CN115231825A - 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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- CN115231825A CN115231825A CN202210932576.6A CN202210932576A CN115231825A CN 115231825 A CN115231825 A CN 115231825A CN 202210932576 A CN202210932576 A CN 202210932576A CN 115231825 A CN115231825 A CN 115231825A
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- C—CHEMISTRY; METALLURGY
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- C03C4/02—Compositions for glass with special properties for coloured glass
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- 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
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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. and (4) firing. The method successfully adopts resources such as local kaolin, red mud and iron oxide ore of Panzhihua to prepare the black glaze, and has the characteristics of convenient material taking, low cost, no toxicity of raw ore, environmental protection, health, suitability for industrial production and the like. The black glaze raw material of the invention has good associativity of glaze slip and biscuit, is suitable for firing in oxidizing atmosphere, is suitable for common electric kilns, and has simple working procedures. The black glaze surface of the ceramic raw material disclosed by the invention has no pinholes, shrinkage glaze and flowing glaze, and is strong in color and luster feeling and good in 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 black glaze decorated ceramic ware is a traditional process method for ceramic preparation in China. The black glaze ceramic is popular with people for thousands of years due to the characteristics of modesty, simple, elegant, noble and stable glaze color. The development and improvement of black glaze has never been interrupted since ancient times. The traditional black glaze process has unstable color generation, easily generates a large number of defects of pinholes, glaze contraction and the like on the glaze surface, is difficult to master the firing process, and has low product percent of pass and higher production cost. How to simplify the process under the precondition of ensuring high blackness of the black glaze, pure color and stable performance, properly reduce the production cost and meet the requirements of green and environment-friendly production is a hotspot in the current research field.
The traditional black enamel porcelain takes the natural materials in Jiangxi province as main raw materials, the firing temperature is 1230-1320 ℃, the traditional black enamel porcelain is purely made by hand, and the traditional firewood kiln firing needs reduction firing. The traditional black glaze is generally subjected to oxidation burning and reduction burning, and if the reduction burning is not carried out, the blackness is lower and the whiteness is higher.
The black glaze firing has more influence factors, and no technology for preparing the black glaze raw material with pure color development and stable performance by using local resources of Panzhihua exists at present.
Disclosure of Invention
The first purpose of the invention is to provide a new preparation method of the green ceramic black glaze.
In order to achieve the first object of the present invention, the method for preparing the green ceramic black glaze comprises:
A. preparing glaze slip: mixing Panzhihua local red mud, panzhihua local kaolin, quartz, potash feldspar, talc, hematite, calcium oxide, chromium oxide and cobalt carbonate according to the weight ratio: 15-25; wherein the screen residue after passing through a 250-mesh standard screen is less than 0.5 percent;
B. and (3) staling: sealing the glaze slip, and standing for 24 hours in a cool and dry place;
C. glazing: stirring the aged glaze slip uniformly, detecting and controlling the viscosity of the glaze slip to be 10-13 mPa s, and then uniformly attaching the glaze slip to the surface of a clean biscuit ceramic body;
D. and (3) drying: drying the glazed ceramic blank;
E. and (3) firing: d, heating the ceramic blank dried in the step D to 300-400 ℃ from room temperature at a heating rate of 2-3 ℃/min; then the temperature is raised to 750-800 ℃ at the temperature rising speed of 4-5 ℃/min, and the temperature is kept for 30-60 min; then the temperature is raised to 1250-1280 ℃ at the temperature rising speed of 3-4 ℃/min, and the temperature is preserved for 15-30 min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze product.
In one embodiment, the Panzhihua local red mud, panzhihua local kaolin, quartz, potash feldspar, talc, hematite, calcium oxide, chromium oxide, cobalt carbonate are mixed according to the weight ratio: 20-25;
the total mass of Panzhihua local red mud, panzhihua local kaolin, quartz, potash feldspar, talc, hematite, calcium oxide, chromium oxide and cobalt carbonate is M, and the mass ratio of M to balls to water during ball milling is preferably 1: 1.5-2: 1;
the raw materials of the red mud comprise the following components in parts by weight: 20-25.
In one embodiment, the ball milling time is 5 to 10min.
In one embodiment, 0.5-1% by weight of sodium humate and 0.2-0.5% by weight of sodium tripolyphosphate are added before the ball milling in step A.
The addition of the sodium humate and the 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, and the glaze surface of the fired black glaze is smoother and is beneficial to improving the color stability of the black glaze.
In a specific embodiment, before glazing, the clean biscuit ceramic body is also subjected to pretreatment, the pretreatment is to wipe dust on the surface of the biscuit ceramic body by using a wet sponge, supplement water, and glaze after the surface of the ceramic body is dried by air. In the process of wiping ash by using the wet sponge, the wet sponge can properly replenish water to the green body, and the green body absorbs too thick glaze in glaze soaking and has the possibility of glaze flowing in sintering due to no water replenishment.
In a specific embodiment, the method for uniformly adhering the glaze slip to the surface of the clean biscuit ceramic body is glaze dipping.
In one embodiment, the method for dipping glaze comprises the following steps: and 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 1-1.4 mm.
In a specific embodiment, the drying in the step D is drying at 100-120 ℃ for 30-60 min or natural air drying.
The second purpose of the invention is to provide a new green ceramic black glaze.
In order to achieve the second object of the present invention, the green ceramic black glaze is prepared by the method for preparing the green ceramic black glaze as described above.
In a specific embodiment, the green ceramic black glaze is a 1-1.4 mm thin glaze layer black glaze, and the whiteness is less than 2%.
In one specific embodiment, the ceramic green black glaze has a gloss of 20% or more, and preferably has a thermal shock resistance: quenching for 3 times at 200-20 ℃ without cracking. The quenching is to put the hot piece at 200 ℃ into cold water at 20 ℃.
Has the advantages that:
1. the invention successfully adopts local kaolin, red mud, iron oxide ore and other resources of the Panzhihua, does not introduce any toxic raw materials containing lead, cadmium and the like in the process of preparing the black glaze, does not have the harm of dissolving out lead and cadmium, has the characteristics of convenient material obtaining, low cost, no toxicity of raw ore, environmental protection, health, suitability for industrial production and the like, and opens up a new technical line for developing and utilizing local mineral resources of the Panzhihua.
2. The black glaze raw material of the invention has good associativity of glaze slip and biscuit, is suitable for firing in oxidizing atmosphere, is suitable for common electric kilns, has simple process, wider glaze firing temperature range, high blackness of the obtained black glaze product, pure color, stable performance, low cost, simple process, environmental protection, suitability for industrialized production and the like.
3. The invention discloses a black glaze of a ceramic raw material, belonging to raw ore glaze. The color of the original ore glaze is different from that of other black glaze products, the color development is more natural, stable and elegant, the method is greatly superior to that of chemical glaze, the method is safe and reliable, the application is wider, and the method can be used for overglaze color and underglaze color and the chemical glaze can only be used for underglaze color.
4. The ceramic raw material black glaze disclosed by the invention is bright black in glaze color, free of pinholes, shrinkage glaze and flowing glaze, 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 the whiteness of less than 2.7 percent, the glossiness of more than 10.2 percent and thermal shock resistance: the glass fiber is quenched 3 times at 200-20 ℃ without cracking, and preferably the whiteness is below 2 and the glossiness is above 20.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a photograph of dark colored ceramic bodies made according to examples 1-5 of the present invention with black glaze; nos. 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 to 5 of the present invention; nos. 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 on a ceramic body of comparative example 1 of the present invention, a is a photograph on a dark colored ceramic body, and b is a photograph on a light colored ceramic body.
FIG. 6 is a graph of the sintering temperature of the black glaze of the present invention.
Detailed Description
In order to achieve the first object of the present invention, the method for preparing the green ceramic black glaze comprises:
A. preparing glaze slip: mixing Panzhihua local red mud, panzhihua local kaolin, quartz, potash feldspar, talc, hematite, calcium oxide, chromium oxide and cobalt carbonate according to the weight ratio: 15-25; wherein the screen residue after passing through a 250-mesh standard screen is less than 0.5 percent;
B. and (3) staling: sealing the glaze slip, and standing for 24 hours in a cool and dry place;
C. glazing: stirring the aged glaze slip uniformly, detecting and controlling the viscosity of the glaze slip to be 10-13 mPa.s, and then uniformly attaching the glaze slip to the surface of a clean biscuit ceramic body;
D. and (3) drying: drying the glazed ceramic blank;
E. firing: d, heating the ceramic blank dried in the step D to 300-400 ℃ from room temperature at a heating rate of 2-3 ℃/min; then the temperature is raised to 750-800 ℃ at the temperature rising speed of 4-5 ℃/min, and the temperature is kept for 30-60 min; then the temperature is raised to 1250-1280 ℃ at the heating rate of 3-4 ℃/min, and the temperature is preserved for 15-30 min; and finally stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze product.
In one embodiment, the Panzhihua native red mud, panzhihua native kaolin, quartz, potash feldspar, talc, hematite, calcium oxide, chromium oxide, cobalt carbonate are mixed according to the weight ratio: 20-25;
the total mass of Panzhihua local red mud, panzhihua local kaolin, quartz, potash feldspar, talc, hematite, calcium oxide, chromium oxide and cobalt carbonate is M, and the mass ratio of M to balls to water during ball milling is preferably 1: 1.5-2: 1;
in one embodiment, the ball milling time is 5 to 10min.
In one embodiment, 0.5-1% by weight of sodium humate and 0.2-0.5% by weight of sodium tripolyphosphate are added before the ball milling in step A.
In a specific embodiment, before glazing, the clean biscuit ceramic body is also subjected to pretreatment, the pretreatment is to wipe dust on the surface of the biscuit ceramic body by using a wet sponge, supplement water, and glaze after the surface of the ceramic body is dried by air. In the process of wiping ash by using the wet sponge, the wet sponge can properly replenish water to the green body, and the green body absorbs too thick glaze in glaze soaking and has the possibility of glaze flowing in sintering due to no water replenishment.
In a specific embodiment, the method for uniformly adhering the glaze slip to the surface of the clean biscuit ceramic body is glaze dipping.
In one embodiment, the method for dipping glaze comprises the following steps: and 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 1-1.4 mm.
In a specific embodiment, the drying in the step D is drying at 100-120 ℃ for 30-60 min or natural air drying.
The second purpose of the invention is to provide a new green ceramic black glaze.
In order to achieve the second object of the present invention, the green ceramic black glaze is prepared by the method for preparing the green ceramic black glaze as described above.
In a specific embodiment, the green ceramic black glaze is a 1-1.4 mm thin glaze layer black glaze, and the whiteness is less than 2%.
In one specific embodiment, the ceramic green black glaze has a gloss of 20% or more, and preferably has a thermal shock resistance: quenching for 3 times at 200-20 ℃ without cracking. The quenching is to put the hot piece at 200 ℃ into cold water at 20 ℃.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the invention to the embodiments described.
Example 1
1. Weighing the following materials in percentage by mass: 20% of local red mud of the Panzhihua, 12% of local kaolin of the Panzhihua, 5.7% of local hematite of the Panzhihua, 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 which is 1 percent of the total mass fraction of the raw materials and 0.3 percent of sodium tripolyphosphate into the raw materials in the step 1;
3. adding water into the raw materials in the step 2, placing the mixture in a rapid ball mill, controlling the ratio of the materials to the balls to the water to be = 1: 2: 1, and performing rapid ball milling for 6min;
4. sieving the glaze slurry obtained in the step 3 by a 250-mesh standard sieve, wherein the screen residue is less than 0.5%;
5. putting the glaze slip obtained in the step 4 into a glaze cup, sealing the glaze cup by using a preservative film, and standing the glaze cup in a dry and cool place for 24 hours for ageing;
6. uniformly stirring the glaze slurry obtained in the step 5, testing the viscosity of the glaze slurry by using a viscometer, adjusting the viscosity of the glaze slurry by using water, and controlling the viscosity of the glaze slurry to be 10mPa & s;
7. glazing by adopting a glaze dipping mode, wiping dust on the surface of the biscuit firing ceramic body by using wet sponge, properly supplementing water, glazing after the surface of the ceramic body is dried by air, dipping the ceramic body into glaze for 1-2s and dipping glaze for 2 times each time to keep the thickness of a glaze layer at 1mm;
8. putting the glazed ceramic blank into a drying oven to dry for 30min at 100 ℃;
9. putting the sample obtained in the step 8 into an electric kiln for firing, and heating to 400 ℃ from room temperature at a heating rate of 2 ℃/min; heating to 750 deg.C at a rate of 5 deg.C/min, and maintaining for 30min; then the temperature is raised to 1250 ℃ at the temperature raising speed of 4 ℃/min, and the temperature is preserved for 30min; and finally, stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The whiteness of the black glaze ceramic prepared by the embodiment is as follows: 2.5 percent; gloss: 10.7 percent; thermal shock resistance: the hot piece at 200 ℃ is directly put into cold water at 20 ℃ to be quenched for 3 times without cracking.
Example 2
1. Weighing the following materials in percentage by mass: 15% of local red mud of the Panzhihua, 10% of local kaolin of the Panzhihua, 6.5% of local hematite of the Panzhihua, 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 1 percent of sodium humate and 0.3 percent of sodium tripolyphosphate which are equivalent to 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 mixture in a rapid ball mill, controlling the ratio of the materials to the balls to the water = 1: 2: 1, and performing rapid ball milling for 6min;
4. sieving the glaze slurry obtained in the step 3 by a 250-mesh standard sieve, wherein the screen residue is less than 0.5%;
5. putting the glaze slip obtained in the step 4 into a glaze cup, sealing the glaze cup by using a preservative film, and standing the sealed glaze slip in a dry and cool place for 24 hours for ageing;
6. uniformly stirring the glaze slurry obtained in the step 5, testing the viscosity of the glaze slurry by using a viscometer, adjusting the viscosity of the glaze slurry by using water, and controlling the viscosity of the glaze slurry to be 13mPa & s;
7. glazing by adopting a glaze dipping mode, wiping dust on the surface of a biscuit firing ceramic body by using wet sponge, properly supplementing water, glazing after the surface of the ceramic body is dried by air, dipping the ceramic body into glaze for 1-2s and dipping glaze for 1 time each time to keep the thickness of a glaze layer about 1mm;
8. putting the glazed ceramic blank into a drying oven to dry for 30min at 100 ℃;
9. putting the sample obtained in the step 8 into an electric kiln for firing, and starting from room temperature, and raising the temperature to 300 ℃ at a speed of 2 ℃/min; heating to 750 deg.C at a rate of 5 deg.C/min, and maintaining for 30min; then the temperature is raised to 1280 ℃ at the temperature rise speed of 4 ℃/min, and the temperature is preserved for 30min; and finally, stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The whiteness of the black glaze ceramic prepared by the embodiment is as follows: 2.1 percent; gloss: 10.2 percent; thermal shock resistance: the hot piece at 200 ℃ is directly put into cold water at 20 ℃ to be quenched for 3 times without cracking.
Example 3
1. Weighing the following materials in percentage by mass: 20% of local red mud of the Panzhihua, 10% of local kaolin of the Panzhihua, 5.7% of local hematite of the Panzhihua, 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 1 percent of sodium humate and 0.3 percent of sodium tripolyphosphate which are equivalent to 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 mixture in a rapid ball mill, controlling the ratio of the materials to the balls to the water = 1: 2: 1, and performing rapid ball milling for 6min;
4. sieving the glaze slip obtained in the step 3 by a 250-mesh standard sieve, wherein the screen residue is 0.5 percent;
5. putting the glaze slip obtained in the step 4 into a glaze cup, sealing the glaze cup by using a preservative film, and standing the sealed glaze slip in a dry and cool place for 24 hours for ageing;
6. uniformly stirring the glaze slurry obtained in the step 5, testing the viscosity of the glaze slurry by using a viscometer, adjusting the viscosity of the glaze slurry by using water, and controlling the viscosity of the glaze slurry to be 10mPa & s;
7. glazing by adopting a glaze dipping mode, wiping dust on the surface of a biscuit firing ceramic body by using wet sponge, properly supplementing water, glazing after the surface of the ceramic body is dried by air, dipping the ceramic body into glaze for 1-2s and dipping glaze for 2 times each time to keep the thickness of a glaze layer about 1.3 mm;
8. naturally drying the glazed ceramic blank;
9. putting the sample obtained in the step 8 into an electric kiln for firing, and heating to 400 ℃ from room temperature at a heating rate of 2 ℃/min; heating to 750 deg.C at a speed of 5 deg.C/min, and maintaining for 30min; then the temperature is raised to 1250 ℃ at the temperature raising speed of 4 ℃/min, and the temperature is preserved for 30min; and finally, stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The whiteness of the black glaze ceramic prepared by the embodiment is as follows: 2.7 percent; gloss: 15.5 percent; thermal shock resistance: the hot piece at 200 ℃ is directly put into cold water at 20 ℃ to be quenched for 3 times without cracking.
Example 4
1. Weighing the following materials in percentage by mass: 20% of local red mud of the Panzhihua, 14% of local kaolin of the Panzhihua, 5.7% of local hematite of the Panzhihua, 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 which is 1 percent of the total mass fraction of the raw materials and 0.3 percent of sodium tripolyphosphate into the raw materials in the step 1;
3. adding water into the raw materials in the step 2, placing the mixture in a rapid ball mill, controlling the ratio of the materials to the balls to the water = 1: 2: 1, and performing rapid ball milling for 6min;
4. sieving the glaze slurry obtained in the step 3 by a 250-mesh standard sieve, wherein the screen residue is less than 0.5%;
5. putting the glaze slip obtained in the step 4 into a glaze cup, sealing the glaze cup by using a preservative film, and standing the sealed glaze slip in a dry and cool place for 24 hours for ageing;
6. uniformly stirring the glaze slurry obtained in the step 5, testing the viscosity of the glaze slurry by using a viscometer, adjusting the viscosity of the glaze slurry by using water, and controlling the viscosity of the glaze slurry to be 13mPa & s;
7. glazing by adopting a glaze dipping mode, wiping dust on the surface of the biscuit firing ceramic body by using wet sponge, properly supplementing water, glazing after the surface of the ceramic body is dried by air, dipping the ceramic body into glaze for 1-2s and dipping glaze for 2 times each time to keep the thickness of a glaze layer at about 1.4 mm;
8. putting the glazed ceramic blank into a drying box, and drying for 30min at 120 ℃;
9. putting the sample obtained in the step 8 into an electric kiln for firing, and starting from room temperature, and raising the temperature to 300 ℃ at a speed of 2 ℃/min; heating to 750 deg.C at a rate of 5 deg.C/min, and maintaining for 30min; then heating to 1280 ℃ at the 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 whiteness of the black glaze ceramic prepared by the embodiment is as follows: 1.7 percent; glossiness: 20.5 percent; thermal shock resistance: the hot piece at 200 ℃ is directly put into cold water at 20 ℃ to be quenched for 3 times without cracking.
Example 5
1. Weighing the following materials in percentage by mass: 20% of local red mud of the Panzhihua, 12% of local kaolin of the Panzhihua, 5.7% of local hematite of the Panzhihua, 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 1 percent of sodium humate and 0.3 percent of sodium tripolyphosphate which are equivalent to 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 mixture in a rapid ball mill, controlling the ratio of the materials to the balls to the water to be = 1: 2: 1, and performing rapid ball milling for 6min;
4. sieving the glaze slurry obtained in the step 3 by a 250-mesh standard sieve, wherein the screen residue is less than 0.5%;
5. putting the glaze slip obtained in the step 4 into a glaze cup, sealing the glaze cup by using a preservative film, and standing the sealed glaze slip in a dry and cool place for 24 hours for ageing;
6. uniformly stirring the glaze slurry obtained in the step 5, testing the viscosity of the glaze slurry by using a viscometer, adjusting the viscosity of the glaze slurry by using water, and controlling the viscosity of the glaze slurry to be 13mPa & s;
7. glazing by adopting a glaze dipping mode, wiping dust on the surface of the biscuit firing ceramic body by using wet sponge, properly supplementing water, glazing after the surface of the ceramic body is dried by air, dipping the ceramic body into glaze for 1-2s and dipping glaze for 2 times each time to keep the thickness of a glaze layer at about 1.4 mm;
8. putting the glazed ceramic blank into a drying oven to dry for 30min at 100 ℃;
9. putting the sample obtained in the step 8 into an electric kiln for burning, and heating to 400 ℃ from room temperature at a heating rate of 2 ℃/min; heating to 750 deg.C at a rate of 5 deg.C/min, and maintaining for 30min; then the temperature is raised to 1250 ℃ at the temperature raising speed of 4 ℃/min, and the temperature is preserved for 30min; and finally, stopping heating, and cooling to room temperature along with the furnace to obtain the black glaze ceramic product.
The whiteness of the black glaze ceramic prepared by the embodiment is as follows: 1.5 percent; gloss: 21.2 percent; thermal shock resistance: the hot piece at 200 ℃ is directly put into cold water at 20 ℃ to be quenched for 3 times without cracking.
Comparative example 1
1. Weighing the following materials in percentage by mass: 28% of local red mud of the Panzhihua, 14% of local kaolin of the Panzhihua, 4% of local hematite of the Panzhihua, 22% of potassium feldspar, 18% of quartz, 6% of talc, 5% of calcium oxide, 2.27% of chromium oxide and 2.62% of cobalt carbonate;
2. adding sodium humate which is 0.5 percent of the total mass fraction of the raw materials and sodium tripolyphosphate which is 0.5 percent 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 mixture in a rapid ball mill, controlling the ratio of the materials to the balls to the water = 1: 2: 1, and performing rapid ball milling for 6min;
4. sieving the glaze slip obtained in the step 3 by a 250-mesh standard sieve, wherein the screen residue is 0.5 percent;
5. putting the glaze slip obtained in the step 4 into a glaze cup, sealing the glaze cup by using a preservative film, and standing the sealed glaze slip in a dry and cool place for 24 hours for ageing;
6. uniformly stirring the glaze slurry obtained in the step 5, testing the viscosity of the glaze slurry by using a viscometer, adjusting the viscosity of the glaze slurry by using water, and controlling the viscosity of the glaze slurry to be 13mPa & s;
7. glazing by adopting a glaze dipping mode, wiping dust on the surface of the biscuit firing ceramic body by using wet sponge, properly supplementing water, glazing after the surface of the ceramic body is dried by air, dipping the ceramic body into glaze for 1-2s and dipping glaze for 2 times each time to keep the thickness of a glaze layer at about 1.4 mm;
8. putting the glazed ceramic blank into a drying oven to dry for 60min at 100 ℃;
9. putting the sample obtained in the step 8 into an electric kiln for burning, and heating to 300 ℃ from room temperature at a heating rate of 2 ℃/min; heating to 750 deg.C at a rate of 5 deg.C/min, and maintaining for 30min; then heating to 1280 ℃ at the 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 whiteness of the black glaze ceramic prepared by the comparative example is as follows: 7.5 percent; gloss: 10.8 percent; thermal shock resistance: the hot piece at 200 ℃ is directly put into cold water at 20 ℃ to be quenched for 3 times without cracking.
Claims (10)
1. The preparation method of the ceramic raw material black glaze is characterized by comprising the following steps:
A. preparing glaze slip: mixing Panzhihua local red mud, panzhihua local kaolin, quartz, potash feldspar, talc, 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, adding water for ball milling, and sieving by a 250-mesh standard sieve to obtain glaze slurry; wherein the screen residue after passing through a 250-mesh standard screen is less than 0.5 percent;
B. and (3) staling: sealing the glaze slip, and standing for more than 24 hours in a cool and dry place;
C. glazing: stirring aged glaze slip uniformly, detecting and adding water to adjust the viscosity of the glaze slip to be 10-13 mPa s, and then uniformly attaching the glaze slip to the surface of a clean biscuit ceramic body;
D. and (3) drying: drying the glazed ceramic blank;
E. firing: d, heating the ceramic blank dried in the step D to 300-400 ℃ from room temperature at a heating rate of 2-3 ℃/min; then the temperature is raised to 750-800 ℃ at the temperature rising speed of 4-5 ℃/min, and the temperature is kept for 30-60 min; then the temperature is raised to 1250-1280 ℃ at the temperature rising speed of 3-4 ℃/min, and the temperature is preserved 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 a black glaze as a raw material of ceramics according to claim 1, wherein the Panzhihua local red mud, the Panzhihua local kaolin, the quartz, the potash feldspar, the talc, the hematite, the calcium oxide, the chromium oxide and the cobalt carbonate are mixed according to the weight ratio: 20-25: 12-14: 16-20: 27-32: 5-8: 5.7-10;
the total mass of Panzhihua local red mud, panzhihua local kaolin, quartz, potash feldspar, talc, hematite, calcium oxide, chromium oxide and cobalt carbonate is M, and the mass ratio of M to balls to water during ball milling is preferably 1: 1.5-2: 1;
the time for ball milling is preferably 5 to 10min.
3. The method for preparing a black glaze as raw material for ceramic according to claim 2, wherein the percentage of sodium humate in 0.5-1% by weight and sodium tripolyphosphate in 0.2-0.5% by weight are added before the ball milling in the step A.
4. The method for preparing a black glaze as raw material of ceramics according to claim 1 or 2, wherein the clean biscuit is further subjected to a pretreatment before glazing, the pretreatment is to wipe dust on the surface of the biscuit with a wet sponge and replenish water, and glazing is carried out after the water on the surface of the biscuit is air-dried.
5. The method for preparing a green ceramic black glaze according to claim 1 or 2, wherein the method for uniformly adhering the glaze slip to the surface of the clean biscuit ceramic body is glaze dipping.
6. The method for preparing the green ceramic black glaze according to claim 5, wherein the glaze dipping method comprises the following steps: and immersing the ceramic blank body into the glaze for 1-2 s, and immersing the glaze for many times to keep the thickness of the glaze layer between 1-1.4 mm.
7. The method for preparing a black glaze as raw material for ceramic 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. The green ceramic black glaze according to any one of claims 1 to 7, which is prepared by the method for preparing the green ceramic black glaze.
9. The green ceramic black glaze according to claim 8, wherein the green ceramic black glaze is a black glaze of a 1-1.4 mm thin glaze layer, and has a whiteness of less than 2%.
10. The green ceramic black glaze according to claim 8 or 9, wherein the green ceramic black glaze has a gloss of 20% or more, preferably a thermal shock resistance: quenching for 3 times at 200-20 ℃ without cracking.
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