CN114031297A - Cordierite-based porous glass ceramic and preparation method thereof - Google Patents
Cordierite-based porous glass ceramic and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The application provides a cordierite-based porous glass ceramic and a preparation method thereof, wherein the method comprises the following steps: mixing magnesium oxide, aluminum oxide, silicon dioxide and boron oxide raw materials, and then sequentially carrying out high-temperature melting, water quenching, crushing and screening to obtain glass powder; and (3) after the glass powder is subjected to pressure molding, sintering at high temperature to obtain the cordierite-based porous glass ceramic. The preparation method of the application prepares and obtains the cordierite-based porous glass ceramic at lower sintering temperature without sintering aids. The cordierite-based porous glass ceramic has the advantages of small thermal expansion coefficient, high open porosity, low volume density and high bending strength. In addition, the method also has the advantages of low dielectric constant and low dielectric loss.
Description
Technical Field
The application relates to the technical field of porous glass ceramics, in particular to cordierite-based porous glass ceramics and a preparation method thereof.
Background
The cordierite porous ceramic has the advantages of low density, low thermal expansion, high temperature resistance, corrosion resistance, good heat insulation and permeability and excellent dielectric property, and can be applied to various fields, such as filter materials, heat insulation materials, catalyst carrier materials, wave-transmitting materials and the like. Therefore, cordierite porous ceramic materials have been the material of interest and focus of research.
For ceramic materials, the manufacturing process typically requires higher sintering temperatures, and similar problems exist for cordierite porous ceramics as well. In many studies, in order to reduce the preparation temperature of the ceramic material, the ceramic material may be prepared by a sol-gel method, or the sintering temperature may be reduced by adding a sintering aid to the ceramic material in the sintering process. However, the sol-gel method is complicated in process, high in cost and liable to pollute the environment, and the addition of the sintering aid has a disadvantage in that the sintering aid may impair the thermal expansion or dielectric properties of the material.
Disclosure of Invention
The purpose of the application is to provide a cordierite-based porous glass ceramic and a preparation method thereof, so that the cordierite-based porous glass ceramic is prepared under the conditions of no addition of a sintering aid and low sintering temperature. The specific technical scheme is as follows:
a first aspect of the present application provides a method for producing a cordierite-based porous glass ceramic, comprising the steps of:
mixing raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide, and forming a mixed ingredient after uniformly mixing;
sequentially carrying out high-temperature melting, water quenching, crushing and screening on the mixed ingredients to obtain glass powder;
carrying out pressure molding on the glass powder to obtain a blank body;
and sintering the green body at high temperature to obtain the cordierite-based porous glass ceramic.
In one embodiment of the present application, the content of each oxide in the mixed batch is, based on the total mass of the mixed batch: MgO: 18-24 wt% of Al2O3:16-24wt%、SiO2:47-55wt%、B2O3:4-14wt%。
In one embodiment of the present application, the purity of the magnesia, alumina, silica, and boria feedstock is 98% to 100%.
In one embodiment of the present application, the melting temperature of the high-temperature melting is 1400-1600 ℃, and the melting time is 2-3 h.
In one embodiment of the present application, the glass powder has an average particle diameter of 50 to 80 μm.
In one embodiment of the present application, the pressure forming has a forming pressure of 20 to 40 MPa.
In one embodiment of the present application, the high temperature sintering comprises holding at 950-; then the temperature is kept for 2-3h at 1015-1040 ℃.
A second aspect of the present application provides a cordierite-based porous glass-ceramic prepared by the method of any one of the embodiments of the first aspect of the present application.
In an embodiment of the present applicationIn the embodiment, the cordierite-based porous glass ceramic has the porosity of 40-65%; the bulk density is 1.00-1.60g/cm3(ii) a Coefficient of thermal expansion of 4.20X 10-6-5.00×10-6K-1(ii) a The bending strength is 12.0-45.0 MPa.
In one embodiment of the present application, the cordierite-based porous glass-ceramic has a dielectric constant of 2 to 3.5 and a dielectric loss of 2.0X 10 at a measuring frequency of 21 to 38GHz-3-4.0×10-3。
The beneficial effect of this application includes:
according to the method for preparing the cordierite-based porous glass ceramic, the cordierite-based porous glass ceramic can be prepared at a lower sintering temperature under the condition of not adding a sintering aid. The cordierite-based porous glass-ceramic of the second aspect of the present application has uniform pores and a narrow pore size distribution. Further, the cordierite-based porous glass ceramic of the second aspect of the present application has advantages of a small thermal expansion coefficient, a high open porosity, a low volume density, and a high bending strength. In addition, the method also has the advantages of low dielectric constant and low dielectric loss.
Of course, not all advantages described above need to be achieved at the same time in the practice of any one product or method of the present application.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only one embodiment of the present application, and it is obvious for those skilled in the art to obtain other embodiments according to the drawings.
FIG. 1 is an X-ray powder diffraction pattern of a cordierite-based porous glass ceramic of example 1.
FIG. 2 is a scanning electron micrograph of the cordierite-based porous glass-ceramic microstructure of example 1.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the description herein are intended to be within the scope of the present disclosure.
A first aspect of the present application provides a method for producing a cordierite-based porous glass ceramic, comprising the steps of:
mixing raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide, and forming a mixed ingredient after uniformly mixing;
sequentially carrying out high-temperature melting, water quenching, crushing and screening on the mixed ingredients to obtain glass powder;
carrying out pressure molding on the glass powder to obtain a blank body;
and sintering the green body at high temperature to obtain the cordierite-based porous glass ceramic.
In one embodiment of the present application, the content of each oxide in the mixed batch is, based on the total mass of the mixed batch: MgO: 18-24 wt% of Al2O3:16-24wt%、SiO2:47-55wt%、B2O3:4-14wt%。
In one embodiment of the present application, the purity of the magnesia, alumina, silica, and boria feedstock is 98% to 100%.
In the present application, the manner of the above-described mixing to form the mixed ingredients is not particularly limited as long as the object of the present application is achieved. For example, a mixing device such as a mixer or a ball mill is used.
In one embodiment of the present application, the melting temperature of the high-temperature melting is 1400-1600 ℃, and the melting time is 1-2 h.
In the present application, the high-temperature melting apparatus is not particularly limited as long as the purpose of the present application is achieved, and may be, for example, a box-type high-temperature furnace or other high-temperature furnaces known to those skilled in the art.
In one embodiment of the present application, the glass powder has an average particle diameter of 50 to 80 μm.
In one embodiment of the present application, the pressure forming has a forming pressure of 20 to 40 MPa.
In the present application, the manner of the press molding is not particularly limited as long as the object of the present application is achieved, and examples thereof include one-way press molding, two-way press molding, and isostatic press molding.
In one embodiment of the present application, the high temperature sintering comprises holding at 950-; then the temperature is kept for 2-3h at 1015-1040 ℃.
In the present application, the high-temperature sintering apparatus is not particularly limited, and may be, for example, a muffle furnace or other high-temperature furnaces known to those skilled in the art.
The inventor finds that the cordierite-based porous glass ceramic can be prepared at a lower sintering temperature without adding a sintering aid by the method for preparing the cordierite-based porous glass ceramic. According to the preparation method, the process for preparing the glass ceramic by sintering the glass powder at the high temperature is adopted, and the crystallization rate in the high-temperature sintering process is controlled by controlling the granularity, the composition, the forming and the high-temperature sintering process of the glass powder, so that the crystal phase structure, the pore distribution of the porous structure, the open porosity, the thermal expansion coefficient, the volume density, the bending strength and the dielectric property of the obtained cordierite-based porous glass ceramic are controlled.
A second aspect of the present application provides a cordierite-based porous glass-ceramic prepared by the method of any one of the embodiments of the first aspect of the present application.
In one embodiment of the present application, the cordierite-based porous glass-ceramic has a porosity of 40% to 65%; the bulk density is 1.00-1.60g/cm3(ii) a Coefficient of thermal expansion of 4.20X 10-6-5.00×10-6K-1(ii) a The bending strength is 12.0-45.0 MPa.
In one embodiment of the present application, the cordierite-based porous glass-ceramic has a dielectric constant of 2 to 3.5 and a dielectric loss of 2.0X 10 at a measuring frequency of 21 to 38GHz-3-4.0×10-3。
The cordierite-based porous glass ceramic has the advantages of small thermal expansion coefficient, high open porosity, low volume density and high bending strength. In addition, the method also has the advantages of low dielectric constant, small dielectric loss and the like.
Examples
Hereinafter, the present application will be explained in more detail by examples. Various tests and evaluations were carried out according to the following methods.
The test method and the test equipment are as follows:
the open porosity and the bulk density of the cordierite-based porous glass ceramic obtained in the examples of the present application were measured by the "water boiling method" (astm c373) established by the american society for testing and materials standards; measuring the thermal expansion coefficient of the obtained cordierite-based porous glass ceramic by using a thermal expansion meter; measuring the bending strength of the obtained cordierite-based porous glass ceramic on an electronic universal material testing machine by adopting a three-point bending method; the dielectric constant and the dielectric loss of the obtained cordierite-based porous glass ceramic were measured on an Agilent PNA-L series network vector analyzer at a measurement frequency of 21 to 38 GHz.
Example 1
Putting raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide into a mixing tank for mixing, and forming a mixed ingredient after uniformly mixing; wherein, the purities of the raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide are all 99.5%; the content of each oxide in the mixed ingredients is as follows: MgO: 19.0 wt% of Al2O3:23.8wt%、SiO2:52.4wt%、B2O3:4.8wt%;
Placing the obtained mixed ingredients into a crucible, heating the mixed ingredients to 1500 ℃ in a box-type high-temperature furnace for high-temperature melting, keeping the temperature for 2 hours, taking out the glass melt, and performing water quenching to obtain glass slag; drying and simply crushing the glass slag, then placing the glass slag into an agate grinder, grinding the glass slag for 2 hours, and then sieving the glass slag by a 200-mesh sieve to obtain glass powder; wherein the average grain diameter of the obtained glass powder is 75 μm;
putting the obtained glass powder into a steel grinding tool, and carrying out pressure forming on the steel grinding tool on a press machine to obtain a blank body; wherein the molding pressure is 20MPa, and the pressure maintaining time is 10 min;
and placing the obtained blank body in a muffle furnace for high-temperature sintering, heating to 950 ℃ from room temperature at the heating rate of 5 ℃/min, preserving heat for 1h, then heating to 1015 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, and finally naturally cooling to room temperature to obtain the cordierite-based porous glass ceramic.
FIG. 1 shows an XRD pattern of a cordierite-based porous glass ceramic of example 1.
As can be seen from fig. 1, the cordierite-based porous glass-ceramic of example 1 has a primary crystal phase of cordierite phase and a secondary crystal phase of α -quartz phase.
FIG. 2 shows a scanning electron micrograph of the microstructure of the cordierite-based porous glass-ceramic of example 1.
As can be seen from FIG. 2, the cordierite-based porous glass ceramic of example 1 has a porous structure with uniform pores and a pore size distribution of 5 to 20 μm.
Example 2
Putting raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide into a mixing tank for mixing, and forming a mixed ingredient after uniformly mixing; wherein, the purities of the raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide are all 99.5%; the content of each oxide in the mixed ingredients is as follows: MgO: 20.9 wt% of Al2O3:16.4wt%、SiO2:53.6wt%、B2O3:9.1wt%;
Placing the obtained mixed ingredients into a crucible, heating the mixed ingredients to 1500 ℃ in a box-type high-temperature furnace for high-temperature melting, keeping the temperature for 2 hours, taking out the glass melt, and performing water quenching to obtain glass slag; drying and simply crushing the glass slag, then placing the glass slag into an agate grinder, grinding the glass slag for 2 hours, and then sieving the glass slag by a 200-mesh sieve to obtain glass powder; wherein the average grain diameter of the obtained glass powder is 75 μm;
putting the obtained glass powder into a steel grinding tool, and carrying out pressure forming on the steel grinding tool on a press machine to obtain a blank body; wherein the molding pressure is 30MPa, and the pressure maintaining time is 10 min;
and placing the obtained blank body in a muffle furnace for high-temperature sintering, heating to 970 ℃ from room temperature at the heating rate of 5 ℃/min, preserving heat for 1h, then heating to 1030 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, and finally naturally cooling to room temperature to obtain the cordierite-based porous glass ceramic.
Example 3
Putting raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide into a mixing tank for mixing, and forming a mixed ingredient after uniformly mixing; wherein, the purities of the magnesium oxide, the aluminum oxide, the silicon dioxide and the boron oxide are all 99.5 percent; the content of each oxide in the mixed ingredients is as follows: MgO: 18.2 wt% of Al2O3:18.2wt%、SiO2:54.5wt%、B2O3:9.1wt%;
Placing the obtained mixed ingredients into a crucible, heating the mixed ingredients to 1500 ℃ in a box-type high-temperature furnace for high-temperature melting, keeping the temperature for 2 hours, taking out the glass melt, and performing water quenching to obtain glass slag; drying and simply crushing the glass slag, then placing the glass slag into an agate grinder, grinding the glass slag for 2 hours, and then sieving the glass slag by a 200-mesh sieve to obtain glass powder; wherein the average grain diameter of the obtained glass powder is 75 μm;
putting the obtained glass powder into a steel grinding tool, and carrying out pressure forming on the steel grinding tool on a press machine to obtain a blank body; wherein the molding pressure is 40MPa, and the pressure maintaining time is 10 min;
and (3) placing the obtained blank body in a muffle furnace for high-temperature sintering, heating to 975 ℃ from room temperature at the heating rate of 5 ℃/min, preserving heat for 1h, then heating to 1035 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, and finally naturally cooling to room temperature to obtain the cordierite-based porous glass ceramic.
Example 4
Putting raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide into a mixing tank for mixing, and forming a mixed ingredient after uniformly mixing; wherein, the purities of the raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide are all 99.5%; the content of each oxide in the mixed ingredients is as follows: MgO: 21.7 wt% of Al2O3:21.7wt%、SiO2:43.5wt%、B2O3:13.1wt%;
Placing the obtained mixed ingredients into a crucible, heating the mixed ingredients to 1500 ℃ in a box-type high-temperature furnace for high-temperature melting, keeping the temperature for 2 hours, taking out the glass melt, and performing water quenching to obtain glass slag; drying and simply crushing the glass slag, then placing the glass slag into an agate grinder, grinding the glass slag for 2 hours, and then sieving the glass slag by a 200-mesh sieve to obtain glass powder; wherein the average grain diameter of the obtained glass powder is 75 μm;
putting the obtained glass powder into a steel grinding tool, and carrying out pressure forming on the steel grinding tool on a press machine to obtain a blank body; wherein the molding pressure is 40MPa, and the pressure maintaining time is 10 min;
and placing the obtained blank body in a muffle furnace for high-temperature sintering, heating to 980 ℃ from room temperature at the heating rate of 5 ℃/min, preserving heat for 1h, then heating to 1040 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, and finally naturally cooling to room temperature to obtain the cordierite-based porous glass ceramic.
Table 1 shows the open porosity, bulk density, thermal expansion coefficient, bending strength, and dielectric constant and dielectric loss of the cordierite-based porous glass ceramics obtained in examples 1 to 4.
As can be seen from examples 1 to 4, with the production method of the present application, cordierite-based porous glass ceramics can be obtained at a lower sintering temperature without a sintering aid. As shown in Table 1, the cordierite-based porous glass ceramic of the present application has an open porosity of 40% to 65%; the bulk density is 1.00-1.60g/cm3(ii) a Coefficient of thermal expansion of 4.20X 10-6-5.00×10-6K-1(ii) a The bending strength is 12.0-45.0 Mpa; the cordierite-based porous glass-ceramic of the present application has a dielectric constant of 2 to 3.5 and a dielectric loss of 2.0X 10 at a measurement frequency of 21 to 38GHz-3-4.0×10-3。
TABLE 1
The above description is only for the preferred embodiment of the present application and is not intended to limit the scope of the present application. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application are included in the protection scope of the present application.
Claims (10)
1. A method for preparing cordierite-based porous glass ceramic is characterized by comprising the following steps:
mixing raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide, and forming a mixed ingredient after uniformly mixing;
sequentially carrying out high-temperature melting, water quenching, crushing and screening on the mixed ingredients to obtain glass powder;
carrying out pressure molding on the glass powder to obtain a blank body;
and sintering the green body at high temperature to obtain the cordierite-based porous glass ceramic.
2. The preparation method according to claim 1, wherein the content of each oxide in the mixed ingredients is, based on the total mass of the mixed ingredients: MgO: 18-24 wt% of Al2O3:16-24wt%、SiO2:47-55wt%、B2O3:4-14wt%。
3. The method of claim 1, wherein the purity of the raw materials of magnesium oxide, aluminum oxide, silicon dioxide and boron oxide is 98% -100%.
4. The method as claimed in claim 1, wherein the melting temperature of the high-temperature melting is 1400 ℃ to 1600 ℃ and the melting time is 2-3 h.
5. The production method according to claim 1, wherein the average particle diameter of the glass powder is 50 to 80 μm.
6. The production method according to claim 1, wherein the pressure molding is performed at a molding pressure of 20 to 40 MPa.
7. The method as claimed in claim 1, wherein the high-temperature sintering comprises maintaining at 950-; then the temperature is kept for 2-3h at 1015-1040 ℃.
8. Cordierite-based porous glass-ceramics prepared according to the method of any one of claims 1-7.
9. The cordierite-based porous glass-ceramic of claim 8, wherein the cordierite-based porous glass-ceramic has a porosity of 40% to 65%; the bulk density is 1.00-1.60g/cm3(ii) a Coefficient of thermal expansion of 4.20X 10-6-5.00×10-6K-1(ii) a The bending strength is 12.0-45.0 MPa.
10. The cordierite-based porous glass-ceramic according to claim 8, wherein the cordierite-based porous glass-ceramic has a dielectric constant of 2 to 3.5 and a dielectric loss of 2.0 x 10 at a measuring frequency of 21 to 38GHz-3-4.0×10-3。
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CN114634372A (en) * | 2022-03-25 | 2022-06-17 | 山东国瓷功能材料股份有限公司 | Porous ceramic material for atomizing core, porous ceramic body, ceramic atomizing core, preparation method and electronic cigarette |
CN115650700A (en) * | 2022-10-26 | 2023-01-31 | 航天材料及工艺研究所 | High-temperature-resistant light wave-transparent porous Al 5 BO 9 Ceramic material and preparation method thereof |
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