CN111233502B - Light heat-insulating high-strength mullite material and preparation method thereof - Google Patents

Light heat-insulating high-strength mullite material and preparation method thereof Download PDF

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CN111233502B
CN111233502B CN202010049410.0A CN202010049410A CN111233502B CN 111233502 B CN111233502 B CN 111233502B CN 202010049410 A CN202010049410 A CN 202010049410A CN 111233502 B CN111233502 B CN 111233502B
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mullite
porous
whisker
frame
slurry
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CN111233502A (en
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张海宝
王振军
曾德军
王红波
桑可正
张瑜
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Changan University
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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
    • C04B35/16—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 silicates other than clay
    • C04B35/18—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 silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Abstract

The invention provides a light heat-insulating high-strength mullite material and a preparation method thereof. The preparation method comprises the following steps: step 1, preparing a porous mullite whisker frame; preparing compact mullite precursor slurry; step 2, uniformly spraying the compact mullite precursor slurry on the outer surface of the porous mullite whisker frame, and drying to obtain a porous mullite green body; and 3, sintering the porous mullite green body at high temperature in the air atmosphere to form a compact mullite coating on the outer surface of the porous mullite whisker frame, thereby obtaining the light, heat-insulating and high-strength mullite material. The material of the invention realizes the combination of light weight, heat insulation and high strength on the premise of high porosity.

Description

Light heat-insulating high-strength mullite material and preparation method thereof
Technical Field
The invention relates to preparation of a bionic porous ceramic material, in particular to a light heat-insulating high-strength mullite material and a preparation method thereof.
Background
The porous ceramic has the advantages of high temperature resistance, corrosion resistance, high rigidity and the like, and also has the properties of light weight, heat insulation (low heat conductivity), low thermal expansion, large specific surface area and the like. The porous silicon-aluminum-based mullite is used as one member of porous ceramic, has outstanding performances such as good thermal shock resistance, high-temperature strength, good high-temperature oxidation resistance and the like, and has wide application prospects in the fields of high-temperature catalyst carriers, high-temperature sealing, engine tail gas filtration, high-temperature heat insulation and the like. The porous mullite material is particularly suitable for a heat insulation protective layer of an apparatus under a high-temperature working condition due to high porosity and low heat conductivity, so that the resource loss caused by high-temperature oxidation can be effectively reduced, and the energy consumption can be well reduced. In the aspect of porous mullite products, products such as mullite fiber reinforced porous mullite special-shaped parts (DLR), diesel engine tail gas filters (Dow) and the like are applied.
At present, porous ceramics often adopt a method for improving porosity to reduce the thermal conductivity of materials, thereby obtaining light-weight high-quality heat-insulating materials. Yang et al prepared porous mullite with porosity of 81% by using a foaming gel grouting forming method, the thermal conductivity of 0.14W/m and the conductivity of 0.61g/cm3. Bourret et al added kaolin into the foam slurry to produce mullite having a porosity of greater than 94% and a density reduced to 0.19g/cm3The thermal conductivity is reduced to 0.063W/mm, but the strength is only 0.23 MPa. In the mechanical properties of porous ceramics, the strength of the material generally decreases exponentially with increasing porosity. How to enhance the strength of high porosity materials has been an important research topic. Mullite fibers and whiskers are increasingly paid more attention to improving the strength of porous mullite. Firstly, mullite whiskers can be added into equiaxed mullite grains as an additive body; secondly, the mullite fiber or whisker can also be used as a matrix to form the frame structure mullite. Xu, etc. prepares porous mullite by using mullite whisker as a matrix, prepares a sillimanite whisker frame by calcining a mixture of ammonium hexafluoroaluminate and kaolin at 1000 ℃, and then calcines at 1500 ℃ to obtain the mullite whisker frame. But the strength of the whisker framework obtained here is low. The reason for this is that the solid phase sintering mechanism is between the whiskers, and high-strength sintering is difficult to achieve at 1500 ℃. In conclusion, the preparation of the light heat-insulating high-strength mullite is a difficult technical problem in material preparation.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a light heat-insulating high-strength mullite material and a preparation method thereof, which realize the combination of light heat insulation and high strength on the premise of high porosity.
The invention is realized by the following technical scheme:
the mullite material takes a porous mullite whisker frame as a substrate, and a dense mullite coating is covered and combined on the outer surface of the substrate.
Preferably, the thickness of the compact mullite coating is 5-50 microns.
The preparation method of the light heat-insulating high-strength mullite material comprises the following steps:
step 1, preparing a porous mullite whisker frame; preparing compact mullite precursor slurry;
step 2, uniformly spraying the compact mullite precursor slurry on the outer surface of the porous mullite whisker frame, and drying to obtain a porous mullite green body;
and 3, sintering the porous mullite green body at high temperature in the air atmosphere to form a compact mullite coating on the outer surface of the porous mullite whisker frame, thereby obtaining the light, heat-insulating and high-strength mullite material.
Preferably, in the step 1, the preparation of the porous mullite whisker frame specifically comprises: preparing uniformly dispersed slurry A from nano aluminum oxide powder and aluminum fluoride powder by using a ball milling mixture; mixing TEOS, water and ethanol to prepare sol; mixing the sol with the slurry A to obtain slurry B, enabling the slurry B to generate a gel effect under the catalytic action of ammonia water, drying the obtained gel to obtain mullite whisker raw material powder, then performing dry pressing to obtain a green body, and sintering at a high temperature in a closed crucible to obtain a porous mullite whisker frame; wherein the molar ratio of Al to Si is 3: 1.
Preferably, the sintering temperature of the green body in a closed environment is 1300-1650 ℃, and the heat preservation time is 1-5 h.
Preferably, in the step 1, the specific process for preparing the compact mullite precursor slurry is as follows: mixing nano Al2O3Powder, nano SiO2The powder and the PVA binder are mixed uniformly by ball milling, wherein the molar ratio of Al to Si is 3: 1.
Further, the solid content of the mullite precursor slurry is 20-50%.
Furthermore, the content of the binder in the mullite precursor slurry is 1-5 wt%.
Preferably, in step 3, the calcination system used for calcination is: preserving the heat for 1 to 5 hours at 1500 to 1650 ℃.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention prepares the compact mullite layer on the surface of the porous mullite whisker frame. As a result, it was found that the bending strength of the porous mullite was improved by about 30% by the dense surface layer of several tens of micrometers. This is because when the porous ceramic material is broken, cracks first initiate on the surface of the material and then propagate into the interior until the entire body is broken. The breaking strength of the material is very sensitive to the surface condition of the material. When the surface of the material is a compact layer, the difficulty of crack generation is improved, so that the strength of the whole material is improved. Therefore, the structure can have high porosity and mechanical strength, and realizes the combination of low thermal conductivity, light weight and high strength.
Drawings
Fig. 1 is a microscopic morphology of the composite structure mullite prepared in the first example.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative only and not to be limiting of the scope of the invention, and various equivalent modifications of the invention which fall within the limits of the appended claims will be suggested to persons skilled in the art after reading this disclosure.
The invention firstly uses the mullite whisker with high strength as a base material to prepare the porous mullite whisker frame matrix with high porosity. The high porosity lays a good foundation for light weight and heat insulation performance. After the composite material is compounded with the compact mullite coating on the surface, the bending strength of the porous mullite whisker frame matrix is obviously improved. And the porosity of the whole material is slightly influenced by the compact layer, so that the mullite with the composite structure realizes the combination of light heat insulation and high strength.
A preparation method of a light heat-insulating high-strength mullite material comprises the following steps:
step 1: preparing a porous mullite whisker frame: firstly, carrying out ball milling on nano aluminum oxide powder and aluminum fluoride powder to obtain slurry A; then TEOS, water and ethanol are prepared into sol; and finally, mixing the sol with the slurry A to obtain slurry B, and enabling the slurry B to generate a gel effect under the catalytic action of ammonia water. And completely drying the gel to obtain mullite whisker raw material powder, wherein the mass ratio of Al: the molar ratio of Si is 3: 1. And then, dry pressing and forming to obtain a green body, and sintering at high temperature in a closed crucible to obtain the porous mullite whisker frame.
Step 2: preparing a compact mullite coating on the surface of the porous mullite whisker frame: al with the grain diameter of 500 nanometers2O3Powder, 30nm SiO2The powder and the PVA binder are uniformly mixed by ball milling to obtain compact mullite precursor slurry, wherein the molar ratio of Al to Si is 3:1, the PVA content in the compact mullite precursor slurry is 1-5 wt%, and the solid content of the slurry is 20-50%. And then uniformly spraying the compact mullite precursor slurry on the surface layer of the porous mullite whisker frame, and drying to obtain a porous mullite green body. Different solid contents here result in different coating thicknesses and finally in different thicknesses of the dense mullite coating.
And 3, step 3: high-temperature calcination of the porous mullite green body: and (3) placing the mullite green body with the coating obtained by drying in an air furnace, and preserving the heat at 1500-1650 ℃ for 1-5 hours to realize high-temperature sintering, so that the compact mullite coating with the thickness of 5-50 microns can be obtained on the surface of the porous mullite whisker frame.
The nano Al2O3The powder has a particle size of 500nm and SiO2The particle size of the powder was 30 nm.
Example one
The embodiment combines a preparation method of a light heat-insulating high-strength mullite material, which comprises the following steps:
step 1: preparing a porous mullite whisker frame: firstly, ball-milling nano aluminum oxide powder and aluminum fluoride powder to obtain slurry A; then TEOS, water and ethanol are prepared into sol; and finally, mixing the sol with the slurry A to obtain slurry B, and enabling the slurry B to generate a gel effect under the catalytic action of ammonia water. And completely drying the gel to obtain mullite whisker raw material powder, wherein the mass ratio of Al: the molar ratio of Si is 3: 1. And then, carrying out dry pressing forming to obtain a green body, and sintering for 5 hours at 1300 ℃ in a relatively closed crucible to obtain the porous mullite whisker frame.
Step 2: preparing a compact mullite layer on the surface of the whisker frame: al with the grain diameter of 500 nanometers2O3Powder, 30nm SiO2The powder and the PVA binder are uniformly mixed by ball milling, wherein the molar ratio of Al to Si is 3:1, the content of PVA is 5 wt%, and the solid content of the slurry is 40%. And then uniformly spraying the mullite precursor slurry on the surface layer of the porous mullite whisker frame, and drying to obtain the porous mullite green body.
And 3, step 3: high-temperature calcination of the porous mullite green body: and placing the mullite green body with the coating obtained by drying in an air furnace, and preserving the heat at 1600 ℃ for 1 hour to realize high-temperature sintering, thus obtaining a compact mullite coating with the thickness of 35 microns on the surface of the porous mullite whisker frame.
As shown in fig. 1, a dense coating is formed on the surface of the porous mullite whisker frame substrate. The coating enables the material to still have the bending strength of 62MPa under the high porosity of 60%, lays a good foundation for improving the bending strength of the porous mullite whisker frame matrix, and the measured thermal conductivity of the coating is 0.63W/(m × K), and the dense coating effectively blocks the convective thermal conductivity of air along the porous mullite whisker frame matrix, thereby reducing the thermal conductivity of the material.
Example two
The embodiment combines a preparation method of a light heat-insulating high-strength mullite material, which comprises the following steps:
step 1: preparing a porous mullite whisker frame: firstly, ball-milling nano aluminum oxide powder and aluminum fluoride powder to obtain slurry A; then TEOS, water and ethanol are prepared into sol; and finally, mixing the sol with the slurry A to obtain slurry B, and enabling the slurry B to generate a gel effect under the catalytic action of ammonia water. And completely drying the gel to obtain mullite whisker raw material powder, wherein the mass ratio of Al: the mol ratio of Si is 3: 1. And then, carrying out dry pressing and forming to obtain a green body, and sintering the green body in a relatively closed crucible at 1400 ℃ for 3h to obtain the porous mullite whisker frame.
Step 2: preparing a compact mullite layer on the surface of the whisker frame: al with the grain diameter of 500 nanometers2O3Powder, 30nm SiO2Powders andthe PVA binder is uniformly mixed by ball milling, wherein the molar ratio of Al to Si is 3:1, the content of PVA is 1 wt%, and the solid content of the slurry is 20%. And then uniformly spraying the mullite precursor slurry on the surface layer of the porous mullite whisker frame, and drying to obtain the porous mullite green body.
And step 3: high-temperature calcination of the porous mullite green body: and (3) placing the mullite green body with the coating obtained by drying in an air furnace, and preserving the heat at 1500 ℃ for 3 hours to realize high-temperature sintering, thus obtaining the mullite coating with the thickness of 5 microns on the surface of the porous mullite whisker frame.
EXAMPLE III
The embodiment combines a preparation method of a light heat-insulating high-strength mullite material, which comprises the following steps:
step 1: preparing a porous mullite whisker frame: firstly, ball-milling nano aluminum oxide powder and aluminum fluoride powder to obtain slurry A; then preparing TEOS, water and ethanol into sol; and finally, mixing the sol with the slurry A to obtain slurry B, and enabling the slurry B to generate a gel effect under the catalytic action of ammonia water. And completely drying the gel to obtain mullite whisker raw material powder, wherein the mass ratio of Al: the mol ratio of Si is 3: 1. And then, carrying out dry pressing and forming to obtain a green body, and sintering the green body in a relatively closed crucible at 1500 ℃ for 4h to obtain the porous mullite whisker frame.
And 2, step: preparing a compact mullite layer on the surface of the whisker frame: al with the grain diameter of 500 nanometers2O3Powder, 30nm SiO2The powder and the PVA binder are mixed evenly by ball milling, wherein the molar ratio of Al to Si is 3:1, the content of PVA is 5 wt%, and the solid content of the slurry is 50%. And then spraying the mullite precursor slurry on the surface layer of the porous mullite whisker frame uniformly, and drying to obtain a porous mullite green body.
And 3, step 3: high-temperature calcination of the porous mullite green body: and placing the mullite green body with the coating obtained by drying in an air furnace, and preserving the heat for 5 hours at 1600 ℃ to realize high-temperature sintering, thus obtaining the mullite coating with the thickness of 50 microns on the surface of the porous mullite whisker frame.
Example four
The embodiment combines a preparation method of a light heat-insulating high-strength mullite material, which comprises the following steps:
step 1: preparing a porous mullite whisker frame: firstly, carrying out ball milling on nano aluminum oxide powder and aluminum fluoride powder to obtain slurry A; then TEOS, water and ethanol are prepared into sol; and finally, mixing the sol with the slurry A to obtain slurry B, and enabling the slurry B to generate a gel effect under the catalytic action of ammonia water. And completely drying the gel to obtain mullite whisker raw material powder, wherein the mass ratio of Al: the mol ratio of Si is 3: 1. And then, dry pressing and forming to obtain a green body, and sintering for 1h at 1650 ℃ in a relatively closed crucible to obtain the porous mullite whisker frame.
Step 2: preparing a compact mullite layer on the surface of the whisker frame: al with the grain diameter of 500 nanometers2O3Powder, 30nm SiO2The powder and the PVA binder are uniformly mixed by ball milling, wherein the molar ratio of Al to Si is 3:1, the content of PVA is 3 wt%, and the solid content of the slurry is 40%. And then uniformly spraying the mullite precursor slurry on the surface layer of the porous mullite whisker frame, and drying to obtain the porous mullite green body.
And 3, step 3: high-temperature calcination of the porous mullite green body: and placing the mullite green body with the coating obtained by drying in an air furnace, and preserving the heat at 1650 ℃ for 1 hour to realize high-temperature sintering, thereby obtaining the mullite coating with the thickness of 40 microns on the surface of the porous mullite whisker frame.
The invention prepares the compact coating on the surface of the high-porosity porous mullite whisker frame by using slurry spraying and high-temperature sintering methods. Firstly, coating mullite precursor slurry on the surface of a mullite whisker frame, slowly drying to obtain a green body, and then sintering at high temperature to densify the surface layer and tightly combine the surface layer with the whisker frame. The microstructure of the coating and the matrix can be regulated and controlled by adjusting the process parameters such as slurry property, coating thickness and the like, so that the porous mullite with the bionic structure, which has high bending strength and reduced thermal conductivity, is obtained. Compared with the existing porous mullite material, the mullite material has the advantages of higher strength, high sealing effect and the like, and is expected to be well applied to high-temperature heat-insulating materials of military and civil spacecrafts.
The above description is only about four embodiments of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modification of the present invention using this concept shall fall within the scope of the present invention. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the protection scope of the technical solution of the present invention.

Claims (4)

1. The preparation method of the light heat-insulating high-strength mullite material is characterized in that the mullite material takes a porous mullite whisker frame as a substrate, and a layer of compact mullite coating is covered and combined on the outer surface of the substrate; the thickness of the compact mullite coating is 5-50 mu m;
the method comprises the following steps:
step 1, preparing a porous mullite whisker frame; preparing compact mullite precursor slurry;
step 2, uniformly spraying the compact mullite precursor slurry on the outer surface of the porous mullite whisker frame, and drying to obtain a porous mullite green body;
step 3, sintering the porous mullite green body at high temperature in the air atmosphere to form a compact mullite coating on the outer surface of the porous mullite whisker frame to obtain a light heat-insulating high-strength mullite material;
in the step 1, the specific process for preparing the compact mullite precursor slurry comprises the following steps: mixing nano Al2O3Powder, nano SiO2Uniformly mixing the powder and the PVA binder by ball milling, wherein the molar ratio of Al to Si is 3: 1;
the solid content of the mullite precursor slurry is 20 to 50 percent;
the content of the binder in the mullite precursor slurry is 1-5 wt%,
in the step 3, the calcination system adopted by the calcination is as follows: preserving heat for 1-5 hours at 1500-1650 ℃.
2. The preparation method of the mullite material with light weight, heat insulation and high strength as claimed in claim 1, wherein in the step 1, the porous mullite whisker frame is prepared by: preparing uniformly dispersed slurry A from nano aluminum oxide powder and aluminum fluoride powder by using a ball milling mixed material; mixing TEOS, water and ethanol to prepare sol; mixing the sol and the slurry A to obtain slurry B, allowing the slurry B to generate a gel effect under the catalytic action of ammonia water, drying the obtained gel to obtain mullite whisker raw material powder, then performing dry pressing to obtain a green body, and sintering at a high temperature in a closed crucible to obtain a porous mullite whisker frame; wherein the molar ratio of Al to Si is 3: 1.
3. The preparation method of the light heat-insulating high-strength mullite material as claimed in claim 2, wherein the sintering temperature of the green body in a closed environment is 1300-1650 ℃, and the heat preservation time is 1-5 h.
4. The light heat-insulating high-strength mullite material obtained by the preparation method of any one of claims 1-3.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6129954A (en) * 1998-12-22 2000-10-10 General Electric Company Method for thermally spraying crack-free mullite coatings on ceramic-based substrates
CN1793017A (en) * 2005-11-22 2006-06-28 武汉理工大学 Mullite whisker-mullite composite coating and preparation process thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6129954A (en) * 1998-12-22 2000-10-10 General Electric Company Method for thermally spraying crack-free mullite coatings on ceramic-based substrates
CN1793017A (en) * 2005-11-22 2006-06-28 武汉理工大学 Mullite whisker-mullite composite coating and preparation process thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Microstructure and property of porous mullites with a whiskers framework obtained by a sol-gel process;Dejun Zeng et al.;《Ceramics International》;20160419;第42卷;第11271页第2.1节 *

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