CN113213905A - Cordierite-based microcrystalline glass combined Al2O3-SiO2System ceramic material and preparation method thereof - Google Patents
Cordierite-based microcrystalline glass combined Al2O3-SiO2System ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses cordierite-based microcrystalline glass combined Al2O3‑SiO2The system ceramic material comprises a base material and a bonding agent, wherein the base material comprises 5-30 wt% of cordierite-based microcrystalline glass powder, 10-60 wt% of mullite aggregate, 10-60 wt% of corundum aggregate and 0-30 wt% of quartz aggregate; the cordierite-based microcrystalline glass powder comprises 15-22 wt% of MgO, 320-25 wt% of Al2O and 256-60 wt% of SiO; the dosage of the binder is 8-12 wt% of the base material. In addition, the cordierite-based microcrystalline glass combined with Al is also disclosed2O3‑SiO2A method for preparing a systematic ceramic material. The invention takes cordierite-based microcrystalline glass as a sintering aid, and Al is added2O3‑SiO2Cordierite crystals are added in an in-situ synthesis mode in a ceramic matrix of the system, so that a low-temperature sintering aid is providedAnd effectively improve Al2O3‑SiO2Property of systematic ceramic material for improving Al2O3‑SiO2The quality of the system ceramic material and the saving of the product cost have important significance, and the popularization and the application as well as the progress and the development of the industrial technology are facilitated.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to cordierite-based microcrystalline glass combined Al2O3-SiO2Systematic ceramic materials and methods of making the same.
Background
Al2O3-SiO2The ceramic material is ceramic (corundum, mullite, corundum-mullite ceramic and the like) and has excellent refractoriness, mechanical property and chemical stability, so that the ceramic material is widely applied to the fields of refractory materials, aerospace, environmental protection, energy sources and the like. Along with the scientific and technological worker to Al2O3-SiO2The recognition of the excellent performance of the ceramic is deepened, and the application range of the ceramic is further expanded. However, high thermal expansion coefficients and high sintering temperatures (> 1600 ℃) have been limiting Al2O3-SiO2Is a key problem in the development of high-temperature structural ceramics. This is because high thermal expansion is the main cause of thermal shock damage to the material, and high sintering temperatures increase the manufacturing difficulty and cost of the product.
The cordierite has the advantages of small thermal expansion coefficient, small dielectric loss, good thermal shock resistance and the like, and the advantages can exactly compensate for Al2O3-SiO2The disadvantage of ceramic. Introduction of cordierite into Al2O3-SiO2The ceramic not only can improve the thermal shock resistance of the material by utilizing a complex phase ceramic thermal mismatch mechanism, but also can improve the heat-resisting temperature of cordierite. However, the sintering effect of directly adding cordierite is not good, and it is difficult to solve Al well2O3-SiO2The ceramic is difficult to sinter, and has high thermal expansion coefficient. Therefore, how to effectively bond cordierite is effective for increasing Al2O3-SiO2The quality of the system ceramic material and the saving of the product cost are of great significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide cordierite-based microcrystalline glass combined with Al2O3-SiO2System ceramic material, uses cordierite-base glass ceramics as Al2O3-SiO2Sintering aids for system ceramics to pass throughCordierite is introduced in a position synthesis mode, so that Al with high density and excellent thermal shock resistance is obtained2O3-SiO2And (3) system ceramics. Another object of the present invention is to provide the above cordierite-based glass-ceramic in combination with Al2O3-SiO2A method for preparing a systematic ceramic material.
The purpose of the invention is realized by the following technical scheme:
the invention provides cordierite-based microcrystalline glass combined with Al2O3-SiO2The system ceramic material comprises a base material and a bonding agent, wherein the base material comprises 5-30 wt% of cordierite-based microcrystalline glass powder, 10-60 wt% of mullite aggregate, 10-60 wt% of corundum aggregate and 0-30 wt% of quartz aggregate; the cordierite-based microcrystalline glass powder comprises 15-22 wt% of MgO and Al2O320～25wt％，SiO256-60 wt%; the dosage of the binder is 8-12 wt% of the base material.
Furthermore, the particle size of the cordierite-based microcrystalline glass powder is 10-75 μm, the particle size of the mullite aggregate is 30-325 meshes, the particle size of the corundum aggregate is 30-500 meshes, and the particle size of the quartz aggregate is 100-325 meshes.
In the scheme, the binding agent is a PVA solution with the concentration of 5 wt%.
The other purpose of the invention is realized by the following technical scheme:
the cordierite-based microcrystalline glass provided by the invention is combined with Al2O3-SiO2The preparation method of the system ceramic material comprises the following steps:
(1) mixing the cordierite-based microcrystalline glass powder according to the composition ratio, placing the mixture in an electric furnace to be melted into glass liquid, pouring the glass liquid into water to be quenched to obtain glass blocks, and carrying out ball milling to obtain the cordierite-based microcrystalline glass powder;
(2) mixing the base materials according to a ratio, adding a binding agent, uniformly mixing, and then performing compression molding and drying to obtain a green body;
(3) the green body is sintered in a multi-stage mode, namely at 800-900 DEG CPreserving heat for 2-3 h at 1450-1500 ℃ for 2-3 h, then cooling to 1100-1200 ℃ for 1-3 h, and naturally cooling to room temperature to obtain the cordierite-based microcrystalline glass combined with Al2O3-SiO2Systematic ceramic materials.
Further, in the preparation method, in the step (1), the melting temperature is 1500-1600 ℃, and the melting time is 2-3 h. The moisture content of the green compact dried in the step (2) is less than 1%.
The invention has the following beneficial effects:
(1) the invention adopts cordierite-based microcrystalline glass which is easy to form liquid phase as Al2O3-SiO2The sintering aid of the system ceramic utilizes the characteristic that glass is easy to generate liquid phase, is beneficial to removing pores in the ceramic, enables aggregates such as corundum and mullite to easily achieve the effect of particle rearrangement under the action of the liquid phase, and realizes the reduction of Al2O3-SiO2The purpose of the sintering temperature of the system ceramic is to greatly reduce Al2O3-SiO2Sintering temperature of system ceramic.
(2) The invention mainly solves the problem of poor sintering performance of low-expansion cordierite. Generally, cordierite has a narrow sintering temperature range and is not satisfactory in sintering effect. The cordierite-based microcrystalline glass has the advantages of excellent sintering performance and low expansibility, and can just compensate for Al2O3-SiO2The ceramic is difficult to sinter, and has high thermal expansion coefficient. The cordierite-based glass ceramics is used as sintering aid, so that the problem of poor sintering performance of cordierite can be effectively solved, and the thermal expansion coefficient of the ceramic can be reduced (to 4-5 x 10-6℃-1) (ii) a The thermal expansion coefficient of the composite ceramic can be controlled by controlling the content of cordierite crystals in the glass, so that the purpose of improving the thermal shock resistance (no cracking after 30 times of thermal shock at room temperature to 1100 ℃) is achieved.
(3) The invention utilizes cordierite-based microcrystalline glass and Al2O3-SiO2Good chemical compatibility between system ceramics, on one hand, the glass can easily wet coarse particles and strengthen particlesThe bonding between the glass particles and the particles effectively improves the product strength (the compressive strength is improved to 250-300 MPa), and on the other hand, the bonding between the glass and the particles is enhanced.
(4) The invention has simple process and low firing temperature, and can improve Al content2O3-SiO2The quality of the system ceramic material and the saving of the product cost have important significance, so the system ceramic material has wide market prospect and is beneficial to popularization and application and the progress and development of industrial technology.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 shows cordierite-based glass-ceramic bonded Al prepared in accordance with an example of the present invention2O3-SiO2Sectional microscopic structure of system ceramics (scanning electron microscope secondary electron image).
Detailed Description
The first embodiment is as follows:
1. this example is a cordierite-based glass-ceramic bonded Al2O3-SiO2The system ceramic material comprises a base material and a bonding agent, wherein the base material comprises 30 wt% of cordierite-based microcrystalline glass powder (with the granularity of 75 mu m), 60 wt% of mullite aggregate (wherein, 30 wt% of the granularity of 30 meshes, 10 wt% of the granularity of 80 meshes, 20 wt% of the granularity of 325 meshes) and 10 wt% of corundum aggregate (with the granularity of 120 meshes). Wherein the cordierite-based microcrystalline glass powder comprises 17 wt% of MgO and Al2O323 wt％、SiO260 wt%. The binder is a PVA solution with a concentration of 5 wt%, and the dosage of the PVA solution is 8 wt% of the base material.
2. The cordierite-based glass ceramic of the present embodiment is combined with Al2O3-SiO2The preparation method of the system ceramic material comprises the following steps:
(1) mixing the cordierite-based microcrystalline glass powder according to the composition proportion, placing the mixture in an electric furnace, preserving heat for 2 hours at the temperature of 1600 ℃, melting the mixture into glass liquid, pouring the glass liquid into water, quenching the glass liquid to obtain glass blocks, and carrying out ball milling to obtain the cordierite-based microcrystalline glass powder;
(2) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, then performing compression molding, and drying at a temperature of 110 ℃ to obtain a green body (the moisture in the kiln is less than 1%);
(3) the green body is sintered in a multi-stage mode, namely the green body is subjected to heat preservation at 850 ℃ for 2h, at 1450 ℃ for 2h, then is cooled to 1100 ℃ for heat preservation for 1h, and then is naturally cooled to the room temperature, so that the cordierite-based microcrystalline glass combined with Al is prepared2O3-SiO2Systematic ceramic materials.
Example two:
1. this example is a cordierite-based glass-ceramic bonded Al2O3-SiO2The system ceramic material comprises a base material and a bonding agent, wherein the base material comprises 20 wt% of cordierite-based microcrystalline glass powder (with the granularity of 35 mu m), 10 wt% of mullite aggregate (with the granularity of 50 meshes), 60 wt% of corundum aggregate (with the granularity of 40 wt% with 30 meshes, 10 wt% with 200 meshes and 10 wt% with 325 meshes), and 10 wt% of quartz aggregate (with the granularity of 325 meshes). Wherein the cordierite-based microcrystalline glass powder comprises 15 wt% of MgO and Al2O325 wt％、SiO260 wt%. The binder is a PVA solution with a concentration of 5 wt%, and the dosage of the PVA solution is 12 wt% of the base material.
2. The cordierite-based glass ceramic of the present embodiment is combined with Al2O3-SiO2The preparation method of the system ceramic material comprises the following steps:
(1) mixing the cordierite-based microcrystalline glass powder according to the composition proportion, placing the mixture in an electric furnace, preserving heat for 3 hours at the temperature of 1600 ℃, melting the mixture into glass liquid, pouring the glass liquid into water, quenching the glass liquid to obtain glass blocks, and carrying out ball milling to obtain the cordierite-based microcrystalline glass powder;
(2) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, then performing compression molding, and drying at a temperature of 110 ℃ to obtain a green body (the moisture in the kiln is less than 1%);
(3) the green body is sintered in a multi-stage way, namely, the green body is insulated for 3h at 900 ℃, insulated for 2h at 1500 ℃, cooled to 1200 ℃ and insulated for 3h, and then naturally cooled to room temperature, thus obtaining the cordierite-based microcrystalline glass combined with Al2O3-SiO2Systematic ceramic materials.
Example three:
1. this example is a cordierite-based glass-ceramic bonded Al2O3-SiO2The system ceramic material comprises a base material and a bonding agent, wherein the base material comprises 5 wt% of cordierite-based microcrystalline glass powder (with the granularity of 10 mu m), 10 wt% of mullite aggregate (with the granularity of 60 meshes), 60 wt% of corundum aggregate (with the granularity of 30 meshes and 30 wt% of 500 meshes), and 25 wt% of quartz aggregate (with the granularity of 120 meshes and 10 wt% of 325 meshes). Wherein the cordierite-based microcrystalline glass powder comprises 19 wt% of MgO and Al2O325 wt％、SiO256 wt%. The binder is a PVA solution with a concentration of 5 wt%, and the dosage of the PVA solution is 10 wt% of the base material.
2. The cordierite-based glass ceramic of the present embodiment is combined with Al2O3-SiO2The preparation method of the system ceramic material comprises the following steps:
(1) mixing the cordierite-based microcrystalline glass powder according to the composition proportion, placing the mixture in an electric furnace, preserving heat for 3 hours at the temperature of 1550 ℃ to prepare glass liquid, pouring the glass liquid into water to quench the glass liquid to obtain glass blocks, and carrying out ball milling to obtain the cordierite-based microcrystalline glass powder;
(2) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, then performing compression molding, and drying at a temperature of 110 ℃ to obtain a green body (the moisture in the kiln is less than 1%);
(3) the green body is sintered in a multi-stage mode, namely, the green body is subjected to heat preservation at 850 ℃ for 2h, 1500 ℃ for 2h, then is cooled to 1150 ℃ for 2h, and then is naturally cooled to room temperature, so that the cordierite-based microcrystalline glass combined Al is obtained2O3-SiO2Systematic ceramic materials.
Example four:
1. this example is a cordierite-based glass-ceramic bonded Al2O3-SiO2The system ceramic material comprises a base material and a bonding agent, wherein the base material comprises 10 wt% of cordierite-based microcrystalline glass powder (with the granularity of 20 mu m), 50 wt% of mullite aggregate (30 wt% of 30 meshes and 20 wt% of 100 meshes), 10 wt% of corundum aggregate (100 meshes), 30 wt% of quartz aggregate (10 wt% of 200 meshes and 20 wt% of 325 meshes)%). Wherein the cordierite-based microcrystalline glass powder comprises 22 wt% of MgO and Al2O320 wt％、SiO258 wt%. The binder is a PVA solution with a concentration of 5 wt%, and the dosage of the PVA solution is 8 wt% of the base material.
2. The cordierite-based glass ceramic of the present embodiment is combined with Al2O3-SiO2The preparation method of the system ceramic material comprises the following steps:
(1) mixing the cordierite-based microcrystalline glass powder according to the composition proportion, placing the mixture in an electric furnace, preserving heat for 3 hours at 1500 ℃, melting the mixture into glass liquid, pouring the glass liquid into water, quenching the glass liquid to obtain glass blocks, and carrying out ball milling to obtain the cordierite-based microcrystalline glass powder;
(2) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, then performing compression molding, and drying at a temperature of 110 ℃ to obtain a green body (the moisture in the kiln is less than 1%);
(3) the green body is sintered in a multi-stage way, namely, the green body is insulated at 800 ℃ for 2h, at 1500 ℃ for 3h, then is cooled to 1100 ℃ for 2h, and then is naturally cooled to room temperature, thus obtaining the cordierite-based microcrystalline glass combined with Al2O3-SiO2Systematic ceramic materials.
As shown in FIG. 1, cordierite-based glass-ceramic obtained in accordance with an example of the present invention was combined with Al2O3-SiO2The system ceramic material, cordierite-based microcrystalline glass, comprises mullite and corundum aggregate, and can play a role in reducing the thermal expansion coefficient and improving the thermal shock resistance.
Claims (6)
1. Cordierite-based microcrystalline glass combined Al2O3-SiO2The system ceramic material is characterized in that: the material comprises a base material and a bonding agent, wherein the base material comprises 5-30 wt% of cordierite-based microcrystalline glass powder, 10-60 wt% of mullite aggregate, 10-60 wt% of corundum aggregate and 0-30 wt% of quartz aggregate; the cordierite-based microcrystalline glass powder comprises 15-22 wt% of MgO and Al2O320～25wt％，SiO256-60 wt%; the dosage of the binder is 8-12 wt% of the base material.
2. The cordierite-based microcrystalline glass bonded Al of claim 12O3-SiO2The system ceramic material is characterized in that: the particle size of the cordierite-based microcrystalline glass powder is 10-75 mu m, the particle size of the mullite aggregate is 30-325 meshes, the particle size of the corundum aggregate is 30-500 meshes, and the particle size of the quartz aggregate is 100-325 meshes.
3. The cordierite-based microcrystalline glass bonded Al of claim 12O3-SiO2The system ceramic material is characterized in that: the binding agent is PVA solution with the concentration of 5 wt%.
4. The cordierite-based glass-ceramic bonded Al of any one of claims 1 to 32O3-SiO2The preparation method of the system ceramic material is characterized by comprising the following steps:
(1) mixing the cordierite-based microcrystalline glass powder according to the composition ratio, placing the mixture in an electric furnace to be melted into glass liquid, pouring the glass liquid into water to be quenched to obtain glass blocks, and carrying out ball milling to obtain the cordierite-based microcrystalline glass powder;
(2) mixing the base materials according to a ratio, adding a binding agent, uniformly mixing, and then performing compression molding and drying to obtain a green body;
(3) the green body is subjected to multi-stage sintering, namely, the green body is subjected to heat preservation for 2-3 h at 800-900 ℃, for 2-3 h at 1450-1500 ℃, then is cooled to 1100-1200 ℃ and is subjected to heat preservation for 1-3 h, and then is naturally cooled to room temperature, so that the cordierite-based microcrystalline glass combined with Al is prepared2O3-SiO2Systematic ceramic materials.
5. The cordierite-based microcrystalline glass bonded Al of claim 42O3-SiO2The preparation method of the system ceramic material is characterized by comprising the following steps: in the step (1), the melting temperature is 1500-1600 ℃, and the melting time is 2-3 h.
6. According to claimRequirement 4 the cordierite-based glass-ceramic described in conjunction with Al2O3-SiO2The preparation method of the system ceramic material is characterized by comprising the following steps: the moisture content of the green compact dried in the step (2) is less than 1%.
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| CN113336479A (en) * | 2021-05-21 | 2021-09-03 | 景德镇陶瓷大学 | Cordierite-based microcrystalline glass high-temperature binder and preparation method and application thereof |
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| US20180037493A1 (en) * | 2016-07-08 | 2018-02-08 | Schott Ag | Cordierite Glass-Ceramic |
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