CN104311116A - Magnesium aluminate spinel foam ceramic and preparation method thereof - Google Patents
Magnesium aluminate spinel foam ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to magnesium aluminate spinel foam ceramic and a preparation method thereof. According to the technical scheme, the preparation method comprises the following steps: mixing aluminum oxide fine powder and magnesite fine powder in a mass ratio of (2.4-2.7): 1 as raw materials; then, mixing sugar with the raw materials in a mass ratio of 1: (0.6-1.8); then, adding 0.1-0.5wt% of sintering aids and 0.1-0.5wt% of an AC foaming agent into the mixture, and mixing to obtain mixed powder; raising the temperature of the mixed powder to 100-200 DEG C and insulating for 1-3 hours to obtain a dispersing system of the mixed powder which is dispersed in a sugar solution, and then placing the dispersing system in an incubator to foam and cure for 8-25 hours; and finally, raising the temperature of the cured blank to 1500-1700 DEG C and insulating for 3-9 hours to obtain the magnesium aluminate spinel foam ceramic. The magnesium aluminate spinel foam ceramic provided by the invention is simple in process and environment-friendly. The prepared magnesium aluminate spinel foam ceramic is free of cracks, low in volume density, high in through hole rate and great in strength.
Description
Technical field
The invention belongs to foamed ceramics technical field.Be specifically related to a kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.
Background technology
The development of foamed ceramics starts from 20 century 70s, and it is a kind of porous ceramic articles with 3 D stereo network skeleton and mutual through air hole structure.Foamed ceramics has the premium propertiess such as void content is high, high temperature resistant, resist chemical, Heat stability is good, is widely used as the aspects such as molten metal strainer, high-temperature gas exchange filter, ion-exchange filter and support of the catalyst.
Magnesium-aluminium spinel (MgAl
2o
4) there is fusing point high (2135 DEG C), the series of advantages such as thermal expansivity is low, thermal conductivity good and high-temperature stability is strong.Magnesium-aluminium spinel foamed ceramics is the multiduty lightweight refractory such as a kind of important metallurgical industry heat insulating refractory material and metallurgical industry filtration.
At present, magnesium-aluminium spinel foamed ceramics mainly adopts hanging preparation technology, and foam sponge is immersed in ceramic size, then removes unnecessary slurry by extruding, then obtains foamed ceramics through super-dry, sintering.As the patented technology of " a kind of magnesium-aluminium spinel foam ceramic filter and preparation method thereof " (CN201310539992.0), though this technology has certain advantage, but still there is following shortcoming: (1) basic craft course comprises slurrying, hanging, drying, sintering etc., complicated process of preparation; (2) intensity of foamed ceramics is not high; (3) goods have fine cracks even to ftracture; (4) toxic gas is produced in the sintering stage, contaminate environment.
The preparation method of magnesium-aluminium spinel foamed ceramics also has gel injection method and foaming process etc.As the patented technology of " a kind of method preparing lightweight magnesium-aluminum spinel lagging material " (CN201210123564.5), though this technology adopts the method for foaming process attached gel casting to have certain advantage, but also there is following shortcoming: (1) has certain toxicity due to organic monomer, initiator and the catalyzer used, to HUMAN HEALTH and environment unfavorable; (2) owing to using the one in the gelling system of Methacrylamide, acrylamide and vinyl pyrrole ketone, improve cost, limit promoting the use of of product.
Summary of the invention
The object of the invention is to provide the preparation method of the simple and eco-friendly magnesium-aluminium spinel foamed ceramics of a kind of technique; The magnesium-aluminium spinel foamed ceramics flawless prepared by the method, volume density is low, through-hole rate is high and intensity is large.
For achieving the above object, the technical solution used in the present invention is: the step of described preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.4 ~ 2.7) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (0.6 ~ 1.8).
Step 3, in compound, add the sintering agent of described compound 0.1 ~ 0.5wt% and the AC whipping agent of 0.1 ~ 0.5wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 100 ~ 200 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 8 ~ 25h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1500 ~ 1700 DEG C, insulation 3 ~ 9h, obtain magnesium-aluminium spinel foamed ceramics.
Described aluminum oxide fine powder is commercial alumina fine powder, α-Al
2o
3one in fine powder, white fused alumina fine powder, Brown Alundum fine powder, compact alumina fine powder and plate diamond spar fine powder, the particle diameter of described aluminum oxide fine powder is less than 44 μm.
Described magnesia powder is electrosmelted magnesite clinker fine powder or is magnesite clinker fine powder, and the particle diameter of described magnesia powder is less than 44 μm.
Described sugar is the one in fructose, sucrose, glucose and maltose, and the purity of described sugar is greater than 99.0wt%.
The temperature of described thermostat container is 120 ~ 180 DEG C.
Described sintering agent is B
2o
3micro mist, BC
4micro mist, MgF
2micro mist and AlF
3one or both in micro mist.
Owing to adopting technique scheme, the advantage that the present invention compared with prior art has and positively effect:
1, the present invention is due to aluminum oxide fine powder and the wetting ability interaction between magnesia powder surface and glycan molecule-OH, powder can comparatively be evenly dispersed in the sugared liquation of melting, the dispersion system uniform composition of gained, can not crack due to powder skewness when burning till.
2, the present invention is using sugar as whipping agent, the water vapor that between-OH of glycan molecule, condensation produces is utilized to foam, the bubble produced is adsorbed on liquid-gas interface and dispersion system viscosity increase by fine particle is stablized, be conducive to forming uniform pore, the interconnective cellular microstructure of final formation, has higher through-hole rate and intensity.
3, present invention process is simple, and without noxious gas emission in whole preparation process, is beneficial to environment protection.
The volume density of the magnesium-aluminium spinel foamed ceramics 4, obtained by the present invention is 0.12 ~ 0.54g/cm
3, compressive strength reaches 2.50 ~ 10.2Mpa, and apparent porosity is 85% ~ 97%.
Therefore, the present invention has the simple and eco-friendly feature of technique; Prepared magnesium-aluminium spinel foamed ceramics flawless, volume density is low, through-hole rate is high and intensity is large.
Embodiment
Below in conjunction with embodiment, the invention will be further described, the restriction not to its protection domain.
For avoiding repetition, the existing technical parameter Unify legislation this embodiment related to is as follows, repeats no more in embodiment:
The particle diameter of described aluminum oxide fine powder is less than 44 μm.
The particle diameter of described magnesia powder is less than 44 μm.
The purity of described sugar is greater than 99.0wt%.
embodiment 1
A kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.Described in the present embodiment, the step of preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.4 ~ 2.55) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (0.6 ~ 0.8).
Step 3, in compound, add the sintering agent of described compound 0.1 ~ 0.3wt% and the AC whipping agent of 0.1 ~ 0.3wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 100 ~ 120 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 8 ~ 15h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1500 ~ 1600 DEG C, insulation 3 ~ 5h, obtain magnesium-aluminium spinel foamed ceramics.
In the present embodiment: described aluminum oxide fine powder is commercial alumina fine powder; Described magnesia powder is electrosmelted magnesite clinker fine powder; Described sugar is fructose; Described sintering agent is B
2o
3micro mist; The temperature of described thermostat container is 120 ~ 150 DEG C.
The volume density of the magnesium-aluminium spinel foamed ceramics obtained by the present embodiment is 0.12 ~ 0.20g/cm
3, compressive strength reaches 2.50 ~ 4.00Mpa, and apparent porosity is 93% ~ 97%.
embodiment 2
A kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.Described in the present embodiment, the step of preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.4 ~ 2.55) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (0.8 ~ 1.0).
Step 3, in compound, add the sintering agent of described compound 0.1 ~ 0.3wt% and the AC whipping agent of 0.3 ~ 0.5wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 180 ~ 200 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 15 ~ 25h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1500 ~ 1600 DEG C, insulation 3 ~ 5h, obtain magnesium-aluminium spinel foamed ceramics.
In the present embodiment: described aluminum oxide fine powder is α-Al
2o
3fine powder; Described magnesia powder is magnesite clinker fine powder; Described sugar is sucrose; Described sintering agent is BC
4micro mist; The temperature of described thermostat container is 150 ~ 180 DEG C.
The volume density of the magnesium-aluminium spinel foamed ceramics obtained by the present embodiment is 0.18 ~ 0.30g/cm
3, compressive strength reaches 3.60 ~ 6.10Mpa, and apparent porosity is 92% ~ 95%.
embodiment 3
A kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.Described in the present embodiment, the step of preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.4 ~ 2.55) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (1.0 ~ 1.2).
Step 3, in compound, add the sintering agent of described compound 0.1 ~ 0.3wt% and the AC whipping agent of 0.1 ~ 0.3wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 150 ~ 180 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 8 ~ 15h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1500 ~ 1600 DEG C, insulation 5 ~ 7h, obtain magnesium-aluminium spinel foamed ceramics.
In the present embodiment: described aluminum oxide fine powder is white fused alumina fine powder; Described magnesia powder is electrosmelted magnesite clinker fine powder; Described sugar is glucose; Described sintering agent is MgF
2micro mist; The temperature of described thermostat container is 150 ~ 180 DEG C.
The volume density of the magnesium-aluminium spinel foamed ceramics obtained by the present embodiment is 0.22 ~ 0.36g/cm
3, compressive strength reaches 3.85 ~ 6.80Mpa, and apparent porosity is 90% ~ 94%.
embodiment 4
A kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.Described in the present embodiment, the step of preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.4 ~ 2.55) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (1.2 ~ 1.4).
Step 3, in compound, add the sintering agent of described compound 0.3 ~ 0.5wt% and the AC whipping agent of 0.3 ~ 0.5wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 120 ~ 150 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 8 ~ 15h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1500 ~ 1600 DEG C, insulation 7 ~ 9h, obtain magnesium-aluminium spinel foamed ceramics.
In the present embodiment: described aluminum oxide fine powder is Brown Alundum fine powder; Described magnesia powder is magnesite clinker fine powder; Described sugar is maltose; Described sintering agent is AlF
3micro mist; The temperature of described thermostat container is 150 ~ 180 DEG C.
The volume density of the magnesium-aluminium spinel foamed ceramics obtained by the present embodiment is 0.27 ~ 0.38g/cm
3, compressive strength reaches 5.24 ~ 7.20Mpa, and apparent porosity is 90% ~ 92%.
embodiment 5
A kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.Described in the present embodiment, the step of preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.55 ~ 2.7) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (1.4 ~ 1.6).
Step 3, in compound, add the sintering agent of described compound 0.1 ~ 0.3wt% and the AC whipping agent of 0.1 ~ 0.3wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 100 ~ 120 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 8 ~ 15h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1600 ~ 1700 DEG C, insulation 3 ~ 5h, obtain magnesium-aluminium spinel foamed ceramics.
In the present embodiment: described aluminum oxide fine powder is compact alumina fine powder; Described magnesia powder is electrosmelted magnesite clinker fine powder; Described sugar is fructose; Described sintering agent is B
2o
3micro mist and BC
4the mixture of micro mist; The temperature of described thermostat container is 120 ~ 150 DEG C.
The volume density of the magnesium-aluminium spinel foamed ceramics obtained by the present embodiment is 0.38 ~ 0.49g/cm
3, compressive strength reaches 7.20 ~ 9.60Mpa, and apparent porosity is 86% ~ 89%.
embodiment 6
A kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.Described in the present embodiment, the step of preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.55 ~ 2.7) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (1.6 ~ 1.8).
Step 3, in compound, add the sintering agent of described compound 0.3 ~ 0.5wt% and the AC whipping agent of 0.3 ~ 0.5wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 150 ~ 180 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 8 ~ 15h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1500 ~ 1600 DEG C, insulation 7 ~ 9h, obtain magnesium-aluminium spinel foamed ceramics.
In the present embodiment: described aluminum oxide fine powder is plate diamond spar fine powder; Described magnesia powder is electrosmelted magnesite clinker fine powder; Described sugar is glucose; Described sintering agent is BC
4micro mist and MgF
2the mixture of micro mist; The temperature of described thermostat container is 150 ~ 180 DEG C.
The volume density of the magnesium-aluminium spinel foamed ceramics obtained by the present embodiment is 0.45 ~ 0.54g/cm
3, compressive strength reaches 8.40 ~ 10.20Mpa, and apparent porosity is 85% ~ 87%.
embodiment 7
A kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.Described in the present embodiment, the step of preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.4 ~ 2.55) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (1.0 ~ 1.2).
Step 3, in compound, add the sintering agent of described compound 0.3 ~ 0.5wt% and the AC whipping agent of 0.1 ~ 0.3wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 180 ~ 200 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 15 ~ 25h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1600 ~ 1700 DEG C, insulation 5 ~ 7h, obtain magnesium-aluminium spinel foamed ceramics.
In the present embodiment: described aluminum oxide fine powder is commercial alumina fine powder; Described magnesia powder is electrosmelted magnesite clinker fine powder; Described sugar is sucrose; Described sintering agent is MgF
2micro mist and AlF
3the mixture of micro mist; The temperature of described thermostat container is 150 ~ 180 DEG C.
The volume density of the magnesium-aluminium spinel foamed ceramics obtained by the present embodiment is 0.24 ~ 0.36g/cm
3, compressive strength reaches 4.25 ~ 7.80Mpa, and apparent porosity is 90% ~ 94%.
embodiment 8
A kind of magnesium-aluminium spinel foamed ceramics and preparation method thereof.Described in the present embodiment, the step of preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.55 ~ 2.7) ︰ 1.
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (1.2 ~ 1.4).
Step 3, in compound, add the sintering agent of described compound 0.1 ~ 0.3wt% and the AC whipping agent of 0.3 ~ 0.5wt%, mix, obtain mixed powder.
Step 4, mixed powder is warming up to 100 ~ 120 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 8 ~ 15h, obtain the base substrate after solidifying.
Step 5, by solidification after base substrate be warming up to 1600 ~ 1700 DEG C, insulation 7 ~ 9h, obtain magnesium-aluminium spinel foamed ceramics.
In the present embodiment: described aluminum oxide fine powder is α-Al
2o
3fine powder; Described magnesia powder is electrosmelted magnesite clinker fine powder; Described sugar is fructose; Described sintering agent is B
2o
3micro mist and AlF
3the mixture of micro mist; The temperature of described thermostat container is 120 Ah ~ 150 DEG C.
The volume density of the magnesium-aluminium spinel foamed ceramics obtained by the present embodiment is 0.27 ~ 0.38g/cm
3, compressive strength reaches 6.04 ~ 8.20Mpa, and apparent porosity is 90% ~ 92%.
The advantage that this embodiment compared with prior art has and positively effect:
1, this embodiment is due to aluminum oxide fine powder and the wetting ability interaction between magnesia powder surface and glycan molecule-OH, powder can comparatively be evenly dispersed in the sugared liquation of melting, the dispersion system uniform composition of gained, can not crack due to powder skewness when burning till.
2, this embodiment is using sugar as whipping agent, the water vapor that between-OH of glycan molecule, condensation produces is utilized to foam, the bubble produced is adsorbed on liquid-gas interface and dispersion system viscosity increase by fine particle is stablized, be conducive to forming uniform pore, the interconnective cellular microstructure of final formation, has higher through-hole rate and intensity.
3, this embodiment technique is simple, and without noxious gas emission in whole preparation process, is beneficial to environment protection.
The volume density of the magnesium-aluminium spinel foamed ceramics 4, obtained by this embodiment is 0.12 ~ 0.54g/cm
3, compressive strength reaches 2.50 ~ 10.2Mpa, and apparent porosity is 85% ~ 97%.
Therefore, this embodiment has the simple and eco-friendly feature of technique; Prepared magnesium-aluminium spinel foamed ceramics flawless, volume density is low, through-hole rate is high and intensity is large.
Claims (7)
1. a preparation method for magnesium-aluminium spinel foamed ceramics, is characterized in that the step of described preparation method is:
Step one, be raw material mixing by aluminum oxide fine powder and magnesia powder, wherein: the mass ratio of Yangization aluminium Xi Fen ︰ magnesia powder is (2.4 ~ 2.7) ︰ 1;
Step 2, be that compound mixes by sugar and described raw material, wherein the mass ratio of raw material described in: Tang ︰ is 1 ︰ (0.6 ~ 1.8);
Step 3, in compound, add the sintering agent of described compound 0.1 ~ 0.5wt% and the AC whipping agent of 0.1 ~ 0.5wt%, mix, obtain mixed powder;
Step 4, mixed powder is warming up to 100 ~ 200 DEG C, insulation 1 ~ 3h, obtains mixed powder and be dispersed in dispersion system in sugared liquation, more described dispersion system is placed in thermostat container, bubble and solidification 8 ~ 25h, obtain the base substrate after solidifying;
Step 5, by solidification after base substrate be warming up to 1500 ~ 1700 DEG C, insulation 3 ~ 9h, obtain magnesium-aluminium spinel foamed ceramics.
2. the preparation method of magnesium-aluminium spinel foamed ceramics according to claim 1, is characterized in that described aluminum oxide fine powder is commercial alumina fine powder, α-Al
2o
3one in fine powder, white fused alumina fine powder, Brown Alundum fine powder, compact alumina fine powder and plate diamond spar fine powder, the particle diameter of described aluminum oxide fine powder is less than 44 μm.
3. the preparation method of magnesium-aluminium spinel foamed ceramics according to claim 1, it is characterized in that described magnesia powder is electrosmelted magnesite clinker fine powder or is magnesite clinker fine powder, the particle diameter of described magnesia powder is less than 44 μm.
4. the preparation method of magnesium-aluminium spinel foamed ceramics according to claim 1, it is characterized in that described sugar is the one in fructose, sucrose, glucose and maltose, the purity of described sugar is greater than 99.0wt%.
5. the preparation method of magnesium-aluminium spinel foamed ceramics according to claim 1, is characterized in that the temperature of described thermostat container is 120 ~ 180 DEG C.
6. the preparation method of magnesium-aluminium spinel foamed ceramics according to claim 1, is characterized in that described sintering agent is B
2o
3micro mist, BC
4micro mist, MgF
2micro mist and AlF
3one or both in micro mist.
7. a magnesium-aluminium spinel foamed ceramics, is characterized in that described magnesium-aluminium spinel foamed ceramics is the magnesium-aluminium spinel foamed ceramics prepared by preparation method of the magnesium-aluminium spinel foamed ceramics according to any one in claim 1 ~ 6.
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