CN115286249A - Self-cleaning glaze and application thereof - Google Patents
Self-cleaning glaze and application thereof Download PDFInfo
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- CN115286249A CN115286249A CN202211009478.1A CN202211009478A CN115286249A CN 115286249 A CN115286249 A CN 115286249A CN 202211009478 A CN202211009478 A CN 202211009478A CN 115286249 A CN115286249 A CN 115286249A
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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
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
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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
- 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
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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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
- 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
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
Abstract
The invention discloses a self-cleaning glaze and a preparation method thereof, wherein the raw materials comprise glaze frit, quartz, basic fluxing components, zinc oxide, kaolin, fluorite, barium sulfate, cerium oxide and sodium carbonate; mixing the raw materials with water, grinding to obtain glaze slip, spraying the glaze slip on the surface of white glaze of sanitary ceramics to form a self-cleaning glaze layer, and then sintering in an oxygen atmosphere, wherein the highest sintering temperature is controlled at 1200-1250 ℃, and the temperature is kept for 0.5-1.5 h. The invention reduces the number of glaze bubbles and improves the compactness, the strength and the smoothness of the self-cleaning glaze.
Description
Technical Field
The invention belongs to the field of sanitary ceramics, and particularly relates to a self-cleaning glaze and application thereof.
Background
The self-cleaning glaze is processed on the surface layer of the original glaze, and finally forms a clean surface of the sanitary ceramic after high-temperature firing, and the sanitary ceramic is expected to have ultra-smooth texture, so that dirt is difficult to attach. The self-cleaning glaze technology generally takes frit as a main body, adds quartz, feldspar, kaolin, zinc oxide and other materials to form a self-cleaning glaze formula system, sprays the self-cleaning glaze formula system on the surface of common white glaze, and simultaneously burns the self-cleaning glaze formula system and the white glaze at a high temperature to form the self-cleaning glaze.
The method is characterized in that a blank and a glaze material can be decomposed to generate gas (the decomposition temperature is mainly concentrated at the stage of 800-1150 ℃) when the ceramic is fired, the gas is directly discharged from pores before the glaze material is not melted, the firing temperature of the self-cleaning glaze is relatively lower than that of white glaze, the self-cleaning glaze material is gradually melted at about 850 ℃ to generate a liquid phase, the generated liquid phase plays a role of sealing to cause unsmooth exhaust, the gas is firstly dissolved in the melted liquid phase, bubbles can be separated out on a white glaze layer and a self-cleaning glaze layer after saturation is achieved, small bubbles are left on the surface of the self-cleaning glaze material and are not completely discharged to form micropores after cooling, bubble cavities are left in the self-cleaning glaze material, the bubbles are sealed in the self-cleaning glaze material as defects, the compactness of the self-cleaning glaze surface can be influenced, the strength and the optical permeability are reduced, and if more bubbles on the surface of the self-cleaning glaze material applied to the sanitary ceramic industry can also store dirt to cause the difficulty in cleaning of the ceramic surface.
The existing solution is mainly to reduce bubbles in the glaze by prolonging the heat preservation time of a high-temperature section, but the glaze has large high-temperature viscosity, large surface tension and very large additional pressure of bubbles with small radius, the bubbles are difficult to move and grow, the bubbles capable of being discharged are very limited, and the effect is not ideal.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an ultra-compact and ultra-smooth self-cleaning glaze and application thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a self-cleaning glaze comprises the following raw materials in parts by mass: 60-80 parts of glaze frit, 10-15 parts of quartz, 1-5 parts of first basic component, 0.5-2 parts of second basic component, 2-4 parts of zinc oxide, 3-6 parts of kaolin, 0.5-2 parts of fluorite, 0.5-2 parts of barium sulfate, 0.2-0.5 part of cerium oxide and 0.1-0.2 part of sodium carbonate; the first base component is selected from at least one of potassium feldspar, albite and nepheline, and the second base component is selected from at least one of dolomite, wollastonite and talc.
Optionally, the melting start temperature of the glaze frit is 800-1000 ℃.
Optionally, the frit for glaze comprises the following components in parts by mass: siO 2 2 60 to 68 portions of Al 2 O 3 10 to 14 portions of K 2 O2.5-3.5 parts, na 2 1.0 to 2.5 portions of O, 9 to 13 portions of CaO, 1 to 2.5 portions of MgO and 4.5 to 7 portions of ZnO.
A preparation method of sanitary ceramics comprises the following steps:
1) Mixing the self-cleaning glaze raw material with water, grinding until the grain size is less than or equal to 10 mu m, wherein the proportion is 70-75%, taking out of the mill, sieving to remove iron, and adding an auxiliary agent to adjust the performance of the glaze slip;
2) Spraying the glaze slip on the surface of a white glaze layer of the sanitary ceramic to form a self-cleaning glaze layer, and drying;
3) Sintering in oxygen atmosphere, controlling the highest temperature of sintering at 1200-1250 ℃, and keeping the temperature for 0.5-1.5 h.
Optionally, in the step 1), the concentration of the glaze slip is 350-353 g/200ml, the viscosity is marrioto V060-70 seconds, and the drying time is 6-10 min.
Optionally, in the step 2), the spraying thickness is 0.1-0.3 mm.
Optionally, in the step 2), the spraying pressure is 0.3-0.5 Mpa, and the discharge rate is 80-110 seconds/200 ml.
Optionally, in the step 3), the firing period is 15 to 30 hours, wherein the cooling period is 6 to 10 hours, and the peroxide coefficient is 1 to 4 percent.
Further, the temperature rise stage comprises the steps of rising the temperature to 750-850 ℃ at a first temperature rise rate, then rising the temperature to 1050-1150 ℃ at a second temperature rise rate, and then rising the temperature to 1200-1250 ℃ at a third temperature rise rate, wherein the third temperature rise rate is larger than the first temperature rise rate and larger than the second temperature rise rate.
Optionally, the white glaze layer is prepared by the following method:
a. weighing the following raw materials in parts by mass: 30-40 parts of potassium feldspar, 25-35 parts of quartz, 10-20 parts of calcite, 3-10 parts of dolomite, 5-15 parts of zirconium silicate, 2-10 parts of kaolin, 1-5 parts of alumina and 1-5 parts of zinc oxide;
b. mixing the raw materials with water, grinding until the particle size is less than or equal to 10 mu m and the ratio is 67-72%, taking out the mixture, grinding to obtain white glaze slip, and spraying the white glaze slip on the surface of a blank to form a white glaze layer.
Furthermore, the concentration of the white glaze slip is 350-360g/200ml, the viscosity is Mariotron V0 for 90-120 seconds, and the drying time is 15-25min.
Optionally, the auxiliary agent comprises 0.1-0.5 parts by mass of CMC and 0.01-0.1 parts by mass of dispergator.
The sanitary ceramic with the ultra-compact and ultra-smooth self-cleaning glaze prepared by the preparation method.
The invention has the beneficial effects that:
1. decomposition of 4CeO at high temperature by means of cerium oxide 2 →2Ce 2 O 3 +O 2 ℃,. According to Stokes law, the radius of bubbles is increased, the rising speed of the bubbles is increased, so that the purpose of reducing the bubbles remained in the self-cleaning glaze layer is achieved, the quantity of the bubbles of the glaze surface is correspondingly reduced, and the compactness, the strength and the smoothness of the glaze surface of the self-cleaning glaze are improved;
2. the high-temperature viscosity of the glaze can be reduced by introducing stronger network disruptors such as fluorite, barium sulfate, cerium oxide and the like into a formula system, and the fluorite (calcium fluoride) is the strongest silica network disruptor, so that the high-temperature viscosity of the glaze is greatly reduced, the additional pressure of small bubbles is reduced by 2 sigma/r, and the large-size high-temperature glaze is more beneficial to gathering, growing and accelerating discharge of the bubbles;
3. in the process of ceramic sintering and temperature reduction, the temperature is reduced, and the cerium oxide can gradually absorb the dissolved oxygen 2Ce in the liquid phase 2 O 3 +O 2 →4CeO 2 The generation of small bubbles in the cooling and hardening time period of the self-cleaning glaze is reduced, the small bubbles are promoted to be dissolved in the liquid phase, and the number of residual bubbles in the glaze is further reduced.
Detailed Description
The following specific examples further illustrate the invention.
Example 1
The self-cleaning glaze is prepared from the following components in parts by weight: 809 fusion cake 75 parts, quartz 14 parts, potassium feldspar 2 parts, zinc oxide 1 part, kaolin 5 parts, dolomite 1 part, fluorite 1.0 part, barium sulfate 1 part, cerium oxide 0.3 part and sodium carbonate 0.12 part. Wherein the 809 fusion cake comprises the following components in parts by mass: siO 2 2 65.3 parts of Al 2 O 3 11.9 parts of K 2 O2.81 parts and Na 2 1.28 parts of O, 9.80 parts of CaO9, 2.10 parts of MgO2 and 6.57 parts of ZnO6.
The self-cleaning glaze is prepared according to the proportion as follows: grinding with water =100, ball-milling until the particle size is less than or equal to 10 μm, and sieving with a 180-mesh sieve; adding 0.2 mass part of CMC and 0.05 mass part of dispergator to adjust the slurry properties to be as follows: concentration 350/200ml, viscosity Marrioot tube V0 65 seconds, drying time about 8min.
Spraying self-cleaning glaze on the surface of white glaze layer of sanitary ceramic to form self-cleaning glaze layer, spraying at 0.4Mpa and discharge rate of 100 s/200 ml and thickness of 0.15mm, and drying for 15-20min. Wherein the white glaze layer surface of the sanitary ceramic can be firstly formed according to the following method: weighing 30-40 parts of potash feldspar, 25-35 parts of quartz, 10-20 parts of calcite, 3-10 parts of dolomite, 5-15 parts of zirconium silicate, 2-10 parts of kaolin, 1-5 parts of aluminum oxide and 1-5 parts of zinc oxide according to the mass parts, mixing with water, grinding, adding 0.15% of sodium carbonate until the granularity is less than or equal to 10 mu m, wherein the percentage is 67-72%, grinding, sieving, removing iron, adding 0.5% of CMC and 0.05% of dispergator to adjust the performance of the glaze slurry to 355g/200ml, adjusting the viscosity of a Mario tube V for 0 second 100 seconds, and drying for about 20min; and spraying the white glaze slurry on the surface of a green body of the sanitary ceramic to form a white glaze layer. The green body can be sanitary ceramic green body of known technology.
After the spraying of the self-cleaning glaze layer is finished, the self-cleaning glaze layer is sintered in a tunnel kiln, the peroxide coefficient is 2%, the sintering period is 18.6 hours, the temperature is firstly increased to 800 ℃ for 6 hours, then is increased to 1100 ℃ for 4 hours, is increased to the highest sintering temperature of 1240-1250 ℃ for 1 hour, is kept warm for 0.6 hour, and is then reduced to room temperature for about 7 hours, so that the sanitary ceramic with the ultra-compact and ultra-smooth self-cleaning glaze on the surface is obtained.
Example 2
The self-cleaning glaze is prepared from the following components in parts by weight: 809 fusion cake 75 parts, quartz 14 parts, potash feldspar 2 parts, zinc oxide 1 part, kaolin 5 parts, dolomite 1 part, fluorite 1.0 part, barium sulfate 1.5 parts, cerium oxide 0.2 part and sodium carbonate 0.12 part. The rest is the same as example 1.
Example 3
The self-cleaning glaze is prepared from the following components in parts by weight: 809 fusion cake 75 parts, quartz 14 parts, potash feldspar 2 parts, zinc oxide 1 part, kaolin 5 parts, dolomite 1 part, fluorite 0.9 part, barium sulfate 1.5 parts, cerium oxide 0.25 part and sodium carbonate 0.12 part. The rest is the same as example 1. The rest is the same as example 1.
Example 4
The self-cleaning glaze is prepared from the following components in parts by weight: 809 fusion cake 75 parts, quartz 14 parts, albite 2 parts, zinc oxide 1 part, kaolin 5 parts, wollastonite 1 part, fluorite 0.9 part, barium sulfate 1.5 parts, cerium oxide 0.25 part and sodium carbonate 0.12 part. The rest is the same as example 1. The rest is the same as example 1.
Example 5
The self-cleaning glaze is prepared from the following components in parts by weight: 809 fusion cake 75 parts, quartz 14 parts, nepheline 2 parts, zinc oxide 1 part, kaolin 5 parts, talc 1 part, fluorite 0.9 part, barium sulfate 1.5 parts, cerium oxide 0.25 part and sodium carbonate 0.12 part. The rest is the same as example 1.
Comparative examples 1 to 3
Comparative examples 1 to 3 are different from example 1 mainly in the addition amount of cerium oxide. The rest is the same as example 1.
Comparative examples 4 to 6
Comparative examples 4 to 6 are different from example 1 mainly in the amount of fluorite added. The rest is the same as example 1.
The glaze surface pores of examples 1 to 3 and comparative examples 1 to 6 were detected by comparison using an optical magnifier, and 9 sites were randomly detected to take an average value, and hardness was detected using a microhardness tester, and 3 sites were randomly detected to take an average value.
The proportioning and test results of the examples and comparative examples are as follows:
the main difference between examples 1 and 3 is that the addition amounts of cerium oxide and fluorite are slightly different, but the key characteristics of the glaze surface are all within acceptable ranges. The main difference between the example 4 and the example 3 is that albite replaces potassium feldspar, wollastonite replaces dolomite, the main difference between the example 5 and the example 3 is that nepheline replaces potassium feldspar, and talc replaces dolomite, all of the above are common ceramic glaze fluxing agents, and replacement fine adjustment is performed mainly according to the thermal expansion coefficient, the firing temperature range, the gloss requirement and the like of blanks of different companies, and no obvious difference exists in other characteristics of the glaze slip.
The proportion of cerium oxide is changed in comparative examples 1 to 3, and it can be seen that the quantity of bubbles is gradually reduced and the hardness is gradually increased with the increase of cerium oxide, but the excessive cerium oxide causes the increase of bubbles and the reduction of hardness, because the excessive cerium oxide has too large reduction range of viscosity, and the bubbles dissolved in the liquid phase during the temperature reduction process are more easily separated out to generate small bubbles, so that the cerium oxide is preferably added in the range of 0.2 to 0.3 percent.
Comparative examples 4 to 6 change the amount of fluorite added, and it can be seen that with the increase of fluorite, the number of bubbles is gradually reduced, and the hardness is gradually increased, but the excessive fluorite causes the increase of bubbles, because the excessive fluorite causes the rapid reduction of viscosity and surface tension in a high-temperature section, a large amount of small bubbles are generated and slowly rise to be discharged, and the bubbles which can not be discharged in the cooling process are sealed and glazed, so the bubbles can not be converged to be rapidly discharged to achieve the purpose of reducing the bubbles. The hardness is reduced, and mainly Si-F and B-F bonds are stronger than Si-O and B-O bonds and are easy to break.
The above embodiments are only used to further illustrate a self-cleaning glaze and its application, but the present invention is not limited to the embodiments, and any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. The self-cleaning glaze is characterized by comprising the following raw materials in parts by mass: 60-80 parts of glaze frit, 10-15 parts of quartz, 1-5 parts of first basic component, 0.5-2 parts of second basic component, 2-4 parts of zinc oxide, 3-6 parts of kaolin, 0.5-2 parts of fluorite, 0.5-2 parts of barium sulfate, 0.2-0.5 part of cerium oxide and 0.1-0.2 part of sodium carbonate; the first base component is selected from at least one of potassium feldspar, albite and nepheline, and the second base component is selected from at least one of dolomite, wollastonite and talc.
2. A self-cleaning glaze according to claim 1, wherein: the melting start temperature of the frit for glaze is 800-1000 ℃.
3. A self-cleaning glaze according to claim 1, wherein: the frit for glaze comprises the following components in parts by mass: siO 2 2 60 to 80 portions of Al 2 O 3 10 to 14 portions of K 2 2.5 to 3.5 portions of O and Na 2 1.0 to 2.5 portions of O, 9 to 13 portions of CaO, 1 to 2.5 portions of MgO and 4.5 to 7 portions of ZnO.
4. The preparation method of the sanitary ceramic with the self-cleaning glaze is characterized by comprising the following steps:
1) Mixing the self-cleaning glaze raw material of claim 1 with water, grinding until the proportion of the particle size of less than or equal to 10 μm is 70-75%, taking out, sieving to remove iron, and adding an auxiliary agent to adjust the performance of the glaze slip;
2) Spraying the glaze slip on the surface of a white glaze layer of the sanitary ceramic to form a self-cleaning glaze layer, and drying;
3) Sintering in oxygen atmosphere, controlling the highest temperature of sintering at 1200-1250 ℃, and keeping the temperature for 0.5-1.5 h.
5. The method of claim 4, wherein: in the step 1), the concentration of the glaze slip is 350-353 g/200ml, the viscosity is Marriot tube V0-70 seconds, and the drying time is 6-10 min.
6. The method of manufacturing according to claim 4, characterized in that: in the step 2), the spraying thickness is 0.1-0.3 mm.
7. The method of manufacturing according to claim 4, characterized in that: in the step 2), the spraying pressure is 0.3-0.5 Mpa, and the discharge rate is 80-110 seconds/200 ml.
8. The method of manufacturing according to claim 4, characterized in that: in the step 3), the sintering period is 15-30 hours, wherein the cooling period is 6-10 hours, and the peroxide coefficient is 1% -4%.
9. The method according to claim 4, wherein the white glaze layer is prepared by:
a. weighing the following raw materials in parts by mass: 30 to 40 parts of potash feldspar, 25 to 35 parts of quartz, 10 to 20 parts of calcite, 3 to 10 parts of dolomite, 5 to 15 parts of zirconium silicate, 2 to 10 parts of kaolin, 1 to 5 parts of aluminum oxide and 1 to 5 parts of zinc oxide;
b. mixing the raw materials with water, grinding until the particle size is less than or equal to 10 mu m and the ratio is 67-72%, grinding to obtain white glaze slip, and spraying the white glaze slip on the surface of a blank body to form a white glaze layer.
10. A sanitary ceramic having a self-cleaning glaze prepared by the preparation method according to any one of claims 4 to 9.
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| CN116986922A (en) * | 2023-08-03 | 2023-11-03 | 潮州市德科陶瓷有限公司 | Nano self-cleaning ceramic glaze and preparation method thereof |
| CN117024119A (en) * | 2023-10-10 | 2023-11-10 | 淄博坤阳陶瓷有限公司 | Preparation method of self-cleaning glazed ceramic cup |
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| CN114213158A (en) * | 2022-01-04 | 2022-03-22 | 佛山东鹏洁具股份有限公司 | High-quality sanitary ceramic and glazing process and preparation method thereof |
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| CN116986922A (en) * | 2023-08-03 | 2023-11-03 | 潮州市德科陶瓷有限公司 | Nano self-cleaning ceramic glaze and preparation method thereof |
| CN117024119A (en) * | 2023-10-10 | 2023-11-10 | 淄博坤阳陶瓷有限公司 | Preparation method of self-cleaning glazed ceramic cup |
| CN117024119B (en) * | 2023-10-10 | 2023-12-12 | 淄博坤阳陶瓷有限公司 | Preparation method of self-cleaning glazed ceramic cup |
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