CN109678460B - Preparation method of high-simulation-degree ceramic tile blank - Google Patents

Preparation method of high-simulation-degree ceramic tile blank Download PDF

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CN109678460B
CN109678460B CN201910143244.8A CN201910143244A CN109678460B CN 109678460 B CN109678460 B CN 109678460B CN 201910143244 A CN201910143244 A CN 201910143244A CN 109678460 B CN109678460 B CN 109678460B
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sintering
pug
powder
blank
ceramic tile
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CN109678460A (en
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肖春燕
廖花妹
潘婷
刘畅
李丽芳
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Heyuan Dongyuan Yingpai Ceramics Co. Ltd
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Heyuan Dongyuan Eagle Ceramics Co ltd
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
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    • C04B33/131Inorganic additives
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3281Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof

Abstract

The invention provides a preparation method of a high-simulation-degree ceramic tile blank, which is characterized by comprising the following steps of: the method comprises the following steps: 1) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder; 2) spreading the pug in a grinding tool, then pressing and forming, and sintering at 850-; 3) applying the powder material to the blank of the pug fired in the step 2) to form a powder material layer with fine lines of textures and carrying out HIP treatment; 4) carrying out secondary sintering on the blank obtained in the step 4), wherein the temperature of the secondary sintering is lower than that of the primary sintering; 5) repeating steps 2) -4) at least once; 6) sintering the finally obtained blank at 1200-1300 ℃. The blank obtained by the method has excellent fidelity and strong stereoscopic impression on a longitudinal section.

Description

Preparation method of high-simulation-degree ceramic tile blank
Technical Field
The invention relates to a preparation method of a ceramic tile blank, in particular to a preparation method of a high-simulation ceramic tile blank.
Background
Natural marble has been a stone decorative material sought after by people because of its noble and elegant appearance, however, natural marble as a non-renewable resource has higher and higher exploitation and manufacturing costs, and more artificial marbles are appearing on the market at present in order to meet the increasing demand of people for natural marble and reasonably control manufacturing cost. However, due to poor technology, the artificial marble prepared by the method has unsatisfactory simulation degree and stereoscopic impression, and the fidelity of the marble is greatly influenced.
The Chinese patent with the patent application number of CN201810587557.8 discloses a method for manufacturing ceramic tiles with three-dimensional decorative effect, which comprises the following steps: A. carrying out primary firing on the mud blank with the concave-convex texture on the surface at the temperature of 600-1050 ℃; B. distributing organic penetrating glaze ink and organic penetration assisting agent ink on the green body after the first firing; C. a second firing is carried out at 1150-1250 ℃; D. and polishing and edging to obtain a ceramic tile product. Although the first low-temperature firing is carried out at the temperature of 600-1050 ℃, the air holes in the green brick can be fully opened and then permeation is carried out after the air holes are opened, the permeation glaze ink can diffuse channels among the air holes, the diffusion effect is enhanced, the using amount of the organic ink is reduced, and the diffusion can be more uniform. However, the above method cannot control the distribution and fidelity of the texture in the blank, so that the stereoscopic impression of the longitudinal section is not ideal.
The Chinese patent with the patent application number of CN201510798689.1 discloses a production method of a porcelain tile with a stone-like three-dimensional decorative effect, which comprises the following steps of A, preparing porcelain tile body powder by a conventional method for later use; B. preparing a ceramic brick substrate and a ceramic brick fabric, wherein the adopted ceramic brick substrate and the adopted ceramic brick fabric have the same dry material chemical composition, and are similar to the blank powder in the step A, but the K2O + Na 2O: 6-8% and impurity less than or equal to 4% (all weight percentage); the dry materials of the bottom material are burdened by barren raw materials of feldspar and plastic raw materials of kaolin, but the dry materials of the face material are burdened by barren raw materials of alumina, quartz and feldspar; controlling the fineness of the slurry of the backing material and the slurry of the fabric to be within 0.5 percent of the balance of a 325-mesh sieve, and controlling the specific gravity to be 1.60g/cm 3-1.90 g/cm3, wherein the dry material of the backing material and the auxiliary additive are subjected to wet ball milling to form the slurry meeting the requirements of spraying performance, and the dry material of the fabric and the auxiliary additive are subjected to wet ball milling to form the slurry meeting the requirements of the slurry performance, then are dried to form dry powder, and then are mixed with the printing oil and the auxiliary additive to prepare the printing fabric meeting the printing performance for later use; C. preparing a porcelain brick blank: b, performing multi-tube material distribution on the ceramic tile green body powder prepared in the step A according to the designed pattern texture, then paving the multi-tube material in a die cavity of a brick press, and pressing the ceramic tile green body powder into a ceramic tile green body under the pressure of 20-50 MPa; D. drying the blank: c, drying the ceramic tile green body prepared in the step C in a drying kiln at the temperature of 150-300 ℃; E. pouring base materials: and B, coating the ceramic tile backing material prepared in the step B on the surface of the dried ceramic tile green body by using a glaze pouring process, wherein the weight of the coating backing material in unit area is 400g/m 2-800 g/m2, and the like. Although the method improves the fidelity of the texture to a certain extent through multi-pipe distribution, the method has the advantages that the pigment penetration of the obtained blank is obvious and the distortion degree of the texture of the longitudinal section is high because the heating process parameters are not reasonably optimized.
The above is only for the purpose of assisting understanding of the technical aspects of the present invention, and does not represent an admission that the above is prior art.
Disclosure of Invention
Based on the problem of low fidelity of the existing ceramics, the invention aims to provide a preparation method of a ceramic tile blank with high fidelity, and aims to improve the fidelity and the stereoscopic impression of the ceramic tile.
In order to solve the problems, the invention provides a preparation method of a high-simulation-degree ceramic tile blank, which comprises the following steps:
1) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder;
2) spreading the pug in a grinding tool, then pressing and forming, and sintering at 850-;
3) applying the powder material to the blank of the pug fired in the step 2) to form a powder material layer with fine lines of textures and carrying out HIP treatment;
4) carrying out secondary sintering on the blank obtained in the step 3), wherein the temperature of the secondary sintering is lower than that of the primary sintering;
5) repeating the steps 2) -4) at least once, wherein in the second circulation, firstly, the pug is paved on the green body obtained in the step 4) and then the subsequent treatment is carried out, and in addition, the sintering temperature TN of the Nth time is controlled to be lower than the sintering temperature TN-1 of the Nth time;
6) sintering the finally obtained green body at 1200-1300 ℃, wherein the sintering time is kept above 3-5min/cm, and cm is the thickness of the ceramic tile green body.
Further, the pug comprises: 20-25% of black mud, 2-3% of high alumina stone particles, 17-24% of Longchuan stone powder, 7-10% of Qingyuan stone particles, 2-6% of raw talc, 9-17% of bentonite, 17-30% of potassium-sodium sandstone, 0.25-0.6% of water reducing agent and 0.3-0.5% of zirconium oxide.
Further, the powder lot comprises: 20-25% of black mud, 2-3% of high alumina stone particles, 17-24% of Longchuan stone powder, 7-10% of Qingyuan stone particles, 2-6% of raw talc, 9-17% of bentonite, 17-30% of potassium-sodium sandstone, 0.25-0.6% of water reducing agent and 4-5% of pigment.
Further, the pigment comprises more than one of copper oxide, zinc oxide, titanium oxide and iron oxide.
Further, the number of cycles of the control step 5) is kept at 3 or more.
The invention makes the texture path and width easier to control and closer to the real marble texture in the blank preparation process by respectively preparing the pug and the powder and strictly controlling the component content ratio, and in addition, the longitudinal section fidelity of the blank is further increased by the selection of multilayer paving materials.
The invention carries out sintering treatment after each material spreading, and strictly controls each sintering temperature, thereby effectively preventing the mutual permeation of the powder layer and the mud layer and further avoiding the texture distortion of the longitudinal section of the blank.
Compared with the prior art, the invention has the following beneficial effects: the technical scheme of the invention has unique sintering process control, and the mutual permeation layers are not formed among all the layers of the prepared green body, so that the stereoscopic impression and the texture simulation degree of the longitudinal section of the ceramic tile are greatly improved.
Detailed Description
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of a high-simulation ceramic tile blank comprises the following steps:
1) raw material preparation, wherein the formula of the basic powder is as follows: 20% of black mud, 2% of high alumina stone particles, 17% of Longchuan stone powder, 8% of Qingyuan stone particles, 4% of raw talc, 12% of bentonite, 25% of potassium-sodium sandstone and 0.25% of water reducing agent; the mud material formula comprises basic powder and 0.3 percent of zirconia; the powder formula comprises basic powder and 4% of copper oxide;
2) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder;
3) spreading the pug in a grinding tool, then pressing and molding the pug and sintering the pug at 1000 ℃ for one time;
4) applying the powder material to the blank of the pug fired in the step 3) to form a powder material layer with fine lines of textures and carrying out HIP treatment;
5) carrying out secondary sintering on the blank obtained in the step 4) at 970 ℃;
6) spreading pug on the blank obtained in the step 5), and then carrying out three times of sintering at 950 ℃;
7) applying the blank obtained in the step 6) with a powder layer with fine lines of textures and carrying out HIP treatment;
8) sintering the blank obtained in the step 7) for four times at 900 ℃;
9) and sintering the finally obtained blank at 1200 ℃, wherein the sintering time is kept at 40 min.
According to the blank prepared by the embodiment, the texture distribution is controllable, the phenomenon of mutual permeation does not occur between layers, the texture of the ceramic tile in the longitudinal direction is vivid, and the stereoscopic impression is strong.
Example 2
A preparation method of a high-simulation ceramic tile blank comprises the following steps:
1) raw material preparation, wherein the formula of the basic powder is as follows: 25% of black mud, 3% of high alumina stone particles, 17% of Longchuan stone powder, 10% of Qingyuan stone particles, 5% of raw talc, 14% of bentonite, 18% of potassium-sodium sandstone and 0.6% of water reducing agent; the formula of the pug is basic powder and 0.5 percent of zirconia; the powder formula is basic powder and 5 percent of zinc oxide;
2) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder;
3) spreading the pug in a grinding tool, then pressing and molding the pug and sintering the pug at 950 ℃ for one time;
4) applying the powder material to the blank of the pug fired in the step 3) to form a powder material layer with fine lines of textures and carrying out HIP treatment;
5) carrying out secondary sintering on the blank obtained in the step 4) at 920 ℃;
6) spreading pug on the blank obtained in the step 5), and then carrying out three times of sintering at 880 ℃;
7) applying the blank obtained in the step 6) with a powder layer with fine lines of textures and carrying out HIP treatment;
8) sintering the blank obtained in the step 7) for four times at 850 ℃;
9) and sintering the finally obtained blank at 1300 ℃, wherein the sintering time is kept at 50 min.
According to the blank prepared by the embodiment, the texture distribution is controllable, the phenomenon of mutual permeation does not occur between layers, the texture of the ceramic tile in the longitudinal direction is vivid, and the stereoscopic impression is strong.
Example 3
A preparation method of a high-simulation ceramic tile blank comprises the following steps:
1) raw material preparation, wherein the formula of the basic powder is as follows: 23% of black mud, 2% of bauxite grains, 22% of Longchuan stone powder, 8% of Qingyuan stone grains, 4% of raw talc, 15% of bentonite, 21% of potassium-sodium sandstone and 0.5% of water reducing agent; the formula of the pug is basic powder and 0.4 percent of zirconia; the powder formula is basic powder and 4 percent of titanium oxide;
2) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder;
3) spreading the pug in a grinding tool, then pressing and molding the pug and sintering the pug at 1000 ℃ for one time;
4) applying the powder material to the blank of the pug fired in the step 3) to form a powder material layer with fine lines of textures and carrying out HIP treatment;
5) carrying out secondary sintering on the blank obtained in the step 4) at 960 ℃;
6) spreading pug on the blank obtained in the step 5), and then carrying out three times of sintering at 940 ℃;
7) applying the blank obtained in the step 6) with a powder layer with fine lines of textures and carrying out HIP treatment;
8) sintering the blank obtained in the step 7) for four times at 900 ℃;
9) spreading pug on the blank obtained in the step 8), and then carrying out five times of sintering at 880 ℃;
10) applying a powder layer with fine lines to the blank obtained in the step 9) and carrying out HIP treatment;
11) sintering the blank obtained in the step 10) for six times at 850 ℃;
12) and sintering the finally obtained blank at 1250 ℃ for 50 min.
According to the blank prepared by the embodiment, the texture distribution is controllable, the phenomenon of mutual permeation does not occur between layers, the texture of the ceramic tile in the longitudinal direction is vivid, and the stereoscopic impression is strong.
Example 4
A preparation method of a high-simulation ceramic tile blank comprises the following steps:
1) raw material preparation, wherein the formula of the basic powder is as follows: 23% of black mud, 3% of bauxite grains, 20% of Longchuan stone powder, 9% of Qingyuan stone grains, 6% of raw talc, 9% of bentonite, 23% of potassium-sodium sandstone and 0.25% of water reducing agent; the formula of the pug is basic powder and 0.5 percent of zirconia; the powder formula is basic powder and 5 percent of copper oxide;
2) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder;
3) spreading the pug in a grinding tool, then pressing and molding the pug, and sintering the pug at 930 ℃ for one time;
4) applying the powder material to the blank of the pug fired in the step 3) to form a powder material layer with fine lines of textures and carrying out HIP treatment;
5) carrying out secondary firing on the green body obtained in the step 4) at 900 ℃;
6) spreading pug on the blank obtained in the step 5), and then carrying out three times of sintering at 880 ℃;
7) applying the blank obtained in the step 6) with a powder layer with fine lines of textures and carrying out HIP treatment;
8) sintering the blank obtained in the step 7) for four times at 850 ℃;
9) and sintering the finally obtained blank at 1200 ℃, wherein the sintering time is kept at 60 min.
According to the blank prepared by the embodiment, the texture distribution is controllable, the phenomenon of mutual permeation does not occur between layers, the texture of the ceramic tile in the longitudinal direction is vivid, and the stereoscopic impression is strong.
Comparative example 1
1) Raw material preparation, wherein the formula of the basic powder is as follows: 23% of black mud, 3% of bauxite grains, 20% of Longchuan stone powder, 9% of Qingyuan stone grains, 6% of raw talc, 9% of bentonite, 23% of potassium-sodium sandstone and 0.25% of water reducing agent; the formula of the pug is basic powder and 0.5 percent of zirconia; the powder formula is basic powder and 5 percent of copper oxide;
2) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder;
3) spreading the pug in a grinding tool and then pressing and forming;
4) applying powder on the blank of the pug fired in the step 3) to form a powder layer with fine lines;
5) spreading pugs on the blank obtained in the step 4);
6) applying a powder layer for forming fine lines on the blank obtained in the step 5);
7) and sintering the finally obtained blank at 1200 ℃, wherein the sintering time is kept at 60 min.
According to the blank prepared according to the comparative example, although the texture distribution is controllable, the blank does not adopt a reasonable pre-sintering process, so that a mud layer has an obvious mutual permeation phenomenon between powder layers, the texture distortion of the ceramic tile in the longitudinal direction is obvious, and the stereoscopic impression is poor.
Comparative example 2
A preparation method of a high-simulation ceramic tile blank comprises the following steps:
1) raw material preparation, wherein the formula of the basic powder is as follows: 20% of black mud, 2% of high alumina stone particles, 17% of Longchuan stone powder, 8% of Qingyuan stone particles, 4% of raw talc, 12% of bentonite, 25% of potassium-sodium sandstone and 0.25% of water reducing agent; the mud material formula comprises basic powder and 0.3 percent of zirconia; the powder formula is basic powder and 4 percent of copper oxide;
2) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder;
3) spreading the pug in a grinding tool, then pressing and molding the pug and sintering the pug at 1000 ℃ for one time;
4) applying the powder material to the blank of the pug fired in the step 3) to form a powder material layer with fine lines of textures and carrying out HIP treatment;
5) carrying out secondary sintering on the green body obtained in the step 4) at 1200 ℃;
6) spreading pug on the blank obtained in the step 5), and then carrying out three times of sintering at 1250 ℃;
7) applying the blank obtained in the step 6) with a powder layer with fine lines of textures and carrying out HIP treatment;
8) sintering the blank obtained in the step 7) for four times at 1180 ℃;
9) and sintering the finally obtained blank at 1200 ℃, wherein the sintering time is kept at 40 min.
According to the blank prepared according to the comparative example, although the texture distribution is controllable, the first, second and third layers have obvious mutual permeation phenomenon due to overhigh pre-sintering temperature of the second and third times, the texture distortion of the ceramic tile in the longitudinal direction is obvious, and the stereoscopic impression is poor.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (3)

1. A preparation method of a high-simulation ceramic tile blank is characterized by comprising the following steps: the method comprises the following steps:
1) respectively putting the pug and the powder into a ball mill for ball milling and spray drying to obtain hard powder;
2) spreading the pug in a mold, then pressing and molding the pug, and sintering the pug once at 850-;
3) applying the powder material to the blank of the pug fired in the step 2) to form a powder material layer with fine lines of textures and carrying out HIP treatment;
4) carrying out secondary sintering on the blank obtained in the step 3), wherein the temperature of the secondary sintering is lower than that of the primary sintering;
5) repeating the steps 2) -4) at least once, wherein in the second circulation, firstly, the pug is paved on the green body obtained in the step 4) and then the subsequent treatment is carried out, and in addition, the sintering temperature TN of the Nth time is controlled to be lower than the sintering temperature TN-1 of the Nth time;
6) sintering the finally obtained green body at 1200-1300 ℃, wherein the sintering time is kept above 3-5min/cm, and cm is the thickness of the green body of the ceramic tile;
and controlling the circulation frequency of the step 5) to be 3 times.
2. A method of making according to claim 1, wherein: the pug comprises: 23% of black mud, 2% of bauxite grains, 22% of Longchuan stone powder, 8% of Qingyuan stone grains, 4% of raw talc, 15% of bentonite, 21% of potassium-sodium sandstone, 0.5% of water reducing agent and 0.4% of zirconium oxide.
3. A method of preparation according to claim 1 or 2, characterized in that: the powder material comprises: 23% of black mud, 2% of bauxite grains, 22% of Longchuan stone powder, 8% of Qingyuan stone grains, 4% of raw talc, 15% of bentonite, 21% of potassium-sodium sandstone, 0.5% of water reducing agent and 4% of titanium oxide.
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