CN111574214B - Calcium hexaluminate complex phase material and preparation method thereof - Google Patents

Calcium hexaluminate complex phase material and preparation method thereof Download PDF

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CN111574214B
CN111574214B CN202010254679.2A CN202010254679A CN111574214B CN 111574214 B CN111574214 B CN 111574214B CN 202010254679 A CN202010254679 A CN 202010254679A CN 111574214 B CN111574214 B CN 111574214B
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calcium hexaluminate
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侯新梅
王恩会
杨涛
方志
郭春雨
徐林超
康俊一
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University of Science and Technology Beijing USTB
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    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3895—Non-oxides with a defined oxygen content, e.g. SiOC, TiON
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/46—Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase

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Abstract

The invention discloses a calcium hexaluminate complex phase material and a preparation method thereof, wherein the method comprises the following steps: putting aluminum powder, alumina powder and calcium oxide powder into a high-energy ball mill for ball milling to obtain mixed powder; mixing the mixed powder with a binding agent, and performing mechanical pressing to obtain a green body; and putting the green body into a high-temperature atmosphere furnace, and carrying out carbon-embedding sintering on the green body in a nitrogen atmosphere to obtain the calcium hexaluminate complex-phase material containing calcium hexaluminate/aluminum oxynitride. According to the invention, the performance of the calcium hexaluminate material is improved by introducing AlON, and the compactness and the slag erosion resistance of the calcium hexaluminate material can be greatly improved on the basis of ensuring the chemical stability of the calcium hexaluminate material. Meanwhile, in the process of preparing the calcium hexaluminate complex phase refractory material, aluminum nitride is generated by directly nitriding aluminum powder and is used as a nitrogen source, and a part of aluminum powder is used as a reducing agent, so that the purity of the calcium hexaluminate AlON complex phase refractory material is ensured.

Description

Calcium hexaluminate complex phase material and preparation method thereof
Technical Field
The invention belongs to the technical field of inorganic non-metallic materials, and particularly relates to a calcium hexaluminate complex phase material and a preparation method thereof.
Background
Under the large environment of ever-increasing world population and severe greenhouse effect, the requirement for more effective utilization and secondary utilization of raw materials and energy sources in related industries is required, especially for related industries such as metallurgy, chemical industry, building materials and the like. Also, the need to recycle waste is environmentally friendly, and thus a strong push for the development of related efficient processes or alternative design techniques. Reducing heat loss and improving the utilization efficiency of heat energy by a high-efficiency heat insulation method so as to reduce CO2Emission has become the industry first choice.
Meanwhile, with the rapid development of the high-temperature industry, higher requirements are put forward on the heat-insulating material, and in the application of the refractory material, the lining loss is reduced by the design of long service life. Among them, the development of the insulation material industry is vigorous, the high-quality heat insulation material is widely adopted, and the heat insulation material is important for sustainable developmentPractical significance, and further achievement of the set goals described above requires more innovative concepts and product solutions. Among them, calcium hexaluminate (CA)6) As a heat-insulating material with excellent performance, the material not only meets the requirement of achieving open source throttling on energy, but also can meet the condition of a functional material, so that in recent years, CA (cellulose acetate)6The use of refractory materials as a new refractory material in high temperature industries is rapidly increasing.
Although CA6High melting point, good stability in high-temperature reducing atmosphere, sufficient erosion resistance in alkaline environment, and low alkaline environment (high SiO)2) The lower anti-erosion ability is not good, and anorthite (CaO. Al) is easy to generate2O3·2SiO2) And gehlenite (2 CaO. Al)2O3·SiO2) A low melting phase. In the use of steel making, the slag for steel making is different due to different steel types, so that more comprehensive performance requirements are provided for the refractory materials.
Furthermore, hexaaluminate cells are composed of spinel blocks and mirror layers which are alternately stacked to form a layer structure, each cell being composed of two spinel blocks and two mirror layers, the mirror layers being preferential diffusion paths for oxygen, O perpendicular to the C-axis direction, since the ideal oxygen density of the mirror is only one quarter of that of the spinel blocks2-The diffusion rate is higher than the diffusion rate in the direction parallel to the C axis, which means that the growth of crystals in the direction parallel to the C axis is suppressed, and thus the pure calcium hexaluminate material has a characteristic of preferentially forming flaky crystals or plate-like crystals, resulting in a problem of low density.
AlON is Al2O3And AlN, which has good high temperature resistance and thermal shock resistance, has poor wettability to molten substances such as metals and oxides due to its nitride material, and is very stable when in contact with these substances, so AlON is an additive component used as a refractory material in steel production. Therefore, it is urgent to provide a method for introducing AlON into calcium hexaluminate.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a calcium hexaluminate complex phase material and a preparation method thereof.
The invention provides a preparation method of a calcium hexaluminate complex phase material on one hand, which comprises the following steps:
putting aluminum powder, alumina powder and calcium oxide powder into a high-energy ball mill for ball milling to obtain mixed powder;
mixing the mixed powder with a binding agent, and performing mechanical pressing to obtain a green body;
and putting the green body into a high-temperature atmosphere furnace, and carrying out carbon-embedding sintering on the green body in a nitrogen atmosphere to obtain the calcium hexaluminate complex-phase material containing calcium hexaluminate/aluminum oxynitride.
Further, when the aluminum powder, the alumina powder and the calcium oxide powder are put into a high-energy ball mill for ball milling, the method comprises the following steps:
aluminum powder, alumina powder and calcium oxide powder are mixed according to the weight ratio of 1: 102-181: 9-16, putting into a high-energy ball mill, and adding absolute ethyl alcohol into the high-energy ball mill;
controlling the ball milling speed of the high-energy ball mill at 230-250rpm/min, and drying the mixed slurry after ball milling for 12h to obtain mixed powder.
Further, when the aluminum powder, the alumina powder and the calcium oxide powder are subjected to ball milling, the mass ratio of balls, mixed powder and absolute ethyl alcohol in the high-energy ball mill is 5-7: 0.5-2: 1-3.
Further, before mixing the mixed powder with a binder, the method further comprises: and crushing the mixed powder to enable the particle size of the mixed powder to be smaller than 200 meshes.
Further, when the green body is subjected to carbon burying sintering, the sintering temperature is 1700-1750 ℃, the temperature is kept at the temperature for 1-3h, and then the green body is cooled along with the furnace to obtain the calcium hexaluminate/aluminum oxynitride-containing calcium hexaluminate complex phase material.
Further, the particle size of the alumina powder is 0.5-6 μm.
Furthermore, the particle size of the calcium oxide powder is 0.5-10 μm.
Further, the binding agent is phenolic resin.
In another aspect, the present invention provides a calcium hexaluminate complex phase material, comprising a calcium hexaluminate complex phase material prepared by the above-mentioned method for preparing a calcium hexaluminate complex phase material.
According to the calcium hexaluminate complex phase material and the preparation method thereof, the performance of the calcium hexaluminate material is improved by introducing AlON, and the compactness and the slag erosion resistance of the calcium hexaluminate material can be greatly improved on the basis of ensuring the chemical stability of the calcium hexaluminate material. Meanwhile, in the process of preparing the calcium hexaluminate complex phase refractory material, aluminum nitride is generated by directly nitriding aluminum powder and is used as a nitrogen source, and a part of aluminum powder is used as a reducing agent, so that the purity of the calcium hexaluminate AlON complex phase refractory material is ensured. In a word, the preparation method of the calcium hexaluminate complex phase material provided by the invention is simple to operate, has low equipment requirement and does not pollute the environment, and meanwhile, the prepared calcium hexaluminate aluminum oxynitride complex phase material has the advantages of relatively compact microstructure, stable structure in the sintering process, excellent slag corrosion resistance and the like.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a calcium hexaluminate complex phase material according to an embodiment of the present invention;
FIG. 2 is an XRD pattern of a refractory material prepared by the preparation method of a calcium hexaluminate complex phase material according to an embodiment of the present invention;
FIG. 3 is an SEM image of a refractory material prepared by the preparation method of a calcium hexaluminate complex phase material according to an embodiment of the present invention;
FIG. 4 shows N according to the present invention2An atmosphere control map.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In one aspect of the present invention, a method for preparing a calcium hexaluminate complex phase material is provided, referring to fig. 1, and comprises:
s100, mixing aluminum powder, alumina powder and calcium oxide powder in a weight ratio of 1: 102-181: 9-16, putting the mixture into a high-energy ball mill, adding absolute ethyl alcohol into the high-energy ball mill, controlling the ball milling rotating speed at 230-250rpm/min, and drying the slurry obtained by mixing after ball milling for 12 hours to obtain mixed powder;
s200, crushing the mixed powder to enable the particle size of the mixed powder to be smaller than 200 meshes, mixing the mixed powder with a binding agent, and performing mechanical compression molding to obtain a green body;
s300, placing the green body into a high-temperature atmosphere furnace, carrying out carbon-embedding sintering on the green body in a nitrogen atmosphere, wherein the sintering temperature is 1700-1750 ℃, preserving heat for 1-3h at the temperature, and then cooling the green body along with the furnace to obtain the calcium hexaluminate complex phase material containing calcium hexaluminate/aluminum oxynitride. Referring to fig. 2, by analyzing the XRD pattern of the refractory obtained according to the present invention, it can be seen that when the sintering temperature is set to 1700 ℃, the phases after sintering are calcium hexaaluminate and AlON, and no other impurity is generated, and thus, the sintering temperature for the green compact is set to 1700-1750 ℃.
As a preferred embodiment, when the aluminum powder, the alumina powder and the calcium oxide powder are ball-milled, the mass ratio of the balls, the mixed powder and the absolute ethyl alcohol in the high-energy ball mill is 5-7: 0.5-2: 1-3.
As a preferred embodiment, the particle size of the alumina powder is 0.5 to 6 μm. In the embodiment, the raw material of the alpha-alumina powder is ball milled for 24 hours to obtain alpha-alumina powder slurry with the particle size of 2-10 μm, and the alpha-alumina powder slurry is dried to obtain the alpha-alumina powder, namely the alumina powder in the embodiment.
As a preferred embodiment, the calcium oxide powder has a particle size of 0.5 to 10 μm. In the embodiment, the calcium oxide powder raw material is ball-milled to obtain a calcium oxide powder slurry with a particle size of 5-12 μm, and the calcium oxide powder slurry is dried to obtain calcium oxide powder, i.e. the calcium oxide powder in the embodiment.
As a preferred embodiment, the binder is a phenolic resin.
In another aspect of the present invention, there is provided a calcium hexaluminate complex phase material, comprising a calcium hexaluminate complex phase material prepared by the above method for preparing a calcium hexaluminate complex phase material.
Referring to fig. 3, it can be seen that the introduction and filling of AlON into the gaps of calcium hexaluminate in the present invention improves the compactness of the calcium hexaluminate material.
Referring to fig. 4, it can be seen that the generation of AlON must be controlled at a certain low partial oxygen pressure.
According to the invention, the novel calcium hexaluminate/aluminum oxynitride multiphase material is prepared by taking the fine powder of the aluminum oxide and the calcium oxide as raw materials and adding the metal aluminum powder and compounding in situ under a certain low-oxygen-pressure nitrogen atmosphere, so that the AlON is introduced into the calcium hexaluminate material, the performance of the calcium hexaluminate material is further improved, the chemical stability of the calcium hexaluminate material can be ensured, and the material density and the slag erosion resistance of the calcium hexaluminate material can be greatly improved. Meanwhile, in the process of preparing the calcium hexaluminate complex phase refractory material, aluminum powder is directly nitrided to generate aluminum nitride as a nitrogen source, and part of the aluminum powder can serve as a reducing agent, so that the purity of the calcium hexaluminate AlON complex phase material is ensured.
Example 1
A preparation method of a calcium hexaluminate complex phase material comprises the following steps:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 24 hours to obtain alpha-alumina powder slurry with the particle size of 2 mu m, and drying the alpha-alumina powder slurry to obtain alpha-alumina powder; performing ball milling treatment on a calcium oxide powder raw material to obtain a calcium oxide powder slurry with the particle size of 4 mu m, and drying the calcium oxide powder slurry to obtain calcium oxide powder;
(2) ball milling and mixing: adding metal aluminum powder into the treated aluminum oxide and calcium oxide powder, mixing the mixture with absolute ethyl alcohol, putting the mixture into a high-energy ball mill, and performing ball milling for 12 hours to uniformly mix the raw materials, wherein the weight ratio of the aluminum powder to the calcium oxide powder is 1: 102: ball milling speed 240rpm/min, ball: mixing powder: the mass ratio of the absolute ethyl alcohol is 6: 1: 2, quickly drying the mixed slurry to avoid layering;
(3) mixing material treatment: fully grinding the dried mixed materials, and sieving the materials through a 200-mesh sieve to ensure that the raw materials are fully mixed;
(4) preparing a green body: adding the mixed material into phenolic resin, mixing, forming by mechanical pressing, and drying the formed green body to obtain a green body;
(5) sintering and synthesizing: and (3) placing the green body into a high-temperature atmosphere furnace, burying carbon, controlling the temperature to be 1750 ℃ for 2 hours under a certain nitrogen atmosphere, and then cooling along with the furnace to obtain the high-performance calcium hexaluminate/aluminum oxynitride novel complex phase material.
Example 2
A preparation method of a calcium hexaluminate complex phase material comprises the following steps:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 16h to obtain alpha-alumina powder slurry with the particle size of 4 mu m, and drying the alpha-alumina powder slurry to obtain alpha-alumina powder; performing ball milling treatment on a calcium oxide powder raw material to obtain a calcium oxide powder slurry with the particle size of 6 mu m, and drying the calcium oxide powder slurry to obtain calcium oxide powder;
(2) ball milling and mixing: adding metal aluminum powder into the treated aluminum oxide and calcium oxide powder, mixing the mixture with absolute ethyl alcohol, putting the mixture into a high-energy ball mill, and performing ball milling for 12 hours to uniformly mix the raw materials, wherein the aluminum powder, the aluminum oxide powder and the calcium oxide powder are mixed according to the weight ratio of 1: 181: 16, ball milling rotation speed 230rpm/min, ball: mixing powder: the mass ratio of the absolute ethyl alcohol is 7: 0.5: 1, quickly drying the mixed slurry to avoid layering;
(3) mixing material treatment: fully grinding the dried mixed materials, and sieving the materials through a 200-mesh sieve to ensure that the raw materials are fully mixed;
(4) preparing a green body: adding the mixed material into phenolic resin, mixing, forming by mechanical pressing, and drying the formed green body to obtain a green body;
(5) sintering and synthesizing: and (3) placing the green body into a high-temperature atmosphere furnace, burying carbon, keeping the temperature of 1750 ℃ for 1.5h under a certain nitrogen atmosphere, and then cooling along with the furnace to obtain the high-performance calcium hexaluminate/aluminum oxynitride novel complex phase material.
Example 3
A preparation method of a calcium hexaluminate complex phase material comprises the following steps:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 16h to obtain alpha-alumina powder slurry with the particle size of 0.5 mu m, and drying the alpha-alumina powder slurry to obtain alpha-alumina powder; performing ball milling treatment on a calcium oxide powder raw material to obtain a calcium oxide powder slurry with the particle size of 0.5 mu m, and drying the calcium oxide powder slurry to obtain calcium oxide powder;
(2) ball milling and mixing: adding metal aluminum powder into the treated aluminum oxide and calcium oxide powder, mixing the mixture with absolute ethyl alcohol, putting the mixture into a high-energy ball mill, and performing ball milling for 12 hours to uniformly mix the raw materials, wherein the aluminum powder, the aluminum oxide powder and the calcium oxide powder are mixed according to the weight ratio of 1: 125: 11, ball milling rotation speed 230rpm/min, ball: mixing powder: the mass ratio of the absolute ethyl alcohol is 5: 2: 3, quickly drying the mixed slurry to avoid layering;
(3) mixing material treatment: fully grinding the dried mixed materials, and sieving the materials through a 200-mesh sieve to ensure that the raw materials are fully mixed;
(4) preparing a green body: adding the mixed material into phenolic resin, mixing, forming by mechanical pressing, and drying the formed green body to obtain a green body;
(5) sintering and synthesizing: and putting the green body into a high-temperature atmosphere furnace, burying carbon, controlling the temperature of 1720 ℃ under a certain nitrogen atmosphere for 3 hours, and then cooling along with the furnace to obtain the high-performance calcium hexaluminate/aluminum oxynitride novel complex phase material.
Example 4
A preparation method of a calcium hexaluminate complex phase material comprises the following steps:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 36h to obtain alpha-alumina powder slurry with the particle size of 6 mu m, and drying the alpha-alumina powder slurry to obtain alpha-alumina powder; performing ball milling treatment on a calcium oxide powder raw material to obtain a calcium oxide powder slurry with the particle size of 10 mu m, and drying the calcium oxide powder slurry to obtain calcium oxide powder;
(2) ball milling and mixing: adding metal aluminum powder into the treated aluminum oxide and calcium oxide powder, mixing the mixture with absolute ethyl alcohol, putting the mixture into a high-energy ball mill, and performing ball milling for 12 hours to uniformly mix the raw materials, wherein the aluminum powder, the aluminum oxide powder and the calcium oxide powder are mixed according to the weight ratio of 1: 146: ball mill rotation speed 230rpm/min, ball: mixing powder: the mass ratio of the absolute ethyl alcohol is 6: 1: 1.5, quickly drying the mixed slurry to avoid layering;
(3) mixing material treatment: fully grinding the dried mixed materials, and sieving the materials through a 200-mesh sieve to ensure that the raw materials are fully mixed;
(4) preparing a green body: adding the mixed material into phenolic resin, mixing, forming by mechanical pressing, and drying the formed green body to obtain a green body;
(5) sintering and synthesizing: and (3) placing the green body into a high-temperature atmosphere furnace, burying carbon, keeping the temperature of 1740 ℃ for 2.5 hours under a certain nitrogen atmosphere, and then cooling along with the furnace to obtain the high-performance calcium hexaluminate/aluminum oxynitride novel complex phase material.
Example 5
A preparation method of a calcium hexaluminate complex phase material comprises the following steps:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 24 hours to obtain alpha-alumina powder slurry with the particle size of 5 mu m, and drying the alpha-alumina powder slurry to obtain alpha-alumina powder; performing ball milling treatment on a calcium oxide powder raw material to obtain a calcium oxide powder slurry with the particle size of 6 mu m, and drying the calcium oxide powder slurry to obtain calcium oxide powder;
(2) ball milling and mixing: adding metal aluminum powder into the treated aluminum oxide and calcium oxide powder, mixing the mixture with absolute ethyl alcohol, putting the mixture into a high-energy ball mill, and performing ball milling for 12 hours to uniformly mix the raw materials, wherein the aluminum powder, the aluminum oxide powder and the calcium oxide powder are mixed according to the weight ratio of 1: 152: 12, ball milling rotation speed of 250rpm/min, ball: mixing powder: the mass ratio of the absolute ethyl alcohol is 5: 1: 2, quickly drying the mixed slurry to avoid layering;
(3) mixing material treatment: fully grinding the dried mixed materials, and sieving the materials through a 200-mesh sieve to ensure that the raw materials are fully mixed;
(4) preparing a green body: adding the mixed material into phenolic resin, mixing, forming by mechanical pressing, and drying the formed green body to obtain a green body;
(5) sintering and synthesizing: and (3) placing the green body into a high-temperature atmosphere furnace, burying carbon, controlling the temperature to be 1750 ℃ for 1h under a certain nitrogen atmosphere, and then cooling along with the furnace to obtain the high-performance calcium hexaluminate/aluminum oxynitride novel complex phase material.
According to the calcium hexaluminate complex phase material and the preparation method thereof, the performance of the calcium hexaluminate material is improved by introducing AlON, and the compactness and the slag erosion resistance of the calcium hexaluminate material can be greatly improved on the basis of ensuring the chemical stability of the calcium hexaluminate material. Meanwhile, in the process of preparing the calcium hexaluminate complex phase refractory material, aluminum nitride is generated by directly nitriding aluminum powder and serves as a nitrogen source, and a part of aluminum powder serves as a reducing agent, so that the purity of the calcium hexaluminate AlON complex phase material is ensured.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (9)

1. A preparation method of a calcium hexaluminate complex phase material is characterized by comprising the following steps:
aluminum powder, alumina powder and calcium oxide powder are mixed according to the weight ratio of 1: 102-181: 9-16, putting the mixture into a high-energy ball mill for ball milling to obtain mixed powder;
mixing the mixed powder with a binding agent, and performing mechanical pressing to obtain a green body;
and putting the green body into a high-temperature atmosphere furnace, and carrying out carbon-embedding sintering on the green body in a nitrogen atmosphere to obtain the calcium hexaluminate complex-phase material containing calcium hexaluminate/aluminum oxynitride.
2. The method for preparing the calcium hexaluminate complex phase material as claimed in claim 1, wherein the steps of placing the aluminum powder, the alumina powder and the calcium oxide powder into a high energy ball mill for ball milling comprise:
putting aluminum powder, alumina powder and calcium oxide powder into a high-energy ball mill, and adding absolute ethyl alcohol into the high-energy ball mill;
controlling the ball milling speed of the high-energy ball mill at 230-250rpm/min, and drying the mixed slurry after ball milling for 12h to obtain mixed powder.
3. The preparation method of the calcium hexaluminate complex phase material as claimed in claim 2, wherein when the aluminum powder, the alumina powder and the calcium oxide powder are ball-milled, the mass ratio of the balls, the mixed powder and the absolute ethyl alcohol in the high-energy ball mill is 5-7: 0.5-2: 1-3.
4. The method as claimed in claim 1, further comprising, before mixing the mixed powder with a binder: and crushing the mixed powder to enable the particle size of the mixed powder to be smaller than 200 meshes.
5. The method as claimed in claim 1, wherein the sintering temperature is 1700-1750 ℃ during the carbon-embedding sintering of the green body, the green body is kept at the temperature for 1-3h, and then the green body is cooled along with the furnace to obtain the calcium hexaluminate/aluminum oxynitride-containing complex phase material.
6. The method for preparing the calcium hexaluminate complex phase material as claimed in claim 1, wherein the particle size of the alumina powder is 0.5-6 μm.
7. The method for preparing a calcium hexaluminate multiphase material as claimed in claim 1, wherein the particle size of the calcium oxide powder is 0.5-10 μm.
8. The method for preparing a calcium hexaluminate multiphase material as claimed in claim 1, wherein the binder is phenolic resin.
9. A calcium hexaluminate complex phase material comprising a calcium hexaluminate complex phase material prepared by the method for preparing a calcium hexaluminate complex phase material as claimed in any one of claims 1 to 8.
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CN103964871B (en) * 2014-05-05 2015-09-02 武汉科技大学 A kind of calcium hexaluminate-carbon composite powder and preparation method thereof
FR3039538B1 (en) * 2015-07-27 2017-08-25 Kerneos CALCIUM ALUMINATE CEMENT WITH LONG OUVABILITY AND HARDENING PROMOTED BY TEMPERATURE ELEVATION, AND USE THEREOF
CN105152666B (en) * 2015-10-14 2018-07-03 武汉科技大学 A kind of AlON combinations aluminum-carbon refractory material and preparation method thereof
CN107892575B (en) * 2017-11-24 2021-06-29 中钢集团洛阳耐火材料研究院有限公司 Silicon carbide-calcium hexaluminate composite refractory material

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