Fine concave-convex surface matte ceramic tile and preparation method thereof

文档序号:399310 发布日期:2021-12-17 浏览:14次 中文

阅读说明:本技术 一种精细凹凸面哑光瓷砖及其制备方法 (Fine concave-convex surface matte ceramic tile and preparation method thereof ) 是由 黄春林 谢怡伟 徐雪英 伍志良 朱光耀 陈育昆 仝松贞 傅建涛 宁毓胜 简润桐 于 2021-10-21 设计创作,主要内容包括:本发明提供一种精细凹凸面哑光瓷砖及其制备方法,其中瓷砖包括具有凹凸肌理的坯体层,在坯体层之上设置由长石质钙釉组成的面釉层,在面釉层之上设置图案层,且在图案层之上设置有干粒釉层,其中按质量份计,干粒釉层的釉料包括以下组分:低温釉浆20~50份、高温干粒10~50份、中温干粒50~100份、高温哑光粉30~50份、干粒悬浮剂200~400份,其低温釉浆的比重为1.85-1.95g/ml,本发明独创性的给出了干粒釉层各组分及面釉的组合成分配比方案,且在哑光瓷砖的工艺流程中,采用“精细模具+淋精细干粒釉+刷抛”的制作工艺,将哑光瓷砖进一步调哑,得到一种立体感、层次感好,微光和无光对比反差明显,润滑细腻的瓷砖,增加了整体装饰空间的舒适感。(The invention provides a fine concavo-convex matte ceramic tile and a preparation method thereof, wherein the ceramic tile comprises a blank layer with concavo-convex texture, a glaze layer consisting of feldspar calcium glaze is arranged on the blank layer, a pattern layer is arranged on the glaze layer, and a dry particle glaze layer is arranged on the pattern layer, wherein the glaze of the dry particle glaze layer comprises the following components in parts by mass: the invention provides a low-temperature glaze slip, a high-temperature dry grain, a medium-temperature dry grain, a high-temperature matte powder and a dry grain suspending agent, wherein the low-temperature glaze slip comprises 20-50 parts of the low-temperature glaze slip, 10-50 parts of the high-temperature dry grain, 50-100 parts of the medium-temperature dry grain, 30-50 parts of the high-temperature matte powder and 200-400 parts of the dry grain suspending agent, and the specific gravity of the low-temperature glaze slip is 1.85-1.95 g/ml.)

1. The fine concavo-convex matte ceramic tile is characterized by comprising a blank layer (1) with concavo-convex texture, wherein a overglaze layer (2) consisting of feldspar calcium glaze is arranged on the blank layer (1), a pattern layer (3) is arranged on the overglaze layer (2), and a dry grain glaze layer (4) is arranged on the pattern layer (3), wherein the glaze of the dry grain glaze layer (4) comprises the following main components in parts by mass:

2. the fine uneven-surface matte ceramic tile according to claim 1, wherein the specific gravity of the low-temperature glaze slip is 1.85-1.95 g/ml.

3. The fine concavo-convex matte ceramic tile according to claim 2, wherein the low-temperature glaze slip comprises the following components in percentage by mass:

and the sum of the mass percentages of the components is 100 percent.

4. The fine concavo-convex matte ceramic tile according to claim 1, wherein the particle mesh number of the high-temperature dry particles is 100-300 meshes, and the high-temperature dry particles comprise the following components in percentage by mass:

and the sum of the mass percentages of the components is 100 percent.

5. The fine concavo-convex surface matte ceramic tile according to claim 1, wherein the particle mesh number of the medium-temperature dry particles is 100-250 meshes, and the medium-temperature dry particles comprise the following components in percentage by mass:

and the sum of the mass percentages of the components is 100 percent.

6. The fine concavo-convex matte ceramic tile according to claim 1, wherein the particle mesh number of the high-temperature matte powder is less than 300 meshes, and the high-temperature matte powder comprises the following components in percentage by mass:

and the sum of the mass percentages of the components is 100 percent.

7. The fine concavo-convex surface matte ceramic tile as claimed in claim 1, wherein the dry particle suspending agent comprises the following main components in parts by weight:

8. a fine embossed surface matt ceramic tile according to claim 1 wherein the glaze of the cover glaze layer (2) comprises the following components in mass percent:

and the sum of the mass percentages of the components is 100 percent.

9. A preparation method of a fine concave-convex surface matte ceramic tile is characterized by comprising the following steps:

step 1: preparing blank powder: ball-milling according to a conventional blank formula to obtain slurry, and granulating the slurry in a spray drying tower to obtain powder;

step 2: pressing and forming a fine concave-convex surface blank: pressing and molding the powder obtained in the step 1 on a press to obtain a green body;

and step 3: drying the green body in a drying kiln: sending the green body obtained in the step 2 into a drying kiln for drying at the drying temperature of 180-230 ℃ for 60-80 min to obtain a dried green body, wherein the water content of the dried green body is controlled to be 0.3-0.6%;

and 4, step 4: spraying surface glaze: and (3) applying the overglaze glaze material on the surface of the dried blank obtained in the step (3) by spraying through a bell jar, wherein the glaze amount is 375-440 g/m2The specific gravity is 1.85-1.95g/ml, and the flow rate is 30-40 s; the overglaze material composition is as defined in claim 8;

and 5: ink-jet printing pattern color: printing the pattern on the brick surface sprayed with the glaze in the step 4 by ink jet;

step 6: spraying dry granular glaze: and (3) applying the dry granular glaze material on the brick surface sprayed with the pattern in the step (5) by spraying through a bell jar, wherein the glaze amount of the process parameter of spraying is 280-340 g/m2The specific gravity is 1.35-1.45 g/ml; the dry particle glaze material has the composition as described in any one of claims 1 to 7;

and 7: firing in a kiln: firing the semi-finished product obtained in the step 6 in a kiln at the firing temperature of 1190-1220 ℃ for 60-70 min;

and 8: brushing and polishing by a polishing machine: and (3) brushing and polishing the product obtained in the step (7) on a polishing machine, wherein the specification of the grinding blocks is 38 x 9.5 x 14.5mm, the distribution condition of the grinding blocks is that the grinding blocks are 7 groups of silicon carbide matte fiber brushes with 120 meshes and 6 groups of silicon carbide matte fiber brushes with 150 meshes, and the brushing and polishing time is 2-5 min.

10. The method for preparing fine concavo-convex matte ceramic tiles according to claim 9, wherein the mould used in the pressing process in the step 2 is PETG material which is carved with fine concavo-convex natural texture by a laser carving machine, the width of the lines of the concavo-convex natural texture is 0.04-0.1 mm, and the depth or height of the lines is 0.05-1.1 mm.

Technical Field

The invention relates to the field of ceramic tiles, in particular to a fine concave-convex matte ceramic tile and a preparation method thereof.

Background

Investigation shows that the long-term invasion of various light pollutions in the surrounding environment is one of the main reasons that the myopia rate of teenagers in China is high at present, and the investigation also shows that after the people continuously watch television for several hours, the vision of the people is temporarily reduced by 30 percent, so that in a living environment with smooth walls and floors, light reflection generated by the smooth walls and the floors can stimulate retina and exceed the coordination of eyes, the eyes are fatigued, and even the visual function is reduced. Therefore, in order to minimize light pollution at home, smooth tiles need to be replaced by matt tiles (the glossiness is less than or equal to 35 degrees), and after specular reflection light of the smooth tiles is replaced by diffuse reflection light, the phenomena of dazzling and dazzling are avoided, and a stable, heavy and elegant feeling can be presented indoors.

The existing matte ceramic tile after improvement is improved to a certain extent, but the glossiness of the existing matte ceramic tile is closer to that of a soft-light ceramic tile, the existing matte ceramic tile is not matte enough, the existing matte ceramic tile needs to be further improved and adjusted to be matte, in the process flow of the existing matte ceramic tile, a spraying method is mostly adopted when dry granular glaze is applied, the method is easy to fog, further harm can be caused to the breathing of workers, and meanwhile, the maintenance of the on-site sanitary environment is not facilitated. For example, in "matte dry-grain glazed tile and preparation method thereof" (authorization notice number CN108911701B), it provides a tile blank, and a ground glaze and a dry-grain glaze sequentially disposed on the surface of the tile blank, wherein the ground glaze comprises, by mass: SiO 22 40-55%、Al2O3 10-15%、CaO 8-10%、MgO 5-8%、ZnO 10-15%、K2O 4-6%、Na21-3% of O and 1-3% of BaO; the dry granular glaze comprises, by weight, 40-50 parts of dry granules, 10-20 parts of protective glaze,1-3 parts of kaolin slurry, 0.5-1.5 parts of calcined talc slurry, 1-3 parts of additive, 90-110 parts of suspending agent and 0.05-0.1 part of ink discharging agent; wherein, the dry granules comprise the following components in percentage by mass: al (Al)2O3 5-15%、SiO2 40-55%、CaO 10-18%、K2O 5-10%、MgO 5-12%、BaO4-10%、ZnO 2-5%、RuO2 0.1-0.5%、V2O5 0.1-0.5%、Bi2O30.1-0.5% and TiO20.1 to 0.5 percent; the protective glaze comprises 59-65% of transparent glaze powder, 0.2-0.5% of sodium carboxymethylcellulose, 0.2-0.4% of sodium tripolyphosphate, 1-2% of aluminum chloride, 1-2% of aluminum sulfate, 1-2% of potassium aluminum sulfate dodecahydrate and 30-36% of water by mass percent; the transparent glaze powder comprises Al in percentage by mass2O3 10%、SiO2 52%、CaO 15%、K2O 8%、MgO 5%、BaO 4.5%、ZnO 5%、Lu2O30.5 percent; the patent also provides a preparation method of the matte dry particle glazed tile, which comprises the following steps: A. the free water in the green bricks which are pressed by the press is removed through primary drying, and the moisture content in the green bricks is controlled to be less than 0.5 percent of the total mass of the green bricks; spraying water mist on the surface of the green brick after the green brick is discharged from the drying kiln; B. then spraying base glaze on the surface of the blank, then using an ink jet printer to spray and paint patterns, and drying through a secondary drying kiln; C. spraying dry granular glaze, drying for the third time in a drying kiln, and firing for 60-70min at 1170-1185 ℃ to obtain a semi-finished product; D. and (4) grinding the semi-finished product, combining the semi-finished product with a fiber polishing module for soft polishing, checking the quality and packaging to obtain the finished product.

The product of the existing scheme still has the problem of insufficient glossiness, the matte performance of the product still cannot meet the practical use requirement, and further improvement or alternative schemes are urgently needed.

Disclosure of Invention

The technical problem to be solved by the invention is to provide the fine concave-convex surface matte ceramic tile, and the matte ceramic tile is further subjected to matte adjustment by adopting a manufacturing process of fine mold, fine dry grain glaze spraying and brushing and polishing.

The technical means adopted by the invention are as follows:

the utility model provides a fine unsmooth face matt ceramic tile, includes the body layer that has unsmooth texture, sets up the overglaze layer of constituteing by the feldspar matter calcium glaze on the body layer, sets up the pattern layer on the overglaze layer, and is provided with dry grain glaze layer on the pattern layer, wherein according to the mass fraction, the glaze on dry grain glaze layer includes following main component: 20-50 parts of low-temperature glaze slip, 10-50 parts of high-temperature dry particles, 50-100 parts of medium-temperature dry particles, 30-50 parts of high-temperature matte powder and 200-400 parts of dry particle suspending agent.

Preferably, the specific gravity of the low-temperature glaze slip is 1.85-1.95 g/ml.

Preferably, the low-temperature glaze slip comprises the following components in percentage by mass: SiO 2248~51%、AI2O318~21%、K2O 0.5~2%、Na22-4% of O, 12-14% of CaO, 2-3% of MgO, 4-6% of ZnO, 5-7% of BaO, and less than or equal to 4% of causticity, wherein the sum of the mass percentages of the components is 100%. The low-temperature glaze slip is mainly used for adjusting the lubricating texture of dry granular glaze, can generate a filling effect in gaps between dry granules, further improves the internal structure of the dry granular glaze, enables the lubricating texture of the glaze surface to be better and greatly improves the anti-fouling capability of products.

Preferably, the high-temperature dry granules are high-temperature matte transparent dry granules, the particle mesh number of the high-temperature dry granules is 100-300 meshes, and the high-temperature dry granules comprise the following components in percentage by mass: SiO 2244~47%、AI2O318~21%、K2O 2~4%、Na2O 3~5%、CaO 4~7%、MgO 1~3%、ZnO 4~6%、BaO 12~14%、SrO24-7%, the ignition loss is less than or equal to 1%, and the sum of the mass percentages of the components is 100%.

Preferably, the medium-temperature dry granules are medium-temperature slightly bright transparent dry granules, the particle mesh number of the medium-temperature dry granules is 100-250 meshes, and the medium-temperature dry granules comprise the following components in percentage by mass: SiO 2248~51%、AI2O319~21%、K2O 2~4%、Na2O 3~4%、CaO 5~6%、MgO 1~2%、ZnO 7~9%、BaO 0.1~0.5%、SrO26-7%, the ignition loss is less than or equal to 2%, and the sum of the mass percentages of the components is 100%.

Preferably, the high-temperature matte powder has a particle mesh number of less than 300 meshes, and comprises the following components in percentage by mass: SiO 2238~42%、AI2O318~21%、K2O 1~3%、Na2O 4~6%、CaO 1~3%、MgO 0.5~1%、ZnO 16~19%、BaO 6~9%、SrO26-9%, the ignition loss is less than or equal to 1%, and the sum of the mass percentages of the components is 100%. The high-temperature matte powder is mainly used for adjusting the temperature and the glossiness of a formula.

Preferably, the dry particle suspending agent is viscous, and comprises the following main components in parts by weight: 20-30 parts of methyl glycol, 20-30 parts of sodium carboxymethylcellulose, 2-3 parts of sodium metaphosphate and 10-40 parts of water.

The dry particle suspending agent can enable large and small particles of dry particles to be completely suspended and dispersed in the dry particle suspending agent, and can improve the overall suspensibility and flowability of the dry particles.

The matching application of the dry particle types in the dry particle glaze and the selection of the components and the dosage can obtain a product with excellent performance and better texture effect, wherein, especially SrO2The addition of the (C) can improve the wear resistance and toughness of the dry granules and reduce the problem that the dry granules have large granular brittleness and are easy to break.

Preferably, the glaze of the overglaze layer comprises the following components in percentage by mass: SiO 2257~60%、AI2O326~28%、K2O 2~3%、Na2O 3~5%、CaO 0.5~1.5%、MgO 0~0.5%、ZnO 0.1~0.3%、BaO 0.1~0.4%、ZrO24-6%, the ignition loss is less than or equal to 6%, and the sum of the mass percentages of the components is 100%.

A preparation method of a fine concave-convex surface matte ceramic tile comprises the following steps:

step 1: preparing blank powder: ball-milling according to a conventional blank formula to obtain slurry, and granulating the slurry in a spray drying tower to obtain powder with certain grain composition and water;

step 2: pressing and forming a fine concave-convex surface blank: pressing and molding the powder obtained in the step 1 on a press to obtain a green body;

and step 3: drying the green body in a drying kiln: sending the green body obtained in the step 2 into a drying kiln for drying at the drying temperature of 180-230 ℃ for 60-80 min to obtain a dried green body, wherein the water content of the dried green body is controlled to be 0.3-0.6%;

and 4, step 4: spraying surface glaze: and (3) applying the overglaze glaze material on the surface of the dried blank obtained in the step (3) by spraying through a bell jar, wherein the glaze amount is 375-440 g/m2The specific gravity is 1.85-1.95g/ml, and the flow rate is 30-40 s; the overglaze glaze material comprises the following components in percentage by mass: SiO 2257~60%、AI2O326~28%、K2O 2~3%、Na2O 3~5%、CaO 0.5~1.5%、MgO 0~0.5%、ZnO 0.1~0.3%、BaO 0.1~0.4%、ZrO24-6%, the ignition loss is less than or equal to 6%, and the sum of the mass percentages of the components is 100%;

wherein, the selection of the blank body with the fine concave-convex surface in the step 2 lays a foundation for the whole effect of the fine concave-convex surface matte ceramic tile and simultaneously ensures the basic physical properties of the product, and on the basis, the overglaze is applied in the step 4, wherein K in overglaze components2O、Na2O, CaO has fluxing action, CaO can enhance the surface hardness and wear resistance of the overglaze, and the selection of the components and proportion of the overglaze ensures that the pattern printed by ink-jet printing can obtain better and clear effect, and provides good color development capability and effect for the ink-jet printed pattern.

And 5: ink-jet printing pattern color: printing the pattern on the brick surface sprayed with the glaze in the step 4 by ink jet; the patterns can be lyme stone patterns, marble patterns, cement patterns and sandstone patterns;

step 6: spraying dry granular glaze: and (3) applying the dry granular glaze material on the brick surface sprayed with the pattern in the step (5) by spraying through a bell jar, wherein the glaze amount of the process parameter of spraying is 280-340 g/m2The specific gravity is 1.35-1.45 g/ml; the overglaze material comprises the following main components in parts by weight: 20-50 parts of low-temperature glaze slip, 10-50 parts of high-temperature dry particles, 50-100 parts of medium-temperature dry particles, 30-50 parts of high-temperature matte powder and 200-400 parts of dry particle suspending agent; wherein the specific gravity of the low-temperature glaze slip is 1.85-1.95 g/ml;the low-temperature glaze slip comprises the following components in percentage by mass: SiO 2248~51%、AI2O318~21%、K2O 0.5~2%、Na22-4% of O, 12-14% of CaO, 2-3% of MgO, 4-6% of ZnO, 5-7% of BaO, and less than or equal to 4% of causticity, wherein the sum of the mass percentages of the components is 100%; the high-temperature dry granules are high-temperature matte transparent dry granules, the particle mesh number of the high-temperature dry granules is 100-300 meshes, and the high-temperature dry granules comprise the following components in percentage by mass: SiO 2244~47%、AI2O318~21%、K2O 2~4%、Na2O 3~5%、CaO 4~7%、MgO 1~3%、ZnO 4~6%、BaO 12~14%、SrO24-7%, wherein the ignition loss is less than or equal to 1%, and the sum of the mass percentages of the components is 100%; the medium-temperature dry granules are medium-temperature slightly bright transparent dry granules, the particle mesh number of the medium-temperature dry granules is 100-250 meshes, and the medium-temperature dry granules comprise the following components in percentage by mass: SiO 2248~51%、AI2O319~21%、K2O 2~4%、Na2O 3~4%、CaO 5~6%、MgO 1~2%、ZnO 7~9%、BaO 0.1~0.5%、SrO26-7%, the ignition loss is less than or equal to 2%, and the sum of the mass percentages of the components is 100%; the particle mesh number of the high-temperature matte powder is less than 300 meshes, and the high-temperature matte powder comprises the following components in percentage by mass: SiO 2238~42%、AI2O318~21%、K2O 1~3%、Na2O 4~6%、CaO 1~3%、MgO 0.5~1%、ZnO 16~19%、BaO 6~9%、SrO26-9%, the ignition loss is less than or equal to 1%, and the sum of the mass percentages of the components is 100%; the dry particle suspending agent is sticky, and comprises the following main components in parts by weight: 20-30 parts of methyl glycol, 20-30 parts of sodium carboxymethylcellulose, 2-3 parts of sodium metaphosphate and 10-40 parts of water;

and 7: firing in a kiln: firing the semi-finished product obtained in the step 6 in a kiln at the firing temperature of 1190-1220 ℃ for 60-70 min;

and 8: brushing and polishing by a polishing machine: and (3) brushing and polishing the product obtained in the step (7) on a polishing machine, wherein the specification of the grinding blocks is 38 x 9.5 x 14.5mm, the distribution condition of the grinding blocks is that the grinding blocks are 7 groups of silicon carbide matte fiber brushes with 120 meshes and 6 groups of silicon carbide matte fiber brushes with 150 meshes, and the brushing and polishing time is 2-5 min.

And further, edging, quality testing, packaging and warehousing products obtained through the steps 1-8.

Preferably, the mold used in the pressing process in step 2 is a PETG material which has been engraved with a laser engraving machine to have a fine concavo-convex natural texture having a line width of 0.04 to 0.1mm and a line depth or height of 0.05 to 1.1 mm.

The PETG material is amorphous copolyester, is high-temperature resistant, has outstanding toughness and high impact strength which is 3-10 times of that of modified polyacrylate, has a wide processing range, high mechanical strength and excellent flexibility, and is more favorable for engraving fine concave-convex natural texture on the surface.

The invention has the beneficial effects that:

(1) in the selection of the mould, a novel high-molecular polyester material PETG is selected, so that the high-molecular polyester material PETG has high mechanical strength and excellent flexibility, fine concave-convex natural textures are more favorably engraved on the surface of the mould, a foundation is laid for the overall effect of the fine concave-convex matte ceramic tile, and the basic physical properties of the product are ensured;

(2) through the creative selection of the components and the proportion of the overglaze, the pattern printed by ink-jet printing can obtain a clearer effect, and meanwhile, good color development capability and effect are provided for the ink-jet printed pattern;

(3) further improving the matching application of dry particle types such as high-temperature dry particles in dry particle glaze, medium-temperature dry particles, low-temperature glaze slip and the like, and the selection of components and dosage, so that the stereoscopic impression and the layering sense of the ceramic tile are better, and a product with superior performance and better texture effect is obtained;

(4) the gloss of the product obtained by the invention is 5-9 degrees after brushing and polishing, the contrast between glimmer light and dull light is obvious visually, the product is quiet and comfortable, the surface is shallow and concave, the surface has fine touch, and the product is anti-skid, wear-resistant and anti-fouling.

Drawings

FIG. 1 is a schematic structural view of a fine concavo-convex matte ceramic tile of the present invention;

fig. 2-3 are photographs of the appearance of the product of the present invention.

Wherein, 1-a body layer, 2-a surface glaze layer, 3-a pattern layer and 4-a dry grain glaze layer.

Detailed Description

If not specifically stated, the percentage contents related in the scheme are mass percentage contents, the proportions are mass proportions, and the parts of the related components are mass parts.

The invention provides a fine concavo-convex surface matte ceramic tile, as shown in figure 1, which comprises a blank layer 1 with concavo-convex texture, a glaze layer 2 consisting of feldspar calcium glaze is arranged on the blank layer 1, a pattern layer 3 is arranged on the glaze layer 2, and a dry particle glaze layer 4 is arranged on the pattern layer 3, wherein the glaze of the dry particle glaze layer comprises the following main components in parts by mass: 20-50 parts of low-temperature glaze slip, 10-50 parts of high-temperature dry particles, 50-100 parts of medium-temperature dry particles, 30-50 parts of high-temperature matte powder and 200-400 parts of dry particle suspending agent. In one embodiment, the specific gravity of the low-temperature glaze slip is 1.85-1.95 g/ml. In one embodiment, the low-temperature glaze slip comprises the following components in percentage by mass: SiO 2248~51%、AI2O318~21%、K2O 0.5~2%、Na22-4% of O, 12-14% of CaO, 2-3% of MgO, 4-6% of ZnO, 5-7% of BaO, and less than or equal to 4% of causticity, wherein the sum of the mass percentages of the components is 100%. In one embodiment, the high-temperature dry granules are high-temperature matte transparent dry granules, the particle mesh number of the high-temperature dry granules is 100-300 meshes, and the high-temperature dry granules comprise the following components in percentage by mass: SiO 2244~47%、AI2O318~21%、K2O 2~4%、Na2O 3~5%、CaO 4~7%、MgO 1~3%、ZnO 4~6%、BaO 12~14%、SrO24-7%, the ignition loss is less than or equal to 1%, and the sum of the mass percentages of the components is 100%. In one embodiment, the medium-temperature dry granules are medium-temperature slightly bright transparent dry granules, the particle mesh number of the medium-temperature dry granules is 100-250 meshes, and the medium-temperature dry granules are counted by mass percentThe warm dry granules comprise the following components: SiO 2248~51%、AI2O319~21%、K2O 2~4%、Na2O 3~4%、CaO 5~6%、MgO 1~2%、ZnO 7~9%、BaO 0.1~0.5%、SrO26-7%, the ignition loss is less than or equal to 2%, and the sum of the mass percentages of the components is 100%. In one embodiment, the high-temperature matte powder has a particle mesh number of less than 300 meshes, and comprises the following components in percentage by mass: SiO 2238~42%、AI2O318~21%、K2O 1~3%、Na2O 4~6%、CaO 1~3%、MgO 0.5~1%、ZnO 16~19%、BaO 6~9%、SrO26-9%, the ignition loss is less than or equal to 1%, and the sum of the mass percentages of the components is 100%. In one embodiment, the dry particle suspending agent is viscous, and comprises the following main components in parts by weight: 20-30 parts of methyl glycol, 20-30 parts of sodium carboxymethylcellulose, 2-3 parts of sodium metaphosphate and 10-40 parts of water. In one embodiment, the glaze of the overglaze layer comprises the following components in percentage by mass: SiO 2257~60%、AI2O326~28%、K2O 2~3%、Na2O 3~5%、CaO 0.5~1.5%、MgO 0~0.5%、ZnO 0.1~0.3%、BaO 0.1~0.4%、ZrO24-6%, the ignition loss is less than or equal to 6%, and the sum of the mass percentages of the components is 100%.

The photographs of the appearance of the present invention are shown in fig. 2 and 3.

The preparation method of the fine concave-convex surface matte ceramic tile comprises the following steps:

step 1: preparing blank powder: ball-milling according to a conventional blank formula to obtain slurry, and granulating the slurry in a spray drying tower to obtain powder with certain grain composition and water;

step 2: pressing and forming a fine concave-convex surface blank: pressing and molding the powder obtained in the step 1 on a press to obtain a green body;

and step 3: drying the green body in a drying kiln: sending the green body obtained in the step 2 into a drying kiln for drying at the drying temperature of 180-230 ℃ for 60-80 min to obtain a dried green body, wherein the water content of the dried green body is controlled to be 0.3-0.6%;

and 4, step 4: spraying surface glaze: and (3) applying the overglaze glaze material on the surface of the dried blank obtained in the step (3) by spraying through a bell jar, wherein the glaze amount is 375-440 g/m2The specific gravity is 1.85-1.95g/ml, and the flow rate is 30-40 s; the overglaze glaze material comprises the following components in percentage by mass: SiO 2257~60%、AI2O326~28%、K2O 2~3%、Na2O 3~5%、CaO 0.5~1.5%、MgO 0~0.5%、ZnO 0.1~0.3%、BaO 0.1~0.4%、ZrO24-6%, the ignition loss is less than or equal to 6%, and the sum of the mass percentages of the components is 100%;

and 5: ink-jet printing pattern color: printing the pattern on the brick surface sprayed with the glaze in the step 4 by ink jet; the patterns can be lyme stone patterns, marble patterns, cement patterns and sandstone patterns;

step 6: spraying dry granular glaze: and (3) applying the dry granular glaze material on the brick surface sprayed with the pattern in the step (5) by spraying through a bell jar, wherein the glaze amount of the process parameter of spraying is 280-340 g/m2The specific gravity is 1.35-1.45 g/ml; the overglaze material comprises the following main components in parts by weight: 20-50 parts of low-temperature glaze slip, 10-50 parts of high-temperature dry particles, 50-100 parts of medium-temperature dry particles, 30-50 parts of high-temperature matte powder and 200-400 parts of dry particle suspending agent; wherein the specific gravity of the low-temperature glaze slip is 1.85-1.95 g/ml; the low-temperature glaze slip comprises the following components in percentage by mass: SiO 2248~51%、AI2O318~21%、K2O 0.5~2%、Na22-4% of O, 12-14% of CaO, 2-3% of MgO, 4-6% of ZnO, 5-7% of BaO, and less than or equal to 4% of causticity, wherein the sum of the mass percentages of the components is 100%; the high-temperature dry granules are high-temperature matte transparent dry granules, the particle mesh number of the high-temperature dry granules is 100-300 meshes, and the high-temperature dry granules comprise the following components in percentage by mass: SiO 2244~47%、AI2O318~21%、K2O 2~4%、Na2O 3~5%、CaO 4~7%、MgO 1~3%、ZnO 4~6%、BaO 12~14%、SrO24-7%, wherein the ignition loss is less than or equal to 1%, and the sum of the mass percentages of the components is 100%; medium temperature dry granules are medium temperature slightly bright lightThe transparent dry granules have the particle mesh number of 100-250 meshes, and the medium-temperature dry granules comprise the following components in percentage by mass: SiO 2248~51%、AI2O319~21%、K2O 2~4%、Na2O 3~4%、CaO 5~6%、MgO 1~2%、ZnO 7~9%、BaO 0.1~0.5%、SrO26-7%, the ignition loss is less than or equal to 2%, and the sum of the mass percentages of the components is 100%; the particle mesh number of the high-temperature matte powder is less than 300 meshes, and the high-temperature matte powder comprises the following components in percentage by mass: SiO 2238~42%、AI2O318~21%、K2O 1~3%、Na2O 4~6%、CaO 1~3%、MgO 0.5~1%、ZnO 16~19%、BaO 6~9%、SrO26-9%, the ignition loss is less than or equal to 1%, and the sum of the mass percentages of the components is 100%; the dry particle suspending agent is sticky, and comprises the following main components in parts by weight: 20-30 parts of methyl glycol, 20-30 parts of sodium carboxymethylcellulose, 2-3 parts of sodium metaphosphate and 10-40 parts of water;

and 7: firing in a kiln: firing the semi-finished product obtained in the step 6 in a kiln at the firing temperature of 1190-1220 ℃ for 60-70 min;

and 8: brushing and polishing by a polishing machine: and (3) brushing and polishing the product obtained in the step (7) on a polishing machine, wherein the specification of the grinding blocks is 38 x 9.5 x 14.5mm, the distribution condition of the grinding blocks is that the grinding blocks are 7 groups of silicon carbide matte fiber brushes with 120 meshes and 6 groups of silicon carbide matte fiber brushes with 150 meshes, and the brushing and polishing time is 2-5 min.

And then, edging, quality inspection, packaging and warehousing are carried out on the product obtained after the steps 1-8.

In one embodiment, the mold used in the pressing process in step 2 is a PETG material which has been engraved with a laser engraving machine to have a fine concavo-convex natural texture with a line width of 0.04-0.1 mm and a line depth or height of 0.05-1.1 mm.

And according to the above embodiments, the following specific examples are proposed:

example 1:

the preparation method of the fine concave-convex surface matte ceramic tile comprises the following process flows:

step 1: preparing blank powder: ball-milling according to a conventional blank formula to obtain slurry, and granulating the slurry in a spray drying tower to obtain powder with certain grain composition and water;

step 2: pressing and forming a fine concave-convex surface blank: pressing and molding the powder obtained in the step 1 on a press to obtain a green body, wherein the pressed die is a PETG material which is carved into fine concave-convex natural texture by a laser engraving machine;

and step 3: drying the green body in a drying kiln: conveying the green body obtained in the step 2 into a drying kiln for drying at the drying temperature of 190 ℃ for 70min to obtain a dried green body, wherein the water content of the dried green body is controlled to be 0.4%;

and 4, step 4: spraying surface glaze: and (3) applying the overglaze glaze material on the surface of the dried blank obtained in the step (3) by spraying through a bell jar, wherein the glaze amount is 390g/m2The specific gravity is 1.90g/ml, and the flow rate is 35 s; the overglaze glaze material comprises the following components in percentage by mass: SiO 2257.5%、AI2O326.2%、K2O 2.45%、Na2O 3.55%、CaO 0.65%、MgO 0.25%、ZnO 0.3%、BaO 0.25%、ZrO24.55 percent and 4.3 percent of scorch, wherein the sum of the mass percent of the components is 100 percent;

and 5: ink-jet printing pattern color, namely ink-jet printing patterns such as lyme stone patterns, marble patterns, cement patterns, sandstone patterns and the like on the brick surface sprayed with the glaze in the step 4;

step 6: and (3) spraying dry granular glaze, namely spraying the dry granular glaze material on the surface of the brick sprayed with the pattern in the step (5) by using a bell jar, wherein the spraying process parameter glaze amount is 290g/m2The specific gravity is 1.38 g/ml; the overglaze material comprises the following main components in parts by weight: 30 parts of low-temperature glaze slip, 15 parts of high-temperature dry particles, 85 parts of medium-temperature dry particles, 35 parts of high-temperature matte powder and 220 parts of dry particle suspending agent, wherein the specific gravity of the low-temperature glaze slip is 1.90 g/ml. The low-temperature glaze slip comprises the following components in percentage by mass: SiO 2249.08%、AI2O319.19%、K2O 0.68%、Na2O 2.61%、CaO 12.63%、MgO 2.46%、ZnO 4.39 percent of BaO, 5.91 percent of BaO and 3.05 percent of scorch, wherein the sum of the mass percent of the components is 100 percent; the high-temperature dry granules comprise the following components in percentage by mass: SiO 2245.02%、AI2O318.24%、K2O 2.41%、Na2O 3.84%、CaO 5.24%、MgO 1.56%、ZnO 4.88%、BaO 13.17%、SrO25.19 percent and 0.45 percent of scorch, and the sum of the mass percent of the components is 100 percent; the warm-drying granules comprise the following components in percentage by mass: SiO 2250.43%、AI2O320.34%、K2O 3.2%、Na2O 3.81%、CaO 5.59%、MgO 1.17%、ZnO 7.65%、BaO 0.25%、SrO26.59 percent of the total weight of the components, the ignition loss is less than or equal to 0.97 percent, and the total weight percent of the components is 100 percent; the high-temperature matte powder comprises the following components in percentage by mass: SiO 2240.1%、AI2O318.84%、K2O 1.49%、Na2O 5.19%、CaO 1.6%、MgO 0.56%、ZnO 17.19%、BaO 7.39%、SrO27.07 percent of the weight percentage of the components, the ignition loss is less than or equal to 0.57 percent, and the sum of the mass percentages of the components is 100 percent; the dry particle suspending agent is sticky and comprises the following main components in parts by weight: 25 parts of methyl glycol, 25 parts of sodium carboxymethylcellulose, 4 parts of sodium metaphosphate and 30 parts of water;

and 7: firing in a kiln, namely firing the semi-finished product obtained in the step 6 in the kiln at the firing temperature of 1195 ℃ for 65 min;

and 8: brushing and polishing the product obtained in the step 7 on a polishing machine, wherein the specification of the grinding blocks is 38 x 9.5 x 14.5mm, the distribution condition of the grinding blocks is that the silicon carbide matte fiber brushes 7 with 120 meshes and the silicon carbide matte fiber brushes 6 with 150 meshes, and the brushing and polishing time is 2 min;

and then, edging, quality inspection, packaging and warehousing are carried out on the product obtained after the steps 1-8.

And on the basis of example 1, the following 6 comparative examples are provided:

comparative example 1:

the green body compression molding step of step 2 in the example 1 is simplified, the PETG material mold carved with fine concave-convex natural texture by a laser engraving machine is not used for compression, but is commonly pressed into a flat blank, and other processes and materials are the same as those in the example 1, so that a product is obtained.

Comparative example 2:

the overglaze material sprayed in the step 4 of the embodiment 1 is replaced by the common overglaze material, and other manufacturing processes and materials are the same as those of the embodiment 1, so that a product is obtained.

Comparative example 3:

the high-temperature dry particle component of the dry particle glaze in the step 6 of the example 1 is removed, and other manufacturing processes and materials are the same as those of the example 1, so that a product is obtained.

Comparative example 4:

the medium temperature dry particle component of the dry particle glaze in the step 6 of the example 1 is removed, and other manufacturing processes and materials are the same as those of the example 1, so that a product is obtained.

Comparative example 5:

and (3) removing the high-temperature matte powder component of the dry granular glaze in the step 6 of the example 1, and obtaining a product by the same other manufacturing processes and materials as the example 1.

Comparative example 6:

the low-temperature glaze slurry component of the dry granular glaze in the step 6 of the example 1 is removed, and other manufacturing processes and materials are the same as those of the example 1, so that a product is obtained.

The surface appearance, touch, gloss, stain resistance, slip resistance, abrasion resistance and breaking strength of the products obtained in example 1 and comparative examples 1 to 6 were tested, wherein the gloss, stain resistance, slip resistance, abrasion resistance and breaking strength were tested according to the corresponding national standards, and the test results are shown in table 1 below:

TABLE 1

The test results of the products of example 1 and comparative examples 1 to 6 are analyzed to show that:

1. comparing a product corresponding to the comparative example 1 with a product corresponding to the example 1, only replacing the blank with the fine concave-convex surface in the example 1 with a flat blank in the comparative example 1, wherein although the surface of the plate tested by the flat blank is smooth and fine, the surface appearance has only a micro-gloss effect, and the stereoscopic impression and the layering impression of the fine concave-convex blank and the light and shadow layering effect of the micro-light and no-light contrast are lacked;

2. compared with the product corresponding to the embodiment 1, the product corresponding to the comparative example 2 is compared, an original overglaze scheme is selected in the embodiment 1, and the selection of the components and the proportion of the overglaze ensures that the pattern printed by ink-jet printing can obtain a clearer effect, and simultaneously provides good color development capability and effect for the ink-jet printed pattern.

3. The results of comparing comparative example 3 with the product corresponding to example 1, not using the high temperature dry granules in comparative example 3, and comparing comparative example 4 with the product corresponding to example 1, not using the medium temperature dry granules in comparative example 4 show that the matching application of the high temperature dry granules and the medium temperature dry granules in the dry granule glaze, and the selection of the components and the dosage can obtain the effects of superior performance and better texture.

4. Comparing the product in comparative example 5 with the product in example 1, the high-temperature matte powder is additionally added in example 1, wherein the addition of the high-temperature matte powder in the dry particle glaze reduces the glossiness of the product, reduces the light pollution caused by excessively strong reflected light, and simultaneously does not roughen the surface to cause poor texture or dirt absorption;

5. compared with the product corresponding to the embodiment 1, the low-temperature glaze slip is added in the embodiment 1, wherein the addition of the low-temperature glaze slip in the dry granular glaze is beneficial to improving the glossiness of the surface of the product, the filling effect is generated in gaps between dry granules and dry granules, the internal structure of the dry granular glaze is further improved, the lubricating texture of the glaze surface is better, and the anti-fouling capability of the product is greatly improved.

In conclusion, the invention selects the original surface glaze and dry particle glaze combination formula, and adopts the manufacturing process of 'fine mould + fine dry particle glaze spraying + brushing polishing' in the manufacturing process flow to prepare the fine concave-convex matte ceramic tile, the fine concave-convex matte ceramic tile has the delicate touch feeling of shallow concave-convex on the surface of the ceramic tile, not only has the advantages of skid resistance, wear resistance, pollution resistance and high breaking strength, but also has the decorative effect of a simple and lasting smell, and the light and shadow layering effect of low light and no light contrast, is just like the trace remained after years of milling, and has the aesthetic feeling after years of precipitation. Brings the historic precipitation feeling and the temperature feeling of the times to the family life, and endows the whole space with harmonious comfortable feeling.

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