CN107399959B - Preparation method for reinforcing aluminum oxide-magnesium oxide-calcium oxide composite material by using nano oxide - Google Patents
Preparation method for reinforcing aluminum oxide-magnesium oxide-calcium oxide composite material by using nano oxide Download PDFInfo
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Abstract
A preparation method of an alumina-magnesia-calcium oxide composite material reinforced by nano oxides belongs to the technical field of preparation of refractory materials for clean steel metallurgy. The preparation method comprises the following steps: firstly, using fused corundum, alumina micropowder, light-burned magnesia powder and calcium oxide powder as main raw materials and nano-oxide as an additive, and performing wet ball milling on the raw materials according to an experimental proportion; preparing a biscuit under a certain pressure; and sintering the biscuit in a high-temperature furnace to obtain the alumina-magnesia-calcium oxide composite material. The method is characterized in that the composite material composed of different phases is prepared in one step by adjusting the type and content of the nano oxide and adopting a solid-phase reaction sintering method, so that the method is beneficial to improving the comprehensive performance of the composite material, can reduce the production cost, and has important significance for improving the service performance of composite material parts in clean steel metallurgy.
Description
Technical Field
The invention belongs to the technical field of preparation of refractory materials for clean steel metallurgy, and particularly relates to a preparation method of an alumina-magnesia-calcium oxide composite material reinforced by nano oxides.
Background
In the field of clean steel metallurgy, a ladle argon blowing process is an important link in a ladle refining process, and has the functions of homogenizing the temperature of molten steel and removing impurities. Wherein, the main element in the argon blowing treatment is the air brick. In modern steel-making production, except the air brick for the external refining ladle, the air supply of smelting containers such as an oxygen converter, an electric furnace and the like is completed by the air brick, but the air brick is still the ladle air brick when being used most.
The corundum-spinel refractory material is widely applied to the air brick of the steel ladle, but the service condition of the steel ladle is very harsh, so that the service life of the air brick is very short, generally, the service life is only 20-25 heats, and the service life is greatly shorter than that of other refractory materials in the steel ladle, and the overall service life of the refractory material of the steel ladle is seriously influenced. Therefore, the key to the success of ladle refining is to improve the comprehensive performance of the ladle air brick.
Al2O3the-MgO-CaO series composite material has excellent high temperature resistance, erosion resistance and thermal shock resistance, and is often used as a functional refractory material of a steel ladle air brick, a bottom brick, an impact plate and the like. The nanometer oxide has the characteristics of high specific surface area and high activity, and can be used as an additive to improve the microscopic structure of a product and improve the quality of the product. Al is optimized by adding different kinds and contents of nano oxides2O3The microstructure of the-MgO-CaO series composite material improves the comprehensive performance and has important significance for improving the service performance of the-MgO-CaO series composite material in clean steel metallurgy.
Disclosure of Invention
In order to improve the comprehensive performance of the air brick of the steel ladle, the invention provides a preparation method for enhancing an alumina-magnesia-calcium oxide composite material by utilizing a nano oxide. The method mainly comprises the following steps: firstly, using fused corundum, alumina micropowder, light-burned magnesia powder and calcium oxide powder as main raw materials, using nano oxide as an additive, and performing wet ball milling on the raw materials according to an experimental proportion; preparing a biscuit under a certain pressure; and sintering the biscuit in a high-temperature furnace to obtain the alumina-magnesia-calcium oxide composite material.
The invention relates to a preparation method of an alumina-magnesia-calcium oxide series composite material reinforced by nano oxides, which comprises the following steps:
step 1: ball milling mixing material
(1) According to the experimental proportion, carrying out wet ball milling on raw materials of fused corundum, alumina micro powder, light-burned magnesia powder, calcium oxide powder and nano oxide;
(2) fully drying the ball-milled raw materials;
step 2: shaping and drying
Applying certain pressure to prepare a biscuit, and fully drying;
and step 3: high temperature sintering
And sintering the biscuit in a high-temperature furnace to obtain the alumina-magnesia-calcium oxide composite material.
In the step 1(1), the nano oxide is ZrO2、TiO2、MnO2One of (1);
the CaO is a main raw material and is also a stabilizer of the nano oxide;
the main raw materials comprise 20 to 50 to 20 mass percent of fused corundum particles, 50 to 20 mass percent of alumina micro powder and light-burned magnesia powder;
among the raw materials, fused corundum particles: alumina micropowder: light-burned magnesia powder: when the mass ratio of the calcium oxide powder to the nano oxide is 20 percent to 50 percent to 20 percent to 10 percent, the molar ratio of calcium oxide/(calcium oxide and nano oxide) is 5 to 80mol percent;
when the mass of the fused corundum particles, the alumina micro powder, the light-burned magnesia powder and the calcium oxide powder is fixed, the mass fraction of the additive nano oxide is 0-15%;
in the wet ball milling, absolute ethyl alcohol and deionized water are preferably added;
the ball milling equipment is a planetary ball mill with the speed of 300 r.min-1The rotating speed runs for 3 hours in a single direction;
in the step 1(2), the drying temperature is 120 ℃, and the drying time is 12-24 hours;
in the step 2, the forming pressure of the biscuit is 50-400 MPa;
in the step 2, the biscuit is molded by one of compression molding and isostatic pressing;
in the step 2, the drying temperature is 120 ℃, and the drying time is 12-24 hours;
in the step 3, the high-temperature furnace is one of a box type resistance furnace, a tubular resistance furnace and a tunnel kiln;
in the step 3, the high-temperature sintering temperature is 1450-1700 ℃, and the heat preservation time is 2-10 h.
The invention has the beneficial effects that:
1. the preparation method of the alumina-magnesia-calcium oxide composite material reinforced by the nano oxide improves the comprehensive performance of the refractory material of the air brick of the steel ladle, and is beneficial to improving the metallurgical effect of clean steel and prolonging the service life of metallurgical parts.
2. The preparation method of the nano-oxide reinforced alumina-magnesia-calcium oxide composite material takes the fused corundum, the alumina micro powder, the light-burned magnesia powder and the calcium oxide powder as main raw materials, and the raw materials are cheap and easy to obtain, so that the production cost of the product is easy to reduce.
3. The invention relates to a method for preparing an alumina-magnesia-calcium oxide composite material reinforced by nano oxides, which can prepare composite materials with different phase compositions and excellent performance by adjusting the types and the contents of additive nano oxides and adopting a solid-phase reaction sintering method.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, the starting materials are commercially available unless otherwise indicated.
In the following examples, a process flow chart of a preparation method of a nano-oxide reinforced alumina-magnesia-calcia-based composite material is shown in fig. 1.
Example 1
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano oxides comprises the following steps:
step 1: ball milling mixing material
(1) According to the proportion of the fused corundum: alumina micropowder: light-burned magnesia powder: (calcium oxide powder + Nano ZrO)2) Mixing 20 percent to 50 percent to 20 percent to 10 percent, and wet ball milling, wherein CaO/(CaO + ZrO)2) Selecting the molar ratio to be 60 mol%;
(2) drying the ball-milled raw materials at 120 ℃ for 12 h;
step 2: dry pressing and drying
Preparing a columnar sample with the diameter of 15mm multiplied by 12mm under the pressure of 200MPa, and drying for 12 hours at the temperature of 120 ℃;
and step 3: high temperature sintering
Placing the columnar sample with the diameter of 15mm multiplied by 12mm in a high-temperature furnace, and preserving the heat for 2 hours at 1450 ℃ to obtain the alumina-magnesia-calcium oxide composite material.
The detection shows that the main crystal phase of the obtained alumina-magnesia-calcia composite material is MgAl2O4With m-ZrO2，CaAl4O7Is the main component Al in the raw material2O3Formed by reaction with CaO.
Example 2
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano-oxide, which is the same as example 1, except that the high-temperature sintering temperature is 1500 ℃.
The obtained alumina-magnesia-calcia series composite material has a new phase of c-ZrO after detection2Formation of, at the same time, m-ZrO2Disappearance of CaAl4O7The diffraction intensity of (2) is reduced; the main crystal phase is MgAl2O4And c-ZrO2。CaAl4O7Is the main component Al in the raw material2O3Formed by reaction with CaO.
Example 3
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano-oxide, which is the same as example 1, except that the high-temperature sintering temperature is 1550 ℃.
The MgAl in the obtained alumina-magnesia-calcia series composite material sample is detected2O4The diffraction intensity is further enhanced, and the main crystal phase of the material is MgAl2O4And c-ZrO2Also, a small amount of MgO and CaAl is present4O7And Al2O3And (4) phase(s). MgAl2O4Is the main component Al in the raw material2O3And reacting with MgO.
Example 4
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano-oxide, which is the same as the preparation method of the alumina-magnesia-calcia-based composite material in example 1, and is characterized in that:
(1)nCaO/n(CaO+ZrO2) 20 mol% of the total amount.
(2) In step 3, the sintering temperature is 1500 ℃.
The t-ZrO of the obtained alumina-magnesia-calcia composite material sample is detected2m-ZrO of2The strength of (2) is reduced; at the same time, a new phase CaAl appears4O7Description of part of CaO and Al in the sample2O3A reaction takes place.
Example 5
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano-oxide, which is the same as the preparation method of the alumina-magnesia-calcia-based composite material in example 1, and is characterized in that:
(1)nCaO/n(CaO+ZrO2) Is 40 mol%.
(2) In step 3, the sintering temperature is 1500 ℃.
The obtained alumina-magnesia-calcia composite material sample is detected to have a new phase of c-ZrO2Formation of, at the same time, t-ZrO2Disappearance, m-ZrO2The strength of which is reduced, and whose main crystal phase is MgAl2O4And c-ZrO2. Description of MgO and Al in the sample2O3A reaction takes place.
Example 6
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano-oxide, which is the same as the preparation method of the alumina-magnesia-calcia-based composite material in example 1, and is characterized in that:
(1)nCaO/n(CaO+ZrO2) The molar percentage was 60 mol%.
(2) In step 3, the sintering temperature is 1500 ℃.
The m-ZrO of the obtained alumina-magnesia-calcia composite material sample is detected2Disappear, its main crystal phase is MgAl2O4And c-ZrO2A small amount of MgO and CaAl still exist4O7And Al2O3And (4) phase(s).
Example 7
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano-oxide, which is the same as the preparation method of the alumina-magnesia-calcia-based composite material in example 1, and is characterized in that:
(1) when the mass fractions of the matrix raw material and the calcium oxide are fixed, nano ZrO is added2Is 0.
(2) In the step 3, the sintering temperature is 1580 ℃, and the temperature is kept for 4 hours.
The phase composition of the obtained alumina-magnesia-calcia composite material is MgAl through detection2O4With CaAl2SiO7Two phases. Ca2Al2SiO7Is made of Al in the sample2O3CaO component and SiO in the raw material2Compounds formed by impurities; the particles of the sample are irregular round, and have an average particle size of about 5 μm, a maximum particle diameter of about 10 μm, and a minimum particle diameter of about 1 to 2 μm. Apparent porosity and volume density were 1.12% and 3.15 g.cm, respectively-3(ii) a The normal temperature compressive strength is 140 MPa;
example 8
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano-oxide, which is the same as the preparation method of the alumina-magnesia-calcia-based composite material in example 1, and is characterized in that:
(1) when the mass fractions of the matrix raw material and the calcium oxide are fixed, nano ZrO is added2The mass fraction of (2.5%).
(2) In the step 3, the sintering temperature is 1580 ℃, and the temperature is kept for 4 hours.
The detection shows that the new phase c-ZrO appears in the obtained alumina-magnesia-calcia series composite material sample2(Ca0.15Zr0.85O1.85) And CaO. Al2O3The former is composed of CaO and ZrO in the raw material2Form a solid solution of Al in the raw material2O3Reaction sintered product with CaO. The particles of the sample became more regular, prismatic and their particle size was significantly reduced, with an average particle size of about 2 μm; the apparent porosity and the volume density were 0.99% and 3.20 g.cm, respectively-3(ii) a The normal temperature compressive strength is 188 MPa;
example 9
A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano-oxide, which is the same as the preparation method of the alumina-magnesia-calcia-based composite material in example 1, and is characterized in that:
(1) when the mass fractions of the matrix raw material and the calcium oxide are fixed, nano ZrO is added2Is 7.5 percent.
(2) In the step 3, the sintering temperature is 1580 ℃, and the temperature is kept for 4 hours.
The detection shows that the new phase m-ZrO appears in the obtained alumina-magnesia-calcia series composite material sample2And CaO. Al2O3. The microscopic appearance of the sample is better than that of the sample without adding ZrO2The sample of (1). With addition of ZrO2Is beneficial to inhibiting the growth of magnesia-alumina spinel particles; the apparent porosity and the volume density of the prepared composite material are respectively 1.26 percent and 3.23 g.cm-3(ii) a The normal temperature compressive strength is 236 MPa.
Claims (4)
1. A method for preparing an alumina-magnesia-calcia-based composite material reinforced by nano oxides is characterized by comprising the following steps:
step 1: ball milling mixing material
(1) Wet ball milling the fused corundum, the alumina micro powder, the light-burned magnesia powder, the calcium oxide powder and the nano oxide; electrically melting corundum particles: alumina micropowder: light-burned magnesia powder: the mass ratio of (calcium oxide powder and nano oxide) is 20 percent to 50 percent to 20 percent to 10 percent, and the molar ratio of calcium oxide/(calcium oxide and nano oxide) is 5mol percent to 80mol percent;
(2) fully drying the ball-milled raw materials;
step 2: dry pressing, forming and drying, applying certain pressure to prepare a biscuit, and fully drying; the forming pressure of the biscuit is 50-400 MPa;
and step 3: high temperature sintering
Sintering the biscuit in a high-temperature furnace to obtain an alumina-magnesia-calcia composite material;
the nano oxide is ZrO2、TiO2、MnO2One of (1);
in the step 1(2), the drying temperature is 120 ℃, and the drying time is 12-24 hours; in the step 2, the drying temperature is 120 ℃, and the drying time is 12-24 hours;
in the step 2, the biscuit is molded by one of compression molding and isostatic pressing;
in the step 3, the high-temperature furnace is one of a box type resistance furnace, a tubular resistance furnace and a tunnel kiln;
in the step 3, the high-temperature sintering temperature is 1450-1700 ℃, and the heat preservation time is 2-10 h.
2. The method according to claim 1, wherein in step 1(1), when the mass of the fused corundum particles, the alumina micropowder, the light-burned magnesia powder and the calcium oxide powder is fixed, the mass fraction of the nano oxide of the additive is 0-15%.
3. The method of claim 2, wherein in step 1(1), absolute ethanol and deionized water are added during the wet ball milling.
4. The method of claim 3, wherein in step 1(1), the ball milling device is a planetary ball mill operated at 300 r-min-1The rotating speed runs for 3 hours in a single direction.
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| CN107399959A (en) | 2017-11-28 |
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