CN113336563B - Sialon whisker-corundum composite ceramic material using natural mineral as raw material, preparation method thereof and prepared product - Google Patents
Sialon whisker-corundum composite ceramic material using natural mineral as raw material, preparation method thereof and prepared product Download PDFInfo
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Abstract
The invention discloses a sialon whisker-corundum composite ceramic material taking natural minerals as raw materials, which comprises a base material and a bonding agent; the base material comprises 60-80 wt% of aluminosilicate mineral, 10-30 wt% of metal aluminum powder, 5-20 wt% of metal silicon powder and 1-3 wt% of aluminum fluoride; the dosage of the binder is 6-12 wt% of the base material. In addition, the preparation method of the sialon whisker-corundum composite ceramic material using natural minerals as raw materials and the prepared product are also disclosed. The invention adopts natural aluminosilicate mineral-metal aluminum powder-metal silicon powder-aluminum fluoride as a raw material system, introduces the sialon crystal whisker and corundum in an in-situ synthesis mode, not only saves the raw material cost and simplifies the preparation process, but also effectively solves the problem that industrial powder and aggregate are not easy to mix uniformly in the prior art, and improves the performance of the corundum-based composite ceramic material. The method has important significance for improving the quality of the corundum-based composite ceramic material and saving the product cost, and is beneficial to popularization and application and the progress and development of industrial technology.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a sialon whisker-corundum composite ceramic material, a preparation method thereof and a prepared product.
Background
The corundum ceramics has the characteristics of high-temperature strength, good chemical stability, high refractoriness and the like, and can be used as a crucible, a ceramic roller way and other high-temperature applications. However, corundum ceramics have poor resistance to rapid cooling and quenching due to their high thermal expansion coefficient, and also have poor toughness of sintered bodies, thereby limiting the range of applications. The sialon whisker has the advantages of higher thermal conductivity, low expansion, high thermal shock resistance and the like, and can just make up for the defects in the aspect of corundum ceramic performance, so that the sialon whisker-corundum composite ceramic material is a complex phase ceramic material integrating the advantages of the sialon whisker and the corundum ceramic material.
However, no sialon whisker product is available on the market at present. Even though the sialon whisker appears as a commercial product, the problem that the whisker material is difficult to mix uniformly is solved. The most possible method for solving the problem of non-uniform mixing of the whiskers accepted by academia at present is to adopt an in-situ synthesis method, namely, the step of mixing is avoided by in-situ synthesis of whisker materials in the materials, so that the problem that the whiskers are not easy to mix uniformly is solved. However, even if the sialon whisker is introduced by adopting an in-situ synthesis mode, the corundum still adopts industrial raw materials, so that the product cost is high, the forming is difficult, and the product yield is low.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a sialon whisker-corundum composite ceramic material which uses natural minerals as raw materials, and the sialon whisker-corundum composite ceramic material which uses natural minerals, metal aluminum powder, metal silicon powder and aluminum fluoride as raw material systems is convenient for introducing sialon whiskers and corundum in an in-situ synthesis mode, so that the sialon whisker-corundum composite ceramic material with high performance and low cost is obtained. The invention also aims to provide a preparation method of the sialon whisker-corundum composite ceramic material by using natural minerals as raw materials and a prepared product.
The purpose of the invention is realized by the following technical scheme:
the invention provides a sialon whisker-corundum composite ceramic material using natural minerals as raw materials, which comprises a base material and a bonding agent; the base material comprises 60-80 wt% of aluminosilicate mineral, 10-30 wt% of metal aluminum powder, 5-20 wt% of metal silicon powder and 1-3 wt% of aluminum fluoride; the dosage of the binder is 6-12 wt% of the base material.
Furthermore, the aluminosilicate mineral is one, two or three of natural kaolin, ball clay, andalusite, sillimanite, kyanite and bauxite. The particle size of the aluminosilicate mineral is 80-325 meshes, the particle size of the metal aluminum powder is 100-700 meshes, and the particle size of the metal silicon powder is 100-700 meshes. The binding agent is water, dextrin, waste paper pulp liquid and PVA solution with the concentration of 5 wt%.
The other purpose of the invention is realized by the following technical scheme:
the preparation method of the sialon whisker-corundum composite ceramic material by using natural minerals as raw materials, which is provided by the invention, comprises the following steps:
(1) mixing the base materials according to a ratio, adding a binding agent, uniformly mixing, stirring, ageing, carrying out compression molding, and drying to obtain a green body;
(2) carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely carrying out vacuum firing at the temperature of below 1200 ℃, carrying out nitrogen atmosphere sintering at the temperature of above 1200 ℃, and finally firing for 1-3 h at the temperature of 1350-1600 ℃ in a nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
Further, the green body dried in the step (1) of the preparation method has the moisture content of less than 1%.
The product prepared by the preparation method of the sialon whisker-corundum composite ceramic material by using natural minerals as raw materials is provided by the invention.
The invention has the following beneficial effects:
(1) the invention adopts a raw material system of natural aluminosilicate mineral-metal aluminum powder-metal silicon powder-aluminum fluoride, and adopts aluminum powder, aluminum fluoride and mineral aluminum oxide to synthesize Al2O and AlAF gas phase, metal silicon reacts with silicon dioxide of mineral in situ to generate SiO gas phase product, Al2Reacting the O, AlAF and SiO gas-phase products with nitrogen to generate a large amount of sialon whiskers in situ; silicon dioxide in the aluminosilicate mineral is continuously replaced by aluminum powder in the sintering process to generate metal siliconAnd the rest alumina is synthesized in situ to obtain corundum. The sialon whiskers synthesized in situ can be uniformly distributed among corundum particles, so that the problem that industrial powder and aggregate are not easy to mix uniformly in the prior art is effectively solved, and the performance of the sialon whisker-corundum composite ceramic material is greatly improved.
(2) The invention mainly uses natural minerals, wherein ball clay and kaolin have good plasticity and are beneficial to improving the forming performance, thereby obviously improving the yield of products; in addition, the used natural minerals have the advantages of large reserves, wide distribution, low price and the like, and are beneficial to reducing the product cost. The used metal aluminum powder has a lower melting point, can form a liquid phase at a lower sintering temperature and disperse in a blank, and is not only favorable for sintering materials, but also favorable for solving the problem of uneven performance.
(3) The invention adopts vacuum-nitrogen atmosphere two-stage sintering, effectively avoids the reduction of the content of reducing agents such as aluminum powder, silicon powder and the like and the caused Al-to-Al ratio caused by the reaction of the aluminum powder and the silicon powder with nitrogen at a low temperature stage to synthesize aluminum nitride and silicon nitride in the temperature rising process2The influence of the gas phase formation rate of the synthetic sialon whisker such as O, SiO and the like.
(4) The sialon whisker-corundum composite ceramic material synthesized in situ has good thermal shock resistance, low firing shrinkage and high mechanical strength, and the main performance indexes are as follows: the addition amount of the natural minerals is more than or equal to 50 percent, the firing shrinkage is less than 2 percent, the thermal conductivity is more than 10W/(m.K), the bending strength is more than or equal to 40MPa, the natural minerals are not cracked after being subjected to thermal shock resistance circulation for 30 times at 1100 ℃ to room temperature, and the natural minerals are not softened and deformed after being kept warm for 1 hour at 1400 ℃.
(5) The invention has the advantages of easily obtained raw materials, simple process and low sintering temperature, and has important significance for improving the quality of the corundum-based ceramic material and saving the product cost, thereby having wide market prospect and being beneficial to popularization and application and the improvement 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 is an X-ray diffraction pattern of a sialon whisker-corundum composite ceramic material prepared by the embodiment of the invention;
FIG. 2 is a transmission electron image of sialon whiskers in the sialon whisker-corundum composite ceramic material prepared in the examples of the present invention.
Detailed Description
The first embodiment is as follows:
1. the embodiment discloses a sialon whisker-corundum composite ceramic material taking natural minerals as raw materials, which comprises a base material and a bonding agent. Wherein:
the raw material composition of the base material is 64 wt% of aluminosilicate mineral (wherein andalusite (granularity of 80 meshes) is 34 wt%, kaolin (granularity of 250 meshes) is 30 wt%, metal aluminum powder (granularity of 180 meshes) is 30 wt%, metal silicon powder (granularity of 100 meshes) is 5 wt%, and aluminum fluoride is 1 wt%. The binding agent is formed by mixing water and 5 wt% PVA solution (according to the mass ratio of 1: 1), and the dosage of the binding agent is 8 wt% of the base material.
2. In this embodiment, the preparation method of the sialon whisker-corundum composite ceramic material using natural minerals as raw materials includes the following steps:
(1) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, stirring, ageing, selecting proper pressure according to the size of a product, pressing and molding, and drying at the temperature of 110 ℃ to obtain a green body (the moisture in a kiln is less than 1%);
(2) carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely heating to 1200 ℃ in vacuum, introducing nitrogen at 1200 ℃, heating to 1450 ℃, and firing for 2 hours in nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
The second embodiment:
1. the embodiment discloses a sialon whisker-corundum composite ceramic material taking natural minerals as raw materials, which comprises a base material and a bonding agent. Wherein:
the raw material composition of the base material is 60 wt% of aluminosilicate mineral (wherein, 10 wt% of ball clay (granularity 325 meshes), 50 wt% of bauxite (granularity 180 meshes)), 17 wt% of metal aluminum powder (granularity 100 meshes), 20 wt% of metal silicon powder (granularity 700 meshes) and 3 wt% of aluminum fluoride. The binding agent is formed by mixing water and dextrin (according to the mass ratio of 1: 1), and the dosage of the binding agent is 6 wt% of the base material.
2. In this embodiment, the preparation method of the sialon whisker-corundum composite ceramic material using natural minerals as raw materials includes the following steps:
(1) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, stirring, ageing, selecting proper pressure according to the size of a product, pressing and molding, and drying at the temperature of 110 ℃ to obtain a green body (the moisture in a kiln is less than 1%);
(2) carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely heating to 1200 ℃ in vacuum, introducing nitrogen at 1200 ℃, heating to 1500 ℃ and firing for 2 hours in nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
Example three:
1. the embodiment discloses a sialon whisker-corundum composite ceramic material taking natural minerals as raw materials, which comprises a base material and a bonding agent. Wherein:
the raw material composition of the base material is 75 wt% of aluminosilicate mineral (wherein 35 wt% of kaolin (granularity of 250 meshes), 40 wt% of andalusite (granularity of 100 meshes)), 13 wt% of metal aluminum powder (granularity of 700 meshes), 10 wt% of metal silicon powder (granularity of 325 meshes) and 2 wt% of aluminum fluoride. The binding agent is waste paper pulp liquid, and the dosage of the binding agent is 6 wt% of the base material.
2. In this embodiment, the preparation method of the sialon whisker-corundum composite ceramic material using natural minerals as raw materials includes the following steps:
(1) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, stirring, ageing, selecting proper pressure according to the size of a product, pressing and molding, and drying at the temperature of 110 ℃ to obtain a green body (the moisture in a kiln is less than 1%);
(2) carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely heating to 1200 ℃ in vacuum, introducing nitrogen at 1200 ℃, heating to 1550 ℃ and firing for 2 hours in nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
Example four:
1. the embodiment discloses a sialon whisker-corundum composite ceramic material taking natural minerals as raw materials, which comprises a base material and a bonding agent. Wherein:
the raw material composition of the base material is 80 wt% of aluminosilicate mineral (wherein 40 wt% of kyanite (granularity 120 meshes), 25 wt% of sillimanite (granularity 120 meshes), 15 wt% of kaolin (granularity 325 meshes), 14 wt% of metal aluminum powder (granularity 325 meshes), 5 wt% of metal silicon powder (granularity 325 meshes) and 1 wt% of aluminum fluoride. 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. In this embodiment, the preparation method of the sialon whisker-corundum composite ceramic material using natural minerals as raw materials includes the following steps:
(1) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, stirring, ageing, selecting proper pressure according to the size of a product, pressing and molding, and drying at the temperature of 110 ℃ to obtain a green body (the moisture in a kiln is less than 1%);
(2) carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely heating to 1200 ℃ in vacuum, introducing nitrogen at 1200 ℃, heating to 1600 ℃ and firing for 1h in nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
Example five:
1. the embodiment discloses a sialon whisker-corundum composite ceramic material taking natural minerals as raw materials, which comprises a base material and a bonding agent. Wherein:
the raw material composition of the base material is 80 wt% (wherein 40 wt% of kaolin (granularity 250 meshes), 30 wt% of kyanite (granularity 180 meshes), 10 wt% of ball clay (granularity 325 meshes), 10 wt% of metal aluminum powder (granularity 325 meshes), 7 wt% of metal silicon powder (granularity 325 meshes) and 3 wt% of aluminum fluoride. The binding agent is formed by mixing water and waste paper pulp liquid (according to the mass ratio of 1: 1), and the consumption of the binding agent is 8 wt% of the base material.
2. In this embodiment, the preparation method of the sialon whisker-corundum composite ceramic material using natural minerals as raw materials includes the following steps:
(1) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, stirring, ageing, selecting proper pressure according to the size of a product, pressing and molding, and drying at the temperature of 110 ℃ to obtain a green body (the moisture in a kiln is less than 1%);
(2) carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely heating to 1200 ℃ in vacuum, introducing nitrogen at 1200 ℃, heating to 1580 ℃ and firing for 1h in nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
Example six:
1. the embodiment discloses a sialon whisker-corundum composite ceramic material taking natural minerals as raw materials, which comprises a base material and a bonding agent. Wherein:
the raw material composition of the base material is 70 wt% of aluminosilicate mineral (wherein 50 wt% of kaolin (granularity of 250 meshes), 20 wt% of sillimanite (granularity of 180 meshes)), 24 wt% of metal aluminum powder (granularity of 325 meshes), 5 wt% of metal silicon powder (granularity of 325 meshes) and 1 wt% of aluminum fluoride. The binder is water and its amount is 12 wt% of the base material.
2. In this embodiment, the preparation method of the sialon whisker-corundum composite ceramic material using natural minerals as raw materials includes the following steps:
(1) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, stirring, ageing, selecting a proper pressure according to the size of a product, performing compression molding, and drying at the temperature of 110 ℃ to obtain a green body (the moisture in a kiln is less than 1%);
(2) carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely heating to 1200 ℃ in vacuum, introducing nitrogen at 1200 ℃, heating to 1400 ℃ and firing for 1h in nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
Example seven:
1. the embodiment discloses a sialon whisker-corundum composite ceramic material taking natural minerals as raw materials, which comprises a base material and a bonding agent. Wherein:
the raw material composition of the base material is 70 wt% of aluminosilicate mineral (wherein, 50 wt% of sillimanite (granularity of 250 meshes), 10 wt% of bauxite (granularity of 180 meshes), 10 wt% of kaolin (granularity of 325 meshes), 15 wt% of metal aluminum powder (granularity of 700 meshes), 13 wt% of metal silicon powder (granularity of 325 meshes) and 2 wt% of aluminum fluoride. 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. In this embodiment, the preparation method of the sialon whisker-corundum composite ceramic material using natural minerals as raw materials includes the following steps:
(1) mixing the base materials according to a ratio, adding a bonding agent, uniformly mixing, stirring, ageing, selecting proper pressure according to the size of a product, pressing and molding, and drying at the temperature of 110 ℃ to obtain a green body (the moisture in a kiln is less than 1%);
(2) vacuum-nitrogen atmosphere two-stage sintering is carried out on the green body, namely the temperature is increased to 1200 ℃ in vacuum, then nitrogen is introduced at 1200 ℃, and the temperature is increased to 1560 ℃ and the sintering is carried out for 2 hours in nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
As shown in FIG. 1, the sialon whisker-corundum composite ceramic material prepared by the embodiment of the invention has only two crystal phases, namely sialon and corundum. As shown in fig. 2, in the sialon whisker-corundum composite ceramic material prepared in the embodiment of the present invention, sialon whiskers are distributed among corundum, and can play a role in improving thermal conductivity, breaking strength and thermal shock resistance.
Claims (6)
1. A sialon whisker-corundum composite ceramic material using natural minerals as raw materials is characterized in that: comprises a base material and a bonding agent; the base material comprises 60-80 wt% of aluminosilicate mineral, 10-30 wt% of metal aluminum powder, 5-20 wt% of metal silicon powder and 1-3 wt% of aluminum fluoride; the dosage of the binder is 6-12 wt% of the base material; mixing the base materials according to the raw material composition ratio, adding a binding agent, uniformly mixing, stirring, ageing, performing compression molding, and drying to obtain a green body; carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely carrying out vacuum firing at the temperature of below 1200 ℃, carrying out nitrogen atmosphere sintering at the temperature of above 1200 ℃, and finally firing for 1-3 h at the temperature of 1350-1600 ℃ under nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
2. The sialon whisker-corundum composite ceramic material using natural minerals as raw materials according to claim 1, characterized in that: the aluminosilicate mineral is one, two or three of natural kaolin, ball clay, andalusite, sillimanite, kyanite and bauxite.
3. The sialon whisker-corundum composite ceramic material using natural minerals as raw materials according to claim 1, characterized in that: the particle size of the aluminosilicate mineral is 80-325 meshes, the particle size of the metal aluminum powder is 100-700 meshes, and the particle size of the metal silicon powder is 100-700 meshes.
4. The sialon whisker-corundum composite ceramic material using natural minerals as raw materials according to claim 1, characterized in that: the binding agent is water, dextrin, waste paper pulp liquid and PVA solution with the concentration of 5 wt%.
5. A method for preparing the sialon whisker-corundum composite ceramic material using natural minerals as raw materials according to any one of claims 1 to 4, characterized in that:
(1) mixing the base materials according to a ratio, adding a binding agent, uniformly mixing, stirring, ageing, carrying out compression molding, and drying to obtain a green body;
(2) carrying out vacuum-nitrogen atmosphere two-stage sintering on the green body, namely carrying out vacuum firing at the temperature of below 1200 ℃, carrying out nitrogen atmosphere sintering at the temperature of above 1200 ℃, and finally firing for 1-3 h at the temperature of 1350-1600 ℃ in a nitrogen atmosphere; and then naturally cooling to room temperature to obtain the sialon whisker-corundum composite ceramic material.
6. The method for preparing the sialon whisker-corundum composite ceramic material by using natural minerals as the raw materials according to claim 5, characterized in that: the moisture content of the green compact dried in the step (1) is less than 1%.
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| CN115724680B (en) * | 2022-11-21 | 2023-05-26 | 景德镇陶瓷大学 | Low-temperature in-situ preparation method of SiC nanowire coating surface modified alumina-based honeycomb ceramic and product prepared by same |
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