CN115838245B - Micro-gloss glaze material for separating microcrystals, micro-gloss ceramic rock plate with ultra-flat fine glaze surface and preparation method thereof - Google Patents

Micro-gloss glaze material for separating microcrystals, micro-gloss ceramic rock plate with ultra-flat fine glaze surface and preparation method thereof Download PDF

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CN115838245B
CN115838245B CN202211455886.XA CN202211455886A CN115838245B CN 115838245 B CN115838245 B CN 115838245B CN 202211455886 A CN202211455886 A CN 202211455886A CN 115838245 B CN115838245 B CN 115838245B
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glaze
parts
micro
oxide
gloss
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CN115838245A (en
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黄春林
谢怡伟
徐雪英
朱光耀
陈育昆
仝松贞
傅建涛
宁毓胜
袁小娣
戴志梅
简润桐
叶德林
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New Pearl Guangdong New Materials Co ltd
Foshan Sanshui Newpearl Building Ceramic Industry Co Ltd
Hubei Newpearl Green Building Material Technology Co Ltd
Jiangxi Xinmingzhu Building Materials Co Ltd
Newpearl Group Co Ltd
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New Pearl Guangdong New Materials Co ltd
Foshan Sanshui Newpearl Building Ceramic Industry Co Ltd
Hubei Newpearl Green Building Material Technology Co Ltd
Jiangxi Xinmingzhu Building Materials Co Ltd
Newpearl Group Co Ltd
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/60Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

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Abstract

The invention relates to the technical field of preparation of ceramic rock plates, and discloses a micro-gloss glaze material for separating microcrystals, a micro-gloss ceramic rock plate with an ultra-flat fine glaze surface and a preparation method thereof, wherein the micro-gloss ceramic rock plate is prepared by firing a green body layer, a ground glaze layer, a pattern layer and a dry grain glaze layer which are sequentially stacked from bottom to top, the material for preparing the dry grain glaze layer is the micro-gloss glaze material, and the micro-gloss glaze material comprises the following components in parts by weight: 100-160 parts of transparent protective glaze slurry, 25-55 parts of dry granular powder and 20-50 parts of suspending agent, wherein the raw materials for preparing the dry granular powder comprise, by weight, 20-40 parts of potassium feldspar, 10-30 parts of albite, 5-20 parts of nepheline, 5-10 parts of kaolin, 10-20 parts of barium carbonate, 5-10 parts of wollastonite, 3-8 parts of zinc oxide, 5-15 parts of strontium carbonate, 5-10 parts of calcite and 2-8 parts of aluminum oxide. The glossiness of the prepared micro-gloss ceramic rock plate is between 10 and 15 ℃, and the surface of the micro-gloss ceramic rock plate has ultra-flat and fine particle touch feeling.

Description

Micro-gloss glaze material for separating microcrystals, micro-gloss ceramic rock plate with ultra-flat fine glaze surface and preparation method thereof
Technical Field
The invention relates to the technical field of ceramic rock plates, in particular to a micro-gloss glaze material for precipitation microcrystals, a micro-gloss ceramic rock plate with an ultra-flat fine glaze surface and a preparation method thereof.
Background
As a novel material, the ceramic rock plate has physical properties obviously superior to those of the traditional ceramic tiles, and has an increasing share in the ceramic market. The technical effects of the rock plate surface mainly comprise from the luster point of view: three kinds of light, soft light and matte. The bright light is the mirror surface effect with the brightness of more than 50 degrees after polishing, wherein the glossiness is relatively bright; soft light refers to a mirror effect with a gloss of about 15-30 degrees after polishing; matte is generally defined as a photometric texture with a gloss level of less than 15 degrees and even zero degrees. With the emergence of new generation consumers, the demand for matte products is continuously rising, and the matte texture is higher and resistant to seeing, so that the requirements of young consumers are met.
At present, a matte glaze is generally adopted for a ceramic rock plate to realize a matte effect, for example, anorthite glaze is adopted, a large amount of fine crystals are precipitated in a glaze glass body, the fine crystals are uniformly distributed from the surface of a glaze layer to the inside, the surface of the glaze layer is uneven and is observed in an SEM scanning electron microscope image to be in a wavy state, the specular reflection of incident light is weakened, the diffuse reflection is enhanced, and the precipitated fine crystals are mainly anorthite crystals and albite crystals. Although the matte glaze can realize a matte effect, the proportion of the glaze with more phases and less crystal phases in the internal microstructure is unreasonable, and the matte glaze is characterized by planeness deviation in a macroscopic sense, so that ultra-flat and fine particle touch feeling is not achieved.
Accordingly, the prior art is still in need of improvement and development.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a micro-gloss glaze material for separating microcrystals, a micro-gloss ceramic rock plate with an ultra-flat fine glaze surface and a preparation method thereof, and aims to solve the problem that the existing micro-gloss ceramic rock plate does not have ultra-flat fine particle touch feeling.
The technical scheme of the invention is as follows:
A micro-gloss glaze for separating microcrystals, wherein the micro-gloss glaze comprises the following components in parts by weight: 100-160 parts of transparent protective glaze slip, 25-55 parts of dry particle powder and 20-50 parts of suspending agent, wherein the chemical composition of the dry particle powder comprises the following components in percentage by mass: 50-55% of silicon dioxide, 18-21% of aluminum oxide, 2-5% of potassium oxide, 3-6% of sodium oxide, 3-6% of calcium oxide, 0.1-0.5% of magnesium oxide, 2-5% of zinc oxide, 10-16% of barium oxide, 4-8% of strontium oxide and the balance of trace impurities and burning.
The micro-gloss glaze for separating microcrystals comprises the following raw materials in parts by weight: 20-40 parts of potassium feldspar, 10-30 parts of albite, 5-20 parts of nepheline, 5-10 parts of kaolin, 10-20 parts of barium carbonate, 5-10 parts of wollastonite, 3-8 parts of zinc oxide, 5-15 parts of strontium carbonate, 5-10 parts of calcite and 2-8 parts of alumina.
The micro-gloss glaze for the separation microcrystals comprises the following chemical components in percentage by mass: 46-49% of silicon dioxide, 18-21% of aluminum oxide, 3-6% of potassium oxide, 2-5% of sodium oxide, 2-5% of calcium oxide, 3-6% of magnesium oxide, 3-7% of zinc oxide, 0.3-1.0% of strontium oxide, 10-15% of barium oxide and the balance of trace impurities and burning.
The micro-gloss glaze for the microcrystalline glass comprises the following suspending agents in parts by weight: 20-30 parts of methyl glycol, 20-30 parts of sodium carboxymethylcellulose, 2-3 parts of sodium metaphosphate and 10-40 parts of water.
The micro-gloss ceramic rock plate comprises a green body layer, a ground glaze layer, a pattern layer and a dry grain glaze layer which are sequentially laminated from bottom to top, wherein the material of the dry grain glaze layer comprises the micro-gloss glaze for microcrystal separation.
The micro-gloss ceramic rock plate with the ultra-flat fine glaze comprises the following chemical components in percentage by mass: 56-60% of silicon dioxide, 17-20% of aluminum oxide, 2-5% of potassium oxide, 2-6% of sodium oxide, 3-5% of calcium oxide, 0.1-0.5% of magnesium oxide, 8-12% of zirconium dioxide, 0.5-1.0% of barium oxide, 2-5% of zinc oxide and the balance of trace impurities and burning.
A preparation method of a micro-gloss ceramic rock plate with an ultra-flat fine glaze surface comprises the following steps:
Preparing a green body layer;
applying a primer layer on the green body layer;
ink-jet printing a pattern layer on the primer layer;
The pattern layer is coated with a dry grain glaze layer and then is subjected to firing treatment to prepare initial ceramic;
And brushing and polishing the initial ceramic to obtain the micro-gloss ceramic rock plate with the ultra-flat fine glaze.
The preparation method of the micro-gloss ceramic rock plate with the ultra-flat fine glaze comprises the step of distributing a ground coat on the green body layer, wherein the glazing specific gravity of the ground coat is 1.85-1.95g/ml, the glazing flow rate of glazing slurry is 30-40 seconds, and the glazing weight is 470-560g/m 2.
The preparation method of the micro-gloss ceramic rock plate with the ultra-flat fine glaze comprises the following steps of distributing a dry grain glaze layer on the pattern layer, wherein the glazing proportion of the dry grain glaze layer is as follows: 1.35-1.45 g/ml, and the glazing weight is 280-380g/m 2.
The preparation method of the micro-gloss ceramic rock plate with the ultra-flat fine glaze comprises the steps of spreading a dry grain glaze layer on the pattern layer and then firing, wherein the firing temperature is 1190-1220 ℃, and the firing time is 60-90min.
The beneficial effects are that: according to the invention, the material of a dry grain glaze layer in a micro-gloss ceramic rock plate is optimized and improved, the material for preparing the dry grain glaze layer is micro-gloss glaze, the micro-gloss glaze comprises transparent protective glaze slurry, dry grain powder and a suspending agent, the dry grain powder is formed by crushing and sieving high-calcium high-barium high-strontium frit, a large amount of calcium oxide, barium oxide and strontium oxide are introduced into the dry grain powder to play a fluxing role on the glaze, the firing temperature can be reduced, a large amount of microcrystals are formed on the basis of a base glaze layer of a high-temperature system, the microcrystals extend from the glaze surface layer to the inside and are uniformly distributed, the surface of the glaze is uneven under the microcosmic surface, the specular reflection of incident light is effectively weakened, the diffuse reflection is enhanced, and the micro-light effect is formed; macroscopically, the glaze is fine and smooth and granular, and the glaze with ultra-flat fine and smooth fine and granular touch feeling is formed after brushing and polishing. The glossiness of the prepared micro-gloss ceramic rock plate is between 10 and 15 ℃, and the surface of the micro-gloss ceramic rock plate has ultra-flat and fine particle touch feeling.
Drawings
FIG. 1 is a schematic diagram of a micro-gloss ceramic rock plate with ultra-flat fine glaze.
Fig. 2 is a physical diagram of the micro-gloss ceramic rock plate prepared in example 1 of the present invention.
Fig. 3 is an XRD phase analysis chart of the micro-gloss ceramic rock plate prepared in example 1 of the present invention.
Fig. 4 is a microscopic image of a SEM of a micro-gloss ceramic rock plate prepared in example 1 of the present invention before brushing.
Fig. 5 is a SEM scanning electron microscope micrograph of the micro-polished ceramic rock plate prepared in example 1 of the present invention.
FIG. 6 is a physical view of a ceramic rock plate prepared in comparative example 1 of the present invention.
FIG. 7 is a physical view of a ceramic rock plate prepared in comparative example 2 of the present invention.
FIG. 8 is a physical view of a ceramic rock plate prepared in comparative example 3 of the present invention.
FIG. 9 is a physical view of a ceramic rock plate prepared in comparative example 4 of the present invention.
FIG. 10 is a physical view of a ceramic rock plate prepared in comparative example 5 of the present invention.
FIG. 11 is a physical view of a ceramic rock plate prepared in comparative example 6 of the present invention.
Detailed Description
The invention provides a micro-gloss glaze material for separating microcrystals, a micro-gloss ceramic rock plate with an ultra-flat fine glaze surface and a preparation method thereof, and the invention is further described in detail below for making the purposes, the technical scheme and the effects of the invention more clear and definite. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Referring to fig. 1, fig. 1 is a micro-gloss ceramic rock plate with ultra-flat fine glaze, as shown in the drawing, the micro-gloss ceramic rock plate includes a green body layer 1, a primer layer 2, a pattern layer 3 and a dry grain glaze layer 4 which are sequentially stacked from bottom to top, the material of the dry grain glaze layer 4 includes micro-gloss glaze, and the micro-gloss glaze includes, by weight: 100-160 parts of transparent protective glaze slip, 25-55 parts of dry particle powder and 20-50 parts of suspending agent, wherein the chemical composition of the dry particle powder comprises the following components in percentage by mass: 50-55% of silicon dioxide, 18-21% of aluminum oxide, 2-5% of potassium oxide, 3-6% of sodium oxide, 3-6% of calcium oxide, 0.1-0.5% of magnesium oxide, 2-5% of zinc oxide, 10-16% of barium oxide, 4-8% of strontium oxide and the balance of trace impurities and burning.
In the invention, the dry powder in the micro-gloss glaze is formed by crushing and sieving high-calcium high-barium high-strontium frit, a large amount of calcium oxide, barium oxide and strontium oxide are introduced into the dry powder, the fluxing effect is achieved on the glaze, the firing temperature can be reduced, a large amount of microcrystals are formed, the microcrystals extend from the surface layer of the glaze to the inside and are uniformly distributed, the microcrystals are block-shaped, flake-shaped and columnar-shaped barium strontium feldspar and potassium sodium feldspar, the surface of the glaze is uneven, the specular reflection of incident light is effectively weakened, the diffuse reflection is enhanced, and the micro-light effect is formed; macroscopically, the glaze is fine and smooth and fine particle texture, and the glaze can form ultra-flat fine and fine particle touch after brushing and polishing. The glossiness of the prepared micro-gloss ceramic rock plate is between 10 and 15 ℃, the surface of the micro-gloss ceramic rock plate has ultra-flat and fine particle touch feeling, the microcrystal can also greatly improve the flexural strength, hardness, wear resistance and toughness of the glaze, and the strontium oxide can also reduce the problem that micron-sized particles in dry particle powder are fragile and become powder because of large brittleness.
In some embodiments, the dry powder is prepared from the following raw materials in parts by weight: 20-40 parts of potassium feldspar, 10-30 parts of albite, 5-20 parts of nepheline, 5-10 parts of kaolin, 10-20 parts of barium carbonate, 5-10 parts of wollastonite, 3-8 parts of zinc oxide, 5-15 parts of strontium carbonate, 5-10 parts of calcite and 2-8 parts of alumina. The preparation process of the dry powder comprises the following steps: adding 20-40 parts of potassium feldspar, 10-30 parts of albite, 5-20 parts of nepheline, 5-10 parts of kaolin, 10-20 parts of barium carbonate, 5-10 parts of wollastonite, 3-8 parts of zinc oxide, 5-15 parts of strontium carbonate, 5-10 parts of calcite and 2-8 parts of aluminum oxide into a high-temperature melting furnace, firing the mixture within the range of 1450-1510 ℃, and flowing the fired molten liquid into a cooling water tank for quenching to prepare a frit; crushing the frit, sieving the crushed fine powder with a 250-300 mesh sieve, and taking dry granule fine powder in a range of 250-300 meshes to obtain dry granule powder.
In the invention, the suspending agent is a conventional dry particle suspending agent, and the dry particle suspending agent can enable the dry particle powder to be well and completely suspended and dispersed in the dry particle glaze, so that the suspension property and the fluidity of the whole dry particle powder can be improved. The suspending agent comprises the following components in parts by weight: 20-30 parts of methyl glycol, 20-30 parts of sodium carboxymethylcellulose, 2-3 parts of sodium metaphosphate and 10-40 parts of water.
In the invention, the chemical composition of the transparent protective glaze slip comprises the following components in percentage by mass: 46-49% of silicon dioxide, 18-21% of aluminum oxide, 3-6% of potassium oxide, 2-5% of sodium oxide, 2-5% of calcium oxide, 3-6% of magnesium oxide, 3-7% of zinc oxide, 0.3-1.0% of strontium oxide, 10-15% of barium oxide and the balance of trace impurities and burning. The transparent protective glaze slurry is low-temperature transparent glaze slurry, the melting temperature of the transparent protective glaze slurry is controlled to 1160-1180 ℃, the low-temperature transparent glaze slurry is mainly used for adjusting the lubrication and fineness of the micro-gloss glaze, and the low-temperature transparent glaze slurry can be filled in gaps between dry grains to play a role in filling, so that the internal structure of the dry grain glaze is further improved, the lubrication and fineness of the glaze surface is better, and the anti-fouling capability of the glaze surface is greatly improved.
In the invention, the chemical composition of the primer layer comprises the following components in percentage by mass: 56-60% of silicon dioxide, 17-20% of aluminum oxide, 2-5% of potassium oxide, 2-6% of sodium oxide, 3-5% of calcium oxide, 0.1-0.5% of magnesium oxide, 8-12% of zirconium dioxide, 0.5-1.0% of barium oxide, 2-5% of zinc oxide, and the balance of trace impurities and burning loss is less than or equal to 4%. The ground coat is a glaze material with a higher temperature system, the melting temperature of the glaze material of the ground coat is controlled to be 1220-1250 ℃, and if the temperature of the ground coat is lower and is less than or equal to 1220 ℃, more glass phase is generated, so that the glaze surface is brighter, and the micro-gloss effect is affected.
In the invention, the blank layer 1 is a conventional blank, and the chemical composition of the blank layer comprises the following components in percentage by mass: 59% -63% of silicon dioxide, 21% -24% of aluminum oxide, 2% -4% of potassium oxide, 1% -3% of sodium oxide, 3% -6% of calcium oxide, 3% -5% of magnesium oxide, and the balance of trace impurities and burning loss is less than or equal to 5%.
In some embodiments, a method for preparing a micro-gloss ceramic rock plate with ultra-flat fine glaze is also provided, which comprises the steps of: preparing a green body layer; applying a primer layer on the green body layer; ink-jet printing a pattern layer on the primer layer; the pattern layer is coated with a dry grain glaze layer and then is subjected to firing treatment to prepare initial ceramic; and brushing and polishing the initial ceramic to obtain the micro-gloss ceramic rock plate with the ultra-flat fine glaze. The preparation method of the micro-gloss ceramic rock plate provided by the invention has the advantages of simple process and easiness in operation.
In the invention, the material for preparing the dry grain glaze layer is a micro-gloss glaze, the micro-gloss glaze comprises transparent protective glaze slurry, dry grain powder and suspending agent, the dry grain powder is formed by crushing and sieving high-calcium high-barium high-strontium frit, a large amount of calcium oxide, barium oxide and strontium oxide are introduced into the dry grain powder to play a fluxing role on the glaze, the firing temperature can be reduced, a large amount of microcrystals are formed on the basis of the ground glaze layer of a high-temperature system, the microcrystals extend from the glaze surface layer to the inside and are uniformly distributed, the surface of the glaze is uneven from the microcosmic part, the specular reflection of incident light is effectively weakened, the diffuse reflection is enhanced, and the micro-light effect is formed; macroscopically, the glaze is fine and smooth and granular, and the glaze with ultra-flat fine and smooth fine and granular touch feeling is formed after brushing and polishing. The glossiness of the prepared micro-gloss ceramic rock plate is between 10 and 15 ℃, and the surface of the micro-gloss ceramic rock plate has ultra-flat and fine particle touch feeling.
In the invention, the purpose of applying the base glaze is to cover the base color and flaws of a green body layer, increase the whiteness of the glaze surface, be favorable for the color development of the subsequent ink-jet printing pattern, and the glazing weight is too small to reach the effect of covering the base color, be unfavorable for the color development of the subsequent ink-jet printing pattern, the too high glazing weight can cause the glaze layer to be too thick, the glaze slurry flows to the edge, not only causes waste, but also causes the glaze slurry to flow into a kiln roller in the firing process, and the roller nails are formed in a cumulative period to cause kiln blockage. Based on the above, in the process of applying the primer layer on the blank layer, the glazing specific gravity of the primer layer is 1.85-1.95g/ml, the glazing flow rate of the glazing slurry is 30-40 seconds, and the glazing weight is 470-560g/m 2.
In the invention, too little glazing weight of a plurality of glaze layers can lead to rough surface and cannot obtain fine and smooth low-light effect; if the glazing weight is too much, the surface glossiness is larger, the texture is worse, so the glazing weight is set to be in a preferable range of 280-380g/m 2, and the glazing specific gravity of the dry grain glaze layer is as follows: 1.35-1.45g/ml. In the invention, the surface particles are obvious due to the fact that the number of the powder particles is too large (the particle size is too large), and the texture of the powder particles is not smooth and fine; the particle size of the dry powder is too small (the particle size is too small) which leads to a brighter surface texture, and the cost of the dry powder is also increased sharply, so the particle size of the dry powder is set to be in a preferable range of 250-300 meshes.
In the step of brushing and polishing the initial ceramic, the invention preferably uses the 80-mesh silicon carbide fiber abrasive blocks to brush and polish the initial ceramic in 4-8 groups, thereby obtaining better smooth effect, not increasing gloss and meeting the qualification of antifouling property.
In the step of firing treatment after the dry grain glaze layer is distributed on the pattern layer, the firing temperature is 1190-1220 ℃ and the firing time is 60-90min. In the firing temperature and time range, a large number of fine barium strontium feldspar and potassium sodium feldspar crystals are precipitated in the glaze glass body, extend from the glaze surface layer to the inside and are uniformly distributed, and the microcrystals have strong diffuse reflection effect on light, so that the glaze surface of the micro-gloss ceramic rock plate has a stable micro-gloss effect.
The invention is further illustrated by the following examples:
Example 1
The utility model provides a little gloss ceramic rock board with super flat fine and smooth glaze, little gloss ceramic rock board is by blank layer, ground coat layer, pattern layer and the dry grain glaze layer that from bottom to top stacks gradually set up are fired and are formed, and the preparation dry grain glaze layer's material is little gloss glaze, little gloss glaze includes according to the weight portion: 130 parts of transparent protective glaze slip, 40 parts of dry particle powder and 35 parts of suspending agent. Wherein the chemical composition of the dry powder comprises the following components in percentage by mass: 52% of silicon dioxide, 19% of aluminum oxide, 3% of potassium oxide, 3% of sodium oxide, 4% of calcium oxide, 0.3% of magnesium oxide, 3% of zinc oxide, 11% of barium oxide and 4% of strontium oxide, and the balance of trace impurities and burning.
The dry powder is sieved by a 250-300 mesh screen, and the dry powder in the interval of 250-300 mesh is taken for standby;
The suspending agent comprises the following components in parts by weight: 20-30 parts of methyl glycol, 20-30 parts of sodium carboxymethylcellulose, 2-3 parts of sodium metaphosphate and 10-40 parts of water;
The chemical composition of the transparent protective glaze slip comprises the following components in percentage by mass: 47.59% of silicon dioxide, 18.77% of aluminum oxide, 3.39% of potassium oxide, 2.98% of sodium oxide, 3.09% of calcium oxide, 4.16% of magnesium oxide, 4.5% of zinc oxide, 10.88% of barium oxide, 0.33% of strontium oxide, and 4.31% of trace impurities and burning loss;
The chemical composition of the green body layer comprises the following components in percentage by mass: 60.5% of silicon dioxide, 21.9% of aluminum oxide, 2.82% of potassium oxide, 3.17% of sodium oxide, 3.31% of calcium oxide and 3.6% of magnesium oxide, and the balance of trace impurities and burning.
The chemical composition of the primer layer comprises the following components in percentage by mass: silica 58.58%, aluminum oxide 17.44%, potassium oxide 2.43%, sodium oxide 2.92%, calcium oxide 3.28%, magnesium oxide 0.21%, zinc oxide 3.07%, zirconium dioxide 8.79%, barium oxide 0.81%, and trace impurities and burning loss.
The preparation method of the micro-gloss ceramic rock plate with the ultra-flat fine glaze comprises the following steps:
S1, preparing a green body layer: ball milling and pulping according to the formula of the raw material rock plate blank, spray drying and pulverizing, and pressing and forming to obtain a blank layer;
S2, spreading a ground coat layer on the green body layer, wherein the glazing proportion of the ground coat layer is as follows: 1.90g/ml, the glazing weight is 500g/m 2, and the flow rate of the glaze slurry is 35s;
S3, printing a pattern layer on the base glaze layer in an ink-jet mode, wherein the color and the pattern of the ink-jet printing pattern are flexibly set according to the requirement;
s5, distributing a dry grain glaze layer on the pattern layer, wherein the dry grain glaze layer has the following specific gravity: 1.40g/ml, weight 330g/m 2;
S6: firing, wherein the firing temperature is 1200 ℃ and the firing time is 75min;
and S7, brushing and polishing, namely, brushing and polishing 6 groups of 80-mesh silicon carbide fiber grinding blocks to obtain the micro-gloss ceramic rock plate with the ultra-flat fine glaze as shown in figure 2.
The micro-gloss ceramic rock plate prepared in the embodiment is subjected to physical XRD phase analysis, and the result is shown in figure 3; an SEM microscopic image of the micro-gloss ceramic rock plate before brushing is shown in fig. 4, and an SEM microscopic image of the micro-gloss ceramic rock plate after brushing is shown in fig. 5. When the SEM scanning electron microscope microscopic images 4-5 of the real objects are combined with the corresponding XRD phase analysis image analysis of the real objects of FIG. 3 for analysis, the surface of the glaze is uneven under the microscopic images, so that the specular reflection of incident light is effectively weakened, the diffuse reflection is enhanced, the micro-light effect is formed, a large number of fine barium strontium feldspar and potassium sodium feldspar crystals are separated from the glaze glass body, and the glaze surface layer extends to the inside and is uniformly distributed; macroscopically, the glaze is fine and smooth and granular, and the glaze with ultra-flat fine and smooth granular touch feeling is formed after brushing, and the microscopic images of the SEM scanning electron microscope are compared between the figure 4 before brushing and the figure 5 after brushing. Meanwhile, a large number of fine crystals including barium strontium feldspar and potassium sodium feldspar are formed after sintering, so that the breaking strength, hardness, wear resistance and toughness of the glaze are greatly improved, and the problem that micron-sized particles in dry powder are large in brittleness and easy to be broken into powder can be solved by strontium oxide.
Through tests, the gloss of the micro-gloss ceramic rock plate prepared by the embodiment is 13 degrees, the surface is smooth and fine, the micro-gloss ceramic rock plate has ultra-flat fine particle touch, wear resistance is level 4, antifouling property is level 5, mohs hardness is level 6, and the micro-gloss ceramic rock plate can be used in all places of a household.
Example 2
The utility model provides a little gloss ceramic rock board with super flat fine and smooth glaze, little gloss ceramic rock board is by blank layer, ground coat layer, pattern layer and the dry grain glaze layer that from bottom to top stacks gradually set up are fired and are formed, and the preparation dry grain glaze layer's material is little gloss glaze, little gloss glaze includes according to the weight portion: 100 parts of transparent protective glaze slurry, 25 parts of dry particle powder and 20 parts of suspending agent. Wherein the chemical composition of the dry powder comprises the following components in percentage by mass: 55% of silicon dioxide, 18% of aluminum oxide, 2% of potassium oxide, 3% of sodium oxide, 5% of calcium oxide, 0.1% of magnesium oxide, 2% of zinc oxide, 10% of barium oxide and 4% of strontium oxide, and the balance of trace impurities and burning. The dry powder is sieved by a 250-300 mesh screen, and the dry powder in the interval of 250-300 mesh is taken for standby;
the suspending agent comprises the following components in parts by weight: 20 parts of methyl glycol, 20 parts of sodium carboxymethylcellulose, 2 parts of sodium metaphosphate and 10 parts of water;
The chemical composition of the transparent protective glaze slip comprises the following components in percentage by mass: silica 48.62%, aluminum oxide 18.96%, potassium oxide 3.24%, sodium oxide 3.26%, calcium oxide 2.81%, magnesium oxide 3.17%, zinc oxide 4.02%, barium oxide 11.23%, strontium oxide 0.52%, and trace impurities and burning loss;
The chemical composition of the green body layer comprises the following components in percentage by mass: 61.2% of silicon dioxide, 22.3% of aluminum oxide, 2.96% of potassium oxide, 2.66% of sodium oxide, 3.55% of calcium oxide and 3.13% of magnesium oxide, and the balance of trace impurities and burning.
The chemical composition of the primer layer comprises the following components in percentage by mass: 57.72% of silicon dioxide, 18.14% of aluminum oxide, 2.19% of potassium oxide, 3.62% of sodium oxide, 3.5% of calcium oxide, 0.34% of magnesium oxide, 3.56% of zinc oxide, 8.01% of zirconium dioxide and 0.63% of barium oxide, and the balance of trace impurities and burning.
The preparation method of the micro-gloss ceramic rock plate with the ultra-flat fine glaze comprises the following steps:
S1, preparing a green body layer: ball milling and pulping according to the formula of the raw material rock plate blank, spray drying and pulverizing, and pressing and forming to obtain a blank layer;
S2, spreading a ground coat layer on the green body layer, wherein the glazing proportion of the ground coat layer is as follows: 1.85g/ml, the glazing weight is 470g/m 2, and the flow rate of the glaze slurry is 30s;
S3, printing a pattern layer on the base glaze layer in an ink-jet mode, wherein the color and the pattern of the ink-jet printing pattern are flexibly set according to the requirement;
S5, distributing a dry grain glaze layer on the pattern layer, wherein the dry grain glaze layer has the following specific gravity: 1.35g/ml, weight 280g/m 2;
s6: firing, wherein the firing temperature is 1190 ℃ and the firing time is 90min;
And S7, brushing and polishing, namely, brushing and polishing 6 groups of 80-mesh silicon carbide fiber grinding blocks to obtain the micro-gloss ceramic rock plate with the ultra-flat and fine glaze.
Through tests, the gloss of the micro-gloss ceramic rock plate prepared by the embodiment is 10 degrees, the surface is smooth and fine, the ultra-flat micro-particle touch feeling is achieved, the wear resistance is level 4, the antifouling property is level 5, the Mohs hardness is level 6, and the micro-gloss ceramic rock plate can be used in all places of a household.
Example 3
The utility model provides a little gloss ceramic rock board with super flat fine and smooth glaze, little gloss ceramic rock board is by blank layer, ground coat layer, pattern layer and the dry grain glaze layer that from bottom to top stacks gradually set up are fired and are formed, and the preparation dry grain glaze layer's material is little gloss glaze, little gloss glaze includes according to the weight portion: 160 parts of transparent protective glaze slurry, 55 parts of dry particle powder and 50 parts of suspending agent. Wherein the chemical composition of the dry powder comprises the following components in percentage by mass: 50% of silicon dioxide, 20% of aluminum oxide, 3% of potassium oxide, 4% of sodium oxide, 3% of calcium oxide, 0.5% of magnesium oxide, 2% of zinc oxide, 13% of barium oxide and 4% of strontium oxide, and the balance of trace impurities and burning. The dry powder is sieved by a 250-300 mesh screen, and the dry powder in the interval of 250-300 mesh is taken for standby;
The suspending agent comprises the following components in parts by weight: 30 parts of methyl glycol, 30 parts of sodium carboxymethyl cellulose, 3 parts of sodium metaphosphate and 40 parts of water;
The chemical composition of the transparent protective glaze slip comprises the following components in percentage by mass: 48.12% of silicon dioxide, 19.52% of aluminum oxide, 3.01% of potassium oxide, 4.56% of sodium oxide, 2.31% of calcium oxide, 3.01% of magnesium oxide, 4.61% of zinc oxide, 10.37% of barium oxide, 0.47% of strontium oxide, and trace impurities and burning loss;
the chemical composition of the green body layer comprises the following components in percentage by mass: 61.98% of silicon dioxide, 22.48% of aluminum oxide, 3.16% of potassium oxide, 2.96% of sodium oxide, 2.39% of calcium oxide and 2.53% of magnesium oxide, and trace impurities and burning off;
The chemical composition of the primer layer comprises the following components in percentage by mass: silica 59.16%, aluminum oxide 17.21%, potassium oxide 1.03%, sodium oxide 3.26%, calcium oxide 3.05%, magnesium oxide 0.31%, zinc oxide 3.6%, zirconium dioxide 8.29%, barium oxide 0.94%, and trace impurities and burning loss.
The preparation method of the micro-gloss ceramic rock plate with the ultra-flat fine glaze comprises the following steps:
S1, preparing a green body layer: ball milling and pulping according to the formula of the raw material rock plate blank, spray drying and pulverizing, and pressing and forming to obtain a blank layer;
s2, spreading a ground coat layer on the green body layer, wherein the glazing proportion of the ground coat layer is as follows: 1.95g/ml, the glazing weight is 560g/m 2, and the flow speed of the glaze slurry is 40s;
S3, printing a pattern layer on the base glaze layer in an ink-jet mode, wherein the color and the pattern of the ink-jet printing pattern are flexibly set according to the requirement;
S5, distributing a dry grain glaze layer on the pattern layer, wherein the specific gravity of the ink glaze layer is as follows: 1.45g/ml, weight 380g/m 2;
s6: firing, wherein the firing temperature is 1220 ℃ and the firing time is 60min;
And S7, brushing and polishing, namely, brushing and polishing 6 groups of 80-mesh silicon carbide fiber grinding blocks to obtain the micro-gloss ceramic rock plate with the ultra-flat and fine glaze.
Through tests, the gloss of the micro-gloss ceramic rock plate prepared by the embodiment is 15 degrees, the surface is smooth and fine, the micro-gloss ceramic rock plate has ultra-flat fine particle touch, wear resistance is level 4, antifouling property is level 5, mohs hardness is level 6, and the micro-gloss ceramic rock plate can be used in all places of a household.
Comparative example 1
The preparation method of the ceramic rock plate provided in the comparative example 1 is basically the same as that of the example 1, and the difference is only that the chemical composition and the proportion of the micro-gloss glaze are different, and the micro-gloss glaze in the comparative example 1 only uses transparent protective glaze slurry and suspending agent and does not contain dry particle powder. The physical diagram of the ceramic rock plate prepared in the comparative example is shown in fig. 6, and compared with the ceramic rock plate prepared in the example 1, the ceramic rock plate prepared in the comparative example 1 has more glass phase and less crystal phase. The ceramic rock plate prepared in the comparative example 1 has a smooth surface and no ultra-flat and fine particle touch, and has a glossiness of 29 degrees, a wear resistance of 3 degrees, a stain resistance of 3 degrees and a Mohs hardness of 3 degrees through testing.
Comparative example 2
The preparation method of the ceramic rock plate provided in the comparative example 2 is basically the same as that of the example 1, except that the chemical composition and the proportion of the micro-gloss glaze are different, and the micro-gloss glaze in the comparative example 2 only uses dry particle powder and suspending agent and does not contain transparent protective glaze slurry. A physical diagram of the ceramic rock plate prepared in the comparative example is shown in FIG. 7, and the ceramic rock plate prepared in the comparative example 2 has coarse and fine grain texture on the surface after test. The glossiness is 2 degrees, the antifouling performance is unqualified, the wear resistance is 4 grades, and the Mohs hardness is 6 grades.
Comparative example 3
The preparation method of the ceramic rock plate provided in the comparative example 3 is basically the same as that of the example 1, except that the chemical composition and the proportion of the micro-gloss glaze are different, the dry particle powder in the comparative example 3 does not contain calcium oxide, and the dry particle powder in the comparative example 3 comprises the following components in percentage by mass: 51.33% of silicon dioxide, 18.92% of aluminum oxide, 3.39% of potassium oxide, 4.69% of sodium oxide, 2.63% of magnesium oxide, 4.47% of zinc oxide, 5.06% of barium oxide, 8.15% of strontium oxide, and 1.36% of trace impurities and burning loss. As shown in FIG. 8, the ceramic rock plate prepared in comparative example 3 has a smooth surface and no fine particle touch due to the fact that the ceramic rock plate in comparative example 3 has more glass phase, and has a glossiness of 20 degrees, a wear resistance of 3 degrees, an antifouling property of 3 degrees and a Mohs hardness of 4 degrees.
Comparative example 4
The preparation method of the ceramic rock plate provided in the comparative example 4 is basically the same as that of the example 1, except that the chemical composition and the proportion of the micro-gloss glaze are different, the dry particle powder in the comparative example 4 does not contain barium oxide, and the dry particle powder in the comparative example 4 comprises the following components in percentage by mass: silica 53.79%, aluminum oxide 19.42%, potassium oxide 5.63%, sodium oxide 4.49%, calcium oxide 1.95%, magnesium oxide 2.65%, zinc oxide 1.95%, strontium oxide 9.03%, and trace impurities and 1.09% of burning loss. The physical diagram of the ceramic rock plate prepared in the comparative example 3 is shown in fig. 9, and the ceramic rock plate prepared in the comparative example 3 has a smooth surface and no fine particle touch due to more glass phase generated by the ceramic rock plate in the comparative example 4, and has a glossiness of 22 degrees, a wear resistance of 2 degrees, an antifouling property of 3 degrees and a mohs hardness of 3 degrees through testing.
Comparative example 5
The preparation method of the ceramic rock plate provided in the comparative example 5 is basically the same as that of the example 1, except that the chemical composition and the proportion of the micro-gloss glaze are different, the dry particle powder in the comparative example 5 does not contain strontium oxide, and the dry particle powder in the comparative example 5 comprises the following components in percentage by mass: 52.65% of silicon dioxide, 20.31% of aluminum oxide, 6.49% of potassium oxide, 2.23% of sodium oxide, 7.65% of calcium oxide, 1.13% of magnesium oxide, 6.04% of zinc oxide, 2.38% of barium oxide, and 1.12% of trace impurities and burning loss. As shown in FIG. 10, the ceramic rock plate prepared in comparative example 3 has a smooth surface and no fine particle touch due to the fact that the ceramic rock plate in comparative example 5 has a large amount of glass phase, and has a glossiness of 21 degrees, a wear resistance of 3 degrees, an antifouling property of 3 degrees and a Mohs hardness of 3 degrees.
Comparative example 6
The preparation method of the ceramic rock plate provided in the comparative example 6 is basically the same as that of the example 1, except that the chemical composition and the proportion of the micro-gloss glaze are different, the dry particle powder in the comparative example 6 does not contain strontium oxide and barium oxide, and the dry particle powder in the comparative example 6 comprises the following components in percentage by mass: silica 54.79%, aluminum oxide 22.82%, potassium oxide 6.59%, sodium oxide 7.3%, magnesium oxide 2.92%, zinc oxide 3.89%, and trace impurities and 1.69% of burning. As shown in FIG. 11, the ceramic rock plate prepared in comparative example 6 has a smoother surface and no fine particle touch due to the fact that the ceramic rock plate in comparative example 6 has more glass phase, and has a glossiness of 28 degrees, a wear resistance of 1 grade, an anti-fouling property of 3 grades and a Mohs hardness of 2 grades.
Results analysis of examples and comparative examples
The ceramic rock plates of examples 1 to 3 and comparative examples 1 to 6 were subjected to performance test, and the results are shown in table 1.
Table 1 test results
As can be seen from the results in Table 1, the gloss of the micro-gloss ceramic rock plate prepared in the embodiment is between 10 and 15 degrees, and the micro-gloss ceramic rock plate has ultra-fine and smooth hand feeling, granular texture and good antifouling performance.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.

Claims (8)

1. The micro-gloss ceramic rock plate with the ultra-flat fine glaze is characterized by comprising a green body layer, a ground glaze layer, a pattern layer and a dry grain glaze layer which are sequentially stacked from bottom to top, wherein the material of the dry grain glaze layer comprises micro-gloss glaze with microcrystalline precipitation; the micro-gloss glaze comprises the following components in parts by weight: 100-160 parts of transparent protective glaze slip, 25-55 parts of dry particle powder and 20-50 parts of suspending agent, wherein the chemical composition of the dry particle powder comprises the following components in percentage by mass: 50-55% of silicon dioxide, 18-21% of aluminum oxide, 2-5% of potassium oxide, 3-6% of sodium oxide, 3-5% of calcium oxide, 0.1-0.5% of magnesium oxide, 2-5% of zinc oxide, 10-20% of barium oxide, 4-8% of strontium oxide and trace impurities and burning loss of the other components, wherein the sum of the chemical compositions of the dry particle powder is 100%; the chemical composition of the transparent protective glaze slip comprises the following components in percentage by mass: 46-49% of silicon dioxide, 18-21% of aluminum oxide, 3-6% of potassium oxide, 2-5% of sodium oxide, 2-5% of calcium oxide, 3-6% of magnesium oxide, 3-7% of zinc oxide, 0.3-1.0% of strontium oxide, 10-15% of barium oxide and the balance of trace impurities and burning loss; the surface of the dry granular glaze layer is provided with a large number of microcrystals which extend from the glaze surface layer to the inside and are uniformly distributed.
2. The micro-gloss ceramic rock plate with ultra-flat fine glaze according to claim 1, wherein the raw materials for preparing the dry powder comprise the following raw materials in parts by weight: 20-40 parts of potassium feldspar, 10-30 parts of albite, 5-20 parts of nepheline, 5-10 parts of kaolin, 10-20 parts of barium carbonate, 5-10 parts of wollastonite, 3-8 parts of zinc oxide, 5-15 parts of strontium carbonate, 5-10 parts of calcite and 2-8 parts of alumina.
3. The micro-gloss ceramic rock plate with ultra-flat fine glaze according to claim 1, wherein the suspending agent comprises the following components in parts by weight: 20-30 parts of methyl glycol, 20-30 parts of sodium carboxymethylcellulose, 2-3 parts of sodium metaphosphate and 10-40 parts of water.
4. The micro-gloss ceramic rock plate with ultra-flat fine glaze according to claim 1, wherein the chemical composition of the under-glaze layer comprises, in mass percent: 56-60% of silicon dioxide, 17-20% of aluminum oxide, 2-5% of potassium oxide, 2-6% of sodium oxide, 3-5% of calcium oxide, 0.1-0.5% of magnesium oxide, 8-12% of zirconium dioxide, 0.5-1.0% of barium oxide, 2-5% of zinc oxide and the balance of trace impurities and burning.
5. A method of producing a micro-gloss ceramic rock plate with ultra-flat fine glaze according to any one of claims 1 to 4, comprising the steps of:
Preparing a green body layer;
applying a primer layer on the green body layer;
ink-jet printing a pattern layer on the primer layer;
The pattern layer is coated with a dry grain glaze layer and then is subjected to firing treatment to prepare initial ceramic;
And brushing and polishing the initial ceramic to obtain the micro-gloss ceramic rock plate with the ultra-flat fine glaze.
6. The method for producing a micro-gloss ceramic rock plate with an ultra-flat fine glazed surface according to claim 5, wherein in the step of applying a primer layer on the green body layer, the specific gravity of the primer layer is 1.85-1.95g/ml, the flow rate of the glazed glaze slurry is 30-40 seconds, and the weight of the glazed glaze is 470-560g/m 2.
7. The method for producing a micro-gloss ceramic rock plate with an ultra-flat fine glaze according to claim 5, wherein in the step of applying a dry grain glaze layer on the pattern layer, the glazing specific gravity of the dry grain glaze layer is: 1.35-1.45g/ml, and the glazing weight is 280-380g/m 2.
8. The method for producing a micro-gloss ceramic rock plate with an ultra-flat fine glaze according to claim 5, wherein in the step of firing treatment after applying a dry grain glaze layer on the pattern layer, the firing temperature is 1190-1220 ℃ and the firing time is 60-90min.
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CN113860887A (en) * 2021-10-22 2021-12-31 新明珠集团股份有限公司 Ceramic plate and preparation method thereof
CN114735935A (en) * 2022-03-31 2022-07-12 佛山市阿特贝尔建材有限公司 5-degree low-light-level diffuse reflection ceramic rock plate and preparation method thereof
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