CN111362577A - A kind of bright glaze for ceramic antique brick and preparation method thereof - Google Patents

Abstract

A bright glaze for ceramic antique tiles and a preparation method thereof. The bright glaze is prepared by ball milling of glaze and additives. The glaze includes the following raw materials in weight percentages: zirconium white frit 37-84%, transparent frit 9-56% of block, 5-7% of clay, the additives are sodium tripolyphosphate and sodium polymethyl cellulose, and the addition amounts are respectively 0.2-0.4% and 0.3-0.6% of the weight of the glaze; the raw materials After mixing, drying, ball milling and glazing, it can form a bright glaze with the surface of the antique brick body. The invention develops a bright glaze that can be applied to the body of the antique brick, and has the advantages of flat, smooth and delicate glaze surface, high microhardness, high gloss, environmental protection and no pollution, good wear resistance and decorative performance, and the antique brick has the advantages of The brightening effect is obvious.

Description

A kind of bright glaze for ceramic antique brick and preparation method thereof

technical field

The invention relates to the technical field of ceramic preparation, in particular to a bright glaze for ceramic antique bricks and a preparation method thereof.

Background technique

As a kind of architectural ceramic product, in order to reflect the heavy sense of history and the vicissitudes of time, the surface of ceramic antique tile is usually applied with a layer of low-gloss matt glaze. In recent years, with the change of people's aesthetics and the pursuit of visual impact, the glazed decoration of antique tiles has gradually developed from matt glaze to bright glaze.

The Chinese invention patent "a ceramic bright glaze ink and its preparation method" (CN105131716A) discloses a preparation method of a bright glaze ink for inkjet printing. The components and weight ratios in the bright glaze are: SiO ₂ : Al ₂ O ₃ : CaO: MgO: KNaO: Li ₂ O: BaO: ZnO: B ₂ O ₃ : P ₂ O ₅ =55~65:7~13:4~10:2.1~4.5:4~ 10:0.8～2:4～6:2.1～5.5:6～10:0～3, although the glaze obtained after firing has excellent properties such as smooth glaze, bright, no pinholes and glossiness above 91, but There is 0-3wt% P ₂ O ₅ in the glaze, and its potential toxicity limits its application. In addition, its wear resistance has not been reported. The Chinese invention patent "a ceramic glaze and its preparation method" (CN107417117A) discloses a bright glaze with a smooth surface and no pinholes or bubbles and good gloss and a preparation method. The components of the bright glaze are SiO ₂ 55~ 80wt%, Al ₂ O ₃ 8～15wt%, B ₂ O ₃ 0～5wt%, CaO 5～13wt%, MgO 2～6wt%, BaO 1～8wt%, ZnO 0～5wt%, K ₂ O 1～4wt% %, Na ₂ O 1-4wt%, but no report on wear resistance and bright light performance has been reported.

SUMMARY OF THE INVENTION

In order to solve the above-mentioned problems, the present invention proposes a bright glaze for ceramic antique tiles and a preparation method thereof, and the specific technical scheme is:

A bright glaze for ceramic antique tiles, the bright glaze is prepared by ball milling of glaze and additives, and the glaze includes the following raw materials in weight percentage: 37-84% of zirconium white frit, 9-56% of transparent frit %, clay 5-7%, the additives are sodium tripolyphosphate and sodium polymethyl cellulose, and the addition amounts are 0.2-0.4% and 0.3-0.6% of the glaze weight respectively.

Preferably, the weight percentage of each component of the glaze is: 60% of zirconium white frit, 34% of transparent frit, and 6% of clay, and the addition amounts of the sodium tripolyphosphate and sodium polymethylcellulose are respectively 0.3% and 0.5% of the glaze weight.

A preparation method of bright glaze for ceramic antique tiles, comprising the following steps:

(1) ball mill described zirconium white frit, transparent frit and clay to a certain particle size;

(2) placing the ball-milled raw materials in a ball mill in proportion, and mixing with wet ball milling for 60-120 min to obtain a mixture;

(3) drying the mixture in a drying oven at 90° C. for 24-48 hours to obtain dry glaze powder;

(4) ball-milling the glaze dry powder, additives, ball mill and water in a ball-milling jar for 20-24 hours in a certain proportion to obtain slurry;

(5) applying the slurry to the surface of the antique brick body, and placing it at room temperature for natural drying for 12-24 hours to obtain a sample;

(6) The sample is fired at 1050-1150°C, and a bright glaze is formed on the surface of the antique brick body.

Further, the chemical components of the white zirconium frit are: SiO ₂ 51-58%, Al ₂ O ₃ 6-7%, Fe ₂ O ₃ 0.01-1%, TiO ₂ 0.01-1%, CaO 6-9%, MgO 2-4%, K ₂ O 3-5%, Na ₂ O 0.01-1%, ZrO ₂ 3-5%, ZnO 12-14%, BaO 0.01-1%.

Further, the chemical composition of the transparent frit is: SiO ₂ 62-65%, Al ₂ O ₃ 8-12%, Fe ₂ O ₃ 0.01-1%, CaO 12-14%, MgO 1 -2%, K ₂ O 2-3%, Na ₂ O 0.01-1%, ZrO ₂ 0.01-1%, ZnO 6-7%, BaO 0.01-1%.

Further, the chemical composition of the clay is: 60-66% of SiO ₂ , 32-36% of Al ₂ O ₃ , 0.01-1% of Fe ₂ O ₃ , 0.01-1% of TiO ₂ , 0.01-1% of CaO 1%, K ₂ O 0.01 to 1%.

Further, the average particle sizes of the zirconium white frit, the transparent frit and the clay are 375 mesh, 325 mesh and 250 mesh, respectively.

Further, the additives are sodium tripolyphosphate and sodium polymethylcellulose, and the addition amounts thereof are respectively 0.2-0.4% and 0.3-0.6% of the weight of the glaze.

Further, the ratio described in step (4) is: (dry powder and additives): ball mill: water mass ratio of 1:2:0.6-0.7.

Further, the temperature regime of the sintering is as follows: when the temperature is less than 1000°C, the heating rate is 5°C/min, and the temperature is maintained at every 100°C for 30 minutes. ℃ for 60 minutes, and the highest temperature for 15 to 30 minutes.

Beneficial effects:

The invention develops a bright glaze that can be applied to the body of the antique brick, makes up the blank of the domestic bright glaze for the antique brick, and the chemical composition of the raw materials does not contain harmful heavy metal elements such as lead and cadmium, and the prepared bright glaze has a smooth glaze surface. , smooth, delicate, high microhardness, high gloss and environmental protection and pollution-free advantages, good wear resistance and decorative performance, the bright effect of antique brick is obvious.

Detailed ways

Below in conjunction with specific embodiment, the present invention will be further described:

A bright glaze for ceramic antique tiles, the bright glaze is prepared by ball milling of glaze and additives, and the glaze includes the following raw materials in weight percentage: 37-84% of zirconium white frit, 9-56% of transparent frit %, clay 5-7%, the additives are sodium tripolyphosphate and sodium polymethyl cellulose, and the addition amounts are 0.2-0.4% and 0.3-0.6% of the glaze weight respectively.

Preferably, the weight percentage of each component of the glaze is: 60% of zirconium white frit, 34% of transparent frit, and 6% of clay, and the addition amounts of the sodium tripolyphosphate and sodium polymethylcellulose are respectively 0.3% and 0.5% of the glaze weight.

Example 1:

A preparation method of bright glaze for ceramic antique tiles, the bright glaze is prepared by ball milling of glaze and additives, and weighs 37% of zirconium white frit, 56% of transparent frit and 7% of clay by weight percentage, wherein, The chemical composition of the zirconium white frit is: SiO ₂ 58%, Al ₂ O ₃ 6%, Fe ₂ O ₃ 0.01%, TiO ₂ 0.01%, CaO 6%, MgO 4%, K ₂ O 5 %, Na ₂ O 1%, ZrO ₂ 5%, ZnO 14%, BaO 0.98%; the chemical composition of the transparent frit is: SiO ₂ 65%, Al ₂ O ₃ 10%, Fe ₂ O ₃ 1%, CaO 14%, MgO 1%, K ₂ O 2%, Na ₂ O 0.01%, ZrO ₂ 0.01%, ZnO 6%, BaO 0.98%; the chemical composition of the clay by weight percentage is: _SiO2 60%, _Al2O3 36%, _{Fe2O3 1} %, _{TiO2 1} %, CaO 1%, K2O ₁ %.

The preparation method comprises the following steps:

(1) Preparation of raw materials: after ball-milling zirconium white frit, transparent frit, and clay into powders, respectively; Mesh, 325 mesh, 250 mesh.

(2) Mixing: Weigh zirconium white clinker, transparent clinker and clay by weight percentage, place them in a ball mill and wet ball milling and mix for 120min to obtain a mixture.

(3) Drying: The mixed slurry was dried in a drying oven at 90° C. for 48 hours to obtain dry glaze powder.

(4) Grinding and pulping: the glaze dry powder, additives, ball mill and water are ball-milled in a ball mill tank for 24 hours in a certain proportion to obtain a slurry; wherein, the ratio of the material is (dry powder and additives): ball mill: water The mass ratio of 1:2:0.6; the additives are sodium tripolyphosphate (STTP) and sodium polymethyl cellulose (CMC), and their addition amounts are 0.2% and 0.3% of the glaze weight, respectively.

(5) glazing: applying the slurry to the surface of the antique brick body, and placing it at room temperature for natural drying for 12h to obtain a sample;

(6) Firing: the sample is fired at 1050°C, and a bright glaze is formed on the surface of the antique brick body, that is, a bright glaze decorative antique tile product is obtained.

The temperature regime of the firing is as follows: when the temperature is less than 1000°C, the heating rate is 5°C/min, and the temperature is kept at 100°C for 30 minutes. , the maximum temperature is kept for 30 minutes, and the antique bricks with bright glaze are obtained.

After testing, the bright glaze for antique tiles prepared in the above-mentioned embodiment has a flat, smooth and delicate glaze surface, a high microhardness of 673.03HV, a high glossiness of 80°, and a good glaze decoration effect.

Example 2:

A preparation method of bright glaze for ceramic antique tiles, the bright glaze is prepared by ball milling of glaze and additives, and weighs 84% of zirconium white frit, 9% of transparent frit and 7% of clay by weight percentage, wherein, The chemical composition of the zirconium white frit is: SiO ₂ 52%, Al ₂ O ₃ 7%, Fe ₂ O ₃ 1%, TiO ₂ 1%, CaO 9%, MgO 4%, K ₂ O5 %, Na ₂ O 1%, ZrO ₂ 5%, ZnO 14%, BaO 1%; the chemical composition of the transparent frit is: SiO ₂ 62%, Al ₂ O ₃ 12%, Fe ₂ O ₃ 1%, CaO 12%, MgO 2%, K ₂ O 2%, Na ₂ O 1%, ZrO ₂ 1%, ZnO 6%, BaO 1%; the chemical composition of the clay by weight is: SiO ₂ 66%, _Al2O3 32%, _Fe2O3 0.01 _% , _TiO2 0.01 _% , CaO 0.99%, _K2O 0.99%.

The preparation method comprises the following steps:

(1) Preparation of raw materials: after ball-milling zirconium white frit, transparent frit, and clay into powders, respectively; Mesh, 325 mesh, 250 mesh.

(2) Mixing: Weigh zirconium white frit, transparent frit and clay by weight percentage, place them in a ball mill for wet ball milling and mix for 60 minutes to obtain a mixture.

(3) Drying: Dry the mixed slurry at 90° C. for 24 hours in a drying oven to obtain dry glaze powder.

(4) Grinding and pulping: the dry powder of the glaze, additives, ball mill and water are ball-milled in a ball-milling tank for 20 hours in a certain proportion to obtain a slurry; wherein, the ratio of the material is (dry powder and additives): ball mill: water The mass ratio of 1:2:0.7; the additives are sodium tripolyphosphate (STTP) and sodium polymethyl cellulose (CMC), and their addition amounts are 0.4% and 0.6% of the glaze weight, respectively.

(5) Glazing: applying the slurry to the surface of the antique brick body, and placing it at room temperature for natural drying for 24h to obtain a sample;

(6) Firing: the sample is fired at 1150°C, and a bright glaze is formed on the surface of the antique brick body, that is, a bright glaze decorative antique tile product is obtained.

The temperature regime of the firing is as follows: when the temperature is less than 1000°C, the heating rate is 5°C/min, and the temperature is kept at 100°C for 30 minutes. , the highest temperature was kept for 15 minutes, and the antique bricks with bright glaze were obtained.

After testing, the bright glaze for antique tiles prepared in the above-mentioned embodiment has a flat, smooth and delicate glaze surface, a high microhardness of 741.90HV, a high glossiness of 90°, and a good glaze decoration effect.

Example 3:

A preparation method of bright glaze for ceramic antique tiles, the bright glaze is prepared by ball milling of glaze and additives, and weighs 60% of zirconium white frit, 34% of transparent frit and 6% of clay by weight percentage, wherein, The chemical composition of the zirconium white frit is: SiO ₂ 54.5%, Al ₂ O ₃ 6.5%, Fe ₂ O ₃ 0.5%, TiO ₂ 0.5%, CaO 7%, MgO 5%, K ₂ O by weight percentage 6%, Na ₂ O 0.5%, ZrO ₂ 5%, ZnO 14%, BaO 0.5%; the chemical composition of the transparent frit is 63.5% by weight: SiO ₂ 63.5%, Al ₂ O ₃ 10%, Fe ₂ O ₃ 0.5%, CaO 14%, MgO 1.5%, K ₂ O 2.5%, Na ₂ O 0.5%, ZrO ₂ 0.5%, ZnO 6.5%, BaO 0.5%; : SiO ₂ 63%, Al ₂ O ₃ 35%, Fe ₂ O ₃ 0.5%, TiO ₂ 0.5%, CaO 0.5%, K ₂ O 0.5%.

The preparation method comprises the following steps:

(1) Preparation of raw materials: after ball-milling zirconium white frit, transparent frit, and clay into powders, respectively; Mesh, 325 mesh, 250 mesh.

(2) Mixing: Weigh the zirconium white frit, the transparent frit and the clay by weight percentage, place them in a ball mill and mix them by wet ball milling for 90 minutes to obtain a mixture.

(3) Drying: The mixed slurry was dried in a drying oven at 90° C. for 36 hours to obtain dry glaze powder.

(4) Grinding and pulping: the glaze dry powder, additives, ball mill and water are ball-milled in a ball mill tank for 24 hours in a certain proportion to obtain a slurry; wherein, the ratio of the material is (dry powder and additives): ball mill: water The mass ratio of 1:2:0.6; the additives are sodium tripolyphosphate (STTP) and sodium polymethyl cellulose (CMC), and their addition amounts are 0.3% and 0.5% of the glaze weight, respectively.

(5) glazing: applying the slurry to the surface of the antique brick body, and placing it at room temperature for natural drying for 18h to obtain a sample;

(6) Firing: the sample is fired at 1100°C, and a bright glaze is formed on the surface of the antique brick body, that is, a bright glaze decorative antique tile product is obtained.

The temperature regime of the firing is as follows: when the temperature is less than 1000°C, the heating rate is 5°C/min, and the temperature is kept at 100°C for 30 minutes. , the maximum temperature is kept for 20 minutes, and the antique bricks with bright glaze are obtained.

After testing, the bright glaze for antique tiles prepared in the above-mentioned embodiment has a flat, smooth and delicate glaze surface, a high microhardness of 713.60HV, a high glossiness of 86°, and a good glaze decoration effect.

To sum up, and after repeated implementation of various ratios, the microhardness of the bright glaze for antique bricks obtained is 673.03-741.90HV, and the gloss is 80°-90°, which has a good glaze decoration effect. .

Claims (10)

1. a glaze glaze for ceramic antique bricks, the glaze glaze is prepared after glaze and additive ball milling, it is characterized in that, described glaze comprises each raw material of following percentage by weight: zirconium white frit 37～84%, The transparent frit is 9-56% and the clay is 5-7%. The additives are sodium tripolyphosphate and sodium polymethyl cellulose, and the addition amounts thereof are respectively 0.2-0.4% and 0.3-0.6% of the glaze weight. 2. The bright glaze for a ceramic antique tile according to claim 1, wherein the weight percentage of each component of the glaze is: zirconium white frit 60%, transparent frit 34%, clay 6% , the added amounts of the sodium tripolyphosphate and sodium polymethylcellulose are respectively 0.3% and 0.5% of the glaze weight. 3. a preparation method of bright glaze for ceramic antique bricks, is characterized in that, comprises the following steps: (1) zirconium white frit described in claim 1, transparent frit, clay ball are ground to certain particle size; (2) placing the ball-milled raw materials in a ball mill according to the ratio described in claim 1 or 2, and mixing with wet ball milling for 60-120 min to obtain a mixture; (3) drying the mixture in a drying oven at 90° C. for 24-48 hours to obtain dry glaze powder; (4) Ball milling the glaze dry powder, additives, ball mill and water in a ball mill in a certain proportion for 20 to 24 hours to obtain slurry; (5) applying the slurry to the surface of the antique brick body, and placing it at room temperature for natural drying for 12-24 hours to obtain a sample; (6) The sample is fired at 1050-1150°C, and a bright glaze is formed on the surface of the antique brick body. 4. The preparation method of a bright glaze for ceramic antique tiles according to claim 3, wherein the chemical composition of the zirconium white frit is: SiO ₂ 51-58%, Al ₂ O ₃ 6-7%, Fe ₂ O ₃ 0.01-1%, TiO ₂ 0.01-1%, CaO 6-9%, MgO 2-4%, K ₂ O 3-5%, Na ₂ O 0.01-1%, ZrO ₂ 3-5%, ZnO 12-14%, BaO 0.01-1%. 5 . The method for preparing a bright glaze for ceramic antique tiles according to claim 3 , wherein the chemical composition of the transparent frit is: SiO ₂ 62-65%, Al ₂ O ₃ by weight percentage. 8-12%, Fe ₂ O ₃ 0.01-1%, CaO 12-14%, MgO 1-2%, K ₂ O 2-3%, Na ₂ O 0.01-1%, ZrO ₂ 0.01-1%, ZnO 6 to 7%, BaO 0.01 to 1%. 6 . The preparation method of bright glaze for ceramic antique tiles according to claim 3 , wherein the chemical components of the clay are: SiO ₂ 60～66%, Al ₂ O ₃ 32～ 36%, Fe ₂ O ₃ 0.01-1%, TiO ₂ 0.01-1%, CaO 0.01-1%, K ₂ O 0.01-1%. 7. the preparation method of a kind of ceramic antique tile bright glaze according to claim 3, is characterized in that, the average particle diameter after the described zirconium white frit of step (1), transparent frit, clay ball milling is respectively 375 mesh, 325 mesh and 250 mesh. 8. the preparation method of a kind of ceramic antique tile bright glaze according to claim 3, is characterized in that, described additive is sodium tripolyphosphate and sodium polymethyl cellulose, and its addition is respectively the weight of glaze 0.2 to 0.4% and 0.3 to 0.6%. 9. the preparation method of a kind of ceramic antique tile bright glaze according to claim 8, is characterized in that, the ratio described in step (4) is: (dry powder and additive): ball mill: the mass ratio of water is 1: 2: 0.6 to 0.7. 10. The preparation method of a bright glaze for ceramic antique tiles according to claim 6, wherein the temperature regime of the firing is: when the temperature is less than 1000°C, the temperature rise rate is 5°C/min, and the temperature is 5°C/min. Hold at 100°C for 30min, when the temperature is ≥1000°C, the heating rate is 3°C/min, and the temperature is kept at every 100°C for 60min, and the maximum temperature is kept for 15-30min.