CN115231925A - Method for preparing calcium hexaluminate combined silicon carbide ceramic by microwave - Google Patents
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Abstract
The invention relates to a method for preparing calcium hexaluminate combined silicon carbide ceramic by microwaves, which comprises the following steps: (1) Uniformly mixing an aluminum source, a calcium source and silicon carbide powder and then molding to obtain a blank; (2) And placing the formed blank in a microwave sintering furnace, heating the material by virtue of the wave-absorbing property of the silicon carbide powder, and carrying out in-situ reaction on an aluminum source and a calcium source to realize the preparation of the calcium hexaluminate-silicon carbide ceramic. The calcium hexaluminate-bonded silicon carbide ceramic prepared by the method realizes sintering by means of the self heating of silicon carbide during microwave sintering, does not need to use an external heat source, and has the advantages of low energy consumption in the adding process, rapid sintering of calcium hexaluminate, good bonding uniformity, low sintering temperature, short heat preservation time and high strength of the prepared calcium hexaluminate-bonded silicon carbide product.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a method for preparing calcium hexaluminate combined silicon carbide ceramic by microwaves.
Background
The SiC ceramic has excellent oxidation resistance, high hardness, high thermal conductivity and excellent thermal shock resistance, so the SiC ceramic is widely applied to high-temperature industry. However, the covalent bond of Si-C is extremely strong, so that the sintering temperature needs to be raised to more than 2000 ℃, which causes great energy consumption. In order to lower the firing temperature, researchers have tried to add a sintering aid to fire SiC ceramics. Most sintering aids can significantly reduce the sintering performance of silicon carbide ceramics.
The calcium hexaluminate is a compound with the highest melting point in an aluminum-calcium binary system, has excellent high-temperature stability and erosion resistance, and has wide application prospects in the fields of high-performance combustors, gas turbine blades and the like. However, the firing temperature of the calcium hexaluminate-silicon carbide ceramic is generally above 1500 ℃ at present, the heat preservation time is generally above 3h, the energy consumption is increased, and the product is unevenly heated under the action of the traditional heating mode, so that the well-developed flaky calcium hexaluminate is difficult to prepare, and the service performance of the silicon carbide-calcium hexaluminate material is influenced.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention aims to provide a method for preparing calcium hexaluminate combined silicon carbide ceramic by microwaves. No external heat source is needed, the energy consumption in the heating process is low, the calcium hexaluminate is rapidly generated, the crystal growth is good, the firing temperature is low (1000-1300 ℃), the heat preservation time is short (< 20 min), and the prepared calcium hexaluminate-silicon carbide product has high strength.
The invention is realized by the following technical scheme, and the method for preparing calcium hexaluminate combined silicon carbide ceramic by microwaves provided by the invention specifically comprises the following steps:
uniformly mixing an aluminum source, a calcium source and silicon carbide powder to form mixed powder, and preparing a blank body in a certain forming mode;
the aluminum source comprises one or more of alumina, aluminum hydroxide, polyaluminum chloride, aluminum dihydrogen phosphate, alumina sol and calcium aluminate cement;
the calcium source comprises one or more of calcium oxide, calcium hydroxide, calcium carbonate and calcium aluminate cement;
the molar ratio of the alumina in the aluminum source to the calcium oxide in the calcium source to the silicon carbide in the silicon carbide powder is (2);
placing the formed blank in a microwave sintering furnace, heating the microwave sintering furnace to 1000-1300 ℃, preserving the temperature for 10-20 min, and carrying out in-situ reaction on an aluminum source and a calcium source to obtain calcium hexaluminate combined silicon carbide ceramic;
the obtained calcium hexaluminate-bonded silicon carbide ceramic is compact ceramic or porous ceramic.
Preferably, the molding method in the step (1) is one of dry pressing, isostatic pressing, gel molding and extrusion molding.
Preferably, a pore-forming process is added in the step (1) to enable the finally prepared calcium hexaluminate-bonded silicon carbide ceramic to be porous ceramic, wherein the pore-forming process adopts one of a foaming method, an emulsion template method, a solid pore-forming agent method, an organic foam impregnation method and a phase inversion method.
Preferably, the increasing speed of the microwave input power is 0.1 KW/min-1 KW/min, the temperature is kept for 10-20 min after the temperature is raised to 1000-1300 ℃, and the firing atmosphere is air or argon.
The preparation method for preparing calcium hexaluminate-bonded silicon carbide ceramic by microwave can specifically adopt the following scheme:
weighing aluminum hydroxide powder, calcium hydroxide powder and silicon carbide powder according to the molar ratio of aluminum oxide, calcium oxide and silicon carbide 2:3 (10-50), uniformly mixing to form mixed powder, adding a binding agent accounting for 2-4% of the total mass of the mixed powder, stirring and mixing, and preparing a blank by adopting a dry pressing or isostatic pressing or gel forming or extrusion forming mode;
and (2) placing the blank body in a microwave sintering furnace, increasing the microwave input power at the speed of 0.1-1 KW/min in the air atmosphere or argon atmosphere, heating to 1000-1200 ℃, and preserving the heat for 20min to obtain the calcium hexaluminate combined silicon carbide ceramic.
Preferably, the binding agent in step (1) is aluminum dihydrogen phosphate or dextrin.
The preparation method for preparing calcium hexaluminate-bonded silicon carbide ceramic by microwave can specifically adopt the following scheme:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the molar ratio of the alumina to the calcium oxide to the silicon carbide of 2 to 50, uniformly mixing, placing the mixture in a ball milling tank, taking the calcium aluminate cement as a binding agent, adding water accounting for 50 percent of the total mass of the mixed powder into the ball milling tank, pouring the mixture in a mold after ball milling for 30min, drying the mixture for 3d in an air atmosphere, demolding, and baking the mixture at 110 ℃ for 12h;
and (2) placing the blank body in a microwave sintering furnace, increasing the microwave input power at the rate of 0.3KW/min in the air atmosphere, heating to 1200 ℃, and preserving the heat for 20min to obtain the calcium hexaluminate combined silicon carbide ceramic.
The preparation method for preparing calcium hexaluminate-bonded silicon carbide ceramic by microwave can specifically adopt the following scheme:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the molar ratio of the alumina to the calcium oxide to the silicon carbide of 2 to 50, uniformly mixing to form mixed powder, placing the mixed powder into a ball milling tank, simultaneously adding water and a foaming agent into the ball milling tank, ball milling and mixing for 30min to prepare ceramic slurry, pouring the ceramic slurry into a mold, drying for 7d in an air atmosphere, demolding, and baking for 24h at 100 ℃ to obtain a molded blank;
and (2) placing the blank body in a microwave sintering furnace, increasing the microwave input power at the speed of 0.6KW/min under the argon atmosphere, heating to 1300 ℃, and preserving the temperature for 20min to obtain the porous calcium hexaluminate-bonded silicon carbide ceramic.
Preferably, the foaming agent is sodium dodecyl benzene sulfonate, the adding mass of the sodium dodecyl benzene sulfonate accounts for 5% of the total mass of the mixed powder, and the adding mass of the water accounts for 50% of the total mass of the mixed powder.
The preparation method for preparing calcium hexaluminate-bonded silicon carbide ceramic by microwave can specifically adopt the following scheme:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the molar ratio of the alumina to the calcium oxide to the silicon carbide of 2 to 70, uniformly mixing to form mixed powder, placing the mixed powder in a ball milling tank, simultaneously adding water accounting for 50 percent of the total mass of the mixed powder in the ball milling tank as a dispersion medium, taking n-octane accounting for twice the volume of the water as an organic dispersion phase, taking Tween 80 accounting for 2 percent of the mass of the water as an emulsifier, mixing in the ball milling tank for 30min to prepare ceramic slurry, pouring the ceramic slurry into a mold, drying in an air atmosphere for 3d, demolding, and baking at 110 ℃ for 24h to obtain a molded blank;
and (2) placing the blank body in a microwave sintering furnace, increasing the microwave input power at the speed of 0.2KW/min in the air atmosphere, heating to 1100 ℃, and preserving the heat for 10min to obtain the porous calcium hexaluminate-bonded silicon carbide ceramic.
Compared with the prior art, the invention has the following advantages:
uniformly mixing an aluminum source, a calcium source and silicon carbide powder, molding to obtain a blank, placing the blank in a microwave sintering furnace after molding the blank, heating the blank by microwaves, and carrying out in-situ reaction on the aluminum source and the calcium source by virtue of the wave-absorbing property of the silicon carbide powder so as to realize the preparation of the calcium hexaluminate combined silicon carbide ceramic.
According to the invention, the sintering is realized by means of the self-heating of the silicon carbide during microwave sintering, an external heat source is not needed by adopting a microwave heating method, the energy consumption in the heating process is low, the calcium hexaluminate is sintered quickly, the bonding uniformity is good, the sintering temperature is low, the heat preservation time is short, and the prepared calcium hexaluminate bonded silicon carbide product has high strength.
The foregoing is a summary of the present invention, and for the purpose of making the technical means of the present invention more comprehensible, the present invention may be implemented in accordance with the contents of the present specification, and the above and other objects, features, and advantages thereof may be more clearly understood, and the following detailed description is given of preferred embodiments:
drawings
FIG. 1 is a scanning electron microscope image of porous calcium hexaluminate-bonded silicon carbide ceramic prepared in example 3 of the present invention.
FIG. 2 is an X-ray diffraction pattern of the porous calcium hexaluminate-bonded silicon carbide ceramic prepared in example 3 of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined purpose, the following embodiments are given in detail based on the technology of the present invention and the detailed implementation manner and the operation steps in combination with the drawings and the specific embodiments, but the scope of the present invention is not limited to the following embodiments.
Example 1:
weighing aluminum hydroxide, calcium hydroxide and silicon carbide powder according to the mol ratio of the aluminum oxide to the calcium oxide to the silicon carbide being 2.
Example 2:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the molar ratio of the alumina to the calcium oxide to the silicon carbide being 2.
Example 3:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the mol ratio of the alumina to the calcium oxide to the silicon carbide of 2:3, placing the alumina to the calcium aluminate cement to the silicon carbide powder in a ball milling tank, simultaneously adding water accounting for 50% of the total mass of the mixed powder in the ball milling tank, adding 5% of sodium dodecylbenzenesulfonate as a foaming agent, performing ball milling and mixing for 30min to obtain ceramic slurry, pouring the ceramic slurry in a mold, drying for 7d in air atmosphere, demolding, baking for 24h at 100 ℃ to obtain a blank, finally placing the blank in a microwave sintering furnace, increasing the microwave input power at the rate of 0.6KW/min in argon atmosphere, heating to 1300 ℃, and preserving the temperature for 20min to obtain the porous calcium hexaluminate combined silicon carbide ceramic.
FIG. 1 is a scanning electron micrograph of the calcium hexaluminate-bonded silicon carbide ceramic prepared in example 3, from which it can be seen that: calcium hexaluminate with hexagonal plate structure and good crystal grain development grows among the silicon carbide particles.
FIG. 2 is an X-ray diffraction pattern of the calcium hexaluminate-bonded silicon carbide ceramic prepared in example 3, from which it can be seen that: the calcium hexaluminate is synthesized in situ by microwave sintering.
Example 4:
weighing aluminum hydroxide, calcium hydroxide and silicon carbide powder according to the molar ratio of the aluminum oxide to the calcium oxide to the silicon carbide being 2; and finally, placing the blank body in a microwave sintering furnace, increasing the microwave input power at the speed of 1KW/min in the air atmosphere, heating to 1000 ℃, and preserving the heat for 20min to obtain the calcium hexaluminate bonded silicon carbide ceramic.
Example 5:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the molar ratio of the alumina to the calcium oxide to the silicon carbide being 2; and finally, placing the blank in a microwave sintering furnace, increasing the microwave input power at the rate of 0.2KW/min in the air atmosphere, heating to 1100 ℃, and preserving the heat for 10min to obtain the porous calcium hexaluminate-bonded silicon carbide ceramic.
The above description is only an individual example of the present invention, and is not intended to limit the present invention in any way, as long as the aluminum source, the silicon source and the silicon carbide powder are uniformly mixed, and a green body is prepared by a certain forming method; and (3) placing the obtained blank in a microwave sintering furnace, taking air or argon as sintering atmosphere, heating to 1000-1300 ℃ under certain microwave input power, and then preserving heat for 0-30 min to obtain the calcium hexaluminate combined silicon carbide ceramic. The prepared calcium hexaluminate-bonded silicon carbide ceramic can be compact ceramic or porous ceramic, if the porous ceramic is prepared, a pore-forming process can be added before a green body is prepared to realize the preparation of the porous ceramic, and the pore-forming process can adopt one of a foaming method, an emulsion template method, a solid pore-forming agent method, an organic foam impregnation method and a phase conversion method. The invention adopts a microwave heating method, does not need an external heat source, has low energy consumption in the heating process, quick sintering of calcium hexaluminate, good combination uniformity, low sintering temperature and short heat preservation time, and the prepared calcium hexaluminate combined silicon carbide product has high strength.
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A method for preparing calcium hexaluminate combined silicon carbide ceramic by microwave is characterized by comprising the following steps:
uniformly mixing an aluminum source, a calcium source and silicon carbide powder to form mixed powder, and preparing a blank body in a certain forming mode;
the aluminum source comprises one or more of alumina, aluminum hydroxide, polyaluminum chloride, aluminum dihydrogen phosphate, alumina sol and calcium aluminate cement;
the calcium source comprises one or more of calcium oxide, calcium hydroxide, calcium carbonate and calcium aluminate cement;
the molar ratio of the alumina in the aluminum source, the calcium oxide in the calcium source and the silicon carbide in the silicon carbide powder is 2;
placing the molded blank in a microwave sintering furnace, heating the microwave sintering furnace to 1000-1300 ℃, preserving the temperature for 10-20 min, and carrying out in-situ reaction on an aluminum source and a calcium source to obtain calcium hexaluminate combined silicon carbide ceramic;
the obtained calcium hexaluminate-bonded silicon carbide ceramic is compact ceramic or porous ceramic.
2. The method for preparing calcium hexaluminate bonded silicon carbide ceramic by microwave as claimed in claim 1, wherein: the forming mode in the step (1) is one of dry pressing forming, isostatic pressing forming, gel forming and extrusion forming.
3. The method for preparing calcium hexaluminate bonded silicon carbide ceramic by microwave as claimed in claim 2, wherein: and (2) adding a pore-forming process in the step (1) to enable the finally prepared calcium hexaluminate-bonded silicon carbide ceramic to be porous ceramic, wherein the pore-forming process adopts one of a foaming method, an emulsion template method, a solid pore-forming agent method, an organic foam impregnation method and a phase conversion method.
4. The method for preparing calcium hexaluminate bonded silicon carbide ceramic by using microwaves as claimed in claim 1, wherein the microwave preparation method comprises the following steps: the increasing speed of the microwave input power is 0.1 KW/min-1 KW/min, the temperature is kept for 10-20 min after the temperature is raised to 1000-1300 ℃, and the firing atmosphere is air or argon.
5. The method for preparing calcium hexaluminate bonded silicon carbide ceramic by microwave as claimed in claim 1, comprising the steps of:
weighing aluminum hydroxide powder, calcium hydroxide powder and silicon carbide powder according to the molar ratio of aluminum oxide, calcium oxide and silicon carbide 2:3 (10-50), uniformly mixing to form mixed powder, adding a binding agent accounting for 2-4% of the total mass of the mixed powder, stirring and mixing, and preparing a blank by adopting a dry pressing or isostatic pressing or gel forming or extrusion forming mode;
and (2) placing the blank body in a microwave sintering furnace, increasing the microwave input power at the speed of 0.1-1 KW/min in the air atmosphere or argon atmosphere, heating to 1000-1200 ℃, and preserving the heat for 20min to obtain the calcium hexaluminate combined silicon carbide ceramic.
6. The method for preparing calcium hexaluminate bonded silicon carbide ceramic by microwave as claimed in claim 5, wherein the binder used in step (1) is aluminum dihydrogen phosphate or dextrin.
7. The method for preparing calcium hexaluminate bonded silicon carbide ceramic by microwave as claimed in claim 1, comprising the steps of:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the molar ratio of the alumina to the calcium oxide to the silicon carbide of 2 to 3, uniformly mixing, placing the mixture in a ball milling tank, taking the calcium aluminate cement as a binding agent, adding water accounting for 50% of the total mass of the mixed powder into the ball milling tank, pouring the mixture in a mold after ball milling for 30min, drying the mixture in an air atmosphere for 3d, demolding, and baking the mixture at 110 ℃ for 12h;
and (2) placing the blank in a microwave sintering furnace, increasing the microwave input power at the rate of 0.3KW/min in the air atmosphere, heating to 1200 ℃, and preserving the heat for 20min to obtain the calcium hexaluminate combined silicon carbide ceramic.
8. The method for preparing calcium hexaluminate bonded silicon carbide ceramic by microwave as claimed in claim 3, comprising the steps of:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the molar ratio of the alumina to the calcium oxide to the silicon carbide of 2 to 50, uniformly mixing to form mixed powder, placing the mixed powder into a ball milling tank, simultaneously adding water and a foaming agent into the ball milling tank, ball milling and mixing for 30min to prepare ceramic slurry, pouring the ceramic slurry into a mold, drying for 7d in an air atmosphere, demolding, and baking for 24h at 100 ℃ to obtain a molded blank;
and (2) placing the blank body in a microwave sintering furnace, increasing the microwave input power at the speed of 0.6KW/min under the argon atmosphere, heating to 1300 ℃, and preserving the temperature for 20min to obtain the porous calcium hexaluminate-bonded silicon carbide ceramic.
9. The method for preparing calcium hexaluminate combined silicon carbide ceramic by microwaves as claimed in claim 8, wherein the foaming agent is sodium dodecylbenzenesulfonate, the added mass of the sodium dodecylbenzenesulfonate accounts for 5% of the total mass of the mixed powder, and the added mass of water accounts for 50% of the total mass of the mixed powder.
10. The method for preparing calcium hexaluminate bonded silicon carbide ceramic by using microwaves as claimed in claim 3, wherein the method comprises the following steps:
weighing alumina, calcium aluminate cement and silicon carbide powder according to the molar ratio of the alumina to the calcium oxide to the silicon carbide of 2 to 70, uniformly mixing to form mixed powder, placing the mixed powder in a ball milling tank, simultaneously adding water accounting for 50 percent of the total mass of the mixed powder in the ball milling tank as a dispersion medium, taking n-octane accounting for twice the volume of the water as an organic dispersion phase, taking Tween 80 accounting for 2 percent of the mass of the water as an emulsifier, mixing in the ball milling tank for 30min to prepare ceramic slurry, pouring the ceramic slurry into a mold, drying in an air atmosphere for 3d, demolding, and baking at 110 ℃ for 24h to obtain a molded blank;
and (2) placing the blank body in a microwave sintering furnace, increasing the microwave input power at the speed of 0.2KW/min in the air atmosphere, heating to 1100 ℃, and preserving the heat for 10min to obtain the porous calcium hexaluminate-bonded silicon carbide ceramic.
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| CN115744949A (en) * | 2022-10-27 | 2023-03-07 | 中国长城铝业有限公司 | Preparation method of high-aluminum calcium aluminate powder |
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| CN105753507A (en) * | 2016-03-01 | 2016-07-13 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of silicon carbide-calcium hexaluminate complex phase porous ceramic |
| CN107892575A (en) * | 2017-11-24 | 2018-04-10 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of carborundum calcium hexaluminate composite refractory |
| CN108101520A (en) * | 2017-12-23 | 2018-06-01 | 深圳万佳互动科技有限公司 | Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115744949A (en) * | 2022-10-27 | 2023-03-07 | 中国长城铝业有限公司 | Preparation method of high-aluminum calcium aluminate powder |
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