CN111470774B - Production method of microcrystal antiskid ceramic tile - Google Patents
Production method of microcrystal antiskid ceramic tile Download PDFInfo
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- CN111470774B CN111470774B CN202010368214.XA CN202010368214A CN111470774B CN 111470774 B CN111470774 B CN 111470774B CN 202010368214 A CN202010368214 A CN 202010368214A CN 111470774 B CN111470774 B CN 111470774B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
- C04B41/5023—Glass-ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
Abstract
The invention relates to a production method of a microcrystal antiskid ceramic tile, which comprises the following steps: (1) preparing a microcrystal anti-skid glaze material to form a base glaze ingredient; (2) preparing base glaze and pre-ball-milling into semi-finished glaze slip; (3) adding a microcrystal nuclear material and then performing ball milling to obtain microcrystal antiskid glaze slip; (4) firstly, spraying a layer of ground glaze on a ground blank, and then spraying a microcrystalline anti-slip glaze slurry layer on the surface of the ground glaze layer; (5) and (3) forming a microcrystal antiskid layer on the surface of the ceramic tile by sintering under a specific temperature condition, thereby obtaining the microcrystal antiskid ceramic tile. The product produced by the invention effectively solves the problem of falling injury of personnel caused by slippery of wet ground water, achieves the perfect combination of the anti-skid function and the soft texture of the surface, and has very high practical value.
Description
Technical Field
The invention relates to a production method of a building decoration material, in particular to a production method of a microcrystal antiskid ceramic tile.
Background
The surface of the traditional glazed ceramic tile product is a plane glass body, the surface is smooth, and the anti-skid performance is poor; the dry particle anti-skid process can achieve good anti-skid performance, but the surface is too rough, and the use place is limited.
Disclosure of Invention
The invention provides a microcrystal antiskid ceramic tile, which is characterized in that zinc oxide with a coarse grain size is added into a special base glaze to form a new formula system, under a specific firing condition, the zinc oxide and quartz are combined into a fine crystal, the microcrystal and a glaze surface are combined on the glaze surface to obtain a microcrystal antiskid layer, the microcrystal antiskid layer has nanoscale micro crystal grains, micro grooves are formed among the crystal grains, the micro grooves can be filled with water when the water is in contact with the crystal grains, when a sole or a sole is in contact with the surface of the ceramic tile, the water is extruded out of the micro grooves after being pressed, the holes in the grooves are in a vacuum state, so that the sole or the sole is in contact with the surface of the ceramic tile to generate the functions of a physical sucking disc and antiskid, the friction coefficient of the ground is greatly increased by utilizing atmospheric pressure, and the antiskid effect of being more antiskid when the water is in contact with the ceramic tile is realized. The invention effectively solves the problem that the wet ground water becomes slippery to cause the injury of the personnel, achieves the perfect combination of the anti-skid function and the soft texture of the surface, and has very high practical value.
The technical means adopted by the invention are as follows.
The microcrystal antiskid ceramic tile and its production process features the following key steps.
(1) Preparing a formula of the microcrystal antiskid glaze and preparing raw materials.
(2) The base glaze is mixed and pre-ball-milled into semi-finished glaze slip.
(3) Adding a microcrystal nuclear material and then performing ball milling to obtain the microcrystal antiskid glaze slip.
(4) And (3) spraying a layer of ground coat, and then spraying an anti-slip glaze slurry layer on the surface of the ground coat.
(5) And (3) forming a microcrystal antiskid layer on the surface of the ceramic tile by sintering under a specific temperature condition, thereby obtaining the microcrystal antiskid ceramic tile.
In the step (1), the formula of the microcrystal anti-skid glaze slip comprises the following components in percentage by weight: 22-25% of quartz, 12-18% of limestone, 15-21% of albite, 5-6% of black mud, 3-4% of aluminum oxide and 23-27% of zinc oxide.
According to the formula of the microcrystal anti-slip glaze, zinc oxide is selected as a microcrystal core material, a microcrystal core and silicon oxide are chemically synthesized into willemite during a high-temperature calcination process to form a microcrystal, the addition amount of the zinc oxide in the formula is controlled to be 23-27%, the number of crystallized crystals is increased due to excessive content of the zinc oxide, and the glaze surface and crystal patterns are unsmooth; if the content of zinc oxide is too low, microcrystals cannot be formed due to insufficient saturation of high-temperature melt; the addition amount of Al2O3 should not be more than 3% -4%, otherwise the crystal development is affected by the increase of glaze viscosity.
Wherein, the preparation of the antiskid glaze layer material in the step (1) comprises the following steps: quartz powder with the grain diameter of phi 0.15mm, albite with the grain diameter of phi 2.0mm, limestone with the grain diameter of phi 1.0mm, black mud and zinc oxide with the grain diameter of phi 1.0mm are prepared.
In the step (2), the basic glaze is put into a ball mill, wherein the material is that water (wt%) =1:1:0.6, the ball milling time is 40 hours, the obtained glaze slurry passes through a standard sieve with 325 meshes, and the screen residue is 0.2-0.5%, so that semi-finished glaze slurry is obtained for later use.
Wherein, the process method in the step (3) comprises the following steps: and (3) after the step (2) is finished, adding zinc oxide, and continuing ball milling for 1 hour to obtain finished glaze slurry for later use.
The fineness of the microcrystal antiskid glaze slip is controlled, and large particles are easy to crystallize as zinc oxide of microcrystal fusant, and the zinc oxide of coarse particles has strong high-temperature melting resistance and relatively high local supersaturation degree, so that the microcrystal nuclei are formed, and the fineness of the microcrystal antiskid glaze slip is controlled to be 0.1-0.2% of 80-mesh screen residue.
Wherein, the glazing technical scheme of the anti-slip glaze layer in the step (4) is as follows: the specific gravity of the prepared glaze slip is 1.70-1.80, and the thickness of the glaze layer is controlled to be 1.6-2 mm. The thickness is thicker than the common glaze layer, so that the glaze fluidity is good in the high-temperature sintering process, a larger suspension space can be formed in the direction vertical to the glaze layer and the glaze layer, and a larger vortex can be formed in the glaze material crystallization process to promote the growth and development of microcrystals, so that the microcrystal glaze layer with the anti-slip function is formed.
The firing process of the anti-skid glaze layer in the step (5) comprises the following steps: the firing temperature is 1190 ℃, then the temperature is reduced to 1080 ℃, then the temperature is raised to 1120 ℃, the temperature is kept for 20 minutes, and then the temperature is gradually reduced and the temperature is cooled to be accurate, so that the ceramic tile with a fine surface and a crystal anti-slip layer is obtained.
The firing process of the anti-skid glaze layer in the step (5) comprises the following steps: the kiln firing atmosphere is an oxidizing atmosphere.
Wherein, the sintering temperature in the step (5) has great influence on the crystals, the crystal nucleus can be melted when the temperature is too high, and the crystals are not easy to appear or only a few large crystals and residual crystals appear or the surface is rough; too low a temperature results in a glaze with a high viscosity, too small crystals and a high amount of crystals that are not slip-resistant. The heat preservation time after cooling is the key for determining the amount and the size of crystals, when the crystallization temperature is close to the melting point, the crystals are few and large, and when the crystallization temperature is far away from the melting point, the crystals are many and small; the crystallization is not easy to occur when the temperature reduction amplitude exceeds 250 ℃; in addition, the size of the crystal is influenced by the length of the heat preservation time, and the crystal is too large and not fine and smooth if the heat preservation time is too long.
The invention has the advantages that the problem that people are hurt by falling due to the fact that the surface of the ceramic tile is too smooth, particularly when the ceramic tile is paved on the ground and has water is solved, the whole surface of the microcrystal ceramic tile is smooth and soft, the microcrystal ceramic tile has an anti-slip effect on soft glaze, micro grooves can be formed among microcrystal grains of the glaze, the micro grooves can generate the functions of a physical sucking disc and anti-slip when meeting water, the ground friction coefficient is greatly increased by utilizing atmospheric pressure, the anti-slip effect is realized when meeting water, the perfect combination of the anti-slip function and the soft texture of the surface is achieved, and the practical value is very high.
Detailed Description
A microcrystal antiskid ceramic tile and its production method are disclosed, which includes the following key steps.
(1) Preparing a formula of the microcrystal antiskid glaze and preparing raw materials.
(2) The base glaze is mixed and pre-ball-milled into semi-finished glaze slip.
(3) Adding a microcrystal nuclear material and then performing ball milling to obtain the microcrystal antiskid glaze slip.
(4) And (3) spraying a layer of ground coat, and then spraying an anti-slip glaze slurry layer on the surface of the ground coat.
(5) And (3) forming a microcrystal antiskid layer on the surface of the ceramic tile by sintering under a specific temperature condition, thereby obtaining the microcrystal antiskid ceramic tile.
In the step (1), the formula of the microcrystal anti-skid glaze slip comprises the following components in percentage by weight: 25% of quartz, 18% of limestone, 20% of albite, 6% of black mud, 4% of aluminum oxide and 27% of zinc oxide.
The microcrystalline core material is zinc oxide, the microcrystalline core and silicon oxide are chemically synthesized into willemite to form microcrystals in the high-temperature calcination process, the addition amount of the zinc oxide in the formula is controlled to be 23-27%, the excessive content of the zinc oxide can increase the number of crystallized bodies, and the glaze surface and crystal flowers are unsmooth; if the content of zinc oxide is too low, microcrystals cannot be formed due to insufficient saturation of high-temperature melt; the addition amount of Al2O3 should not be more than 3% -4%, otherwise the crystal development is affected by the increase of glaze viscosity.
Wherein, the preparation of the antiskid glaze layer material in the step (1) comprises the following steps: quartz powder with the grain diameter of phi 0.15mm, albite with the grain diameter of phi 2.0mm, limestone with the grain diameter of phi 1.0mm, black mud and zinc oxide with the grain diameter of phi 1.0mm are prepared.
In the step (2), the basic glaze is put into a ball mill, wherein the ball is water (wt%) =1:1:0.6, the ball milling time is 40 hours, the obtained glaze slurry passes through a standard sieve with 325 meshes, and the screen residue is 0.4%, so that semi-finished glaze slurry is obtained for later use;
wherein, the process method in the step (3) comprises the following steps: and (3) after the step (2) is finished, adding zinc oxide, and continuing ball milling for 1 hour to obtain finished glaze slurry for later use.
The fineness of the microcrystal antiskid glaze slip is controlled, and large particles are easier to crystallize as the zinc oxide of microcrystal fusant, and the zinc oxide of coarse particles has strong high-temperature melting resistance and relatively high local supersaturation, so that the zinc oxide is beneficial to forming microcrystal nuclei and is controlled to be 0.15 percent of 80-mesh screen residue.
Wherein, the glazing technical scheme of the anti-slip glaze layer in the step (4) is as follows: the specific gravity of the prepared glaze slip is 1.70-1.80, and the thickness of the glaze layer is controlled to be 1.9 mm. The thickness is thicker than the common glaze layer, so that the glaze fluidity is good in the high-temperature sintering process, a larger suspension space can be formed in the direction vertical to the glaze layer and the glaze layer, and a larger vortex can be formed in the glaze material crystallization process to promote the growth and development of microcrystals, so that the microcrystal glaze layer with the anti-slip function is formed.
The firing process of the anti-skid glaze layer in the step (5) comprises the following steps: the firing temperature is 1190 ℃, then the temperature is reduced to 1080 ℃, then the temperature is raised to 1120 ℃, the temperature is kept for 20 minutes, and then the temperature is gradually reduced and the temperature is cooled to be accurate, so that the ceramic tile with a fine surface and a crystal anti-slip layer is obtained.
The firing process of the anti-skid glaze layer in the step (5) comprises the following steps: the kiln firing atmosphere is an oxidizing atmosphere.
Wherein, the sintering temperature in the step (5) has great influence on the crystals, the crystal nucleus can be melted when the temperature is too high, and the crystals are not easy to appear or only a few large crystals and residual crystals appear or the surface is rough; too low a temperature results in a glaze with a high viscosity, too small crystals and a high amount of crystals that are not slip-resistant. The heat preservation time after cooling is the key for determining the amount and the size of crystals, when the crystallization temperature is close to the melting point, the crystals are few and large, and when the crystallization temperature is far away from the melting point, the crystals are many and small; the crystallization is not easy to occur when the temperature reduction amplitude exceeds 250 ℃; in addition, the size of the crystal is influenced by the length of the heat preservation time, and the crystal is too large and not fine and smooth if the heat preservation time is too long.
According to the microcrystal antiskid ceramic tile obtained by the process method, the surface of the ceramic tile is not a concave-convex surface pressed by a mold, but a soft flat surface with an antiskid function, an antiskid layer is provided with nanoscale micro crystal grains, micro grooves can be formed among the crystal grains, the micro grooves can generate the functions of a physical sucking disc and antiskid when meeting water, the ground friction coefficient is greatly increased by utilizing atmospheric pressure, and the antiskid effect when meeting water is realized. The invention effectively solves the problem that the wet ground water becomes slippery to cause the injury of the personnel, achieves the perfect combination of the anti-skid function and the soft texture of the surface, and has very high practical value.
Claims (6)
1. A production method of a microcrystal antiskid ceramic tile,
the production method comprises the following steps:
(1) preparing a microcrystal anti-skid glaze material to form a base glaze ingredient;
(2) preparing base glaze and pre-ball-milling into semi-finished glaze slip;
(3) adding a microcrystal nuclear material and then performing ball milling to obtain microcrystal antiskid glaze slip;
(4) firstly, spraying a layer of ground glaze on a ground blank, and then spraying a microcrystalline anti-slip glaze slurry layer on the surface of the ground glaze layer;
(5) sintering the surface under a specific temperature condition to form a microcrystal antiskid layer, thereby obtaining a microcrystal antiskid ceramic tile;
the preparation of the anti-skid glaze layer material in the step (1) comprises the following steps: preparing quartz powder with the particle size of phi 0.15mm, albite with the particle size of phi 2.0mm, limestone with the particle size of phi 1.0mm, black mud and zinc oxide with the particle size of phi 1.0 mm;
in the step (2), the basic glaze is put into a ball mill, wherein the ball is water (1: 1: 0.6) according to the mass percentage, the ball milling time is 40 hours, the obtained glaze slurry passes through a standard sieve with 325 meshes, and the screen residue is 0.2-0.5%, so that semi-finished glaze slurry is obtained for later use;
the technical scheme of glazing the anti-slip glaze layer in the step (4) is as follows: the specific gravity of the prepared glaze slip is 1.70-1.80, and the thickness of a glaze layer is controlled to be 1.6-2 mm;
and the microcrystal anti-skid glaze material comprises the following components in percentage by weight: 22-25% of quartz, 12-18% of limestone, 15-21% of albite, 5-6% of black mud, 3-4% of aluminum oxide and 23-27% of zinc oxide.
2. A process for the production of microcrystalline non-slip tiles as claimed in claim 1, wherein: in the formula of the microcrystal antiskid glaze, zinc oxide is selected as a microcrystal core material, and a microcrystal core and silicon oxide are synthesized into willemite to form a microcrystal in a high-temperature calcination process.
3. A process for the production of microcrystalline non-slip tiles as claimed in claim 1, wherein: wherein, the process method in the step (3) comprises the following steps: and (3) after the step (2) is finished, adding zinc oxide, and performing ball milling for 1 hour together with the base glaze slurry to obtain the microcrystal anti-skidding glaze slurry for later use.
4. A process for the production of microcrystalline non-slip tiles as claimed in claim 1, wherein: wherein, the fineness of the microcrystal antiskid glaze slip is controlled, and the residual amount of the 80-mesh sieve is 0.1-0.2%.
5. A process for the production of microcrystalline non-slip tiles as claimed in claim 1, wherein: wherein, the specific firing conditions of the antiskid glaze layer in the step (5) are as follows: the sintering temperature is 1190 ℃, then the temperature is reduced to 1080 ℃, then the temperature is raised to 1120 ℃, the temperature is preserved for 20 minutes, then the temperature is gradually reduced and the temperature is cooled, and the total sintering time is 100 minutes, thus obtaining the ceramic tile with the fine surface and the crystal anti-skid layer.
6. A process for the production of microcrystalline non-slip tiles as claimed in claim 5, wherein: the kiln firing atmosphere is an oxidizing atmosphere, and in the process of cooling, the cooling amplitude is less than 250 ℃ every 10 minutes before 250 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010368214.XA CN111470774B (en) | 2020-04-30 | 2020-04-30 | Production method of microcrystal antiskid ceramic tile |
| PCT/CN2020/133066 WO2021218151A1 (en) | 2020-04-30 | 2020-12-01 | Production method for microcrystalline anti-slip ceramic tile |
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| CN202010368214.XA CN111470774B (en) | 2020-04-30 | 2020-04-30 | Production method of microcrystal antiskid ceramic tile |
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| CN111470774B true CN111470774B (en) | 2022-03-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111470774B (en) * | 2020-04-30 | 2022-03-08 | 佛山市三水新明珠建陶工业有限公司 | Production method of microcrystal antiskid ceramic tile |
| CN112340990B (en) * | 2020-11-25 | 2022-05-24 | 珠海市白兔陶瓷有限公司 | Antiskid brick and production process thereof |
| CN112408797A (en) * | 2020-12-04 | 2021-02-26 | 湖南华联瓷业股份有限公司 | Crystalline glaze and preparation method thereof |
| CN112939465A (en) * | 2021-03-31 | 2021-06-11 | 江西太阳陶瓷有限公司 | Anti-slip glaze and processing method of anti-slip glazed brick |
| CN112939463B (en) * | 2021-04-07 | 2022-06-14 | 亚细亚建筑材料股份有限公司 | Anti-slip antifouling glaze |
| CN116535246A (en) * | 2023-05-12 | 2023-08-04 | 清远市简一陶瓷有限公司 | High-skid-resistance transparent dry particles, skid-resistance glaze using same, high-skid-resistance ceramic tile with water-repellent function and preparation method |
| CN116283364B (en) * | 2023-05-24 | 2023-09-19 | 新明珠集团股份有限公司 | Anti-skid and anti-fouling ceramic tile and preparation method thereof |
| CN117125967B (en) * | 2023-08-25 | 2024-04-26 | 福建省南安宝达建材有限公司 | Wet anti-slip brick and manufacturing process thereof |
| CN116986925B (en) * | 2023-09-27 | 2023-12-15 | 佛山市金舵陶瓷有限公司 | Anti-skid wear-resistant ceramic tile with island-shaped structure and preparation method thereof |
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| JPH05105559A (en) * | 1991-10-22 | 1993-04-27 | Inax Corp | Antislip tile and its production |
| CN104311155A (en) * | 2014-10-11 | 2015-01-28 | 杭州诺贝尔陶瓷有限公司 | Crystal glaze ceramic tile and production method thereof |
| CN109336393A (en) * | 2018-11-14 | 2019-02-15 | 宁波联城住工科技有限公司 | Anti-skidding glaze and preparation method thereof and a kind of production method of skid-resistance ceramic |
| CN109354406A (en) * | 2018-11-14 | 2019-02-19 | 宁波联城住工科技有限公司 | Anti-skidding glaze and preparation method thereof and a kind of production method of skid-resistance ceramic |
| CN109455933A (en) * | 2018-12-19 | 2019-03-12 | 蒙娜丽莎集团股份有限公司 | A kind of crystalline glaze and use Ceramic Tiles made from the crystalline glaze |
| CN111039570A (en) * | 2020-01-09 | 2020-04-21 | 景德镇陶瓷大学 | Zirconium-free anorthite-based opaque glaze and preparation method thereof |
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| WO2021218151A1 (en) | 2021-11-04 |
| CN111470774A (en) | 2020-07-31 |
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