CN112142327B

CN112142327B - Glaze composition, glaze and preparation method thereof, and ceramic tile and preparation method thereof

Info

Publication number: CN112142327B
Application number: CN202011065599.9A
Authority: CN
Inventors: 吴超; 李飞
Original assignee: Jingdezhen Oushennuo Ceramic Co ltd
Current assignee: Jingdezhen Oushennuo Ceramic Co ltd
Priority date: 2020-09-30
Filing date: 2020-09-30
Publication date: 2022-05-27
Anticipated expiration: 2040-09-30
Also published as: CN112142327A

Abstract

The invention provides a glaze composition, a glaze and a preparation method thereof, and a ceramic tile and a preparation method thereof. The glaze composition comprises the following raw materials in percentage by mass: 25-27% of zirconium white frit, 3-5% of quartz, 5-7% of wollastonite, 21-23% of matte frit, 8-10% of water-washed kaolin, 5-7% of calcined kaolin and 23-25% of zirconium silicate. A glaze, comprising a glaze composition and a solvent. A method of preparing a glaze comprising: the glaze composition and the solvent are mixed to obtain the glaze. The ceramic tile comprises a green brick and a glaze layer arranged on at least one surface of the green brick, wherein the glaze layer is made of the glaze material. The preparation method of the ceramic tile comprises the following steps: and firing the green brick for the first time, glazing after cooling, and then firing for the second time to obtain the ceramic tile. By using the glaze provided by the application, the ceramic tile with good texture, obvious details and lines and low cost can be prepared by one-time glazing and one-time firing after glazing.

Description

Glaze composition, glaze and preparation method thereof, and ceramic tile and preparation method thereof

Technical Field

The invention relates to the field of ceramics, in particular to a glaze composition, a glaze and a preparation method thereof, and a ceramic tile and a preparation method thereof.

Background

The existing ceramic chip products are generally glazed products twice: the first step is ground glaze, which covers the green body, improves whiteness and controls brick shape; the second is overglaze, generally divided into bright type, soft type and matte type, and special products are satisfied by glazing for three times even because of serious color edges (color depth is inconsistent due to inconsistent water collection of ceramic green sheets after bisque firing).

The processes have the problems of complex process, high control difficulty, high labor cost, large equipment investment and the like.

In view of this, the present application is specifically made.

Disclosure of Invention

The invention aims to provide a glaze composition, a glaze and a preparation method thereof, a ceramic tile and a preparation method thereof, so as to solve the problems.

In order to achieve the above purpose, the invention adopts the following technical scheme:

the glaze composition comprises the following raw materials in percentage by mass:

25-27% of zirconium white frit, 3-5% of quartz, 5-7% of wollastonite, 21-23% of matte frit, 8-10% of water-washed kaolin, 5-7% of calcined kaolin and 23-25% of zirconium silicate.

Alternatively, the raw materials of the glaze composition may have a content of zirconium white frit, calculated as mass%, of any one of 25%, 26%, 27% and 25-27%; the content of the quartz stone can be any value between 3%, 4%, 5% and 3-5%; the content of wollastonite can be any value between 5%, 6%, 7% and 5-7%; the content of the matte frit may be any value between 21%, 22%, 23% and 21-23%; the content of the water-washed kaolin can be any value between 8%, 9%, 10% and 8-10%; the calcined kaolin can be present in an amount of any of 5%, 6%, 7%, and 5-7%; the zirconium silicate content may be any value between 23%, 24%, 25% and 23-25%.

Preferably, the glaze composition further comprises the following raw materials in percentage by mass:

0.15 to 0.3 percent of sodium tripolyphosphate and 0.3 to 0.6 percent of sodium carboxymethyl cellulose.

Sodium tripolyphosphate and sodium carboxymethyl cellulose are used as auxiliary materials, which is beneficial to adjusting physicochemical property parameters of the glaze.

Alternatively, the content of sodium tripolyphosphate in the raw materials of the glaze composition can be any value between 0.15%, 0.20%, 0.25%, 0.3% and 0.15% -0.3%; the content of sodium carboxymethylcellulose can be any value between 0.3%, 0.4%, 0.5%, 0.6% and 0.3% -0.6%.

A glaze comprising the glaze composition and a solvent;

preferably, the solvent comprises water;

preferably, the water accounts for 38 to 40% of the total mass of the glaze composition.

The common glaze only has bright, soft or matte effects, any glaze can not meet the target requirements regardless of texture and color development, and most details and lines can be lost when the glaze is used on the ground glaze. And generally cannot meet the requirements of one glazing operation.

Alternatively, the water may account for any value between 38%, 39%, 40%, and 38-40% of the total mass of the enamel composition.

Preferably, the glaze has a specific gravity of 1.66 to 1.68 g/ml.

Alternatively, the specific gravity of the glaze may be any value between 1.66g/ml, 1.67g/ml, 1.68g/ml and 1.66-1.68 g/ml.

A preparation method of the glaze material comprises the following steps:

and mixing the glaze composition and water to obtain the glaze.

Preferably, the glaze composition is pretreated before use;

preferably, the pre-treatment comprises ball milling;

preferably, the ball milling time is 4-5 h;

preferably, the fineness of the glaze is: the residue after 325 mesh sieve is 0.3-0.6 wt%.

Alternatively, the ball milling time can be any value between 4h, 4.5h, 5h and 4-5 h; the glaze may have a surplus of 0.3wt%, 0.4 wt%, 0.5 wt%, 0.6wt%, and any value between 0.3wt% and 0.6wt% when sieved through a 325 mesh sieve.

A ceramic tile comprises a green brick and a glaze layer arranged on at least one surface of the green brick, wherein the glaze layer is prepared by using the glaze.

Preferably, the thickness of the green brick is 9.2-9.5 mm;

preferably, the glaze layer is applied in an amount of 128-132g/0.18m of the glaze²。

Alternatively, the thickness of the green brick can be any value between 9.2mm, 9.3mm, 9.4mm, 9.5mm and 9.2-9.5 mm; the glaze layer may be applied with the amount of glaze of 128g/0.18m²、129g/0.18m²、130g/0.18m²、131g/0.18m²、132g/0.18m²And 128-132g/0.18m²Any value in between.

A method of making a ceramic tile comprising:

and firing the green brick for the first time, glazing after cooling, and then firing for the second time to obtain the ceramic tile.

Preferably, the temperature of the first firing is 942-1125 ℃, and the time is 40-45 min;

preferably, the temperature of the second firing is 931-1114 ℃, and the time is 45-50 min;

preferably, the glazing is performed by adopting a glaze spraying mode;

preferably, the pressure of the glaze spraying is 6-7 bar;

preferably, the green brick is obtained by pressing a fine carving mould;

preferably, the fine carving mould is obtained by adopting four-dimensional laser carving;

preferably, the diameter of the light source of the four-dimensional laser engraving is 0.02-0.04 mm;

preferably, the pressing pressure is 24000 and 26000 KN;

preferably, inkjet printing is further included after the glazing and before the second firing.

If a common mould is adopted, the texture is not fine enough, the defects of gelatinization and the like are easily caused in the glazing process, the advantages of the glaze can not be embodied, and the finished product rate can be improved by about 3-5% by using the fine carving mould.

Optionally, the temperature of the first firing may be any value between 942 ℃, 950 ℃, 960 ℃, 970 ℃, 980 ℃, 990 ℃, 1000 ℃, 1010 ℃, 1020 ℃, 1030 ℃, 1040 ℃, 1050 ℃, 1060 ℃, 1070 ℃, 1080 ℃, 1090 ℃, 1100 ℃, 1110 ℃, 1120 ℃, 1125 ℃ and 942-1125 ℃, and the time may be any value between 40min, 41min, 42min, 43min, 44min, 45min and 40-45 min; the temperature of the second firing can be any value between 931 ℃, 940 ℃, 950 ℃, 960 ℃, 970 ℃, 980 ℃, 990 ℃, 1000 ℃, 1010 ℃, 1020 ℃, 1030 ℃, 1040 ℃, 1050 ℃, 1060 ℃, 1070 ℃, 1080 ℃, 1090 ℃, 1100 ℃, 1110 ℃, 1114 ℃ and 931 and 1114 ℃, and the time can be any value between 45min, 46min, 47min, 48min, 49min, 50min and 45-50 min; the pressure of the glaze spraying can be any value between 6bar, 6.5bar, 7bar and 6-7 bar; the diameter of the light source of the four-dimensional laser engraving can be any value between 0.02mm, 0.03mm, 0.04mm and 0.02-0.04 mm; the pressing pressure may be any value between 24000KN, 25000KN, 26000KN, and 24000-26000 KN.

Compared with the prior art, the invention has the beneficial effects that:

according to the glaze composition and the glaze provided by the application, the whiteness of the glaze is improved by using the zirconium white frit and the zirconium silicate, the glaze composition and the glaze have good covering capacity for the ground color of a green brick, and meanwhile, the color development level of the glaze can be improved, and the surface texture is changed; the matte frit enables the glaze to have a smooth hand feeling after firing and is also helpful for improving the color development level; quartz mainly changes the glossiness of glaze, and improves the hardness and the wear resistance; the matching of the water-washed kaolin and the calcined kaolin ensures that the glaze has good suspension property, viscosity and fluidity; by selecting the components and the dosage, the raw materials are determined to be selected from zirconium white frit, quartz stone, wollastonite, matte frit, washing kaolin, calcined kaolin and zirconium silicate and the dosage ranges of the zirconium white frit, the calcined kaolin and the zirconium silicate are determined, so that the glaze composition has excellent performances in the aspects of covering capacity, surface texture, strong and weak color development and the like, and can meet the production requirement by glazing once;

the preparation method of the glaze provided by the application is simple in process;

the ceramic tile provided by the application has good surface texture and low production cost;

the preparation method of the ceramic tile only needs glazing once, and is simple in process, low in operation difficulty, and capable of greatly reducing labor cost, material consumption and the like.

Drawings

To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, and it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope of the present invention.

Fig. 1 is a photograph showing the appearance of the tiles obtained in examples 1 to 4.

Detailed Description

The terms as used herein:

"prepared from … …" is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

The conjunction "consisting of … …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of … …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.

When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when the range "1 ~ 5" is disclosed, the ranges described should be construed to include the ranges "1 ~ 4", "1 ~ 3", "1 ~ 2 and 4 ~ 5", "1 ~ 3 and 5", and the like. When a range of values is described herein, unless otherwise specified, the range is intended to include the endpoints thereof, and all integers and fractions within the range.

In these examples, the parts and percentages are by mass unless otherwise indicated.

"part by mass" means a basic unit of measure indicating a mass ratio of a plurality of components, and 1 part may represent any unit mass, for example, 1g or 2.689 g. If we say that the part by mass of the component A is a part by mass and the part by mass of the component B is B part by mass, the ratio of the part by mass of the component A to the part by mass of the component B is a: b. alternatively, the mass of the A component is aK and the mass of the B component is bK (K is an arbitrary number, and represents a multiple factor). It is unmistakable that, unlike the parts by mass, the sum of the parts by mass of all the components is not limited to 100 parts.

"and/or" is used to indicate that one or both of the illustrated conditions may occur, e.g., a and/or B includes (a and B) and (a or B).

Embodiments of the present invention will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.

The zirconium white frit, quartz stone, wollastonite, matte frit, washed kaolin and calcined kaolin used in the examples of the present application were obtained from Dajia precision ceramics, Inc., of Foshan city, zirconium silicate was obtained from Cissus, Kyoho, Chemie, Inc., sodium tripolyphosphate was obtained from Cissus, Kiwayobo, and sodium carboxymethylcellulose was obtained from Yansen, Chemie, Foshan city, Inc.

Example 1

The present embodiment provides an enamel composition comprising: 27kg of zirconium white frit, 5kg of quartz stone, 5kg of wollastonite, 23kg of matte frit, 10kg of water-washed kaolin, 7kg of calcined kaolin and 23kg of zirconium silicate.

Mixing the raw materials, ball-milling for 4h, detecting fineness and discharging.

And (3) obtaining the fine carving mould by using four-dimensional laser carving, wherein the diameter of a light source of the four-dimensional laser carving is 0.02 mm. Then, an isostatic pressing mold press is used for pressing under the condition of 24000KN of pressure to obtain a green brick, and the thickness of the green brick is 9.2 mm.

Firing the green brick at 942 deg.C for 45min, and cooling to room temperature.

And transferring the prepared glaze to a glaze spraying room, sieving by a 325-mesh sieve until the screen residue is 0.6wt%, adding 38kg of water after sieving, and stirring to obtain the glaze, wherein the specific gravity of the glaze is controlled to be 1.68 g/ml. Adjusting the pressure of the pump to 6bar, observing whether the pressure and atomization are uniform, and adjusting the glazing amount to 132g/0.18m²And then starting glaze spraying.

And (4) carrying out ink-jet printing after the glaze spraying is finished, and then firing in a kiln at the firing temperature of 931 ℃ for 50 min. And after firing, cooling, edging, sorting, packaging and warehousing.

The appearance of the resulting tile is shown in fig. 1 (leftmost).

Example 2

This example provides a glaze composition, which is composed of the following raw materials: 25kg of zirconium white frit, 4kg of quartz stone, 7kg of wollastonite, 22.3kg of matte frit, 10kg of water-washed kaolin, 6kg of calcined kaolin, 25kg of zirconium silicate, 0.2kg of sodium tripolyphosphate and 0.5kg of sodium carboxymethylcellulose.

Mixing the raw materials, ball-milling for 5h, detecting fineness and discharging.

And (3) obtaining the fine carving mould by using four-dimensional laser carving, wherein the diameter of a light source of the four-dimensional laser carving is 0.03 mm. Then, an isostatic pressing die press was used to press the green bricks with a thickness of 9.5mm under a pressure of 26000 KN.

Firing the green brick at 1125 ℃ for 40min, and then cooling to room temperature.

And transferring the prepared glaze to a glaze spraying room, sieving by a 325-mesh sieve until the screen residue is 0.3wt%, adding 40kg of water after sieving, and stirring to obtain the glaze, wherein the specific gravity of the glaze is controlled to be 1.66 g/ml. Adjusting the pressure of the pump to 7bar, observing whether the pressure and atomization are uniform, and adjusting the glazing amount to 128g/0.18m²And then starting glaze spraying.

And (4) carrying out ink-jet printing after glaze spraying is finished, and then firing in a kiln at 1114 ℃ for 45 min. And after firing, cooling, edging, sorting, packaging and warehousing.

The appearance of the resulting tile is shown in fig. 1 (second from left).

Example 3

The present embodiment provides an enamel composition comprising: 26.5kg of zirconium white frit, 3.5kg of quartz, 6.55kg of wollastonite, 21.5kg of matte frit, 10kg of washing kaolin, 7kg of calcined kaolin, 24.5kg of zirconium silicate, 0.15kg of sodium tripolyphosphate and 0.3kg of sodium carboxymethylcellulose.

Mixing the raw materials, ball-milling for 4.5h, detecting fineness and discharging.

And (3) obtaining the fine carving mould by using four-dimensional laser carving, wherein the diameter of a light source of the four-dimensional laser carving is 0.04 mm. Then, an isostatic pressing mold press was used to press the green bricks with a thickness of 9.3mm under a pressure of 25000 KN.

And firing the green brick at 1100 ℃ for 42min, and then cooling to room temperature.

And transferring the prepared glaze to a glaze spraying room, sieving by a 325-mesh sieve until the screen residue is 0.4 wt%, adding 39kg of water after sieving, and stirring to obtain the glaze, wherein the specific gravity of the glaze is controlled to be 1.67 g/ml. Adjusting the pressure of the pump to 6bar, observing whether the pressure and atomization are uniform, and adjusting the glazing amount to 130g/0.18m²And then starting glaze spraying.

And (4) carrying out ink-jet printing after the glaze spraying is finished, and then firing in a kiln at the firing temperature of 1000 ℃ for 48 min. And after firing, cooling, edging, sorting, packaging and warehousing.

The appearance of the resulting tile is shown in fig. 1 (third from left).

Example 4

This example provides a glaze composition, which is composed of the following raw materials: 27kg of zirconium white frit, 4kg of quartz stone, 6kg of wollastonite, 22.5kg of matte frit, 10kg of water-washed kaolin, 7kg of calcined kaolin, 23kg of zirconium silicate, 0.3kg of sodium tripolyphosphate and 0.2kg of sodium carboxymethylcellulose.

And (3) obtaining the fine carving mould by using four-dimensional laser carving, wherein the diameter of a light source of the four-dimensional laser carving is 0.03 mm. Then, an isostatic pressing die press was used to press the green bricks with a thickness of 9.4mm under a pressure of 26000 KN.

Firing the green brick at 1050 ℃ for 44min, and then cooling to room temperature.

And transferring the prepared glaze to a glaze spraying room, sieving by a 325-mesh sieve until the screen residue is 0.5 wt%, adding 39kg of water after sieving, and stirring to obtain the glaze, wherein the specific gravity of the glaze is controlled to be 1.66 g/ml. Adjusting the pressure of the pump to 7bar, observing whether the pressure and atomization are uniform, and adjusting the glazing amount to 130g/0.18m²And then starting glaze spraying.

And (4) carrying out ink-jet printing after glaze spraying is finished, and then, firing in a kiln at the firing temperature of 1100 ℃ for 48 min. And after firing, cooling, edging, sorting, packaging and warehousing.

The appearance of the resulting tile is shown in fig. 1 (rightmost side).

The properties of the tiles obtained in examples 1 to 4 were tested and the results are shown in table 1 below:

table 1 results of performance testing

Item	Breaking Strength/N	Modulus of rupture/MPa
			Example 1	1258.6	25.89
Example 2	1386.2	26.85
			Example 3	1278.6	26.27
Examples4	1354.3	26.45

As can be seen from table 1 above, the ceramic tiles obtained in the present application have high strength.

The average value of the glossiness of the ceramic tiles obtained in the embodiments 1 to 4 is 12 to 15 by performing glossiness detection; the tiles obtained in examples 1 to 4 all had a smooth hand, as evaluated subjectively on hand.

Comparative example 1

This comparative example provides an enamel composition comprising: 27kg of zirconium white frit, 2kg of quartz, 6kg of wollastonite, 22.5kg of matte frit, 10kg of water-washed kaolin, 7kg of calcined kaolin, 25kg of zirconium silicate, 0.3kg of sodium tripolyphosphate and 0.2kg of sodium carboxymethylcellulose.

The preparation method is the same as example 4.

Compared with example 4, the comparative example reduces the amount of quartz, and the average value of the glossiness of the comparative example is only 11, while the average value of the glossiness of example 4 can reach 17.5. It is demonstrated that quartz can improve the surface gloss of the tiles provided herein.

Comparative example 2

This comparative example provides an enamel composition comprising: 27kg of zirconium white frit, 4kg of quartz stone, 4kg of wollastonite, 23kg of matte frit, 10kg of water-washed kaolin, 7kg of calcined kaolin, 24.5kg of zirconium silicate, 0.3kg of sodium tripolyphosphate and 0.2kg of sodium carboxymethylcellulose.

The preparation method is the same as example 4.

Compared with example 4, the comparative example reduces the amount of wollastonite, has an average value of gloss of only 11 to 12, and has a rough hand compared with the tile obtained in example 4. It is stated that wollastonite has some effect on the surface gloss of the tile provided herein, but primarily affects the smoothness of the tile surface, and that suitable wollastonite usage helps to enhance the smoothness of the tile surface.

According to the glaze composition and the glaze, through the research on the formula, the performances of covering capacity, surface texture, color development strength and the like of a blank body are considered. The zirconium white frit and the matte frit mainly improve whiteness, cover a blank, improve the color development level of glaze, change surface texture and match the expansion coefficient of the blank; if the formula does not contain the zirconium white frits, the color development is poor, the hand feeling is not smooth enough, the body color is easy to expose, and the brick shape is not easy to control; quartz mainly changes the glossiness of glaze, improves the hardness and the wear resistance, and if quartz is not used or the content is low, the glossiness is insufficient, and the physical and chemical properties do not reach the standard; the kaolin provides Al in the formula structure, is a main bracket of the formula, improves the suspension property and viscosity of glaze, and ensures that the glazing process is simple and convenient to operate, otherwise, the glaze slip is easy to thixotropy due to poor performance.

Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.

Claims

1. A ceramic tile is characterized by comprising a green tile and a glaze layer arranged on at least one surface of the green tile, wherein the glaze layer is made of glaze; the green brick is obtained by pressing a precise engraving mould, the precise engraving mould is obtained by engraving with four-dimensional laser, and the diameter of a light source for engraving with the four-dimensional laser is 0.02-0.04 mm;

the glaze comprises a glaze composition and water;

25-27% of zirconium white frit, 3-5% of quartz, 5-7% of wollastonite, 21-23% of matte frit, 8-10% of water-washed kaolin, 5-7% of calcined kaolin and 23-25% of zirconium silicate;

the water accounts for 38-40% of the total mass of the glaze composition.

2. The tile according to claim 1, wherein the raw materials of the glaze composition further comprise, in mass percent:

3. The tile of claim 1 wherein said glaze has a specific gravity of 1.66 to 1.68 g/mL.

4. The tile according to claim 1, characterized in that the glaze is prepared by a method comprising:

and mixing the glaze composition and water to obtain the glaze.

5. The tile of claim 4, wherein the glaze composition is pretreated prior to use, the pretreatment comprising ball milling.

6. The tile according to claim 5, wherein the ball milling time is 4-5 h.

7. The tile according to claim 4, characterized in that the fineness of the glaze is: the residue after 325 mesh sieve is 0.3-0.6 wt%.

8. The tile according to claim 1, wherein the thickness of the green tile is 9.2-9.5 mm.

9. The tile as claimed in claim 1, wherein the glaze layer is applied in an amount of 128-132g/0.18m of said glaze²。

10. A process for the preparation of a ceramic tile according to any one of claims 1 to 9, comprising:

11. The method as claimed in claim 10, wherein the first firing is carried out at 942-1125 ℃ for 40-45 min;

the temperature of the second firing is 931-1114 ℃, and the time is 45-50 min.

12. The method for manufacturing a ceramic tile according to claim 10, wherein the glazing is performed by means of glaze spraying.

13. A process for the preparation of a tile according to claim 12 wherein the pressure of the spray is 6-7 bar.

14. The method for the preparation of ceramic tiles according to claim 10, wherein the pressing pressure is 24000 and 26000 kN.

15. The method of claim 10, further comprising ink-jet printing after the glazing and before the second firing.