze has good fluidity and increase the melting temperature range of the glaze. In some embodiments, the bright metal overglaze has a melting temperature of 1060-1120 ℃ (preferably 1090 ℃). Preferably, the starting melting temperature of the bright metal overglaze is lower than that of the ultra-flat ground glaze. More preferably, the difference of the melting start temperature between the bright metal overglaze and the ultra-flat bottom glaze is 10-20 ℃. The proper range of the initial melting temperature difference value is beneficial to less decomposed substances and harmful substances entering the bright metal overglaze before the blank and the ultra-flat ground glaze are sintered, and meanwhile, the lower initial melting temperature of the metal overglaze is more beneficial to the precipitation of metal crystals of the bright metal overglaze in the high-temperature heat preservation stage, so that the glaze surface forms a bright mirror surface effect.
In some embodiments, the chemical composition of the bright metallic overglaze comprises: by mass percent, IL: 1.5 to 2.5 percent; SiO 22：38-41％；Al2O3：10-12％；TiO2：13-15％；CaO：16-18％；Fe2O3：0.1-0.2％；MgO：1.5-2.0％；K2O：5.0-6.0％；Na2O：0.1-0.2％；CuO：5-6％；ZnO：8-10％；PbO：0.5-0.8％；Li2O：0.1-0.3％。
The bright metal overglaze comprises the following raw materials: 30-40% of potash feldspar, 7-8% of quartz, 10-13% of calcite, 8-10% of calcined zinc oxide, 13-15% of superfine titanium dioxide, 5-6% of calcined talc, 15-18% of lead clinker, 3-4% of corundum and 5-6% of copper oxide. The mesh number of the ultrafine titanium dioxide can be 250 meshes and 325 meshes. The addition of a proper amount of corundum and the reduction of the dosage of zinc oxide can ensure that the mirror surface of the glaze surface is better and the high-temperature sintering is more stable.
The chemical composition of the lead frit may include: by mass percent, SiO2：53-55％；Al2O3：10-12％；TiO2：1-2％；CaO：23-25％；MgO：1.5-2.0％；K2O：3.0-4.0％；Na2O：2.0-3.0％；ZnO：8-10％；PbO：4-6％；Li2O: 0.5 to 1.0 percent. The addition of the lead frit can reduce the loss of ignition, reduce the viscosity of the glaze, enable the glaze to have good fluidity and increase the melting temperature range of the glaze.
The bright metal overglaze contains a large amount of ultrafine titanium dioxide, calcium oxide and lead frits, and can form metal texture with good mirror surface bright decorative effect, excellent ultraviolet light shielding property and good light reflection effect. Wherein, the titanium dioxide in the bright metal overglaze has better ultraviolet masking effect, which leads the glaze layer of the bright metal overglaze to also contain titanium dioxide rutile crystals with high reflectivity for full-wave-band sunlight. The above combined action enhances the reflection of the ceramic tile of the present invention to solar thermal radiation.
The raw materials of the bright metal glaze are uniformly mixed and are uniformly mixed with water and other auxiliary agents such as sodium carboxymethyl cellulose to form the glaze material. The fineness of the bright metal overglaze is 0.1-0.3 wt% of the screen residue of a 200-mesh screen.
The application mode of the bright metal overglaze is glaze spraying. The bell jar glaze pouring has high requirement on the suspension property of the glaze slip, and meanwhile, the bell jar glaze pouring cannot ensure the thickness stability of the glaze layer and easily generates the defects of arc and the like. The specific gravity of the bright metal overglaze is 1.55-1.56g/cm3The glazing amount is 360-390g/m2. The over-high or over-low specific gravity of the bright metal surface glaze is not beneficial to the stable water collection of the glaze surfaceWhich affects the flatness of the glaze. The glaze slip has higher specific gravity and higher viscosity, and can not be leveled due to poor fluidity when being spread on the surface of the brick. The excessively low specific gravity and viscosity of the glaze slip can cause partial substances in the glaze slip to be deposited too fast, and the glaze slip can be forked to form lines in the process of pouring glaze on a bell jar, so that the flatness of the glaze surface is influenced. The glazing amount of the bright metal overglaze can ensure the mature glaze layer, the brick shape is stable, and the effect of metal precipitation of the glaze layer is more stable. In some embodiments, the bright metal overglaze layer has a thickness of 4 to 5 mm.
And screen printing fancy glaze on the surface of the blank body after the bright metal surface glaze is applied. The process aims to reduce the unevenness of the surface accumulation of the glaze spraying slip and further ensure the flatness of the glaze surface. The raw material composition and chemical composition of the fancy glaze are consistent with those of the bright metal overglaze. Therefore, the method is more favorable for sintering and forming, and avoids the defects of other glazes caused by the component difference of the bright metal overglaze and the fancy glaze.
The fineness of the fancy glaze can be 0.02-0.04 wt% of the screen residue of a 200-mesh screen, and the flow rate is 30-32s (the outflow aperture of an Engler viscometer is 4.75mm, 200 mL). The fancy glaze can be printed through a screen with 140 meshes and 160 meshes. All-through screen printing may be used. In some embodiments, the fancy glaze has a specific gravity of 1.26 to 1.30g/cm3The glazing amount is 30-60g/m2. The glazing parameters of the fancy glaze are in the range, so that the glaze surface can be ensured to be smoother.
And drying the blank after screen printing of the glaze. The drying temperature is 120-150 ℃, and the moisture of the dried blank is controlled within 0.5 wt%.
And (5) firing in a kiln. The metal in the glaze layer is saturated and precipitated by high-temperature sintering, so that the ceramic surface has bright metal plating texture. The maximum firing temperature is 1200-1225 ℃, and the firing period is 65-75 minutes. Preferably, in the firing system, the holding time at the maximum firing temperature is 8 to 10 min. The purpose of this is to make the glaze layer have enough heat preservation time in the high temperature section, so as to be favorable to separating out metal, make the glaze level more. When the heat preservation time of the highest sintering temperature is less than 8min, the effect of metal precipitation is poor, and the glossiness of the glaze surface is low.
And (6) edging and packaging. The gloss surface gloss of the ceramic tile with the imitated gloss mirror surface metal plating texture is 100-110 degrees. The series of products do not need a polishing process.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
Step 1, distributing the blank powder and pressing and forming to obtain the blank.
And 2, polishing and flattening the blank body by a blank polishing machine, and then drying in a drying kiln. The drying temperature is 130-150 ℃, and the drying is carried out until the moisture of the blank body reaches below 0.8wt percent. After the polished green body is swept, spraying water on the surface of the green body, wherein the water spraying amount is 15-20g/m2。
And 3, spraying the super-flat ground coat on the surface of the blank. The chemical composition of the ultra-flat ground glaze comprises: by mass percent, IL: 2.5 to 3.5 percent; SiO 22：58-65％；Al2O3：18-25％；Fe2O3：0.3-0.5％；TiO2：0.05-0.3％；CaO：0.5-0.8％；MgO：0.7-1.2％；K2O：1.0-1.3％；Na2O：1.6-2.0％；ZrO2: 5 to 6 percent. The specific gravity of the ultra-flat ground coat is 1.42-1.45g/cm3The glazing amount is 260-280g/m2。
And 4, spraying a bright metal overglaze on the surface of the blank body sprayed with the ultra-flat underglaze. The chemical composition of the bright metal overglaze comprises: by mass percent, IL: 1.5 to 2.5 percent; SiO 22：38-41％；Al2O3：10-12％；Fe2O3：0.1-0.2％；TiO2：13-15％；CaO：16-18％；MgO：1.5-2.0％；K2O：5.0-6.0％；Na2O：0.1-0.2％；CuO：5-6％；ZnO：8-10％；PbO：0.5-0.8％；LiO：0.1-0.3％。
Step 5, screen printing fancy glaze on the surface of the blank sprayed with the bright metal glaze, and adopting two groups of 160-mesh all-through fancy screens for printing, wherein the glazing amount is 30-60g/m2。
And 6, drying the blank body after the screen printing glaze. The drying temperature is 120-150 ℃, and the moisture of the dried blank is controlled within 0.5 wt%.
And 7, firing in a kiln. The maximum firing temperature is 1200-1225 ℃, and the firing period is 65-75 minutes.
XRD analysis and EDS analysis were performed on the brick face of this example. The main phase of the glaze surface is CaTiSiO through XRD5A crystalline phase. According to EDS (electron-dispersive spectroscopy) analysis, main elements of the detection area are O, Na, Si, K, Mg, Zn and Ti, and the content of each element in the test crystal area and the amorphous area is shown in Table 1.
TABLE 1 analysis of element content
Element(s) Mass percent of crystalline region Mass percent of amorphous region
O K 34.9 35.5
Na K 1.6 0.3
Al K 4.6 4.6
Si K 25.3 24.3
K K 2.0 1.9
Ca K 12.2 6.9
Ti K 10.9 6.0
Zn K 7.6 15.9
The ceramic tile flatness is detected by a 2m guiding rule and a wedge-shaped clearance gauge. During detection, the side face of the guiding rule is tightly close to the detected face of the ceramic tile, and the size of the gap is detected by the wedge-shaped feeler gauge. Three points, namely a vertical point, are detected at each position, and a point of 45 degrees is inserted in the left and right positions of the position, and the uniform values of the three points are obtained. Four corners and middle values are taken, and the positive and negative deviation of the flatness is within 0.5 mm.
The abrasion resistance is locally measured mainly by a scoring method using a microscope and a hardness meter. Vickers hardness test parameters: loading: 300gf pressure maintaining: and 10S. The indentation of the conventional polished tile with glossy surface (manufactured and polished by comparative example 2) as a comparison increased the crack propagation length at the positions of the four corners, and only the indentation was observed in the ceramic tile with metallic plating texture imitating glossy mirror surface according to the present invention.
TABLE 2 hardness testing table
Figure BDA0003142383740000081
Example 2
Essentially the same as in example 1, except that: step 4 to step 6 are omitted. The glossiness of the baked brick surface is 7-8 degrees, the glaze surface has good flatness, the texture of the glaze surface is fine, the prickly heat blistering defect cannot be seen on the brick surface, the deviation range of the brick shape (the flatness of the brick surface) is within +/-0.2 mm, and no obvious deformation exists.
Comparative example 1
Essentially the same as example 1, except that:
the chemical composition of the ground coat in the step 3 comprises: in mass percent, IL: 3.0 to 4.5 percent; SiO 22：55-60％；Al2O3：18-28％；Fe2O3：0.3-0.5％；TiO2：0.05-0.3％；CaO：0.5-0.8％；MgO：0.7-1.2％；K2O：2.0-3.0％；Na2O：0.2-0.3％；ZrO2: 5 to 6 percent. The ground glaze comprises the following raw materials: by mass percentage, 40-45% of potash feldspar, 25-30% of quartz, 0.5-1.5% of wollastonite, 1.5-2.0% of calcined talc, 8-10% of kaolin, 6-8% of calcined clay, 2.0-3.0% of alumina and 5-6% of zirconium silicate. The expansion coefficient of the ground coat at this time was 7.1X 10-6℃-1-7.4×10-6℃-1And the glossiness of the sintered glaze is between 3 and 4 degrees.
The ceramic tile of comparative example 1 has warped ceramic tile surface, poor sintering of glaze surface and open bubble defect after firing. The consumption of the potassium feldspar in the raw material composition of the ground glaze is higher, the expansion coefficient of the ground glaze is far smaller than that of the green body, the shrinkage of the green body in the cooling process is larger than that of the ground glaze, the ground glaze is warped after being sintered under the compression action of the green body, and even when the compressive stress generated in the ground glaze is larger, cracks are generated on the surface of the ceramic brick.
Comparative example 2
Essentially the same as example 1, except that:
and replacing the bright metal overglaze in the step 4 with the bright overglaze. The chemical composition of the bright overglaze comprises: by mass percent, SiO2：58-65％；Al2O3：13-20％；Fe2O3：0.1-0.3％；TiO2：0.01-0.02％；CaO：10-15％；MgO：2.5-4.0％；K2O：2.0-4.0％；Na2O：1.0-3.0％；ZnO 3-4％，BaO：3.0-5.0％，P2O5：0.2-0.3％。
The glossy overglaze of comparative example 2 does not exhibit metallic texture, and the fancy glaze sinks into the glossy overglaze, causing local dry glaze bubbling. In addition, the chemical component fusion reaction between the bright overglaze and the ground glaze is severe, a large amount of alkaline substances can be absorbed and fused by the ground glaze, so that more components of the bright overglaze permeate into the ground glaze, and the dry glaze phenomenon of the glaze surface is caused.
Comparative example 3
Essentially the same as example 1, except that:
the ground glaze in the step 3 comprises the following raw materials: 45-50% of albite, 15-20% of quartz, 0.5-1.0% of wollastonite, 0.8-1.2% of calcined talc, 8-10% of kaolin, 10-15% of calcined clay and 5-6% of zirconium silicate by mass percentage.
The ground glaze of comparative example 3 has a relatively narrow firing range and easily causes miliaria defects after firing. The reason is that the excessive consumption of albite causes the firing temperature of the formula to be lower and the firing range to be narrower, and the excessive quartz causes the glaze surface to have higher glossiness and generate miliaria and other defects.
Comparative example 4
Essentially the same as example 1, except that:
and replacing the bright metal overglaze in the step 4 with the metal overglaze. The metal overglaze comprises the following raw materials: 35-40% of potash feldspar, 7-8% of quartz, 10-13% of calcite, 10-15% of calcined zinc oxide, 13-15% of superfine titanium dioxide, 5-6% of calcined talc, 10-15% of lead clinker and 5-6% of copper oxide by mass percentage.
The glaze of comparative example 4 exhibited more crystal spots. The crystal spots are mainly the crystallization phenomenon of crystal flowers formed on the glaze surface after crystallization saturation in the glaze. Too many crystal spots can affect the mirror reflection effect of the brick surface, but are not beneficial to the formation of the bright metal mirror surface.
Comparative example 5
Essentially the same as example 1, except that:
the ground glaze in the step 3 comprises the following raw materials: by mass percentage, 25-30% of albite, 25-30% of quartz, 25-30% of high-expansion frit, 8-10% of kaolin and 5-6% of zirconium silicate. The expansion coefficient of the ultra-flat bottom glaze is large, the blank glaze has poor associativity, a blank glaze intermediate layer cannot be generated (the intermediate layer is formed to offset partial deviation caused by the blank glaze expansion coefficient), the glaze is cracked and falls off, the whole brick-shaped turtle glaze is burnt, and the glaze is rough.

Claims (10)

1. The ultra-flat ground coat is characterized by comprising the following chemical components: by mass percent, SiO2：58-65%；Al2O3: 18 to 25 percent; alkaline earth metal oxide: 1 to 2 percent; alkali metal oxides: 2 to 4 percent; ZrO (ZrO)2：5-6%。
2. The ultra-flat ground glaze according to claim 1, wherein Na in the alkali metal oxide of the ultra-flat ground glaze2The content of O is higher than K2O; preferably, the chemical composition of the ultra-flat bottom glaze is K in percentage by mass2O accounts for 1.0-1.3%, and Na2O accounts for 1.6 to 2.0 percent.
3. The ultra-flat ground glaze according to claim 1 or 2, wherein the chemical composition of the ultra-flat ground glaze comprises: by mass percent, IL: 2.5 to 3.5 percent; SiO 22：58-65%；Al2O3：18-25%；Fe2O3：0.3-0.5%；TiO2：0.05-0.3%；CaO：0.5-0.8%；MgO：0.7-1.2%；K2O：1.0-1.3%；Na2O：1.6-2.0%；ZrO2：5-6%。
4. The ultra-flat ground glaze according to any one of claims 1 to 3, wherein the coefficient of expansion of the ultra-flat ground glaze is 7.7 x 10-6℃-1-7.9×10-6℃-1In the meantime.
5. The ultra-flat ground glaze according to any one of claims 1 to 4, wherein the coefficient of expansion of the ultra-flat ground glaze is lower than the coefficient of expansion of a blank body located under the ultra-flat bottom glaze layer; preferably, the expansion coefficient of the blank is 8.0 x 10-6℃-1-8.3×10-6℃-1(ii) a More preferably, the difference of the expansion coefficients of the ultra-flat ground coat and the blank body is controlled to be 0.2 multiplied by 10-6℃-1-0.3×10-6℃-1In the meantime.
6. The ultra-flat ground glaze according to claim 5, wherein the chemical composition of the body comprises: by mass percent, SiO2：65-68%；Al2O3: 22 to 25 percent; alkaline earth metal oxide: 1 to 3 percent; alkali metal oxides: 2 to 3 percent.
7. The ultra-flat ground glaze according to claim 6, wherein the ultra-flat ground glaze reacts with the green body to form a green glaze intermediate layer with anorthite and mullite crystals as main phases in the firing process.
8. The ultra-flat ground glaze according to claim 7, wherein the maximum firing temperature is 1200-1225 ℃, and the firing period is 65-75 minutes.
9. The use of the ultra-flat base glaze according to any one of claims 1 to 8 in ceramic tiles, wherein the ultra-flat base glaze is applied on top of a green body and then fired; the application mode of the ultra-flat ground coat is glaze spraying, and the specific gravity is 1.42-1.45g/cm3The glazing amount is 260-280g/m2。
10. The use of the ultra-flat ground glaze according to claim 9 in ceramic tiles, wherein the ultra-flat ground glaze has a glaze gloss of 7 to 8 degrees and a tile surface flatness deviation of ± 0.5 mm.
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