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CN1323051C - A kind of aluminum borate composite porous ceramic and preparation method thereof - Google Patents

A kind of aluminum borate composite porous ceramic and preparation method thereof Download PDF

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CN1323051C
CN1323051C CNB2005100189565A CN200510018956A CN1323051C CN 1323051 C CN1323051 C CN 1323051C CN B2005100189565 A CNB2005100189565 A CN B2005100189565A CN 200510018956 A CN200510018956 A CN 200510018956A CN 1323051 C CN1323051 C CN 1323051C
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fine powder
composite porous
aluminum
aluminum borate
powder
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CN1730427A (en
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李远兵
李楠
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Wuhan University of Science and Technology WHUST
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Wuhan University of Science and Technology WHUST
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Abstract

本发明涉及一种硼酸铝复合多孔陶瓷及其制备方法。其方案是将骨料与混合粉按重量比为20~90/10~80混合,外加1~6wt%的结合剂,混合后成型。在90~120℃条件下干燥20~30小时,升温到200~500℃保温20~280分钟,再升温至700~1700℃保温30~600分钟,自然冷却。其中:混合粉的制备方法是,将含铝化合物细粉与硼酸粉混合,混合后的AlxByOz为,x=16~22、y=2~5、z=30~36。含铝的化合物细粉由Al2O3、Al2O3·3H2O、Al2O3·H2O组成,分别为混合粉的0~70wt%、0~80wt%、0~70wt%。本发明工艺简单、成本低廉、易于控制,生产的陶瓷具有保温和透气性好的特点。该陶瓷和其它材料复合可作为保温材料、金属熔体精炼用透气陶瓷等。The invention relates to an aluminum borate composite porous ceramic and a preparation method thereof. The solution is to mix the aggregate and the mixed powder at a weight ratio of 20-90/10-80, add 1-6 wt% of binder, and form the mixture after mixing. Dry at 90-120°C for 20-30 hours, raise the temperature to 200-500°C for 20-280 minutes, then raise the temperature to 700-1700°C for 30-600 minutes, and cool naturally. Wherein: the preparation method of the mixed powder is to mix the aluminum-containing compound fine powder with boric acid powder, and the mixed AlxByOz is x=16-22, y=2-5, z=30-36. Aluminum-containing compound fine powder is composed of Al 2 O 3 , Al 2 O 3 ·3H 2 O, Al 2 O 3 ·H 2 O, respectively 0-70wt%, 0-80wt%, 0-70wt% of the mixed powder . The invention has the advantages of simple process, low cost and easy control, and the produced ceramics have the characteristics of good heat preservation and air permeability. The composite of the ceramics and other materials can be used as thermal insulation materials, gas-permeable ceramics for metal melt refining, and the like.

Description

A kind of aluminium borate composite porous ceramics and preparation method thereof
One, technical field
The invention belongs to the porous ceramics technical field, especially relate to a kind of aluminium borate composite porous ceramics and preparation method thereof.
Two, background technology
Because porous ceramics has advantages such as low density, high permeability, corrosion-resistant, excellent heat insulation property, high temperature resistant and long service life, they can be used as high-temperature gas filter, solid particle filter, filter for molten metal, be used at high temperature using the equipment that needs resist chemical, good penetrability, and, handle the aspects such as support of the catalyst of chemical plant refuse and vehicle exhaust as the physical sepn dividing plate.They also can be used as refractory materials, lagging material, transmitter, thermistor and porous piezoceramics, heat exchanger etc.In addition, they also have the potential application prospect in the bio-medical field.In a word, porous ceramics has been widely used in fields such as metallurgy, chemical industry, the energy, environmental protection, biology.
In recent years, the research of aluminum borate pottery is mainly concentrated in the preparation and application of aluminium borate whisker, because the low (2.93g/cm of the density of aluminum borate 3), fusing point height (1440 ℃), its mechanical property can with SiC, Si 3N 4Comparable to; The thermal expansivity of aluminum borate is little by (4.2 * 10 -6/ K), the little (4~5w/ (m.k), thereby have well insulated of thermal conductivity; Aluminum borate has good anti-corrosion, and it boils 8h in 90 ℃ 1 mol HCl solution, and weight only reduces 1%.Thereby aluminum borate makes various matrix materials as add strengthening, and can improve physical strength, thermostability and the erosion resistance of material.
At present, because preparation technology's more complicated of aluminium borate whisker and whisker size are difficult to control, limited the application aspect much of aluminium borate whisker.
(US 4 for a kind of aluminum borate stupalith of high-strength compact, 774,210), for example aluminum oxide, aluminum chloride, aluminium hydroxide, a diaspore and aluminum nitrate and boron trioxide are raw material to adopt aluminum contained compound, add 0.25~10% short burning agent for example boron calcium aluminate, boron magnesium aluminate, boron aluminum phosphate and boron sikicate aluminum etc., though prepare a kind of adiabatic aluminum borate pottery intensity height, density is low, complex process, cost height.
Adopting Burow Solution and boric acid is feedstock production aluminum borate pottery (US 5,183,785), be to calcine at a certain temperature, the powder mix after will calcining then, moulding, sintering processes obtains high porosity, the controlled aluminum borate pottery of pore opening distribution at a certain temperature.Be earlier Burow Solution to be become mud with boric acid, calcining then will be calcined back powder mix moulding again, obtain the aluminum borate pottery at a certain temperature behind the sintering.Though this invention can be prepared void content 40~60%, pore size is the aluminum borate pottery of 0.5 μ m~5 μ m, but the two step calcining procesies that adopt, the technology more complicated.
Three, summary of the invention
The purpose of this invention is to provide a kind of technology simple, with low cost, produce be easy to control, aluminum borate porous ceramics that insulation and permeability are good and preparation method thereof.
For realizing above-mentioned task, the technical solution used in the present invention is: with aggregate and powder mix is 20~90/10~80 to mix by weight, add the wedding agent of 1~6wt%, mixed 5~60 minutes, moulding, drying is 20~30 hours under 90~120 ℃ of conditions, is warmed up to 200~500 ℃ of insulations 20~280 minutes, be warming up to 700~1700 ℃ of insulations 30~600 minutes again, naturally cooling.
Wherein: the preparation method of powder mix is the aluminum contained compound fine powder to be mixed mixed Al with boric acid powder xB yO zFor, x=16~22, y=2~5, z=30~36, aluminiferous compound fine powder is by Al 2O 3Fine powder, Al 2O 33H 2O fine powder, Al 2O 3H 2The O fine powder is formed, and is respectively 0~70wt%, 0~80wt%, the 0~70wt% of powder mix.
Described aggregate is that one or both or two or more particulate matter are formed in corundum, mullite, alumina, magnesia, the magnesium-aluminium spinel.
The granularity of described corundum, mullite, alumina, magnesia, magnesium-aluminium spinel is 5~0mm, Al 2O 3Fine powder, Al 2O 33H 2O fine powder, Al 2O 3H 2The granularity of O fine powder, boric acid powder is less than 180 orders.
Described wedding agent is one or both or the two or more combination in starch, clay, resin, silicon sol, aluminium colloidal sol, polyvinyl alcohol, glycerine, the methylcellulose gum.
Described moulding or press or be ramming or for pouring into a mould, the pressure of mechanical pressing is 45~350MPa for machine.
The speed of described intensification is 50~300 ℃/h, and the speed of Sheng Wening is 50~300 ℃/h again.
Owing to adopt technique scheme, technology of the present invention is simple, with low cost, production is easy to control, utilize aluminiferous compound and boric acid to decompose the preparation hole, by changing raw material granularity and control process parameters, can obtain different apertures, apparent porosity and be 15~80%, porous ceramics, the porous ceramics of being produced has insulation and the good characteristics of permeability.The porous ceramics that makes and other material are compound, can be used as lagging material, metal melt refining with permeable-gas ceramics etc.
Four, embodiment
Embodiment 1
With the fused white corundum of 1.0~0.2mm and powder mix is 60~80/20~40 to mix by weight.Powder mix is by the fused white corundum fine powder of 9-15wt%, α-Al of 15~30wt% 2O 3The aluminium hydroxide fine powder of micro mist, 20~50wt% and boric acid powder mix.Mixed Al xB yO zScope be that x=18, y=4, z=33 add 2~5wt% clay, mix after 10~15 minutes mechanical pressing under 100~300MPa pressure.Drying is 24 hours under 100~110 ℃ of conditions, and the heat-up rate with 100~200 ℃/h is heated to 280~450 ℃ then, is incubated 30~200 minutes; Heat-up rate with 100~200 ℃/h is heated to 800~1600 ℃ again, is incubated 30~240 minutes, takes out behind the naturally cooling.
Adopt X-ray diffraction to analyze its thing phase composite, main thing is aluminum borate (9Al mutually 2O 32B 2O 3) with corundum mutually.Recording its volume density is 2.54g/cm 3, apparent porosity is 35%, and compressive strength is 45MPa, and Gas permeability is 0.44 μ m 2Sample φ 36 * 36mm was immersed in 870 ℃ of molten aluminiums 48 hours, take out sample, cut section, observe, do not see that sample is permeated by molten aluminium.
Embodiment 2
With the magnesium-aluminium spinel of 1-0.5mm and powder mix is 50~70/30~50 to mix by weight.Powder mix is by the fused white corundum fine powder of 12~25wt%, α-Al of 20~35wt% 2O 3The pseudo-boehmite fine powder of micro mist, 20~35wt% mixes with boric acid powder, mixes back Al xB yO zScope be that x=18, y=4, z=33 add the silicon sol of 2~5wt%.Mix after 10~15 minutes mechanical pressing under 150~200MPa pressure.Drying is 24 hours under 100~110 ℃ of conditions, and the heat-up rate with 100~200 ℃/h is heated to 280~450 ℃ then, is incubated 30~200 minutes; Heat-up rate with 100~200 ℃/h is heated to 800~1600 ℃ again, is incubated 30~240 minutes, takes out behind the naturally cooling.
Adopt X-ray diffraction to analyze its thing phase composite, main thing is aluminum borate (9Al mutually 2O 32B 2O 3) with magnesium-aluminium spinel mutually.Recording its volume density is 2.12g/cm 3, apparent porosity is 40%, and compressive strength is 40MPa, and Gas permeability is 0.56 μ m 2Sample φ 36 * 36mm was immersed in 870 ℃ of molten aluminiums 48 hours, take out sample, cut section, observe, do not see that sample is permeated by molten aluminium.

Claims (7)

1、一种硼酸铝复合多孔陶瓷的制备方法,其特征在于将骨料与混合粉按重量比为20~90/10~80混合,外加1~6wt%的结合剂,混合5~60分钟,成型,在90~120℃条件下干燥20~30小时,升温到200~500℃保温20~280分钟,再升温至700~1700℃保温30~600分钟,自然冷却;1. A method for preparing aluminum borate composite porous ceramics, characterized in that aggregate and mixed powder are mixed in a weight ratio of 20 to 90/10 to 80, and 1 to 6 wt% of a binder is added for mixing for 5 to 60 minutes. Forming, drying at 90-120°C for 20-30 hours, raising the temperature to 200-500°C for 20-280 minutes, then raising the temperature to 700-1700°C for 30-600 minutes, and cooling naturally; 其中:混合粉的制备方法是,将含铝化合物细粉与硼酸粉混合,混合后的AlxByOz为,x=16~22、y=2~5、z=30~36,含铝的化合物细粉由Al2O3细粉、Al2O3·3H2O细粉、Al2O3·H2O细粉组成,分别为混合粉的0~70wt%、0~80wt%、0~70wt%。Wherein: the preparation method of the mixed powder is to mix the aluminum-containing compound fine powder with boric acid powder, and the AlxByOz after mixing is, x=16~22, y=2~5, z=30~36, the aluminum-containing compound fine powder Composed of Al 2 O 3 fine powder, Al 2 O 3 ·3H 2 O fine powder, Al 2 O 3 ·H 2 O fine powder, respectively 0~70wt%, 0~80wt%, 0~70wt% of the mixed powder . 2、根据权利要求1所述的硼酸铝复合多孔陶瓷的制备方法,其特征在于所述的骨料为刚玉、莫来石、矾土、镁砂、镁铝尖晶石中一种或两种或两种以上颗粒物组成。2. The method for preparing aluminum borate composite porous ceramics according to claim 1, characterized in that the aggregate is one or two of corundum, mullite, bauxite, magnesia, and magnesium aluminum spinel Or composed of two or more particles. 3、根据权利要求2所述的硼酸铝复合多孔陶瓷的制备方法,其特征在于所述的刚玉、莫来石、矾土、镁砂、镁铝尖晶石的粒度为5~0mm,Al2O3细粉、Al2O3·3H2O细粉、Al2O3·H2O细粉、硼酸粉的粒度小于180目。3. The method for preparing aluminum borate composite porous ceramics according to claim 2, characterized in that the particle size of the corundum, mullite, bauxite, magnesia, and magnesia-aluminum spinel is 5-0 mm, and the Al 2 The particle size of O 3 fine powder, Al 2 O 3 ·3H 2 O fine powder, Al 2 O 3 ·H 2 O fine powder and boric acid powder is less than 180 mesh. 4、根据权利要求1所述的硼酸铝复合多孔陶瓷的制备方法,其特征在于所述的结合剂为淀粉、粘土、树脂、硅溶胶、铝溶胶、聚乙烯醇、甘油、甲基纤维素中的一种或两种或两种以上的组合。4. The method for preparing aluminum borate composite porous ceramics according to claim 1, characterized in that the binder is starch, clay, resin, silica sol, aluminum sol, polyvinyl alcohol, glycerin, methylcellulose, etc. one or a combination of two or more. 5、根据权利要求1所述的硼酸铝复合多孔陶瓷的制备方法,其特征在于所述的成型或为机压、或为捣打或为浇注,机压成型的压力为45~350MPa。5. The preparation method of aluminum borate composite porous ceramics according to claim 1, characterized in that the forming is either machine pressing, ramming or casting, and the pressure of machine pressing is 45-350 MPa. 6、根据权利要求1所述的硼酸铝复合多孔陶瓷的制备方法,其特征在于所述的升温的速度为50~300℃/h,再升温的速度为50~300℃/h。6. The method for preparing aluminum borate composite porous ceramics according to claim 1, characterized in that the heating rate is 50-300°C/h, and the heating-up rate is 50-300°C/h. 7、根据权利要求1~6项中任一项所述的硼酸铝复合多孔陶瓷的制备方法所制备的硼酸铝复合多孔陶瓷。7. The aluminum borate composite porous ceramic prepared according to the method for preparing aluminum borate composite porous ceramic according to any one of claims 1-6.
CNB2005100189565A 2005-06-20 2005-06-20 A kind of aluminum borate composite porous ceramic and preparation method thereof Expired - Fee Related CN1323051C (en)

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CN104418608B (en) * 2013-08-20 2016-08-10 中国科学院上海硅酸盐研究所 Low temperature firing method of silicon carbide porous ceramics
CN108751968B (en) * 2018-06-13 2020-12-22 北京科技大学 A kind of preparation method of intrinsically porous porous ceramic material
CN111205067B (en) * 2020-01-15 2022-04-01 武汉科技大学 Glass-ceramic material for cooperative protection of neutrons and gamma rays and preparation method thereof
CN116218491B (en) * 2023-05-09 2023-07-21 山东省地质矿产勘查开发局第二水文地质工程地质大队(山东省鲁北地质工程勘察院) Hydrogel plugging agent, preparation method of hydrogel plugging agent and water-based drilling fluid
CN116751073B (en) * 2023-08-23 2023-10-24 天津南极星隔热材料有限公司 Preparation method of lightweight heat-insulating aluminum borate porous ceramic with multistage pore structure

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5053364A (en) * 1989-06-12 1991-10-01 Aluminum Company Of America Aluminum borate ceramic matrix composite
WO1992000253A1 (en) * 1990-06-29 1992-01-09 Coors Porcelain Company Aluminum borate ceramics and process for producing same
US5098871A (en) * 1990-12-13 1992-03-24 Aluminum Company Of America Aluminum borate ceramic matrix composite
JPH10251076A (en) * 1997-03-11 1998-09-22 Nichias Corp Manufacturing method of porous inorganic material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5053364A (en) * 1989-06-12 1991-10-01 Aluminum Company Of America Aluminum borate ceramic matrix composite
WO1992000253A1 (en) * 1990-06-29 1992-01-09 Coors Porcelain Company Aluminum borate ceramics and process for producing same
US5098871A (en) * 1990-12-13 1992-03-24 Aluminum Company Of America Aluminum borate ceramic matrix composite
JPH10251076A (en) * 1997-03-11 1998-09-22 Nichias Corp Manufacturing method of porous inorganic material

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