CN112441845B - Preparation method of low-color-difference ceramic - Google Patents
Preparation method of low-color-difference ceramic Download PDFInfo
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- CN112441845B CN112441845B CN202011483688.5A CN202011483688A CN112441845B CN 112441845 B CN112441845 B CN 112441845B CN 202011483688 A CN202011483688 A CN 202011483688A CN 112441845 B CN112441845 B CN 112441845B
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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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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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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
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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Abstract
The invention relates to the field of ceramic tile production, and provides a preparation method of a low-color-difference ceramic, which is used for solving the problem of large color difference of ceramic tiles. The preparation method of the low-color-difference ceramic provided by the invention comprises the following steps: applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 45-55% of modified graphene, 4.5-5.5% of amine chloride and 39.5-50.5% of water; applying base coat on the first blank, firing at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 25-40% of quartz stone, 20-45% of potassium feldspar, 3-10% of kaolin, 1-5% of borax, 2-5% of zinc oxide, 2-5% of zirconium silicate, 1-5% of calcium carbonate, 2-5% of magnesium carbonate, 2-5% of strontium carbonate, 1-3% of phosphorus pentoxide, 1-3% of lithium carbonate and 0.5-2% of modified graphene; and applying transparent glaze on the intermediate, sintering at 1150-1200 ℃, soft polishing and edging to obtain the low-color-difference ceramic. The color difference can be effectively reduced, the glaze surface is uniform and flat, the color of the glaze surface is uniform, and the firing process is simple.
Description
Technical Field
The invention relates to the field of ceramic tile production, in particular to a preparation method of low-color-difference ceramic.
Background
Ceramic tiles are plate-like or block-like ceramic products produced from clay and other inorganic non-metallic materials by forming, sintering and other processes, and are used for decorating and protecting walls and floors of buildings and structures. Usually, the molding is carried out at room temperature by dry pressing, extrusion or other molding methods, followed by drying and firing at a certain temperature.
The ceramic glaze is in a glass rheological state at high temperature, moves downwards along the surface of a product under the action of gravity, and the coloring pigment is mixed in the glaze and moves along with the glaze layer, so that the color of the part with the thick glaze layer is dark, the color of the part with the thin glaze layer is light, the integral color of the product is uneven, and the color difference is more obvious.
How to reduce the color difference of the ceramic is a technical problem to be solved urgently.
Disclosure of Invention
The invention solves the technical problem of large color difference of ceramic tiles and provides a preparation method of low-color-difference ceramic.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 45-55% of modified graphene, 4.5-5.5% of amine chloride and 39.5-50.5% of water;
applying base coat on the first blank, sintering at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 25-40% of quartz, 20-45% of potassium feldspar, 3-10% of kaolin, 1-5% of borax, 2-5% of zinc oxide, 2-5% of zirconium silicate, 1-5% of calcium carbonate, 2-5% of magnesium carbonate, 2-5% of strontium carbonate, 1-3% of phosphorus pentoxide, 1-3% of lithium carbonate and 0.5-2% of modified graphene;
and (3) applying transparent glaze on the intermediate, sintering at 1150-1200 ℃, performing soft polishing and edging to obtain the low-color-difference ceramic.
The modified graphene is used for coloring the glaze, so that sufficient color development can be ensured, the color is uniform, the color glaze similar to the standard carbon black on the same color card can be formed, and the color glaze is covered with the transparent glaze, so that the color durability can be further improved.
The color difference can be effectively reduced, the glaze surface is uniform and flat, the color of the glaze surface is uniform, and the firing process is simple.
Preferably, the mass ratio of the coloring agent to the ground coat is 0.01-0.02: 1.
Preferably, the ground glaze includes: 35-40% of quartz, 35-45% of potassium feldspar, 5-10% of kaolin, 3-5% of borax, 3-5% of zinc oxide, 4-5% of zirconium silicate, 3-5% of calcium carbonate, 4-5% of magnesium carbonate, 3-5% of strontium carbonate, 2-3% of phosphorus pentoxide, 2-3% of lithium carbonate and 1-2% of modified graphene.
Preferably, the ground glaze includes: 35% of quartz, 35% of potassium feldspar, 5% of kaolin, 3% of borax, 3% of zinc oxide, 4% of zirconium silicate, 3% of calcium carbonate, 4% of magnesium carbonate, 3% of strontium carbonate, 2% of phosphorus pentoxide, 2% of lithium carbonate and 1% of modified graphene.
Preferably, the transparent glaze comprises: 15-20% of potassium feldspar, 30-35% of hectorite, 10-20% of quartz powder, 14-20% of kaolin, 14-16% of black clay, 3-7% of pyrophyllite powder, 3-7% of porcelain powder and 1-3% of potassium titanate whisker. The quality of the transparent glaze can influence the color difference of the ceramic, the potassium titanate whisker is added, the mechanical property of the ceramic tile can be improved, and the quality of the transparent glaze can be adjusted without influencing the color difference of the ceramic.
Preferably, the transparent glaze comprises: 18-20% of potassium feldspar, 30-35% of hectorite, 11-20% of quartz powder, 16-20% of kaolin, 15-16% of black clay, 4-7% of pyrophyllite powder, 4-7% of porcelain powder and 2-3% of potassium titanate whisker.
Preferably, the transparent glaze comprises: 18% of potassium feldspar, 30% of hectorite, 11% of quartz powder, 16% of kaolin, 15% of black clay, 4% of pyrophyllite powder, 4% of ceramic powder and 2% of potassium titanate whisker.
Preferably, the preparation method of the modified graphene comprises the following steps:
the preparation method of the ferroferric oxide modified graphene comprises the following steps:
ultrasonically dispersing graphite oxide in a 10% ethanol aqueous solution, wherein the mass ratio of the graphite oxide to the 10% ethanol aqueous solution is 0.001-0.005: 1, so as to obtain a dispersion liquid;
respectively stirring and dissolving ferric chloride and ferrous chloride in ethanol, wherein the mass ratio of the ferric chloride to the ferrous chloride is 1: 0.7-0.8, and the mass ratio of the ferric chloride to the ethanol is 1: 40-50, so as to obtain an iron salt solution;
and mixing and stirring an iron salt solution and the dispersion liquid, wherein the mass ratio of ferric chloride to graphite oxide is 15-25: 1, heating to 50-90 ℃, adding ammonia water to adjust the pH value to 9-11, reacting for 2-5 h, separating a product, washing and drying to obtain the modified graphene. The ferroferric oxide modified graphene is adopted to obtain a colorant with high quality, and a uniform black glaze surface can be formed without a complex firing process.
Preferably, the preparation method of the potassium titanate whisker comprises the following steps:
taking 55-65% of stearic acid, 10-20% of ethyl titanate and 20-30% of 20% potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing and cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
Preferably, 60% stearic acid, 15% ethyl titanate and 25% potassium nitrate solution with a concentration of 20% are taken.
Compared with the prior art, the invention has the beneficial effects that: the color difference can be effectively reduced, the glaze surface is uniform and flat, the color of the glaze surface is uniform, and the firing process is simple.
The transparent glaze is used for protecting the ground glaze, so that the chromatic aberration is not excessively influenced, and the color can be kept lasting.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Example 1
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 7.5g of modified graphene, 0.75g of amine chloride and 6g of water;
applying base coat on the first blank, firing at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide, 20g of lithium carbonate and 10g of modified graphene;
applying transparent glaze on the intermediate, sintering at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potassium feldspar, 300g of lithium porcelain stone, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The preparation method of the modified graphene comprises the following steps:
the preparation method of the ferroferric oxide modified graphene comprises the following steps:
ultrasonically dispersing 1.5g of graphite oxide in 300g of 10% ethanol aqueous solution, wherein the mass ratio of the graphite oxide to the 10% ethanol aqueous solution is 0.001-0.005: 1, so as to obtain a dispersion liquid;
respectively stirring and dissolving 32g of ferric chloride and 24g of ferrous chloride in 1500g of ethanol to obtain an iron salt solution;
and mixing and stirring the iron salt solution and the dispersion liquid, heating to 50-90 ℃, adding ammonia water to adjust the pH value to 9-11, reacting for 2-5 hours, separating a product, washing and drying to obtain the modified graphene.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of a 20% potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid at a speed of 40 drops/min, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing and cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker
The modified graphene is used for coloring the glaze, so that sufficient color development can be ensured, the color is uniform, the color glaze similar to the standard carbon black on the same color card can be formed, and the color glaze is covered with the transparent glaze, so that the color durability can be further improved. The color difference can be effectively reduced, the glaze surface is uniform and flat, the color of the glaze surface is uniform, and the firing process is simple. The quality of the transparent glaze can influence the color difference of the ceramic, the potassium titanate whisker is added, the mechanical property of the ceramic tile can be improved, and the quality of the transparent glaze can be adjusted without influencing the color difference of the ceramic. The ferroferric oxide modified graphene is adopted to obtain a colorant with high quality, and a uniform black glaze surface can be formed without a complex firing process.
Example 2
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 7.5g of modified graphene, 0.75g of amine chloride and 6g of water;
applying base coat on the first blank, sintering at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide, 20g of lithium carbonate and 10g of modified graphene;
applying transparent glaze on the intermediate, firing at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potassium feldspar, 300g of lithium porcelain stone, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The modified graphene is chromium-modified graphene.
The preparation method of the chromium modified graphene comprises the following steps:
dissolving chromium nitrate in absolute ethyl alcohol to prepare a solution with the concentration of 10mg/mL, dripping a saturated ethanol solution of urea under the stirring condition, heating while stirring, controlling the temperature of the solution at 60 ℃, continuously generating green precipitate in the solution, stopping dripping when the pH value reaches 7, completely precipitating, carrying out vacuum filtration and separation on the precipitate, and drying at 60 ℃ to obtain a chromium nitrate urea complex;
weighing 12g of natural graphite, putting the natural graphite into N-methyl-2-pyrrolidone, carrying out ultrasonic dispersion for stripping treatment for 3 hours under the conditions of ultrasonic frequency of 20kHz and ultrasonic power of 1800W, then carrying out ultrasonic dispersion for 1 hour under the conditions of ultrasonic frequency of 40kHz and ultrasonic power of 150W, then centrifuging for 0.5 hour at the rotating speed of 600r/min, removing black dispersion liquid on the upper layer of the centrifugal liquid, and then preparing graphene suspension liquid with the concentration of 1.5 mg/mL;
weighing 8g of water of the chromium nitrate urea complex to prepare a chromium nitrate urea complex aqueous solution with the concentration of 2mol/L, adding the chromium nitrate urea complex aqueous solution into the graphene suspension liquid under the stirring condition, and continuously stirring for 5 hours to obtain a uniform dispersion liquid;
putting the obtained dispersion liquid into a hydrothermal reaction kettle, reacting for 10 hours at 180 ℃, then washing with water and alcohol, and drying at 80 ℃ to obtain graphene/Cr2O3A composite material;
mixing graphene/Cr2O3And putting the composite material into an atmosphere furnace, introducing nitrogen, heating to 900 ℃ at the flow rate of 5mL/min, preserving the heat for 5h, and then cooling to room temperature under the protection of the nitrogen to obtain the graphene/chromium nitride nanocomposite material.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of 20 percent potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid at the speed of 40 drops/min, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing, cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker
Example 3
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 7.5g of modified graphene, 0.75g of amine chloride and 6g of water;
applying base coat on the first blank, sintering at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide, 20g of lithium carbonate and 10g of modified graphene;
applying transparent glaze on the intermediate, sintering at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potassium feldspar, 300g of lithium porcelain stone, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The preparation method of the chromium modified graphene comprises the following steps:
ultrasonically dispersing 1.5g of graphite oxide in 300g of 10% ethanol aqueous solution to obtain a dispersion liquid;
dissolving 50g of chromium nitrate in 1500g of ethanol by stirring to obtain a chromium salt solution;
and mixing and stirring the chromium salt solution and the dispersion liquid, heating to 50-90 ℃, adding ammonia water to adjust the pH value to 10, reacting for 2-5 hours, separating a product, washing and drying to obtain the ferroferric oxide modified graphene.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of a 20% potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid at a speed of 40 drops/min, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing and cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
Example 4
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 7.5g of modified graphene, 0.75g of amine chloride and 6g of water;
applying base coat on the first blank, firing at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide, 20g of lithium carbonate and 10g of modified graphene;
applying transparent glaze on the intermediate, sintering at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potash feldspar, 300g of hectorite, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The preparation method of the modified graphene comprises the following steps:
the preparation method of the ferroferric oxide modified graphene comprises the following steps:
ultrasonically dispersing 1.5g of graphite oxide in 300g of 10% ethanol aqueous solution, wherein the mass ratio of the graphite oxide to the 10% ethanol aqueous solution is 0.001-0.005: 1, so as to obtain a dispersion liquid;
respectively stirring and dissolving 32g of ferric chloride and 24g of ferrous chloride in 1500g of ethanol to obtain an iron salt solution;
and mixing and stirring the iron salt solution and the dispersion liquid, heating to 50-90 ℃, adding ammonia water to adjust the pH value to 9-11, reacting for 2-5 hours, separating a product, washing and drying to obtain the modified graphene.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of 5% potassium hydroxide aqueous solution;
dropwise adding 5% of potassium hydroxide water solution into molten stearic acid, adding ethyl titanate after dropwise adding is finished, stirring for 1-2 h, standing and cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
Comparative example 1
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 7.5g of graphene, 0.75g of amine chloride and 6g of water;
applying base coat on the first blank, firing at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide, 20g of lithium carbonate and 10g of graphene;
applying transparent glaze on the intermediate, firing at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potassium feldspar, 300g of lithium porcelain stone, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of 20 percent potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid at the speed of 40 drops/min, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing, cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker
Comparative example 2
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 0.5g of graphene, 8g of ferroferric oxide, 0.75g of amine chloride and 6g of water;
applying base coat on the first blank, firing at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide, 20g of lithium carbonate, 1g of graphene and 8g of ferroferric oxide;
applying transparent glaze on the intermediate, sintering at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potassium feldspar, 300g of lithium porcelain stone, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of a 20% potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid at the speed of 40 drops/min, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing, cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker
Comparative example 3
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank;
applying base coat on the first blank, firing at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide, 20g of lithium carbonate and 17.5g of modified graphene;
applying transparent glaze on the intermediate, firing at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potassium feldspar, 300g of lithium porcelain stone, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The preparation method of the modified graphene comprises the following steps:
the preparation method of the ferroferric oxide modified graphene comprises the following steps:
ultrasonically dispersing 1.5g of graphite oxide in 300g of 10% ethanol aqueous solution, wherein the mass ratio of the graphite oxide to the 10% ethanol aqueous solution is 0.001-0.005: 1, so as to obtain a dispersion liquid;
respectively stirring and dissolving 32g of ferric chloride and 24g of ferrous chloride in 1500g of ethanol to obtain an iron salt solution;
and mixing and stirring the ferric salt solution and the dispersion liquid, heating to 50-90 ℃, adding ammonia water to adjust the pH to 9-11, reacting for 2-5 h, separating a product, washing and drying to obtain the modified graphene.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of 20 percent potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid at the speed of 40 drops/min, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing, cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker
Comparative example 4
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 7.5g of ferroferric oxide, 0.75g of amine chloride and 6g of water;
applying base coat on the first blank, sintering at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide, 20g of lithium carbonate and 10g of ferroferric oxide;
applying transparent glaze on the intermediate, firing at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potassium feldspar, 300g of lithium porcelain stone, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of a 20% potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid at the speed of 40 drops/min, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing, cooling, roasting for 2h at 550 ℃, and cooling;
ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker
Comparative example 5
The preparation method of the low-color-difference ceramic comprises the following steps:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 17.5g of modified graphene, 1.75g of amine chloride and 14g of water;
applying base coat on the first blank, sintering at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 350g of quartz stone, 350g of potassium feldspar, 50g of kaolin, 30g of borax, 30g of zinc oxide, 40g of zirconium silicate, 30g of calcium carbonate, 40g of magnesium carbonate, 30g of strontium carbonate, 20g of phosphorus pentoxide and 20g of lithium carbonate;
applying transparent glaze on the intermediate, sintering at 1150-1200 ℃, soft polishing and edging; the transparent glaze comprises: 180g of potassium feldspar, 300g of lithium porcelain stone, 110g of quartz powder, 160g of kaolin, 150g of black clay, 40g of pyrophyllite powder, 40g of ceramic powder and 20g of potassium titanate whisker to obtain the low-color-difference ceramic.
The preparation method of the modified graphene comprises the following steps:
the preparation method of the ferroferric oxide modified graphene comprises the following steps:
ultrasonically dispersing 1.5g of graphite oxide in 300g of 10% ethanol aqueous solution, wherein the mass ratio of the graphite oxide to the 10% ethanol aqueous solution is 0.001-0.005: 1, so as to obtain a dispersion liquid;
respectively stirring and dissolving 32g of ferric chloride and 24g of ferrous chloride in 1500g of ethanol to obtain an iron salt solution;
and mixing and stirring the ferric salt solution and the dispersion liquid, heating to 50-90 ℃, adding ammonia water to adjust the pH to 9-11, reacting for 2-5 h, separating a product, washing and drying to obtain the modified graphene.
The preparation method of the potassium titanate whisker comprises the following steps:
taking 3.5g of stearic acid, 1g of ethyl titanate and 1.1g of a 20% potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid at a speed of 40 drops/min, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing and cooling, roasting for 2h at 550 ℃, and cooling;
and ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
Examples of the experiments
The glaze chromaticity of the ceramic tiles in examples 1 to 4 and comparative examples 1 to 5 was measured by a WSD-3C type whiteness-color difference meter, and the measurement results are shown in the following table:
from the above table, it can be seen that the brightness value in example 1 is closest to the brightness value (5.0) of standard carbon black, the glaze quality is good, and the color formation is more uniform. In examples 2 and 3, the effect of the graphene dyeing modified by chrome black is still different from that of example 1, and the chrome black is a common black dye, but the toxicity of the chrome is gradually eliminated. The whiskers in example 4 are different from those in example 1, and columnar whiskers cannot form a uniform transparent glaze in the firing process of the present application.
In comparative example 1, only graphene is adopted, in comparative example 2, ferroferric oxide and graphene are adopted, modified graphene in comparative example 3 is not in the ground coat, in comparative example 4, ferroferric oxide is adopted, and modified graphene in comparative example 5 is completely in the colorant, and the brightness value of the modified graphene is greatly different from that of standard carbon black.
The above detailed description is specific to possible embodiments of the present invention, and the above embodiments are not intended to limit the scope of the present invention, and all equivalent implementations or modifications that do not depart from the scope of the present invention should be included in the present claims.
Claims (6)
1. The preparation method of the low-color-difference ceramic is characterized by comprising the following steps of:
applying a coloring agent on the blank, firing for 90min at 1250-1300 ℃, and cooling to obtain a first blank; the colorant comprises 45-55% of modified graphene, 4.5-5.5% of amine chloride and 39.5-50.5% of water;
applying base coat on the first blank, sintering at 1200-1250 ℃, and half-polishing to obtain an intermediate; the ground glaze comprises: 25-40% of quartz stone, 20-45% of potassium feldspar, 3-10% of kaolin, 1-5% of borax, 2-5% of zinc oxide, 2-5% of zirconium silicate, 1-5% of calcium carbonate, 2-5% of magnesium carbonate, 2-5% of strontium carbonate, 1-3% of phosphorus pentoxide, 1-3% of lithium carbonate and 0.5-2% of modified graphene;
applying transparent glaze on the intermediate, firing at 1150-1200 ℃, soft polishing and edging to obtain low-color-difference ceramic;
the ground glaze comprises: 35-40% of quartz, 35-45% of potassium feldspar, 5-10% of kaolin, 3-5% of borax, 3-5% of zinc oxide, 4-5% of zirconium silicate, 3-5% of calcium carbonate, 4-5% of magnesium carbonate, 3-5% of strontium carbonate, 2-3% of phosphorus pentoxide, 2-3% of lithium carbonate and 1-2% of modified graphene;
the transparent glaze comprises: 15-20% of potassium feldspar, 30-35% of hectorite, 10-20% of quartz powder, 14-20% of kaolin, 14-16% of black clay, 3-7% of pyrophyllite powder, 3-7% of porcelain powder and 1-3% of potassium titanate whisker;
the preparation method of the modified graphene comprises the following steps:
ultrasonically dispersing graphite oxide in a 10% ethanol aqueous solution, wherein the mass ratio of the graphite oxide to the 10% ethanol aqueous solution is 0.001-0.005: 1, so as to obtain a dispersion liquid;
respectively stirring and dissolving ferric chloride and ferrous chloride in ethanol, wherein the mass ratio of the ferric chloride to the ferrous chloride is 1: 0.7-0.8, and the mass ratio of the ferric chloride to the ethanol is 1: 40-50, so as to obtain an iron salt solution;
mixing and stirring an iron salt solution and a dispersion liquid, heating the mixture to 50-90 ℃ with the mass ratio of ferric chloride to graphite oxide being 15-25: 1, adding ammonia water to adjust the pH value to 9-11, reacting for 2-5 h, separating a product, washing and drying to obtain modified graphene;
the preparation method of the potassium titanate whisker comprises the following steps:
taking 55-65% of stearic acid, 10-20% of ethyl titanate and 20-30% of 20% potassium nitrate aqueous solution;
dripping 20% potassium nitrate into molten stearic acid, adding ethyl titanate after dripping is finished, stirring for 1-2 h, standing and cooling, roasting for 2h at 550 ℃, and cooling;
and ball-milling the cooled product for 30min, calcining at 900 ℃ for 2h, and cooling to obtain the potassium titanate whisker.
2. The method for preparing the low-color-difference ceramic according to claim 1, wherein the mass ratio of the coloring agent to the ground coat is 0.01-0.02: 1.
3. The method for preparing low color difference ceramic according to claim 1, wherein the ground coat comprises: 35% of quartz, 35% of potassium feldspar, 5% of kaolin, 3% of borax, 3% of zinc oxide, 4% of zirconium silicate, 3% of calcium carbonate, 4% of magnesium carbonate, 3% of strontium carbonate, 2% of phosphorus pentoxide, 2% of lithium carbonate and 1% of modified graphene.
4. The method for preparing a low color difference ceramic according to claim 1, wherein the transparent glaze comprises: 18-20% of potassium feldspar, 30-35% of hectorite, 11-20% of quartz powder, 16-20% of kaolin, 15-16% of black clay, 4-7% of pyrophyllite powder, 4-7% of porcelain powder and 2-3% of potassium titanate whisker.
5. The method for preparing a low-color-difference ceramic according to claim 1, wherein the transparent glaze comprises: 18% of potassium feldspar, 30% of lithium porcelain stone, 11% of quartz powder, 16% of kaolin, 15% of black clay, 4% of pyrophyllite powder, 4% of porcelain powder and 2% of potassium titanate whisker.
6. The method for preparing low color difference ceramic according to claim 1, wherein the mixture is prepared from stearic acid 60%, ethyl titanate 15%, and 25% 20% potassium nitrate aqueous solution.
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