CN114409434A - Low-thermal-expansion aluminum titanate ceramic and preparation method thereof - Google Patents
Low-thermal-expansion aluminum titanate ceramic and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 89
- 229910000505 Al2TiO5 Inorganic materials 0.000 title claims abstract description 64
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 46
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 238000001125 extrusion Methods 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 239000004033 plastic Substances 0.000 claims abstract description 16
- 229920003023 plastic Polymers 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- 239000003381 stabilizer Substances 0.000 claims abstract description 15
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000011148 porous material Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 13
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 13
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 229910001597 celsian Inorganic materials 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 42
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 33
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical group [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 18
- 239000012752 auxiliary agent Substances 0.000 claims description 13
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000005642 Oleic acid Substances 0.000 claims description 11
- 235000019484 Rapeseed oil Nutrition 0.000 claims description 11
- 239000001913 cellulose Substances 0.000 claims description 11
- 229920002678 cellulose Polymers 0.000 claims description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 11
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 11
- 244000061456 Solanum tuberosum Species 0.000 claims description 10
- 235000002595 Solanum tuberosum Nutrition 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 235000013312 flour Nutrition 0.000 claims description 3
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- KAKVFSYQVNHFBS-UHFFFAOYSA-N (5-hydroxycyclopenten-1-yl)-phenylmethanone Chemical compound OC1CCC=C1C(=O)C1=CC=CC=C1 KAKVFSYQVNHFBS-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 6
- 235000011187 glycerol Nutrition 0.000 description 10
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 9
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C04B35/462—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 titanium oxides or titanates based on titanates
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Abstract
The invention relates to low-thermal-expansion aluminum titanate ceramic and a preparation method thereof. The ceramic body crystalline phase in the low thermal expansion aluminum titanate ceramic comprises an aluminum titanate phase and a celsian phase, and the thermal expansion coefficient is less than 2 multiplied by 10‑6The porosity of the ceramic body is 30-50%, the median pore diameter of the ceramic body is 10-20 μm, and the ceramic body is of a honeycomb structure. The preparation method comprises the following steps: uniformly mixing aluminum oxide, titanium oxide, silicon oxide, a barium oxide source and a stabilizer to obtain a mixture A, and uniformly mixing the mixture A, a plastic agent, a dispersing agent, an extrusion aid and a pore-forming agent to obtain a mixture B; adding an organic solvent and water into the mixture B, and uniformly stirring to obtain pug C; extruding and forming the pug C to obtain a honeycomb ceramic green body; honeycomb ceramic green bodyAnd sintering after drying to obtain the low-thermal-expansion aluminum titanate honeycomb porous ceramic. The low thermal expansion aluminum titanate honeycomb porous ceramic has low thermal expansion rate, high porosity, uniform pore size distribution and higher strength.
Description
Technical Field
The invention relates to aluminum titanate ceramics, in particular to low-thermal expansion aluminum titanate ceramics and a preparation method thereof.
Background
The aluminum titanate ceramic has a high melting point (1860 ℃) and a low thermal expansion coefficient (0.2 to 1 x 10)-6K), corrosion resistance and the like, and is one of the ceramic materials which are found at present and have high temperature resistance and low thermal expansion coefficient. The porous ceramic is a ceramic material with cavities in the ceramic, has the excellent characteristics of large specific surface area, low thermal conductivity, low density and the like, and is widely applied to the fields of high-temperature heat insulation materials, filter materials, piezoelectric materials and the like. Aluminum titanate ceramics have potential in the application of refractory materials due to their combination of high temperature resistance, low coefficient of thermal expansion, and excellent thermal shock resistance. However, the moderate thermal instability and low strength of aluminum titanate make its use less widespread.
Disclosure of Invention
The invention provides low thermal expansion aluminum titanate ceramic and a preparation method thereof aiming at the problems of medium temperature thermal instability and low strength of the existing aluminum titanate ceramic.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a low thermal expansion aluminum titanate ceramic, the ceramic body crystal phase includes aluminum titanate phase and celsian phase, the thermal expansion coefficient is less than 2 x 10-6The porosity of the ceramic body is 30-50%, the median pore diameter of the ceramic body is 10-20 μm, and the ceramic body is of a honeycomb structure.
The preparation method of the low thermal expansion aluminum titanate ceramic comprises the following specific steps:
(1) uniformly mixing aluminum oxide, titanium oxide, silicon oxide, a barium oxide source and a stabilizer to obtain a mixture A, and uniformly mixing the mixture A, a plastic agent, a dispersing agent, an extrusion aid and a pore-forming agent to obtain a mixture B;
(2) adding an organic solvent and water into the mixture B, and uniformly stirring to obtain pug C;
(3) extruding and forming the pug C to obtain a honeycomb ceramic green body;
(4) and drying and sintering the honeycomb ceramic green body to obtain the low-thermal-expansion aluminum titanate honeycomb porous ceramic.
Based on the total content of the mixture A in the step (1) being 100 wt%, 40-60 wt% of alumina, 30-50 wt% of titanium oxide, 2-8 wt% of silicon oxide, 1-10 wt% of barium oxide and 1-10 wt% of stabilizer.
Based on the total content of the mixture A in the step (1) being 100 wt%, 1-5 wt% of dispersing agent, 1-5 wt% of extrusion auxiliary agent, 1-5 wt% of plastic agent and 1-60 wt% of pore-forming agent; preferably, the weight percentage of the dispersing agent is 2-3%, the weight percentage of the extrusion auxiliary agent is 2-4%, the weight percentage of the plastic agent is 3-4%, and the weight percentage of the pore-forming agent is 20-40%.
The stabilizer in the step (1) is magnesium oxide, ferric oxide or calcium oxide;
the barium oxide source is barium carbonate or barium hydroxide;
the plasticizer is one or more of cellulose, polyethylene glycol and flour; preferably, the plastic agent is cellulose and/or flour;
the pore-forming agent is graphite and/or potato powder;
the dispersant is oleic acid or/and potassium metasilicate;
the extrusion auxiliary agent is one or more of oleic acid, potassium laurate, glycerol and rapeseed oil; preferably, the extrusion aid is glycerol and/or rapeseed oil.
The organic solvent in the step (2) is glycerol.
Based on the total content of the mixture A in the step (1) being 100 wt%, the organic solvent accounts for 2-4 wt%, and the deionized water accounts for 20-25 wt%.
The specific method for sintering in the step (4) is
Sequentially heating from room temperature to 250 ℃ at a heating rate of 0.5-1 ℃/min; heating to 850-950 ℃ at the heating rate of 1-1.5 ℃/min, and preserving heat for 2-6 h; heating to 1350 ℃ at a heating rate of 0.5-1 ℃/min; heating to 1450-1550 ℃ at a speed of 0.3-0.5 ℃/min, and preserving heat for 4-8 h; cooling to 1300 ℃ and 1400 ℃ at a cooling rate of 0.5-1 ℃/min, and then cooling along with the furnace.
And a relatively slow temperature rise rate is needed in the stage of raising the temperature to 150-250 ℃, water which is not removed in the microwave drying process is further removed, the temperature rise rate is increased, the temperature is kept at 850-950 ℃ to completely oxidize organic matters in the ceramic, and a relatively long temperature preservation time is needed after the temperature is raised to the sintering temperature of the aluminum titanate to ensure the complete synthesis of the aluminum titanate.
The invention has the beneficial effects that:
(1) the raw materials needed by the invention are low in price and easy to obtain;
(2) the aluminum titanate honeycomb porous ceramic prepared by the method has low thermal expansion coefficient, and has high porosity and pore diameter.
Drawings
FIG. 1 is the XRD pattern of the low thermal expansion aluminum titanate honeycomb porous ceramic of example 1;
FIG. 2 is the pore size distribution of the low thermal expansion aluminum titanate honeycomb porous ceramic of example 3;
FIG. 3 is a graph showing the thermal expansion curves of the low thermal expansion aluminum titanate honeycomb porous ceramic materials of examples 1-4 at room temperature to 800 ℃;
FIG. 4 is a scanning electron micrograph of the low thermal expansion aluminum titanate honeycomb porous ceramic of example 4.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1: a preparation method of low thermal expansion aluminum titanate ceramics comprises the following steps:
(1) uniformly mixing aluminum oxide, titanium oxide, silicon oxide, barium carbonate and a stabilizer (ferric oxide) to obtain a mixture A, and uniformly mixing the mixture A, a plastic agent (cellulose), a dispersing agent (oleic acid), an extrusion auxiliary agent (rapeseed oil) and a pore-forming agent (potato powder) to obtain a mixture B; wherein the total content of the mixture A in the step (1) is 100 wt%, the content of aluminum oxide is 49.04 wt%, the content of titanium oxide is 38.46 wt%, the content of silicon oxide is 3.85 wt%, the content of barium carbonate is 3.85 wt%, the content of a stabilizer (ferric oxide) is 4.8 wt%, the total content of the mixture A in the step (1) is 100 wt%, the content of a dispersing agent (oleic acid) is 2.42 wt%, the content of an extrusion auxiliary agent (rapeseed oil) is 3.54 wt%, the content of a plastic agent (cellulose) is 3.97 wt%, and the content of a pore-forming agent (potato powder) is 36.27 wt%;
(2) adding an organic solvent (glycerol) and water into the mixture B, and uniformly stirring to obtain pug C; 3.22 percent by weight of organic solvent and 21.28 percent by weight of water based on 100 percent by weight of the total content of the mixture A in the step (1);
(3) extruding and forming the pug C to obtain a honeycomb ceramic green body;
(4) drying and sintering the green honeycomb ceramic blank to obtain the low-thermal-expansion aluminum titanate honeycomb porous ceramic, wherein the specific sintering method comprises the following steps
Sequentially heating from room temperature to 250 ℃ at the heating rate of 0.8 ℃/min; heating to 850 ℃ at the heating rate of 1.2 ℃/min, and keeping the temperature for 4 h; heating to 1350 deg.C at a rate of 0.6 deg.C/min; heating to 1500 ℃ at the heating rate of 0.4 ℃/min, and keeping the temperature for 6 hours; cooling to 1350 ℃ at a cooling rate of 0.8 ℃/min, and then cooling along with the furnace;
a relatively slow temperature rise rate is needed in the stage of raising the temperature to 250 ℃ at room temperature, water which is not removed in the microwave drying process is further removed, the temperature is kept for 4 hours at 850 ℃ to completely oxidize organic matters in the ceramic, and a relatively long temperature keeping time is needed after the temperature is raised to 1500 ℃ to ensure that the aluminum titanate is completely synthesized;
the XRD spectrum of the low thermal expansion aluminum titanate honeycomb porous ceramic of the embodiment is shown in figure 1, and as can be seen from figure 1, the analysis in the XRD spectrum can show that the crystalline phases in the aluminum titanate ceramic are an aluminum titanate phase and a celsian phase;
the low thermal expansion aluminum titanate ceramic body crystal phase of the present example comprises an aluminum titanate phase and a celsian phase and has a thermal expansion coefficient of 0.7415X 10-6The porosity of the ceramic body is 52.55 percent, the median pore diameter of the ceramic body is 13.49 mu m, and the ceramic body has a honeycomb structure.
Example 2: a preparation method of low thermal expansion aluminum titanate ceramics comprises the following steps:
(1) uniformly mixing aluminum oxide, titanium oxide, silicon oxide, barium carbonate and a stabilizer (ferric oxide) to obtain a mixture A, and uniformly mixing the mixture A, a plastic agent (cellulose), a dispersing agent (oleic acid), an extrusion auxiliary agent (rapeseed oil) and a pore-forming agent (potato powder) to obtain a mixture B; wherein, based on the total content of the mixture A in the step (1) being 100 wt%, the aluminum oxide is 57 wt%, the titanium oxide is 34.4 wt%, the silicon oxide is 3.44 wt%, the barium carbonate is 3.44 wt%, the stabilizing agent (ferric oxide) is 1.72 wt%, based on the total content of the mixture A in the step (1) being 100 wt%, the dispersing agent (oleic acid) is 2.36 wt%, the extrusion auxiliary agent (rapeseed oil) is 3.48 wt%, the plastic agent (cellulose) is 3.97 wt%, and the pore-forming agent (potato powder) is 30.50 wt%;
(2) adding an organic solvent (glycerol) and water into the mixture B, and uniformly stirring to obtain pug C; 3.29 percent by weight of organic solvent (glycerin) and 20.18 percent by weight of water based on 100 percent by weight of the total content of the mixture A in the step (1);
(3) extruding and forming the pug C to obtain a honeycomb ceramic green body;
(4) drying and sintering the green honeycomb ceramic blank to obtain the low-thermal-expansion aluminum titanate honeycomb porous ceramic, wherein the specific sintering method comprises the following steps
Sequentially heating from room temperature to 250 ℃ at the heating rate of 0.8 ℃/min; heating to 850 ℃ at the heating rate of 1.2 ℃/min, and keeping the temperature for 4 h; heating to 1350 deg.C at a rate of 0.6 deg.C/min; heating to 1500 ℃ at the heating rate of 0.4 ℃/min, and keeping the temperature for 8 hours; cooling to 1350 ℃ at a cooling rate of 0.8 ℃/min, and then cooling along with the furnace;
the sintering heat preservation time has influence on the aluminum titanate ceramic crystal grains and microcracks, and the heat preservation time is prolonged to reduce the thermal expansion coefficient of the aluminum titanate ceramic;
the low thermal expansion aluminum titanate ceramic body crystal phase of the present example comprises an aluminum titanate phase and a celsian phase and has a thermal expansion coefficient of 0.0869X 10-6The porosity of the ceramic body is 43.11 percent, the median pore diameter of the ceramic body is 12.63 mu m, and the ceramic body has a honeycomb structure.
Example 3: a preparation method of low thermal expansion aluminum titanate ceramics comprises the following steps:
(1) uniformly mixing aluminum oxide, titanium oxide, silicon oxide, barium carbonate and a stabilizer (ferric oxide) to obtain a mixture A, and uniformly mixing the mixture A, a plastic agent (cellulose), a dispersing agent (oleic acid), an extrusion auxiliary agent (rapeseed oil) and a pore-forming agent (potato powder) to obtain a mixture B; wherein the total content of the mixture A in the step (1) is 100 wt%, the content of aluminum oxide is 54.21 wt%, the content of titanium oxide is 32.71 wt%, the content of silicon oxide is 4.91 wt%, the content of barium carbonate is 4.91 wt%, the content of stabilizer (ferric oxide) is 3.26 wt%, the total content of the mixture A in the step (1) is 100 wt%, the content of dispersant (oleic acid) is 2.44 wt%, the content of extrusion auxiliary agent (rapeseed oil) is 3.36 wt%, the content of plastic agent (cellulose) is 3.86 wt%, and the content of pore-forming agent (potato powder) is 32.84 wt%;
(2) adding an organic solvent (glycerol) and water into the mixture B, and uniformly stirring to obtain pug C; 3.84 wt% of organic solvent (glycerin) and 21.46 wt% of water, wherein the total content of the mixture A in the step (1) is 100 wt%;
(3) extruding and forming the pug C to obtain a honeycomb ceramic green body;
(4) drying and sintering the green honeycomb ceramic blank to obtain the low-thermal-expansion aluminum titanate honeycomb porous ceramic, wherein the specific sintering method comprises the following steps
Sequentially heating from room temperature to 250 ℃ at the heating rate of 0.8 ℃/min; heating to 850 ℃ at the heating rate of 1.2 ℃/min, and keeping the temperature for 4 h; heating to 1350 deg.C at a rate of 0.6 deg.C/min; heating to 1550 ℃ at the heating rate of 0.4 ℃/min, and keeping the temperature for 6 hours; cooling to 1350 ℃ at a cooling rate of 0.8 ℃/min, and then cooling along with the furnace;
according to the reference data, the sintering temperature has great influence on the performance of the aluminum titanate, and the improvement of the sintering temperature of the aluminum titanate can reduce the thermal expansion coefficient of the aluminum titanate and improve the strength;
the pore size distribution of the low-thermal-expansion aluminum titanate honeycomb porous ceramic is shown in figure 3, and as can be seen from figure 2, the median pore size of the ceramic is about 20 micrometers;
the low thermal expansion aluminum titanate ceramic body crystal phase of the present example comprises an aluminum titanate phase and a celsian phase and has a thermal expansion coefficient of 1.1849X 10-6The porosity of the ceramic body is 48.26 percent, the median pore diameter of the ceramic body is 19.96 mu m, and the ceramic body is of a honeycomb structure.
Example 4: a preparation method of low thermal expansion aluminum titanate ceramics comprises the following steps:
(1) uniformly mixing aluminum oxide, titanium oxide, silicon oxide, barium carbonate and a stabilizer (ferric oxide) to obtain a mixture A, and uniformly mixing the mixture A, a plastic agent (cellulose), a dispersing agent (oleic acid), an extrusion auxiliary agent (rapeseed oil) and a pore-forming agent (potato powder) to obtain a mixture B; wherein the total content of the mixture A in the step (1) is 100 wt%, the content of aluminum oxide is 52.49 wt%, the content of titanium oxide is 32.67 wt%, the content of silicon oxide is 5.01 wt%, the content of barium carbonate is 3.50 wt%, the content of a stabilizing agent (ferric oxide) is 6.33 wt%, the total content of the mixture A in the step (1) is 100 wt%, the content of a dispersing agent (potassium metasilicate) is 2.67 wt%, the content of an extrusion auxiliary agent (rapeseed oil) is 3.64 wt%, the content of a plastic agent (cellulose) is 3.79 wt%, and the content of a pore-forming agent (potato powder) is 34.19 wt%;
(2) adding an organic solvent (glycerol) and water into the mixture B, and uniformly stirring to obtain pug C; 3.15 wt% of organic solvent (glycerin) and 20.05 wt% of water, wherein the total content of the mixture A in the step (1) is 100 wt%;
(3) extruding and forming the pug C to obtain a honeycomb ceramic green body;
(4) drying and sintering the green honeycomb ceramic blank to obtain the low-thermal-expansion aluminum titanate honeycomb porous ceramic, wherein the specific sintering method comprises the following steps
Sequentially heating from room temperature to 250 ℃ at the heating rate of 0.8 ℃/min; heating to 850 ℃ at the heating rate of 1.2 ℃/min, and keeping the temperature for 4 h; heating to 1350 deg.C at a rate of 0.6 deg.C/min; heating to 1550 ℃ at the heating rate of 0.4 ℃/min, and keeping the temperature for 6 hours; cooling to 1350 ℃ at a cooling rate of 0.8 ℃/min, and then cooling along with the furnace;
the scanning electron micrograph of the low thermal expansion aluminum titanate honeycomb porous ceramic of the embodiment is shown in fig. 4, and as can be seen from fig. 4, obvious microcracks exist among aluminum titanate crystal grains;
examples 1-4 thermal expansion curves of the low thermal expansion aluminum titanate honeycomb porous ceramic material at room temperature to 800 ℃ are shown in FIG. 3, and it can be seen from FIG. 3 that the thermal expansion coefficient of No. 4 is 1.9614X 10-6℃-1；
The low thermal expansion aluminum titanate ceramic body crystal phase of the present example comprises an aluminum titanate phase and a celsian phase and has a thermal expansion coefficient of 1.9614X 10-6V, the porosity of the ceramic body is 50.21 percent, the median pore diameter of the ceramic body is 17.98 mu m, and the ceramic body is of a honeycomb structure;
table 1 examples 1-4 physical property data
| |
1# | 2# | 3# | 4# |
| CTE(30-800℃)10-6℃-1 | 0.7415 | 0.0869 | 1.1849 | 1.9614 |
| Strength (perpendicular to the pore canal direction) | 1.5249MPa | 1.9538MPa | 1.873MPa | 1.3184MPa |
| Median pore diameter | 13.49μm | 12.63μm | 19.96μm | 17.98μm |
| Porosity of the material | 52.55％ | 43.11％ | 48.26％ | 50.21％ |
| Water absorption rate | 37.27％ | 29.36％ | 31.29％ | 36.25％ |
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes and modifications can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (8)
1. A low thermal expansion aluminum titanate ceramic characterized by: the ceramic body crystal phase comprises an aluminum titanate phase and a celsian phase, and has a thermal expansion coefficient of less than 2 x 10-6The porosity of the ceramic body is 30-50%, the median pore diameter of the ceramic body is 10-20 μm, and the ceramic body is of a honeycomb structure.
2. The method for preparing the low thermal expansion aluminum titanate ceramic according to claim 1, comprising the steps of:
(1) uniformly mixing aluminum oxide, titanium oxide, silicon oxide, a barium oxide source and a stabilizer to obtain a mixture A, and uniformly mixing the mixture A, a plastic agent, a dispersing agent, an extrusion aid and a pore-forming agent to obtain a mixture B;
(2) adding an organic solvent and water into the mixture B, and uniformly stirring to obtain pug C;
(3) extruding and forming the pug C to obtain a honeycomb ceramic green body;
(4) and drying and sintering the honeycomb ceramic green body to obtain the low-thermal-expansion aluminum titanate honeycomb porous ceramic.
3. The method for producing a low thermal expansion aluminum titanate ceramic according to claim 2, wherein: based on the total content of the mixture A in the step (1) being 100 wt%, 40-60 wt% of alumina, 30-50 wt% of titanium oxide, 2-8 wt% of silicon oxide, 1-10 wt% of barium oxide and 1-10 wt% of stabilizer.
4. The method for producing a low thermal expansion aluminum titanate ceramic according to claim 3, wherein: based on the total content of the mixture A in the step (1) being 100 wt%, 1-5 wt% of dispersing agent, 1-5 wt% of extrusion auxiliary agent, 1-5 wt% of plastic agent and 1-60 wt% of pore-forming agent.
5. The method for producing a low thermal expansion aluminum titanate ceramic according to claim 3, wherein: the stabilizer in the step (1) is magnesium oxide, iron oxide or calcium oxide, the barium oxide source is barium carbonate or barium hydroxide, the plastic agent is one or more of cellulose, polyethylene glycol and flour, the pore-forming agent is graphite and/or potato powder, and the dispersant is oleic acid and/or potassium metasilicate; the extrusion auxiliary agent is one or more of oleic acid, potassium laurate, glycerol and rapeseed oil.
6. The method for producing a low thermal expansion aluminum titanate ceramic according to claim 2, wherein: the organic solvent in the step (2) is glycerol.
7. The method for producing a low thermal expansion aluminum titanate ceramic according to claim 2, wherein: and (2) taking the total content of the mixture A in the step (1) as 100 wt%, and taking the total content of the organic solvent and the water in the step (2) as 20-25 wt%.
8. The method for producing a low thermal expansion aluminum titanate ceramic according to claim 2, wherein: the specific method for sintering in the step (4) is that
Sequentially heating from room temperature to 250 ℃ at a heating rate of 0.5-1 ℃/min; heating to 850-950 ℃ at the heating rate of 1-1.5 ℃/min, and preserving heat for 2-6 h; heating to 1350 ℃ at a heating rate of 0.5-1 ℃/min; heating to 1450-1550 ℃ at a speed of 0.3-0.5 ℃/min, and preserving heat for 4-8 h; cooling to 1300 ℃ and 1400 ℃ at a cooling rate of 0.5-1 ℃/min, and then cooling along with the furnace.
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