Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a matte overglaze, a matte ceramic tile and a preparation method thereof, and aims to solve the technical problem that crystallization is easy to occur in the firing process of the matte overglaze in the prior art.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the matte overglaze comprises the following components in parts by weight: 65-72 parts of XW-1816 frit, 11-14 parts of zirconium silicate, 5-7 parts of air knife soil and 12-15 parts of XT-1705 frit.
The matte overglaze comprises the following chemical compositions in percentage by weight: siO (SiO) 2 57%~62%、Al 2 O 3 5.7%~7%、Fe 2 O 3 0.08%~0.12%、MgO 1.3%~1.45%、CaO 8.5%~9.2%、Na 2 O 0.2%~0.3%、K 2 O 3.5%~4.2%、ZrO 2 0~0.15%、BaO 3%~5%、ZnO 10%~13%、B 2 O 3 4 to 6 percent, 0.1 to 0.3 percent of burning loss and the balance of impurities.
The matte overglaze comprises the following raw materials in parts by weight: 25-30 parts of potassium feldspar, 3-5 parts of dolomite, 12-15 parts of calcite, 3-5 parts of barium carbonate, 8-10 parts of zinc oxide, 5-8 parts of boric acid, 30-35 parts of quartz sand, 1-2 parts of alumina and 1-3 parts of potassium carbonate.
The matte overglaze comprises the following chemical components in percentage by weight: siO (SiO) 2 48%~53%、Al 2 O 3 10%~13%、Fe 2 O 3 0~0.2%、MgO 0~0.5%、CaO 7.5%~9.5%、Na 2 O 1%~1.5%、K 2 O 4%~5%、ZrO 2 0~0.2%、BaO 10%~15%、ZnO 5.5%~7.5%、B 2 O 3 2 to 4 percent, 0.06 to 0.08 percent of burning loss and the balance of impurities.
The matte overglaze comprises the following raw materials in parts by weight: 40-50 parts of potassium feldspar, 1-2 parts of dolomite, 3-5 parts of calcined bauxite, 11-14 parts of calcite, 12-16 parts of barium carbonate, 4-6 parts of zinc oxide, 2-4 parts of boric acid and 12-15 parts of quartz sand.
The surface of the matte ceramic tile is provided with an overglaze layer, and the preparation raw materials of the overglaze layer comprise the matte overglaze.
A method for preparing a matte tile as described above, comprising the steps of: covering Shi Yaguang overglaze on the surface of the green brick, and firing to obtain a finished product; the matte glaze passes through a 325 mesh screen, and the screen residue is 0.3-0.6%.
The preparation method of the matte ceramic tile comprises the step of enabling the glazing quantity of the matte overglaze to be 100-110 g/(300 mm multiplied by 600 mm).
The preparation method of the matte ceramic tile comprises the step of firing for 40-50 min.
The preparation method of the matte ceramic tile comprises the step of firing at 1060-1075 ℃.
The beneficial effects are that:
the invention provides a matte overglaze which comprises XW-1816 frit, zirconium silicate, air knife soil and XT-1705 frit, wherein the matte overglaze with higher glossiness is obtained after firing through the collocation of the two frits, and the crystallization problem does not occur.
The invention also provides a matte ceramic tile, wherein the surface of the matte ceramic tile is provided with the overglaze layer, the preparation raw materials of the overglaze layer comprise the matte overglaze, the glossiness of the matte ceramic tile is between 36 and 40 ℃, the matte ceramic tile meets the product requirements, and the surface is fine and smooth and has no obvious concave or obvious orange peel texture.
The invention also provides a preparation method of the matte ceramic tile, which is used for preparing the matte ceramic tile, and the preparation method can effectively reduce crystallization problem and glaze defects by controlling the fineness of the matte glaze.
Detailed Description
The invention provides a matte overglaze, a matte ceramic tile and a preparation method thereof, which are used for making the purposes, the technical scheme and the effects of the invention clearer and more definite, and the invention is further described in detail below by referring to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides a matte overglaze which comprises the following components in parts by weight: 65-72 parts of XW-1816 frit, 11-14 parts of zirconium silicate, 5-7 parts of air knife soil and 12-15 parts of XT-1705 frit. The invention adopts the XW-1816 frit to match with the XT-1705 frit, which can improve the glossiness after firing and avoid the crystallization problem. In addition, the clinker can be used as clinker, and compared with raw materials, a low-temperature glaze firing and rapid firing process can be adopted in firing, so that the loss of the clinker in firing is less, and the clinker is also beneficial to reducing glaze defects. The XW-1816 frit is taken as a main component to endow the matt glaze with basic glossiness, color development and fineness. The XT-1705 frit plays a main adjusting role, optimizes the fineness and the glossiness of the matte overglaze and does not cause crystallization problem. Zirconium silicate is used for improving whiteness of the matte overglaze and adjusting thermal stability of the matte overglaze, and air knife soil is used for improving suspension property of the glaze.
The chemical composition of the XT-1705 frit comprises in weight percent: siO (SiO) 2 57%~62%、Al 2 O 3 5.7%~7%、Fe 2 O 3 0.08%~0.12%、MgO 1.3%~1.45%、CaO 8.5%~9.2%、Na 2 O 0.2%~0.3%、K 2 O 3.5%~4.2%、ZrO 2 0~0.15%、BaO 3%~5%、ZnO 10%~13%、B 2 O 3 4 to 6 percent, 0.1 to 0.3 percent of burning loss and the balance of impurities. The XT-1705 frit has high zinc oxide content, can play a role of fluxing agent and improve the glossiness of the overglaze, and compared with the method of introducing zinc oxide by adding calcined zinc oxide, the method of introducing zinc oxide into the frit can effectively avoid crystallization, and the properties of each component in the XT-1705 frit are more stable after high-temperature calcination. The potassium oxide in the XT-1705 frit also acts as a fluxing agent. In addition, the barium oxide in the XT-1705 frit can improve the fineness of the glaze layer and reduce the appearance of orange peel texture.
In one embodiment, the XT-1705 frit is prepared from the following raw materials in parts by weight: 25-30 parts of potassium feldspar, 3-5 parts of dolomite, 12-15 parts of calcite, 3-5 parts of barium carbonate, 8-10 parts of zinc oxide, 5-8 parts of boric acid and 3 parts of quartz sand0 to 35 parts of aluminum oxide, 1 to 2 parts of potassium carbonate and 1 to 3 parts of potassium carbonate. Wherein, barium carbonate can form barium oxide after melting, increases the fineness of glaze layer. Zinc oxide can form zinc aluminate spinel with aluminum oxide in the high temperature process, znO.Al 2 O 3 The crystal can improve the glossiness and the fineness of the glaze.
The chemical composition of the XW-1816 frit comprises the following components in percentage by weight: siO (SiO) 2 48%~53%、Al 2 O 3 10%~13%、Fe 2 O 3 0~0.2%、MgO 0~0.5%、CaO 7.5%~9.5%、Na 2 O 1%~1.5%、K 2 O 4%~5%、ZrO 2 0~0.2%、BaO 10%~15%、ZnO 5.5%~7.5%、B 2 O 3 2 to 4 percent, 0.06 to 0.08 percent of burning loss and the balance of impurities. The W-1816 frit has higher barium oxide content, and the barium oxide is a hard flux, has better fluxing effect at high temperature, can increase glaze gloss and improve acid and alkali resistance. The glaze material with XW-1816 frit as the main component has the characteristics of fine and smooth surface and matte.
In one embodiment, the XW-1816 frit is prepared from the following raw materials in parts by weight: 40-50 parts of potassium feldspar, 1-2 parts of dolomite, 3-5 parts of calcined bauxite, 11-14 parts of calcite, 12-16 parts of barium carbonate, 4-6 parts of zinc oxide, 2-4 parts of boric acid and 12-15 parts of quartz sand.
The surface of the matte ceramic tile is provided with an overglaze layer, and the preparation raw materials of the overglaze layer comprise the matte overglaze. The matte ceramic tile can adopt a low-temperature glaze firing and rapid firing process, can ensure that the crystallization problem does not occur, has the glossiness of 36-40 ℃ and still is in a matte range, and can obtain a matte ceramic product with higher glossiness value.
A method for preparing a matte tile as described above, comprising the steps of: covering Shi Yaguang overglaze on the surface of the green brick, and firing to obtain a finished product; the matte glaze passes through a 325 mesh screen, and the screen residue is 0.3-0.6%. In the fineness range, the obtained matte ceramic tile has no crystallization problem. When the fineness is too small, a crystallization problem occurs. When the fineness is too large, there is caused a problem that the fineness is insufficient.
Preferably, the glazing amount of the matte overglaze is 100-110 g/(300 mm by 600 mm). When the glazing amount is too large, the crystallization problem is caused. If the glazing quantity is too small, the smoothness of the surface of the glaze layer can be affected, and the glazing difficulty is increased.
Preferably, the firing time of the matte ceramic tile is 40-50 min. If the firing time is too long, the glaze layer is easy to be crystallized; if the time is too short, firing may be incomplete.
Preferably, the firing temperature of the matte ceramic tile is 1060-1075 ℃. If the firing temperature is too high, crystallization problems tend to occur.
The invention is further illustrated by the following examples and comparative examples:
example 1
The preparation method of the matte ceramic tile comprises the following steps: the matt glaze is spread on the green bricks, and the green bricks are fired for 50min at 1075 ℃.
Wherein the glazing amount of the matte surface glaze is 110 g/(300 mm x 600 mm); the matte glaze passes through a 325 mesh screen, and the screen residue is 0.6%.
The formula of the matte surface glaze is shown in the table I, the chemical composition ratio of the XT-1705 frit is shown in the table II, and the chemical composition ratio of the XW-1816 frit is shown in the table III.
Example 2
The preparation method of the matte ceramic tile comprises the following steps: the matt glaze is spread on the green bricks, and the green bricks are fired for 50min at 1060 ℃.
Wherein the glazing amount of the matte surface glaze is 100 g/(300 mm x 600 mm); the matte glaze passes through a 325 mesh screen, and the screen residue is 0.3%.
The formula of the matte surface glaze is shown in the table I, the chemical composition ratio of the XT-1705 frit is shown in the table II, and the chemical composition ratio of the XW-1816 frit is shown in the table III.
Example 3
The preparation method of the matte ceramic tile comprises the following steps: and (3) spreading matte glaze on the green bricks, and firing for 45min at 1075 ℃.
Wherein the glazing amount of the matte surface glaze is 100 g/(300 mm x 600 mm); the matte glaze passes through a 325 mesh screen, and the screen residue is 0.6%.
The formula of the matte surface glaze is shown in the first table, the chemical composition ratio of the XT-1705 frit is shown in the second table, and the chemical composition ratio of the XW-1816 frit is shown in the third table.
List one
Unit (portion)
|
Example 1
|
Example 2
|
Example 3
|
XW-1816 frit
|
69
|
72
|
66
|
Zirconium silicate
|
12
|
11
|
14
|
Air knife soil
|
6
|
7
|
5
|
XT-1705 frit
|
13
|
10
|
15 |
Watch II
%
|
Example 1
|
Example 2
|
Example 3
|
SiO 2 |
60.03
|
57
|
61.7
|
Al 2 O 3 |
6.53
|
6.9
|
5.7
|
Fe 2 O 3 |
0.11
|
0.08
|
0.1
|
MgO
|
1.39
|
1.42
|
1.3
|
CaO
|
9.06
|
9.12
|
8.5
|
Na 2 O
|
0.28
|
0.3
|
0.2
|
K 2 O
|
3.9
|
3.5
|
4.2
|
ZrO 2 |
0.12
|
0.1
|
0.13
|
BaO
|
3.27
|
4.5
|
3
|
ZnO
|
10.11
|
12.86
|
10
|
B 2 O 3 |
4.93
|
4
|
5
|
Burning loss
|
0.24
|
0.2
|
0.14
|
Impurity(s)
|
0.03
|
0.02
|
0.03 |
Watch III
Comparative example 1
A matt tile was prepared in the same manner as in example 1, with the difference that: frit a was used instead of XT-1705 frit.
The chemical composition ratio of the frit A is shown in Table IV.
Comparative example 2
A matt tile was prepared in the same manner as in example 1, with the difference that: frit B was used instead of XT-1705 frit.
The chemical composition ratio of the frit B is shown in Table IV.
Comparative example 3
A matt tile was prepared in the same manner as in example 1, with the difference that: frit C was used instead of XT-1705 frit.
The chemical composition ratio of the frit C is shown in Table IV.
Table four
Comparative example 4
A matt tile was prepared in the same manner as in example 1, with the difference that: the formulation of the matte overglaze was different, in this comparative example, frit D and calcined zinc oxide were used instead of XT-1705 frit. The formula of the matte overglaze is shown in Table five, and the chemical composition ratio of the frit D is shown in Table four.
Comparative example 5
A matt tile was prepared in the same manner as in example 1, with the difference that: the formulation of the matte overglaze is different, and the formulation of the matte overglaze is shown in a fifth table.
Comparative example 6
A matt tile was prepared in the same manner as in example 1, with the difference that: the formulation of the matte overglaze is different, and the formulation of the matte overglaze is shown in a fifth table.
Comparative example 7
A matt tile was prepared in the same manner as in example 1, with the difference that: the formulation of the matte overglaze is different, and the formulation of the matte overglaze is shown in a fifth table.
TABLE five
Comparative example 8
A matt tile was prepared in the same manner as in example 1, with the difference that: the fineness requirement of the matte overglaze is that the overglaze passes through a mesh screen with 325 meshes, and the screen residue is 0.1-0.2%.
Comparative example 9
A matt tile was prepared in the same manner as in example 1, with the difference that: the glazing amount of the matte overglaze is 130 g/(300 mm by 600 mm).
Comparative example 10
A matt tile was prepared in the same manner as in example 1, with the difference that: the firing time of the matte ceramic tile is 60 minutes.
Comparative example 11
A matt tile was prepared in the same manner as in example 1, with the difference that: the firing temperature of the matte ceramic tile is 1130 ℃.
The gloss, fineness, heat stability and whiteness of examples 1 to 3 were measured.
The gloss and the fineness of comparative examples 1 to 3 were measured.
The gloss, fineness, heat stability and whiteness of comparative examples 4 to 7 were measured.
The glossiness is measured by adopting a glossiness meter, and 5 points of the matte ceramic tile glaze are randomly selected to measure the glossiness.
Measurement of the smoothness of the surface was observed by visual inspection.
The measurement of the thermal stability was carried out with reference to GB/T-3810.9-2016.
Whiteness is measured using a whiteness meter.
The corresponding detection results are shown in a sixth table and a seventh table respectively.
TABLE six
|
Gloss level
|
Fineness degree
|
Example 1
|
36-40
|
Visual inspection of normal
|
Example 2
|
36-39
|
Visual inspection of normal
|
Example 3
|
36-40
|
Visual inspection of normal
|
Comparative example 1
|
30-34
|
Visual inspection of normal
|
Comparative example 2
|
29-31
|
Visual inspection of normal
|
Comparative example 3
|
36-40
|
Visual inspection of orange peel is obvious |
Watch seven
|
Gloss level
|
Fineness degree
|
Thermal stability
|
Whiteness degree
|
Example 1
|
36-40
|
Visual inspection of normal
|
Qualified product
|
79
|
Example 2
|
36-39
|
Visual inspection of normal
|
Qualified product
|
78
|
Example 3
|
36-40
|
Visual inspection of normal
|
Qualified product
|
78
|
Comparative example 4
|
36-39
|
With crystallization points
|
Qualified product
|
77
|
Comparative example 5
|
36-40
|
Visual inspection of normal
|
Failure to pass
|
76
|
Comparative example 6
|
40-48
|
Polarized light and obvious wavy shape
|
Qualified product
|
78
|
Comparative example 7
|
36-40
|
Visual inspection of normal
|
Failure to pass
|
72 |
Referring to tables six and seven, the gloss of the matt tile obtained by firing examples 1 to 3 was stable between 36 and 40 degrees, and was satisfactory (the gloss was 36 degrees or more in the matt range in export to korea), and the fineness was normal (see fig. 1), the heat stability was satisfactory, and there was no crystallization problem.
The comparative example 1 uses a frit A, the magnesia content in the frit A is higher than that of the XT-1705 frit, the obtained glaze gloss is lower than 36 degrees, and the product requirement cannot be met.
The comparative example 2 uses a frit B, the zirconia content in the frit B is higher than that of the XT-1705 frit, the obtained glaze gloss is also lower than 36 degrees, and the product requirement cannot be met.
Comparative example 3 used a frit C having a lower barium oxide content than the XT-1705 frit, and a glaze having a pronounced orange peel (see fig. 2) although the gloss was satisfactory.
Comparative example 4 uses the frit D and calcined zinc oxide to adjust the gloss of the glaze, and although the gloss can meet the requirement, there is a problem of crystallization (see fig. 3).
Comparative examples 5 and 7 have lower zirconium silicate content and higher XW-1816 frit content than example 1, and although the gloss and fineness are satisfactory, they are inferior in heat stability.
Comparative example 6 has a higher content of XT-1705 frit and a lower content of XW-1816 frit, compared to example 1, and has an excessive gloss, unsatisfactory, and a pronounced moire pattern on the glaze.
Referring to fig. 4-7, there are physical diagrams of the matt ceramic tile of comparative example 8, comparative example 9, comparative example 10 and comparative example 11, respectively, and it can be seen from the diagrams that the comparative examples 8-11 all have obvious crystallization problems, which indicate that the crystallization problems are caused when the fineness of the matt overglaze is too low, the glazing amount is too much, the firing time of the matt ceramic tile is too long or the firing temperature is too high.
In conclusion, the matte glaze provided by the invention effectively solves the crystallization problem by matching the XW-1816 frit with the XT-1705 frit, and meanwhile, the glossiness of the matte glaze can be improved without affecting the fineness and the thermal stability of the glaze. The invention also provides a matte ceramic tile, and the quality of the matte ceramic tile is further stabilized by optimizing the preparation method of the matte ceramic tile, so that the crystallization problem after firing is avoided.
It will be understood that equivalents and modifications will occur to those skilled in the art in light of the present invention and their spirit, and all such modifications and substitutions are intended to be included within the scope of the present invention as defined in the following claims.