CN115340358B - Crystal jade material with smooth and white appearance and preparation method thereof - Google Patents

Crystal jade material with smooth and white appearance and preparation method thereof Download PDF

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Publication number
CN115340358B
CN115340358B CN202211283046.XA CN202211283046A CN115340358B CN 115340358 B CN115340358 B CN 115340358B CN 202211283046 A CN202211283046 A CN 202211283046A CN 115340358 B CN115340358 B CN 115340358B
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blank
white
layer
parts
glaze
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CN115340358A (en
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蓝胥元
梁伟鸿
贺鸿斌
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Guangdong Sanfi Ceramics Group Co ltd
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Guangdong Sanfi Ceramics Group Co ltd
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Abstract

The invention discloses a brilliant jade material with a white and smooth appearance and a preparation method thereof, and belongs to the technical field of artificial stones. The invention comprises a blank layer, a pattern layer distributed on the surface of the blank and a surface glaze layer distributed on the surface of the pattern layer, wherein the blank layer comprises blank powder and a pigment, and the blank powder comprises the following raw materials in parts by weight: 20 to 30 parts of ultrawhite kaolin, 5 to 8 parts of high-plasticity mud, 5 to 10 parts of ceramic black mud, 18 to 30 parts of high-white frit, 15 to 25 parts of high-white potassium sodium sand, 0 to 5 parts of wollastonite, 0 to 5 parts of high-white bentonite and 0.2 to 0.5 part of blank reinforcing agent. The crystal jade material prepared by the method has the advantages of white appearance, jade-like texture, richer pattern layers and closer to the natural texture of marble.

Description

Crystal jade material with smooth and white appearance and preparation method thereof
Technical Field
The invention relates to the technical field of artificial stones, in particular to a brilliant jade material with a white and smooth appearance and a preparation method thereof.
Background
The natural marble belongs to medium-hard stone, is metamorphic rock formed by the original rock in the crust through the action of high temperature and high pressure in the crust, and mainly comprises calcite, limestone, serpentine and dolomite. The decorative plate has high hardness, good hand feeling, natural patterns and good appearance, and is widely used in the field of interior decoration. However, natural marble has high manufacturing cost and is difficult to process into a large-scale rock plate material; therefore, artificial rock plate materials having a marble appearance have been produced. The artificial marble slab material has relatively low cost, and different marble grains can be customized according to market demands. In addition, the artificial marble rock plate material is formed by artificial firing, and a large rock plate can be prepared by changing the size of the blank body, so that the application range in the field is expanded.
The Chinese patent CN114380625A provides a full-body rock plate and a preparation method thereof, and the full-body rock plate provided by the invention sequentially comprises a blank layer, a ground glaze layer, a surface glaze layer and a dry grain layer from bottom to top; the dry particle layer is formed by spraying dry particles, and the application amount of the dry particles is 180 to 220g/m 2 The expansion coefficient of the dry granules is 230 to 275/DEG C, and the granularity of the dry granules is 100 to 300 meshes; according to the technical scheme, the dry particle layer is added to the whole rock plate, so that the prepared product has a good quicksand effect, excellent wear resistance and flatness, and high antifouling grade; in addition, the invention also provides a preparation method of the full-body rock plate, and the preparation method adopts ink-jet printing and appliesThe mold effect ensures that the prepared full-body rock plate has a full body with high precision, is simple to operate, has low requirement on equipment and high preparation efficiency, and is beneficial to mass production.
Chinese patent CN106187212A discloses a method for preparing a full body marble tile, which combines a dry color mixing process and a three-dimensional distribution process to prepare a blank, applying a cover glaze on the surface of the blank, then sequentially spraying a stripping ink and a stripping glaze on the surface of the cover glaze, and finally firing to obtain the full body marble tile. The method is simple, energy-saving and environment-friendly, breaks through the bottleneck of the traditional process, and is widely applied, the texture of the natural stone is really restored by the prepared ceramic tile, and the ceramic tile is attractive in whole, more vivid in space decoration effect and more textured.
Chinese patent CN107500744A discloses an imitation marble whole body ceramic tile and a preparation method thereof, which comprises a whole body tile blank layer and a cover glaze layer arranged on the whole body tile blank layer, wherein the whole body tile blank layer comprises 22 to 40 percent of potassium sand, 15 to 30 percent of potassium-sodium feldspar, 10 to 20 percent of potassium feldspar, 10 to 22 percent of black mud, 2 to 10 percent of kaolin, 2 to 6 percent of bentonite, 1 to 4 percent of raw talc and 2 to 10 percent of pigment according to the weight percentage of the raw materials; the overglaze layer comprises, by weight, 30-60% of potash feldspar, 15-30% of kaolin, 5-10% of wollastonite, 5-10% of alumina, 2-8% of talc, 2-10% of zinc oxide and 10-20% of calcium carbonate. The invention solves the problem that the whole ceramic tile is difficult to oxidize in the firing process, can prepare the whole ceramic tile with the thickness of more than 1cm, has good oxidation performance, is not easy to generate pinholes, black lines, bubbles and the like in the intermediate layer, and simultaneously solves the problem that the surface glaze texture of the whole ceramic tile cannot reach the surface texture of natural marble by adjusting the components and the proportion of the surface glaze, so that the surface texture of the whole ceramic tile is closer to the surface texture of the natural marble.
It can be seen from the above disclosure that the application system is commonly used in the art to form marble patterns and various different types of glaze layers on the surface of a green body. The technical problem to be solved in the prior art is mainly to improve the performance of a glaze layer, and in the actual firing process, because the green body pattern, the glaze layer pattern and the ink-jet printing pattern are different in properties, the sintering process of the components in the same temperature environment is difficult to unify, so that the patterns of each layer of a finished product deviate, the green body pattern and other patterns are difficult to be in one-to-one correspondence, the staggered pattern is generated, and the attractiveness is influenced.
Disclosure of Invention
In view of the above-mentioned defects of the prior art, the present invention provides a brilliant jade material with a white appearance and a marble texture and a preparation method thereof.
A crystal jade material with a white and moist appearance comprises a blank body layer, a pattern layer and a surface glaze layer, wherein the pattern layer is distributed on the surface of the blank body; the green body layer comprises green powder and pigment; the blank powder comprises the following raw materials in parts by weight:
20 to 30 parts of ultrawhite kaolin, 5 to 8 parts of high-plasticity mud, 5 to 10 parts of ceramic black mud, 18 to 30 parts of high-white frit, 15 to 25 parts of high-white potassium sodium sand, 0 to 5 parts of wollastonite, 0 to 5 parts of high-white bentonite and 0.2 to 0.5 part of blank reinforcing agent.
Preferably, the iron content of the ultrawhite kaolin, the high plasticity mud, the ceramic black mud and the high white bentonite is less than 0.2wt%, and the iron content of the high white potassium-sodium sand is less than 0.1wt%.
In the process of firing the crystal jade material, the blank, the glaze layer and the pattern can bear larger temperature change, the thickness of the blank is higher than that of the pattern, and due to different heating degrees, the difference of thermal stress among the layers is large, and the pattern is distorted and deviated in severe cases. Moreover, the overgrowth of ceramic grains is not beneficial to keeping the marble patterns consistent, the shrinkage rate of the ceramic is too large, and the originally designed patterns are distorted and deformed along with the shrinkage, so that the quality of finished products is uneven.
In order to solve the technical problem of excessive growth of ceramic grains, tiO is adopted in the invention 2 、Y 2 O 3 As a component of the green body reinforcing agent, a certain liquid phase is formed in the sintering process to help the densification of the ceramic. TiO 2 2 Provide good connection between ceramic grains, with Y 2 O 3 The combined action of the two components can limit the growth of ceramic grains and inhibit the formation of loose stacking structureThe grain size of the ceramic crystal grains is reduced, the microstructure is uniform and compact, and the finished product shows jade texture.
Preferably, the green body reinforcing agent is Y-alpha-SiAlON or TiO 2 、Y 2 O 3 And (2) mixing the following components in a mass ratio of 5-12.5: 4 to 7:2 to 4, wherein the three components are all powder.
TiO 2 、Y 2 O 3 Although the growth of ceramic grains can be limited, densification and strength of finished products are facilitated, the effect of preventing pattern deviation and dislocation is limited. The inventors found that this phenomenon is caused by TiO 2 、Y 2 O 3 The thermal conductivity of the green body is reduced and the firing shrinkage is increased. The thermal conductivity of the green body is related to grain boundaries and lattice oxygen, the lattice oxygen occupies a dominant position in influencing the thermal conductivity, and the oxidation phase with low thermal conductivity reduces the thermal conductivity of the ceramic; furthermore, tiO is added 2 、Y 2 O 3 Then, the transient oxidation liquid phase formed by the two in the sintering process can not only cause larger shrinkage in the sintering process, but also generate excessive crystal boundaries to block heat conduction, so that the thermal stress received by the blank, the pattern layer and the like is unequal; under the combined action of the two, the uniformity of the pattern is difficult to optimize.
Therefore, compared with metal oxides, the addition of the Y-alpha-SiAlON can reduce the content of lattice oxygen, improve the heat-conducting property of the ceramic, more effectively transfer heat inside the ceramic and prevent deformation caused by non-uniform heating degree. As the temperature increases, Y-alpha-SiAlON does not participate in TiO 2 、Y 2 O 3 A process that forms a uniform transient liquid phase, but slowly dissolves in the liquid phase over time; therefore, under the same conditions, the content of transient liquid phase in the ceramic is lower than that of the transient liquid phase in the ceramic only by adding TiO 2 、Y 2 O 3 Thereby reducing the firing shrinkage. Meanwhile, the Y-alpha-SiAlON reduces the growth space of large-size columnar grains and is in contact with TiO in the process of promoting the densification of the ceramic 2 、Y 2 O 3 Has the same function, and the addition of the substance does not cause the mechanical property of the ceramicIs reduced.
Further preferably, the Y-alpha-SiAlON is prepared by the following method:
silicon, aluminum, silicon nitride, silicon dioxide and yttrium oxide are mixed according to a molar ratio of 10:5:3.3:0.7:0.4 until all the components are uniformly dispersed, wherein all the raw materials are powdery and have the average grain diameter of less than 1 mu m; sintering the mixed raw material under the pressure of 30-50MPa, firstly heating the mixed raw material from normal temperature to 550-650 ℃ at the heating rate of 110-120 ℃/min, then heating the mixed raw material to 1350-1400 ℃ at the heating rate of 20-30 ℃/min, keeping the temperature for 10-15min, finally cooling the sintered blank to normal temperature at the cooling rate of 50-75 ℃/min, and grinding and crushing to obtain the Y-alpha-SiAlON.
The preparation method of the crystal jade material with the white and smooth appearance comprises the following steps:
s1, mixing and ball-milling a blank powder material, a pigment and water to obtain blank slurry, and spraying powder to the blank slurry through a spray granulation tower to prepare a blank;
s2, forming textures on the blank by using a digital material distributing machine and pressing to obtain a blank layer and a pattern layer distributed on the surface of the blank;
s3, applying a surface glaze on the surface of the pattern layer to obtain a surface glaze layer applied on the surface of the pattern layer;
s4, printing ink-jet patterns on the overglaze layer in an aligned mode, wherein the ink-jet patterns are consistent with the pattern layer; continuously applying glaze after the pattern is sprayed to obtain a tile blank;
and S5, firing the ceramic tile blank to obtain the crystal jade material with a white and moist appearance.
Preferably, the grain composition mass percentage of the base powder material in step S1 is as follows: less than or equal to 2 percent of 20 meshes, 3 to 8 percent of 30 meshes, 30 to 40 percent of 40 meshes, 40 to 50 percent of 60 meshes, less than or equal to 10 percent of 100 meshes, and less than 2 percent of more than 100 meshes.
Preferably, the thickness of the green body layer in the step S2 is 6 to 30mm.
Preferably, the green strength of the green body layer in step S2 is >0.5MPa and the dry strength is >3MPa.
Preferably, the moisture content of the green body layer in the step S2 is 8.5-9.5%.
Preferably, the glaze in step S4 is any one of protective glaze, glaze polishing, dry particle polishing and antique dry particle.
Preferably, the firing temperature in the step S5 is 1160-1220 ℃, and the firing time is 1.5-2.5 h.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The introduction and the function of part of raw materials in the formula of the invention are as follows:
ultra white kaolin: a non-metal mineral is a kind of clay and claystone mainly made of kaolinite group clay mineral, so it is white and fine, so it is also called as dolomite. The pure kaolin is in a white, fine and soft soil shape and has good physical and chemical properties such as plasticity, fire resistance and the like.
High plasticity mud: one kind of ceramic mud has higher plasticity than that of common ceramic mud, and the main mineral component of the ceramic mud is montmorillonite, so that the ceramic mud has higher bearing capacity.
Wollastonite: wollastonite is an inorganic acicular mineral, belongs to a chain metasilicate, and is fibrous and acicular. Its advantages are no poison, high resistance to chemical corrosion, high thermal stability and size stability, high lustre to glass and pearl, low water absorption and oil absorption, and high mechanical and electric performance.
High-whiteness bentonite: the non-metallic mineral product mainly composed of montmorillonite has hygroscopicity and expansibility, can absorb water with volume of 8 to 15 times of the self volume, and has volume expansion of several times to 30 times. In water medium, the bentonite can be dispersed into a gelatinous state and a suspended state, the mixed solution has certain viscosity, thixotropy and lubricity, and the mixed solution is bonded with water, mud, sand and other fine crumbs and has better plasticity and better cohesiveness.
The invention has the beneficial effects that:
compared with the prior art, the invention takes the ultra-white kaolin, the high-plasticity mud, the ceramic black mud, the high-white frit, the high-white potassium sodium sand, the wollastonite, the high-white bentonite and the green body reinforcing agent as the green powder to prepare the crystal jade material with a white and moist appearance, a jade-like texture, and richer pattern levels which are more similar to the natural texture of the marble.
Compared with the prior art, the green body reinforcing agent with a specific substance proportion is adopted, a certain liquid phase is formed in the sintering process, the ceramic is densified, good connection is provided among ceramic crystal grains, the growth of the ceramic crystal grains and the formation of a loose stacking structure are limited, the grain size of the ceramic crystal grains is reduced, the microstructure is uniform and dense, and the finished product has jade texture.
Compared with the prior art, the blank reinforcing agent disclosed by the invention has the advantages that the content of generated lattice oxygen is low, the heat conducting property of the ceramic is improved, heat can be more effectively transferred in the ceramic, and deformation caused by non-uniform heating degree is prevented; the green body reinforcing agent reduces the content of transient liquid phase formed in the ceramic, reduces the firing shrinkage rate and improves the matching degree of marble patterns.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the invention thereto. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Some raw material parameters in the comparative examples and examples of the invention are as follows:
ultrawhite kaolin, cat No.: glt-0046, whiteness: 88 to 89% by weight, provided by Gangshou county Yuanda Muscovitum;
high plasticity mud, provided by Lingshou county color Rui mineral processing factories;
ceramic black mud, type: DC-812, whiteness: 38 to 45 percent, provided by eastern porcelain ceramics of Dongguan city, inc.;
high white frit, type: 808, new materials of Foshan Fuyu, inc.;
high-whiteness sodium-potassium sand, whiteness: 70 percent, provided by Jiangxi province Jia and mining company Limited;
wollastonite, CAS number: 13983-17-0 percent, the whiteness is more than 90 percent and is provided by Hebei yuran building materials science and technology company;
high-white bentonite, CAS No.: 1302-78-9, whiteness: 70 percent of the total nutrient provided by Shuangcheng bridge area Shuangcheng bentonite powder factories.
Example 1
A crystal jade material with a white and smooth appearance is prepared by the following method:
s1, mixing and ball-milling a blank powder material, a pigment and water to obtain blank slurry, and spraying powder to the blank slurry through a spray granulation tower to prepare a blank;
s2, forming textures on the blank by using a digital material distributor and pressing the blank to obtain a blank layer and a pattern layer distributed on the surface of the blank, wherein the thickness of the blank layer is 12mm, and the moisture content of the blank layer is 9%;
s3, applying overglaze on the surface of the pattern layer to obtain an overglaze layer applied on the surface of the pattern layer;
s4, printing ink-jet patterns on the overglaze layer in an aligned mode, wherein the ink-jet patterns are consistent with the pattern layer; continuously applying protective glaze after the pattern is sprayed to obtain a tile blank;
and S5, firing the ceramic tile blank at 1200 ℃ for 1.5h to obtain the crystal jade material with a white appearance.
The blank powder is as follows: 25kg of ultrawhite kaolin, 6.5kg of high plastic mud, 7.5kg of ceramic black mud, 24kg of high white clinker, 20kg of high white potassium sodium sand, 2.5kg of wollastonite, 2.5kg of high white bentonite and 0.5kg of green body reinforcing agent.
The iron content of the ultrawhite kaolin, the high plasticity mud, the ceramic black mud and the high white bentonite is less than 0.2wt%, and the iron content of the high white potassium-sodium sand is less than 0.1wt%.
The grain composition mass percentage of the blank powder material is as follows: the content of 20 meshes is 1%, the content of 30 meshes is 3%, the content of 40 meshes is 40%, the content of 60 meshes is 50%, the content of 100 meshes is 5%, and the content of more than 100 meshes is 1%.
The green body reinforcing agent is TiO 2 、Y 2 O 3 According to the mass ratio of 6:3.5, both the above two ingredients are in powder form.
Example 2
A crystal jade material with a white and smooth appearance is prepared by the following method:
s1, mixing and ball-milling a blank powder material, a pigment and water to obtain blank slurry, and spraying powder to the blank slurry through a spray granulation tower to prepare a blank;
s2, forming textures on the blank by using a digital material distributor and pressing to obtain a blank layer and a pattern layer distributed on the surface of the blank, wherein the thickness of the blank layer is 12mm, and the moisture content of the blank layer is 9%;
s3, applying overglaze on the surface of the pattern layer to obtain an overglaze layer applied on the surface of the pattern layer;
s4, printing ink-jet patterns on the overglaze layer in an aligned mode, wherein the ink-jet patterns are consistent with the pattern layer; continuously applying protective glaze after the pattern is sprayed to obtain a tile blank;
and S5, firing the ceramic tile blank at 1200 ℃ for 1.5h to obtain the crystal jade material with a white appearance.
The blank powder is as follows: 25kg of ultrawhite kaolin, 6.5kg of high plasticity mud, 7.5kg of ceramic black mud, 24kg of high white clinker, 20kg of high white potassium sodium sand, 2.5kg of wollastonite, 2.5kg of high white bentonite and 0.5kg of blank reinforcing agent.
The iron content of the ultrawhite kaolin, the high plasticity mud, the ceramic black mud and the high white bentonite is less than 0.2wt%, and the iron content of the high white potassium sodium sand is less than 0.1wt%.
The grain composition mass percentage of the blank powder material is as follows: 20 mesh is 1%,30 mesh is 3%,40 mesh is 40%,60 mesh is 50%,100 mesh is 5%, and more than 100 mesh is 1%.
The green body reinforcing agent is Y-alpha-SiAlON or TiO 2 According to the mass ratio of 10.5:3.5, both the above two ingredients are in powder form.
The Y-alpha-SiAlON is prepared by adopting the following method: silicon, aluminum, silicon nitride, silicon dioxide and yttrium oxide are mixed in a molar ratio of 10:5:3.3:0.7:0.4 until all the components are uniformly dispersed, wherein all the raw materials are powdery and have the average grain diameter of less than 1 mu m; sintering the mixed raw material under the pressure of 40MPa, firstly heating the mixed raw material from normal temperature to 600 ℃ at the heating rate of 115 ℃/min, then heating the mixed raw material to 1350 ℃ at the heating rate of 25 ℃/min, keeping the temperature for 10min, finally cooling the sintered blank to normal temperature at the cooling rate of 50 ℃/min, and grinding and crushing to obtain the Y-alpha-SiAlON.
Example 3
A crystal jade material with a white and smooth appearance is prepared by the following method:
s1, mixing and ball-milling a blank powder material, a pigment and water to obtain blank slurry, and spraying powder to the blank slurry through a spray granulation tower to prepare a blank;
s2, forming textures on the blank by using a digital material distributor and pressing to obtain a blank layer and a pattern layer distributed on the surface of the blank, wherein the thickness of the blank layer is 12mm, and the moisture content of the blank layer is 9%;
s3, applying a surface glaze on the surface of the pattern layer to obtain a surface glaze layer applied on the surface of the pattern layer;
s4, printing ink-jet patterns on the overglaze layer in an aligned mode, wherein the ink-jet patterns are consistent with the pattern layer; continuously applying protective glaze after the pattern is sprayed to obtain a tile blank;
and S5, firing the ceramic tile blank at 1200 ℃ for 1.5h to obtain the crystal jade material with a white appearance.
The blank powder is as follows: 25kg of ultrawhite kaolin, 6.5kg of high plasticity mud, 7.5kg of ceramic black mud, 24kg of high white clinker, 20kg of high white potassium sodium sand, 2.5kg of wollastonite, 2.5kg of high white bentonite and 0.5kg of blank reinforcing agent.
The iron content of the ultrawhite kaolin, the high plasticity mud, the ceramic black mud and the high white bentonite is less than 0.2wt%, and the iron content of the high white potassium sodium sand is less than 0.1wt%.
The grain composition mass percentage of the blank powder material is as follows: 20 mesh is 1%,30 mesh is 3%,40 mesh is 40%,60 mesh is 50%,100 mesh is 5%, and more than 100 mesh is 1%.
The green body reinforcing agent is Y-alpha-SiAlON or Y 2 O 3 According to the mass ratio of 10.5:3.5, both the above two ingredients are in powder form.
The Y-alpha-SiAlON is prepared by adopting the following method: silicon, aluminum, silicon nitride, silicon dioxide and yttrium oxide are mixed according to a molar ratio of 10:5:3.3:0.7:0.4 until all the components are uniformly dispersed, wherein all the raw materials are powdery and have the average grain diameter of less than 1 mu m; sintering the mixed raw material under the pressure of 40MPa, firstly heating the mixed raw material from normal temperature to 600 ℃ at the heating rate of 115 ℃/min, then heating the mixed raw material to 1350 ℃ at the heating rate of 25 ℃/min, keeping the temperature for 10min, finally cooling the sintered blank to normal temperature at the cooling rate of 50 ℃/min, and grinding and crushing to obtain the Y-alpha-SiAlON.
Example 4
A crystal jade material with a white and smooth appearance is prepared by the following method:
s1, mixing and ball-milling a blank powder material, a pigment and water to obtain blank slurry, and spraying powder to the blank slurry through a spray granulation tower to prepare a blank;
s2, forming textures on the blank by using a digital material distributor and pressing to obtain a blank layer and a pattern layer distributed on the surface of the blank, wherein the thickness of the blank layer is 12mm, and the moisture content of the blank layer is 9%;
s3, applying overglaze on the surface of the pattern layer to obtain an overglaze layer applied on the surface of the pattern layer;
s4, printing ink-jet patterns on the overglaze layer in an aligned mode, wherein the ink-jet patterns are consistent with the pattern layer; continuously applying protective glaze after the pattern is sprayed to obtain a tile blank;
and S5, firing the ceramic tile blank for 1.5 hours at 1200 ℃ to obtain the crystal jade material with a white and moist appearance.
The blank powder is as follows: 25kg of ultrawhite kaolin, 6.5kg of high plastic mud, 7.5kg of ceramic black mud, 24kg of high white clinker, 20kg of high white potassium sodium sand, 2.5kg of wollastonite, 2.5kg of high white bentonite and 0.5kg of green body reinforcing agent.
The iron content of the ultrawhite kaolin, the high plasticity mud, the ceramic black mud and the high white bentonite is less than 0.2wt%, and the iron content of the high white potassium sodium sand is less than 0.1wt%.
The grain composition mass percentage of the blank powder material is as follows: 20 mesh is 1%,30 mesh is 3%,40 mesh is 40%,60 mesh is 50%,100 mesh is 5%, and more than 100 mesh is 1%.
The green body reinforcing agent is Y-alpha-SiAlON or TiO 2 、Y 2 O 3 According to the mass ratio of 10.5:6:3.5 formation ofThe mixture of (1), wherein all three components are in powder form.
The Y-alpha-SiAlON is prepared by adopting the following method: silicon, aluminum, silicon nitride, silicon dioxide and yttrium oxide are mixed in a molar ratio of 10:5:3.3:0.7:0.4 until all the components are uniformly dispersed, wherein all the raw materials are powdery and have the average grain diameter of less than 1 mu m; sintering the mixed raw material under the pressure of 40MPa, firstly heating the mixed raw material from normal temperature to 600 ℃ at the heating rate of 115 ℃/min, then heating the mixed raw material to 1350 ℃ at the heating rate of 25 ℃/min, keeping the temperature for 10min, finally cooling the sintered blank to normal temperature at the cooling rate of 50 ℃/min, and grinding and crushing to obtain the Y-alpha-SiAlON.
Comparative example 1
A crystal jade material with a white and smooth appearance is prepared by the following method:
s1, mixing and ball-milling a blank powder material, a pigment and water to obtain blank slurry, and spraying powder to the blank slurry through a spray granulation tower to prepare a blank;
s2, forming textures on the blank by using a digital material distributor and pressing to obtain a blank layer and a pattern layer distributed on the surface of the blank, wherein the thickness of the blank layer is 12mm, and the moisture content of the blank layer is 9%;
s3, applying a surface glaze on the surface of the pattern layer to obtain a surface glaze layer applied on the surface of the pattern layer;
s4, printing ink-jet patterns on the overglaze layer in an aligned mode, wherein the ink-jet patterns are consistent with the pattern layer; continuously applying protective glaze after the pattern is sprayed to obtain a tile blank;
and S5, firing the ceramic tile blank at 1200 ℃ for 1.5h to obtain the crystal jade material with a white appearance.
The blank powder is as follows: 25kg of ultrawhite kaolin, 6.5kg of high plasticity mud, 7.5kg of ceramic black mud, 24kg of high white clinker, 20kg of high white potassium sodium sand, 2.5kg of wollastonite and 2.5kg of high white bentonite.
The iron content of the ultrawhite kaolin, the high plasticity mud, the ceramic black mud and the high white bentonite is less than 0.2wt%, and the iron content of the high white potassium sodium sand is less than 0.1wt%.
The grain composition mass percentage of the blank powder material is as follows: 20 mesh is 1%,30 mesh is 3%,40 mesh is 40%,60 mesh is 50%,100 mesh is 5%, and more than 100 mesh is 1%.
Test example 1
The whiteness test of the crystal jade material with the white and moist appearance is carried out according to the method and the steps in recommended industry standard QB/T1503-2011 & lt method for measuring whiteness of domestic ceramics. 3 samples meeting the standard are prepared in each embodiment or the comparison example, and the size of the flat surface of each sample meets the measurement requirement of an instrument probe. The surface of the sample to be measured is a white part without decoration, and the surface is clean and flat and has no cracks or other scars. For the part of the crystal jade material with the white appearance and marble lines, the matching degree between the crystal jade material and the design pattern is expressed by an integer part of 1-10 minutes, and the higher the score is, the better the matching degree is; the 1 to 4 marks represent that the grain pattern has distortion and staggered layers and has poor correspondence; 5 to 8 minutes represent that a small part of the grain pattern has defects or fuzzy double images; the marks of 9 to 10 represent that the fit degree between the grain pattern and the design pattern is high and the consistency is strong.
The results of whiteness test and judgment of the degree of coincidence of grain and pattern of the crystal jade material with a white and glossy appearance are shown in table 1.
TABLE 1
Name(s) Whiteness degree Degree of anastomosis
Example 1 77 6
Example 2 78 7
Example 3 75 7
Example 4 80 10
Comparative example 1 73 4
According to the classification of the whiteness grades of the ceramics, the ceramic is a superior product with the whiteness of more than or equal to 75, the ceramic is an superior product with the whiteness of less than 70 and less than 75, and the ceramic is a qualified product with the whiteness of less than 70. The test results in table 1 show that the whiteness of the white crystal jade material reaches the level of the superior product.
Test example 2
The bending strength test of the crystal jade material with the white appearance is carried out according to the method and the steps in GB/T4741-1999 ceramic material bending strength test method. The length of the sample is 120mm, and the width-thickness ratio is 1:1, 10 specimens were prepared for each group. The materials and process conditions adopted for preparing the samples are the same as those of the examples and the comparative examples, and each sample is regularly processed without obvious defects. During testing, the sample is placed in an oven with the temperature of 110 +/-5 ℃, dried to constant weight and then placed in a dryer to be cooled to room temperature; placing a sample on a supporting knife edge, adjusting the distance between the supporting knife edges to ensure that the length of the sample outside the supporting knife edges is 10mm, wherein the two supporting knife edges are necessarily in the same plane and are parallel to each other, and the loading knife edge is positioned in the middle of the two supporting knife edges; and starting a bending strength testing machine, enabling an loading knife edge to be in contact with the sample without impact, loading at a constant speed of 30N/s on average until the sample is damaged, and recording the maximum load of the sample when the sample is damaged. The arithmetic mean value of the test results is taken as the bending strength value of the sample, and the data is trimmed to 0.1MPa. The bending strength test results of the white and glossy crystal jade material are shown in table 2.
TABLE 2
Name(s) Bending strength (MPa)
Example 1 43.9
Example 2 45.2
Example 3 47.4
Example 4 48.7
Comparative example 1 38.1
The examples using the green body reinforcing agent showed higher flexural strength as a whole than comparative example 1, and example 4 showed the highest flexural strength. The flexural strength during the firing of the ceramic is related to its degree of densification and the presence of structural defects. The reason why the above-mentioned results are obtained may be that TiO is added 2 、Y 2 O 3 As a component of a green body reinforcing agent, a certain liquid phase is formed in the sintering process, which is beneficial to ceramic densification; tiO 2 2 Provide good connection between ceramic grains, with Y 2 O 3 The growth of ceramic grains is limited by the combined action, and the growth of large-size columnar grains is reduced by the Y-alpha-SiAlONThe space inhibits the formation of a loose stacking structure, so that the grain size of ceramic grains is reduced, the microstructure is uniform and compact, the finished product has jade texture, and the bending strength is improved.
Test example 3
The firing shrinkage rate test of the crystal jade material with white and moist appearance is carried out according to the method and the steps in recommended industry standard QB/T1548-2015 ceramic blank linear shrinkage rate measuring method. Preparation of a sample refers to preparation of a plastic pug sample, the size of the sample is phi 60mm multiplied by 8mm, and 5 samples are prepared in each group; the materials used for the samples and the firing conditions were the same as those in each example and comparative example. The results are arithmetically averaged and are shown to the two last decimal places. The results of the test of the firing shrinkage of the crystal jade material with a white and moist appearance are shown in table 3.
TABLE 3
Name (R) Firing shrinkage (%)
Example 1 12.27
Example 2 7.12
Example 3 6.95
Example 4 4.28.
Comparative example 1 13.06
As the firing shrinkage is lower, the degree of deformation dislocation caused by shrinkage of grains of the crystal jade material is lower, and as can be seen from the results of matching degree in table 1, the shrinkage of the example to which Y- α -SiAlON is added is lower than that of the example 1 and the comparative example, wherein the shrinkage of the example 4 is the lowest, and the matching degree between the grain pattern and the design pattern is high and the uniformity is strong. The reason for this may be that TiO 2 、Y 2 O 3 The heat conductivity of the green body can be reduced, and the firing shrinkage rate can be increased; the thermal conductivity of the green body is related to grain boundaries and lattice oxygen, the lattice oxygen occupies a dominant position in influencing the thermal conductivity, and the oxidation phase with low thermal conductivity reduces the thermal conductivity of the ceramic; furthermore, tiO is added 2 、Y 2 O 3 Then, the transient oxidation liquid phase formed by the two in the sintering process can not only cause larger shrinkage in the sintering process, but also generate excessive crystal boundaries to block heat conduction, so that the thermal stress received by the blank, the pattern layer and the like is unequal; under the combined action of the two, the uniformity of the pattern is difficult to optimize. After the Y-alpha-SiAlON is added, the content of lattice oxygen is reduced, so that the heat conducting property of the ceramic is improved, heat can be more effectively transferred in the ceramic, and deformation caused by non-uniform heating degree is prevented; on the other hand, as the temperature increases, Y- α -SiAlON does not participate in TiO 2 、Y 2 O 3 Forming a uniform transient liquid phase in which Y-alpha-SiAlON is slowly dissolved over time, the content of the transient liquid phase in the ceramic is lower than that of the transient liquid phase in which only TiO is added under the same conditions 2 、Y 2 O 3 The firing shrinkage of the ceramic is reduced.

Claims (11)

1. A preparation method of a crystal jade material with a white and moist appearance is characterized by comprising the following steps:
s1, mixing and ball-milling a blank powder material, a pigment and water to obtain blank slurry, and spraying powder to the blank slurry through a spray granulation tower to prepare a blank;
s2, forming textures on the blank by using a digital material distributor and pressing to obtain a blank layer and a pattern layer distributed on the surface of the blank;
s3, applying overglaze on the surface of the pattern layer to obtain an overglaze layer applied on the surface of the pattern layer;
s4, printing ink-jet patterns on the overglaze layer in an alignment mode, wherein the ink-jet patterns are consistent with the pattern layer; continuously applying glaze after the pattern is sprayed to obtain a tile blank;
s5, firing the ceramic tile blank to obtain a crystal jade material with a white and smooth appearance;
the blank powder comprises the following raw materials in parts by weight:
20 to 30 parts of ultrawhite kaolin, 5 to 8 parts of high-plasticity mud, 5 to 10 parts of ceramic black mud, 18 to 30 parts of high-white frit, 15 to 25 parts of high-white potassium sodium sand, 0 to 5 parts of wollastonite, 0 to 5 parts of high-white bentonite and 0.2 to 0.5 part of blank reinforcing agent;
the green body reinforcing agent is Y-alpha-SiAlON or TiO 2 、Y 2 O 3 And (2) mixing the following components in a mass ratio of 5-12.5: 4 to 7:2 to 4, wherein the three components are powder;
the iron content of the ultrawhite kaolin, the high plasticity mud, the ceramic black mud and the high white bentonite is less than 0.2wt%, and the iron content of the high white potassium-sodium sand is less than 0.1wt%.
2. The method for preparing a brilliant jade material with a white and smooth appearance according to claim 1, wherein the grain composition of the green powder material in step S1 is as follows: less than or equal to 2 percent of 20 meshes, 3 to 8 percent of 30 meshes, 30 to 40 percent of 40 meshes, 40 to 50 percent of 60 meshes, less than or equal to 10 percent of 100 meshes, and less than 2 percent of more than 100 meshes.
3. The method for preparing a brilliant jade material with a white and smooth appearance according to claim 1, wherein the method comprises the following steps: and in the step S2, the thickness of the blank layer is 6 to 30mm.
4. The method for preparing a crystal jade material with a white and moist appearance according to claim 1, which is characterized in that: in the step S2, the green strength of the green body layer is more than 0.5MPa, and the drying strength is more than 3MPa; the moisture content of the blank layer is 8.5-9.5%.
5. The method for preparing a crystal jade material with a white and moist appearance according to claim 1, which is characterized in that: and step S4, the glaze is protective glaze.
6. The method for preparing a brilliant jade material with a white and smooth appearance according to claim 1, wherein the method comprises the following steps: and step S4, the glaze is polished glaze.
7. The method for preparing a brilliant jade material with a white and smooth appearance according to claim 1, wherein the method comprises the following steps: and step S4, the glaze is dry grain polishing.
8. The method for preparing a brilliant jade material with a white and smooth appearance according to claim 1, wherein the method comprises the following steps: in the step S4, the glaze is antique dry particles.
9. The method for preparing a brilliant jade material with a white and smooth appearance according to claim 1, wherein the method comprises the following steps: in the step S5, the firing temperature is 1160-1220 ℃, and the firing time is 1.5-2.5 h.
10. The method for preparing a crystal jade material with a white and smooth appearance according to claim 1, wherein the Y-alpha-SiAlON is prepared by the following method:
silicon, aluminum, silicon nitride, silicon dioxide and yttrium oxide are mixed in a molar ratio of 10:5:3.3:0.7:0.4 until all the components are uniformly dispersed, wherein all the raw materials are powdery and have the average grain diameter of less than 1 mu m; sintering the mixed raw material under the pressure of 30-50MPa, firstly heating the mixed raw material from normal temperature to 550-650 ℃ at the heating rate of 110-120 ℃/min, then heating the mixed raw material to 1350-1400 ℃ at the heating rate of 20-30 ℃/min, keeping the temperature for 10-15min, finally cooling the sintered blank to normal temperature at the cooling rate of 50-75 ℃/min, and grinding and crushing to obtain the Y-alpha-SiAlON.
11. A crystal jade material with a white and moist appearance is characterized in that: prepared by the method of any one of claims 1 to 10.
CN202211283046.XA 2022-10-20 2022-10-20 Crystal jade material with smooth and white appearance and preparation method thereof Active CN115340358B (en)

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CN115784711B (en) * 2022-12-15 2024-02-09 佛山欧神诺陶瓷有限公司 Ceramic sheet and preparation method thereof
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CN107721380A (en) * 2017-10-25 2018-02-23 武汉理工大学 A kind of preparation method of inexpensive High-Alumina ceramic thin plate
CN108285331A (en) * 2018-01-02 2018-07-17 航天特种材料及工艺技术研究所 A kind of ceramic material, preparation method and application
CN112759368A (en) * 2021-01-25 2021-05-07 中国地质大学（北京） Rare earth oxide reinforced and toughened ceramic rock plate and preparation method thereof
CN113754406A (en) * 2021-10-15 2021-12-07 广东翠贝卡建材科技有限公司 Ceramic plate with jade fish maw effect, blank, preparation method and application
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CN107721380A (en) * 2017-10-25 2018-02-23 武汉理工大学 A kind of preparation method of inexpensive High-Alumina ceramic thin plate
CN108285331A (en) * 2018-01-02 2018-07-17 航天特种材料及工艺技术研究所 A kind of ceramic material, preparation method and application
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CN112759368A (en) * 2021-01-25 2021-05-07 中国地质大学（北京） Rare earth oxide reinforced and toughened ceramic rock plate and preparation method thereof
CN113754406A (en) * 2021-10-15 2021-12-07 广东翠贝卡建材科技有限公司 Ceramic plate with jade fish maw effect, blank, preparation method and application

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