CN115231825B - Ceramic raw material black glaze and preparation method thereof - Google Patents
Ceramic raw material black glaze and preparation method thereof Download PDFInfo
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- CN115231825B CN115231825B CN202210932576.6A CN202210932576A CN115231825B CN 115231825 B CN115231825 B CN 115231825B CN 202210932576 A CN202210932576 A CN 202210932576A CN 115231825 B CN115231825 B CN 115231825B
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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
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/02—Compositions for glass with special properties for coloured glass
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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 relates to a ceramic raw material black glaze and a preparation method thereof, belonging to the technical field of inorganic materials. The preparation method of the ceramic raw material black glaze comprises the following steps: A. preparing glaze slip; B. aging; C. glazing; D. drying; E. firing. The invention successfully adopts the resources of Panzhihua local kaolin, red mud, iron oxide ore and the like to prepare the black glaze, and has the characteristics of convenient material taking, low cost, non-toxic raw ore, environmental protection, health, suitability for industrialized production and the like. The black glaze of the ceramic raw material has good combination property of glaze slurry and biscuit, is applicable to firing in oxidizing atmosphere, is applicable to common electric kiln, and has simple procedures. The black glaze surface of the ceramic raw material disclosed by the invention has no pinholes, shrinkage glaze and flowing glaze, and has strong color sense and good overall artistic effect.
Description
Technical Field
The invention relates to a ceramic raw material black glaze and a preparation method thereof, belonging to the technical field of inorganic materials.
Background
The decoration of ceramic ware with black glaze is a traditional technological method for ceramic preparation in China. Black glazed ceramics are still popular for thousands of years due to their modesty, elegant, noble and stable glaze color. The development and improvement of black glaze have never been interrupted. The traditional black glaze process has unstable color, and the glaze surface is easy to generate a large number of pinholes, glaze shrinkage and other defects, the firing process is difficult to master, the product percent of pass is low, and the production cost is high. On the premise of ensuring high blackness, pure color and stable performance of the black glaze, simplifying the process, properly reducing the production cost and meeting the requirements of green and environment-friendly production is a hot spot in the current research field.
The traditional black glaze porcelain takes Jiangxi local natural materials as main raw materials, the firing temperature is 1230-1320 ℃, the traditional black glaze porcelain is manufactured by pure hands, and the traditional firewood kiln firing is needed to be reduced and fired. The traditional black glaze is generally oxidized and burned firstly and then reduced and burned, if the reduced and burned is not performed, the blackness is lower and the whiteness is higher.
The influence factors of black glaze firing are more, and at present, no technology for preparing ceramic raw black glaze with pure color and stable performance by using local resources of Panzhihua is available.
Disclosure of Invention
The first object of the invention is to provide a new preparation method of ceramic raw black glaze.
In order to achieve the first object of the present invention, the method for preparing the ceramic green black glaze comprises:
A. preparing glaze slip: mixing the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite, calcium oxide, chromium oxide and cobalt carbonate according to the weight ratio: 15-25:10-14:16-20:22-32:5-8:5-10:5-8:2-3:2-3, adding water for ball milling, and passing through a 250-target standard sieve after ball milling to obtain glaze slip; wherein the screen residue after passing through a 250-mesh standard screen is less than 0.5%;
B. and (3) staling: sealing the glaze slip, and standing for 24 hours at a shade and dry place;
C. glazing: firstly, uniformly stirring the aged glaze slurry, detecting and controlling the viscosity of the glaze slurry to be 10-13 mPa.s, and then uniformly attaching the glaze slurry to the surface of a clean biscuit firing ceramic body;
D. and (3) drying: drying the glazed ceramic body;
E. firing: starting the ceramic body dried in the step D to reach 300-400 ℃ from room temperature at a heating speed of 2-3 ℃/min; then the temperature rising speed of 4-5 ℃/min reaches 750-800 ℃, and the temperature is kept for 30-60 min; then the temperature rising speed of 3-4 ℃/min reaches 1250-1280 ℃, and the temperature is kept for 15-30 min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze product.
In a specific embodiment, the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite ore, calcium oxide, chromium oxide and cobalt carbonate are mixed according to the weight ratio: 20-25:12-14:16-20:27-32:5-8:5.7-10:5-8:2-3:2-3;
the total mass of the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite, calcium oxide, chromium oxide and cobalt carbonate is M, and the mass ratio of M to ball to water is preferably 1:1.5-2:1 during ball milling;
the method comprises the following steps of (by weight ratio) climbing flower local red mud, climbing flower local kaolin, quartz, potassium feldspar, talcum, hematite, calcium oxide, chromium oxide and cobalt carbonate: 20-25:12-14:16-20:27-32:5-8:5.7-10:5-8:2-3:2-3, and the whiteness can be below 2 and the glossiness can be above 20.
In one embodiment, the ball milling time is 5 to 10 minutes.
In one embodiment, sodium humate 0.5-1%M and sodium tripolyphosphate 0.2-0.5% M are added before ball milling in step A.
The added sodium humate and sodium tripolyphosphate can effectively improve the suspension property of particles in the black glaze slurry after ball milling, so that the glaze slurry has good dispersibility and high chemical stability, the glaze surface of the black glaze after firing is smoother, and the color stability of the black glaze is improved.
In a specific embodiment, the clean biscuit firing ceramic body is further subjected to pretreatment before glazing, wherein the pretreatment is to wipe dust on the surface of the biscuit firing ceramic body with wetted sponge, supplement water, and glazing after the surface of the ceramic body is air-dried with moisture. In the process of wiping ash by using the wet sponge, the wet sponge is used for properly supplementing water to the green body, so that the green body is too thick in glaze absorption during glaze soaking and the possibility of glaze flowing during sintering can be caused by no water supplementing.
In one embodiment, the glaze slip is uniformly adhered to the surface of the clean biscuit firing ceramic body by a method of dipping glaze.
In one embodiment, the method of glazing comprises: immersing the ceramic blank in the glaze for 1-2 s, and immersing the glaze for multiple times to keep the thickness of the glaze layer between 1 and 1.4 mm.
In one specific embodiment, the drying in the step D is drying at 100-120 ℃ for 30-60 min or natural air drying.
A second object of the invention is to provide a new ceramic green black glaze.
In order to achieve the second purpose of the invention, the ceramic raw material black glaze is prepared by adopting the preparation method of the ceramic raw material black glaze.
In a specific embodiment, the ceramic raw black glaze is a black glaze of a 1-1.4 mm thin glaze layer, and the whiteness is less than 2%.
In a specific embodiment, the ceramic green black glaze has a gloss level of 20% or more, preferably thermal shock resistance: quenching at 200-20 deg.c for 3 times without cracking. The quenching is to directly put a hot piece at 200 ℃ into cold water at 20 ℃.
The beneficial effects are that:
1. the invention successfully adopts the resources of the Panzhihua local kaolin, red mud, iron oxide ore and the like, does not introduce any toxic raw materials such as lead, cadmium and the like in the black glaze preparation process, does not have the harm of lead and cadmium leaching, has the characteristics of convenient material taking, low cost, non-toxic raw ore, environmental protection and health, suitability for industrial production and the like, and opens up a new technical line for the development and utilization of the Panzhihua local mineral resources.
2. The ceramic raw material black glaze has the characteristics of good combination of glaze slurry and biscuit, suitability for firing in oxidizing atmosphere, applicability for common electric kilns, simple working procedure, wider glaze firing temperature range, high blackness, pure color, stable performance, low cost, simple working procedure, green and environment-friendly performance and the like of the obtained black glaze product.
3. The invention discloses a ceramic raw material black glaze, belonging to raw ore glaze. The color of the raw ore glaze is different from that of other black glaze products, the color development is more natural, stable and elegant, the color development is greatly superior to that of chemical glaze, the application is more extensive, the method can be used for overglaze underglaze color, and the chemical glaze can only be used for underglaze color.
4. The black glaze of the ceramic raw material disclosed by the invention is bright and black in glaze color, has no pinholes, shrinkage and flowing glaze on the glaze surface, and is strong in color sense and good in overall artistic effect. The black glaze of the ceramic raw material has high blackness, pure color and stable performance, the black glaze of a 1-1.4 mm thin glaze layer has whiteness of less than 2.7 percent, glossiness of more than 10.2 percent and thermal shock resistance: quenching at 200-20 deg.c for 3 times to avoid cracking, and the whiteness below 2 and the glossiness above 20 may be obtained.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a photograph of a dark ceramic tire with black glaze according to examples 1-5 of the present invention; examples 1 to 5 are examples 1 to 5, respectively.
FIG. 3 is a photograph of a light-colored porcelain body with black glaze according to examples 1-5 of the present invention; examples 1 to 5 are examples 1 to 5, respectively.
Fig. 4 is a photograph of a black glazed cup prepared in example 5 of the present invention.
FIG. 5 is a photograph of a black glaze of comparative example 1 of the present invention on a dark green ceramic, and b on a light green ceramic.
FIG. 6 is a graph showing the sintering temperature of the black glaze according to the present invention.
Detailed Description
In order to achieve the first object of the present invention, the method for preparing the ceramic green black glaze comprises:
A. preparing glaze slip: mixing the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite, calcium oxide, chromium oxide and cobalt carbonate according to the weight ratio: 15-25:10-14:16-20:22-32:5-8:5-10:5-8:2-3:2-3, adding water for ball milling, and passing through a 250-target standard sieve after ball milling to obtain glaze slip; wherein the screen residue after passing through a 250-mesh standard screen is less than 0.5%;
B. and (3) staling: sealing the glaze slip, and standing for 24 hours at a shade and dry place;
C. glazing: firstly, uniformly stirring the aged glaze slurry, detecting and controlling the viscosity of the glaze slurry to be 10-13 mPa.s, and then uniformly attaching the glaze slurry to the surface of a clean biscuit firing ceramic body;
D. and (3) drying: drying the glazed ceramic body;
E. firing: starting the ceramic body dried in the step D to reach 300-400 ℃ from room temperature at a heating speed of 2-3 ℃/min; then the temperature rising speed of 4-5 ℃/min reaches 750-800 ℃, and the temperature is kept for 30-60 min; then the temperature rising speed of 3-4 ℃/min reaches 1250-1280 ℃, and the temperature is kept for 15-30 min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze product.
In a specific embodiment, the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite ore, calcium oxide, chromium oxide and cobalt carbonate are mixed according to the weight ratio: 20-25:12-14:16-20:27-32:5-8:5.7-10:5-8:2-3:2-3;
the total mass of the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite, calcium oxide, chromium oxide and cobalt carbonate is M, and the mass ratio of M to ball to water is preferably 1:1.5-2:1 during ball milling;
in one embodiment, the ball milling time is 5 to 10 minutes.
In one embodiment, sodium humate 0.5-1%M and sodium tripolyphosphate 0.2-0.5% M are added before ball milling in step A.
In a specific embodiment, the clean biscuit firing ceramic body is further subjected to pretreatment before glazing, wherein the pretreatment is to wipe dust on the surface of the biscuit firing ceramic body with wetted sponge, supplement water, and glazing after the surface of the ceramic body is air-dried with moisture. In the process of wiping ash by using the wet sponge, the wet sponge is used for properly supplementing water to the green body, so that the green body is too thick in glaze absorption during glaze soaking and the possibility of glaze flowing during sintering can be caused by no water supplementing.
In one embodiment, the glaze slip is uniformly adhered to the surface of the clean biscuit firing ceramic body by a method of dipping glaze.
In one embodiment, the method of glazing comprises: immersing the ceramic blank in the glaze for 1-2 s, and immersing the glaze for multiple times to keep the thickness of the glaze layer between 1 and 1.4 mm.
In one specific embodiment, the drying in the step D is drying at 100-120 ℃ for 30-60 min or natural air drying.
A second object of the invention is to provide a new ceramic green black glaze.
In order to achieve the second purpose of the invention, the ceramic raw material black glaze is prepared by adopting the preparation method of the ceramic raw material black glaze.
In a specific embodiment, the ceramic raw black glaze is a black glaze of a 1-1.4 mm thin glaze layer, and the whiteness is less than 2%.
In a specific embodiment, the ceramic green black glaze has a gloss level of 20% or more, preferably thermal shock resistance: quenching at 200-20 deg.c for 3 times without cracking. The quenching is to directly put a hot piece at 200 ℃ into cold water at 20 ℃.
The following describes the invention in more detail with reference to examples, which are not intended to limit the invention thereto.
Example 1
1. Weighing the following materials in percentage by mass: 20% of Panzhihua local red mud, 12% of Panzhihua local kaolin, 5.7% of Panzhihua local hematite, 22% of potassium feldspar, 20% of quartz, 6% of talcum, 5.6% of calcium oxide, 2.27% of chromium oxide and 2.62% of cobalt carbonate;
2. adding sodium humate and sodium tripolyphosphate which are 1% of the total mass fraction of the raw materials and 0.3% of the total mass fraction of the raw materials into the raw materials in the step 1;
3. adding water into the raw materials in the step 2, placing the raw materials in a rapid ball mill, controlling the ratio of the raw materials to the ball to the water=1:2:1, and performing rapid ball milling for 6min;
4. the glaze slip in the step 3 is screened by a 250-target standard sieve, and the screen residue is 0.5 percent smaller;
5. the glaze slurry obtained in the step 4 is filled in a glaze cup, sealed by a preservative film and placed in a dry and cool place for standing for 24 hours for aging;
6. uniformly stirring the glaze slip in the step 5, testing the viscosity of the glaze slip by using a viscometer, adjusting the viscosity of the glaze slip by using water, and controlling the viscosity of the glaze slip to be 10 mPa.s;
7. glazing by adopting a glaze dipping mode, firstly wiping dust on the surface of a biscuit firing ceramic body by using a wetted sponge, and properly supplementing water, glazing after the surface of the ceramic body is air-dried, and dipping the ceramic body into the glaze for 1-2 s each time, wherein the thickness of the glaze layer is kept at 1mm;
8. placing the glazed ceramic blank into a drying box and drying for 30min at 100 ℃;
9. the sample obtained in the step 8 is put into an electric kiln to be fired, and the temperature rising speed is 2 ℃/min from the room temperature to 400 ℃; then the temperature rising speed of 5 ℃/min reaches 750 ℃, and the temperature is kept for 30min; then the temperature rise rate reaches 1250 ℃ at 4 ℃/min, and the temperature is kept for 30min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The black glaze ceramic prepared by the embodiment has whiteness: 2.5%; gloss level: 10.7%; thermal shock resistance: the 200 ℃ hot piece is directly placed into cold water with the temperature of 20 ℃ for quenching for 3 times without cracking.
Example 2
1. Weighing the following materials in percentage by mass: 15% of Panzhihua local red mud, 10% of Panzhihua local kaolin, 6.5% of Panzhihua local hematite, 22% of potassium feldspar, 16% of quartz, 6% of talcum, 5.6% of calcium oxide, 2.27% of chromium oxide and 2.62% of cobalt carbonate;
2. adding sodium humate and sodium tripolyphosphate which are 1% of the total mass fraction of the raw materials and 0.3% of the total mass fraction of the raw materials into the raw materials in the step 1;
3. adding water into the raw materials in the step 2, placing the raw materials in a rapid ball mill, controlling the ratio of the raw materials to the ball to the water=1:2:1, and performing rapid ball milling for 6min;
4. the glaze slip in the step 3 is screened by a 250-target standard sieve, and the screen residue is 0.5 percent smaller;
5. the glaze slurry obtained in the step 4 is filled in a glaze cup, sealed by a preservative film and placed in a dry and cool place for standing for 24 hours for aging;
6. uniformly stirring the glaze slip in the step 5, testing the viscosity of the glaze slip by using a viscometer, adjusting the viscosity of the glaze slip by using water, and controlling the viscosity of the glaze slip to be 13 mPa.s;
7. glazing by adopting a glaze dipping mode, firstly wiping dust on the surface of a biscuit firing ceramic body by using wetted sponge, and properly supplementing water, glazing after the surface of the ceramic body is air-dried, dipping the ceramic body into the glaze for 1-2 s each time, and dipping the glaze for 1 time to ensure that the thickness of the glaze layer is kept at about 1mm;
8. placing the glazed ceramic blank into a drying box and drying for 30min at 100 ℃;
9. the sample obtained in the step 8 is put into an electric kiln to be fired, and the temperature rising speed is 2 ℃/min from the room temperature to 300 ℃; then the temperature rising speed of 5 ℃/min reaches 750 ℃, and the temperature is kept for 30min; then heating to 1280 ℃ at a heating rate of 4 ℃/min, and preserving heat for 30min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The black glaze ceramic prepared by the embodiment has whiteness: 2.1%; gloss level: 10.2%; thermal shock resistance: the 200 ℃ hot piece is directly placed into cold water with the temperature of 20 ℃ for quenching for 3 times without cracking.
Example 3
1. Weighing the following materials in percentage by mass: 20% of Panzhihua local red mud, 10% of Panzhihua local kaolin, 5.7% of Panzhihua local hematite, 32% of potassium feldspar, 18% of quartz, 6% of talcum, 5.6% of calcium oxide, 2.27% of chromium oxide and 2.62% of cobalt carbonate;
2. adding sodium humate and sodium tripolyphosphate which are 1% of the total mass fraction of the raw materials and 0.3% of the total mass fraction of the raw materials into the raw materials in the step 1;
3. adding water into the raw materials in the step 2, placing the raw materials in a rapid ball mill, controlling the ratio of the raw materials to the ball to the water=1:2:1, and performing rapid ball milling for 6min;
4. the glaze slip in the step 3 is screened by a 250-target standard sieve, and the screen residue is 0.5 percent smaller;
5. the glaze slurry obtained in the step 4 is filled in a glaze cup, sealed by a preservative film and placed in a dry and cool place for standing for 24 hours for aging;
6. uniformly stirring the glaze slip in the step 5, testing the viscosity of the glaze slip by using a viscometer, adjusting the viscosity of the glaze slip by using water, and controlling the viscosity of the glaze slip to be 10 mPa.s;
7. glazing by adopting a glaze dipping mode, firstly wiping dust on the surface of a biscuit firing ceramic body by using wetted sponge, and properly supplementing water, glazing after the surface of the ceramic body is air-dried, dipping the ceramic body into the glaze for 1-2 s each time, and dipping the glaze for 2 times to ensure that the thickness of the glaze layer is kept to be about 1.3 mm;
8. naturally air-drying the glazed ceramic blank;
9. the sample obtained in the step 8 is put into an electric kiln to be fired, and the temperature rising speed is 2 ℃/min from the room temperature to 400 ℃; then the temperature rising speed of 5 ℃/min reaches 750 ℃, and the temperature is kept for 30min; then the temperature rise rate reaches 1250 ℃ at 4 ℃/min, and the temperature is kept for 30min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The black glaze ceramic prepared by the embodiment has whiteness: 2.7%; gloss level: 15.5%; thermal shock resistance: the 200 ℃ hot piece is directly placed into cold water with the temperature of 20 ℃ for quenching for 3 times without cracking.
Example 4
1. Weighing the following materials in percentage by mass: 20% of Panzhihua local red mud, 14% of Panzhihua local kaolin, 5.7% of Panzhihua local hematite, 32% of potassium feldspar, 16% of quartz, 6% of talcum, 5.6% of calcium oxide, 2.27% of chromium oxide and 2.62% of cobalt carbonate;
2. adding sodium humate and sodium tripolyphosphate which are 1% of the total mass fraction of the raw materials and 0.3% of the total mass fraction of the raw materials into the raw materials in the step 1;
3. adding water into the raw materials in the step 2, placing the raw materials in a rapid ball mill, controlling the ratio of the raw materials to the ball to the water=1:2:1, and performing rapid ball milling for 6min;
4. the glaze slip in the step 3 is screened by a 250-target standard sieve, and the screen residue is less than 0.5%;
5. the glaze slurry obtained in the step 4 is filled in a glaze cup, sealed by a preservative film and placed in a dry and cool place for standing for 24 hours for aging;
6. uniformly stirring the glaze slip in the step 5, testing the viscosity of the glaze slip by using a viscometer, adjusting the viscosity of the glaze slip by using water, and controlling the viscosity of the glaze slip to be 13 mPa.s;
7. glazing by adopting a glaze dipping mode, firstly wiping dust on the surface of a biscuit firing ceramic body by using wetted sponge, and properly supplementing water, glazing after the surface of the ceramic body is air-dried, dipping the ceramic body into the glaze for 1-2 s each time, and dipping the glaze for 2 times to ensure that the thickness of the glaze layer is kept to be about 1.4 mm;
8. placing the glazed ceramic blank into a drying box and drying for 30min at 120 ℃;
9. the sample obtained in the step 8 is put into an electric kiln to be fired, and the temperature rising speed is 2 ℃/min from the room temperature to 300 ℃; then the temperature rising speed of 5 ℃/min reaches 750 ℃, and the temperature is kept for 30min; then heating to 1280 ℃ at a heating rate of 4 ℃/min, and preserving heat for 15min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The black glaze ceramic prepared by the embodiment has whiteness: 1.7%; gloss level: 20.5%; thermal shock resistance: the 200 ℃ hot piece is directly placed into cold water with the temperature of 20 ℃ for quenching for 3 times without cracking.
Example 5
1. Weighing the following materials in percentage by mass: 20% of Panzhihua local red mud, 12% of Panzhihua local kaolin, 5.7% of Panzhihua local hematite, 27% of potassium feldspar, 18% of quartz, 6% of talcum, 5.6% of calcium oxide, 2.27% of chromium oxide and 2.62% of cobalt carbonate;
2. adding sodium humate and sodium tripolyphosphate which are 1% of the total mass fraction of the raw materials and 0.3% of the total mass fraction of the raw materials into the raw materials in the step 1;
3. adding water into the raw materials in the step 2, placing the raw materials in a rapid ball mill, controlling the ratio of the raw materials to the ball to the water=1:2:1, and performing rapid ball milling for 6min;
4. the glaze slip in the step 3 is screened by a 250-target standard sieve, and the screen residue is less than 0.5%;
5. the glaze slurry obtained in the step 4 is filled in a glaze cup, sealed by a preservative film and placed in a dry and cool place for standing for 24 hours for aging;
6. uniformly stirring the glaze slip in the step 5, testing the viscosity of the glaze slip by using a viscometer, adjusting the viscosity of the glaze slip by using water, and controlling the viscosity of the glaze slip to be 13 mPa.s;
7. glazing by adopting a glaze dipping mode, firstly wiping dust on the surface of a biscuit firing ceramic body by using wet sponge, and properly supplementing water, glazing after the surface of the ceramic body is air-dried, dipping the ceramic body into the glaze for 1-2 s each time, and dipping the glaze for 2 times to ensure that the thickness of the glaze layer is kept to be about 1.4 mm;
8. placing the glazed ceramic blank into a drying box and drying for 30min at 100 ℃;
9. the sample obtained in the step 8 is put into an electric kiln to be fired, and the temperature rising speed is 2 ℃/min from the room temperature to 400 ℃; then the temperature rising speed of 5 ℃/min reaches 750 ℃, and the temperature is kept for 30min; then the temperature rise rate reaches 1250 ℃ at 4 ℃/min, and the temperature is kept for 30min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The black glaze ceramic prepared by the embodiment has whiteness: 1.5%; gloss level: 21.2%; thermal shock resistance: the 200 ℃ hot piece is directly placed into cold water with the temperature of 20 ℃ for quenching for 3 times without cracking.
Comparative example 1
1. Weighing the following materials in percentage by mass: 28% of Panzhihua local red mud, 14% of Panzhihua local kaolin, 4% of Panzhihua local hematite, 22% of potassium feldspar, 18% of quartz, 6% of talcum, 5% of calcium oxide, 2.27% of chromium oxide and 2.62% of cobalt carbonate;
2. adding sodium humate and sodium tripolyphosphate which are 0.5% of the total mass fraction of the raw materials into the raw materials in the step 1;
3. adding water into the raw materials in the step 2, placing the raw materials in a rapid ball mill, controlling the ratio of the raw materials to the ball to the water=1:2:1, and performing rapid ball milling for 6min;
4. the glaze slip in the step 3 is screened by a 250-target standard sieve, and the screen residue is 0.5 percent smaller;
5. the glaze slurry obtained in the step 4 is filled in a glaze cup, sealed by a preservative film and placed in a dry and cool place for standing for 24 hours for aging;
6. uniformly stirring the glaze slip in the step 5, testing the viscosity of the glaze slip by using a viscometer, adjusting the viscosity of the glaze slip by using water, and controlling the viscosity of the glaze slip to be 13 mPa.s;
7. glazing by adopting a glaze dipping mode, firstly wiping dust on the surface of a biscuit firing ceramic body by using wetted sponge, and properly supplementing water, glazing after the surface of the ceramic body is air-dried, dipping the ceramic body into the glaze for 1-2 s each time, and dipping the glaze for 2 times to ensure that the thickness of the glaze layer is kept to be about 1.4 mm;
8. placing the glazed ceramic blank into a drying box and drying at 100 ℃ for 60min;
9. the sample obtained in the step 8 is put into an electric kiln to be fired, and the temperature rising speed is 2 ℃/min from the room temperature to 300 ℃; then the temperature rising speed of 5 ℃/min reaches 750 ℃, and the temperature is kept for 30min; then heating to 1280 ℃ at a heating rate of 4 ℃/min, and preserving heat for 15min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The black glaze ceramic prepared in the comparative example has whiteness: 7.5%; gloss level: 10.8%; thermal shock resistance: the 200 ℃ hot piece is directly placed into cold water with the temperature of 20 ℃ for quenching for 3 times without cracking.
Claims (10)
1. The preparation method of the ceramic raw black glaze is characterized by comprising the following steps:
A. preparing glaze slip: mixing the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite, calcium oxide, chromium oxide and cobalt carbonate according to the weight ratio: adding water into the mixture of 15-25:10-14:16-20:22-32:5-8:5-10:5-8:2-3:2-3 for ball milling, and passing through a 250-target standard sieve after ball milling to obtain glaze slip; wherein the screen residue after passing through a 250-mesh standard screen is less than 0.5%;
B. and (3) staling: sealing the glaze slip, and standing for more than 24 hours at a shade and dry place;
C. glazing: firstly, uniformly stirring the aged glaze slurry, detecting and adding water to adjust the viscosity of the glaze slurry to 10-13 mPa.s, and then uniformly attaching the glaze slurry to the surface of a clean biscuit firing ceramic body;
D. and (3) drying: drying the glazed ceramic body;
E. firing: starting the ceramic body dried in the step D to reach 300-400 ℃ from room temperature at a heating speed of 2-3 ℃/min; then the temperature rising speed of 4-5 ℃/min reaches 750-800 ℃, and the temperature is kept for 30-60 min; then the temperature rising speed of 3-4 ℃/min reaches 1250-1280 ℃, and the temperature is kept for 15-30 min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze product.
2. The method for preparing the black glaze of ceramic raw materials according to claim 1, wherein the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite ore, calcium oxide, chromium oxide and cobalt carbonate are prepared by the following weight ratio: 20-25:12-14:16-20:27-32:5-8:5.7-10:5-8:2-3:2-3;
the total mass of the Panzhihua local red mud, panzhihua local kaolin, quartz, potassium feldspar, talcum, hematite, calcium oxide, chromium oxide and cobalt carbonate is M, and the mass ratio of M to ball to water is 1:1.5-2:1 during ball milling;
the ball milling time is 5-10 min.
3. The method for preparing a ceramic raw black glaze according to claim 2, wherein sodium humate of 0.5-1%M and sodium tripolyphosphate of 0.2-0.5% m are added before ball milling in step a.
4. The method for preparing a ceramic green black glaze according to claim 1 or 2, wherein the clean biscuit firing ceramic body is further subjected to pretreatment before glazing, the pretreatment is to wipe dust on the surface of the biscuit firing ceramic body with a wet sponge, and to replenish water, and glazing is performed after the surface of the ceramic body is air-dried with moisture.
5. The method for preparing the ceramic green black glaze according to claim 1 or 2, wherein the glaze slurry is uniformly adhered to the surface of a clean biscuit firing ceramic body by glaze dipping.
6. The method for preparing a ceramic green black glaze according to claim 5, wherein the method for impregnating the glaze comprises: immersing the ceramic blank in the glaze for 1-2 s, and immersing the glaze for multiple times to keep the thickness of the glaze layer between 1 and 1.4 mm.
7. The method for preparing a ceramic green black glaze according to claim 1 or 2, wherein the drying in step D is drying at 100-120 ℃ for 30-60 min or natural air drying.
8. A ceramic green black glaze characterized in that the ceramic green black glaze is prepared by the preparation method of the ceramic green black glaze according to any one of claims 1 to 7.
9. The ceramic green black glaze according to claim 8, wherein the ceramic green black glaze is a black glaze of a 1-1.4 mm thin glaze layer, the whiteness being less than 2%.
10. The ceramic green black glaze according to claim 8 or 9, wherein the ceramic green black glaze has a gloss of 20% or more, thermal shock resistance: quenching at 200-20 deg.c for 3 times without cracking.
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