CN113603497A - Porous ceramic, quickly fired light high-strength ceramic plate and preparation method thereof - Google Patents
Porous ceramic, quickly fired light high-strength ceramic plate and preparation method thereof Download PDFInfo
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Abstract
The invention relates to porous ceramic, a quickly fired light high-strength ceramic plate and a preparation method thereof, belonging to the technical field of building ceramics. The porous ceramic comprises the following preparation raw materials in percentage by weight: 10-20% of clay, 6-20% of wollastonite, 10-20% of bauxite, 1-5% of talc, 28-50% of potassium-sodium feldspar water abrasive and 2-7% of aluminum oxide; the preparation method of the quickly fired light high-strength ceramic plate is characterized in that a high-temperature foaming agent with a certain proportion is added into a substrate porous ceramic formula, and the firing time, the heat preservation temperature and the time are controlled to prepare the quickly fired light high-strength ceramic plate, so that the light high-strength ceramic plate with the internal pore structure with two different formation mechanisms and different size effects is realized; the light high-strength ceramic plate has the characteristics of short sintering time, flexible and controllable realization of an internal porous structure by adopting two different formation mechanisms, higher whiteness and strong high-temperature deformation resistance.
Description
Technical Field
The invention relates to porous ceramic, a quickly fired light high-strength ceramic plate and a preparation method thereof, belonging to the technical field of building ceramics.
Background
The light high-strength ceramic material is combined with the advantages of heat preservation, low water absorption, weather resistance, rich surface decoration effect and the like, and is applied to building curtain walls or outer walls in recent years. According to the industry standard requirement of ' light high-strength ceramic plate for building ' issued by JG/T567-2019, the definition of the light high-strength ceramic plate is ' volume weight of 1.75 g/cm3~1.95g/cm3And the average bending strength is more than or equal to 28MPa, and the minimum bending strength is more than or equal to 23 MPa. At present, the light high-strength ceramic plate realizes low volume weight,The preparation process of high strength usually directly adds carbon black with foaming function, silicon carbide or polishing slag containing silicon carbide component and other high temperature additives. For example, a chinese patent with publication number "CN 106431488B" discloses a light-weight high-strength ceramic plate and a method for preparing the same, which specifically discloses a method for preparing light-weight high-strength ceramic by using silicon carbide as a foaming agent; for example, a Chinese patent with a publication number of 'CN 110171955A' discloses a light-weight high-strength pure-color ceramic plate and a preparation method thereof, and particularly discloses a method for preparing light-weight high-strength ceramic by directly adding a solid waste foaming agent. However, since the foaming agent is not easily controlled at the high temperature foaming stage during the firing process of the kiln, the prior art can only control the uniformity of the internal structure of the porous ceramic material by prolonging the heat preservation time and the temperature reduction time. At present, the production and preparation of the light high-strength ceramic plate for the building are generally carried out at the sintering temperature of 1150-1200 ℃, the production sintering period is generally as high as 180-240 minutes, compared with the conventional ceramic plate for the building (the sintering period is generally 60-100 minutes), more fuel is consumed, and more CO is discharged2And (4) exhaust gas.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a porous ceramic which has low density and high strength and can be quickly sintered.
The invention also aims to provide a preparation method of the quickly fired light high-strength ceramic plate, the sintering time of the quickly fired light high-strength ceramic plate prepared by the preparation method is greatly shortened compared with the existing light high-strength ceramic plate, and the product performance of the quickly fired light high-strength ceramic plate meets the industrial standard requirements of light high-strength ceramic plates for buildings and can be applied to decorative plates of building curtain walls.
In order to achieve the purpose, the invention adopts the technical scheme that: the porous ceramic comprises the following preparation raw materials in percentage by weight: 10-20% of clay, 6-20% of wollastonite, 10-20% of bauxite, 1-5% of talcum, 28-50% of potassium-sodium feldspar water abrasive and 2-7% of aluminum oxide.
In a preferred embodiment of the porous ceramic according to the present invention, the porous ceramic has a chemical composition in which calcium oxide is contained in an amount of 4.2% by mass or more.
In a preferred embodiment of the porous ceramic according to the present invention, the chemical composition of the porous ceramic has a ratio of calcium oxide to magnesium oxide in percentage by mass of 4.7 or more.
The porous ceramic of the present invention may be prepared according to a conventional method for preparing a construction ceramic, and is not particularly limited herein.
The porous ceramic is a low-density ceramic product taking anorthite and quartz as main crystal phases after being sintered at a proper temperature, wollastonite and talcum which have low-temperature quick-sintering functions and have a reduction effect on volume weight are introduced into a raw material formula, and Ca is contained in the formula by adjusting2+、K+ 、Na+ 、Mg2+The proportion of the four fluxed raw materials is matched with the optimal firing system, so that the porous ceramic with high strength, low water absorption and rapid firing is realized. The volume weight of the porous ceramic and the conventional architectural ceramic tile is 2.4g/cm3About) and the breaking strength (about 40 MPa), the volume weight is reduced by about 10 percent, the strength is reduced by about 5 percent, and the water absorption is lower than 0.1 percent.
In addition, another object of the present invention is to provide a method for preparing a lightweight high-strength ceramic plate that is rapidly fired, comprising the steps of:
(1) weighing the raw materials according to the formula of the porous ceramic;
(2) adding a certain amount of high-temperature foaming agent and dispersing agent into the raw materials of the porous ceramic in the step (1), uniformly mixing, performing wet ball milling to obtain ceramic slurry, and performing spray drying to obtain ceramic powder;
(3) pressing the ceramic powder obtained in the step (2) into a ceramic blank, and then sequentially drying, glazing and firing to obtain the quickly fired light-weight high-strength ceramic plate;
the porous ceramic in the step (1) is the porous ceramic provided by the invention.
As a preferable embodiment of the preparation method of the present invention, in the step (2), the weight ratio of the porous ceramic to the high-temperature foaming agent is 85 to 99.95: 0.05-20 percent, and the addition amount of the dispersant is 0.7-1.8 percent of the total weight of the raw materials of the porous ceramic.
In a preferred embodiment of the preparation method of the present invention, the high-temperature foaming agent is at least one of carbon black, silicon carbide and polishing slag containing silicon carbide; the dispersant is at least one of water glass and sodium tripolyphosphate. Specifically, the inorganic dispersant added in the preparation method provided by the invention has the effects that the inorganic dispersant is adsorbed on the surface of the ceramic powder particles after being ionized into ions, so that the surface charge density is improved, the van der Waals attractive force among the particles is overcome through the repulsion effect of the same kind of charges on the surface, the dispersion effect is realized, and the ball milling time is shortened.
In a preferred embodiment of the method of the present invention, the carbon black is added in an amount of 1 to 3% by weight, the silicon carbide is added in an amount of 0.1 to 0.4% by weight, and the polishing residue containing a silicon carbide component is 5 to 15% by weight, based on the total weight of the raw materials of the porous ceramic.
As a preferred embodiment of the preparation method, in the step (2), the ball milling medium of the wet ball milling is water, and the time of the wet ball milling is 4-6 h; the flow rate of the ceramic slurry is 40-60s, and the residue of the ceramic slurry after passing through a 250-mesh sieve is less than 1.0%; the water content of the ceramic powder is 5-8%. Specifically, the flow rate control and the granularity setting of the ceramic slurry ensure that the ceramic has good forming performance and the uniformity of the whole ceramic is good.
As a preferred embodiment of the preparation method of the invention, in the step (3), the firing temperature for firing is 1150-1200 ℃, and the firing time is 100-120 min. Specifically, according to different types of added high-temperature foaming agents, the firing temperature and the firing time need to be properly adjusted to be matched with the formula of the substrate ceramic, so that two pore structures with different formation mechanisms and different size effects are realized, and a light-weight high-strength ceramic product with lower volume weight is obtained; the volume weight of the light high-strength ceramic product is 1.75-1.95g/cm3The water absorption is less than or equal to 0.5 percent, and the breaking strength is more than 28 MPa.
As a preferable embodiment of the production method of the present invention, the production method further includes a step (4) of performing a post-treatment process after the completion of the step (3); the step (4) is a treatment process conventionally applied in the field, and the invention is not limited; for example, the method comprises edging, surface treatment, back grooving and the like of the light high-strength ceramic.
Meanwhile, the invention also aims to provide a quickly fired light-weight high-strength ceramic plate, which is prepared by the preparation method.
The quickly fired light high-strength ceramic plate is prepared by combining two pore-forming processes, and the volume weight of the quickly fired light high-strength ceramic plate is obtained by a novel self-developed porous ceramic formula at first, and is 2.1-2.3 g/cm3The rupture strength is not lower than 38MPa, and the content of anorthite crystals is about 8 percent; secondly, by adding a high-temperature foaming agent in a certain proportion into the porous ceramic formula, controlling the firing time, the heat preservation temperature and the time, increasing the number of closed pores, and controlling the pore size and the distribution, the light high-strength ceramic plate which is rapidly fired by the internal pore structure with two different formation mechanisms and different size effects is realized. The final product performance meets the industrial standard requirements of light high-strength ceramic plates for buildings, the firing period is within 120 minutes, 1/3 is shortened compared with the firing period (more than 180 minutes) of the prior art, the whiteness of the product reaches 65 ℃, the production process flow is consistent with that of the traditional building ceramics, and the production investment is less.
The porous ceramic has the following functions in the quickly fired light high-strength ceramic: the substrate formula system has the advantages of reducing the density to a certain degree, retaining higher flexural strength and high-temperature deformation resistance and realizing quick sintering.
Compared with the prior art, the invention has the beneficial effects that:
(1) the sintering time is short: because the growth time of the anorthite crystal is faster than that of the mullite crystal, the quick-fired light-weight high-strength ceramic plate prepared by adopting the low-density porous ceramic taking the anorthite and the quartz as main crystal phases as the substrate and adding the foaming agent is adopted, compared with the light-weight high-strength ceramic plate prepared by the method in the prior art (directly adding the foaming agent in a mullite substrate ceramic system), the firing period of the light-weight high-strength ceramic plate is shortened by 1/3-1/4, the problem of long firing time of the light-weight high-strength ceramic is solved, the energy is greatly saved, and the emission of waste gas is reduced;
(2) the internal porous structure is designed by adopting two different formation mechanisms, and is flexible and controllable: by adding a high-temperature foaming agent in a certain proportion into the formula of the porous ceramic and controlling the sintering time, the heat preservation temperature and the sintering time, an internal composite porous structure with two different pore sizes and uniform distribution is realized, wherein foaming macropores (100-250 mu m) and pores (less than or equal to 70 mu m) formed in an anorthite crystal system exist in the material at the same time; according to the relationship between porosity and strength, the more macropores, the more rapid the effective area rate is reduced, so that the load of the material which is damaged integrally is smaller for porous materials with the same matrix strength and porosity, and under the condition of the same porosity, the existence of the small pores in the anorthite crystal system can not only assist in reducing the density of the product, ensure the flexural strength and the product flatness of the product, but also reduce the requirement of an additional foaming agent on the high strength of the substrate ceramic;
(3) and the whiteness is higher: under the condition that whitening agents (such as zirconium silicate and the like) are not added, the whiteness of the quickly fired light high-strength ceramic plate reaches about 65 degrees, so that the vividness and diversity of decorative effect colors in the traditional glazing process are more prominent, the addition amount of zirconium silicate in overglaze is reduced, the production cost of products is obviously reduced, and the grade and the health and environmental protection grade of the products are improved;
(4) and the high-temperature deformation resistance is strong: the formula system of the quickly-fired light high-strength ceramic plate provided by the invention has higher high-temperature deformation resistance in the firing process, and can prepare a product with a thickness (10-22 mm) thinner than the thickness (18 mm and 22 mm) of the product in the industry standard under the condition of meeting the industry standard requirement of light high-strength ceramic plate for buildings;
(5) and the production investment is less: all raw materials in the rapidly fired light high-strength ceramic plate provided by the invention are from traditional building ceramic raw materials or industrial waste materials, the sources are wide, the production process flow is basically consistent with that of the traditional building ceramic, and the equipment investment of online production is reduced.
Drawings
FIG. 1 is a high scanning electron microscope photograph of the microstructure at the fracture of a rapidly fired, lightweight, high strength ceramic plate according to example 1 of the present invention;
FIG. 2 is a high-power scanning electron microscope photograph of the microstructure at the fracture of the porous ceramic substrate in comparative example 1 of the present invention;
FIG. 3 is a high scanning electron microscope photomicrograph of the microstructure of the ceramic fracture in comparative example 2 of the present invention;
FIG. 4 is a graph comparing the resistance to deformation at high temperatures for four different formulations of ceramic; wherein, the sample a is the substrate ceramic without anorthite crystal phase described in the comparative example 2, the sample b is the ceramic described in the comparative example 1, the sample c is the light high-strength ceramic plate described in the example 1, and the sample d is the ceramic described in the comparative example 2.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following detailed drawings and examples.
The following examples and comparative examples were all commercially available starting materials unless otherwise specified.
Example 1
The embodiment of the invention relates to a method for preparing a quickly-fired light-weight high-strength ceramic plate, which comprises the following steps:
(1) weighing the raw materials according to the formula of the porous ceramic;
(2) adding a silicon carbide foaming agent (the addition amount accounts for 0.1 percent of the total weight of the porous ceramic raw material) and water glass (the addition amount accounts for 0.7 percent of the total weight of the porous ceramic raw material) into the raw material of the porous ceramic in the step (1); after uniformly mixing, carrying out wet ball milling for 4h by taking water as a medium to obtain ceramic slurry, and carrying out spray drying on the ceramic slurry at the flow rate of 46s to obtain ceramic powder with the screen residue of 0.8 percent and the water content of 6.4 percent of a 250-mesh sieve;
(3) pressing the ceramic powder obtained in the step (2) into a ceramic blank, and then sequentially drying, glazing and firing at 1170 ℃ for 120min to obtain the quickly fired light high-strength ceramic plate;
(4) carrying out subsequent treatment on the quickly fired light ceramic plate obtained in the step (3), wherein the subsequent treatment comprises edge grinding, surface treatment and back grooving;
the porous ceramic comprises the following preparation raw materials in percentage by weight: 16% of clay, 12% of wollastonite, 16% of bauxite, 3% of talc, 49% of potassium-sodium feldspar water abrasive and 4% of aluminum oxide; in the chemical components of the porous ceramic, the mass percentage of calcium oxide is 6.1%, and the mass percentage ratio of calcium oxide to magnesium oxide is 5.
Example 2
The embodiment of the invention relates to a method for preparing a quickly-fired light-weight high-strength ceramic plate, which comprises the following steps:
(1) weighing the raw materials according to the formula of the porous ceramic;
(2) adding high-temperature foaming agent carbon black (the adding amount accounts for 1% of the total weight of the porous ceramic raw materials) and dispersing agent sodium tripolyphosphate (the adding amount accounts for 1.8% of the total weight of the porous ceramic raw materials) into the raw materials of the porous ceramic in the step (1), uniformly mixing, carrying out wet ball milling for 4 hours by taking water as a medium to obtain ceramic slurry, carrying out spray drying on the ceramic slurry at the flow rate of 40s to obtain ceramic powder with the screen residue of a 250-mesh sieve of less than 1.0% and the water content of 5%;
(3) pressing the ceramic powder obtained in the step (2) into a ceramic blank, and then sequentially drying, glazing and firing at 1150 ℃ for 100min to obtain the quickly fired light high-strength ceramic plate;
(4) carrying out subsequent treatment on the quickly fired light ceramic plate obtained in the step (3), wherein the subsequent treatment comprises edge grinding, surface treatment and back grooving;
the porous ceramic comprises the following preparation raw materials in percentage by weight: 20% of clay, 9.8% of wollastonite, 10.2% of bauxite, 2.5% of talc, 45% of potassium-sodium feldspar water abrasive, 2.5% of aluminum oxide, 4.9% of calcium oxide by mass and 5.5% of the ratio of calcium oxide to magnesium oxide by mass.
Example 3
The embodiment of the invention relates to a method for preparing a quickly-fired light-weight high-strength ceramic plate, which comprises the following steps:
(1) weighing the raw materials according to the formula of the porous ceramic;
(2) adding polishing residues containing silicon carbide and sodium tripolyphosphate serving as a dispersing agent (the adding amount accounts for 10% of the total weight of the porous ceramic raw materials) and sodium tripolyphosphate serving as a dispersing agent (the adding amount accounts for 1% of the total weight of the porous ceramic raw materials) into the raw materials of the porous ceramic obtained in the step (1), uniformly mixing, carrying out wet ball milling for 6 hours by taking water as a medium to obtain ceramic slurry, and carrying out spray drying on the ceramic slurry at the flow rate of 60s to obtain ceramic powder with the screen residue of a 250-mesh screen being less than 1.0% and the water content being 8%;
(3) pressing the ceramic powder obtained in the step (2) into a ceramic blank, and then sequentially drying, glazing and firing at 1200 ℃ for 120min to obtain the quickly fired light high-strength ceramic plate;
(4) carrying out subsequent treatment on the quickly fired light ceramic plate obtained in the step (3), wherein the subsequent treatment comprises edge grinding, surface treatment and back grooving;
the porous ceramic comprises the following preparation raw materials in percentage by weight: 12% of clay, 14% of wollastonite, 18% of bauxite, 4% of talc, 50% of potassium-sodium feldspar water abrasive and 2% of aluminum oxide; the mass percentage of the calcium oxide is 5.9 percent, and the mass percentage ratio of the calcium oxide to the magnesium oxide is 4.8.
Example 4
The embodiment of the invention relates to a method for preparing a quickly-fired light-weight high-strength ceramic plate, which comprises the following steps:
(1) weighing the raw materials according to the formula of the porous ceramic;
(2) adding a silicon carbide foaming agent (the addition amount accounts for 0.4 percent of the total weight of the porous ceramic raw material) and a dispersing agent sodium tripolyphosphate (the addition amount accounts for 1.2 percent of the total weight of the porous ceramic raw material) into the raw material of the porous ceramic in the step (1), uniformly mixing, carrying out wet ball milling for 5 hours by taking water as a medium to obtain ceramic slurry, and carrying out spray drying on the ceramic slurry at the flow rate of 50s to obtain ceramic powder with the sieve residue of a 250-mesh sieve of less than 1.0 percent and the water content of 7 percent;
(3) pressing the ceramic powder obtained in the step (2) into a ceramic blank, and then sequentially drying, glazing and firing at 1200 ℃ for 120min to obtain the quickly fired light high-strength ceramic plate;
(4) carrying out subsequent treatment on the quickly fired light ceramic plate obtained in the step (3), wherein the subsequent treatment comprises edge grinding, surface treatment and back grooving;
the porous ceramic comprises the following preparation raw materials in percentage by weight: 20% of clay, 20% of wollastonite, 20% of bauxite, 5% of talc, 28% of potassium-sodium feldspar water abrasive and 7% of aluminum oxide; the mass percentage of the calcium oxide is more than or equal to 4.2 percent, and the mass percentage ratio of the calcium oxide to the magnesium oxide is more than or equal to 4.7.
Example 5
The embodiment of the invention relates to a method for preparing a quickly-fired light-weight high-strength ceramic plate, which comprises the following steps:
(1) weighing the raw materials according to the formula of the porous ceramic;
(2) adding carbon black (the adding amount accounts for 3% of the total weight of the porous ceramic raw materials) and dispersant sodium tripolyphosphate (the adding amount accounts for 1.8% of the total weight of the porous ceramic raw materials) into the porous ceramic raw materials in the step (1), uniformly mixing, carrying out wet ball milling for 5 hours by taking water as a medium to obtain ceramic slurry, and carrying out spray drying on the ceramic slurry at the flow rate of 45s to obtain ceramic powder with the screen residue of a 250-mesh sieve of less than 1.0% and the water content of 6%;
(3) pressing the ceramic powder obtained in the step (2) into a ceramic blank, and then sequentially drying, glazing and firing at 1180 ℃ for 110min to obtain the quickly fired light high-strength ceramic plate;
(4) carrying out subsequent treatment on the quickly fired light ceramic plate obtained in the step (3), wherein the subsequent treatment comprises edge grinding, surface treatment and back grooving;
the porous ceramic comprises the following preparation raw materials in percentage by weight: 20% of clay, 6% of wollastonite, 18% of bauxite, 4% of talc, 50% of potassium-sodium feldspar water abrasive and 2% of aluminum oxide; the mass percentage of the calcium oxide is more than or equal to 4.5 percent, and the mass percentage ratio of the calcium oxide to the magnesium oxide is more than or equal to 5.
Example 6
The embodiment of the invention relates to a method for preparing a quickly-fired light-weight high-strength ceramic plate, which comprises the following steps:
(1) weighing the raw materials according to the formula of the porous ceramic;
(2) adding polishing residues containing silicon carbide and a dispersant sodium tripolyphosphate (the addition accounts for 15% of the total weight of the porous ceramic raw materials) and a dispersant sodium tripolyphosphate (the addition accounts for 1.8% of the total weight of the porous ceramic raw materials) into the porous ceramic raw materials in the step (1), uniformly mixing, carrying out wet ball milling for 6 hours by taking water as a medium to obtain ceramic slurry, and carrying out spray drying on the ceramic slurry at a flow rate of 60s to obtain ceramic powder with a sieve residue of less than 1.0% and a water content of 8% of a 250-mesh sieve;
(3) pressing the ceramic powder obtained in the step (2) into a ceramic blank, and then sequentially drying, glazing and firing at 1200 ℃ for 120min to obtain the quickly fired light high-strength ceramic plate;
(4) carrying out subsequent treatment on the quickly fired light ceramic plate obtained in the step (3), wherein the subsequent treatment comprises edge grinding, surface treatment and back grooving;
the porous ceramic comprises the following preparation raw materials in percentage by weight: 12% of clay, 14% of wollastonite, 18% of bauxite, 4% of talc, 50% of potassium-sodium feldspar water abrasive and 2% of aluminum oxide; the mass percentage of the calcium oxide is 5.9 percent, and the mass percentage ratio of the calcium oxide to the magnesium oxide is 4.8.
Comparative example 1
This comparative example is a ceramic prepared in the same manner as in example 1 except that no high temperature foaming agent was added.
Comparative example 2
This comparative example is a ceramic, compared to example 1, using a conventional anorthite crystal phase-free base ceramic (formulation 25% clay, 20% bauxite, 48% potash-sodalite water abrasive, 3% talc, 4% alumina), other ingredients and preparation steps identical to example 1.
Comparative example 3
This comparative example is three ceramics, which are named as A, B and C, respectively, and the components and preparation steps of the three ceramics are the same as those of examples 1-3 except that the high-temperature foaming agent is added in an amount different from that of examples 1-3 (wherein A, B, C high-temperature foaming agents of the three ceramics are silicon carbide, carbon black and polishing slag containing silicon carbide), and A, B, C high-temperature foaming agents are added in amounts of 0.05%, 0.5% and 4% of the total weight of the porous ceramic raw material, respectively.
Comparative example 4
This comparative example is three ceramics, which are named D, E, F, D, E, F respectively, except that the amounts of the high-temperature foaming agents added are different from those of examples 4-6, the other components and the preparation steps are respectively the same as those of examples 4-6 (wherein D, E, F the high-temperature foaming agents of the three ceramics are respectively silicon carbide, carbon black, and polishing slag containing silicon carbide), and D, E, F the amounts of the high-temperature foaming agents added to the three ceramics are respectively 1%, 4% and 20% of the total weight of the porous ceramic raw material.
Experimental example 1
This experimental example measured the water absorption, the average flexural strength and the volume weight of the ceramic plates according to examples 1 to 6 of the present invention and comparative examples 1 to 4, and the measurement results are shown in table 1.
Sample water absorption and volume weight test methods: according to GB/T3810.3-2016 ceramic tile test method part 3: the method is characterized in that the method comprises the following steps of (1) testing the measurement of water absorption, apparent porosity, apparent relative density and volume weight [ ]: the water absorption is tested by a vacuum method, the brick is placed in a drying oven at the temperature of (110 +/-5) DEG C and dried to constant weight, namely the difference between two continuous masses every 24 hours is less than 0.1 percent, and the m percent of the weight record is weighed1. Vertically placing the bricks in a vacuum container to make the bricks mutually contactNon-contact, vacuumizing to (10 +/-1) KPa, maintaining for 30min, stopping vacuumizing, adding enough water to cover the brick and raise the height by 5cm, soaking the brick for 15min, taking out, wiping off surface water, immediately weighing and recording m2vBy the formula EV=(m2v-m1)/ m1Calculating the x 100% to obtain the water absorption, wherein EVIs made of m2vAnd (4) measuring the water absorption rate. Sample volume weight B the dry weight m of the sample1Divided by the apparent volume V, by the formula B = m1And calculating the volume weight of the sample by using the volume ratio of the water to the water.
The flexural strength test method comprises the following steps: according to GB/T3810.4-2016 ceramic tile test method part 4: the test is carried out according to the determination of modulus of rupture and breaking strength, and the specific test method is as follows: using a three-point method, by the formula R =3Fl2/2bh2Calculating to obtain modulus of rupture, namely breaking strength, and calculating the average value of the breaking strength of the five bricks, wherein R is the modulus of rupture, and F is the breaking load l2Is the span between two support rods, b is the width of the sample, and h is the minimum thickness of the fracture surface of the sample measured along the fracture edge after the test.
TABLE 1 test results of water absorption, flexural strength and volume weight of ceramic plate
As shown from the data results of Table 1, the ceramic plates of examples 1 to 6 (the rapidly fired lightweight, high-strength ceramic plates according to the present invention) all had flexural strengths of more than 28MPa on the average and bulk weights of 1.75 g/cm on the average3-1.95 g/cm3Within the range of (1), the ceramic plate meets the industrial standard requirements of the light high-strength ceramic plate.
Comparative examples 1-2 compared to example 1: the ceramic plate of comparative example 1, which had a water absorption (0.035) and an average flexural strength (43 MPa) in accordance with the industrial requirements without adding a high-temperature foaming agent, had a bulk density (2.25 g/cm)3) Does not meet the industrial standard requirements of the light high-strength ceramic plate; the ceramic plate of comparative example 2, which had an average flexural strength due to the porous ceramic having no anorthite crystal phase as the base ceramic(30 MPa) and volume weight (1.89 g/cm)3) Although the physical properties required by the industry are met, the high-temperature deformation resistance of the alloy is poor, and the appearance and the flatness of the product cannot be ensured.
Comparative example 3 compared to examples 1-3: the three ceramics A, B, C of comparative example 3 were prepared with blowing agents added in the respective amounts: in example 1, the addition amount of silicon carbide is reduced from 0.1% to 0.05%, in example 2, the addition amount of carbon black is reduced from 1% to 0.5%, in example 3, the addition amount of polishing waste slag is reduced from 10% to 4% (the addition amount is percentage of the total weight of the porous ceramic raw material), and the obtained A, B, C three ceramic plates have the water absorption rate of less than 0.1%, the flexural strength of more than 38MPa and the volume weight of more than 2.0 g/cm3(ii) a It can be seen that the water absorption of A, B, C three ceramics is equivalent to that of the ceramics plates of examples 1-3, the average value of the flexural strength also meets the industry standard requirement of the light high-strength ceramics plate, but the volume weight does not meet the industry standard requirement of the light high-strength ceramics plate.
Comparative example 4 compared to examples 4-6: the three ceramics D, E, F of comparative example 4 were prepared with blowing agents added in the respective amounts: the amount of silicon carbide in example 4 was increased to 0.1% to 1%, the amount of carbon black in example 5 was increased to 1% to 4%, and the amount of polishing waste in example 6 was increased to 10% to 20%; the water absorption of the three ceramics D, E, F is lower than 0.1%, the average value of the flexural strength is lower than 15MPa, and the volume weight is lower than 1.6 g/cm3(ii) a It can be seen that the average flexural strength and volume weight of the three ceramics D, E, F do not meet the industry standard requirements of light-weight high-strength ceramic plates.
Since comparative example 1 does not contain the foaming agent, the volume weight of the ceramic material does not meet the industrial standard requirement of the light high-strength ceramic plate, and comparative example 2 does not contain the porous ceramic with anorthite crystal phase as the substrate ceramic, the ceramic material has lower high-temperature deformation resistance, and the appearance and the flatness of the product cannot be ensured. Therefore, the fast-fired light-weight high-strength ceramic plate provided by the invention is prepared by adopting a method combining two pore-forming processes, the independently developed novel porous ceramic is used as a substrate ceramic, a high-temperature foaming agent with a certain proportion is added into a formula of the porous ceramic, the firing time, the heat preservation temperature and the firing time are controlled, the number of closed pores is increased, the pore size and the distribution are controlled, and the fast-fired light-weight high-strength ceramic plate with an internal pore structure with two different formation mechanisms and different size effects is realized; if there is no one of the porous ceramic and the foaming agent, the rapid-fired lightweight high-strength ceramic plate according to the present invention cannot be obtained.
In addition, compared with the three ceramics A, B, C of comparative example 3, the volume weight of the ceramic plate does not meet the industry standard requirement of the light-weight high-strength ceramic plate because the addition amount of the foaming agent is lower than the range of the foaming agent of the invention; compared with the three ceramics D, E, F of comparative example 4 and examples 4-6, the addition amount of the foaming agent is higher than the range of the foaming agent, so that the average flexural strength and the volume weight of the ceramic plate do not meet the industry standard requirements of the lightweight high-strength ceramic plate. Therefore, the addition amount of the foaming agent of the fast-fired light-weight high-strength ceramic plate provided by the invention needs a reasonable range, namely the addition amount of the foaming agent needs to be in the range provided by the invention, otherwise, the fast-fired light-weight high-strength ceramic plate provided by the invention cannot be obtained.
Experimental example 2
In this experimental example, the high-strength ceramic plate of example 1 of the present invention was subjected to phase analysis using a Dmax2500VB X-ray diffractometer (XRD), and the results are shown in Table 2.
TABLE 2 semi-quantitative XRD analysis of the rapidly fired, lightweight, high strength ceramic slabs as described in example 1
The results in table 2 show that: the light high-strength ceramic plate provided by the invention is different from the conventional ceramic formula with main crystal phases of mullite and quartz, and the light high-strength ceramic plate provided by the embodiment 1 of the invention has a high anorthite crystal phase (8%) and a part of quartz phase, and almost no mullite crystal phase. The light high-strength ceramic plate provided by the invention is proved to be essentially different from a formula system mainly comprising anorthite crystals by fully proving that the formula system mainly comprises anorthite crystals.
Experimental example 3
In the experimental example, the microstructure at the fracture of the light high-strength ceramic in example 1 of the invention, the microstructure at the fracture of the porous ceramic of the substrate in comparative example 1 and the microstructure at the fracture of the ceramic in comparative example 2 were subjected to microstructure morphology observation (SEM); FIG. 1 is a high scanning electron microscope photomicrograph of the microstructure at the fracture of a lightweight, high strength ceramic in example 1 of the present invention; FIG. 2 is a high-power scanning electron microscope photograph of the microstructure at the fracture of the porous ceramic substrate in comparative example 1 of the present invention; FIG. 3 is a high-power scanning electron micrograph of the microstructure of the ceramic fracture in comparative example 2 of the present invention.
The results of FIGS. 1-3 illustrate that the addition of the same blowing agent, silicon carbide, in the same proportions in the inventive formulation and in the conventional formulation, respectively, results in very different cell structures and sizes. As shown in FIG. 1, the pore diameter of the light high-strength ceramic in embodiment 1 of the present invention is in the range of 10 to 250 um; from the figure 3, the porous ceramic prepared by adding the same foaming agent silicon carbide in the same proportion into the conventional formula ceramic has the pore diameter within the range of 200-1000 um, which shows that the porous ceramic formula system has excellent effect of controlling the internal pore diameter of the foaming agent. From the SEM results of the sample shown in FIG. 2, the porous ceramic prepared by the base calcium formula of the present invention has uniformly distributed micropores with the pore diameter ranging from 0 to 70um without adding any foaming agent. The results of fig. 1 and 2 show that the lightweight high-strength ceramic product of the present invention has a microporous structure with two different formation mechanisms and two different pore size ranges.
Experimental example 4
In the experimental example, the high-temperature deformation resistance of the ceramic is detected, and the method for testing the high-temperature deformation resistance of the ceramic is to prepare four comparative ceramic samples into sample strips with uniform sizes, wherein the sample strips are all 100mm (length), 20mm (width) and 8.8mm (height). Simultaneously put into side by side about being equipped with support function's resistant firebrick respectively, the sample span sets up to 80mm in unison, and the system of firing sets up to in unison: the firing temperature is 1200 ℃, the temperature rise time is 120 minutes, and the heat preservation time is 30 minutes. Method for comparing high temperature deformation resistance: the samples after firing were taken out and the distance between the most concave point of the sample and the horizontal plane at both ends of the sample was calculated (see table 3 and fig. 4).
Four comparative ceramic samples, having the following sample numbers:
a. a sample of conventional base ceramic (the conventional base ceramic described in comparative example 2 of the present invention, which was formulated with 25% clay, 20% bauxite, 48% potash-soda feldspar water abrasive, 3% talc, 4% alumina);
b. sample of the substrate porous ceramic according to the invention (ceramic according to comparative example 1 according to the invention)
c. Samples of lightweight, high-strength ceramics according to the invention (lightweight, high-strength ceramic plates according to example 1 according to the invention)
d. Conventional lightweight high-strength ceramic sample (ceramic of comparative example 2 according to the invention)
TABLE 3 comparison of the high temperature deformation resistance of the materials of different formulations
The results shown in table 3 and fig. 4 show that: the high temperature deformation resistance of the base porous ceramic of the present invention (sample b, i.e., the ceramic described in comparative example 1) and the conventional base ceramic (sample a, i.e., the base ceramic without anorthite crystal phase described in comparative example 2) at the same temperature (1200 c) were not significantly different (the high temperature deformation amounts were 4mm each) without adding any foaming agent. Samples c and d prepared by adding the same amount of foaming agent of the same type into the two formula systems of the sample a and the sample b respectively show that the high-temperature deformation of the light high-strength ceramic sample (sample c, namely the light high-strength ceramic plate in the embodiment 1) is still 4mm at the same temperature (1200 ℃); compared with the conventional lightweight high-strength ceramic sample (sample d is obtained by directly adding the foaming agent into sample a, namely the ceramic in comparative example 2), the high-temperature deformation of the conventional lightweight high-strength ceramic sample is up to 10mm, and in conclusion, the porous ceramic provided by the invention has better high-temperature deformation capability.
It can be seen from the above examples and experimental examples that the optimum combination of the two different formation mechanisms and the pore-forming processes with different pore structures is the key point for finally realizing high-performance light-weight high-strength ceramic and one-time rapid firing.
Firstly, compared with the conventional ceramic formula, the calcium-based porous ceramic provided by the invention is used as the substrate of the light high-strength ceramic plate, and the formula design needs to meet the conditions of low density, excellent high-temperature deformation resistance, higher rupture strength and capability of realizing quick firing. If the content of calcium and magnesium in the formula of the porous ceramic is too low (or the proportion is not proper), on one hand, the small air holes are difficult to be formed at the positions close to the periphery where the anorthite is formed in a connected mode, the density reduction is realized by adding more high-temperature foaming agents, and the uncontrollable risk of the brick shape is increased; on the other hand, the characteristic of low-temperature solid-phase reaction of calcium-containing silicate cannot be utilized to realize the preparation condition of quick firing; if the content of calcium and magnesium in the formula of the porous ceramic is excessive (or the proportion is improper), the closed pore forming amount is increased, the density, the strength and the high-temperature deformation resistance of a sample are reduced too much, after a high-temperature foaming agent is added, the density, the strength and the flatness of the sample are continuously reduced, and finally, various physical properties of the light high-strength ceramic are difficult to control; in a high-temperature deformation resistance test, the silicon carbide foaming agent with the same mass percentage (0.05%) is respectively added into the porous ceramic formula and the conventional substrate ceramic formula, and the same rapid firing system is adopted, so that the results show that: the porous ceramic provided by the invention has the same volume weight (1.8 g/cm) as a sample prepared by a conventional porous ceramic formula3) However, the tortuosity of the latter (10 mm) is 2.5 times that of the former (4 mm), which shows that the porous ceramic provided by the present invention has a significant advantage in high temperature deformation resistance (see fig. 4 and table 2).
Secondly, in order to optimize the physical properties of the material by the internal closed pore structures with two different formation mechanisms, an optimal firing system needs to be researched, and finally the control of the internal pore structure (pore size and pore distribution) of the porous ceramic substrate is realized so as to achieve the optimal physical properties. Since the smaller the pore size, the stronger the sample at the same porosity, controlling the pore size inside the sample is more helpful to increase the strength of the sample. The patent research shows that the set temperature is necessarily lower than the temperature before the feldspar type flux forms a large amount of glass phase and is at the initial stage of formation of anorthite crystals, and at the time, the anorthite can prevent excessive glass phase from invading pores, so that a plurality of closed pores are formed in a biscuit firing blank, for example, the pore diameter of the closed pores formed in the anorthite substrate ceramic formula system is only 0-70 mu m (see figure 2); meanwhile, a high-viscosity calcium-containing glass phase is easily formed in a formula system, so that the deformation resistance of a sample at high temperature is improved (see figure 4 and table 2), large pores generated by a high-temperature foaming agent are inhibited, the pore diameter of the large pores is controlled within a small range, and the strength and the flatness of a product are ensured. Through the combination of a reasonable formula and a firing system, a comparison experiment shows that: under the same firing system, the pore diameter of pores generated by a high-temperature foaming agent in a conventional ceramic formula system is 200-1000 mu m (see figure 3), the pore diameter of pores generated in an anorthite base ceramic formula system is only 100-250 mu m (see figure 1), and the pore diameter of closed pores in the anorthite base ceramic formula system is controlled by matching a reasonable formula with an optimized firing system, so that the strength and the flatness of a product are ensured.
In conclusion, the invention reasonably designs the formula of the calcium-based substrate porous ceramic and optimizes the sintering system, realizes the shortening of the sintering time, and simultaneously utilizes closed pores generated by two different mechanisms to adjust the internal pore diameter and pore distribution, thereby achieving the product effects of low volume weight and high strength and developing a research scheme for rapidly sintering the light-weight high-strength ceramic at one time.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The porous ceramic is characterized by comprising the following preparation raw materials in percentage by weight: 10-20% of clay, 6-20% of wollastonite, 10-20% of bauxite, 1-5% of talcum, 28-50% of potassium-sodium feldspar water abrasive and 2-7% of aluminum oxide.
2. The porous ceramic according to claim 1, wherein the chemical composition of the porous ceramic contains calcium oxide in an amount of 4.2% by mass or more.
3. The porous ceramic of claim 2, wherein the chemical composition of the porous ceramic is such that the mass percentage ratio of calcium oxide to magnesium oxide is 4.7 or more.
4. The preparation method of the quickly-fired light high-strength ceramic plate is characterized by comprising the following steps of:
(1) weighing the raw materials according to the formula of the porous ceramic;
(2) adding a certain amount of high-temperature foaming agent and dispersing agent into the raw materials of the porous ceramic in the step (1), uniformly mixing, performing wet ball milling to obtain ceramic slurry, and performing spray drying to obtain ceramic powder;
(3) pressing the ceramic powder obtained in the step (2) into a ceramic blank, and then sequentially drying, glazing and firing to obtain the quickly fired light-weight high-strength ceramic plate;
the porous ceramic of step (1) is the porous ceramic according to any one of claims 1 to 3.
5. The method according to claim 4, wherein in the step (2), the weight ratio of the porous ceramic to the high-temperature foaming agent is 85-99.9: 0.1-20, and the amount of the dispersing agent added is 0.7-1.8% of the total weight of the raw materials of the porous ceramic.
6. The method according to claim 5, wherein the high-temperature foaming agent is at least one of carbon black, silicon carbide and polishing slag containing silicon carbide; the dispersant is at least one of water glass and sodium tripolyphosphate.
7. The method according to claim 6, wherein the amount of the carbon black added is 1 to 3% by weight, the amount of the silicon carbide added is 0.1 to 0.4% by weight, and the amount of the polishing slag containing a silicon carbide component is 5 to 15% by weight, based on the total weight of the raw materials of the porous ceramic.
8. The preparation method according to claim 4, wherein in the step (2), the ball milling medium of the wet ball milling is water, and the time of the wet ball milling is 4-6 h; the flow rate of the ceramic slurry is 40-60s, and the residue of the ceramic slurry passing through a 250-mesh sieve is less than 1.0%; the water content of the ceramic powder is 5-8%.
9. The method according to claim 4, wherein in the step (3), the firing temperature is 1150-1200 ℃ and the firing time is 100-120 min.
10. A fast-fired light-weight high-strength ceramic plate, characterized in that it is produced by the method of any one of claims 4 to 8.
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Address after: 528061 1st floor, No.18 taobo Avenue, Huaxia Ceramics Expo City, Nanzhuang Town, Chancheng District, Foshan City, Guangdong Province Patentee after: New Pearl Group Co.,Ltd. Patentee after: New Pearl (Guangdong) New Materials Co.,Ltd. Patentee after: FOSHAN SANSHUI NEW PEARL CONSTRUCTION CERAMICS INDUSTRIAL Co.,Ltd. Patentee after: Jiangxi Xinmingzhu Building Materials Co.,Ltd. Patentee after: Hubei new Ming Zhu Green Building Materials Technology Co.,Ltd. Address before: 528061 1st floor, No.18 taobo Avenue, Huaxia Ceramics Expo City, Nanzhuang Town, Chancheng District, Foshan City, Guangdong Province Patentee before: New Pearl Group Co.,Ltd. Patentee before: GUANGDONG SUMMIT CERAMICS Co.,Ltd. Patentee before: FOSHAN SANSHUI NEW PEARL CONSTRUCTION CERAMICS INDUSTRIAL Co.,Ltd. Patentee before: Jiangxi Xinmingzhu Building Materials Co.,Ltd. Patentee before: Hubei new Ming Zhu Green Building Materials Technology Co.,Ltd. |