CN114956564B - Glaze slip, glazed ceramic and preparation method thereof - Google Patents

Glaze slip, glazed ceramic and preparation method thereof Download PDF

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Publication number
CN114956564B
CN114956564B CN202210795005.2A CN202210795005A CN114956564B CN 114956564 B CN114956564 B CN 114956564B CN 202210795005 A CN202210795005 A CN 202210795005A CN 114956564 B CN114956564 B CN 114956564B
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glaze
glazed ceramic
quick
slip
drying agent
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CN114956564A (en
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聂文志
刘东豪
李雪凤
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Shenzhen Guoci Yongfengyuan Ceramics Co ltd
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Shenzhen Guoci Yongfengyuan Ceramics Co ltd
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/86—Glazes; Cold glazes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

The invention relates to glaze slip, glazed ceramic and a preparation method thereof. The raw materials for preparing the glaze slip comprise: glaze and water, the specific gravity of the glaze slurry is 1.65 g/mL-1.68 g/mL, and the flow rate is 45s/100 mL-55 s/100mL. The glaze slip can glaze the blank body subjected to high-temperature biscuit firing in a glaze dipping mode, so that the problems of more dust, uneven glaze layer, poor adhesive force and the like existing in a glaze spraying mode are avoided, and the product qualification rate is improved.

Description

Glaze slip, glazed ceramic and preparation method thereof
Technical Field
The invention relates to the field of ceramics, in particular to glaze slip, glazed ceramics and a preparation method thereof.
Background
At present, two production methods exist for magnesia porcelain, the first method is to perform low-temperature biscuit firing at 980-1000 ℃, then to coat transparent glaze, and to perform high-temperature glaze firing at 1280-1330 ℃, wherein the high-temperature glaze firing process can be used for firing an oxidizing atmosphere or a reducing atmosphere. The second method is that the high temperature biscuit firing is carried out at 1280-1330 ℃, then a layer of low temperature transparent glaze is sprayed, the glaze firing temperature is 1100-1150 ℃ generally, and the firing atmosphere is an oxidizing atmosphere.
The process for producing the magnesia porcelain by adopting the first method is simple, but the quality of the glaze is poor, the problems of poor glossiness, more pores on the glaze, poor flatness and the like are frequently accompanied, meanwhile, the blank cannot be supported and burned by a profiling sagger, and some products deform and have poor regularity. The second method is adopted for production, because the green body is subjected to high-temperature biscuit firing, some harmful impurities, organic matters and the like are discharged, the green body is completely sintered, and the green body cannot discharge harmful matters during low-temperature glaze firing, so that the glaze is glossy, soft and smooth, the glass texture is extremely strong, and some products which are easy to deform can be fired by adopting a profiling sagger support, so that the regularity of the products is good.
When the second method is adopted for production, the blank body is subjected to high-temperature biscuit firing during glazing, and basically no water is absorbed, so that the glazing is mostly finished in a glaze spraying mode. However, the glaze spraying mode has the following problems: on one hand, glaze spraying needs to 'atomize' glaze, a large amount of dust can be generated, and the human health and the environment are greatly influenced. On the other hand, when manual or machine glaze spraying is adopted, the defects of 'glaze accumulation', 'glaze piling', 'Bao You' and the like are frequently caused, the glaze sprayed on the surface of the green body is powdery, the adhesive force is poor, the defects of 'glaze shrinkage', 'glaze lack' and the like are caused by extremely easy dropping in the transportation and blank loading processes, and the product percent of pass is not high.
Disclosure of Invention
Based on the above, it is necessary to provide a glaze slurry which can glaze a high-temperature biscuit by a glaze dipping method, so as to avoid the problems of more dust, uneven glaze layer, poor adhesive force and the like existing in a glaze spraying method and improve the product yield.
In addition, there is a need to provide a method for preparing a glaze slip, a method for preparing a glazed ceramic using the glaze slip, and the glazed ceramic prepared.
The glaze slip comprises the following raw materials for preparing the glaze slip: glaze and water, wherein the specific gravity of the glaze slip is 1.65 g/mL-1.68 g/mL, and the flow rate is 45s/100 mL-55 s/100mL.
In one embodiment, the raw materials for preparing the glaze slip also comprise a quick-drying agent, and the mass ratio of the quick-drying agent to the glaze is (2-5): 100.
In one embodiment, the quick-drying agent is prepared from the following raw materials: acrylic emulsion, gelatin, glycerin, defoamer, preservative and water.
In one embodiment, the quick-drying agent is prepared from the following raw materials in percentage by mass: 16-20% of acrylic emulsion, 10-15% of gelatin, 4-8% of glycerin, 3-6% of defoamer, 0.5-2% of preservative and 57-62% of water.
In one embodiment, the raw materials for preparing the glaze slip further comprise a suspending agent.
In one embodiment, the mass ratio of the suspending agent to the glaze is (2-5): 100.
In one embodiment, the suspending agent is selected from at least one of bentonite and kaolin.
In one embodiment, the particle size of the glaze slip is less than or equal to 44 μm.
In one embodiment, the number of the glaze slips with the grain diameter less than or equal to 2 μm in the glaze slips accounts for 10-16% of the total number of the glaze slips.
A preparation method of glaze slip comprises the following steps:
The glaze is mixed with water, the specific gravity of the mixed slurry is 1.65 g/mL-1.68 g/mL, and the flow rate is 45 s-55 s/100mL, and the glaze slip is prepared.
In one embodiment, in the step of mixing the glaze with water, a quick-drying agent is also added, wherein the mass ratio of the quick-drying agent to the glaze is (2-5): 100.
In one embodiment, in the step of mixing the glaze, the quick-drying agent and water, a suspending agent is further added, wherein the mass ratio of the suspending agent to the glaze is (2-5): 100.
In one embodiment, the glaze, the quick-drying agent and the suspending agent are mixed with water by ball milling.
In one embodiment, in the ball milling process, the mass ratio of the total mass of the glaze, the quick-drying agent and the suspending agent to the mass of the ball milling medium and the mass of water are 1:2 (0.35-0.5); and/or the number of the groups of groups,
The step of mixing the glaze, the quick-drying agent, the bentonite and water comprises the following steps: ball milling is carried out on the glaze, part of the quick-drying agent, the suspending agent and water for 20-25 h, and then the rest of the quick-drying agent is added for continuous ball milling for 30 min.
A preparation method of glazed ceramic comprises the following steps:
providing a biscuit firing blank, wherein the water absorption rate of the biscuit firing blank is less than or equal to 0.5%;
and immersing the biscuit firing blank body in glaze slurry to form a glaze layer on the biscuit firing blank body, and then performing glaze firing to prepare glazed ceramic, wherein the glaze slurry is the glaze slurry or the glaze slurry prepared by the preparation method of the glaze slurry.
In one embodiment, the thickness of the glaze layer is 0.1 mm-0.2 mm.
In one embodiment, the biscuit firing blank is immersed in the glaze slip for a period of 3s to 5s.
In one embodiment, the temperature of the glaze firing is 1100-1150 ℃, and the time of the glaze firing is 10-12 h.
In one embodiment, the biscuit firing blank is a blank subjected to high-temperature biscuit firing, wherein the temperature of the high-temperature biscuit firing is 1280-1330 ℃, and the time of the high-temperature biscuit firing is 15-18 h.
In one embodiment, the bisque firing blank is a magnesia porcelain bisque firing blank.
The glazed ceramic is prepared by the preparation method of the glazed ceramic.
In one embodiment, the glazed ceramic is a cup or pot ceramic article.
The specific gravity and the flow rate of the glaze slurry are adjusted to be proper values, so that the glaze slurry can be glazed on the surface of a blank body subjected to high-temperature biscuit firing in a glaze dipping mode, the glaze slurry is adhered to the surface of the biscuit with low water absorption rate by using the consistency and the viscosity of the glaze slurry, the obtained glaze layer is more uniform, the adhesion is strong, and the defects of 'glaze accumulation', 'glaze shrinkage', and the like are avoided. Therefore, the glaze slip can glaze the blank body subjected to high-temperature biscuit firing in a glaze dipping mode, so that the problems of more dust, uneven glaze layer, poor adhesive force and the like existing in a glaze spraying mode are avoided, and the product qualification rate is improved.
Drawings
FIG. 1 is a process flow diagram of a method of making a glazed ceramic according to one embodiment.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to specific embodiments that are now described. Preferred embodiments of the invention are given in the detailed description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Aiming at the problems of glazing the green body subjected to high-temperature biscuit firing by adopting a glaze spraying mode in the traditional technology, the invention adjusts the glaze slurry, so that the glaze slurry can be used for glazing the green body subjected to high-temperature biscuit firing by adopting a glaze dipping mode, and the problems of more dust, uneven glaze layer, poor adhesive force and the like existing in the glaze spraying mode are avoided.
Specifically, the glaze slip of one embodiment is prepared from the following raw materials: glaze and water, the specific gravity of the glaze slurry is 1.65 g/mL-1.68 g/mL, and the flow rate is 45s/100 mL-55 s/100mL.
In a specific example, the specific gravity of the glaze slip is 1.65g/mL, 1.66g/mL, 1.67g/mL, 1.68g/mL, or a range consisting of any two of these values. The flow rate of the glaze slip is 45s/100mL、46s/100mL、47s/100mL、48s/100mL、49s/100mL、50s/100mL、51s/100mL、52s/100mL、53s/100mL、54s/100mL、55s/100mL or the range formed by any two of the values. By adopting the glaze slurry with the specific gravity and the flow rate, the glaze slurry can be glazed on the surface of the blank body subjected to high-temperature biscuit firing in a glaze dipping mode, and the consistency and the viscosity of the glaze slurry are utilized to adhere the glaze slurry to the surface of the biscuit with low water absorption, so that the obtained glaze layer is more uniform, the adhesion is strong, and the defects of 'glaze accumulation', 'glaze shrinkage', and the like are avoided. In addition, too little glaze absorbed by the biscuit can cause thin glaze when the flow rate of the glaze slurry is too high, and uneven glaze can flow when the flow rate is too low, so that glaze is accumulated at the positions of handles or grooves and the like to form 'glaze strands'.
Specifically, the glaze is a basic glaze used for glazing a blank body subjected to high-temperature biscuit firing. In a specific example, the glaze is a glaze used for producing magnesia porcelain, and the composition of the glaze is shown in the following table 1:
TABLE 1
In the table, IL refers to loss on ignition. Kaolin, bentonite, etc. contain water of crystallization, which is discharged at high temperatures, and also some organics, which are discharged at high temperatures, causing weight loss, the reduced fraction being loss on ignition, labeled IL.
It will be appreciated that the composition of the glaze is not limited thereto, and may be any glaze commonly used in the art for glazing green bodies after high temperature bisque firing.
In some embodiments, the raw materials for preparing the glaze slip also comprise a quick-drying agent, and the mass ratio of the quick-drying agent to the glaze is (2-5): 100. In one specific example, the mass ratio of the quick-drying agent to the glaze is 2:100, 3:100, 4:100, 5:100, or a range consisting of any two of these values. On the one hand, the addition of a certain amount of quick-drying agent into the glaze can keep the specific gravity and the flow rate of the glaze slurry stable, and avoid the influence of unstable glaze slurry on the quality of the glaze surface. On the other hand, the quick-drying agent is added to make the drying speed of the surface glaze slurry of the green body after the glaze dipping faster. In addition, the quick-drying agent can also reduce the consistency of the glaze slip, and has the functions of dilution and water reduction.
Specifically, the raw materials for preparing the quick-drying agent comprise: acrylic emulsion, gelatin, glycerin, defoamer, preservative and water. In a specific embodiment, the quick-drying agent comprises, in mass percent: 16-20% of acrylic emulsion, 10-15% of gelatin, 4-8% of glycerin, 3-6% of defoamer, 0.5-2% of preservative and 57-62% of water.
In a specific example, the acrylic emulsion has a specific gravity of 1.08g/mL to 1.1g/mL and a viscosity of 2600 MPa.S to 2900 MPa.S.
In a specific example, the defoamer mainly comprises modified polyether, lipidation and high-carbon alcohol substances, and is prepared by adopting a special process. The defoaming speed is high, the foam inhibition time is long, and the efficiency is high. The pH value of the defoamer is 7-8; the content of active substances is 52% -100%; the viscosity (rotor No. 1) is 800 MPa.S-1000 MPa.S. In a specific example, the defoamer is DOW and/or BAYER.
The content of active substances of the preservative is more than or equal to 20 percent+/-1 percent, and the pH value is as follows: 6.5 to 7.5; specific gravity (20 ℃, g/cm 3): 1.02 to 1.06. The pH application range of the preservative is 2-14; high temperature: 150 ℃. In one specific example, the preservative is BASF.
The inventors found in experiments that the addition of additives such as PC67, NH 4 Cl, CMC, etc. to the glaze slip resulted in poor stability of the glaze slip, particularly a large change in flow rate with time, while the drying rate of the glaze slip containing the above additives such as PC67, NH 4 Cl, CMC, etc. after the impregnation of the glaze was slow. Therefore, the glaze slip of the present embodiment does not contain the above-described additives such as PC67, NH 4 Cl, CMC, and the like.
In some embodiments, the raw materials for preparing the glaze slip also comprise a suspending agent, and the mass ratio of the suspending agent to the glaze is (2-5): 100.
In a specific example, the suspending agent is selected from at least one of bentonite and kaolin. In one specific example, the suspending agent is specifically inner bentonite. For example, the chemical composition of bentonite is shown in table 2 below:
TABLE 2
Name of the name SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O IL ZnO Li2O B2O3 Totalizing
Mass percent/% 67.24 15.79 0.24 0.06 2.95 3.22 0.32 0.08 10.10 - - - 100
Because of different processes of dipping glaze and spraying glaze, a certain amount of suspending agent is added into the glaze slip, so that the good suspension property of the glaze slip can be ensured, and the phenomenon of glaze and moisture layering does not occur.
In some embodiments, the particle size of the glaze slip is less than or equal to 44 μm. The particle size of the glaze slip is controlled to be the value, so that the glossiness of the prepared glaze layer can be guaranteed to be good.
Further, the quantity of the glaze slips with the grain diameter less than or equal to 2 mu m in the glaze slips accounts for 10 to 16 percent of the total quantity of the glaze slips. The ratio of the grain diameter of the glaze slip is less than or equal to 2 mu m, so that the shrinkage of the glaze layer prepared by the glaze slip is large, and the defects of glaze shrinkage and the like are easy to occur. The ratio of the grain diameter of the glaze slip is less than or equal to 2 mu m, and the glaze layer prepared by the glaze slip has poor glossiness.
In a specific example, the cumulative particle distribution of the glaze slip is shown in table 3 below:
TABLE 3 Table 3
Particle size 2μm 5μm 10μm 20μm 30μm 44μm
Cumulative particle distribution (%) 10～16 35～45 70～75 90～95 95～99 100
The glaze slip has at least the following advantages:
(1) The specific gravity and the flow rate of the glaze slurry are adjusted to be in a proper state, so that the blank body after high-temperature biscuit firing is immersed in the glaze slurry, the glaze slurry is adhered to the surface of the biscuit with low water absorption rate by using the consistency and the viscosity of the glaze slurry, the obtained glaze layer is more uniform, the adhesion force is strong, and the defects of 'glaze accumulation', 'glaze shrinkage', and the like are avoided. Therefore, the glaze slip can glaze the blank body subjected to high-temperature biscuit firing in a glaze dipping mode, so that the problems of more dust, uneven glaze layer, poor adhesive force and the like existing in a glaze spraying mode are avoided, and the product qualification rate is improved.
(2) The glaze slip also contains a certain amount of quick-drying agent, so that on one hand, the specific gravity and the flow velocity of the glaze slip can be kept stable by the quick-drying agent, and the influence on the quality of the glaze due to unstable glaze slip is avoided. On the other hand, the quick-drying agent is added to make the drying speed of the surface glaze slurry of the green body after the glaze dipping faster. In addition, the quick-drying agent can also reduce the consistency of the glaze slip, and has the functions of dilution and water reduction.
(3) The glaze slip also contains a certain amount of suspending agent, so that the good suspension property of the glaze slip can be ensured, and the phenomenon of glaze and moisture layering does not occur.
(4) The glaze slip can be used for glazing a blank body subjected to high-temperature bisque firing in a glaze dipping mode, and the glaze material is not atomized in the glazing process and is completely in a liquid form, so that the glaze slip is harmless to human bodies and the environment. In addition, the traditional glaze slip is adopted to coat the glaze in a glaze spraying mode, the glaze absorbed by the biscuit only accounts for 30% -35% of the total weight of the glaze, the rest of the glaze needs to be recycled or scrapped, and the cost is high.
The invention also provides a preparation method of the glaze slip in an embodiment, which comprises the following steps:
The glaze is mixed with water, the specific gravity of the mixed slurry is 1.65 g/mL-1.68 g/mL, and the flow rate is 45 s-55 s/100mL, and the glaze slip is prepared.
In a specific example, the specific gravity of the glaze slip is 1.65g/mL, 1.66g/mL, 1.67g/mL, 1.68g/mL, or a range consisting of any two of these values. The flow rate of the glaze slip is 45s/100mL、46s/100mL、47s/100mL、48s/100mL、49s/100mL、50s/100mL、51s/100mL、52s/100mL、53s/100mL、54s/100mL、55s/100mL or the range formed by any two of the values. By adopting the glaze slurry with the specific gravity and the flow rate, the glaze slurry can be glazed on the surface of the blank body subjected to high-temperature biscuit firing in a glaze dipping mode, and the consistency and the viscosity of the glaze slurry are utilized to adhere the glaze slurry to the surface of the biscuit with low water absorption, so that the obtained glaze layer is more uniform, the adhesion is strong, and the defects of 'glaze accumulation', 'glaze shrinkage', and the like are avoided. In addition, too little glaze absorbed by the biscuit can cause thin glaze when the flow rate of the glaze slurry is too high, and uneven glaze can flow when the flow rate is too low, so that glaze is accumulated at the positions of handles or grooves and the like to form 'glaze strands'.
In some embodiments, a quick-drying agent is also added in the step of mixing the glaze with water, wherein the mass ratio of the quick-drying agent to the glaze is (2-5): 100. In one specific example, the mass ratio of the quick-drying agent to the glaze is 2:100, 3:100, 4:100, 5:100, or a range consisting of any two of these values. On the one hand, the addition of a certain amount of quick-drying agent into the glaze can keep the specific gravity and the flow rate of the glaze slurry stable, and avoid the influence of unstable glaze slurry on the quality of the glaze surface. On the other hand, the quick-drying agent is added to make the drying speed of the surface glaze slurry of the green body after the glaze dipping faster. In addition, the quick-drying agent can also reduce the consistency of the glaze slip, and has the functions of dilution and water reduction.
Specifically, the quick-drying agent includes: acrylic emulsion, gelatin, glycerin, defoamer, preservative and water. In a specific embodiment, the quick-drying agent comprises, in mass percent: 16-20% of acrylic emulsion, 10-15% of gelatin, 4-8% of glycerin, 3-6% of defoamer, 0.5-2% of preservative and 57-62% of water. The inventors found in experiments that the addition of additives such as PC67, NH 4 Cl, CMC, etc. to the glaze slip resulted in poor stability of the glaze slip, especially a large change in flow rate with time, while the drying rate of the glaze slip containing the above additives such as PC67, NH4Cl, CMC, etc. after the impregnation was slow. Therefore, the glaze slip of the present embodiment does not contain the above-described additives such as PC67, NH 4 Cl, CMC, and the like.
Specifically, the glaze is a basic glaze used for glazing a blank body subjected to high-temperature biscuit firing. In a specific example, the glaze is a glaze used in the production of magnesia porcelain.
In some embodiments, in the step of mixing the glaze, the quick-drying agent and water, a suspending agent is also added, and the mass ratio of the suspending agent to the glaze is (2-5): 100.
In a specific example, the suspending agent is selected from at least one of bentonite and kaolin. In one specific example, the suspending agent is specifically inner bentonite. For example, bentonite has the chemical composition shown in table 2 above:
TABLE 2
Name of the name SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O IL ZnO Li2O B2O3 Totalizing
Mass percent/% 67.24 15.79 0.24 0.06 2.95 3.22 0.32 0.08 10.10 - - - 100
Because of different processes of glaze dipping and glaze spraying, a certain amount of suspending agent is added in the ball milling process of the glaze, so that the good suspension property of the glaze slurry can be ensured, and the phenomenon of glaze and moisture layering does not occur.
Specifically, the glaze, the quick-drying agent and the suspending agent are mixed with water in a ball milling mode.
In some embodiments, the mass ratio of the total mass of the glaze, the suspending agent and the quick-drying agent to the mass of the ball milling medium and the water in the ball milling process is 1:2 (0.35-0.5). For example, the mass ratio of the total mass of glaze, suspending agent and quick-drying agent to the mass of ball milling medium and water is 1:2:0.35、1:2:0.36、1:2:0.37、1:2:0.38、1:2:0.39、1:2:0.4、1:2:0.41、1:2:0.42、1:2:0.43、1:2:0.44、1:2:0.45、1:2:0.46、1:2:0.48、1:2:0.5 or the range composed of any two of these values.
In one specific example, the ball milling media is ceramic balls, such as high alumina ceramic balls.
Further, the ball milling time is 20-25 h. The grain diameter of the glaze slurry after ball milling is less than or equal to 44 mu m. The particle size of the glaze slip is controlled to be the value, so that the glossiness of the prepared glaze layer can be guaranteed to be good.
Further, the quantity of the glaze slips with the grain diameter less than or equal to 2 mu m in the glaze slips accounts for 10 to 16 percent of the total quantity of the glaze slips. The ratio of the grain diameter of the glaze slip is less than or equal to 2 mu m, so that the shrinkage of the glaze layer prepared by the glaze slip is large, and the defects of glaze shrinkage and the like are easy to occur. The ratio of the grain diameter of the glaze slip is less than or equal to 2 mu m, and the glaze layer prepared by the glaze slip has poor glossiness.
In a specific example, the cumulative particle distribution of the glaze slip is as shown in table 3 above:
TABLE 3 Table 3
Particle size 2μm 5μm 10μm 20μm 30μm 44μm
Cumulative particle distribution (%) 10～16 35～45 70～75 90～95 95～99 100
In some embodiments, the step of mixing the glaze, quick-drying agent, and water comprises: ball milling is carried out on the glaze, part of quick-drying agent and water for 20-25 h, and then the rest quick-drying agent is added and mixed for 30 min. Specifically, the mass percentage of the partial quick-drying agent to the glaze is more than or equal to 2:100. The mass percentage of the rest quick-drying agent and the glaze is less than or equal to 3:100. On the one hand, the quick-drying agent is added twice, so that the seasonal factors are considered, and the whole quick-drying agent can be added once or a small amount of quick-drying agent can be added for the second time when the temperature is higher in summer. When the temperature in winter is low, the adding proportion of the second quick-drying agent can be 3 percent. On the other hand, when the quick-drying agent is added at one time, the time after the preparation of the glaze slip is finished may be prolonged, the flow speed of the glaze slip becomes fast, and the glaze slip adsorbed by the biscuit is reduced during the glaze dipping, so that the defects of thin glaze and the like are caused. The quick-drying agent is added twice, so that the ball milling dispersion can be ensured, the ball milling is facilitated, the stable flow rate of the glaze slip can be ensured, and the flow rate can not be changed after the glaze slip is placed for 7 days.
In some embodiments, after the step of mixing the glaze with water, a step of de-ironing and sieving is also included. Iron and other harmful substances are removed as much as possible by deironing and sieving, and coarse particles are removed after sieving.
The preparation method of the glaze slip has at least the following advantages:
(1) The preparation method of the glaze slip has simple process and is easy to produce.
(2) The glaze slurry prepared by the preparation method of the glaze slurry can be used for glazing a blank body subjected to high-temperature bisque firing in a glaze dipping mode, so that the surface of a glaze layer is flat and firm, the adhesion is strong, the glaze slurry is not easy to drop, and the defect of 'glaze shrinkage' is not easy to cause. In addition, the glaze layer is uniform and has good flatness.
Referring to fig. 1, the present invention further provides a method for preparing a glazed ceramic according to an embodiment, which includes the following steps:
step S110: providing a biscuit firing blank body, wherein the water absorption rate of the biscuit firing blank body is less than or equal to 0.5 percent.
Specifically, the biscuit firing blank is a blank subjected to high-temperature biscuit firing, wherein the temperature of the high-temperature biscuit firing is 1280-1330 ℃, and the time of the high-temperature biscuit firing is 15-18 h. The atmosphere of the high-temperature biscuit firing is an oxidizing atmosphere. The biscuit firing blank has good semi-light transmittance.
In some embodiments, the preparation process of the bisque-fired body is specifically as follows: and (3) shaping and drying the pug, and then sintering at high temperature to ensure that the water absorption rate of the biscuit firing blank body is less than or equal to 0.5 percent. Specifically, the mud material is molded by roll forming, slip casting, isostatic pressing, plastic pressing and the like. It will be appreciated that after the step of shaping the pug, the shaped pug may also be trimmed, e.g. trimmed, glued attachments, etc., before the step of drying. Before the high-temperature biscuit firing, the dried green body can be subjected to a green body repairing and washing treatment. The above only lists a common preparation process of the biscuit firing blank, but is not limited thereto, and the biscuit firing blank of the present embodiment may be obtained by a preparation method of a high temperature biscuit firing blank commonly used in the art.
In one specific example, the bisque-fired body is a bisque-fired body for magnesium porcelain.
Step S120: and immersing the biscuit firing blank in glaze slurry to form a glaze layer on the biscuit firing blank, and then performing glaze firing to prepare the glazed ceramic.
Specifically, the glaze slip is the same as that of the above embodiment, and will not be described here again.
In some embodiments, the thickness of the glaze layer is 0.1mm to 0.2mm. For example, the thickness of the glaze layer is 0.1mm, 0.12mm, 0.15mm, 0.18mm, 0.2mm or a range consisting of any two of these values. When the glaze layer is too thin, the glaze layer is uneven after glaze firing, has water ripple, cannot cover the blank completely, and can cause defects such as pinholes, uneven glaze and the like; when the glaze layer is too thick, the glaze slurry dries slowly, and the glaze slurry flows downwards along the three-dimensional surface, so that the glaze is piled up at the corners or the bottoms to form 'glaze strands' and the later stage of the too thick glaze layer can cause poor thermal shock resistance. Therefore, in this embodiment, the thickness of the glaze layer is controlled to be 0.1mm to 0.2mm.
Further, the time for immersing the biscuit firing blank in the glaze slip is 3 s-5 s. In a specific embodiment, the biscuit firing blank is immersed in the glaze slip by hand or by machine.
In the actual process, the glaze slip at the bottom can be wiped off after the glaze layer is slightly dried. The slightly dry glaze layer means that the upper surface of the three-dimensional product can be grasped by hand, and the lower surface is also wet, and the upper half part can be grasped by hand at the moment to clean the bottom glaze of the three-dimensional piece. If the upper part and the lower part of the glaze are completely dried, the glaze of the foot is rubbed, firstly, the production efficiency is affected, and secondly, the glaze is scraped when the bottom glaze is too dry.
In some embodiments, the temperature of the glaze firing is 1100 ℃ to 1150 ℃ and the time of the glaze firing is 10 hours to 12 hours.
Specifically, the glaze firing is performed in a tunnel kiln. The step of glazing is the same as the conventional step of glazing at low temperature. The glazed ceramic with glossy and smooth glaze surface can be obtained by the method.
In one embodiment, the biscuit firing blank is a biscuit firing blank for magnesia porcelain, and the glazed ceramic is a magnesia porcelain. Through testing, the prepared magnesia porcelain can meet the requirements by testing and performance testing according to GB28114-2011 magnesia reinforced porcelain standards.
In the actual processing, further comprising: and (3) carrying out decal, gold drawing, decoration firing, gold firing, flower inspection and final inspection on the glazed ceramic so as to meet the delivery requirements.
In some embodiments, the bisque-fired body is a bisque-fired body for three-dimensional products such as cups, kettles, and the like. The method can be used for glazing the outside of the stereoscopic product, the internal glazing can be performed by adopting a manual or machine glazing mode, the fact that the interface between the internal glazing and the external glazing is possibly poor after the glazing is soaked is considered, and the glaze is sprayed on the edge of the opening by using a spray gun after the glazing is soaked, so that the seamless connection of the joint part is ensured. Furthermore, the glazed ceramic prepared by the method is a cup-type or kettle-type ceramic product.
The preparation method of the glazed ceramic has at least the following advantages:
(1) The preparation method of the glazed ceramic is simple in process, and the glaze is applied to the high-temperature biscuit firing blank in a glaze dipping mode, so that the surface of a glaze layer is smooth and firm, the adhesive force is strong, the glaze is not easy to drop, and the defect of 'glaze shrinkage' is not easy to cause. In addition, the glaze layer is uniform and has good flatness.
(2) The preparation method of the glazed ceramic adopts a glaze dipping mode to glaze the blank body subjected to high-temperature bisque firing, and the glaze cannot be atomized in the glaze coating process and completely appears in a liquid form, so that the glaze is harmless to human bodies and the environment. In addition, the recycled glaze is not formed, and the waste and the repeated processing of the glaze are not caused.
(3) The preparation method of the glazed ceramic is particularly suitable for preparing three-dimensional products such as cups, kettles and the like.
The invention also provides the glazing ceramic of an embodiment, which is prepared by adopting the preparation method of the glazing ceramic of the embodiment.
The glazed ceramic has the advantages of smooth and firm glaze layer surface, strong adhesion, difficult falling and difficult glaze shrinkage defect. In addition, the glaze layer is uniform, the flatness is good, and the defects of glaze accumulation, glaze stacking, bao You and the like are fewer.
In one specific example, the glazed ceramic is a cup-like or pot-like ceramic article.
In order to make the objects and advantages of the present invention more apparent, the following more detailed description of the glaze slip, glazed ceramic and effects thereof will be given in connection with the specific examples, which are described herein for purposes of illustration only and are not intended to be limiting.
Example 1
The preparation process of the glaze slip of the embodiment comprises the following steps:
ball milling the glaze, bentonite, quick drying agent and water for 20 hours, then removing iron and sieving to prepare glaze slip. The compositions of the glaze, the bentonite and the quick-drying agent are shown in the following table 4, wherein the mass ratio of the glaze to the bentonite to the quick-drying agent is 100:2:5, and the mass ratio of the total mass of the glaze to the bentonite to the quick-drying agent to the ball milling medium to the water is 1:2:0.45.
The specific gravity of the glaze slip of this example was 1.66g/mL, and the flow rate was 48s/100mL.
In the preparation process of the glaze slurry, the quick-drying agent is added once, the flow rate of the glaze slurry can be increased to 38 seconds/100 mL after the preparation for 4 hours, the glaze slurry adsorbed by the biscuit is reduced, and the glaze surface is uneven and has waves after firing, so that the surface of the blank cannot be effectively covered. Therefore, the glaze slip of this example needs to be used within 4 hours after completion of formulation.
TABLE 4 Table 4
Example 2
The preparation process of the glaze slip of the embodiment comprises the following steps:
Ball milling the glaze, bentonite, partial quick-drying agent and water for 20 hours, adding the rest quick-drying agent, mixing for 30 minutes, removing iron, and sieving to prepare the glaze slurry. The compositions of the glaze, the bentonite and the quick-drying agent are shown in the table 4, wherein the mass ratio of the glaze to the bentonite to part of the quick-drying agent is 100:2:2, and the mass ratio of the total mass of the glaze to the bentonite to part of the quick-drying agent to the ball milling medium to the water is 1:2:0.45. The mass ratio of the residual quick-drying agent to the glaze is 3:100.
The specific gravity of the glaze slip of this example was 1.68g/mL, and the flow rate was 54s/100mL.
The quick-drying agent in the glaze slip of the embodiment is added twice, so that the ball milling dispersion can be ensured, the ball milling is facilitated, the stable flow rate of the glaze slip can be ensured, and the flow rate can not be changed after the glaze slip is placed for 7 days.
Example 3
The preparation process of the glaze slip of the embodiment comprises the following steps:
ball milling the glaze, the quick drying agent and water for 20 hours, and then removing iron and sieving to prepare glaze slip. The compositions of the glaze and the quick-drying agent are shown in the table 4, the mass ratio of the glaze to the quick-drying agent is 100:2, and the mass ratio of the total mass of the glaze and the quick-drying agent, the ball milling medium and the water is 1:1:0.45.
The specific gravity of the glaze slip of this example was 1.68g/mL, and the flow rate was 45s/100mL.
The glaze slip of the embodiment is not added with bentonite, has poor suspension property and is easy to precipitate, so that the specific gravity is high, and the flow speed is also high. In the actual process, if the stirring is not in time, the defects of thin glaze, glaze strands, glaze shrinkage and the like can occur.
Example 4
The preparation process of the glaze slip of the embodiment comprises the following steps:
ball milling the glaze, bentonite and water for 20 hours, and then removing iron and sieving to prepare the glaze slurry. The compositions of the glaze and the bentonite are shown in the table 4, the mass ratio of the glaze to the bentonite is 100:2, and the mass ratio of the total mass of the glaze to the bentonite, the ball milling medium and the water is 1:2:0.50.
The specific gravity of the glaze slip of this example was 1.65g/mL, and the flow rate was 55s/100mL.
The drying agent is not accelerated in the glaze slurry in the embodiment, water is added during ball milling, so that the dispersion is convenient, otherwise, the ball milling efficiency is poor, the flow rate of the glaze slurry changes rapidly along with the change of time, and the flow rate becomes 30 seconds/100 mL after 1 hour, so that the glaze slurry in the embodiment needs to be used within 1 hour after the preparation is completed.
Comparative example 1
The preparation process of the glaze slip of the comparative example 1 comprises the following steps:
Ball milling the glaze, bentonite, quick drying agent and water for 20 hours, removing iron after ball milling the glaze, and adjusting the specific gravity and the flow rate of the glaze slurry to 1.60g/mL and 32s/100mL by using water during sieving to prepare the glaze slurry. The compositions of the glaze, the bentonite and the quick-drying agent are shown in the table 4, wherein the mass ratio of the glaze to the bentonite to the quick-drying agent is 100:2:5, and the mass ratio of the total mass of the glaze to the bentonite to the quick-drying agent to the ball milling medium to the water is 1:2:0.45.
Comparative example 2
The preparation process of the glaze slip of comparative example 2 comprises the following steps:
Ball milling the glaze, bentonite, quick drying agent and water for 20 hours, removing iron after ball milling the glaze, and adjusting the specific gravity and the flow rate of the glaze slurry to be 1.72g/mL and 67s/100mL respectively by using water during sieving to prepare the glaze slurry. The compositions of the glaze, the bentonite and the quick-drying agent are shown in the table 4, wherein the mass ratio of the glaze to the bentonite to the quick-drying agent is 100:2:5, and the mass ratio of the total mass of the glaze to the bentonite to the quick-drying agent to the ball milling medium to the water is 1:2:0.45.
Glazing the high-temperature biscuit firing blank by adopting the glaze slurries prepared in the examples 1-4 and the comparative examples 1-2 to prepare glazed ceramics, wherein the concrete steps are as follows:
(1) Providing a magnesia porcelain biscuit firing blank, wherein the water absorption rate of the biscuit firing blank is 0.12 percent.
(2) The biscuit firing blank is immersed in the glaze slip for 4s to form a glaze layer on the biscuit firing blank, and then glaze firing is carried out for 11h at 1125 ℃ under the oxidizing atmosphere, so as to prepare the glazed ceramic.
The performance of glazed ceramics prepared from different glaze slips was tested according to GB28114-2011 magnesia-reinforced porcelain standard, and experimental data shown in the following Table 5 were obtained.
TABLE 5
The glazed ceramic prepared by the embodiment meets the requirements of other performances such as water absorption, whiteness, thermal shock resistance, vickers hardness of the glaze surface and the like besides the appearance quality listed in the table, and meets the GB28114-2011 magnesia reinforced ceramic standard. Therefore, the glaze slip of the embodiment can be used for preparing the glazed ceramic with excellent performance in a glaze dipping mode, and the problem brought by the glaze spraying mode is solved.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present invention, which facilitate a specific and detailed understanding of the technical solutions of the present invention, but are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. It should be understood that, based on the technical solutions provided by the present invention, those skilled in the art can obtain technical solutions through logical analysis, reasoning or limited experiments, which are all within the protection scope of the appended claims. The scope of the patent is therefore intended to be covered by the appended claims, and the description and drawings may be interpreted as illustrative of the contents of the claims.

Claims (17)

1. The preparation method of the glazed ceramic is characterized by comprising the following steps:
providing a biscuit firing blank, wherein the water absorption rate of the biscuit firing blank is less than or equal to 0.5%;
Immersing the biscuit firing blank body in glaze slurry to form a glaze layer on the biscuit firing blank body, and then performing glaze firing to prepare glazed ceramics;
the raw materials for preparing the glaze slip comprise: the specific gravity of the glaze slip is 1.65 g/mL-1.68 g/mL, and the flow rate is 45s/100 mL-55 s/100mL;
The mass ratio of the quick-drying agent to the glaze is (2-5) 100, and the raw materials for preparing the quick-drying agent comprise the following components in percentage by mass: 16-20% of acrylic emulsion, 10-15% of gelatin, 4-8% of glycerin, 3-6% of defoamer, 0.5-2% of preservative and 57-62% of water.
2. The method of producing a glazed ceramic according to claim 1, wherein the raw materials for producing the glaze slip further include a suspending agent.
3. The method for producing a glazed ceramic according to claim 2, wherein the mass ratio of the suspending agent to the glaze is (2-5): 100.
4. The method for producing a glazed ceramic according to claim 2, wherein the suspending agent is at least one selected from bentonite and kaolin.
5. The method for producing a glazed ceramic according to claim 1, wherein the glaze is a glaze used for production of magnesia porcelain.
6. The method of claim 1, wherein the slip does not contain PC67, NH 4 Cl and CMC additives.
7. The method for producing a glazed ceramic according to any one of claims 1 to 6, wherein the particle size of the glaze slip is 44 μm or less.
8. The method for producing a glazed ceramic according to claim 7, wherein the amount of the glaze slips having a particle diameter of 2 μm or less in the glaze slips is 10% to 16% by weight based on the total amount of the glaze slips.
9. The method for preparing glazed ceramic according to any one of claims 1 to 6, wherein the glaze slip further comprises a suspending agent, and the preparation steps of the glaze slip are as follows: and mixing the glaze with water, a quick-drying agent and a suspending agent by adopting a ball milling mode.
10. The method for preparing glazed ceramic according to claim 9, wherein the mass ratio of the total mass of the glaze, the quick-drying agent and the suspending agent to the mass of the ball milling medium and the mass of water in the ball milling process is 1:2 (0.35-0.5).
11. The method of producing a glazed ceramic according to claim 9, wherein the step of mixing the glaze, the quick-drying agent, the suspending agent and water includes: ball milling is carried out on the glaze, part of the quick-drying agent, the suspending agent and water for 20-25 h, then the rest of the quick-drying agent is added for continuous ball milling for 30min.
12. The method for preparing a glazed ceramic according to claim 1, wherein the thickness of the glaze layer is 0.1mm to 0.2mm.
13. The method of producing a glazed ceramic according to claim 1 or 12, wherein the time for immersing the biscuit firing blank in the glaze slip is 3s to 5s.
14. The method for preparing glazed ceramic according to claim 1, wherein the temperature of the glaze firing is 1100 ℃ to 1150 ℃ and the time of the glaze firing is 10h to 12h.
15. The method for preparing the glazed ceramic according to claim 1 or 14, wherein the biscuit firing blank is a blank subjected to high-temperature biscuit firing, the temperature of the high-temperature biscuit firing is 1280-1330 ℃, and the time of the high-temperature biscuit firing is 15-18 h; and/or the number of the groups of groups,
The biscuit firing blank is a magnesia porcelain biscuit firing blank.
16. A glazed ceramic characterized by being prepared by the method for preparing a glazed ceramic according to any one of claims 1 to 15.
17. The glazed ceramic of claim 16, wherein the glazed ceramic is a cup-like or pot-like ceramic article.
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