CN111908929A - Based on N3-Preparation of CA with excellent slag resistance by ion doping6Method for producing a refractory base material - Google Patents
Based on N3-Preparation of CA with excellent slag resistance by ion doping6Method for producing a refractory base material Download PDFInfo
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- CN111908929A CN111908929A CN202010578051.8A CN202010578051A CN111908929A CN 111908929 A CN111908929 A CN 111908929A CN 202010578051 A CN202010578051 A CN 202010578051A CN 111908929 A CN111908929 A CN 111908929A
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Abstract
The invention discloses a nitrogen ion (N) -based catalyst3‑) Doping preparation of calcium hexaluminate (CA) with excellent slag resistance6) A method of making a refractory-based feedstock, the method comprising: carrying out high-temperature heat treatment on the alumina powder and the calcium oxide powder to remove surface adsorbed water and bound water; putting metal aluminum powder, alumina powder and calcium oxide powder into a high-energy ball mill for ball milling to obtain mixed powder; crushing and screening the mixed powder, and performing mechanical pressing to obtain a green body; placing the green body in a high temperature atmosphere furnace at N2Under the atmosphere, the green body is subjected to carbon-embedding sintering to obtain N3‑Ion-doped CA6A material. The invention introduces N3‑Ion regulated CA6Can be used without destroying CA6On the basis of crystal form, increase CA6The length of the c axis of the unit cell enables the thickness of the material to be thicker, the density to be greatly improved and the slag erosion resistance to be excellent. Simultaneously, in the preparation of N3‑Ion-doped CA6Preparation of refractory raw materialIn the process, the site of occurrence of N-doping is determined.
Description
Technical Field
The invention belongs to the technical field of inorganic non-metallic materials, and particularly relates to N3-Ion-doped CA6Materials and methods for their preparation.
Background
In the field of refractories for ferrous metallurgy, calcium hexaluminate (CA)6) Mainly exists in the form of reaction products, is formed by the reaction of aluminate cement combined with corundum or corundum-spinel during the high-temperature use process, and is inserted between a corundum phase and a spinel phase. Due to CA6The material has the characteristics of high melting point, high stability, excellent slag resistance and the like, so that the mechanical property and the slag corrosion resistance of the material are obviously improved.
Based on the data display, CA6The cells are composed of spinel blocks and mirror layers, which are alternately stacked to form a layered structure, each cell being composed of two spinel blocks and two mirror layers in which the mirror layer structure is loosened due to the support of large cations. Thus in CA6In the structure of (1), oxygen ions are more easily diffused in the direction perpendicular to the c-axis, and the spinel-based block units in the c-axis direction are separated by the mirror layer, so that the growth of crystals in the c-axis direction is suppressed, and therefore, the diffusion efficiency of ions in the c-axis direction is relatively low, which also results in CA6Plain Al2O3Like the oxides, the higher bulk density is easily achieved by elevated temperatures, and reaction-sintered CA is difficult to achieve even at sintering temperatures up to 1750 deg.C6The full density of (c). The relatively porous structure facilitates slag penetration into the refractory matrix, which limits CA to a large extent6The method is applied to the fields of metallurgy and petrifaction.
In addition, nitride-based materials have characteristics of high melting point and poor wettability with molten metals and oxides, and bond length of tetrahedral Al — N bond (AlN is, in AlN, Al — N bond)
) Almost equivalent to tetrahedral Al-O bond (CA)6In is
). Thus, if doped N is used3-Ion in place of O2-For increasing CA6The compactness and corrosion resistance of (a) seem to be a viable option.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides N3-Ion-doped CA6Materials and methods for their preparation.
In one aspect of the invention, N is3-Ion-doped CA6A method of preparing a material comprising:
performing ball milling on metal aluminum powder, alumina powder and calcium oxide powder to obtain mixed powder; the ball milling of the metal aluminum powder, the alumina powder and the calcium oxide powder comprises the following steps: respectively carrying out high-temperature heat treatment on the alumina powder and the calcium oxide powder; putting the treated alumina, calcium oxide powder and metal aluminum powder into a high-energy ball mill, and adding absolute ethyl alcohol into the high-energy ball mill; after ball milling, drying the slurry obtained by mixing to obtain mixed powder;
crushing and screening the mixed powder, and then performing mechanical pressing to obtain a green body;
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 N3-Ion-doped CA6A material.
Further, when the metal 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:
respectively keeping the temperature of the alumina powder and the calcium oxide powder at 700-900 ℃ for 0.5-2h, and carrying out high-temperature heat treatment to remove surface adsorbed water, bound water and the like.
Mixing the treated alumina powder, the treated calcium oxide powder and the metal aluminum powder according to the weight ratio of (75-225): (7-21): 1, putting the mixture into a ball mill, and adding absolute ethyl alcohol into a high-energy ball mill;
controlling the ball milling speed of the high-energy ball mill at 200-250rpm/min, ball milling for 12-24h, and drying the mixed slurry 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 the balls, the mixed powder and the absolute ethyl alcohol in the high-energy ball mill is (5-6): (1-2): (1-2).
Further, before pressing the mixed powder into a blank, the method further comprises the following steps: 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-embedding sintering, the sintering temperature is 1650-1750 ℃, the temperature is kept at the temperature for 2-3h, and then the green body is cooled along with the furnace to obtain N3-Ion-doped CA6A material.
Further, the particle size of the alumina powder is 2-6 μm.
Furthermore, the particle size of the calcium oxide powder is 2-10 μm.
In another aspect of the invention, N is3-Ion-doped CA6Material comprising a compound of N as described above3-Ion-doped CA6Preparation method of (2)3-Ion-doped CA6A material.
The invention provides N3-Ion-doped CA6And a process for the preparation thereof by introducing N3-To improve CA6The performance of the material can be ensured in the process of CA6On the basis of the chemical stability of the material, CA is regulated and controlled6The crystal structure of (2) can greatly improve the material density. Simultaneously, in the preparation of N3-Ion-doped CA6During the process of refractory raw materials, the optimal N doping site is determined. In summary, the present invention provides N3-Ion-doped CA6The preparation method of the material is simple to operate, has low equipment requirement, does not pollute the environment, and simultaneously, the prepared N3-Ion-doped CA6The material has the advantages of thicker crystal thickness, high density, stable structure in the sintering process, excellent slag erosion resistance and the like.
Drawings
FIG. 1 is a schematic diagram of an embodiment of the present inventionN3-Ion-doped CA6A process flow diagram of a method of preparing a material;
FIG. 2 shows an embodiment of the present invention with reference to the drawing3-Ion-doped CA6XRD pattern of refractory material prepared by preparation method of material (Explanation N)3-Ions having entered CA6Among the crystal lattices of (1);
FIG. 3 shows an embodiment of the present invention with reference to the drawing3-Ion-doped CA6SEM image of the refractory material prepared by the preparation method (N can be seen)3-Ion-doped CA6The structure of the material is compact);
FIG. 4 shows an embodiment of the present invention with reference to the drawing3-Ion-doped CA6SEM scanning results of the refractory prepared by the preparation method (N can be seen)3-Has been successfully doped with CA6In (1);
FIG. 5 shows an embodiment of the present invention with reference to the drawing3-Ion-doped CA6Sectional view of crucible after LF refining slag invasion of refractory material prepared by the preparation method of the material (N can be seen)3-Ion-doped CA6Slag resistance pure CA6Strong);
FIG. 6 shows N calculated by the first principle of the law3-Ion-doped CA6Most stable crystal structure (indicating that the preferential doping site for N is the O (3) site);
FIG. 7 shows a diagram of N according to the present invention3-Ion-doped CA6The XRD fine modification pattern of the refractory material prepared by the preparation method of the material;
FIG. 8 shows a diagram of N according to the present invention3-Ion-doped CA6XRD refinement of atomic site occupancy information for refractory materials made by the material preparation process (indicating that N doping occurs at the O (3) site and vacancies should form at the O (1) and O (5) sites to maintain overall charge balance);
FIG. 9 shows a diagram of a method for generating N according to the present invention3-Ion-doped CA6Preparation of the Material the cell parameters of the refractory obtained from the preparation of the Material (specification of CA after N doping)6The unit cell c-axis length is increased).
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.
One aspect of the present invention provides a method for producing N3-Ion-doped CA6The preparation method of the material, which is shown in figure 1, comprises the following steps:
s100, mixing the aluminum oxide and calcium oxide powder subjected to high-temperature heat treatment and the metal aluminum powder according to the weight ratio of (75-225): (7-21): 1, putting the mixture into a ball mill, adding absolute ethyl alcohol into a high-energy ball mill, controlling the ball milling rotating speed at 200-250rpm/min, carrying out ball milling for 12-24h, and drying the mixed slurry to obtain mixed powder;
s200, crushing the mixed powder to enable the particle size of the mixed powder to be smaller than 200 meshes, and performing mechanical pressing 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 under the nitrogen atmosphere, wherein the sintering temperature is 1650-1750 ℃, preserving heat for 1-3h at the temperature, and then cooling the green body along with the furnace to obtain N3-Ion-doped CA6A material. Referring to FIG. 2, by analyzing the XRD pattern of the refractory material prepared by the present invention, it can be seen that N is present3-Ion-doped CA6There are no other impurities.
As a preferred embodiment, when aluminum powder, alumina powder and calcium oxide powder are subjected to ball milling, the mass ratio of the balls, the mixed powder and the absolute ethyl alcohol in the high-energy ball mill is (5-6): (1-2): (1-2).
As a preferred embodiment, the particle size of the alumina powder is 2 to 6 μm. In the embodiment, the raw material of the alpha-alumina powder is ball milled for 12 to 24 hours to obtain alpha-alumina powder slurry with the particle size of 2 to 8 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 2 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.
Another aspect of the invention provides a3-Ion-doped CA6Material comprising a compound of N as defined above3-Ion-doped CA6Preparation method of material prepared from N3-Ion-doped CA6A material.
Referring to FIG. 3, it can be seen that the present invention combines N3-Doping to CA6In the unit cell, CA is increased6And (5) compactness of the material.
Referring to FIG. 5, it can be seen that by introducing N element to CA6In addition, the slag resistance can be improved.
The invention successfully synthesizes N under a certain low oxygen pressure nitrogen atmosphere by taking fine powder of aluminum oxide and calcium oxide as raw materials and adding metal aluminum powder3-Ion-doped CA6Novel material having N element introduced into CA6In the material, CA is further increased6Length of c-axis of unit cell, not only can match CA6The thickness of the material is increased, and the compactness and the slag erosion resistance of the material are greatly improved. Simultaneously, in the preparation of N3-Ion-doped CA6In the course of refractory raw material, CA is determined6The material is doped with N generation sites.
Example 1
N3-Ion-doped CA6A method of preparing a material comprising:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 24 hours to obtain alpha-alumina powder slurry with the average particle size of 3 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 average 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 oxide powder to the calcium oxide powder to the metal aluminum powder is 77: 7: 1, ball milling rotation speed 240rpm/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: pressing the mixed material into a cylinder with the size of phi 25mm under 6 MPa;
(5) sintering and synthesizing: putting the green body into a high-temperature atmosphere furnace, burying carbon, controlling the temperature of 1700 ℃ under a certain nitrogen atmosphere for 3 hours, and then cooling along with the furnace to obtain the high-performance N3-Ion-doped CA6Novel materials.
Example 2
N3-Ion-doped CA6A method of preparing a material comprising:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 16h to obtain alpha-alumina powder slurry with the average 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 average 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 weight ratio of the aluminum oxide powder to the calcium oxide powder to the aluminum powder is 111: 10: 1, ball milling rotation speed of 230rpm/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: pressing the mixed material into a cylinder with the size of phi 25mm under 6 MPa;
(5) sintering and synthesizing: placing the green bodyPutting the mixture into a high-temperature atmosphere furnace, burying carbon, keeping the temperature at 1750 ℃ for 1.5h under a certain nitrogen atmosphere, and then cooling the mixture along with the furnace to obtain the high-performance N3-Ion-doped CA6Novel materials.
Example 3
N3-Ion-doped CA6A method of preparing a material comprising:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 16h to obtain alpha-alumina powder slurry with the average particle size of 3 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 alumina 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 24 hours to uniformly mix the raw materials, wherein the weight ratio of the alumina to the calcium oxide powder to the metal aluminum powder is 225: 21: 1, ball milling rotation speed 240rpm/min, ball: mixing powder: the mass ratio of the absolute ethyl alcohol is 5: 2: 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: pressing the mixed material into a cylinder with the size of phi 25mm under 6 MPa;
(5) sintering and synthesizing: placing the green body into a high-temperature atmosphere furnace, burying carbon, controlling the temperature of 1650 ℃ for 3h under a certain nitrogen atmosphere, and then cooling along with the furnace to obtain high-performance N3-Ion-doped CA6Novel materials.
Example 4
N3-Ion-doped CA6A method of preparing a material comprising:
(1) raw material treatment: ball-milling the alpha-alumina powder raw material for 36h to obtain alpha-alumina powder slurry with the average 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 average 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 18 hours to uniformly mix the raw materials, wherein the weight ratio of the aluminum oxide powder to the calcium oxide powder to the aluminum powder is 111: 10: 1, ball milling rotation speed of 250rpm/min, ball: mixing powder: the mass ratio of the absolute ethyl alcohol is 6: 1: 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: pressing the mixed material into a cylinder with the size of phi 25mm under 6 MPa;
(5) sintering and synthesizing: putting 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 N3-Ion-doped CA6Novel materials.
Example 5
N3-Ion-doped CA6A method of preparing a material comprising:
(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 3 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 alumina powder 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 24 hours to uniformly mix the raw materials, wherein the weight ratio of the alumina powder to the calcium oxide powder to the metal aluminum powder is 83: 8: 1, ball milling rotation speed of 250rpm/min, ball: mixing powder: the mass ratio of the absolute ethyl alcohol is 5: 2: 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: pressing the mixed material into a cylinder with the size of phi 25mm under 8MPa
(5) Sintering and synthesizing: placing the green body into a high-temperature atmosphere furnace, burying carbon, controlling the temperature to be 1680 ℃ for 3 hours under a certain nitrogen atmosphere, and then cooling along with the furnace to obtain the high-performance N3-Ion-doped CA6Novel materials.
The invention successfully synthesizes N under a certain low oxygen pressure nitrogen atmosphere by taking fine powder of aluminum oxide and calcium oxide as raw materials and adding metal aluminum powder3-Ion-doped CA6Novel refractory raw material, introducing N element into CA6In the material, CA is further increased6Length of c-axis of unit cell, not only can match CA6The thickness of the material is increased, and the compactness and the slag erosion resistance of the material are greatly improved. Simultaneously, in the preparation of N3-Ion-doped CA6In the process of the refractory raw material, the N-doped occurrence site is determined. In summary, the present invention provides N3-Ion-doped CA6The preparation method of the material is simple to operate, has low equipment requirement, does not pollute the environment, and prepares the N3-Ion-doped CA6The material has the advantages of high density, stable structure in the sintering process, excellent slag erosion resistance and the like.
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 (8)
1. Based on N3-Preparation of CA with excellent slag resistance by ion doping6A method of refractory-based feedstock, comprising:
performing ball milling on metal aluminum powder, alumina powder and calcium oxide powder to obtain mixed powder; the ball milling of the metal aluminum powder, the alumina powder and the calcium oxide powder comprises the following steps: respectively carrying out high-temperature heat treatment on the alumina powder and the calcium oxide powder; putting the treated alumina, calcium oxide powder and metal aluminum powder into a high-energy ball mill, and adding absolute ethyl alcohol into the high-energy ball mill; after ball milling, drying the slurry obtained by mixing to obtain mixed powder;
crushing and screening the mixed powder, and performing mechanical pressing to obtain a green body;
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 N3-Ion-doped CA6A refractory raw material.
2. The method of claim 1, wherein ball milling the metallic aluminum powder, the alumina powder, and the calcium oxide powder further comprises:
respectively keeping the temperature of the alumina powder and the calcium oxide powder at 700-900 ℃ for 0.5-2h, and performing high-temperature heat treatment to remove surface adsorbed water and bound water;
mixing the treated alumina powder, the treated calcium oxide powder and the metal aluminum powder according to the weight ratio of (75-225): (7-21): 1, putting the mixture into a ball mill, and adding absolute ethyl alcohol into a high-energy ball mill;
controlling the ball milling speed of the high-energy ball mill at 200-250rpm/min, ball milling for 12-24h, and drying the mixed slurry to obtain mixed powder.
3. The method according to 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 (5-6): (1-2): (1-2).
4. The method of claim 1, further comprising, prior to the mechanically compacting the mixed powder: and crushing the mixed powder to enable the particle size of the mixed powder to be smaller than 200 meshes.
5. According to claim 1The method is characterized in that when the green body is subjected to carbon burying sintering, the sintering temperature is 1650-1750 ℃, the temperature is kept at the temperature for 1-3h, and then the green body is cooled along with a furnace to obtain N3-Ion-doped CA6A material.
6. The method of claim 1, wherein the alumina powder has a particle size of 2-6 μm.
7. The method according to claim 1, characterized in that the calcium oxide powder has a particle size of 2-10 μm.
8. N3-Ion-doped CA6Material comprising a N according to any one of claims 1 to 73-Ion-doped CA6N prepared by preparation method of base refractory raw material3-Ion-doped CA6A material.
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Citations (3)
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|---|---|---|---|---|
| CN102731109A (en) * | 2012-06-16 | 2012-10-17 | 山东科技大学 | AlON material synthetic method |
| CN103964871A (en) * | 2014-05-05 | 2014-08-06 | 武汉科技大学 | Calcium hexaluminate-carbon composite powder and preparation method thereof |
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2020
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| CN102731109A (en) * | 2012-06-16 | 2012-10-17 | 山东科技大学 | AlON material synthetic method |
| CN103964871A (en) * | 2014-05-05 | 2014-08-06 | 武汉科技大学 | Calcium hexaluminate-carbon composite powder and preparation method thereof |
| 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 |
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