CN110790506A - Granular double-layer reaction glaze and preparation method thereof - Google Patents

Granular double-layer reaction glaze and preparation method thereof Download PDF

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CN110790506A
CN110790506A CN201911308602.2A CN201911308602A CN110790506A CN 110790506 A CN110790506 A CN 110790506A CN 201911308602 A CN201911308602 A CN 201911308602A CN 110790506 A CN110790506 A CN 110790506A
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parts
glaze
calcined
overglaze
slip
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邹建华
汪大谷
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HUNAN HUALIAN CERAMICS CO Ltd
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HUNAN HUALIAN CERAMICS CO Ltd
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    • 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
    • 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
    • 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
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • 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

Abstract

The invention belongs to the technical field of ceramic glaze, and particularly relates to a granular double-layer reaction glaze and a preparation method thereof, wherein the granular double-layer reaction glaze comprises the following components in parts by weight: base glaze: 30-40 parts of albite, 5-15 parts of quartz, 5-15 parts of wollastonite, 2-6 parts of calcined alumina, 25-35 parts of kaolin and 15-25 parts of a coloring agent; overglaze: 35-45 parts of high-boron frit, 15-25 parts of quartz, 5-10 parts of wollastonite, 5-15 parts of spodumene, 10-20 parts of calcined zinc oxide, 5-15 parts of kaolin, 5-10 parts of calcined talc, 5-10 parts of titanium dioxide and 5-15 parts of zirconium silicate; the invention has short sintering time, higher thermal shock resistance and glaze hardness.

Description

Granular double-layer reaction glaze and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic glaze materials, and particularly relates to a granular double-layer reaction glaze and a preparation method thereof.
Background
At present, 1200-cost 1250-DEG C medium-temperature kiln color-changing glaze products produced in China are mainly made of common reaction glaze surfaces, the reaction effect is rough and unstable, the aesthetic feeling of the glaze surfaces is not good enough, the aesthetic feeling and material requirements of consumers which are improved day by day cannot be met, and with the trend of young consumers to good life in the future, higher-grade life ceramics are pursued, so that granular double-layer reaction glaze appears. The granular double-layer reaction glaze is glaze with a Duka reaction effect and a granular crystallization effect on the surface, and has better thermal shock resistance and glaze hardness than common reaction glaze and is very stable. The common reactive glaze is mainly common transmutation color glaze, and granular double-layer reactive color glaze products are very rare in the international market. In general, the granular double-layer reaction glaze product has very strong artistry, good appreciation and high value, and is popular with consumers. The product has strong reproducibility, the process requires the adoption of ground glaze and overglaze, the firing system has no special requirement, and the conditions of the fineness of the glaze, the thickness of the glaze layer, the blank body and the like are the same as those of common glaze, so the granular double-layer reaction glaze can adapt to large-scale production.
The study on firing system of double-layer reaction glaze ceramic products, Yangzhong, Fushan ceramic, No. 4 of 2011, describes the reaction mechanism of double-layer glaze transmutation, namely, an upper layer glaze and a lower layer glaze are applied on a biscuit, the glaze close to the biscuit is called ground glaze, and the glaze applied on the ground glaze is called overglaze. And drying the glazed green body, putting the dried green body into a kiln, and preheating the green body to reach the oxidative decomposition and crystal form conversion period. Due to the special matching composition of the transmutation glaze, at the stage, gas generated by oxidation and decomposition of partial components in the ground glaze penetrates through the overglaze to be discharged. In the burning zone, the bottom and the surface glaze are in a molten state and react with each other. Under the action of kiln atmosphere, owing to the valence change of the elements in the bottom and cover glazes and the biochemical reaction between the bottom and cover glazes, the variegated and variegated kiln transmutation effect is formed. Tables 1-4 show different under and over glaze formulations. Typical ground coat compositions include: feldspar, quartz, suzhou earth, reaction clinker, iron oxide and manganese oxide, and in addition calcite, calcined talc and calcined zinc oxide. Common overglazes include feldspar, quartz, suzhou earth, calcite, zinc oxide, titanium dioxide, reaction frits, bone ash, and barium carbonate. As large flow does not need to be generated between the ground glaze and the overglaze and the ground glaze and the overglaze are required to be fully reacted, the firing temperature of the kiln is lower and is 1160-1200 ℃, the firing heat preservation time is long, so that enough time is provided for the ground glaze and the overglaze to be fully reacted, and the firing period is more than 18 h. If the temperature is high, the bottom glaze and the surface glaze are dislocated, small patterns appear, and the whole decoration effect is easily influenced. The sintering time is longer, and the benefit of the product is influenced.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a granular double-layer reaction glaze and a preparation method thereof, wherein the granular double-layer reaction glaze has short sintering time, and has higher thermal shock resistance and glaze hardness.
The invention relates to a granular double-layer reaction glaze, which comprises the following components in parts by weight:
base glaze: 30-40 parts of albite, 5-15 parts of quartz, 5-15 parts of wollastonite, 2-6 parts of calcined alumina, 25-35 parts of kaolin and 15-25 parts of a coloring agent;
overglaze: 35-45 parts of high-boron frit, 15-25 parts of quartz, 5-10 parts of wollastonite, 5-15 parts of spodumene, 10-20 parts of calcined zinc oxide, 5-15 parts of kaolin, 5-10 parts of calcined talc, 5-10 parts of titanium dioxide and 5-15 parts of zirconium silicate.
Preferably, the composition comprises the following components in parts by weight:
base glaze: 35 parts of albite, 8 parts of quartz, 8 parts of wollastonite, 4 parts of calcined alumina, 25 parts of kaolin and 15-25 parts of a coloring agent;
overglaze: 35 parts of high-boron frit, 18 parts of quartz, 8 parts of wollastonite, 8 parts of spodumene, 12 parts of calcined zinc oxide, 10 parts of kaolin, 6 parts of calcined talc, 6 parts of titanium dioxide and 8 parts of zirconium silicate.
Preferably, the colorant is one of dark brown or cobalt nickel ash.
The invention provides a preparation method of granular double-layer reaction glaze, which comprises the following steps:
1) preparing materials according to the components and the mass parts of the components, and preparing the following raw materials: high alumina ball stone: the mass ratio of water is 1:2:0.6, and wet ball milling is carried out to obtain ground glaze and surface glaze, wherein the fineness of the ground glaze and the surface glaze is 325 meshes, and the residual quantity is 0.05-0.12%; the mass ratio of the large spherulites, the medium spherulites and the small spherulites in the high-alumina spherulites is preferably 2: 5: 3.
2) the ground glaze and the overglaze glaze are sieved by a 120-mesh sieve after going out of a ball mill to obtain ground glaze slip and overglaze slip, water and electrolyte (preferably sodium silicate or sodium humate) are added to adjust the concentration and thixotropy of the ground glaze slip and the overglaze slip, the concentration of the ground glaze slip is 20-30 baume degrees, and the concentration of the overglaze slip is 50-60 baume degrees;
3) soaking the glaze blank in the ground glaze slurry, spraying the surface glaze slurry, drying, sintering in a roller kiln at the highest temperature of 1200-1250 ℃ for 4.5-5.5h to obtain the granular double-layer reaction glaze.
The chemical composition analysis of each component in the raw material of the present invention is shown in table 1.
TABLE 1 analysis table of chemical components of raw materials
SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O ZnO B2O3
Albite 73.39 14.59 0.27 0.02 0.45 0.03 1.6 9.8
Quartz crystal 99.2 0.34 0.1
Calcite 53.7 1.27 0.16
Calcined talc 0.19 4.93 30.18
High boron frit 56.5 4.05 9.04 8.19 4.15 8.25 9.82 8.19
Kaolin clay 47.3 36.66 0.68 0.05 0.06 0.24 1.95 0.13
The high-boron clinker is produced in the city of Hunan eclipta, and is granular or powdery; the albite powder is produced from the Mazizhen of Hengshan county in Hunan province, and is grey white and powdery; the quartz powder is produced in the city of carignane in Hunan province and is in a fine sand shape; the wollastonite powder is produced in Shanghai city in Jiangxi, and the content of calcium oxide is more than or equal to 46 percent; the calcined talcum powder is produced in Yulin city in Guangxi, and the content of magnesium oxide is more than or equal to 34.5%; the calcined zinc oxide is produced in shouxia city of Hunan province, and the content of the zinc oxide is more than or equal to 98.5 percent; the calcined alumina is produced in Henan province, and the alumina content is more than or equal to 99 percent; the kaolin is produced from Longyan city in Fujian province; the toner is produced from Zibo, Shandong province.
The invention has the beneficial effects that the raw materials generate dense granular titanium silicate crystals at the medium temperature, and magnesium oxide introduced by calcined talcum powder is added to form a silicate glass phase and a pyroxene crystal phase with silicon dioxide and metal oxide, so that the two phases are not mutually soluble, the dissolving capacities of the two phases to the coloring agent are different, the color difference is generated, and the ceramic products with various colors can be obtained.
The granular double-layer reaction glaze obtained in the invention has the advantages that the glaze surface of the granular double-layer reaction glaze is blended and distributed in a staggered manner, the whole glaze surface is like a waterfall flowing in the cloud sea, and the glaze surface is bright, good in hand feeling, strong in artistry and ornamental; the product of the invention has short sintering time and low energy consumption, is suitable for large-scale production, and simultaneously has physical and chemical properties of thermal shock resistance, lead and cadmium dissolution, glaze hardness and the like which reach or exceed the national relevant standards of daily fine porcelain.
The high-boron frit is a boron-containing strong flux, has the functions of forming glass with other silicates and promoting phase separation, and can also reduce the high-temperature viscosity of the glaze and increase the glossiness of the glaze surface.
Albite can be a flux of a plurality of glazes, silicon dioxide, aluminum oxide, sodium oxide and potassium oxide can be simultaneously introduced, metal oxide is introduced into the glazes to serve as a suitable raw material, potassium oxide and sodium oxide alkali metal are strong cosolvents, melting temperature and viscosity of the glazes can be reduced, refractive index of the glazes can be increased, glossiness of the glazes can be improved, and chemical stability and mechanical strength of the glazes can be reduced. The expansion coefficient of sodium oxide in alkali metal is the largest, and the expansion coefficient of the glaze can be reduced by silicon dioxide, so that the elasticity, the thermal stability and the chemical stability of the glaze are improved.
Quartz powder: in the glaze, silicon dioxide is a main component for generating glass, and the melting temperature and viscosity of the glaze can be improved and the expansion coefficient of the glaze can be reduced by increasing the quartz content in the glaze. At the same time it is the main reason for imparting high strength, hardness, abrasion resistance and chemical aggressiveness to the glaze.
Wollastonite powder: the main component of the wollastonite is calcium oxide and silicon oxide, and proper calcium oxide is added in experiments to increase glaze glossiness of the glaze, improve the bonding effect of blank glaze and prevent cracking of the glaze; the reaction glaze reacts with zirconium silicate to form crystals, so that the reaction glaze has high thermal shock resistance and glaze hardness on the basis of short sintering time, and the economic benefit is improved.
Calcining talcum powder: the main component of the calcined talcum powder is magnesium oxide, and the magnesium oxide can promote crystallization, reduce expansion coefficient and improve the hardness of a glaze surface.
Calcining zinc oxide: the zinc oxide can increase the elasticity and glossiness of the glaze, so that the glaze is moist, fine and smooth and has jade texture.
Calcined alumina the main component of calcined alumina is α -Al2O3The alumina and the silicon dioxide are matched together, so that the mechanical strength and the hardness of the glaze are improved, the chemical corrosion resistance of the surface of the glaze is improved, the expansion coefficient of the glaze is reduced, the melting temperature of the glaze is increased, and the sintering reaction time is shortened.
Kaolin: and substances such as alumina, silicon dioxide and the like are introduced, so that the glaze has suspension property and stability.
Color agent: the granular reaction glaze products with different colors can be obtained by adjusting the color of the glaze.
The main difference between calcined talc powder and uncalcined talc powder is that the layered structure of the raw talc powder is destroyed after calcination, which is beneficial to improving the ball milling efficiency.
The calcined zinc oxide is mainly different from the uncalcined zinc oxide in that the thixotropy of raw zinc oxide is reduced after calcination, and the operation performance of the glaze slip is improved.
The industrial alumina is mainly composed of α -Al2O3And gamma-Al2O3The composition was a white amorphous powder. gamma-Al2O3Is converted into α -Al by calcination2O3The method is accompanied by about 14 percent of volume shrinkage, so that the industrial alumina powder needs to be pre-sintered before proportioning, and the gamma-Al is added2O3Fully converted into α -Al2O3When preventing firing, due to gamma-Al2O3Conversion to α -Al2O3The volume shrinkage occurs, and the quality problems of product cracking, deformation and the like occur. The calcined alumina is different from uncalcined alumina in that the most stable aluminum powder crystal structure is generated after calcination, and the pinhole defect of the glaze surface is greatly reduced.
The operation of calcining alumina is that industrial alumina is calcined at 1450 deg.C or higher, gamma-Al2O3Conversion to α -Al2O3
The reaction glaze can be prepared by the following three methods: 1. the ground glaze has large high-temperature viscosity and the surface glaze has small high-temperature viscosity, and the reaction is generated by utilizing the high-temperature viscosity difference; 2. the ground glaze is the cosmetic soil, and the surface glaze is the high-zinc high-magnesium reaction glaze; 3. the surface tension of the ground glaze is large, the surface tension of the overglaze is small, and patterns are generated by utilizing the difference of the surface tensions. In actual production, the first method and the second method are adopted more, and the third method has poor aesthetic feeling and insufficient market share.
The above reaction glazes have advantages and disadvantages, and the first reaction glaze has the advantages of easy reaction and wide application range; the disadvantage is that the fluidity of the overglaze is too high and the production is difficult to control. The second reaction glaze has the advantages of good glaze effect and high glossiness; the disadvantage is that it is less stable. The third reaction glaze has the advantages of good stability; the disadvantage is the lack of aesthetic effect of the reaction.
The invention mainly uses the raw materials to generate dense granular titanium silicate crystals at medium temperature, and magnesium oxide introduced by adding calcined talcum powder can form silicate glass phase and pyroxene crystal phase with silicon dioxide and metal oxide, the two phases are not mutually soluble and have different dissolving capacities for a color agent, so that the color difference is generated, and the ceramic products with various colors can be obtained.
The zinc oxide is added, and the components and the proportion of the raw materials are adjusted to ensure the high-temperature viscosity and the surface tension, so that the purposes of improving the glaze quality, enhancing the aesthetic effect and enabling the physical and chemical properties of the product to reach the national standard are achieved.
By adding wollastonite powder and zirconium silicate and adjusting the proportion of quartz powder and kaolin, the thermal shock resistance and the glaze hardness can be improved on the basis of lower firing time.
The glaze is divided into low-temperature glaze, medium-temperature glaze and high-temperature glaze according to the firing temperature.
The firing temperature of the low-temperature glaze is lower, and more glaze materials are easily not melted below 1200 ℃, so that the glaze surface is rough, has gaps and is not smooth, and the attractiveness and the service performance are influenced. The high-temperature glaze firing temperature is higher and is more than 1300 ℃, so that the glaze is easy to be fully melted through, the range of an opacification area is small, the range of a gloss area is large, the matt effect is lost, the energy consumption is high, and the high-temperature glaze firing method is not suitable for large-scale production. Therefore, the invention adopts middle temperature firing at 1200-1250 ℃, and the obtained granular double-layer reaction glaze has good reaction effect, smooth and delicate glaze surface and low production energy consumption.
According to the invention, the thixotropy of the glaze slip is reduced by adding the calcined zinc oxide, the operation performance of the glaze slip is improved, and the thickness of the glaze layer of the glazed blank is 0.3-0.6 mm.
The glaze slurry is sieved to prevent impurities brought by the glaze material in the ball mill process, such as small broken particles of ball milling media (namely ball stones and ball milling linings) in a ball mill, impurity particles brought by a discharge port of the ball mill and the like, and the impurities can be sieved out by a 120-mesh sieve generally.
The thixotropy is mainly tested by a Ford cup in the aspect of ceramic production and is mainly tested by practice, namely the glaze is used well in the using process and glaze defects such as glaze strands, glaze ribs and the like are not generated.
Drawings
Fig. 1 is a diagram of the shape of the glaze of the present invention.
Detailed Description
Example 1
Base glaze in parts by weight: 35 parts of albite powder, 8 parts of quartz powder, 8 parts of wollastonite powder, 4 parts of calcined alumina, 25 parts of kaolin and 20 parts of dark brown. Overglaze: 35 parts of high-boron frit, 18 parts of quartz powder, 8 parts of wollastonite, 8 parts of spodumene, 12 parts of calcined zinc oxide, 10 parts of kaolin, 6 parts of calcined talc, 6 parts of titanium dioxide and 8 parts of zirconium silicate. Adding the materials into a ball mill for ball milling, and then adding water into the ball mill, wherein the raw materials are as follows: ball: the mass ratio of water is 1:2:0.6, and the mass ratio of the medium and large spherulites to the mass ratio of the small spherulites is 2: 5: 3, the mixture is added into a ball mill for 24 hours, and the fineness of the glaze obtained after ball milling is controlled to be 0.05-0.08 percent of the rest of 325 meshes. And (3) sieving the glaze material by a 120-mesh sieve after the glaze material is discharged from a ball mill to obtain glaze slip, then measuring the concentration of the glaze slip, determining the required glaze slip concentration according to different model types, and adding water to adjust the concentration of the glaze slip to be 25 baume degrees of the ground glaze and 55 baume degrees of the overglaze. And simultaneously, sodium humate with five parts per million of total mass is added to adjust the thixotropy of the glaze slip to achieve the optimal condition. And (3) soaking the glaze blank in the glaze slurry, drying for 2h at 50 ℃, putting the dried glaze blank into a roller kiln for sintering, wherein the highest temperature is 1250 ℃, the sintering period is 4.5h, the sintering curve is the conventional moderate-temperature white porcelain sintering curve of the roller kiln, the atmosphere is oxidizing flame, and the thickness of the finally obtained glaze layer of the glaze blank is 0.45 mm.
Example 2
Base glaze in parts by weight: 40 parts of albite powder, 12 parts of quartz powder, 5 parts of wollastonite powder, 2 parts of calcined alumina, 26 parts of kaolin and 15 parts of dark brown. Overglaze: 40 parts of high-boron frit, 13 parts of quartz powder, 10 parts of wollastonite, 5 parts of spodumene, 10 parts of calcined zinc oxide, 7 parts of kaolin, 5 parts of calcined talc, 6 parts of titanium dioxide and 8 parts of zirconium silicate. Adding the materials into a ball mill for ball milling, and then adding water into the ball mill, wherein the raw materials are as follows: ball: the mass ratio of water is 1:2:0.6, and the mass ratio of the medium and large spherulites to the mass ratio of the small spherulites is 2: 5: 3, the mixture is added into a ball mill for 24 hours, and the fineness of the glaze obtained after ball milling is controlled to be 0.1-0.12 percent of the rest of 325 meshes. And (3) sieving the glaze material by a 120-mesh sieve after the glaze material is discharged from a ball mill to obtain glaze slip, then measuring the concentration of the glaze slip, determining the required glaze slip concentration according to different model types, and adding water to adjust the concentration of the glaze slip to be 25 baume degrees of the ground glaze and 55 baume degrees of the overglaze. And simultaneously, sodium humate with five parts per million of total mass is added to adjust the thixotropy of the glaze slip to achieve the optimal condition. Soaking a glaze blank in the glaze slurry, drying at 50 ℃ for 2h, putting the dried glaze blank into a roller kiln for firing, wherein the highest temperature is 1230 ℃, the firing period is 5h, the firing curve is the conventional moderate-temperature white porcelain firing curve of the roller kiln, the atmosphere is oxidizing flame, and the thickness of the finally obtained glaze layer of the glaze blank is 0.55 mm.
Example 3
Base glaze in parts by weight: 30 parts of albite powder, 12 parts of quartz powder, 5 parts of wollastonite powder, 6 parts of calcined alumina, 25 parts of kaolin and 24 parts of dark brown. Overglaze: 45 parts of high-boron frit, 15 parts of quartz powder, 5 parts of wollastonite, 11 parts of spodumene, 10 parts of calcined zinc oxide, 7 parts of kaolin, 5 parts of calcined talc, 6 parts of titanium dioxide and 8 parts of zirconium silicate. Adding the materials into a ball mill for ball milling, and then adding water into the ball mill, wherein the raw materials are as follows: ball: the mass ratio of water is 1:2:0.6, and the mass ratio of the medium and large spherulites to the mass ratio of the small spherulites is 2: 5: 3, the mixture is added into a ball mill for 24 hours, and the fineness of the glaze obtained after ball milling is controlled to be 0.08-0.12 percent of the rest of 325 meshes. Sieving the glaze material with a 120-mesh sieve after the glaze material is discharged from a ball mill to obtain glaze slip, then measuring the concentration of the glaze slip, determining the required glaze slip concentration according to different model types, and adding water to adjust the concentration of the glaze slip to be 30 baume degrees of the ground glaze and 60 baume degrees of the overglaze. And simultaneously, sodium humate with the total mass of eight ten-thousandth is added to adjust the thixotropy of the glaze slip to achieve the optimal condition. And (3) soaking the glaze blank in the glaze slurry, drying for 2h at 50 ℃, putting the dried glaze blank into a roller kiln for sintering, wherein the highest temperature is 1210 ℃, the sintering period is 5.5h, the sintering curve is the conventional moderate-temperature white porcelain sintering curve of the roller kiln, the atmosphere is oxidizing flame, and the thickness of the finally obtained glaze layer of the glaze blank is 0.65 mm.
Comparative example 1
The base glaze comprises the following components in parts by weight: 40 parts of albite powder, 5 parts of quartz powder, 15 parts of wollastonite powder, 2 parts of calcined alumina, 23 parts of kaolin and 15 parts of dark brown. Overglaze: 45 parts of high-boron frit, 5 parts of quartz powder, 15 parts of wollastonite, 3 parts of spodumene, 8 parts of calcined zinc oxide, 7 parts of kaolin, 3 parts of calcined talc, 6 parts of titanium dioxide and 3 parts of zirconium silicate. Adding the materials into a ball mill for ball milling, and then adding water into the ball mill, wherein the raw materials are as follows: ball: the mass ratio of water is 1:2:0.6, and the mass ratio of the medium and large spherulites to the mass ratio of the small spherulites is 2: 5: 3, the mixture is added into a ball mill for 24 hours, and the fineness of the glaze obtained after ball milling is controlled to be 0.1-0.12 percent of the rest of 325 meshes. And (3) sieving the glaze material by a 120-mesh sieve after the glaze material is discharged from a ball mill to obtain glaze slip, then measuring the concentration of the glaze slip, determining the required glaze slip concentration according to different model types, and adding water to adjust the concentration of the glaze slip to be 25 baume degrees of the ground glaze and 55 baume degrees of the overglaze. And simultaneously, sodium humate with five parts per million of total mass is added to adjust the thixotropy of the glaze slip to achieve the optimal condition. Soaking the glaze blank in the glaze slurry, drying at 50 ℃ for 2h, putting the dried glaze blank into a roller kiln for sintering, wherein the highest temperature is 1220 ℃, the sintering period is 5h, the sintering curve is the conventional moderate-temperature white porcelain sintering curve of the roller kiln, the atmosphere is oxidizing flame, and the thickness of the finally obtained glaze layer of the glaze blank is 0.45 mm.
The properties of the matt glazes obtained in examples 1 to 3 and comparative example 1 were compared and the results are given in table 1.
TABLE 1 comparison of the Properties of particulate double-layer reactive glazes
Product(s) Degree of gloss Thermal stability Hardness of glaze
Example 1 70 Without cracks No scratch
Example 2 75 Without cracks No scratch
Example 3 80 Without cracks No scratch
Comparative example 1 85 Without cracks Has slight scratch
The gloss effect of the granular double-layer reaction glaze product was determined by visual inspection, and the gloss value was determined by a german color difference meter.
The thermal shock resistance is measured by heating and quenching, placing the granular double-layer reaction glaze product in an electric furnace heated to 160 ℃, preserving the heat for 30min, quickly putting the granular double-layer reaction glaze product into water at 20 ℃ for 10min, taking out the granular double-layer reaction glaze product, wiping the granular double-layer reaction glaze product, and checking whether cracks and burst cracks exist.
The determination of the glaze hardness is to use a knife and fork tester to detect the glaze, determine the degree of relative glaze scratch, and divide the glaze into a traceless trace, a light grey trace and a dark grey trace.
The data in the table show that the granular double-layer reaction glaze obtained in the embodiment has high glossiness and good reaction effect, magnesium oxide introduced by adding calcined talcum powder can form a silicate glass phase and a pyroxene crystal phase with silicon dioxide and metal oxide, the two phases are not mutually soluble, the dissolving capacity of a colorant is different, color difference is generated, ceramic products with various colors can be obtained, and the artistic value of the ceramic products is greatly improved.

Claims (8)

1. A granular double-layer reaction glaze is characterized by comprising the following components in parts by weight:
base glaze: 30-40 parts of albite, 5-15 parts of quartz, 5-15 parts of wollastonite, 2-6 parts of calcined alumina, 25-35 parts of kaolin and 15-25 parts of a coloring agent;
overglaze: 35-45 parts of high-boron frit, 15-25 parts of quartz, 5-10 parts of wollastonite, 5-15 parts of spodumene, 10-20 parts of calcined zinc oxide, 5-15 parts of kaolin, 5-10 parts of calcined talc, 5-10 parts of titanium dioxide and 5-15 parts of zirconium silicate.
2. The granular double-layer reaction glaze of claim 1, which is characterized by comprising the following components in parts by weight:
base glaze: 35 parts of albite, 8 parts of quartz, 8 parts of wollastonite, 4 parts of calcined alumina, 25 parts of kaolin and 15-25 parts of a coloring agent;
overglaze: 35 parts of high-boron frit, 18 parts of quartz, 8 parts of wollastonite, 8 parts of spodumene, 12 parts of calcined zinc oxide, 10 parts of kaolin, 6 parts of calcined talc, 6 parts of titanium dioxide and 8 parts of zirconium silicate.
3. The granular double-layer reaction glaze according to claim 1 or 2, wherein the colorant is one of dark brown or cobalt nickel ash.
4. A method for producing a granular double-layer reaction glaze according to any one of claims 1 to 3, comprising the steps of:
1) preparing materials according to the components and the mass parts of the components, and preparing the following raw materials: high alumina ball stone: the mass ratio of water is 1:2:0.6, and wet ball milling is carried out to obtain a ground glaze material and a surface glaze material;
2) the ground glaze and the overglaze glaze are sieved by a 120-mesh sieve after being discharged from a ball mill to obtain ground glaze slip and overglaze slip, water and electrolyte are added to adjust the concentration and thixotropy of the ground glaze slip and the overglaze slip, the concentration of the ground glaze slip is 20-30 baume degrees, and the concentration of the overglaze slip is 50-60 baume degrees;
3) taking a glaze blank, soaking the glaze blank in the ground glaze slurry, spraying the surface glaze slurry, drying, and sintering the dried glaze blank in a roller kiln at the maximum temperature of 1200-1250 ℃ for a sintering period of 4.5-5.5h to obtain the granular double-layer reaction glaze.
5. The method according to claim 4, wherein the electrolyte in step 2) is sodium silicate or sodium humate.
6. The method according to claim 4, wherein the fineness of the ground and cover glaze materials of step 1) is 0.05-0.12% of 325 mesh.
7. The method according to any one of claims 4 to 6, wherein the mass ratio of the large pebbles, the medium pebbles and the small pebbles in the high alumina pebbles in the step 1) is 2: 5: 3.
8. the production method according to any one of claims 4 to 6, wherein the firing atmosphere is an oxidizing atmosphere.
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CN111233327A (en) * 2020-04-27 2020-06-05 佛山市东鹏陶瓷有限公司 Low-temperature wear-resistant frit, wear-resistant glaze material using same and glazed tile
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