CN116986819B - Corrosion-resistant ceramic glaze and preparation method thereof - Google Patents
Corrosion-resistant ceramic glaze and preparation method thereofInfo
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- CN116986819B CN116986819B CN202311008224.2A CN202311008224A CN116986819B CN 116986819 B CN116986819 B CN 116986819B CN 202311008224 A CN202311008224 A CN 202311008224A CN 116986819 B CN116986819 B CN 116986819B
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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
- C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a corrosion-resistant ceramic glaze and a preparation method thereof, and relates to the technical field of ceramic glaze production, wherein the corrosion-resistant ceramic glaze is prepared from the following raw material components of feldspar, kaolin, refractory clay, zirconium silicate, zirconium oxide, zircon, graphene oxide, calcium oxide and deionized water; the method comprises the steps of crushing and grinding feldspar, kaolin and zircon, putting the crushed and ground feldspar, kaolin and zircon and the rest solid raw materials into a ball milling tank of ball milling equipment for ball milling for 1-2 hours, heating the ball milling tank to enable glaze particles to be more tiny and uniform, then soaking powder into deionized water, stirring mixed liquid by a high-speed stirrer for 0.5-0.6 hour to form glaze slurry, and adding zirconium silicate into ceramic glaze materials to enable the strength, wear resistance, hydrolysis resistance and corrosion resistance of a ceramic glaze layer to be improved.
Description
Technical Field
The invention relates to the technical field of ceramic glaze production, in particular to a corrosion-resistant ceramic glaze and a preparation method thereof.
Background
Ceramic glazes are a type of suspended powder for the surface of ceramic articles, consisting of a plurality of chemicals. The glaze can be applied to the surface of a ceramic ware in a spray, brush or dip coating mode, and a glaze layer with excellent performances of hardness, smoothness, water resistance, acid and alkali resistance, corrosion resistance and the like is formed after firing, so that the ceramic surface is protected, the ceramic appearance is beautified, and meanwhile, the ceramic can be cleaned more easily.
The surface of the ceramic product is generally provided with a ceramic glaze layer, when the ceramic product is used, the ceramic product is also contacted with water, acid liquor or alkali liquor frequently to generate chemical reaction, the oxide surface layer of the ceramic glaze layer is usually corroded, the surface layer is dissolved or peeled off to reduce the glaze gloss of the ceramic product, the alkaline substance is reacted to generate toxic alkali metal glass to further damage the integrity and the aesthetic property of the ceramic, the corrosion resistance of the traditional ceramic glaze is not ideal and can not meet the requirements in practical use, and therefore, the corrosion-resistant ceramic glaze and the preparation method thereof are provided.
Disclosure of Invention
The technical problem solved by the invention is that in the prior art, a ceramic glaze layer on the surface of a ceramic product is easy to be corroded by acid and alkali, the corrosion resistance of the ceramic glaze is not ideal, and the requirements in actual use cannot be met.
The corrosion-resistant ceramic glaze is prepared from the following raw materials of 15-25 parts of feldspar, 15-20 parts of kaolin, 18-22 parts of refractory clay, 5-10 parts of zirconium silicate, 5-7 parts of zirconium oxide, 5-10 parts of zircon, 10-15 parts of graphene oxide, 18-20 parts of calcium oxide and 20-30 parts of deionized water.
The preparation method of the corrosion-resistant ceramic glaze comprises the steps of weighing raw materials according to the raw material formula of the ceramic glaze, and then preparing according to the following preparation method:
firstly, drying feldspar, kaolin and zirconite, crushing and grinding to form powder, and sieving to obtain powder with the particle size meeting the requirement;
putting the powder obtained in the first step and the residual solid raw materials into a ball milling tank of ball milling equipment for ball milling for 1-2 hours, and heating the ball milling tank to ensure that glaze particle particles are more tiny and uniform;
Step three, soaking the powder obtained in the step two in deionized water, and stirring the mixed solution for 0.5-0.6h by adopting a high-speed stirrer to form glaze slip;
Fourthly, spraying the glaze particles obtained in the third step on the surface of the ceramic ware, and then placing the ceramic ware in a furnace for high-temperature firing at 800-1200 ℃ to obtain the corrosion-resistant ceramic glaze layer.
In the first step, feldspar, kaolin and zirconite are subjected to vacuum drying, and then are placed into a vacuum drying oven, the vacuum degree of the vacuum drying oven is set to be-0.1 MPa, and the temperature is raised to 500-600 ℃ at the speed of 5-8 ℃ per minute in nitrogen, and the temperature is kept for 0.5-1h.
A further technical improvement of the invention is that in the first step, the mesh of the powder is 100-150 mesh.
In the second step, high-temperature nitrogen is introduced into the ball milling tank of the ball milling equipment, so that the temperature in the ball milling tank reaches 1000-1200 ℃.
The invention further technically improves the stirring speed in the step three to be 200-300rpm/min.
Compared with the prior art, the invention has the following beneficial effects:
1. According to the invention, zirconium silicate and graphene oxide are added into the ceramic glaze material, so that the strength, wear resistance, hydrolysis resistance and corrosion resistance of the ceramic glaze layer are improved, meanwhile, the self-cleaning capability is enhanced, and the graphene oxide has excellent acid resistance and alkali resistance, so that the corrosion resistance of the ceramic glaze can be effectively improved.
2. According to the invention, during preparation of the ceramic glaze, the feldspar, the kaolin and the zirconite are firstly subjected to vacuum drying, so that the moisture of the feldspar, the kaolin and the zirconite can be reduced, and powder adhesion on the inner wall of the equipment and subsequent cleaning of workers are reduced when the feldspar, the kaolin and the zirconite are treated by crushing equipment and grinding equipment;
3. In the invention, when the raw materials are further ground, the raw materials are placed in the ball milling tank, and high-temperature nitrogen is introduced, so that the viscosity of zirconium silicate and graphene oxide is reduced, the zirconium silicate and the graphene oxide are not easy to adhere to the inner wall of the ball milling tank, and further, each component in the raw materials is not reduced, thus ensuring that sufficient zirconium silicate and graphene oxide can play a role in corrosion resistance in ceramic glaze.
Detailed Description
In order to further describe the technical means and effects adopted for achieving the preset aim of the invention, the following detailed description is given below of the specific implementation, structure, characteristics and effects according to the present invention in combination with the preferred embodiments.
Example 1
15 Parts of feldspar, 15 parts of kaolin, 18 parts of refractory clay, 5 parts of zirconium silicate, 5 parts of zirconium oxide, 5 parts of zircon, 10 parts of graphene oxide, 18 parts of calcium oxide and 20 parts of deionized water;
Step two, vacuum drying feldspar, kaolin and zirconite, putting the feldspar, the kaolin and the zirconite into a vacuum drying box, setting the vacuum degree of the vacuum drying box to be-0.1 MPa, heating to 500 ℃ at a speed of 5 ℃ per minute in nitrogen, and preserving heat for 0.5h;
Putting the powder obtained in the second step and the residual solid raw materials into a ball milling tank of ball milling equipment for ball milling for 1h, and introducing nitrogen with the temperature of 1000 ℃ into the ball milling tank to ensure that glaze particles are more tiny and uniform;
soaking the powder obtained in the step three in deionized water, stirring the mixed solution for 0.5h by adopting a high-speed stirrer at the stirring speed of 200rpm/min to form glaze slip;
And fifthly, spraying the glaze particles obtained in the step four on the surface of a ceramic ware, and then placing the ceramic ware in a furnace for high-temperature firing, wherein the temperature in the furnace is 800 ℃ to obtain the corrosion-resistant ceramic glaze layer.
Example two
15 Parts of feldspar, 15 parts of kaolin, 18 parts of refractory clay, 5 parts of zirconium silicate, 5 parts of zirconium oxide, 5 parts of zircon, 10 parts of graphene oxide, 18 parts of calcium oxide and 20 parts of deionized water;
step two, vacuum drying feldspar, kaolin and zirconite, putting the feldspar, the kaolin and the zirconite into a vacuum drying box, setting the vacuum degree of the vacuum drying box to be-0.1 MPa, heating to 600 ℃ at the speed of 8 ℃ per minute in nitrogen, and preserving heat for 1h;
putting the powder obtained in the second step and the residual solid raw materials into a ball milling tank of ball milling equipment for ball milling for 2 hours, and introducing nitrogen with the temperature of 1100 ℃ into the ball milling tank to ensure that glaze particles are more tiny and uniform;
Soaking the powder obtained in the step three in deionized water, stirring the mixed solution for 0.6h by adopting a high-speed stirrer at the stirring speed of 300rpm/min to form glaze slip;
spraying the glaze particles obtained in the step four on the surface of a ceramic ware, and then placing the ceramic ware in a furnace for high-temperature firing, wherein the temperature in the furnace is 1200 ℃ to obtain a corrosion-resistant ceramic glaze layer;
example III
15 Parts of feldspar, 15 parts of kaolin, 18 parts of refractory clay, 5 parts of zirconium silicate, 5 parts of zirconium oxide, 5 parts of zircon, 10 parts of graphene oxide, 18 parts of calcium oxide and 20 parts of deionized water;
Step two, vacuum drying feldspar, kaolin and zirconite, putting the feldspar, the kaolin and the zirconite into a vacuum drying box, setting the vacuum degree of the vacuum drying box to be-0.1 MPa, heating to 550 ℃ at the speed of 6 ℃ per minute in nitrogen, and preserving heat for 1h;
putting the powder obtained in the second step and the residual solid raw materials into a ball milling tank of ball milling equipment for ball milling for 1.5 hours, and heating the ball milling tank until the internal temperature of the ball milling tank reaches 110 ℃ so that the particles of the glaze material are more tiny and uniform;
soaking the powder obtained in the step three in deionized water, stirring the mixed solution for 0.55h by adopting a high-speed stirrer at the stirring speed of 250rpm/min to form glaze slip;
Spraying the glaze particles obtained in the step four on the surface of a ceramic ware, and then placing the ceramic ware in a furnace for high-temperature firing at the temperature of 1000 ℃ to obtain a corrosion-resistant ceramic glaze layer;
Comparative example one
15 Parts of feldspar, 15 parts of kaolin, 18 parts of refractory clay, 5 parts of zirconia, 5 parts of zircon, 18 parts of calcium oxide and 20 parts of deionized water;
Step two, vacuum drying feldspar, kaolin and zirconite, putting the feldspar, the kaolin and the zirconite into a vacuum drying box, setting the vacuum degree of the vacuum drying box to be-0.1 MPa, heating to 500 ℃ at a speed of 5 ℃ per minute in nitrogen, and preserving heat for 0.5h;
Putting the powder obtained in the second step and the residual solid raw materials into a ball milling tank of ball milling equipment for ball milling for 1h, and introducing nitrogen with the temperature of 1200 ℃ into the ball milling tank until the internal temperature of the ball milling tank reaches 100 ℃ so as to ensure that glaze particles are more tiny and uniform;
soaking the powder obtained in the step three in deionized water, stirring the mixed solution for 0.5h by adopting a high-speed stirrer at the stirring speed of 200rpm/min to form glaze slip;
spraying the glaze particles obtained in the step four on the surface of a ceramic ware, and then placing the ceramic ware in a furnace for high-temperature firing, wherein the temperature in the furnace is 800 ℃ to obtain a corrosion-resistant ceramic glaze layer;
The difference between the first comparative example and the first example is that zirconium silicate and graphene oxide are not added in the first comparative example, and the rest steps and parameters are the same;
Comparative example two
15 Parts of feldspar, 15 parts of kaolin, 18 parts of refractory clay, 5 parts of zirconium silicate, 5 parts of zirconium oxide, 5 parts of zircon, 10 parts of graphene oxide, 18 parts of calcium oxide and 20 parts of deionized water;
Step two, vacuum drying feldspar, kaolin and zirconite, putting the feldspar, the kaolin and the zirconite into a vacuum drying box, setting the vacuum degree of the vacuum drying box to be-0.1 MPa, heating to 500 ℃ at a speed of 5 ℃ per minute in nitrogen, and preserving heat for 0.5h;
Putting the powder obtained in the second step and the residual solid raw materials into a ball milling tank of ball milling equipment together for ball milling for 1h until the internal temperature of the ball milling tank reaches 100 ℃ so that the particles of the glaze material are more tiny and uniform;
soaking the powder obtained in the step three in deionized water, stirring the mixed solution for 0.5h by adopting a high-speed stirrer at the stirring speed of 200rpm/min to form glaze slip;
spraying the glaze particles obtained in the step four on the surface of a ceramic ware, and then placing the ceramic ware in a furnace for high-temperature firing, wherein the temperature in the furnace is 800 ℃ to obtain a corrosion-resistant ceramic glaze layer;
15-25 parts of feldspar, 15-20 parts of kaolin, 18-22 parts of refractory clay, 5-10 parts of zirconium silicate, 5-7 parts of zirconium oxide, 5-10 parts of zirconite, 10-15 parts of graphene oxide, 18-20 parts of calcium oxide and 20-30 parts of deionized water;
the difference between the second comparative example and the first comparative example is that the second comparative example did not introduce high temperature nitrogen gas into the ball milling pot, and the other steps and parameters were the same.
Performance tests were performed on the corrosion resistant ceramic glaze layers prepared in examples 1-3 and comparative examples 1-2:
(1) According to GB/T3810.13-2016, performing chemical corrosion resistance test, placing ceramic products containing the ceramic glaze layer in 6wt% nitric acid solution and 22wt% potassium hydroxide solution respectively, standing for 12 hours, and observing the surface change of the ceramic products to obtain the following results shown in Table 1;
(2) The abrasion resistance of the glazed tile surface is measured according to GB/T3810.7-2016, and the obtained result is shown in the following table 1, wherein the abrasion resistance of the glazed tile is divided into four grades, namely, grade 1-4 of PEI, the application range is respectively 1 grade which is only suitable for household ground, grade 2 which is used in places with little people flow, grade 3 which is suitable for public places with more people flow, and grade 4 which is used in public places with more people flow such as squares;
the test results are shown in table 1;
TABLE 1
In the second comparative example, when the raw materials are further ground, the raw materials are placed in a ball milling tank, and zirconium silicate and graphene oxide are easy to adhere to the inner wall of the ball milling tank due to the fact that the viscosity of the zirconium silicate and the graphene oxide is high, so that the components of the zirconium silicate and the graphene oxide in the raw materials are reduced, and the ceramic glaze lacks enough zirconium silicate and graphene oxide, so that spots appear on the surface of a ceramic product, and the color of the surface of the ceramic is darkened;
the ceramic glaze layer on the surface of the ceramic product in the comparative example 1-2 is corroded, and the surface of the ceramic product obtained in the embodiment 1-3 of the invention is unchanged, so that the ceramic product has good acid-base corrosion resistance, the ceramic product with the ceramic glaze layer on the surface obtained in the comparative example 1-2 of the invention has the wear resistance reaching the standard grade 3 requirement, and the ceramic product with the ceramic glaze layer on the surface obtained in the embodiment 1-3 of the invention has the wear resistance reaching the standard grade 4 requirement, has good wear resistance and can be used on the ground where pedestrians walk frequently.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The corrosion-resistant ceramic glaze is characterized by being prepared from the following raw materials, by weight, 15-25 parts of feldspar, 15-20 parts of kaolin, 18-22 parts of refractory clay, 5-10 parts of zirconium silicate, 5-7 parts of zirconium oxide, 5-10 parts of zircon, 10-15 parts of graphene oxide, 18-20 parts of calcium oxide and 20-30 parts of deionized water;
firstly, drying feldspar, kaolin and zirconite, crushing and grinding to form powder, and sieving to obtain powder with the particle size meeting the requirement;
Putting the powder obtained in the first step and the residual solid raw materials into a ball milling tank of ball milling equipment for ball milling for 1-2h, and heating the ball milling tank to ensure that glaze particles are more tiny and uniform;
Step three, soaking the powder obtained in the step two in deionized water, and stirring the mixed solution for 0.5-0.6h by adopting a high-speed stirrer to form glaze slip;
Fourthly, spraying the glaze particles obtained in the third step on the surface of the ceramic ware, and then placing the ceramic ware in a furnace for high-temperature firing at 800-1200 ℃ to obtain the corrosion-resistant ceramic glaze layer.
2. A method for preparing the corrosion-resistant ceramic glaze according to claim 1, wherein raw materials are weighed according to the raw material formula of the ceramic glaze in claim 1, and then the preparation is carried out according to the following preparation method:
firstly, drying feldspar, kaolin and zirconite, crushing and grinding to form powder, and sieving to obtain powder with the particle size meeting the requirement;
putting the powder obtained in the first step and the residual solid raw materials into a ball milling tank of ball milling equipment for ball milling for 1-2 hours, and heating the ball milling tank to ensure that glaze particle particles are more tiny and uniform;
Step three, soaking the powder obtained in the step two in deionized water, and stirring the mixed solution for 0.5-0.6h by adopting a high-speed stirrer to form glaze slip;
Fourthly, spraying the glaze particles obtained in the third step on the surface of the ceramic ware, and then placing the ceramic ware in a furnace for high-temperature firing at 800-1200 ℃ to obtain the corrosion-resistant ceramic glaze layer.
3. The method for producing a corrosion-resistant ceramic glaze according to claim 2, wherein in the first step, feldspar, kaolin and zirconite are vacuum-dried, and put into a vacuum drying oven, the vacuum degree of the vacuum drying oven is set to-0.1 MPa, and the temperature is raised to 500-600 ℃ at a rate of 5-8 ℃ per minute in nitrogen and kept for 0.5-1h.
4. The method for producing a corrosion-resistant ceramic glaze according to claim 2, wherein in the first step, the mesh size of the powder to be sieved is 100 to 150 mesh.
5. The method for preparing a corrosion-resistant ceramic glaze according to claim 2, wherein in the second step, high-temperature nitrogen is introduced into the ball milling tank of the ball milling device, so that the internal temperature of the ball milling tank reaches 1000-1200 ℃.
6. The method for producing a corrosion-resistant ceramic glaze according to claim 2, wherein in the third step, the stirring rate is 200 to 300rpm/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204866008U (en) * | 2015-06-19 | 2015-12-16 | 余苏祥 | Production pottery is with adding high -efficient ball mill of hot type |
| CN108585493A (en) * | 2018-06-28 | 2018-09-28 | 泉州市顶优优工业设计有限公司 | A kind of high temperature resistant graphene glaze water and preparation method thereof |
| CN109279780A (en) * | 2018-12-18 | 2019-01-29 | 湖南华联瓷业股份有限公司 | A kind of ceramic glaze and preparation method thereof of resistance to alkali corrosion |
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| CN111517824B (en) * | 2020-04-24 | 2022-06-14 | 佛山科学技术学院 | Wear-resistant corrosion-resistant ceramic glaze as well as preparation method and application thereof |
| CN112939459B (en) * | 2021-02-21 | 2022-07-22 | 潮州市祥发陶瓷有限公司 | Wear-resistant corrosion-resistant ceramic glaze as well as preparation method and application thereof |
| CN113896421B (en) * | 2021-10-14 | 2023-02-10 | 广东欧文莱陶瓷有限公司 | Wear-resistant digital ceramic glaze |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204866008U (en) * | 2015-06-19 | 2015-12-16 | 余苏祥 | Production pottery is with adding high -efficient ball mill of hot type |
| CN108585493A (en) * | 2018-06-28 | 2018-09-28 | 泉州市顶优优工业设计有限公司 | A kind of high temperature resistant graphene glaze water and preparation method thereof |
| CN109279780A (en) * | 2018-12-18 | 2019-01-29 | 湖南华联瓷业股份有限公司 | A kind of ceramic glaze and preparation method thereof of resistance to alkali corrosion |
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