WO2024082637A1 - 一种外观润白的晶玉材料及其制备方法 - Google Patents
一种外观润白的晶玉材料及其制备方法 Download PDFInfo
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- WO2024082637A1 WO2024082637A1 PCT/CN2023/097059 CN2023097059W WO2024082637A1 WO 2024082637 A1 WO2024082637 A1 WO 2024082637A1 CN 2023097059 W CN2023097059 W CN 2023097059W WO 2024082637 A1 WO2024082637 A1 WO 2024082637A1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
- C04B2235/9615—Linear firing shrinkage
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Definitions
- the invention relates to the technical field of artificial stones, and in particular to a crystal jade material with a smooth white appearance and a preparation method thereof.
- Natural marble is a medium-hard stone. It is a metamorphic rock formed by the original rock in the earth's crust under high temperature and high pressure. It is mainly composed of calcite, limestone, serpentine and dolomite. It has high hardness, good hand feel, natural patterns and good appearance, and is widely used in the field of interior decoration.
- the manufacturing cost of natural marble is high, and it is difficult to process it into large rock slabs; therefore, artificial rock slabs with marble appearance came into being.
- the cost of artificial marble rock slabs is relatively low, and different marble patterns can be customized according to market demand.
- artificial marble rock slabs are artificially fired, and large rock slabs can be prepared by changing the size of the blank, thereby expanding the scope of application in this field.
- Chinese patent CN114380625A provides a full-body rock slab and a preparation method thereof.
- the full-body rock slab provided by the invention includes a body layer, a base glaze layer, a surface glaze layer, and a dry particle layer from bottom to top; the dry particle layer is formed by spraying dry particles, the application amount of the dry particles is 180-220 g/ m2 , the expansion coefficient of the dry particles is 230-275/°C, and the particle size of the dry particles is 100-300 meshes;
- the full-body rock slab provided by the technical solution of the invention adds a dry particle layer, so that the prepared product has a good quicksand effect, excellent wear resistance and flatness, and a high anti-fouling grade; in addition, the invention also provides a preparation method for the full-body rock slab, the preparation method adopts inkjet printing and applies a mold effect, so that the prepared full-body rock slab has a high-precision full body, and is simple to operate, has few equipment requirements, and has high preparation efficiency
- Chinese patent CN106187212A discloses a method for preparing a full-body marble tile, which combines a dry color mixing process with a three-dimensional fabric process to prepare a blank, applies a glaze on the surface of the blank, and then sprays peeling ink and peeling glaze on the surface of the glaze in sequence, and finally fires the whole body marble tile.
- the invention is simple, energy-saving and environmentally friendly, breaks through the bottleneck of traditional technology, and has a wide range of applications.
- the prepared tiles truly restore the texture of natural stone, and the overall appearance, space decoration effect is more realistic, and has a better texture.
- Chinese patent CN107500744A discloses a marble-like full-body ceramic tile and a preparation method thereof, which comprises a full-body tile green layer and a surface glaze layer applied on the full-body tile green layer, wherein the full-body tile green layer comprises, by weight percentage of raw materials, 22-40% of potassium sand, 15-30% of potassium feldspar, 10-20% of potassium feldspar, 10-22% of black mud, 2-10% of kaolin, 2-6% of bentonite, 1-4% of raw talc, and 2-10% of colorant; and the surface glaze layer comprises, by weight percentage of raw materials, 30-60% of potassium feldspar, 15-30% of kaolin, 5-10% of wollastonite, 5-10% of aluminum oxide, 2-8% of talc, 2-10% of zinc oxide, and 10-20% of calcium carbonate.
- the invention solves the problem that the whole body ceramic tile is difficult to oxidize during the firing process.
- the invention can prepare whole body ceramic tiles with a thickness greater than 1 cm.
- the whole body ceramic tiles have good oxidation performance, and the middle layer is not prone to pinholes, black lines, bubbles and the like.
- the invention solves the problem that the glaze texture of the whole body ceramic tile cannot reach the surface texture of natural marble, making the surface texture of the whole body ceramic tile closer to natural marble.
- the problem to be solved by the present invention is to provide a crystal jade material with a white appearance and a marble texture and a preparation method thereof.
- a crystal jade material with a smooth white appearance comprising a body layer, a pattern layer applied on the surface of the body, and a glaze layer applied on the surface of the pattern layer;
- the body layer comprises body powder and colorant;
- the body powder comprises the following raw materials in parts by weight:
- the iron content of the ultra-white kaolin, high plasticity mud, ceramic black mud, and 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 body, glaze layer and pattern will be subjected to large temperature changes.
- the thickness of the body is higher than the latter. Due to the different degrees of heating, the thermal stress between the layers is very different.
- the pattern will be distorted and offset. Not only that, the excessive growth of ceramic grains is not conducive to the consistency of the marble pattern.
- the shrinkage rate of ceramics is too large, and the original design pattern will be distorted and deformed with shrinkage, resulting in uneven quality of the finished product.
- the present invention uses TiO 2 and Y 2 O 3 as components of the green body reinforcing agent, forming a certain liquid phase during the sintering process to help the ceramic densification.
- TiO 2 provides a good connection between ceramic grains, and works together with Y 2 O 3 to limit the growth of ceramic grains, inhibiting the formation of loose stacking structures, reducing the size of ceramic grains, and making the microstructure uniform and dense, so that the finished product has a jade texture.
- the green body reinforcing agent is a mixture of Y- ⁇ -SiAlON, TiO 2 , and Y 2 O 3 in a mass ratio of 5-12.5:4-7:2-4, and the above three components are all in powder form.
- TiO 2 and Y 2 O 3 can limit the growth of ceramic grains, facilitate densification and enhance the strength of finished products, their role in preventing pattern deviation and staggering is relatively limited.
- the thermal conductivity of the green body is related to the grain boundary and lattice oxygen, and the lattice oxygen occupies a dominant position in affecting the thermal conductivity.
- the oxidation phase with low thermal conductivity reduces the thermal conductivity of the ceramic; not only that, after adding TiO 2 and Y 2 O 3 , the transient oxidation liquid phase formed by the two during the sintering process will not only cause a large shrinkage during the sintering process, but also produce too many grain boundaries, hinder heat conduction, and make the green body and pattern layer receive unequal thermal stress; under the joint action of the two, it is difficult to optimize the uniformity of the pattern.
- the present invention adds Y- ⁇ -SiAlON to the body reinforcement.
- the addition of Y- ⁇ -SiAlON can reduce the content of lattice oxygen, increase the thermal conductivity of the ceramic, and the heat can be more effectively transferred inside the ceramic to prevent deformation caused by uneven heating.
- Y- ⁇ -SiAlON does not participate in the process of TiO 2 and Y 2 O 3 forming a unified 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 ceramics only adding TiO 2 and Y 2 O 3 , thereby reducing the firing shrinkage.
- Y- ⁇ -SiAlON reduces the growth space of large-sized columnar grains, and plays the same role as TiO 2 and Y 2 O 3 in promoting the densification of ceramics.
- the addition of this substance does not cause a decrease in the mechanical properties of the ceramic.
- the Y- ⁇ -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 each component is evenly dispersed, and each of the above raw materials is in powder form with an average particle size of less than 1 ⁇ m; the mixed raw materials are sintered at a pressure of 30 to 50 MPa, firstly, the mixed raw materials are heated from room temperature to 550 to 650°C at a heating rate of 110 to 120°C/min, then the mixed raw materials are heated to 1350 to 1400°C at a heating rate of 20 to 30°C/min, and kept at this temperature for 10 to 15 minutes, and finally, the sintered blank is cooled to room temperature at a cooling rate of 50 to 75°C/min, and the Y- ⁇ -SiAlON is obtained by grinding and crushing.
- the method for preparing the crystal jade material with a white appearance comprises the following steps:
- the ceramic tile blank is fired to obtain a crystal jade material with a smooth white appearance.
- the particle gradation mass percentage of the green powder material in step S1 is as follows: 20 mesh ⁇ 2%, 30 mesh 3-8%, 40 mesh 30-40%, 60 mesh 40-50%, 100 mesh ⁇ 10%, and above 100 mesh ⁇ 2%.
- the thickness of the green body layer in step S2 is 6 to 30 mm.
- the green strength of the body layer in step S2 is >0.5 MPa, and the dry strength is >3 MPa.
- the moisture content of the green body layer in step S2 is 8.5-9.5%.
- the glaze in step S4 is any one of protective glaze, polished glaze, dry granular polished glaze, and antique dry granular glaze.
- the firing temperature in step S5 is 1160-1220° C., and the firing time is 1.5-2.5 h.
- Ultra-white kaolin a non-metallic mineral, a type of clay and clay rock mainly composed of kaolinite clay minerals, also known as dolomite because of its white and fine texture.
- the pure kaolin is white, fine, soft, and has good physical and chemical properties such as plasticity and fire resistance.
- High plastic mud a type of ceramic mud with higher plasticity than general ceramic mud. Its main mineral component is montmorillonite and it has a higher bearing capacity.
- Wollastonite is an inorganic needle-shaped mineral, a chain metasilicate, and a fibrous, needle-shaped mineral. It is non-toxic, chemically resistant, thermally stable and dimensionally stable, has glass and pearl luster, low water and oil absorption, excellent mechanical and electrical properties, and has a certain reinforcing effect.
- High white bentonite It is a non-metallic mineral product mainly composed of montmorillonite. It is hygroscopic and expansive. It can absorb 8 to 15 times of its own volume of water and expand its volume several times to more than 30 times. In water medium, bentonite can be dispersed in a gelled and suspended state. This mixed liquid has certain viscosity, thixotropy and lubricity. It has good plasticity and good adhesion when combined with fine debris such as water, mud and sand.
- the present invention uses ultra-white kaolin, high plasticity mud, ceramic black mud, high white frit, high white potassium sodium sand, wollastonite, high white bentonite and body reinforcing agent as body powder to produce a crystal jade material with a smooth white appearance.
- the material has a smooth white appearance, a jade-like texture, richer pattern layers and is closer to the natural texture of marble.
- the present invention adopts a green body reinforcing agent with a specific material ratio to form a certain liquid phase during the sintering process, which helps to densify the ceramic, provides a good connection between the ceramic grains, limits the growth of the ceramic grains and the formation of a loose stacking structure, reduces the particle size of the ceramic grains, and makes the microstructure uniform and dense, allowing the finished product to have a jade texture.
- the green body reinforcing agent of the present invention has low lattice oxygen content, and the thermal conductivity of the ceramic is improved. Heat can be transferred more effectively inside the ceramic, preventing deformation caused by uneven heating levels; the body reinforcement controls the content of transient liquid phase formed in the ceramic, reduces the firing shrinkage rate, and improves the matching degree of the marble pattern.
- Ultra-white kaolin item number: glt-0046, whiteness: 88-89%, provided by Lingshou County Yuanda Mica Factory;
- Wollastonite Wollastonite, CAS No.: 13983-17-0, whiteness> 90%, provided by Hebei Weiran Building Materials Technology Co., Ltd.
- High white bentonite CAS number: 1302-78-9, whiteness: 70%, provided by Xinyang Pingqiao District Shuangcheng Bentonite Powder Factory.
- a crystal jade material with a white appearance is prepared by the following method:
- the ceramic tile blank is fired at 1200° C. for 1.5 hours to obtain a crystal jade material with a smooth white appearance.
- the green body powder is as follows: 25kg ultra-white kaolin, 6.5kg high plastic mud, 7.5kg ceramic black mud, 24kg high white frit, 20kg high white potassium sodium sand, 2.5kg wollastonite, 2.5kg high white bentonite, and 0.5kg green body reinforcing agent.
- the iron content of the ultra-white kaolin, high plasticity mud, ceramic black mud and 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 particle gradation mass percentage of the green 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 above 100 mesh is 1%.
- the green body reinforcing agent is a mixture of TiO 2 and Y 2 O 3 in a mass ratio of 6:3.5, and both of the above two components are in powder form.
- a crystal jade material with a white appearance is prepared by the following method:
- the blank is textured and pressed by a digital cloth machine to obtain a blank layer and a blank layer applied on the surface of the blank.
- the pattern layer, the thickness of the green body layer is 12 mm, and the moisture content of the green body layer is 9%;
- the ceramic tile blank is fired at 1200° C. for 1.5 hours to obtain a crystal jade material with a smooth white appearance.
- the green body powder is as follows: 25kg ultra-white kaolin, 6.5kg high plastic mud, 7.5kg ceramic black mud, 24kg high white frit, 20kg high white potassium sodium sand, 2.5kg wollastonite, 2.5kg high white bentonite, and 0.5kg green body reinforcing agent.
- the iron content of the ultra-white kaolin, high plasticity mud, ceramic black mud and 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 particle gradation mass percentage of the green 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 above 100 mesh is 1%.
- the green body reinforcing agent is a mixture of Y- ⁇ -SiAlON and TiO2 in a mass ratio of 10.5:3.5, and the above two components are both in powder form.
- the Y- ⁇ -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 each component is evenly dispersed, and each of the above raw materials is in powder form with an average particle size of less than 1 ⁇ m; the mixed raw materials are sintered under a pressure of 40 MPa, firstly, the mixed raw materials are heated from room temperature to 600°C at a heating rate of 115°C/min, then the mixed raw materials are heated to 1350°C at a heating rate of 25°C/min, and maintained at this temperature for 10 minutes, and finally, the sintered blank is cooled to room temperature at a cooling rate of 50°C/min, and the Y- ⁇ -SiAlON is obtained by grinding and pulverizing.
- a crystal jade material with a white appearance is prepared by the following method:
- the ceramic tile blank is fired at 1200° C. for 1.5 hours to obtain a crystal jade material with a smooth white appearance.
- the green body powder is as follows: 25kg ultra-white kaolin, 6.5kg high plastic mud, 7.5kg ceramic black mud, 24kg high white frit, 20kg high white potassium sodium sand, 2.5kg wollastonite, 2.5kg high white bentonite, and 0.5kg green body reinforcing agent.
- the iron content of the ultra-white kaolin, high plasticity mud, ceramic black mud and 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 particle gradation mass percentage of the green 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 above 100 mesh is 1%.
- the green body reinforcing agent is a mixture of Y- ⁇ -SiAlON and Y 2 O 3 in a mass ratio of 10.5:3.5, and the two components are both in powder form.
- the Y- ⁇ -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 each component is evenly dispersed, and each of the above raw materials is in powder form with an average particle size of ⁇ 1 ⁇ m; the mixed raw material is sintered under a pressure of 40MPa, firstly, the mixed raw material is heated from room temperature to 600°C at a heating rate of 115°C/min, then the mixed raw material is heated to 1350°C at a heating rate of 25°C/min, and maintained at this temperature for 10min, and finally the sintered blank is cooled to room temperature at a cooling rate of 50°C/min, and the Y- ⁇ -SiAlON is obtained by grinding and crushing.
- a crystal jade material with a white appearance is prepared by the following method:
- the ceramic tile blank is fired at 1200° C. for 1.5 hours to obtain a crystal jade material with a smooth white appearance.
- the green body powder is as follows: 25kg ultra-white kaolin, 6.5kg high plastic mud, 7.5kg ceramic black mud, 24kg high white frit, 20kg high white potassium sodium sand, 2.5kg wollastonite, 2.5kg high white bentonite, and 0.5kg green body reinforcing agent.
- the iron content of the ultra-white kaolin, high plasticity mud, ceramic black mud and 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 particle gradation mass percentage of the green 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 above 100 mesh is 1%.
- the green body reinforcing agent is a mixture of Y- ⁇ -SiAlON, TiO 2 and Y 2 O 3 in a mass ratio of 10.5:6:3.5, and the above three components are all in powder form.
- the Y- ⁇ -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 each component is evenly dispersed, and each of the above raw materials is in powder form with an average particle size of less than 1 ⁇ m; the mixed raw materials are sintered under a pressure of 40 MPa, firstly, the mixed raw materials are heated from room temperature to 600°C at a heating rate of 115°C/min, then the mixed raw materials are heated to 1350°C at a heating rate of 25°C/min, and maintained at this temperature for 10 minutes, and finally, the sintered blank is cooled to room temperature at a cooling rate of 50°C/min, and the Y- ⁇ -SiAlON is obtained by grinding and crushing.
- a crystal jade material with a white appearance is prepared by the following method:
- the ceramic tile blank is fired at 1200° C. for 1.5 hours to obtain a crystal jade material with a smooth white appearance.
- the green powder is as follows: 25kg ultra-white kaolin, 6.5kg high plastic mud, 7.5kg ceramic black mud, 24kg high white frit, 20kg high white potassium sodium sand, 2.5kg wollastonite, 2.5kg high white bentonite.
- the iron content of the ultra-white kaolin, high plasticity mud, ceramic black mud and 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 particle gradation mass percentage of the green 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 above 100 mesh is 1%.
- the whiteness test of the crystal jade material with a smooth white appearance is carried out in accordance with the method and steps in the recommended industry standard QB/T 1503-2011 "Method for Determining the Whiteness of Daily Ceramics".
- QB/T 1503-2011 “Method for Determining the Whiteness of Daily Ceramics”.
- three samples that meet the standard are prepared, and the size of the flat surface of the sample meets the measurement requirements of the instrument probe.
- the surface of the sample to be tested is the white part without color decoration, and the surface is clean, flat, and free of cracks and other scars.
- the integer part of 1 to 10 points is used to represent the degree of fit with the design pattern.
- the bending strength test of the crystal jade material with a white appearance is carried out according to the method and steps in GB/T 4741-1999 "Test Method for Bending Strength of Ceramic Materials".
- the sample is a rectangular sample with a length of 120 mm and a width-to-thickness ratio of 1:1, and 10 samples are prepared in each group.
- the materials and process conditions used in the preparation of the sample are the same as those of the embodiments and the control examples. Each sample is processed regularly without obvious defects.
- the sample is placed in an oven at a temperature of 110°C ⁇ 5°C, dried to constant weight, and then placed in a dryer to cool to room temperature; the sample is placed on the support blade, and the spacing between the support blades is adjusted so that the length of the sample outside the support blade is 10 mm.
- the two support blades must be in the same plane and parallel to each other, and the loading blade is located in the middle of the two support blades; the bending strength tester is turned on, and the loading blade must not impact when it contacts the sample, and the load is applied at an average speed of 30N/s until it is destroyed, and the maximum load when the sample is destroyed is recorded.
- the arithmetic mean of the test results is taken as the bending strength value of the sample, and the data is rounded to 0.1MPa.
- the bending strength test results of the crystal jade material with a white appearance are shown in Table 2.
- the overall flexural strength of the examples using the green body reinforcement is higher than that of the control example 1, and the example 4 shows the highest flexural strength.
- the flexural strength is related to its densification degree and whether there are structural defects.
- the reason for the above results may be that TiO2 and Y2O3 are used as components of the green body reinforcement to form a certain liquid phase during the sintering process, which is conducive to the densification of the ceramic; TiO2 provides a good connection between the ceramic grains, and works together with Y2O3 to limit the growth of the ceramic grains.
- Y- ⁇ - SiAlON also reduces the growth space of large-sized columnar grains, inhibits the formation of loose stacking structure, reduces the particle size of the ceramic grains, and makes the microstructure uniform and dense, so that the finished product shows a jade texture and the flexural strength is improved.
- the firing shrinkage test of the white-looking crystal jade material was carried out in accordance with the method and steps in the recommended industry standard QB/T 1548-2015 "Method for Determining Linear Shrinkage of Ceramic Green Clay".
- the preparation of the sample refers to the preparation of the plastic clay sample, the sample size is ⁇ 60mm ⁇ 8mm, and 5 samples are prepared in each group; the materials used in the sample and the firing process conditions are the same as those of each embodiment and control example.
- the results are taken as the arithmetic mean, and the results are expressed to two decimal places.
- the firing shrinkage test results of the white-looking crystal jade material are shown in Table 3.
- the reason for this phenomenon may be that TiO 2 and Y 2 O 3 will reduce the thermal conductivity of the green body and increase the firing shrinkage; the thermal conductivity of the green body is related to the grain boundary and lattice oxygen, and the lattice oxygen occupies a dominant position in affecting the thermal conductivity, and the oxidation phase with low thermal conductivity reduces the thermal conductivity of the ceramic; not only that, after adding TiO 2 and Y 2 O 3 , the transient oxidation liquid phase formed by the two during the sintering process will not only cause a large shrinkage during the sintering process, but also produce too many grain boundaries, hinder heat conduction, and make the green body and the pattern layer receive unequal thermal stress; under the joint action of the two, it is difficult to optimize the uniformity of the pattern.
- the lattice oxygen content decreases, which increases the thermal conductivity of the ceramic. Heat can be transferred more effectively inside the ceramic, preventing deformation caused by uneven heating.
- Y- ⁇ -SiAlON does not participate in the formation of a unified transient liquid phase with TiO 2 and Y 2 O 3.
- Y- ⁇ -SiAlON slowly dissolves in the liquid phase over time. Under the same conditions, the content of transient liquid phase in the ceramic is lower than that of the ceramic with only TiO 2 and Y 2 O 3 added, thereby reducing the firing shrinkage.
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Abstract
一种外观润白的晶玉材料及其制备方法，属于人造石技术领域。外观润白的晶玉材料包括坯体层、布施在坯体表面的图案层以及布施在图案层表面的面釉层，坯体层包括坯粉与色料，坯粉包括下述以重量份计的原料：20~30份超白高岭土，5~8份高塑性泥，5~10份陶瓷黑泥，18~30份高白熔块，15~25份高白钾钠砂，0~5份硅灰石，0~5份高白膨润土，0.2~0.5份坯体增强剂，坯体增强剂为Y-α-SiAlON、TiO 2、Y 2O 3以质量比5~12.5：4~7：2~4形成的混合物。制备方法包括制作坯料，形成纹理并压制得到图案层，图案层表面施釉得到面釉层，面釉层喷墨并施釉得到瓷砖坯，烧制。制备的晶玉材料外观润白、质感如玉，其图案层次更加丰富，更接近大理石的天然纹理。
Description
本发明涉及人造石技术领域，尤其涉及一种外观润白的晶玉材料及其制备方法。
天然大理石属于中硬石材，是地壳中原有的岩石经过地壳内高温高压作用形成的变质岩，主要由方解石、石灰石、蛇纹石和白云石组成。其硬度高、手感好、花纹自然、具有良好的观感，被广泛用于室内装修领域。然而天然大理石的制造成本高，难以加工成大型的岩板材料；因此，具有大理石外观的人造岩板材料应运而生。人造大理石岩板材料成本相对较低，并可根据市场需求定制不同的大理石纹路。此外，人造大理石岩板材料为人工烧制而成，可以通过改变坯体的大小来制备大型的岩板，进而拓展了在本领域的应用范围。
中国专利CN114380625A提供了一种通体岩板及其制备方法，该发明提供的通体岩板从下至上依次包括坯体层、底釉层、面釉层、干粒层；所述干粒层通过喷干粒形成，所述干粒的施料量为180～220g/m2，所述干粒的膨胀系数为230～275/℃，所述干粒的粒度为100～300目；该发明的技术方案提供的通体岩板添加了干粒层，使得制备得到的产品具有良好的流沙效果、优异的耐磨性和平整度，且防污等级高；另外，该发明还提供了所述通体岩板的制备方法，所述制备方法采用喷墨打印并施模具效果，使得制备得到的通体岩板具有高精密度的通体，并且操作简单、对设备要求少、制备效率高，利于大批量生产。
中国专利CN106187212A公开了一种通体大理石瓷砖的制备方法，所述的通体大理石瓷砖的制备方法，是将干法混色工艺和立体布料工艺相结合制备坯体，在坯体表面施面釉，然后在面釉表层依次喷剥开墨水和剥开釉，最后进行烧制得到通体大理石瓷砖。该发明简单、节能环保，突破了传统工艺的瓶颈，应用广泛，制备的瓷砖真实还原了天然石材质感，整体美观、空间装饰效果更加逼真，更有质感。
中国专利CN107500744A公开了一种仿大理石通体陶瓷砖及其制备方法，其包括通体砖坯层和布施在通体砖坯层上的面釉层，所述通体砖坯层按原料重量百分比计包括22～40％的钾砂、15～30％的钾钠长石、10～20％的钾长石、10～22％的黑泥、2～10％的高岭土、2～6％的膨润土、1～4％的生滑石、2～10％的色料；所述面釉层按原料重量百分比计包括30～60％的钾钠长石、15～30％的高岭土、5～10％的硅灰石、5～10％的氧化铝、2～8％滑石、2～10％的氧化锌、10～20％的碳酸钙。该发明解决了通体陶瓷砖在烧成工艺上难氧化的问题，其可制备出厚度大于1cm通体陶瓷砖，该通体陶瓷砖氧化性能好，中间层不易出现针孔、黑线、气泡等现象，同时通过调整面釉组分及配比，解决了通体陶瓷砖面釉质感无法达到天然大理石的表面质感的问题，使得该通体陶瓷砖表面质感更接近天然大理石。
通过上述专利公开的内容可以看出，采用布施系统在坯体表面形成大理石纹路及各种不同类型的釉层是本领域常见的操作。现有技术要解决的技术问题主要是提升釉层的性能，在实际的烧制过程中，由于坯体图案、釉层图案、喷墨打印图案之间的性质不同，各组分之间的在相同温度环境下的烧结进程难以统一，导致成品各层图案出现偏移，坯体图案和其他图案难以做到一一对应，导致错层图案产生，影响美观。
发明内容
有鉴于现有技术的上述缺陷，本发明所要解决的问题是提供一种外观润白、具有大理石质感的晶玉材料及其制备方法。
一种外观润白的晶玉材料，包括坯体层、布施在坯体表面的图案层以及布施在图案层表面的面釉层；所述坯体层包括坯粉与色料；所述坯粉包括下述以重量份计的原料：
20～30份超白高岭土，5～8份高塑性泥，5～10份陶瓷黑泥，18～30份高白熔块，15～25份高白钾钠砂，0～5份硅灰石，0～5份高白膨润土，0.2～0.5份坯体增强剂。
优选的，所述超白高岭土、高塑性泥、陶瓷黑泥、高白膨润土的含铁量<0.2wt％，所述高白钾钠砂含铁量<0.1wt％。
在晶玉材料烧制的过程中，坯体与釉层、图案会承受较大的温度变化，坯体的厚度要高于后者，由于受热程度不一，导致各层之间的热应力差别大，严重时将导致图案出现扭曲、偏移。不仅如此，陶瓷晶粒的过度生长也不利于大理石图案保持一致，陶瓷的收缩率过大，原设计的图案随收缩发生扭曲形变，致使成品质量参差不齐。
为了解决陶瓷晶粒的过度生长的技术问题，本发明采用TiO2、Y2O3作为坯体增强剂的成分，在烧结过程中形成一定的液相，帮助陶瓷致密化。TiO2在陶瓷晶粒之间提供良好的连接，与Y2O3共同作用来限制陶瓷晶粒的生长，抑制了松散的堆积结构形成，使陶瓷晶粒粒径减小，微观组织均匀致密，让成品表现玉质感。
优选的，所述坯体增强剂为Y-α-SiAlON、TiO2、Y2O3以质量比5～12.5：4～7：2～4形成的混合物，上述三种成分均为粉末状。
TiO2、Y2O3虽然能够限制陶瓷晶粒的生长，利于致密化并增强成品强度，但是在防止图案偏移、错层的作用却较为有限。发明人发现，造成这种现象的原因在于TiO2、Y2O3会降低坯体的导热性并增加烧成收缩率。坯体的导热性与晶界和晶格氧相关，而晶格氧在影响导热性中占据了主导地位，热导率低的氧化相降低了陶瓷的导热性；不仅如此，加入TiO2、Y2O3后，在烧结过程中二者形成的瞬态氧化液相，不仅会使烧结过程中收缩较大，还会产生过多的晶界，阻碍热传导，使坯体和图案层等收到的热应力不等；在两者共同的作用下，致使图案的统一性难以得到优化。
为此，本发明在坯体增强剂中加入了Y-α-SiAlON，相比于金属氧化物，添加Y-α-SiAlON能够降低晶格氧的含量，使陶瓷的导热性能上升，热量能够更为有效的在陶瓷内部进行传递，防止受热程度不统一导致的形变。随着温度升高，Y-α-SiAlON并未参与TiO2、Y2O3形成统一瞬态液相的进程，而是随时间缓慢地溶解在液相中；因此，在相同条件下，陶瓷中瞬态液相的含量要低于仅加入TiO2、Y2O3的陶瓷，从而降低了烧成收缩率。与此同时，Y-α-SiAlON减少了大尺寸柱状晶粒的生长空间，在促进陶瓷致密化的进程中与TiO2、Y2O3发挥了相同的作用，该物质的加入并未造成陶瓷力学性能的下降。
进一步优选的，所述Y-α-SiAlON采用如下方法制备而成：
将硅、铝、氮化硅、二氧化硅、氧化钇以摩尔比10：5：3.3：0.7：0.4的比例混合至各组分分散均匀，上述各原料均为粉末状，平均粒径＜1μm；将混合原料在30～50MPa压力下进行烧结，首先以110～120℃/min的升温速率将混合原料从常温加热至550～650℃，随后以20～30℃/min的升温速率将混合原料加热至1350～1400℃，在该温度下保持10～15min，最后以50～75℃/min的降温速率将烧结后的坯料冷却至常温，经研磨粉碎，得到所述Y-α-SiAlON。
所述外观润白的晶玉材料的制备方法，包括如下步骤：
S1、将坯粉材料、色料和水混合并球磨，得到坯浆，通过喷雾造粒塔喷粉将坯浆制成坯料；
S2、将所述坯料用数码布料机形成纹理并压制，得到坯体层与布施在坯体表面的图案层；
S3、在所述图案层的表面施面釉，得到布施在图案层表面的面釉层；
S4、在所述面釉层上对位打印喷墨图案，所述喷墨图案和图案层一致；喷墨图案后继续施加釉料，得到瓷砖坯；
S5、所述瓷砖坯经烧制，得到外观润白的晶玉材料。
优选的，步骤S1中所述坯粉材料的颗粒级配质量百分比如下：20目≤2％，30目为3～8％，40目为30～40％，60目为40～50％，100目≤10％，100目以上<2％。
优选的，步骤S2中所述坯体层的厚度为6～30mm。
优选的，步骤S2中所述坯体层的生坯强度>0.5MPa，干燥强度>3MPa。
优选的，步骤S2中所述坯体层的水份含量为8.5～9.5％。
优选的，步骤S4中所述釉料为保护釉、抛釉、干粒抛、仿古干粒中的任一种。
优选的，步骤S5中所述烧制的温度为1160～1220℃，烧制时间为1.5～2.5h。
在符合本领域常识的基础上，上述各优选条件，可以任意组合，即得本发明各较佳实施例。
本发明配方中部分原料的介绍及作用如下：
超白高岭土：一种非金属矿产，是一种以高岭石族粘土矿物为主的粘土和粘土岩，因呈白色而又细腻，又称白云土。其质纯的高岭土呈洁白细腻、松软土状，具有良好的可塑性和耐火性等理化性质。
高塑性泥：陶瓷泥的一种，塑性高于一般陶瓷泥，其主要矿物成分为蒙脱石，承载力较高。
硅灰石：硅灰石是一种无机针状矿物，属于一种链状偏硅酸盐，又是一种呈纤维状、针状。其特点无毒、耐化学腐蚀、热稳定性及尺寸稳定良好，有玻璃和珍珠光泽，低吸水率和吸油值，力学性能及电性能优良以及具有一定补强作用。
高白膨润土：是一种主要有蒙脱石组成的非金属矿产品，具吸湿性和膨胀性，可吸附8～15倍于自身体积的水量，体积膨胀数倍至30余倍。在水介质中，膨润土能分散呈胶凝状和悬浮状，此混合液具有一定的粘滞性、触变性和润滑性，其与水、泥、沙等细碎屑物的接合，具有较好的可塑性和较好的粘结性。
本发明的有益效果：
与现有技术相比，本发明以超白高岭土、高塑性泥、陶瓷黑泥、高白熔块、高白钾钠砂、硅灰石、高白膨润土、坯体增强剂作为坯粉，制得了一种外观润白的晶玉材料，外观润白、质感如玉，其图案层次更加丰富，更接近大理石的天然纹理。
相比于现有技术，本发明采用特定物质比例的坯体增强剂，在烧结过程中形成一定的液相，帮助陶瓷致密，在陶瓷晶粒之间提供良好的连接，限制了陶瓷晶粒的生长及松散的堆积结构形成，使陶瓷晶粒粒径减小，微观组织均匀致密，让成品表现玉质感。
与现有技术相比，本发明的坯体增强剂产生晶格氧含量低，陶瓷的导热性能上升，
热量能够更为有效的在陶瓷内部进行传递，防止了受热程度不统一导致的形变；坯体增强剂对在陶瓷中形成瞬态液相的含量进行了，降低了烧成收缩率，使大理石图案的匹配程度提高。
下面通过实施例的方式进一步说明本发明，但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法，按照常规方法和条件，或按照商品说明书选择。
本发明对照例及实施例中部分原材料参数如下：
超白高岭土，货号：glt-0046，白度：88～89％，灵寿县远大云母厂提供；
高塑性泥，灵寿县彩瑞矿产品加工厂提供；
陶瓷黑泥，型号：DC-812，白度：38～45％，东莞市东瓷陶瓷原料有限公司提供；
高白熔块，型号：808，佛山富域新材料有限公司提供；
高白钾钠砂，白度：70％，江西省嘉和矿业有限公司提供；
硅灰石，CAS号：13983-17-0，白度＞90％，河北蔚然建材科技有限公司提供；
高白膨润土，CAS号：1302-78-9，白度：70％，信阳市平桥区双诚膨润土粉厂提供。
实施例1
一种外观润白的晶玉材料，采用如下方法制备而成：
S1、将坯粉材料、色料和水混合并球磨，得到坯浆，通过喷雾造粒塔喷粉将坯浆制成坯料；
S2、将所述坯料用数码布料机形成纹理并压制，得到坯体层与布施在坯体表面的图案层，所述坯体层的厚度为12mm，坯体层的水份含量为9％；
S3、在所述图案层的表面施面釉，得到布施在图案层表面的面釉层；
S4、在所述面釉层上对位打印喷墨图案，所述喷墨图案和图案层一致；喷墨图案后继续施加保护釉，得到瓷砖坯；
S5、所述瓷砖坯经烧制，在1200℃，烧制时间为1.5h，得到外观润白的晶玉材料。
所述坯粉如下：25kg超白高岭土，6.5kg高塑性泥，7.5kg陶瓷黑泥，24kg高白熔块，20kg高白钾钠砂，2.5kg硅灰石，2.5kg高白膨润土，0.5kg坯体增强剂。
所述超白高岭土、高塑性泥、陶瓷黑泥、高白膨润土的含铁量<0.2wt％，所述高白钾钠砂含铁量<0.1wt％。
所述坯粉材料的颗粒级配质量百分比如下：20目为1％，30目为3％，40目为40％，60目为50％，100目为5％，100目以上为1％。
所述坯体增强剂为TiO2、Y2O3以质量比6：3.5形成的混合物，上述两种成分均为粉末状。
实施例2
一种外观润白的晶玉材料，采用如下方法制备而成：
S1、将坯粉材料、色料和水混合并球磨，得到坯浆，通过喷雾造粒塔喷粉将坯浆制成坯料；
S2、将所述坯料用数码布料机形成纹理并压制，得到坯体层与布施在坯体表面的
图案层，所述坯体层的厚度为12mm，坯体层的水份含量为9％；
S3、在所述图案层的表面施面釉，得到布施在图案层表面的面釉层；
S4、在所述面釉层上对位打印喷墨图案，所述喷墨图案和图案层一致；喷墨图案后继续施加保护釉，得到瓷砖坯；
S5、所述瓷砖坯经烧制，在1200℃，烧制时间为1.5h，得到外观润白的晶玉材料。
所述坯粉如下：25kg超白高岭土，6.5kg高塑性泥，7.5kg陶瓷黑泥，24kg高白熔块，20kg高白钾钠砂，2.5kg硅灰石，2.5kg高白膨润土，0.5kg坯体增强剂。
所述超白高岭土、高塑性泥、陶瓷黑泥、高白膨润土的含铁量<0.2wt％，所述高白钾钠砂含铁量<0.1wt％。
所述坯粉材料的颗粒级配质量百分比如下：20目为1％，30目为3％，40目为40％，60目为50％，100目为5％，100目以上为1％。
所述坯体增强剂为Y-α-SiAlON、TiO2以质量比10.5：3.5形成的混合物，上述两种成分均为粉末状。
所述Y-α-SiAlON采用如下方法制备而成：将硅、铝、氮化硅、二氧化硅、氧化钇以摩尔比10：5：3.3：0.7：0.4的比例混合至各组分分散均匀，上述各原料均为粉末状，平均粒径＜1μm；将混合原料在40MPa压力下进行烧结，首先以115℃/min的升温速率将混合原料从常温加热至600℃，随后以25℃/min的升温速率将混合原料加热至1350℃，在该温度下保持10min，最后以50℃/min的降温速率将烧结后的坯料冷却至常温，经研磨粉碎，得到所述Y-α-SiAlON。
实施例3
一种外观润白的晶玉材料，采用如下方法制备而成：
S1、将坯粉材料、色料和水混合并球磨，得到坯浆，通过喷雾造粒塔喷粉将坯浆制成坯料；
S2、将所述坯料用数码布料机形成纹理并压制，得到坯体层与布施在坯体表面的图案层，所述坯体层的厚度为12mm，坯体层的水份含量为9％；
S3、在所述图案层的表面施面釉，得到布施在图案层表面的面釉层；
S4、在所述面釉层上对位打印喷墨图案，所述喷墨图案和图案层一致；喷墨图案后继续施加保护釉，得到瓷砖坯；
S5、所述瓷砖坯经烧制，在1200℃，烧制时间为1.5h，得到外观润白的晶玉材料。
所述坯粉如下：25kg超白高岭土，6.5kg高塑性泥，7.5kg陶瓷黑泥，24kg高白熔块，20kg高白钾钠砂，2.5kg硅灰石，2.5kg高白膨润土，0.5kg坯体增强剂。
所述超白高岭土、高塑性泥、陶瓷黑泥、高白膨润土的含铁量<0.2wt％，所述高白钾钠砂含铁量<0.1wt％。
所述坯粉材料的颗粒级配质量百分比如下：20目为1％，30目为3％，40目为40％，60目为50％，100目为5％，100目以上为1％。
所述坯体增强剂为Y-α-SiAlON、Y2O3以质量比10.5：3.5形成的混合物，上述两种成分均为粉末状。
所述Y-α-SiAlON采用如下方法制备而成：将硅、铝、氮化硅、二氧化硅、氧化钇以摩尔比10：5：3.3：0.7：0.4的比例混合至各组分分散均匀，上述各原料均为粉末状，平均粒径
＜1μm；将混合原料在40MPa压力下进行烧结，首先以115℃/min的升温速率将混合原料从常温加热至600℃，随后以25℃/min的升温速率将混合原料加热至1350℃，在该温度下保持10min，最后以50℃/min的降温速率将烧结后的坯料冷却至常温，经研磨粉碎，得到所述Y-α-SiAlON。
实施例4
一种外观润白的晶玉材料，采用如下方法制备而成：
S1、将坯粉材料、色料和水混合并球磨，得到坯浆，通过喷雾造粒塔喷粉将坯浆制成坯料；
S2、将所述坯料用数码布料机形成纹理并压制，得到坯体层与布施在坯体表面的图案层，所述坯体层的厚度为12mm，坯体层的水份含量为9％；
S3、在所述图案层的表面施面釉，得到布施在图案层表面的面釉层；
S4、在所述面釉层上对位打印喷墨图案，所述喷墨图案和图案层一致；喷墨图案后继续施加保护釉，得到瓷砖坯；
S5、所述瓷砖坯经烧制，在1200℃，烧制时间为1.5h，得到外观润白的晶玉材料。
所述坯粉如下：25kg超白高岭土，6.5kg高塑性泥，7.5kg陶瓷黑泥，24kg高白熔块，20kg高白钾钠砂，2.5kg硅灰石，2.5kg高白膨润土，0.5kg坯体增强剂。
所述超白高岭土、高塑性泥、陶瓷黑泥、高白膨润土的含铁量<0.2wt％，所述高白钾钠砂含铁量<0.1wt％。
所述坯粉材料的颗粒级配质量百分比如下：20目为1％，30目为3％，40目为40％，60目为50％，100目为5％，100目以上为1％。
所述坯体增强剂为Y-α-SiAlON、TiO2、Y2O3以质量比10.5：6：3.5形成的混合物，上述三种成分均为粉末状。
所述Y-α-SiAlON采用如下方法制备而成：将硅、铝、氮化硅、二氧化硅、氧化钇以摩尔比10：5：3.3：0.7：0.4的比例混合至各组分分散均匀，上述各原料均为粉末状，平均粒径＜1μm；将混合原料在40MPa压力下进行烧结，首先以115℃/min的升温速率将混合原料从常温加热至600℃，随后以25℃/min的升温速率将混合原料加热至1350℃，在该温度下保持10min，最后以50℃/min的降温速率将烧结后的坯料冷却至常温，经研磨粉碎，得到所述Y-α-SiAlON。
对照例1
一种外观润白的晶玉材料，采用如下方法制备而成：
S1、将坯粉材料、色料和水混合并球磨，得到坯浆，通过喷雾造粒塔喷粉将坯浆制成坯料；
S2、将所述坯料用数码布料机形成纹理并压制，得到坯体层与布施在坯体表面的图案层，所述坯体层的厚度为12mm，坯体层的水份含量为9％；
S3、在所述图案层的表面施面釉，得到布施在图案层表面的面釉层；
S4、在所述面釉层上对位打印喷墨图案，所述喷墨图案和图案层一致；喷墨图案后继续施加保护釉，得到瓷砖坯；
S5、所述瓷砖坯经烧制，在1200℃，烧制时间为1.5h，得到外观润白的晶玉材料。
所述坯粉如下：25kg超白高岭土，6.5kg高塑性泥，7.5kg陶瓷黑泥，24kg高白熔块，
20kg高白钾钠砂，2.5kg硅灰石，2.5kg高白膨润土。
所述超白高岭土、高塑性泥、陶瓷黑泥、高白膨润土的含铁量<0.2wt％，所述高白钾钠砂含铁量<0.1wt％。
所述坯粉材料的颗粒级配质量百分比如下：20目为1％，30目为3％，40目为40％，60目为50％，100目为5％，100目以上为1％。
测试例1
外观润白的晶玉材料的白度测试参照推荐性行业标准QB/T 1503-2011《日用陶瓷白度测定方法》中的方法及步骤进行。每实施例或对照例准备符合标准的试样3件，试样平整面大小满足仪器探头的测定要求。试样待测面为无彩饰的白色部分，表面清洁、平整、无裂纹及其他伤痕。对于外观润白的晶玉材料有大理石纹路的部分，以1～10分的整数部分来表示与设计图案间的吻合程度，得分越高则吻合程度越好；1～4分代表纹路图案有扭曲、错层，对应性差；5～8分代表纹路图案小部分存在缺陷或模糊重影；9～10分代表纹路图案与设计图案间的吻合程度高，一致性强。
外观润白的晶玉材料的白度测试及纹路图案吻合程度判断结果见表1。
表1
根据陶瓷白度等级分类，白度≥75的为优等品，70≤白度＜75的为一等品，白度＜70的为合格品。通过表1的测试结果可以看出，外观润白的晶玉材料的白度均达到了优等品的水平。
测试例2
外观润白的晶玉材料的抗弯强度测试参照GB/T 4741-1999《陶瓷材料抗弯强度试验方法》中的方法及步骤进行。试样为长120mm，宽厚比为1：1的长方体试样，每组准备10根。试样的制备采用的材料及工艺条件与各实施例及对照例的相同，每根试样加工规整，不存在明显缺陷。测试时，将试样置于温度为110℃±5℃的烘箱中，烘干至恒重，然后放入干燥器中冷却至室温；将试样安放在支撑刀口上，调整支撑刀口间距、使支撑刀口以外试样的长度为10mm，两个支撑刀口必须在同一平面内且互相平行、并使加荷刀口位于两支撑刀口的正中；开启弯曲强度试验机，加荷刀口接触试样时不得冲击，以平均30N/s的速度等速加荷直至破坏，记录试样破坏时的最大载荷。测试结果取算术平均值作为该试样的抗弯强度值，数据修约到0.1MPa。外观润白的晶玉材料的抗弯强度测试结果见表2。
表2
采用了坯体增强剂的实施例整体上抗弯强度要高于对照例1，实施例4表现出了最高的抗弯强度。在陶瓷的烧制过程中，抗弯强度与其致密化程度及是否存在结构缺陷有关。出现上述结果的原因可能在于，将TiO2、Y2O3作为坯体增强剂的成分，在烧结过程中形成一定的液相，有助于陶瓷致密化；TiO2在陶瓷晶粒之间提供良好的连接，与Y2O3共同作用来限制陶瓷晶粒的生长，Y-α-SiAlON也减少了大尺寸柱状晶粒的生长空间，抑制了松散的堆积结构形成，使陶瓷晶粒粒径减小，微观组织均匀致密，让成品表现玉质感，抗弯强度得到提升。
测试例3
外观润白的晶玉材料的烧成收缩率测试参照推荐性行业标准QB/T 1548-2015《陶瓷坯泥料线收缩率测定方法》中的方法及步骤进行。试样的制备参照可塑性泥料试样的制备，试样尺寸为Φ60mm×8mm，每组准备5件试样；试样采用的材料及烧成的工艺条件与各实施例及对照例的相同。结果取算术平均值，结果表示至小数点后两位。外观润白的晶玉材料的烧成收缩率测试结果见表3。
表3
烧成收缩率越低则晶玉材料的纹路受到收缩而发生形变错位的程度就越低，结合表1中吻合程度的结果可以看出，添加了Y-α-SiAlON的实施例收缩率比实施例1及对照例更低，其中实施例4的收缩率最低，其纹路图案与设计图案间的吻合程度高、一致性强。出现这种现象的原因可能在于，TiO2、Y2O3会降低坯体的导热性并增加烧成收缩率；坯体的导热性与晶界和晶格氧相关，而晶格氧在影响导热性中占据了主导地位，热导率低的氧化相降低了陶瓷的导热性；不仅如此，加入TiO2、Y2O3后，在烧结过程中二者形成的瞬态氧化液相，不仅会使烧结过程中收缩较大，还会产生过多的晶界，阻碍热传导，使坯体和图案层等收到的热应力不等；在两者共同的作用下，致使图案的统一性难以得到优化。加入Y-α-SiAlON后，晶格氧的含量降低，使陶瓷的导热性能上升，热量能够更为有效的在陶瓷内部进行传递，防止受热程度不统一导致的形变；另一方面，随着温度升高，Y-α-SiAlON并未参与TiO2、Y2O3形成统一的瞬态液相，Y-α-SiAlON随时间缓慢地溶解在液相中，在相同条件下，陶瓷中瞬态液相的含量要低于仅加入TiO2、Y2O3的陶瓷，降低了烧成收缩率。
Claims (11)
- 一种外观润白的晶玉材料的制备方法，其特征在于，包括如下步骤：S1、将坯粉材料、色料和水混合并球磨，得到坯浆，通过喷雾造粒塔喷粉将坯浆制成坯料；S2、将所述坯料用数码布料机形成纹理并压制，得到坯体层与布施在坯体表面的图案层；S3、在所述图案层的表面施面釉，得到布施在图案层表面的面釉层；S4、在所述面釉层上对位打印喷墨图案，所述喷墨图案和图案层一致；喷墨图案后继续施加釉料，得到瓷砖坯；S5、所述瓷砖坯经烧制，得到外观润白的晶玉材料；所述坯粉包括下述以重量份计的原料：20～30份超白高岭土，5～8份高塑性泥，5～10份陶瓷黑泥，18～30份高白熔块，15～25份高白钾钠砂，0～5份硅灰石，0～5份高白膨润土，0.2～0.5份坯体增强剂；所述坯体增强剂为Y-α-SiAlON、TiO2、Y2O3以质量比5～12.5：4～7：2～4形成的混合物，上述三种成分均为粉末状；所述超白高岭土、高塑性泥、陶瓷黑泥、高白膨润土的含铁量<0.2wt％，所述高白钾钠砂含铁量<0.1wt％。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于，步骤S1中所述坯粉材料的颗粒级配质量百分比如下：20目≤2％，30目为3～8％，40目为30～40％，60目为40～50％，100目≤10％，100目以上<2％。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于：步骤S2中所述坯体层的厚度为6～30mm。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于：步骤S2中所述坯体层的生坯强度>0.5MPa，干燥强度>3MPa；所述坯体层的水分含量为8.5～9.5％。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于：步骤S4中所述釉料为保护釉。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于：步骤S4中所述釉料为抛釉。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于：步骤S4中所述釉料为干粒抛。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于：步骤S4中所述釉料为仿古干粒。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于：步骤S5中所述烧制的温度为1160～1220℃，烧制时间为1.5～2.5h。
- 根据权利要求1所述的一种外观润白的晶玉材料的制备方法，其特征在于，所述Y-α-SiAlON采用如下方法制备而成：将硅、铝、氮化硅、二氧化硅、氧化钇以摩尔比10：5：3.3：0.7：0.4的比例混合至各组分分散均匀，上述各原料均为粉末状，平均粒径＜1μm；将混合原料在30～50MPa压力下进行烧结，首先以110～120℃/min的升温速率将混合原料从常温加热至550～650℃，随后以20～30℃/min的升温速率将混合原料加热至1350～1400℃，在该温度下保持10～15min，最后以50～ 75℃/min的降温速率将烧结后的坯料冷却至常温，经研磨粉碎，得到所述Y-α-SiAlON。
- 一种外观润白的晶玉材料，其特征在于：采用如权利要求1～10任一项所述的方法制备而成。
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| KR20200076840A (ko) * | 2018-12-20 | 2020-06-30 | 한국세라믹기술원 | 백옥 질감의 고경도 유약층 형성방법 |
| CN112110750A (zh) * | 2020-08-03 | 2020-12-22 | 湖北杭瑞陶瓷有限责任公司 | 一种超白瓷抛大理石及其制备方法 |
| CN113754406A (zh) * | 2021-10-15 | 2021-12-07 | 广东翠贝卡建材科技有限公司 | 一种玉质鱼肚白效果的陶瓷板、坯料、制备方法及用途 |
| CN115340358A (zh) * | 2022-10-20 | 2022-11-15 | 广东兴辉陶瓷集团有限公司 | 一种外观润白的晶玉材料及其制备方法 |
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