CN115477541A - Preparation method of composite foamed ceramic plate - Google Patents

Preparation method of composite foamed ceramic plate Download PDF

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Publication number
CN115477541A
CN115477541A CN202211256092.0A CN202211256092A CN115477541A CN 115477541 A CN115477541 A CN 115477541A CN 202211256092 A CN202211256092 A CN 202211256092A CN 115477541 A CN115477541 A CN 115477541A
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raw material
ceramic
foamed ceramic
composite foamed
layer
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CN115477541B (en
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张国涛
徐鑫
冯宏坚
柳文龙
聂新超
杨景琪
薛俊东
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Foshan Sanshui Jinyitao Ceramic Co ltd
Guangdong Golden Green Energy Technology Co ltd
Jingdezhen Kito Ceramics Co ltd
Guangdong Kito Ceramics Group Co ltd
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Foshan Sanshui Jinyitao Ceramic Co ltd
Guangdong Golden Green Energy Technology Co ltd
Jingdezhen Kito Ceramics Co ltd
Guangdong Kito Ceramics Group Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64Burning or sintering processes
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/06Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C14/00Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/004Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2214/00Nature of the non-vitreous component
    • C03C2214/30Methods of making the composites
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects 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
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/60Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes

Abstract

The invention provides a preparation method of a composite foamed ceramic plate, and belongs to the field of composite material production. The method comprises the steps of 1) forming a bottom layer, a middle layer and a known foaming ceramic raw material layer which takes silicon carbide as a foaming agent in a refractory kiln furniture with a surrounding edge; step 2) putting the refractory kiln furniture into a kiln for firing, wherein the firing temperature is 1050-1200 ℃; step 3) taking the composite foamed ceramic raw material out of the kiln, and cutting, polishing and grinding the raw material according to the required shape to obtain a composite foamed ceramic plate; the bottom layer is one of a ceramic plate sintered at the temperature of more than or equal to 1000 ℃, a green body formed by pressing ceramic tile powder with the known sintering temperature of 1050-1200 ℃, a known stone plate which can not deform and crack under the sintering condition of the step 2) or a cement plate; the raw material for forming the intermediate layer is a ceramic raw material with the firing temperature of 1050-1200 ℃, and contains corundum and clinker, wherein the content of corundum is more than or equal to 5%, and the content of clinker is more than or equal to 60%. The technical scheme has high process flexibility, and large-size composite foamed ceramics can be obtained.

Description

Preparation method of composite foamed ceramic plate
Technical Field
The invention relates to the field of composite material production, in particular to a preparation method of a composite foamed ceramic plate.
Background
The foamed ceramic has the functions of light weight, heat preservation, flame retardance and the like, has low raw material requirement and low taste, can use a large amount of inorganic barren waste materials such as waste mud, ceramic tile polishing and grinding waste residue and the like generated in ceramic production, and is a green and environment-friendly building material. At present, silicon carbide is mostly used as a foaming agent in the industrially produced foamed ceramics, the prepared powder is scattered in high-temperature kiln furniture, the high-temperature kiln furniture is directly fired after being stacked to a certain thickness according to production needs, the high-temperature kiln furniture is dismantled after sintering and cooling, and the foamed ceramic rough material is polished, cut and processed to be made into required shapes, and usually cut into plates or blocks for use. The foaming temperature of the silicon carbide is 1050-1200 ℃, the addition amount is preferably 0.2-2% by mass of the raw materials (because the addition amount of the foaming agent is less, the foaming agent can also be added in an additional form according to the proportion, namely 0.2-2% of the foaming agent is added on the basis of 100%, in this way, the foaming agent is generally distinguished by adding the foaming agent before the percentage), and the more preferably the foaming temperature is 1120-1190 ℃. In order to improve the foaming effect, a small amount of a substance capable of generating free oxygen at high temperature, such as manganese oxide or ferric trioxide, may be added. The density and strength of the foamed ceramic are related to parameters such as the average pore diameter, pore morphology, whether to open pores, pore wall thickness and the like, and the parameters are generally controlled by the type and amount of the foaming agent and the firing system.
The surface of the polished and ground foamed ceramic is honeycomb-shaped, usually has no decoration, and in order to obtain a surface with a decoration effect, a decoration material can be compounded on the surface of the foamed ceramic, and a common compounding mode is to adhere the foamed ceramic through an adhesive, for example, a layer of ceramic plate with decoration textures is adhered by using cement or tile adhesive, but the mode needs secondary processing and has a complex process. In the process of sintering the foamed ceramics, a plate with decoration or other performance-conforming functions is compounded with the foamed ceramics by utilizing a liquid phase generated at high temperature, which is the key point in recent research and development, for example, the method for preparing the rock plate composite light insulation board disclosed in the domestic invention patent application with the application publication number of CN14105670A adopts a powder accumulation sintering mode, a rock plate is firstly placed in a fire-resistant kiln tool with a surrounding edge, then an intermediate layer raw material and a foamed ceramic raw material are sequentially distributed, and after the fire-resistant kiln tool is placed in a kiln and sintered, the fire-resistant kiln tool is cut and polished to obtain a required product. The intermediate layer powder is prepared by uniformly mixing 25-30 parts of albite, 25-30 parts of glass powder, 8-10 parts of alumina, 10-12 parts of quartz, 6-8 parts of calcite, 4 parts of talcum and 6 parts of kaolin according to the mass parts. The intermediate layer powder with the sintering temperature similar to that of the foamed ceramic is used to form a transition layer between the foamed ceramic and the rock plate, so that the delamination and cracking caused by stress can be effectively relieved. However, this method has at least the following disadvantages in industrial application:
(1) Is not suitable for the high-efficiency production of large-size products. The flatness can be ensured under the condition that the area of the square meter is less than 0.64, but the shape of the existing industrial production foamed ceramic kiln furniture can reach 2.5m multiplied by 1.5m, even larger size, and the surface flatness and the interface bonding property prepared by adopting the process are difficult to ensure.
(2) Is only suitable for sintering the foaming ceramic raw material by adopting a powder accumulation mode. This limits the way the raw material is handled and shaped and the process flexibility is poor.
(3) The green body produced by unsintered building ceramic cannot be sintered together with the foamed ceramic, and the energy consumption of comprehensive production is higher. When the sintered ceramic plate or other plates with certain strength and high sintering temperature resistance are used as the composite layer, the heat energy cannot be comprehensively utilized during high-temperature sintering.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method of a composite foamed ceramic plate, which comprises the following steps:
step 1) forming a bottom layer, a middle layer and a known foaming ceramic raw material layer which takes silicon carbide as a foaming agent in a refractory kiln furniture with a surrounding edge;
step 2) putting the refractory kiln furniture into a kiln for firing, wherein the firing temperature is 1050-1200 ℃;
step 3) taking the composite foamed ceramic raw material out of the kiln, and cutting, polishing and grinding the raw material according to the required shape to obtain a composite foamed ceramic plate;
the bottom layer is one of a ceramic plate sintered at the temperature of more than or equal to 1000 ℃, a green body formed by pressing ceramic tile powder with the known sintering temperature of 1050-1200 ℃, a known stone plate which can not deform and crack under the sintering condition of the step 2) or a cement plate;
the raw material for forming the intermediate layer is a ceramic raw material with the firing temperature of 1050-1200 ℃, wherein the ceramic raw material contains corundum and clinker, and the corundum content is more than or equal to 5 percent and the clinker content is more than or equal to 60 percent in percentage by mass.
It is known to those skilled in the art that the desired architectural ceramic product can be prepared by using common mineral raw materials with reference to the segel formula calculated by oxides under the premise of defining the firing temperature range, and it is noted that the characteristics of different mineral raw materials are matched with the preparation process, for example, the amount of the plastic clay raw material affects the forming performance of the product, which is not described in detail in the prior art. In addition, those skilled in the art also know that silicon carbide is used as a main foaming agent, and the suitable firing temperature is about 1170 ℃, usually not lower than 1050 ℃, below which foaming is difficult; the highest temperature is not more than 1200 ℃, the foaming is violent and is difficult to control, and the formed holes are mainly through holes, so that the strength is difficult to ensure. In addition, it is known that substances which generate free oxygen during high-temperature sintering, such as manganese oxide and iron oxide (preferably iron sesquioxide), can also be added to the foamed ceramic raw material, and of course, those skilled in the art know that manganese and iron have a direct influence on the color of the product, and are usually introduced in small amounts, preferably not more than 1% by mass (also calculated by the added amount). The core improvement point of the scheme is that the raw materials of the middle layer are mainly introduced in the form of frit and corundum, the frit is a glassy substance prepared by melting the raw materials and then water-quenching, the melting temperature is low, a liquid phase can be generated earlier, the corundum is crystallized alumina, the liquid phase viscosity can be well adjusted, so that the frit is suitable for the production of a large-sized foamed ceramic composite plate, the frit is matched with a large-sized kiln tool (2.5 m multiplied by 1.5 m) used for the current foamed ceramic production, the prepared composite foamed ceramic plate product has high flatness, the combination degree of a ground layer and a foamed ceramic layer is good, and products are not layered after being discharged from a kiln or are largely cracked at the combination position to influence the strength of the products. In the production process, the ceramic green body which is not sintered can be used as the bottom layer, and the green body can also shrink and deform in the sintering process, so that the composite foamed ceramic plate can be obtained by sintering once, wherein the green body cannot be used as the bottom layer in the prior art; under the process conditions provided by the scheme, the middle layer can well adjust the stress difference between the foamed ceramic layer and the bottom layer in the firing process, and the deformation of the product is controlled within an acceptable range.
Preferably, the ceramic plate is sintered at the temperature of more than or equal to 1160 ℃ and the water absorption rate of the ceramic plate is less than or equal to 3 percent.
Preferably, the bottom layer is a green body formed by pressing ceramic tile powder with the known sintering temperature of 1120-1190 ℃, and the sintering temperature of the step 2 is 1120-1190 ℃.
Preferably, the middle layer raw material also contains kaolin with the mass percentage of more than or equal to 5%.
Preferably, the interlayer raw material also contains 2 to 7 mass percent of talc.
Preferably, the raw material of the middle layer also contains 0.5 to 3 mass percent of zinc oxide.
Preferably, the firing temperature in the step 2 is 1120-1195 ℃, the raw material for forming the intermediate layer is a ceramic raw material with the firing temperature of 1120-1195 ℃, and the raw material comprises corundum and frit, wherein the corundum content is more than or equal to 7% and the frit content is more than or equal to 70% in percentage by mass.
Preferably, the corundum content is 8-10%, the clinker content is 75-80%, and the raw material of the intermediate layer further contains 8-10% of kaolin, 1-1.5% of zinc oxide and 3-5% of talc.
Preferably, the intermediate layer is formed by coating and/or spraying after raw materials of the intermediate layer are ball-milled into slurry, and the thickness of the intermediate layer is 0.01-0.1 of the thickness of the foamed ceramic raw material layer.
Preferably, the thickness of the bottom layer is more than or equal to 3mm, and the breaking strength is more than or equal to 0.5MPa.
Compared with the prior art, the scheme provided by the invention has wide application range, can be used for compounding the foamed ceramic with different materials, has high process flexibility, low energy consumption and high capacity, and can obtain large-size foamed ceramic products.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Reference examples 1 to 3
Reference is made to application publication No. CN114105670A, and examples 1-3 are prepared as disclosed in example 2. Since the material of the rock plate is not specified, a ceramic plate having a firing temperature of 1200 ℃ and a size of 3m × 1.8m × 0.009m was used as a base material, and the ceramic plate was cut into three sizes of 0.88m × 0.88m × 0.009m, 1.1m × 1.1m × 0.009m, and 2.8m × 1.7m × 0.009m, respectively, and corresponded to reference examples 1, 2, and 3, respectively.
The properties were measured and the results are shown in Table 1 below.
TABLE 1
Sample number Flatness of surface of bottom plate layer Whether the intermediate layer cracks or delaminates
Reference example 1 0.35% Is composed of
Reference example 2 0.53% Slight cracking delamination (about 15%)
Reference example 3 0.86% Large amount of cracking and layering (more than 30 percent)
It is noted that the surface flatness is referred to by the short side length, the deviation of the ceramic tiles is usually required to be within 0.2%, and for composite board products, the thickness of the composite board products can be properly relaxed to 0.5%, which is correspondingly taken as a detection standard.
Examples 1 to 3
In the reference example, 25 parts of albite, 25 parts of glass powder, 10 parts of quartz, 6 parts of calcite, 4 parts of talcum and 6 parts of kaolin in the interlayer powder are melted at high temperature, quenched with water and cooled to prepare frit, the frit and 8 parts of corundum are uniformly mixed, and the frit is mixed by adopting a wet ball milling method and is used after being dried and milled. Ceramic plates having a firing temperature of 1200 ℃ and a size of 3m × 1.8m × 0.009m as the base material in reference examples 1-3 were cut into three sizes of 0.88m × 0.88m × 0.009m, 1.1m × 1.1m × 0.009m, and 2.8m × 1.7m × 0.009m, respectively, corresponding to examples 1, 2, and 3 (the size of the area surrounded by the refractory surrounding edge corresponds to 0.8m × 0.8m, 1.0m × 1.0m, and 2.5m × 1.5 m).
The performance was measured and the comparison results are shown in Table 2 below.
TABLE 2
Sample number Flatness of surface of bottom plate layer Whether the intermediate layer cracks or delaminates
Example 1 0.21% Is free of
Example 2 0.31% Is free of
Example 3 0.44% Very little delamination cracking (about 5%)
Through the comparison, the frit is prepared from the raw material of the middle layer and then is combined with corundum for use, so that the surface smoothness of the product can be improved, the frit is suitable for large-size products, and the frit is suitable for direct transfer of most industrial foamed ceramic production lines (a small amount of layered cracking is allowed in industrial production, and better industrial characteristics can be considered to exist generally when the layered cracking is lower than 10 percent), the equipment transformation investment is low, and the process flexibility is high.
With the technical solution disclosed in application publication No. CN114105670A, it is necessary to machine prefabricated holes or prefabricated grooves for fixing the edge plates on the rock plate, which is also very inconvenient in practical production. The scheme provided by the invention is not required, the bottom layer of the plate can be directly paved at the bottom of the kiln furniture, the side edge of the bottom layer is surrounded by the detachable fixed fire-resistant surrounding edge, then the middle layer and the foamed ceramic material separating layer are sequentially formed, and finally the plate is put into the kiln to be fired, as in embodiment 4.
Example 4
The other process conditions are as in example 3, except that the floor layer is not grooved or perforated, but the fire-resistant surrounding edge is directly surrounded around the floor by a detachable fastening method, and care should be taken during surrounding, at least the surrounding edge is attached to the side edge of the floor or directly placed on the floor. Here we choose the direct placement method, and the size of the enclosed area is 2.5m × 1.5m. And then sequentially forming the middle layer and the foamed ceramic raw material layer, removing the fireproof surrounding edge after sintering and cooling, and cutting, polishing and grinding to obtain the required composite foamed ceramic plate. The properties were tested and the surface flatness was 0.47% and the cracked layered article was about 7.8%. The disassembly and assembly of the fire-resistant surrounding edge are convenient, and the production efficiency can be improved. Although the proportion of cracked layered product is slightly increased, this is within acceptable limits.
In addition, preferably, refractory fiber paper or refractory powder is firstly paved on the kiln furniture to form a separation layer, the bottom of the kiln furniture can be paved, and then the bottom layer is formed, so that the phenomenon that the composite type foamed ceramic is adhered to the kiln furniture after baking is avoided, the phenomenon is the same as the phenomenon that a layer of refractory fiber paper is paved after the refractory surrounding edge is surrounded, the principle of preventing the refractory fiber paper from contacting with the foamed ceramic powder is the same, the refractory fiber at the refractory surrounding edge is paved, an outward flanging is preferably arranged at the bottom of the refractory surrounding edge, namely the refractory surrounding edge is separated from the bottom layer, and therefore the loss of the refractory surrounding edge in the using process can be further reduced.
In addition, the mode of forming the interlayer by laying interlayer powder is relatively unchanged in industrial production, the thickness of the interlayer is relatively thin, and the interlayer is difficult to be uniform for large-size products under the condition that the laying thickness is 2mm or even less. In the preferred embodiment of the present invention, the intermediate layer is obtained by spraying or coating, i.e. the raw material of the intermediate layer is made into slurry which can be sprayed or coated for use.
Example 5
Basically the same as example 4, except that the intermediate layer raw material is treated in a manner of adding kaolin later, that is, the raw materials except for alumina and kaolin are uniformly mixed and then melted to prepare a frit, the frit is mixed with corresponding mass parts of corundum and kaolin and then ball-milled to prepare slurry, and in order to improve the performance of the slurry, sodium carboxymethylcellulose in mass percent is added: 0.25%, sodium tripolyphosphate: 0.2 percent. In this example, the intermediate layer was formed by coating, and the slurry properties in use were as follows: specific gravity: 1.79g/ml; flow rate: 32s; fineness 325 mesh: 1.5-2.0%. Forming an intermediate layer with the thickness of 2mm on the ceramic plate in a coating mode, spreading foamed ceramic powder after drying, putting into a kiln for sintering, removing kiln furniture after cooling, and obtaining the composite foamed ceramic plate after cutting, polishing and grinding. The product performance is tested, the surface flatness of the bottom plate layer is 0.43 percent, the cracking layered products are few, and the loss caused by cracking layering after the product is taken out of the kiln is about 4.3 percent.
Examples 6 to 10
Referring to example 3, corundum was 9.52% by mass, and the balance was frit. We gradually reduced the frit fraction in proportion, for a specific comparison as shown in table 3 below.
TABLE 3
Serial number Mass ratio of clinker Mass ratio of corundum The rest of the mixture ratio
Example 3 90.48% 9.52% ——
Example 6 80.48% 9.52% 10%
Example 7 70.48% 9.52% 20%
Example 8 60.48% 9.52% 30%
Example 9 55.48% 9.52% 35%
Example 10 50.48% 9.52% 40%
For weighing the raw materials of the intermediate layer, the raw materials except corundum are weighed according to the proportion in the embodiment 3, then the raw materials needing to prepare the frit are uniformly mixed, the mixture is weighed according to the proportion in the table 3, the raw materials are melted at high temperature and then water-quenched into the frit, and finally the frit, the corundum and the rest of the mixture are uniformly mixed to prepare the powder of the intermediate layer for later use.
The detection data of the finally prepared composite foamed ceramic plate are shown in table 4 below.
TABLE 4
Figure BDA0003889604130000081
Figure BDA0003889604130000091
Through the tests, the mass percentage of the clinker in the intermediate layer is preferably more than or equal to 60%, and in a similar way, the content of the corundum in the intermediate layer is preferably more than or equal to 6%. Because the suitable temperature for industrially producing the foamed ceramic product is 1050 ℃ -1200 ℃, correspondingly, the known ceramic raw materials which are suitable for being fired at the temperature of the middle layer are matched. The method is difficult to exhaust, the raw material formula of the intermediate layer is also changed in the following examples, but the problems of flatness of a fired product and/or layered cracking of the intermediate layer after firing are solved, the mass percentage of the frit in the intermediate layer is preferably more than or equal to 60%, and the mass percentage of corundum in the intermediate layer is preferably more than or equal to 6. The usage limit of corundum is better not to exceed the limit of the firing temperature range, under the firing temperature range, the usage amount of corundum is better not to exceed 20%, the usage amount range of industrial production is 6% -15% in consideration of comprehensive factors such as raw material cost, and the proportion of corresponding clinker reaches the critical value at 94%.
Another advantage of this solution is that it is possible to use green ceramic tiles as the base material, and we provide example 11 in particular.
Example 11
Selecting SiO as oxide mass percent 2 :69.11%,Al 2 O 3 :17.92%,Fe 2 O 3 :0.94%,TiO 2 :0.16%,CaO:0.95%,MgO:0.98%,K 2 O:3.49%,Na 2 O:2.49%, l.o.i (loss on ignition, 1025 ℃): 4.49 percent of ceramic raw material is ball-milled into slurry, the slurry is prepared after ball-milling processing, the slurry is prepared into powder material by spray granulation, then the powder material is pressed and molded to prepare a mud blank, the specification of the mud blank is 3m multiplied by 1.5m multiplied by 0.15m, and the mud blank is dried for standby.
A layer of refractory fiber paper (made by spreading high-refractory powder such as alumina) is laid on a refractory shed plate of a kiln car, then the mud blank is placed on the refractory shed plate, and then a middle layer is coated, wherein the coating thickness of the middle layer is 2mm.
The middle layer is prepared from the following components in percentage by mass: 77%, talc: 5%, corundum: 7%, zinc oxide: 1%, kaolin: 10 percent. And then adding sodium carboxymethylcellulose in percentage by mass: 0.25% and sodium tripolyphosphate: 0.2 percent. The frit comprises the following components in percentage by mass: ignition loss (1025 ℃): 1.79% of SiO 2 :60.68%,Al 2 O 3 :28.10%,Fe 2 O 3 :0.22%,TiO 2 :0.20%,CaO:0.70%,MgO:0.63%,K 2 O:1.24%,Na 2 O:5.97%,Zr(Hf)O 2 :0.04%,B 2 O 3 <0.05%,BaO<0.05%,Li 2 O:0.02%,PbO<0.01%,ZnO:0.01%,SrO:0.01%,Rb 2 O<0.01%,Cs 2 O<0.01%,CdO<0.01%,P 2 O 5 :0.29%,F<0.05%,SO 3 <0.05%。
The middle layer is ball-milled to prepare slurry, and the slurry has the following properties: specific gravity: 1.79g/ml, flow rate: 32s, fineness 325 mesh: 1.5-2.0%.
And then, enclosing a 2.5m multiplied by 1.5m area on the bottom layer by using the enclosing edge made of refractory materials, wherein the height of the enclosing edge is 200mm, the adjacent parts of the enclosing edge are fixed into a whole through a known detachable buckle, a layer of refractory fiber paper is laid on the inner side of the refractory enclosing edge, and the refractory fiber paper is folded outwards at the bottom of the enclosing edge to separate the bottom and the middle of the refractory enclosing edge so as to bond the refractory enclosing edge without being detached easily after sintering.
Then, the foamed ceramic powder is scattered with the scattering thickness of 60mm. The formula of the foaming ceramic powder is as follows (mass percent): 30% of medium-temperature sand in autumn pavilion, 5% of talc mud, 28% of ceramic tile processing tailings, 2% of wollastonite, 15% of foamed ceramic waste, 20% of ceramic polishing slag, 0.58% of green Silicon (SiC), 0.25% of manganese oxide and ferric oxide: 1.0 percent.
The foaming ceramic powder comprises the following chemical components in percentage by mass: siO 2 2 :64.68%,Al 2 O 3 :20.38%,Fe 2 O 3 :1.01%,TiO 2 :0.22%,CaO:1.71%,MgO:4.12%,K 2 O:2.44%,Na 2 O:2.27%, ignition loss (1025 ℃) 3.36%.
The mixture is fired in a kiln, and the firing system is as follows: 0-650 deg.C, 100min; keeping the temperature at 650 ℃ for 30min;650-950 ℃ for 70min; preserving heat at 950 ℃ for 10min, at 950-1070 ℃ for 2 min, at 1070 ℃ for 35min, at 1070-1120 ℃ for 25min, and at 1120 ℃ for 40min, then naturally cooling and discharging from the kiln, taking out the composite foamed ceramic material from the kiln, cutting, polishing and grinding to obtain the composite foamed ceramic plate.
The surface flatness of the bottom layer of the obtained composite foamed ceramic plate is 0.33%, and the product does not crack and delaminate at the middle layer.
Examples 12 to 15
In this series of examples, we tested the effect of the thinning of the bottom layer, and, with the other parameters unchanged, we gradually reduced the thickness of the blank from 15mm to 5mm. See in particular table 5 below.
TABLE 5
Serial number Thickness of bottom layer Flatness of surface of bottom plate layer Whether the intermediate layer cracks or delaminates
Example 11 15mm 0.33% Is composed of
Example 12 12mm 0.37% Is composed of
Example 13 8mm 0.44% Very little delamination cracking (about 1.8%)
Example 14 6mm 0.45% Very little delamination cracking (about 2.4%)
Example 15 5mm 0.51% Very little delamination cracking (about 4.1%)
The data show that the mud blank has better flatness under the condition that the thickness of the mud blank is more than or equal to 0.6 mm.
Examples 16 to 20
We adjusted the amount of zinc oxide in the interlayer to see the effect of its addition on the composite foamed ceramic composite panel (increasing or decreasing the amount of frit we correspondingly decreased or increased the amount of frit).
Example 13 was chosen as a reference, the bottom layer was a clay body with a thickness of 8mm, and the relationship between the amount of zinc oxide used and the properties of the article was as follows in table 6.
TABLE 6
Figure BDA0003889604130000111
Figure BDA0003889604130000121
In the case of the refractory surrounding edge of example 20, loss increases when the edge comes off after firing, and in view of this, the mass ratio of zinc oxide in the intermediate layer is preferably 1 to 1.5% in industrial production.
Examples 21 to 25
We adjusted the amount of talc in the interlayer (increasing or decreasing the amount of talc we correspond to decreasing or increasing the amount of frit) to see its effect on the properties of the composite foamed ceramic plate. Again, example 13 was chosen as a reference and the relationship between the amount of talc and the properties of the article is given in Table 7 below.
TABLE 7
Serial number Ratio of talc Flatness of bottom plate layer surface Whether the intermediate layer cracks or delaminates
Example 13 5% 0.44% Very little delamination cracking (about 1.8%)
Example 16 —— 0.45% Slight splitting (about 9.8%)
Example 17 1% 0.42% Slight delamination crack (about 7.1%)
Example 18 3% 0.47% Very little delamination cracking (about 3.1%)
Example 19 7% 0.44% Very little delamination cracking (about 2.2%)
Example 20 9% 0.41% Slight delamination crack (about 5.4%)
The amount of talc varied to primarily affect whether the interlayer cracked, preferably at a level of 3% to 7% by the above test.
In addition, after the green body is sintered at 1180 ℃ to form a ceramic plate with water absorption rate less than or equal to 3%, the ceramic plate is used as a bottom material to perform similar tests, and corresponding rules are obtained, which are not described in detail herein.
In addition, the formula and the sintering process of the foamed ceramic can be properly adjusted according to the required density of the prepared composite foamed ceramic plate.
For the bottom layer material, when selecting and using the unburned bricks, need pay attention to the bending strength of unburned bricks should be greater than or equal to 0.5Mpa, otherwise be easy to lose too big in links such as transportation, in addition, when using the unburned bricks as the bottom layer, can use the amalgamation of polylith small-size unburned bricks to adapt to big specification kiln furniture, need pay attention to during the amalgamation can not have the gap at the junction, and the preferred mode that rethread sprays or coats after the amalgamation forms the intermediate level, the intermediate level can be better filled the gap like this, in addition, when follow-up cutting, can follow the amalgamation line and cut.
Example 21
The foaming ceramic powder can also be pressed and formed firstly to prepare a green body matched with the specification of the fire-resistant surrounding edge.
The foamed ceramic powder material of example 11 was press-molded after ball-milling, aging, and spray-drying, and a slab having a specification of 2.5m × 1.5m × 0.3m was used as the bottom layer, which was a ceramic plate having a thickness of 9 mm.
Firstly, a fire-resistant shed plate is laid on a kiln car, then a layer of fire-resistant fiber paper is laid, a ceramic plate is imitated, a middle layer is sprayed, the formula components of the middle layer are as in example 11, the spraying thickness is about 2mm, a foamed ceramic plate blank is stacked after drying, then a fire-resistant surrounding edge is arranged around the plate blank, the fire-resistant fiber paper is laid on one side of the fire-resistant surrounding edge, which faces the foamed ceramic plate blank, the fire-resistant fiber paper is turned outwards at the bottom of the surrounding edge, and the fire-resistant surrounding edge and the middle layer are separated to avoid adhesion after sintering.
Sintering in kiln at 0-650 deg.C for 100min; keeping the temperature at 650 ℃ for 30min;650-950 ℃ for 70min; preserving heat at 950 ℃ for 10min, at 950-1070 ℃ for 2 min, at 1070 ℃ for 35min, at 1070-1120 ℃ for 25min, and at 1120 ℃ for 40min, then naturally cooling, dismantling kiln furniture, cutting and polishing to obtain the composite foamed ceramic plate.
The performance of the material is tested, the surface flatness of the bottom layer is 0.47%, and the delamination and cracking proportion of the middle layer is about 5.8%.
Example 22
The difference is that the intermediate layer used in example 1 is used to obtain a composite foamed ceramic article with a bottom flatness of 0.48% and a delamination cracking percentage of about 9.8%, which can meet the requirements of industrial production.
Example 23
The example 11 was repeated, except that the substrate material was a prefabricated sheet of refractory cement having a thickness of 15mm. The prepared composite foamed ceramic plate also has good performance, the surface flatness of the bottom surface of the composite foamed ceramic plate is 0.35%, and the middle layer does not have the condition of layering and cracking.
Example 24
The difference is that the bottom layer material is artificial stone slab with cement as adhesive, and the thickness is 15mm as in example 11. The bottom surface flatness of the prepared composite foamed ceramic plate is 0.4%, and the middle layer does not have the condition of layering and cracking.
The intermediate layer material using the frit and the corundum as the main raw materials has good adaptability, can be compounded with various bottom layer materials and a foamed ceramic material using silicon carbide as a foaming agent, and is particularly suitable for sintering large-size products. We also tested amorphous alumina, i.e. corundum was replaced by amorphous alumina, which is applicable to small-sized products, but when one side is longer than 1m, the flatness of the bottom surface is difficult to control, and the flatness can exceed the set threshold of 0.5%.
The thickness of the intermediate layer is usually set to 0.5mm to 3mm, and this can be adjusted appropriately according to the thickness of the ceramic foam raw material layer, and is usually between 0.01 and 0.1 of the thickness of the ceramic foam raw material layer.
In addition, cordierite or mullite may be added to the raw material of the ceramic foam as appropriate in order to improve the strength and/or refractoriness of the ceramic foam, and needless to say, similar effects can be obtained by using the raw material containing the above phases, and thus, detailed description thereof is omitted.
For the raw material components of the foamed ceramic layer, when silicon carbide is determined as the main foaming agent, the suitable sintering temperature is 1050-1200 ℃, and the foaming ceramic with low density can be obtained by generally increasing the using amount of the foaming agent, reducing the particle size of the foaming agent, increasing the sintering temperature in the sintering temperature range or increasing the content of flux substances in a basic formula, so that the foaming ceramic raw materials produced by the conventional industrial production can be suitable for the application of the invention.
The arrangement of the fire-resistant surrounding edge ensures that the foaming ceramic raw material only expands and deforms upwards during high-temperature sintering, which is clearly described in the prior art and is not described in detail.
It should be noted here that the rule of formulation change of the middle layer material is substantially the same for different bottom layer materials, and the specific examples are not exhaustive, and those skilled in the art may combine the above examples.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive step, and these embodiments will fall within the scope of the present invention.

Claims (10)

1. A preparation method of a composite foamed ceramic plate comprises the following steps:
step 1) forming a bottom layer, a middle layer and a known foaming ceramic raw material layer which takes silicon carbide as a foaming agent in a refractory kiln furniture with a surrounding edge;
step 2) putting the refractory kiln furniture into a kiln for firing, wherein the firing temperature is 1050-1200 ℃;
step 3), after the ceramic plate is taken out of the kiln, taking out the composite foamed ceramic raw material from the refractory kiln furniture, and cutting and polishing the ceramic raw material according to the required shape to obtain a composite foamed ceramic plate;
the method is characterized in that:
the bottom layer is one of a ceramic plate sintered at the temperature of more than or equal to 1000 ℃, a green body formed by pressing ceramic tile powder with the known sintering temperature of 1050-1200 ℃, a known stone plate which can not deform and crack under the sintering condition of the step 2) or a cement plate;
the raw material for forming the intermediate layer is a ceramic raw material with the firing temperature of 1050-1200 ℃, wherein the ceramic raw material contains corundum and frit, and the corundum content is more than or equal to 5% and the frit content is more than or equal to 60% in percentage by mass.
2. The method for preparing a composite foamed ceramic plate according to claim 1, wherein the ceramic plate is sintered at a temperature of 1160 ℃ or more and has a water absorption of 3% or less.
3. A method for preparing a composite foamed ceramic sheet according to claim 1, wherein said bottom layer is a green body press-formed from ceramic tile powder having a known firing temperature of 1120 ℃ to 1190 ℃, and said firing temperature of step 2 is 1120 ℃ to 1190 ℃.
4. The preparation method of a composite foamed ceramic plate according to claim 1, wherein kaolin is further contained in the intermediate layer raw material in an amount of not less than 5% by mass.
5. A method for manufacturing a composite foamed ceramic plate according to claim 4, wherein the material of the intermediate layer further contains 2 to 7 mass% of talc.
6. A method for making a composite foamed ceramic plate according to claim 1, 4 or 5, wherein the raw material of the intermediate layer further contains 0.5 to 3 mass% of zinc oxide.
7. The method for preparing a composite foamed ceramic plate according to claim 1, wherein the firing temperature in step 2 is 1120-1195 ℃, the raw material for forming the intermediate layer is a ceramic raw material with a firing temperature of 1120-1195 ℃, and the ceramic raw material contains corundum and frit, wherein the corundum content is not less than 7% by mass, and the frit content is not less than 70% by mass.
8. A method for making a composite foamed ceramic plate according to claim 7, wherein said corundum is 8-10%, said clinker is 75-80%, and said intermediate layer further comprises 8-10% kaolin, 1-1.5% zinc oxide and 3-5% talc.
9. A method for preparing a composite foamed ceramic plate according to claim 1, wherein the intermediate layer is formed by ball-milling raw materials into slurry and then coating and/or spraying, and the thickness of the intermediate layer is 0.01 to 0.1 of the thickness of the raw material layer of the foamed ceramic.
10. The method for preparing a composite foamed ceramic sheet according to claim 1, wherein the thickness of the bottom layer is not less than 3mm, and the flexural strength is not less than 0.5Mpa.
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CN112010642A (en) * 2019-05-30 2020-12-01 广东金意陶陶瓷集团有限公司 Production process of foamed ceramic secondary cloth
CN113264783A (en) * 2021-07-20 2021-08-17 佛山市东鹏陶瓷发展有限公司 Prestressed ceramic and preparation method thereof
CN113336444A (en) * 2021-08-05 2021-09-03 佛山市东鹏陶瓷有限公司 High-viscosity middle-layer glaze capable of eliminating polishing glaze pinholes and polishing glazed rock plate using same
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Publication number Priority date Publication date Assignee Title
CN103724023A (en) * 2013-12-16 2014-04-16 广东羚光新材料股份有限公司 Sintering bearing plate for sintering kiln, and preparation method of sintering bearing plate
CN107098705A (en) * 2017-05-25 2017-08-29 佛山市东鹏陶瓷有限公司 A kind of production method of transition zone composite foamed ceramic plate and its application
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CN112010642A (en) * 2019-05-30 2020-12-01 广东金意陶陶瓷集团有限公司 Production process of foamed ceramic secondary cloth
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CN114105670A (en) * 2021-12-09 2022-03-01 洛阳北玻硅巢技术有限公司 Preparation method of rock plate composite light insulation board

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