CN112266271A - Roller kiln low-temperature sintered colorful halo crystal glaze and preparation method thereof - Google Patents

Roller kiln low-temperature sintered colorful halo crystal glaze and preparation method thereof Download PDF

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CN112266271A
CN112266271A CN202011554852.7A CN202011554852A CN112266271A CN 112266271 A CN112266271 A CN 112266271A CN 202011554852 A CN202011554852 A CN 202011554852A CN 112266271 A CN112266271 A CN 112266271A
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glaze
parts
crystal
overglaze
halo
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CN112266271B (en
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陈迪晴
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Foshan Yuji Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52Multiple 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
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/20Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/89Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C2209/00Compositions specially applicable for the manufacture of vitreous glazes
    • C03C2209/02Compositions specially applicable for the manufacture of vitreous glazes to produce non-uniformly coloured glazes

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Abstract

The invention relates to the technical field of new ceramic materials, and particularly discloses a seven-color halo crystal glaze fired by a roller kiln at a low temperature, which comprises a ground glaze and a surface glaze, wherein the ground glaze comprises the following components in parts by weight: 80-90 parts of lead-zinc frit and 10-20 parts of pigment; the overglaze comprises the following components in parts by weight: 50-70 parts of high-boron clinker, 5-10 parts of titanium dioxide, 10-20 parts of zinc oxide, 5-15 parts of talcum, 0-10 parts of calcite and 17-30 parts of seeding coloring agent, wherein the seeding coloring agent is manganese dioxide, vanadium pentoxide and copper oxide. The preparation method of the colorful halo crystal glaze fired at the low temperature in the roller kiln comprises the preparation of ground glaze and overglaze, and the glazing and firing, wherein the highest firing temperature is 1125-shaped and 1135 ℃, the firing period is 190-shaped and 210min, so that the crystal glaze suitable for being fired at the low temperature in the roller kiln is prepared, the glaze surface can present one circle of colorful halo in the sun, and the process effect of metal and crystal glaze is achieved.

Description

Roller kiln low-temperature sintered colorful halo crystal glaze and preparation method thereof
Technical Field
The invention relates to the technical field of new ceramic materials, in particular to a seven-color halo crystal glaze fired by a roller kiln at a low temperature and a preparation method thereof.
Background
In the firing process of the crystallized glaze, as the glaze contains enough crystalline substances, the glaze is in a saturated state after being melted, and crystallization is formed in the slow cooling process. The crystal glaze is an art glaze with strong decoration, is from ancient colored glaze in China, and is fundamentally characterized in that the crystal glaze contains a certain amount of visible crystals. The ancient crystal glaze in China is high-temperature iron crystal glaze, and mature rabbit hair, oil drops and other crystal glaze varieties exist in the Song dynasty; tea dust, iron embroidery and the like in Qing Dynasty benefit hair and are exquisite. The crystal patterns of the crystal glaze can be reasonably controlled by an artificial method, and the shape of the crystal glaze is star-shaped, needle-shaped or flower-leaf-shaped. As a high-grade ceramic artistic glaze, the crystal glaze is beautiful and novel natural crystal flowers, and the appearance thereof is diversified and colorful, thereby giving people strong artistic effect and being popular with domestic and foreign users.
At present, most of crystalline glazes on the market are sintered by adopting a tunnel kiln or an intermittent shuttle kiln, the sintering temperature is 1200-1300 ℃, the heat preservation is required for 4-6 hours to form crystals, the yield is low, the energy consumption is high, and the crystalline glazes appear on the glazes in the forms of star-point crystals, flower-shaped leaf crystals, radial crystals and other crystal flowers. Meanwhile, the method is difficult to adapt to the firing condition of a low-temperature roller kiln to prepare colorful crystalline glaze.
Disclosure of Invention
In order to solve the technical problems of high firing temperature, long heat preservation time and single glaze surface effect in the existing preparation process of the crystalline glaze, the invention provides the seven-color halo crystalline glaze fired at the low temperature of the roller kiln and the preparation method thereof, and the crystalline glaze suitable for being fired at the low temperature of the roller kiln is prepared, wherein the highest firing temperature is 1125-shaped and 1135 ℃, the firing period is 190-shaped and 210min, and the glaze surface can present one circle of seven-color halo in the sun, thereby having the process effects of metal and crystalline glaze.
The technical scheme adopted by the invention for solving the technical problems is as follows: a roller kiln low-temperature sintered colorful halo crystal glaze, which comprises a ground glaze and a surface glaze,
the ground glaze comprises the following components in parts by weight: 80-90 parts of lead-zinc frit and 10-20 parts of pigment;
the overglaze comprises the following components in parts by weight: 50-70 parts of high-boron clinker, 5-10 parts of titanium dioxide, 10-20 parts of zinc oxide, 5-15 parts of talc, 0-10 parts of calcite and 17-30 parts of seeding coloring agent, wherein the seeding coloring agent is manganese dioxide, vanadium pentoxide and copper oxide.
Preferably, the lead zinc frit chemistryThe weight percentage of the components is as follows: SiO 22 51%;Al2O3 4%;K2O 4%;Na2O 7%;CaO 4%;MgO 2%;ZnO 5%;PbO 23%。
Preferably, the high-boron frit comprises the following chemical components in percentage by weight: SiO 22 59%;Al2O3 5%;Na2O 14%;B2O3 22%。
Preferably, the grain size of the seeding colorant is: 20-30 nm.
Preferably, the manganese dioxide is 15-20 parts, the vanadium pentoxide is 1-5 parts, and the copper oxide is 1-5 parts.
Preferably, the colorant is one or both of cobalt blue and cobalt black.
The invention also provides a preparation method of the seven-color halo crystal glaze fired in the roller kiln at low temperature, which comprises the following steps:
s1 preparation of ground coat:
firstly, weighing raw materials according to the weight parts of the components of the ground glaze; then putting the ground glaze into a ball mill, adding 1-4 wt% of dispersant and 2-5 wt% of dispergator, adding water, grinding for 4-6 hours to obtain ground glaze slurry, wherein the fineness of the glaze slurry is 0.1-0.2% of ten thousand holes of screen residue; finally, filtering the ground glaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the ground glaze slip into a slip tank for ageing to prepare the colorful halo crystal ground glaze;
s2 preparation of overglaze:
firstly, weighing high-boron frit, titanium dioxide, zinc oxide, talc and calcite according to the weight parts of the overglaze; then putting the glaze slurry into a ball mill, adding 1-4 wt% of dispersant and 2-5 wt% of dispergator, adding water, grinding for 4-6 hours to obtain overglaze glaze slurry with the fineness of 0.1-0.2% of ten thousand holes of screen residue; filtering the overglaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the overglaze slip into a slip tank for aging; finally, adding a seeding coloring agent into the overglaze slip and uniformly stirring to prepare the colorful halo crystal overglaze;
s3, glazing and sintering:
sequentially applying base glaze and overglaze on the ceramic biscuit by adopting a glaze spraying method, drying and then firing in a roller kiln, sequentially applying the base glaze and the overglaze on the ceramic biscuit by adopting the glaze spraying method, drying and then firing in the roller kiln, wherein the maximum firing temperature is 1125-plus 1135 ℃, the firing period is 190-plus 210min, and simultaneously, the heat preservation is respectively carried out in a crystal nucleation region, a high-temperature firing region and a crystal growth region.
Further, the specific gravity of the ground glaze slip is 1.65-1.70.
Furthermore, the specific gravity of the overglaze slip is 1.70-1.75.
Further, a crystal nucleation area, a high-temperature sintering area and a crystal growth area which are sintered by the colorful halo crystal glaze are respectively insulated for 20-60 min.
The technical scheme provided by the embodiment of the application at least has the following technical effects or advantages:
according to the invention, lead-zinc frit is introduced into the ground glaze, lead oxide serving as a strong fluxing agent is beneficial to improving the thermal stability, the melt viscosity can be reduced, the glaze has good fluidity, and the precipitation of ZnO crystals is promoted while the firing temperature is reduced; meanwhile, the high-boron frit is introduced into the overglaze, boron oxide serving as a strong fluxing agent can form a low-melting-point mixture with silicate, the melting temperature of the glaze is reduced, the viscosity of the glaze melt is reduced when the temperature is raised, the fluidity is increased, and the precipitation of crystals such as ZnO, calcium magnesium spinel, titanium sphene and the like is promoted while the sintering temperature is reduced.
By selecting proper crystallization agent and controlling the mol ratio of crystallization oxide, stable titanium sphene crystal, zinc oxide crystal and calcium magnesium spinel crystal are ensured to be obtained in the sintering process of the glaze, and the crystal presents seven-color metallic luster under the action of coloring ions such as cobalt, copper, manganese, vanadium and the like in the bottom glaze layer.
By introducing the high-boron frit, boron oxide is facilitated to promote phase separation and crystallization, so that a liquid-liquid phase separation transmutation phenomenon is generated in glaze, bubble spots are formed in a glaze layer and are dispersed in the glaze layer, various forms of flow lines are formed around the spots, the light transmittance is gradually weakened from the edges of the flow lines to the central area, and the blue opalescence is gradually lightened to form a halo.
Through controlling the firing system of glaze, in the crystal nucleation district of intensification stage, reduce the programming rate, make the crystal fully nucleate under nucleation temperature, keep warm when continuing to heat up to the highest firing temperature, make most crystal nucleus melting, then cool off to crystal growth district and keep warm, will grow out the crystal speck with remaining few crystal nuclei as the basis center in the glaze fuse-element, in addition the split-phase effect, the colouring ion enriches around the crystal nucleus, the glaze forms and uses the crystal speck as the center, forms the artistic effect of seven various metallic luster's halo all around.
Drawings
FIG. 1 is a low-temperature firing curve of the seven-color halo crystal glaze in the roller kiln of the invention.
Detailed Description
The present invention is described in detail below by way of examples to facilitate understanding of the present invention by those skilled in the art, and it is to be specifically noted that the examples are provided only for the purpose of further illustrating the present invention and are not to be construed as limiting the scope of the present invention.
The invention relates to a low-temperature sintered colorful halo crystal glaze for a roller kiln, which comprises a ground glaze and a cover glaze, wherein: the ground glaze comprises the following components in parts by weight: 80-90 parts of lead-zinc frit and 10-20 parts of pigment, wherein the pigment is one or two of cobalt blue and cobalt black; the overglaze comprises the following components in parts by weight: 50-70 parts of high-boron clinker, 5-10 parts of titanium dioxide, 10-20 parts of zinc oxide, 5-15 parts of talc, 0-10 parts of calcite and 17-30 parts of seeding colorant.
As a preferred embodiment, the lead-zinc frit comprises the following chemical components in percentage by weight: SiO 22 51%;Al2O3 4%;K2O 4%;Na2O7 percent; 4% of CaO; 2% of MgO; 5% of ZnO; PbO 23 percent. The lead oxide as the strong fluxing agent is beneficial to improving the thermal stability of the ground glaze, reducing the melt viscosity, leading the glaze to have good fluidity, reducing the firing temperature and promotingAnd precipitating ZnO crystals. The lead oxide can be introduced by minium, white lead or litharge, and when in use, because PbO has toxicity and is volatile, PbO needs to be made into clinker and is not suitable to be used as raw material.
As a preferred embodiment, the high-boron frit comprises the following chemical components in percentage by weight: SiO 22 59%;Al2O3 5%;Na2O 14%;B2O322 percent. Boron oxide as a strong fluxing agent can form a low-melting-point mixture with silicate, the melting temperature of the glaze is reduced, the viscosity of glaze melt is reduced when the temperature is increased, the fluidity is increased, the sintering temperature is reduced, and the precipitation of crystals such as ZnO, calcium magnesium spinel, titanium sphene and the like in the overglaze is promoted.
At the same time, by introducing a high-boron frit, since B2O3Has a surface energy much lower than that of a general silicic acid melt, contains B2O3The surface energy of the split-phase liquid drop is small, the resistance which needs to be overcome by the growth of the liquid drop is reduced, the liquid drop is easy to grow up, the split-phase and crystallization are facilitated, the liquid-liquid split-phase transmutation phenomenon is generated in the glaze, bubble spots are formed in the glaze layer and dispersed in the glaze layer, various forms of flow lines are formed around the spots, the light transmittance is gradually weakened from the edge of the flow line to the central area, and the blue opalescence is gradually lightened to form the halation.
As a preferred embodiment, the overglaze is also added with a nano-scale seeding coloring agent, the seeding coloring agent is manganese dioxide, vanadium pentoxide and copper oxide, the particle size of the seeding coloring agent is 20-30nm, and the seeding coloring agent is added in 15-20 parts of manganese dioxide, 1-5 parts of vanadium pentoxide and 1-5 parts of copper oxide. The nano-level seeding coloring agent has good dispersibility, and mainly plays double roles of seeding and coloring in overglaze.
By selecting proper crystallization agent and controlling the mol ratio of crystallization oxide, stable titanium sphene crystal, zinc oxide crystal and calcium magnesium spinel crystal are ensured to be obtained in the sintering process of the glaze, and the crystal presents seven-color metallic luster under the action of coloring ions such as cobalt, copper, manganese, vanadium and the like in the bottom glaze layer.
The invention relates to a preparation method of a seven-color halo crystal glaze fired by a roller kiln at a low temperature, which comprises the following steps:
s1 preparation of ground coat:
firstly, weighing raw materials according to the weight parts of the components of the ground glaze; then putting the mixture into a ball mill, and adding 1-4 wt% of dispersing agent and 2-5 wt% of dispergator at the same time, wherein: the dispersant is sodium carboxymethylcellulose, the debonder is sodium tripolyphosphate, and water is added for grinding for 4-6 hours to obtain the ground glaze slip, wherein the specific gravity of the ground glaze slip is 1.65-1.70, and the fineness of the glaze slip is 0.1-0.2% of ten thousand-hole screen residue; finally, filtering the ground glaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the ground glaze slip into a slip tank for ageing to prepare the colorful halo crystal ground glaze;
s2 preparation of overglaze:
firstly, weighing high-boron frit, titanium dioxide, zinc oxide, talc and calcite according to the weight parts of the overglaze; then putting the mixture into a ball mill, and adding 1-4 wt% of dispersing agent and 2-5 wt% of dispergator at the same time, wherein: the dispersing agent is sodium carboxymethylcellulose, the dispergator is sodium tripolyphosphate, and water is added for grinding for 4-6 hours to obtain an overglaze glaze slip, wherein the specific gravity of the overglaze slip is 1.70-1.75, and the fineness of the glaze slip is 0.1-0.2% of ten thousand-hole screen residue; filtering the overglaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the overglaze slip into a slip tank for aging; finally, adding a seeding coloring agent into the overglaze slip and uniformly stirring to prepare the colorful halo crystal overglaze;
s3, glazing and sintering:
sequentially applying base glaze and overglaze on the ceramic biscuit by adopting a glaze spraying method, drying and then firing in a roller kiln, sequentially applying the base glaze and the overglaze on the ceramic biscuit by adopting the glaze spraying method, drying and then firing in the roller kiln, wherein the maximum firing temperature is 1125-doped 1135 ℃, and the firing period is 190-doped 210 min. And simultaneously, heat preservation is respectively carried out in a crystal nucleation area, a high-temperature sintering area and a crystal growth area.
The firing system curve of the invention is shown in figure 1, the temperature is rapidly raised, the temperature raising speed is 16-20 ℃/min, the temperature is raised to the temperature of 800-900 ℃ in the crystal nucleation area, and then the temperature is preserved, the temperature preservation time is 20-30min, so that the crystal is fully nucleated at the nucleation temperature; then reducing the temperature rise speed to 10-15 ℃/min, and carrying out heat preservation when the temperature rises to the maximum firing temperature of 1125-1135 ℃, wherein the heat preservation time is 20-30min, so that most crystal nuclei are melted; cooling to 850-950 ℃ of a crystal growth region, and carrying out heat preservation for 30-60min, wherein crystal spots grow in the glaze melt on the basis of the remaining few crystal nuclei, coloring ions are enriched around the crystal nuclei under the action of phase separation, and the glaze surface forms an artistic effect of forming a halo with seven-color metallic luster around the crystal spots; and finally, naturally cooling to room temperature.
Example 1
The roller kiln low-temperature sintered colorful halo crystal glaze comprises a ground glaze and a cover glaze, wherein: the ground glaze comprises the following components in parts by weight: 80 parts of lead-zinc frit, 1 part of cobalt blue and 10 parts of cobalt black; the overglaze comprises the following components in parts by weight: 50 parts of high-boron clinker, 5 parts of titanium dioxide, 10 parts of zinc oxide, 5 parts of talc, 15 parts of manganese dioxide, 1 part of vanadium pentoxide and 1 part of copper oxide.
The preparation method of the seven-color halo crystal glaze fired by the roller kiln at the low temperature comprises the following steps:
s1 preparation of ground coat:
firstly, weighing raw materials according to the weight parts of the components of the ground glaze; then putting the ground glaze into a ball mill, adding 2 wt% of dispersing agent and 2 wt% of dispergator, adding water, grinding for 5 hours to obtain ground glaze slurry, wherein the specific gravity of the ground glaze slurry is 1.65, and the fineness of the glaze slurry is 0.1% of ten thousand holes of screen residue; finally, filtering the ground glaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the ground glaze slip into a slip tank for ageing to prepare the colorful halo crystal ground glaze;
s2 preparation of overglaze:
firstly, weighing high-boron frit, titanium dioxide, zinc oxide, talc and calcite according to the weight parts of the overglaze; then putting the glaze slurry into a ball mill, adding 2 wt% of sodium hydroxymethyl cellulose and 2 wt% of sodium tripolyphosphate, adding water, and grinding for 5 hours to obtain overglaze glaze slip, wherein the specific gravity of the overglaze slip is 1.70, and the fineness of the glaze slip is 0.1% of ten thousand-hole screen residue; filtering the overglaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the overglaze slip into a slip tank for aging; finally, adding a seeding coloring agent into the overglaze slip and uniformly stirring to prepare the colorful halo crystal overglaze;
s3, glazing and sintering:
sequentially applying base glaze and overglaze on the ceramic biscuit by adopting a glaze spraying method, drying and then sintering in a roller kiln, wherein the sintering system is as follows: quickly heating to 800 ℃ in a crystal nucleation area at a speed of 16 ℃/min, and then carrying out heat preservation for 20 min; then reducing the temperature rise speed by 10 ℃/min, and preserving heat when the temperature rises to the maximum firing temperature of 1125 ℃, wherein the heat preservation time is 20 min; cooling to 850 deg.C for 40 min; and finally, naturally cooling to room temperature.
Example 2
The roller kiln low-temperature sintered colorful halo crystal glaze comprises a ground glaze and a cover glaze, wherein: the ground glaze comprises the following components in parts by weight: 90 parts of lead-zinc fusion cake, 3 parts of cobalt blue and 16 parts of cobalt black; the overglaze comprises the following components in parts by weight: 70 parts of high-boron clinker, 10 parts of titanium dioxide, 20 parts of zinc oxide, 15 parts of talcum, 10 parts of calcite, 20 parts of manganese dioxide, 5 parts of vanadium pentoxide and 5 parts of copper oxide.
The preparation method of the seven-color halo crystal glaze fired by the roller kiln at the low temperature comprises the following steps:
s1 preparation of ground coat:
firstly, weighing raw materials according to the weight parts of the components of the ground glaze; then putting the ground glaze into a ball mill, adding 3 wt% of dispersant and 3 wt% of dispergator, adding water, grinding for 6 hours to obtain ground glaze slurry, wherein the specific gravity of the ground glaze slurry is 1.70, and the fineness of the glaze slurry is 0.2% of ten thousand holes of screen residue; finally, filtering the ground glaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the ground glaze slip into a slip tank for ageing to prepare the colorful halo crystal ground glaze;
s2 preparation of overglaze:
firstly, weighing high-boron frit, titanium dioxide, zinc oxide, talc and calcite according to the weight parts of the overglaze; then putting the glaze slurry into a ball mill, adding 3 wt% of sodium hydroxymethyl cellulose and 3 wt% of sodium tripolyphosphate, adding water, and grinding for 6 hours to obtain overglaze glaze slip, wherein the specific gravity of the overglaze slip is 1.75, and the fineness of the glaze slip is 0.2% of ten thousand-hole screen residue; filtering the overglaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the overglaze slip into a slip tank for aging; finally, adding a seeding coloring agent into the overglaze slip and uniformly stirring to prepare the colorful halo crystal overglaze;
s3, glazing and sintering:
sequentially applying base glaze and overglaze on the ceramic biscuit by adopting a glaze spraying method, drying and then sintering in a roller kiln, wherein the sintering system is as follows: raising the temperature to 900 ℃ in a crystal nucleation area at a speed of 20 ℃/min, and then carrying out heat preservation for 30 min; then reducing the temperature rise speed by 15 ℃/min, and preserving heat when the temperature rises to the highest firing temperature of 1135 ℃, wherein the heat preservation time is 30 min; cooling to 950 deg.C for 60 min; and finally, naturally cooling to room temperature.
Example 3
The roller kiln low-temperature sintered colorful halo crystal glaze comprises a ground glaze and a cover glaze, wherein: the ground glaze comprises the following components in parts by weight: 85 parts of lead-zinc frit, 2 parts of cobalt blue and 12 parts of cobalt black; the overglaze comprises the following components in parts by weight: 60 parts of high-boron clinker, 8 parts of titanium dioxide, 15 parts of zinc oxide, 10 parts of talcum, 5 parts of calcite, 18 parts of manganese dioxide, 3 parts of vanadium pentoxide and 3 parts of copper oxide.
The preparation method of the seven-color halo crystal glaze fired by the roller kiln at the low temperature comprises the following steps:
s1 preparation of ground coat:
firstly, weighing raw materials according to the weight parts of the components of the ground glaze; then putting the ground glaze into a ball mill, adding 3 wt% of dispersant and 4 wt% of dispergator, adding water, grinding for 5 hours to obtain ground glaze slurry, wherein the specific gravity of the ground glaze slurry is 1.68, and the fineness of the glaze slurry is 0.1% of ten thousand holes of screen residue; finally, filtering the ground glaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the ground glaze slip into a slip tank for ageing to prepare the colorful halo crystal ground glaze;
s2 preparation of overglaze:
firstly, weighing high-boron frit, titanium dioxide, zinc oxide, talc and calcite according to the weight parts of the overglaze; then putting the glaze slurry into a ball mill, adding 3 wt% of sodium hydroxymethyl cellulose and 4 wt% of sodium tripolyphosphate, adding water, grinding for 5 hours to obtain a surface glaze slip, wherein the specific gravity of the surface glaze slip is 1.72, and the fineness of the glaze slip is 0.1% of ten thousand-hole screen residue; filtering the overglaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the overglaze slip into a slip tank for aging; finally, adding a seeding coloring agent into the overglaze slip and uniformly stirring to prepare the colorful halo crystal overglaze;
s3, glazing and sintering:
sequentially applying base glaze and overglaze on the ceramic biscuit by adopting a glaze spraying method, drying and then sintering in a roller kiln, wherein the sintering system is as follows: raising the temperature to 850 ℃ in a crystal nucleation area at a speed of 18 ℃/min, and then carrying out heat preservation for 25 min; then reducing the temperature rise speed by 10 ℃/min, and preserving heat when the temperature rises to the maximum firing temperature of 1130 ℃, wherein the heat preservation time is 25 min; cooling to 900 deg.C for 50 min; and finally, naturally cooling to room temperature.
The roller kiln low-temperature firing colorful halo crystal glaze prepared in the above embodiments 1-3 is prepared by selecting a proper formula and firing under a specific temperature system, and the prepared crystal glaze can present a circle of colorful halo on the glaze surface under the sun, has the process effects of metal and crystal glaze, and can adapt to the rapid low-temperature firing of the roller kiln, thereby improving the yield and reducing the cost.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are intended to be within the scope of the invention.

Claims (10)

1. A roller kiln low-temperature firing colorful halo crystal glaze is characterized in that: comprises a ground coat and a surface coat,
the ground glaze comprises the following components in parts by weight: 80-90 parts of lead-zinc frit and 10-20 parts of pigment;
the overglaze comprises the following components in parts by weight: 50-70 parts of high-boron clinker, 5-10 parts of titanium dioxide, 10-20 parts of zinc oxide, 5-15 parts of talc, 0-10 parts of calcite and 17-30 parts of seeding coloring agent, wherein the seeding coloring agent is manganese dioxide, vanadium pentoxide and copper oxide.
2. The roller kiln low-temperature fired seven-color halo crystal glaze according to claim 1, characterized in that: the lead-zinc frit comprises the following chemical components in percentage by weight: SiO 22 51%;Al2O3 4%;K2O 4%;Na2O 7%;CaO 4%;MgO 2%;ZnO 5%;PbO 23%。
3. The roller kiln low-temperature fired seven-color halo crystal glaze according to claim 1, characterized in that: the high-boron frit comprises the following chemical components in percentage by weight: SiO 22 59%;Al2O3 5%;Na2O 14%;B2O3 22%。
4. The roller kiln low-temperature fired seven-color halo crystal glaze according to claim 1, characterized in that: the grain diameter of the seeding coloring agent is as follows: 20-30 nm.
5. The roller kiln low-temperature fired seven-color halo crystal glaze according to claim 4, characterized in that: the seeding coloring agent comprises the following components in parts by weight: 15-20 parts of manganese dioxide, 1-5 parts of vanadium pentoxide and 1-5 parts of copper oxide.
6. The roller kiln low-temperature fired seven-color halo crystal glaze according to claim 1, characterized in that: the pigment is one or two of cobalt blue and cobalt black.
7. The method for preparing the seven-color halo crystal glaze fired by the roller kiln at low temperature according to any one of claims 1 to 6, is characterized in that: the method comprises the following steps:
s1 preparation of ground coat:
firstly, weighing raw materials according to the weight parts of the components of the ground glaze; then putting the ground glaze into a ball mill, adding 1-4 wt% of dispersant and 2-5 wt% of dispergator, adding water, grinding for 4-6 hours to obtain ground glaze slurry, wherein the fineness of the glaze slurry is 0.1-0.2% of ten thousand holes of screen residue; finally, filtering the ground glaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the ground glaze slip into a slip tank for ageing to prepare the colorful halo crystal ground glaze;
s2 preparation of overglaze:
firstly, weighing high-boron frit, titanium dioxide, zinc oxide, talc and calcite according to the weight parts of the overglaze; then putting the glaze slurry into a ball mill, adding 1-4 wt% of dispersant and 2-5 wt% of dispergator, adding water, grinding for 4-6 hours to obtain overglaze glaze slurry with the fineness of 0.1-0.2% of ten thousand holes of screen residue; filtering the overglaze slip by a double-layer sieve of 100 meshes, removing iron, pumping the overglaze slip into a slip tank for aging; finally, adding a seeding coloring agent into the overglaze slip and uniformly stirring to prepare the colorful halo crystal overglaze;
s3, glazing and sintering:
sequentially applying base glaze and overglaze on the ceramic biscuit by adopting a glaze spraying method, drying and then sintering in a roller kiln, wherein the maximum sintering temperature is 1125-shaped and 1135 ℃, the sintering period is 190-shaped and 210min, and simultaneously, the heat preservation is respectively carried out in a crystal nucleation area, a high-temperature sintering area and a crystal growth area.
8. The preparation method of the seven-color halo crystal glaze fired in the roller kiln at low temperature according to claim 7 is characterized in that: the specific gravity of the ground glaze slip is 1.65-1.70.
9. The preparation method of the seven-color halo crystal glaze fired in the roller kiln at low temperature according to claim 7 is characterized in that: the specific gravity of the overglaze slip is 1.70-1.75.
10. The preparation method of the seven-color halo crystal glaze fired in the roller kiln at low temperature according to claim 7 is characterized in that: and respectively preserving the heat of a crystal nucleation area, a high-temperature sintering area and a crystal growth area which are sintered by the colorful halo crystal glaze for 20-60 min.
CN202011554852.7A 2020-12-25 2020-12-25 Roller kiln low-temperature sintered colorful halo crystal glaze and preparation method thereof Active CN112266271B (en)

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CN112794736A (en) * 2021-04-09 2021-05-14 蒙娜丽莎集团股份有限公司 Ceramic plate with colorful cloud surface decoration effect and preparation method thereof
CN113354284A (en) * 2021-06-10 2021-09-07 佛山欧神诺陶瓷有限公司 Ceramic glaze material with seven-color halo effect, ceramic rock plate and preparation method and application thereof
CN114195387A (en) * 2021-12-24 2022-03-18 佛山市玉矶材料科技有限公司 Colorful silver wire glaze and manufacturing process thereof
CN114195387B (en) * 2021-12-24 2023-10-13 佛山市玉矶材料科技有限公司 Colorful silver silk glaze and manufacturing process thereof
CN115784777A (en) * 2022-11-16 2023-03-14 珠海市斗门区旭日陶瓷有限公司 Manufacturing process of furnace transmutation brick
CN115784777B (en) * 2022-11-16 2023-09-29 珠海市斗门区旭日陶瓷有限公司 Process for manufacturing kiln transformation brick

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