CN115215546A - Mullite-reinforced transparent glaze and preparation method and application thereof - Google Patents
Mullite-reinforced transparent glaze and preparation method and application thereof Download PDFInfo
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- CN115215546A CN115215546A CN202210703701.6A CN202210703701A CN115215546A CN 115215546 A CN115215546 A CN 115215546A CN 202210703701 A CN202210703701 A CN 202210703701A CN 115215546 A CN115215546 A CN 115215546A
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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
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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
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- C—CHEMISTRY; METALLURGY
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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Abstract
The invention discloses a mullite reinforced transparent glaze and a preparation method and application thereof. The mullite reinforced transparent glaze comprises transparent base glaze and mullite, wherein the transparent base glaze comprises SiO 2 、CaO、ZnO、Al 2 O 3 、K 2 O, mgO, and BaO. The preparation method of the mullite-reinforced transparent glaze comprises the following steps: mixing the transparent base glaze, mullite and a dispersing agent, carrying out wet ball milling to prepare glaze slurry, glazing the ceramic blank, and firing to obtain the mullite-reinforced transparent glaze. The mullite reinforced transparent glaze has the advantages of high transparency, high hardness, high wear resistance, low cost and the like, and the preparation process is simple and is suitable for large-scale industrial application.
Description
Technical Field
The invention relates to the technical field of ceramic glaze, in particular to mullite-reinforced transparent glaze and a preparation method and application thereof.
Background
The glaze is a colorless or colored vitreous thin layer covered on the surface of the ceramic product, is prepared by applying glaze slurry prepared by grinding mineral raw materials (such as feldspar, quartz, talc, kaolin, and the like) on the surface of a blank and then calcining, can increase the mechanical strength, thermal stability and dielectric strength of the ceramic product, and also has the effects of beautifying ware, being convenient to wipe and wash, being not corroded by fishy dirt, and the like. However, most of the existing transparent glazes cannot simultaneously have the advantages of high transparency, high hardness, high wear resistance and low cost, and are difficult to completely meet the requirements of practical applications, such as: CN 103030435A discloses a wear-resistant glaze for domestic ceramics and a preparation method thereof, which is characterized in that specific alumina is added to improve the hardness and wear resistance of the glaze, and the transparency of the glaze is greatly reduced because the refractive index (1.76) of the alumina is not matched with the glass of the glaze layer; CN 106946460A discloses a cordierite transparent wear-resistant glaze and a preparation method thereof, which need to use lithium carbonate and the like as raw materials and have higher production cost.
Therefore, the development of the transparent glaze with high transparency, high hardness, high wear resistance and low cost is of great significance.
Disclosure of Invention
The invention aims to provide a mullite-reinforced transparent glaze as well as a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
the mullite reinforced transparent glaze comprises the following components in percentage by mass:
transparent base glaze: 75 to 95 percent;
mullite: 5% -25%;
the transparent base glaze comprises the following components in percentage by mass:
SiO 2 ：62％～65％；
CaO：11％～14％；
ZnO：7％～9％；
Al 2 O 3 ：5％～12％；
K 2 O：3％～5％；
MgO：0.8％～1％；
BaO：0.4％～1％。
preferably, the transparent base glaze comprises the following components in percentage by mass:
SiO 2 ：62％～65％；
CaO：11％～14％；
ZnO：7％～9％；
Al 2 O 3 ：5％～12％；
K 2 O：3％～5％；
MgO：0.8％～1％；
BaO：0.4％～1％；
ZrO 2 ：0.16％～0.19％；
Fe 2 O 3 ：0.16％～0.22％；
TiO 2 ：0.07％～0.15％；
PbO：0.03％～0.04％；
As 2 O 3 ：0.015％～0.025％；
NiO：0.015％～0.025％。
preferably, the granularity of the mullite is 100 meshes to 325 meshes.
The preparation method of the mullite reinforced transparent glaze comprises the following steps: mixing the transparent base glaze, mullite and a dispersing agent, carrying out wet ball milling to prepare glaze slurry, glazing the ceramic blank, and firing to obtain the mullite-reinforced transparent glaze.
Preferably, the dispersant is at least one of carboxymethyl cellulose, sodium carboxymethyl cellulose and sodium tripolyphosphate.
Preferably, the addition amount of the dispersing agent is 0.3-0.8% of the total mass of the transparent base glaze and the mullite.
Preferably, the time of the wet ball milling is 15min to 30min.
Preferably, the glazing mode is one of glaze spraying, glaze dipping and glaze pouring.
Preferably, the firing is carried out at 1150-1200 ℃ and the heat preservation time is 5-10 min.
Further preferably, the firing comprises the following specific operations: heating to 1150-1200 ℃ at the heating rate of 10-40 ℃/min, and then preserving the heat for 5-10 min.
The surface of the ceramic product is applied with the mullite reinforced transparent glaze.
Preferably, the ceramic product is one of a wall brick and a floor tile.
The invention has the beneficial effects that: the mullite-enhanced transparent glaze disclosed by the invention has the advantages of high transparency, high hardness, high wear resistance, low cost and the like, and the preparation process is simple and is suitable for large-scale industrial application.
Specifically, the method comprises the following steps:
1) The mullite is added into the glaze by doping, the preparation and firing processes are simple, the firing system does not need to be strictly controlled to separate the mullite (the mullite formed by the traditional crystallization system is limited by thermodynamics, and Al in the glaze is contained 2 O 3 And SiO 2 High content of (b), high temperature is required), can flexibly adapt to the wall/floor tile industrial firing system;
2) The mullite reinforced transparent glaze can be partially melted and small-particle mullite is precipitated again around the mullite when being fired, so that an embedded structure is formed, the binding force between the mullite and a glass phase is increased, and the mullite has higher hardness than a glaze layer, so that the wear resistance of a glaze surface can be improved;
3) According to the invention, the mullite is added into the glaze through external doping, and the refractive index of the mullite is close to that of silicate glass, so that the glaze surface has good transparency.
Drawings
FIG. 1 is an X-ray diffraction pattern of the mullite-reinforced clear glaze of example 1.
Fig. 2 is an SEM image of the mullite-reinforced transparent glaze of example 1.
Fig. 3 is a comparison graph of the physical appearances of the mullite-reinforced transparent glaze and the transparent base glaze of the example 1.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
the preparation method of the mullite reinforced transparent glaze comprises the following steps:
100 parts by mass of a transparent base glaze (chemical composition: 63.84wt% of SiO) 2 13.89wt% CaO, 8.61wt% ZnO, 5.56wt% Al 2 O 3 3.58 wt.% of K 2 O, mgO 0.93wt%, baO 0.53wt%, zrO 0.19wt% 2 0.16wt% of Fe 2 O 3 0.07wt% of TiO 2 0.04wt% of PbO, 0.02wt% of As 2 O 3 0.02wt% of NiO, and the balance of loss on ignition), 25 parts by mass of mullite (the granularity is 100-325 meshes) and 0.375 part by mass of carboxymethyl cellulose are mixed and subjected to wet ball milling for 15min to prepare glaze slurry, then glaze is applied to the biscuit-fired ceramic blank in a glaze spraying manner, drying is carried out, then the ceramic blank is put into a box-type electric furnace to be heated to 1180 ℃ at the heating rate of 10 ℃/min, and then heat preservation is carried out for 10min, and cooling is carried out, thus obtaining the mullite reinforced transparent glaze.
Through tests, the Vickers hardness of the mullite reinforced transparent glaze prepared by the embodiment is 7.39GPa, and is improved by 8.5% compared with that of transparent base glaze (the Vickers hardness is 6.81 GPa).
And (3) performance testing:
1) The X-ray diffraction pattern of the mullite-reinforced clear glaze prepared in the example is shown in FIG. 1.
As can be seen from fig. 1: the appearance of the mullite peak indicates the presence of the mullite crystalline phase in the glaze.
2) The Scanning Electron Microscope (SEM) image of the section of the mullite-reinforced transparent glaze prepared in this example (the section was tested after being etched with 2% hydrofluoric acid solution by volume for 45 s) is shown in fig. 2.
As can be seen from fig. 2: the large particles are mullite grains, and a plurality of small mullite particles are also arranged around the large particles, which shows that the mullite can be partially dissolved and the small mullite particles are separated out again around the mullite reinforced transparent glaze when the mullite reinforced transparent glaze is fired, so that an embedded structure is formed, and the bonding force between the mullite and the glass phase is increased.
3) A comparison graph of the physical appearances of the mullite-reinforced transparent glaze (referred to as "mullite glaze" for short) and the transparent base glaze (referred to as "base glaze" for short) prepared in this example is shown in fig. 3 (a base blank is a yellow and red biscuit which is subjected to ink-jet printing in advance, and is fired at 1180 ℃ after glazing).
As can be seen from fig. 3: the color of the mullite reinforced transparent glaze is very close to that of the transparent base glaze, and the color difference delta E is below 3NBS unit, which shows that the mullite transparent glaze has higher transparency.
Example 2:
the preparation method of the mullite reinforced transparent glaze comprises the following steps:
100 parts by mass of a transparent base glaze (chemical composition: 62.99wt% SiO) 2 CaO 12.64wt%, znO 7.83wt%, al 9.01wt% 2 O 3 3.28 wt.% of K 2 O, 0.86wt% MgO, 0.48wt% BaO, 0.17wt% ZrO 2 0.19wt% Fe 2 O 3 0.12wt% of TiO 2 0.04wt% of PbO, 0.02wt% of As 2 O 3 0.02wt% of NiO, and the balance of loss on ignition), 15 parts of mullite (the granularity is 100-325 meshes) and 0.345 part of carboxymethyl cellulose are mixed and subjected to wet ball milling for 15min to prepare glaze slurry, then glaze is applied to the biscuit-fired ceramic blank in a glaze spraying manner, drying is carried out, then the ceramic blank is put into a box-type electric furnace to be heated to 1180 ℃ at the heating rate of 10 ℃/min, and then heat preservation is carried out for 10min, and cooling is carried out, thus obtaining the mullite reinforced transparent glaze.
Through tests (the test method is the same as that in the example 1), the mullite crystal phase exists in the mullite-reinforced transparent glaze prepared in the embodiment, the mosaic structure formed by the large mullite particles and the small mullite particles exists, the Vickers hardness of the mullite-reinforced transparent glaze is 7.23GPa, the hardness is improved by 3.5% compared with that of a transparent base glaze (the Vickers hardness is 6.98 GPa), the colors of the mullite-reinforced transparent glaze and the transparent base glaze are very close, and the color difference delta E is below 3NBS units.
Example 3:
the preparation method of the mullite-reinforced transparent glaze comprises the following steps:
100 parts by mass of a transparent base glaze (chemical composition: 62.29wt% of SiO) 2 11.60wt% of CaO, 7.17wt% of ZnO, 11.89wt% of Al 2 O 3 3.03wt% of K 2 O, 0.81wt% MgO, 0.44wt% BaO, 0.16wt% ZrO 2 0.22wt% of Fe 2 O 3 0.15wt% of TiO 2 0.03wt% of PbO, 0.02wt% of As 2 O 3 0.02wt% of NiO, and the balance of loss on ignition), 15 parts of mullite (the granularity is 100-325 meshes) and 0.345 part of carboxymethyl cellulose are mixed and subjected to wet ball milling for 15min to prepare glaze slurry, then glaze is applied to the biscuit-fired ceramic blank in a glaze spraying manner, drying is carried out, then the ceramic blank is put into a box-type electric furnace to be heated to 1180 ℃ at the heating rate of 10 ℃/min, and then heat preservation is carried out for 10min, and cooling is carried out, thus obtaining the mullite reinforced transparent glaze.
Through tests (the test method is the same as that in the example 1), the mullite crystal phase exists in the mullite-reinforced transparent glaze prepared in the embodiment, the mosaic structure formed by the large mullite particles and the small mullite particles exists, the Vickers hardness of the mullite-reinforced transparent glaze is 7.26GPa, the hardness is improved by 3.3% compared with that of a transparent base glaze (the Vickers hardness is 7.02 GPa), the colors of the mullite-reinforced transparent glaze and the transparent base glaze are very close, and the color difference delta E is below 3NBS units.
Example 4:
the preparation method of the mullite-reinforced transparent glaze comprises the following steps:
100 parts by mass of a transparent base glaze (chemical composition: 63.84wt% of SiO) 2 13.89 weight percent of CaO, 8.61 weight percent of ZnO, and 5.56 weight percent of Al 2 O 3 3.58 wt.% of K 2 O, mgO 0.93wt%, baO 0.53wt%, zrO 0.19wt% 2 0.16wt% of Fe 2 O 3 0.07wt% of TiO 2 0.04wt% of PbO, 0.02wt% of As 2 O 3 0.02wt% of NiO, and the balance of loss on ignition), 20 parts of mullite (the granularity is 100-325 meshes) and 0.36 part of carboxymethyl cellulose are mixed and subjected to wet ball milling for 15min to prepare glaze slurry, then glaze is applied to a biscuit-fired ceramic blank in a glaze spraying manner, drying is carried out, then the ceramic blank is put into a box-type electric furnace to be heated to 1200 ℃ at the heating rate of 10 ℃/min, and then heat preservation is carried out for 10min, and cooling is carried out, thus obtaining the mullite-reinforced transparent glaze.
Through tests, (the test method is the same as that of the example 1), the mullite enhanced transparent glaze prepared in the example has a mullite crystal phase and a mosaic structure formed by large mullite particles and small mullite particles, the Vickers hardness of the mullite enhanced transparent glaze is 7.20GPa, the hardness is improved by 5.7% compared with that of a transparent base glaze (the Vickers hardness is 6.81 GPa), the colors of the mullite enhanced transparent glaze and the transparent base glaze are very close, and the color difference delta E is below 3NBS unit.
Example 5:
the preparation method of the mullite-reinforced transparent glaze comprises the following steps:
100 parts by mass of a transparent base glaze (chemical composition: 63.84wt% of SiO) 2 13.89 weight percent of CaO, 8.61 weight percent of ZnO, and 5.56 weight percent of Al 2 O 3 3.58 wt.% of K 2 O, mgO 0.93wt%, baO 0.53wt%, zrO 0.19wt% 2 0.16wt% of Fe 2 O 3 0.07wt% of TiO 2 0.04wt% of PbO, 0.02wt% of As 2 O 3 0.02wt% of NiO, and the balance of loss on ignition), 10 parts of mullite (the granularity is 100-325 meshes) and 0.33 part of carboxymethyl cellulose are mixed and subjected to wet ball milling for 15min to prepare glaze slurry, then glaze is applied to a biscuit-fired ceramic blank in a glaze spraying manner, drying is carried out, then the ceramic blank is put into a box-type electric furnace to be heated to 1150 ℃ at the heating rate of 10 ℃/min, and then heat preservation is carried out for 10min, and cooling is carried out, thus obtaining the mullite reinforced transparent glaze.
Through tests, (the test method is the same as that of the example 1), the mullite enhanced transparent glaze prepared in the example has a mullite crystal phase and a mosaic structure formed by large mullite particles and small mullite particles, the Vickers hardness of the mullite enhanced transparent glaze is 7.18GPa, the hardness of the mullite enhanced transparent glaze is improved by 5.4% compared with that of transparent base glaze (the Vickers hardness is 6.81 GPa), the colors of the mullite enhanced transparent glaze and the transparent base glaze are very close, and the color difference delta E is below 3NBS unit.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The mullite reinforced transparent glaze is characterized by comprising the following components in percentage by mass:
transparent base glaze: 75 to 95 percent;
mullite: 5% -25%;
the transparent base glaze comprises the following components in percentage by mass:
SiO 2 ：62％～65％；
CaO：11％～14％；
ZnO：7％～9％；
Al 2 O 3 ：5％～12％；
K 2 O：3％～5％；
MgO：0.8％～1％；
BaO：0.4％～1％。
2. the mullite-reinforced transparent glaze according to claim 1, wherein: the granularity of the mullite is 100 meshes-325 meshes.
3. A process for the preparation of a mullite-reinforced clear glaze according to claim 1 or 2, characterized in that it comprises the following steps: mixing the transparent base glaze, mullite and a dispersing agent, carrying out wet ball milling to prepare glaze slurry, glazing the ceramic blank, and firing to obtain the mullite-reinforced transparent glaze.
4. The production method according to claim 3, characterized in that: the dispersant is at least one of carboxymethyl cellulose, sodium carboxymethyl cellulose and sodium tripolyphosphate.
5. The production method according to claim 3 or 4, characterized in that: the time of the wet ball milling is 15 min-30 min.
6. The production method according to claim 3 or 4, characterized in that: the glazing mode is one of glaze spraying, glaze dipping and glaze pouring.
7. The production method according to claim 3 or 4, characterized in that: the firing is carried out at 1150-1200 ℃ and the heat preservation time is 5-10 min.
8. The method for producing according to claim 7, characterized in that: the firing operation comprises the following steps: heating to 1150-1200 ℃ at the heating rate of 10-40 ℃/min, and then preserving the heat for 5-10 min.
9. A ceramic article characterized by a surface applied with a mullite-reinforced clear glaze of claim 1 or 2.
10. The ceramic article of claim 9, wherein: the ceramic product is one of wall brick and floor tile.
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