CN114956573B - Waxy glaze, waxy 3D ceramic tile and preparation method thereof - Google Patents
Waxy glaze, waxy 3D ceramic tile and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/22—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions containing two or more distinct frits having different compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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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
- C04B41/52—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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- 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
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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Abstract
The invention discloses a waxy glaze, a waxy 3D ceramic tile and a preparation method thereof, relating to the technical field of ceramics, wherein the waxy glaze comprises the following components: 40-50 parts of first frit and 30-40 parts of second frit; according to the mass percentage, the preparation raw material of the first frit contains 7.5-12% of white carbon black, and the preparation raw material of the second frit contains 4.6-7.6% of nano alumina and 5.5-9.5% of white carbon black. The wax glaze is a matt glaze, the main component of the wax glaze is a frit, the porosity of the glaze after firing can be reduced, the transparency of the glaze is greatly improved, the glaze still has good light transmittance under the condition that the thickness of the glaze is thick, and meanwhile, the frit can improve the fineness and the softness of the glaze, so that the glaze has a wax texture like jade.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a waxy glaze, a waxy 3D ceramic tile and a preparation method thereof.
Background
With the popularity of matte products in recent years, the development of the matte ceramic tiles is more rapid, and the matte products are deeply loved by consumers with soft light sensation. At present, most of matte glazed products have gloss of 8-15 degrees, and although the light sense is soft, the defects of rough texture and dark light sense generally exist, and the prior art does not have the hand feeling of the matte glazed ceramic tile like jade.
In addition, the matte glaze material in the prior art mainly utilizes the mode that divalent oxide precipitates crystals in firing to produce the matte effect, and the matte effect is obvious when the glaze thickness is thin, but the thickness is poor, however, when the glaze thickness is thick and has the thickness, because the crystallization of the glaze and the porosity in the glaze exist, the transparency of the glaze is greatly weakened.
It is seen that improvements and enhancements to the prior art are needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a waxy glaze, a waxy 3D ceramic tile and a preparation method thereof, and aims to solve the technical defect of poor permeability of the waxy glaze in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the waxy glaze comprises the following components in parts by weight: 40-50 parts of first frit and 30-40 parts of second frit; according to the mass percentage, the preparation raw material of the first frit contains 7.5-12% of white carbon black, and the preparation raw material of the second frit contains 4.6-7.6% of nano alumina and 5.5-9.5% of white carbon black.
In the waxy glaze, the preparation raw materials of the first frit comprise, by weight: 15 to 18 parts of kaolin, 6 to 8 parts of zinc oxide, 3 to 6 parts of sodium borate, 25 to 36 parts of pyrophyllite, 8 to 12 parts of white carbon black, 5 to 8 parts of strontium carbonate, 10 to 13 parts of sodium carbonate, 12 to 15 parts of barium carbonate and 3 to 5 parts of wollastonite.
In the waxy glaze, the second frit comprises the following raw materials in parts by weight: 20 to 25 portions of kaolin, 5 to 8 portions of nano alumina, 10 to 15 portions of potassium carbonate, 5 to 8 portions of sodium carbonate, 10 to 15 portions of spodumene, 6 to 10 portions of white carbon black, 4 to 7 portions of talc and 30 to 36 portions of pyrophyllite.
In the waxy glaze, the preparation raw materials of the waxy glaze further comprise: 8-12 parts of air knife soil, 3-5 parts of zinc oxide and 5-8 parts of dolomite.
A waxy 3D ceramic tile comprises a tile blank layer, a makeup soil layer, a surface glaze layer, a pattern layer and a waxy glaze layer which are sequentially stacked, wherein sunken textures are further arranged in the surface glaze layer, the pattern layer and the waxy glaze layer, and the waxy glaze layer is prepared from the waxy glaze.
In the waxy 3D tile, the texture is prepared by repelling the glaze layer and the waxy glaze layer with a mold ink, wherein the mold ink comprises, in mass percent: 38 to 48 percent of waxy glaze, 20 to 30 percent of acrylic resin, 20 to 30 percent of ethyl acetate, 3 to 6 percent of dispersant, 0.1 to 0.2 percent of suspending agent, 0.2 to 0.3 percent of defoaming agent, 0.3 to 0.6 percent of flatting agent and 0.15 percent of pH value regulator.
In the waxy 3D ceramic tile, the chemical composition of the overglaze layer comprises the following components in percentage by mass: siO 2 2 50～55%、Al 2 O 3 23～28%、CaO 1.5～3.1%、MgO 2.5～3.0%、K 2 O 3.5～4.5%、Na 2 O2.1-4.1%, znO 4.5-6.5%, and the balance of ignition loss and trace impurities.
In the waxy 3D ceramic tile, the chemical composition of the makeup soil layer comprises the following components in percentage by mass: al (Al) 2 O 3 26～32%、SiO 2 55～60%、CaO 1.5～2.3%、MgO 1.3～2.4%、K 2 O 3.5～4.6%、Na 2 O3.8-4.6%, and trace impurities and ignition loss in balance.
A preparation method of the waxy 3D tile as described above, wherein the preparation method comprises the following steps in sequence:
sequentially forming a brick blank layer and a makeup soil layer;
depositing first mould ink on the surface of the makeup soil layer, and forming a glaze layer on the surface of the first mould ink;
and forming a pattern layer on the surface of the overglaze layer, depositing second mould ink on the surface of the pattern layer, forming a waxy glaze layer on the surface of the second mould ink, and sintering to obtain the waxy 3D ceramic tile.
In the preparation method of the waxy 3D ceramic tile, the method for depositing the first mould ink and the method for depositing the second mould ink are both ink-jet printing methods, and the printing gray scale is 40-100%; in the firing step, the firing temperature is 1180-1300 ℃, and the firing time is 40-60 minutes.
Has the advantages that:
the invention provides a waxy glaze which is a matte glaze, the main component of the waxy glaze is a frit, organic matters and carbonates in each component are decomposed and discharged in advance due to the fact that the frit is calcined in advance, when the frit is calcined together with a blank, the porosity of pores in the glaze is greatly reduced, the transparency of the glaze can be greatly improved, and the frit still has good light transmittance under the condition that the thickness of the glaze is thick.
The invention also provides a waxy 3D ceramic tile, which comprises a tile blank layer, a makeup soil layer, a surface glaze layer, a pattern layer and a waxy glaze layer, wherein through depositing hydrophobic mold ink on the makeup soil layer and the pattern layer, sunken textures can be formed in the surface glaze layer, the pattern layer and the waxy glaze layer, so that the ceramic tile has a 3D stereoscopic effect. Meanwhile, the waxy glaze layer is prepared from waxy glaze materials, accumulation is formed through the repulsion action of mold ink, the waxy glaze materials can improve the fineness of the ceramic tile, the accumulated position has a heavy feeling, and meanwhile, the waxy glaze layer has good permeability, so that the pattern layer can be well displayed and simultaneously has a waxy texture like jade.
The invention also provides a preparation method of the waxy 3D ceramic tile, which can repel the hydrophilic overglaze layer and the waxy glaze by printing the hydrophobic mold ink on the makeup soil layer and the pattern layer so as to form sunken textures, and the waxy glaze layer positioned on the uppermost surface has fine texture and good light transmission, so that the waxy effect can be formed while the 3D effect is achieved, and the ornamental value of the ceramic tile is greatly improved.
Drawings
Fig. 1 is a schematic structural diagram of a waxy 3D tile provided by the present invention.
FIG. 2 is a pictorial representation of the tile of example 5.
Fig. 3 is a pictorial representation of the tile of example 6.
Figure 4 is a pictorial representation of the tile of example 7.
FIG. 5 is a schematic representation of a tile according to example 8.
Fig. 6 is a pictorial representation of the tile of comparative example 1.
Figure 7 is a pictorial view of a tile according to comparative example 2.
Fig. 8 is a pictorial representation of a tile according to comparative example 3.
Fig. 9 is a pictorial representation of a tile according to comparative example 4.
Fig. 10 is a pictorial representation of a tile according to comparative example 5.
FIG. 11 is a schematic representation of a tile according to comparative example 6.
Fig. 12 is a pictorial representation of a tile according to comparative example 7.
Fig. 13 is a pictorial representation of a tile according to comparative example 8.
Figure 14 is an enlarged view, at 150 x magnification, of a portion of the tile described in comparative example 1.
Figure 15 enlarged view of a portion of the tile described in example 5 at 150 x magnification.
Figure 16 is an SEM image of the tile described in example 5.
In the drawings, the reference numbers: 1-blank, 2-makeup soil layer, 3-surface glaze layer, 4-pattern layer, 5-wax glaze layer and 6-texture.
Detailed Description
The invention provides a waxy glaze, a waxy 3D ceramic tile and a preparation method thereof, and the invention is further detailed by the following embodiments in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
The invention provides a waxy glaze, which comprises the following components: 40-50 parts of first frit and 30-40 parts of second frit; according to the mass percentage, the preparation raw material of the first frit contains 7.5-12% of white carbon black, and the preparation raw material of the second frit contains 4.6-7.6% of nano alumina and 5.5-9.5% of white carbon black. The waxy glaze is a matte glaze, the main component of the waxy glaze is a frit, and the frit needs to be calcined at high temperature for melting during preparation, so that organic matters, carbonate and structural water in the components can be discharged in the process of high-temperature calcination for melting, the porosity is reduced (as shown in fig. 15, pores are very few after the waxy glaze is fired), the transparency and the fine greasy feeling of the glaze are greatly increased, the glaze still has good light transmittance under the condition of thick thickness, and the technical problem that the existing glaze is easy to lose transparency when the thickness is too thick is solved.
Moreover, the raw material for preparing the first frit is added with 7.5-12 wt% of white carbon black, the raw material for preparing the second frit is added with 4.6-7.6 wt% of nano alumina and 5.5-9.5 wt% of white carbon black, and the white carbon black and the nano alumina have very small particle sizes and good dispersibility, so that in the frit preparation process, the white carbon black and the nano alumina can fully react with oxides in the raw materials to form a glass phase or a crystal (as shown in fig. 16, a great amount of glass phase and crystal can be observed to be formed after the waxy glaze is fired through an SEM (scanning electron microscope) diagram), so that the waxy glaze taking the first frit and the second frit as main raw materials has fine texture and is lubricous like jade.
However, since both the first frit and the second frit are ridge-like materials, they are easily precipitated in the glaze slip. 8-12 parts of air knife soil is added into the waxy glaze, and the air knife soil has better suspension property, can avoid the precipitation of ridge materials and improve the stability of glaze slip. However, refractory alumina and silica are introduced into the added air knife soil, so that the firing temperature of the glaze is increased, and 3-5 parts of zinc oxide and 5-8 parts of dolomite are also added into the waxy glaze as fluxing agents, so that the firing temperature of the glaze is reduced.
In one embodiment, the first frit is prepared from the following raw materials in parts by weight: 15 to 18 portions of kaolin, 6 to 8 portions of zinc oxide, 3 to 6 portions of sodium borate, 25 to 36 portions of pyrophyllite, 8 to 12 portions of white carbon black, 5 to 8 portions of strontium carbonate, 10 to 13 portions of sodium carbonate and 12 portions of barium carbonate15 portions to 3 portions to 5 portions of wollastonite. Wherein the kaolin is used to provide Al forming the main skeleton 2 O 3 And SiO 2 Providing a basis for forming various crystals; the zinc oxide, barium carbonate, strontium carbonate and wollastonite can respectively provide divalent oxides of ZnO, baO, srO and CaO, have a fluxing effect and can be used as a high-temperature fluxing agent; the sodium borate and the sodium carbonate provide a monovalent oxide Na 2 O is used as a low-temperature flux, and meanwhile, the sodium borate can provide borate ions, so that the wear resistance of the glaze is improved; the white carbon black belongs to nano-scale SiO 2 The quartz glaze with smaller grain size has higher dispersity compared with quartz with larger grain size, can fully react with divalent oxides to form a glass phase with fine texture, has good light transmittance, solves the problem of rough hand feeling after firing the quartz with common grain size, and ensures that the glaze surface has fine and smooth hand feeling like jade; the pyrophyllite can provide Al in the form of silicate 2 O 3 And SiO 2 Compared to SiO in the form of an independent oxide 2 And Al 2 O 3 After being sintered, the pyrophyllite can be fully combined with a flux to form a crystal phase, thereby solving the problem that SiO exists in the form of oxide 2 And Al 2 O 3 The fineness of the hand feeling of the glaze is easy to reduce.
In one embodiment, the second frit is prepared from the following raw materials in parts by weight: 20 to 25 portions of kaolin, 5 to 8 portions of nano alumina, 10 to 15 portions of potassium carbonate, 5 to 8 portions of sodium carbonate, 10 to 15 portions of spodumene, 6 to 10 portions of white carbon black, 4 to 7 portions of talc and 30 to 36 portions of pyrophyllite. Wherein the kaolin and pyrophyllite function as the first frit; the potassium carbonate, the sodium carbonate and the spodumene can respectively provide monovalent low-temperature oxide flux K 2 O、Na 2 O、Li 2 O, and can form a melting effect with gradient temperature change, so that all components are fully melted to form a glass phase or crystal, and the existence of free quartz is avoided; the nano-alumina has the characteristics of nano-grade particle size, fine particle size, good dispersity and large specific surface area, and can react with an oxide solvent to form zinc-aluminum in the sintering processThe zinc aluminate spinel crystal has soft glossiness and exquisite texture, so that the waxy glaze has a jade-like effect; the talc may increase the smoothness of the glaze.
Furthermore, the raw materials of the first frit contain more divalent oxide fluxing agents, and the raw materials of the second frit contain more monovalent oxide fluxing agents, so that the firing temperatures of the first frit and the second frit are different, and therefore when the adding proportion of the first frit and the second frit is different, waxy glazes with different firing temperatures can be obtained, the range of adjustable firing temperatures of the waxy glazes is wide, and the adaptability is better.
The first frit and the second frit are prepared by special raw materials, calcining at high temperature, melting and cold quenching, and the special raw materials enable the frit to have fine texture and transparent texture after calcining at high temperature and melting, so that the glaze added with the first frit and the second frit has soft glossiness, fine texture and good light transmittance, and can meet the dual requirements of consumers on the heavy feeling and the transparent feeling.
The invention also provides a waxy 3D ceramic tile, as shown in figure 1, the waxy 3D ceramic tile comprises a tile blank layer 1, a make-up soil layer 2, a surface glaze layer 3, a pattern layer 4 and a waxy glaze layer 5, and the surface glaze layer, the pattern layer and the waxy glaze layer are also provided with sunken grains 6, and the sunken grains are obtained by the repulsion of mold ink for ink-jet printing on the surface glaze layer and the waxy glaze layer. The waxy glaze layer is prepared by preparing the waxy glaze material into aqueous waxy glaze slip. The mould ink adopts an organic solvent as a solvent, is an oily ink, can generate repulsion action on aqueous waxy glaze slip and surface glaze layer glaze slip, and can enable the waxy glaze layer to be accumulated on two sides of the sunken texture through the repulsion action, thereby not only forming better 3D stereoscopic effect, but also having better thickness, permeability and fineness, particularly the accumulated waxy glaze has a warm and moist decorative effect like jade.
It should be noted that the layered structure of the waxy 3D tile includes two kinds of recessed textures, and the two kinds of recessed textures are respectively prepared from the mold ink printed on the makeup soil layer and the mold ink printed on the pattern layer, but in an actual product, the tile with a three-dimensional effect is not limited to the layered structure, and may be: the ceramic tile comprises a tile blank layer, a makeup soil layer, a pattern layer and a waxy glaze layer, but a surface glaze layer is not arranged, and mould ink is printed on the pattern layer to form a sunken texture; it may also be: the ceramic tile comprises a tile blank layer, a makeup soil layer, a surface glaze layer, a pattern layer and a wax glaze layer, and only the mould ink is printed on the makeup soil layer to form only one sunken texture. The waxy 3D ceramic tile with the three-dimensional effect can be obtained by the structure, and the difference is only that the path and depth of the texture are different, and the three-dimensional effect is different.
In one embodiment, the mold ink comprises, in mass percent: 38 to 48 percent of waxy glaze, 20 to 30 percent of acrylic resin, 20 to 30 percent of ethyl acetate, 3 to 6 percent of dispersant, 0.1 to 0.2 percent of suspending agent, 0.2 to 0.3 percent of defoaming agent, 0.3 to 0.6 percent of flatting agent and 0.15 percent of pH value regulator. The waxy glaze is a fine powdery raw material, and can improve the dispersibility of the waxy glaze in ink; the acrylic resin can improve the adhesiveness of the ink; the ethyl acetate is an organic solvent and has a repelling effect on aqueous glaze slip, so that concave grains can be formed in the place where the mould ink is printed, and a 3D (three-dimensional) effect is obtained.
In one embodiment, the chemical composition of the overglaze layer comprises, in mass percent: siO 2 2 50～55%、Al 2 O 3 23～28%、CaO 1.5～3.1%、MgO 2.5～3.0%、K 2 O 3.5～4.5%、Na 2 O2.1-4.1%, znO 4.5-6.5%, and trace impurities in balance. The cover glaze layer is prepared from cover glaze layer glaze slip, the cover glaze layer glaze slip takes water as a solvent, sodium methylcellulose and sodium tripolyphosphate are added, and the cover glaze layer glaze slip is water-based glaze slip, so that the cover glaze layer glaze slip can be repelled when oily mould ink is encountered, and two sides of a printing texture of the mould ink are stacked to form an uneven three-dimensional effect.
In one embodiment, the chemical composition of the makeup soil layer comprises, in mass percent: al (Al) 2 O 3 26～32%、SiO 2 55～60%、CaO 1.5～2.3%、MgO 1.3～2.4%、K 2 O 3.5～4.6%、Na 2 O3.8-4.6%, and trace impurities and ignition loss in balance. The makeup clay is high-aluminum and high-silicon makeup clay, has excellent binding property with the green body, and can cover the color and air holes of the green body, so that the decoration effect of the brick surface is better.
Further, the die ink is printed by two times of ink-jet printing, the two times of ink-jet printing are respectively printed on the makeup soil layer and the pattern layer, and the die ink printed on the makeup soil layer can repel the glaze layer to form first concave grains; the mould ink printed on the pattern layer can repel the waxy glaze layer and form second sunken grains. The first concave grains and the second concave grains can be overlapped or dislocated, and can be partially overlapped or dislocated. When overlapping, can obtain the line that the degree of depth is darker, when the dislocation, can form the line of different stereovision, specifically can set for according to actual need to obtain more beautiful decorative effect.
The application also discloses a preparation method of the waxy 3D ceramic tile, which comprises the following steps:
sequentially forming a brick blank layer and a makeup soil layer;
depositing first mould ink on the surface of the makeup soil layer, and forming a glaze layer on the surface of the first mould ink;
and forming a pattern layer on the surface of the overglaze layer, depositing second mould ink on the surface of the pattern layer, forming a waxy glaze layer on the surface of the second mould ink, and sintering to obtain the waxy 3D ceramic tile.
In one embodiment, the method of making comprises the steps of:
the method comprises the following steps: and pressing the green brick.
Step two: and drying the green body, wherein the moisture of the dried green body is controlled to be 0.3-0.5%, and the green body has enough strength, so that the sufficient strength guarantee is provided for the subsequent transmission of the green brick on a glaze line.
Step three: and spraying the make-up clay glaze slip on the blank body.
Step four: the mould ink is printed on the makeup soil for the first time, the printing texture of the mould ink can be designed in advance through a computer, and the mould ink takes a hydrophobic organic matter as a solvent.
Step five: and the green brick enters glaze spraying equipment after passing through the first-time printing mould ink, and is sprayed with surface glaze layer glaze slurry. The glaze spraying equipment is a swing arm type high-pressure glaze spraying cabinet and is provided with 6 high-pressure spray guns, and the pressure of each spray gun is set to be 15-20 Bar; the overglaze layer glaze slip adopts glaze slip with the water content of 40-45 percent, and sodium methyl cellulose and sodium tripolyphosphate are added, so that the overglaze layer glaze slip contains electrolyte, so that the overglaze layer glaze slip has larger hydrophilicity, when the overglaze layer glaze slip contacts the pattern printed with the mould ink, the hydrophilicity and the hydrophobicity of the mould ink repel each other, so that the overglaze layer glaze slip is repelled along the grains of the ink to form concave grains or pits, and meanwhile, the overglaze layer glaze slip forms accumulation on two sides printed with the mould ink to form an uneven structure, thereby having a three-dimensional effect.
Step six: drying the blank body sprayed with the overglaze at the drying temperature of 150-180 ℃ for 5 minutes, and shaping the overglaze as soon as possible by drying.
Step seven: and printing a color pattern on the overglaze layer by an ink-jet printer according to the pattern texture set by the computer. The specific pattern can be set according to actual requirements.
Step eight: and printing the mold ink for the second time according to the pattern set by the computer, wherein the mold ink is the same as the mold ink printed for the first time and is hydrophobic ink, and the printed pattern can be the same as or different from the pattern printed for the first time and can be specifically set according to actual requirements.
Step nine: after the mould ink is printed for the second time, wax glaze slip spraying is carried out, a swing arm type high-pressure glaze spraying cabinet is also adopted, the wax glaze slip takes water as a solvent, the water content of the wax glaze slip is 45-50%, and sodium methylcellulose and sodium tripolyphosphate are added simultaneously, so that sodium ion electrolyte exists in the wax glaze slip, and the wax glaze slip has larger hydrophilicity, so that the wax glaze slip can be repelled when meeting the mould ink printed for the second time, and can be discharged at a place with the mould ink and piled at a place without the mould ink to form concave-convex lines with a three-dimensional effect.
Step ten: and (3) putting the ceramic tile into a kiln to be fired, wherein the firing temperature is 1180-1200 ℃, and the firing time is 40-60 minutes, so that the waxy glaze ceramic tile is obtained.
In a preferred embodiment, in the preparation method of the waxy 3D tile, the printing grayscales of the first printing mold ink and the second printing mold ink are 40 to 100%. Through adjusting the printing gray level, the ceramic tile has proper ink jet amount to obtain lines with proper depth and improve the three-dimensional effect of the ceramic tile.
According to the preparation method of the waxy 3D ceramic tile, through printing the mould ink, the action of the mould ink repelling the overglaze layer and the waxy glaze is utilized, the concave lines can be formed on the tile surface, and then the 3D stereoscopic effect is achieved.
To further illustrate the present invention, a waxy glaze, a waxy 3D tile, and methods of making the same, the following examples are provided.
Example 1
This embodiment is a waxy glaze, including, in parts by weight: 45 parts of first frit, 35 parts of second frit, 10 parts of air knife soil, 4 parts of zinc oxide and 6 parts of dolomite. The raw materials for preparing the first frit comprise, by weight: 16 parts of kaolin, 7 parts of zinc oxide, 5 parts of sodium borate, 30 parts of pyrophyllite, 10 parts of white carbon black, 7 parts of strontium carbonate, 11 parts of sodium carbonate, 14 parts of barium carbonate and 4 parts of wollastonite. The raw materials for preparing the second frit comprise: 23 parts of kaolin, 7 parts of nano-alumina, 12 parts of potassium carbonate, 7 parts of sodium carbonate, 12 parts of spodumene, 8 parts of white carbon black, 6 parts of talc and 33 parts of pyrophyllite. The first frit and the second frit are calcined and melted at the high temperature of 1450 ℃, and then are water quenched and ground to obtain the ceramic material.
Example 2
This embodiment is a waxy glaze, including, in parts by weight: 40 parts of first frit, 40 parts of second frit, 8 parts of air knife soil, 5 parts of zinc oxide and 5 parts of dolomite. The raw materials for preparing the first frit comprise, by weight: 18 parts of kaolin, 6 parts of zinc oxide, 6 parts of sodium borate, 25 parts of pyrophyllite, 12 parts of white carbon black, 5 parts of strontium carbonate, 13 parts of sodium carbonate, 12 parts of barium carbonate and 5 parts of wollastonite. The raw materials for preparing the second frit comprise: 20 parts of kaolin, 8 parts of nano-alumina, 10 parts of potassium carbonate, 8 parts of sodium carbonate, 10 parts of spodumene, 10 parts of white carbon black, 4 parts of talc and 36 parts of pyrophyllite. The first frit and the second frit were prepared in the same manner as in example 1.
Example 3
This embodiment is a waxy glaze, including, in parts by weight: 50 parts of first frit, 30 parts of second frit, 12 parts of air knife soil, 3 parts of zinc oxide and 8 parts of dolomite. The first frit is prepared from the following raw materials in parts by weight: 15 parts of kaolin, 8 parts of zinc oxide, 3 parts of sodium borate, 36 parts of pyrophyllite, 8 parts of white carbon black, 8 parts of strontium carbonate, 10 parts of sodium carbonate, 15 parts of barium carbonate and 3 parts of wollastonite. The raw materials for preparing the second frit comprise: 25 parts of kaolin, 5 parts of nano-alumina, 15 parts of potassium carbonate, 5 parts of sodium carbonate, 15 parts of spodumene, 6 parts of white carbon black, 7 parts of talc and 30 parts of pyrophyllite. The first frit and the second frit were prepared in the same manner as in example 1.
Example 4
The embodiment is a waxy glaze, which comprises the following components in parts by weight: 48 parts of first frit, 38 parts of second frit, 11 parts of air knife soil, 4 parts of zinc oxide and 7 parts of dolomite. The raw materials for preparing the first frit comprise, by weight: 17 parts of kaolin, 7 parts of zinc oxide, 4 parts of sodium borate, 25 parts of pyrophyllite, 9 parts of white carbon black, 6 parts of strontium carbonate, 12 parts of sodium carbonate, 13 parts of barium carbonate and 4 parts of wollastonite. The raw materials for preparing the second frit comprise: 22 parts of kaolin, 6 parts of nano-alumina, 13 parts of potassium carbonate, 6 parts of sodium carbonate, 14 parts of spodumene, 9 parts of white carbon black, 5 parts of talc and 35 parts of pyrophyllite. The first frit and the second frit were prepared in the same manner as in example 1.
Example 5
This embodiment is a wax 3D tile, as shown in fig. 2, the tile includes: the glaze comprises a brick blank layer, a make-up soil layer, a surface glaze layer, a pattern layer and a waxy glaze layer, and further comprises a first texture layer and a second texture layer, wherein the first texture layer is arranged between the make-up soil layer and the surface glaze layer, the second texture layer is arranged between the pattern layer and the waxy glaze layer, the first texture layer is prepared through the repulsion action of mold ink printed on the make-up soil layer and the surface glaze layer, the second texture layer is prepared through the repulsion action of the mold ink printed on the pattern layer and the waxy glaze layer, the mold ink is organic solvent type ink and contains waxy glaze powder as described in example 1, the waxy glaze layer and the surface glaze layer are both made of water-based glaze slurry, and the glaze slurry of the waxy glaze layer is prepared from waxy glaze as described in example 1.
The chemical composition of the makeup soil layer comprises the following components in percentage by mass: al (Al) 2 O 3 26%、SiO 2 60%、CaO 2.3%、MgO 2.4%、K 2 O 4.6%、Na 2 4.6 percent of O, and the balance of trace impurities and ignition loss.
The chemical composition of the overglaze layer comprises the following components in percentage by mass: siO 2 2 50%、Al 2 O 3 28%、CaO 1.5%、MgO 3.0%、K 2 O 3.5%、Na 2 4.1 percent of O, 4.5 percent of ZnO and the balance of proper amount and trace impurities.
The pattern layer is prepared by adopting conventional ceramic ink.
The waxy glaze layer was prepared from the waxy glaze described in example 1.
The mould ink comprises the following components in percentage by mass: 38% of waxy glaze, 30% of acrylic resin, 24.75% of ethyl acetate, 6% of dispersing agent, 0.2% of suspending agent, 0.3% of defoaming agent, 0.6% of leveling agent and 0.15% of pH value regulator. The waxy glaze is the waxy glaze described in example 1, and is ground into fine powder.
The waxy 3D ceramic tile is prepared by the following method: pressing a green brick, drying, spraying the makeup soil, printing mould ink for the first time, spraying overglaze, drying, printing patterns, printing mould ink for the second time, spraying wax glaze and firing. The printing gray scale of the first printing mould ink and the printing gray scale of the second printing mould ink are 60%, the firing temperature of the firing step is 1180 ℃, and the firing time is 60 minutes.
Example 6
This example is a waxy 3D tile, as shown in fig. 3, the layered structure of which is the same as that of example 5, except that: (1) The waxy glaze used was the waxy glaze described in example 2;
(2) The chemical composition of the makeup soil layer comprises the following components in percentage by mass: al (aluminum) 2 O 3 32%、SiO 2 55%、CaO 1.5%、MgO 1.3%、K 2 O 3.5%、Na 2 3.8 percent of O, and the balance of trace impurities and ignition loss;
(3) The chemical composition of the overglaze layer comprises the following components in percentage by mass: siO 2 2 55%、Al 2 O 3 23%、CaO 3.1%、MgO 2.5%、K 2 O 4.5%、Na 2 O2.1%, znO 6.5%, and the balance of reduced and trace impurities;
(4) The mould ink comprises the following components in percentage by mass: 48% of waxy glaze, 20% of acrylic resin, 28.25% of ethyl acetate, 3% of dispersing agent, 0.1% of suspending agent, 0.2% of defoaming agent, 0.3% of flatting agent and 0.15% of pH value regulator. The waxy glaze is the waxy glaze described in example 2, and is ground into fine powder.
The waxy 3D tile described in example 6 was prepared the same as in example 5, except that: the printing gray scale of the die ink is 40%, the firing temperature in the firing step is 1200 ℃, and the firing time is 40 minutes.
Example 7
This example is a waxy 3D tile, as shown in fig. 4, the layered structure of which is the same as that of example 5, except that: (1) The waxy glaze used was the waxy glaze described in example 3;
(2) The chemical composition of the makeup soil layer comprises the following components in percentage by mass: al (aluminum) 2 O 3 28%、SiO 2 58%、CaO 2%、MgO 2%、K 2 O 4%、Na 2 O4 percent, and the balance of trace impurities and ignition loss;
(3) The overglaze layer comprises the following chemical components in percentage by mass: siO 2 2 53%、Al 2 O 3 26%、CaO 2.5%、MgO 2.8%、K 2 O 4.0%、Na 2 3.1 percent of O, 5.5 percent of ZnO and the balance of proper and trace impurities;
(3) The mould ink comprises the following components in percentage by mass: 47.85 percent of waxy glaze, 26 percent of acrylic resin, 20 percent of ethyl acetate, 5 percent of dispersing agent, 0.2 percent of suspending agent, 0.3 percent of defoaming agent, 0.5 percent of flatting agent and 0.15 percent of pH value regulator. The waxy glaze was the waxy glaze of example 3 and was ground to a fine powder.
The waxy 3D tile described in example 7 was prepared the same as in example 5, except that: the printing gray level of the die ink is 80%, the firing temperature in the firing step is 1190 ℃, and the firing time is 50 minutes.
Example 8
This example is a waxy 3D tile, as shown in fig. 5, the layered structure of which is the same as that of example 5 except that: (1) The waxy glaze used was the waxy glaze described in example 4;
(2) The chemical composition of the makeup soil layer comprises the following components in percentage by mass: al (aluminum) 2 O 3 30%、SiO 2 56%、CaO 2.3%、MgO 1.5%、K 2 O 4.2%、Na 2 4.4 percent of O, and the balance of trace impurities and ignition loss;
(3) The overglaze layer comprises the following chemical components in percentage by mass: siO 2 2 55%、Al 2 O 3 25%、CaO 3.0%、MgO 3.0%、K 2 O 4.2%、Na 2 3.8 percent of O, 5.0 percent of ZnO and the balance of proper and trace impurities;
(4) The mould ink comprises the following components in percentage by mass: waxy glaze 44%, acrylic resin 20.95%, ethyl acetate 30%, dispersing agent 4%, suspending agent 0.2%, defoaming agent 0.3%, leveling agent 0.4%, and pH value regulator 0.15%. The waxy glaze was the waxy glaze of example 4 and was ground to a fine powder.
The waxy 3D tile described in example 8 was prepared the same as in example 5, except that: the printing gray level of the die ink is 100%, the firing temperature in the firing step is 1190 ℃, and the firing time is 45 minutes.
Comparative example 1
The comparison is a glaze and a ceramic tile.
A glaze, the basic composition of which is the same as that of example 1, except that the white carbon black in the first frit was replaced with quartz powder having a larger particle size in equal amounts.
A ceramic tile produced according to the method for producing a ceramic tile of example 5, except for the difference from example 5, in which the glaze of example 5 was replaced with the glaze of comparative example 1, and the other components and the production method were not changed, the ceramic tile being as shown in fig. 6.
Comparative example 2
The comparison is a glaze and a ceramic tile.
A glaze, the basic composition of which is the same as in example 1, except that the white carbon black in the second frit is replaced with quartz powder having a coarser particle size in equal amounts.
A ceramic tile, prepared according to the method for preparing a ceramic tile described in example 5, which is different from example 5 in that the glaze described in example 5 is replaced with the glaze described in comparative example 2, and the other components and the preparation method are not changed, and the ceramic tile is obtained as shown in fig. 7.
Comparative example 3
The comparison is a glaze and a ceramic tile.
A glaze, the essential ingredients of which are the same as in example 1, except that the nano-alumina in the second frit was replaced equally with alumina powder having a particle size of 325 mesh.
A ceramic tile, produced according to the method for producing a ceramic tile described in example 5, which is different from example 5 in that the glaze described in example 5 is replaced with the glaze described in comparative example 3, and the other components and the production method are not changed, and the ceramic tile is obtained as shown in fig. 8.
Comparative example 4
The comparison is a glaze and a ceramic tile.
A glaze, the essential ingredients of which are the same as in example 1, except that the white carbon black is added in an amount of 4 parts by weight in the first frit.
A ceramic tile, produced according to the method for producing a ceramic tile described in example 5, which is different from example 5 in that the glaze described in example 5 is replaced with the glaze described in comparative example 4, and the other components and the production method are not changed, and the ceramic tile is obtained as shown in fig. 9.
Comparative example 5
The comparison is a glaze and a ceramic tile.
A glaze, the essential ingredients of which are the same as in example 1, except that the white carbon black is added in an amount of 14 parts by weight in the first frit.
A ceramic tile, produced according to the method for producing a ceramic tile described in example 5, which is different from example 5 in that the glaze described in example 5 is replaced with the glaze described in comparative example 5, and the other components and the production method are not changed, and the ceramic tile is obtained as shown in fig. 10.
Comparative example 6
The comparison is a glaze and a ceramic tile.
A glaze, the essential components of which are the same as in example 1, except that the second frit comprises 10 parts by weight of nano-alumina and 12 parts by weight of white carbon black
A ceramic tile produced according to the method for producing a ceramic tile of example 5, except for the difference from example 5, in which the glaze of example 5 was replaced with the glaze of comparative example 6, and the other components and the production method were not changed, the ceramic tile being as shown in fig. 11.
Comparative example 7
The comparison is a glaze and a ceramic tile.
A glaze, the essential ingredients of which are the same as in example 1, except that the second frit comprises, in parts by weight, 3 parts of nano-alumina and 3 parts of white carbon black
A ceramic tile, produced according to the method for producing a ceramic tile described in example 5, which is different from example 5 in that the glaze described in example 5 is replaced with the glaze described in comparative example 7, and the other components and the production method are not changed, and the ceramic tile is obtained as shown in fig. 12.
Comparative example 8
The comparison is a glaze and a ceramic tile.
A glaze, the essential ingredients of which are the same as in example 1, except that the second frit comprises, in parts by weight, 2 parts of nano-alumina and 15 parts of white carbon black
A ceramic tile, produced according to the method for producing a ceramic tile described in example 5, which is different from example 5 in that the glaze described in example 5 is replaced with the glaze described in comparative example 8, and the other components and the production method are not changed, and the ceramic tile is obtained as shown in fig. 13.
It should be noted that the patterns of the pattern layers in examples 4 to 5 and comparative examples 1 to 8 may be the same or different, and the texture structures of the first texture layer and the second texture layer in each example and each comparative example may be the same or different, and may be specifically selected according to actual needs.
Performance testing
The glazes prepared in examples 1 to 4 and comparative examples 1 to 8 were subjected to a light transmission test and a gloss test, wherein the light transmission test was performed by using a spectrophotometer, and specifically, the light transmission test comprises the following steps: first, the glaze described in examples 1 to 4 and comparative examples 1 to 8 was prepared into a square sample having a thickness of 5mm and a length × width of 5cm × 5cm, and then the light transmittance was measured with a spectrophotometer, and the specific results are shown in table 1. The gloss measurement is carried out according to international standard ISO-2813 or national standard GB/T9754, and is carried out by a WGG60-Y series gloss meter, and the specific test result is shown in Table 1.
Table 1 results of performance testing
As can be seen from table 1, the glazes of examples 1 to 4 have excellent light transmittance at the same thickness, and thus have good permeability even when the thickness of the glaze layer is relatively large, so that the pattern of the pattern layer can be fully demonstrated. Meanwhile, the glossiness of the examples 1 to 4 is lower than that of the comparative examples 1 to 6 and 8, so that the matte effect is better, and the lubricous wax texture can be formed. The light transmittance and gloss of comparative examples 1 to 8 were inferior to those of examples 1 to 8 (except for comparative example 7), and the light transmittance of comparative example 7 was inferior although the matte effect was also obtained. This is because the waxy glaze in examples 1 to 4 contains white carbon black and nano alumina having very small particle size, has good dispersibility, and can react with oxides sufficiently to form a fine glass phase or crystal (as shown in fig. 16, from the SEM image of the surface layer of the waxy glaze, it can be seen that the crystal on the surface is fine and fine, and is distributed in the glass phase, and the glaze has small porosity and dense crystal phase and glass phase structure, which are main reasons for the fine and transparent texture of the glaze), and further has softness and fine texture, and forms a waxy feeling like jade. Meanwhile, the tiles prepared in example 5 and comparative example 1 were observed with a magnifying glass (magnification 150 times), and the observation results are shown in fig. 14 and fig. 15, fig. 14 is an enlarged view of comparative example 1, and fig. 15 is an enlarged view of example 5, and it can be seen from fig. 15 that the number of bubbles is small and the light transmittance is better in example 5, and that the number of bubbles is large and the light transmittance is poor in fig. 14, and thus, the glaze described in the present application forms fewer pores and the light transmittance is better.
Apparent comparison
Observing figures 2-13, comparing glaze materials of examples 5-8 and comparative examples 1-8 to obtain the apparent structure of the ceramic tile, finding that the surface of the ceramic tile of examples 4-8 has textures with different depths, 3D stereoscopic effect, clear and visible patterns and obvious stereoscopic effect, the thickness of the waxy glaze layer on the surface is 0.1-0.35 mm, the ceramic tile is thick and heavy, good in permeability, fine and smooth and has jade texture. The tiles prepared by the glaze materials of comparative examples 1 to 8 have textures with different depths, but have insufficient stereoscopic impression, because the surface glaze materials of the tiles of comparative examples 1 to 8 are different from the waxy glaze materials, the reaction products are different at the same sintering temperature as that of example 5, and the sintering degree is different, so that the depths of the formed sunken textures are different, the surface glossiness is different, the heavy feeling is poor, the texture is rough, and the jade feeling is weak. Therefore, the content of the white carbon black in the first frit raw material and the content of the nano aluminum oxide and the white carbon black in the second frit raw material are key factors influencing the texture and the light transmittance of the glaze wax, too much or too little or no addition of the white carbon black can influence the appearance of the glaze wax effect, and the wax effect can be obtained only by the glaze with specific components and proportions. And the waxy glaze can improve the appearance effect of the ceramic tile, can obtain a heavy feeling and has better permeability and fineness, thereby improving the ornamental value of the ceramic tile.
It should be understood that equivalents and modifications to the invention as described herein may occur to those skilled in the art, and all such modifications and alterations are intended to fall within the scope of the appended claims.
Claims (7)
1. The waxy glaze is characterized by comprising the following components in parts by weight: 40-50 parts of first frit, 30-40 parts of second frit, 8-12 parts of air knife soil, 3-5 parts of zinc oxide and 5-8 parts of dolomite; according to the mass percentage, the preparation raw material of the first frit contains 7.5-12% of white carbon black, and the preparation raw material of the second frit contains 4.6-7.6% of nano alumina and 5.5-9.5% of white carbon black;
the preparation raw materials of the first frit comprise, by weight: 15 to 18 parts of kaolin, 6 to 8 parts of zinc oxide, 3 to 6 parts of sodium borate, 25 to 36 parts of pyrophyllite, 8 to 12 parts of white carbon black, 5 to 8 parts of strontium carbonate, 10 to 13 parts of sodium carbonate, 12 to 15 parts of barium carbonate and 3 to 5 parts of wollastonite;
the second frit comprises the following raw materials in parts by weight: 20 to 25 portions of kaolin, 5 to 8 portions of nano alumina, 10 to 15 portions of potassium carbonate, 5 to 8 portions of sodium carbonate, 10 to 15 portions of spodumene, 6 to 10 portions of white carbon black, 4 to 7 portions of talc and 30 to 36 portions of pyrophyllite.
2. A waxy 3D ceramic tile, which is characterized by comprising a tile blank layer, a makeup soil layer, a surface glaze layer, a pattern layer and a waxy glaze layer which are sequentially stacked, wherein the surface glaze layer, the pattern layer and the waxy glaze layer are also provided with sunken textures, and the waxy glaze layer is prepared from the waxy glaze material as claimed in claim 1.
3. The waxy 3D tile according to claim 2, wherein the texture is produced by the repelling effect of a mold ink on the glaze layer and the waxy glaze layer, the mold ink comprising, in mass percent: 38 to 48 percent of waxy glaze, 20 to 30 percent of acrylic resin, 20 to 30 percent of ethyl acetate, 3 to 6 percent of dispersant, 0.1 to 0.2 percent of suspending agent, 0.2 to 0.3 percent of defoamer, 0.3 to 0.6 percent of flatting agent and 0.15 percent of pH value regulator.
4. The waxy 3D tile according to claim 2 wherein the chemical composition of the overglaze layer comprises, in mass percent: siO 2 2 50～55%、Al 2 O 3 23～28%、CaO 1.5～3.1%、MgO 2.5～3.0%、K 2 O 3.5～4.5%、Na 2 O2.1-4.1%, znO 4.5-6.5%, and the balance of ignition loss and trace impurities.
5. The waxy 3D tile according to claim 2, wherein the chemical composition of the makeup soil layer comprises, in mass percent: al (aluminum) 2 O 3 26～32%、SiO 2 55～60%、CaO 1.5～2.3%、MgO 1.3～2.4%、K 2 O 3.5～4.6%、Na 2 O3.8-4.6%, and trace impurities and ignition loss in balance.
6. A method of making the waxy 3D tile according to any of claims 2-5, comprising the steps of:
sequentially forming a brick blank layer and a makeup soil layer;
depositing first mould ink on the surface of the makeup soil layer, and forming a glaze layer on the surface of the first mould ink;
and forming a pattern layer on the surface of the overglaze layer, depositing second mould ink on the surface of the pattern layer, forming a waxy glaze layer on the surface of the second mould ink, and sintering to obtain the waxy 3D ceramic tile.
7. The preparation method of the waxy 3D tile according to claim 6, wherein the method for depositing the first mold ink and the method for depositing the second mold ink are both inkjet printing methods, and the printing gray levels are both 40-100%; in the firing step, the firing temperature is 1180-1300 ℃, and the firing time is 40-60 minutes.
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| CN106186695A (en) * | 2016-07-14 | 2016-12-07 | 佛山科学技术学院 | A kind of throwing glazed brick introducing superfine oxide raising hardness of glaze surface and preparation method thereof |
| CN111943724A (en) * | 2020-08-11 | 2020-11-17 | 佛山市三水新明珠建陶工业有限公司 | Method for manufacturing matt transparent glazed ceramic chip |
| CN112429969A (en) * | 2020-11-24 | 2021-03-02 | 清远市简一陶瓷有限公司 | Wear-resistant glaze, preparation method thereof and marble ceramic tile |
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| CN106186695A (en) * | 2016-07-14 | 2016-12-07 | 佛山科学技术学院 | A kind of throwing glazed brick introducing superfine oxide raising hardness of glaze surface and preparation method thereof |
| CN111943724A (en) * | 2020-08-11 | 2020-11-17 | 佛山市三水新明珠建陶工业有限公司 | Method for manufacturing matt transparent glazed ceramic chip |
| CN112429969A (en) * | 2020-11-24 | 2021-03-02 | 清远市简一陶瓷有限公司 | Wear-resistant glaze, preparation method thereof and marble ceramic tile |
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Address after: 528061 1st floor, No.18 taobo Avenue, Huaxia Ceramics Expo City, Nanzhuang Town, Chancheng District, Foshan City, Guangdong Province Patentee after: New Pearl Group Co.,Ltd. Patentee after: FOSHAN SANSHUI NEW PEARL CONSTRUCTION CERAMICS INDUSTRIAL Co.,Ltd. Patentee after: New Pearl (Guangdong) New Materials Co.,Ltd. Patentee after: Jiangxi Xinmingzhu Building Materials Co.,Ltd. Patentee after: Hubei new Ming Zhu Green Building Materials Technology Co.,Ltd. Address before: 528061 1st floor, No.18 taobo Avenue, Huaxia Ceramics Expo City, Nanzhuang Town, Chancheng District, Foshan City, Guangdong Province Patentee before: New Pearl Group Co.,Ltd. Patentee before: FOSHAN SANSHUI NEW PEARL CONSTRUCTION CERAMICS INDUSTRIAL Co.,Ltd. Patentee before: GUANGDONG SUMMIT CERAMICS Co.,Ltd. Patentee before: Jiangxi Xinmingzhu Building Materials Co.,Ltd. Patentee before: Hubei new Ming Zhu Green Building Materials Technology Co.,Ltd. |
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