CN108298975A - A method of preparing high porosity cordierite of holding one's breath-aluminum phosphate ceramics - Google Patents

A method of preparing high porosity cordierite of holding one's breath-aluminum phosphate ceramics Download PDF

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CN108298975A
CN108298975A CN201810342744.XA CN201810342744A CN108298975A CN 108298975 A CN108298975 A CN 108298975A CN 201810342744 A CN201810342744 A CN 201810342744A CN 108298975 A CN108298975 A CN 108298975A
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breath
holding
temperature
cordierite ceramic
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白佳海
高杰
李向前
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Shandong University of Technology
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Shandong University of Technology
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    • 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
    • C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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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
    • C04B35/447—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 phosphates, e.g. hydroxyapatite
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
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Abstract

A method of preparing high porosity cordierite aluminum phosphate ceramics of holding one's breath, it is characterised in that use following steps：（1）Aluminium dihydrogen phosphate, aluminum nitrate are dissolved into water, solution is configured to；（2）The surface for the solution prepared being dripped at room temperature porous cordierite ceramic, until porous cordierite ceramic reaches adsorption saturation；（3）The dry porous cordierite ceramic for having adsorbed mixed solution at 50 DEG C；（4）Desciccate is heated to 1150 DEG C under air atmosphere and keeps the temperature 2 hours, then with the speed cooling down of 5 DEG C/min to 800 DEG C and keep the temperature 2 hours, finally room temperature is naturally cooled to stove, obtain the cordierite aluminum phosphate ceramics of high porosity of holding one's breath, its open pore rate is not higher than 10%, and porosity of holding one's breath is up to 39%.

Description

A method of preparing high porosity cordierite of holding one's breath-aluminum phosphate ceramics
Technical field
The present invention is to provide a kind of methods for the method preparing high porosity cordierite-aluminum phosphate ceramics of holding one's breath, and belong to special Kind ceramic materials preparation technology field.
Background technology
Cordierite and aluminum phosphate belong to heat-resisting material, and wherein porous cordierite ceramic can be used as soak material Material.But if there are more open pores in porous cordierite ceramic, its heat-insulating property can be seriously affected.Therefore, at present Common method is to add some in cordierite ceramic to generate the auxiliary agent in hole of holding one's breath, such as silicon carbide.Aluminum phosphate is also one The dystectic material of kind, temperature in use are close to 1400 DEG C, it may have heat safe performance.It therefore, can be in porous cordierite Aluminum phosphate is introduced in ceramics, is used in combination technology appropriate that open pore is blocked up, and to increase porosity of holding one's breath, and does not influence cordierite It is used under 1400 DEG C of hot environments below.Although hole of partly holding one's breath, hole aluminium of holding one's breath can be generated with the method for outer adding assistant Incrementss it is limited after all, and cannot effectively reduce open pore rate.In order to overcome above-mentioned problem, invention provides one kind Efficiently, safe and reliable, easily operated, the low-cost method for preparing high porosity cordierite-aluminum phosphate ceramics of holding one's breath.
Invention content
The technology of the present invention provides a kind of efficient, safe and reliable, easily operated, the low-cost height for preparing and holds one's breath porosity violet The method of green stone-aluminum phosphate ceramics, technical solution are：
A method of preparing high porosity cordierite of holding one's breath-aluminum phosphate ceramics, it is characterised in that use following steps：（1）Phosphorus Acid dihydride aluminium, aluminum nitrate are according to molar ratio 1：2 ratio is dissolved into water, be configured to aluminium dihydrogen phosphate solubility be 0.05 M, Aluminum nitrate solubility is the mixed solution of 0.1 M；（2）The solution prepared is dripped at room temperature the table of porous cordierite ceramic It the wherein open pore rate 40-60% of porous cordierite ceramic, holds one's breath until porous cordierite ceramic reaches adsorption saturation in face Porosity is in the range of 5-8%；（3）The dry porous cordierite ceramic for having adsorbed mixed solution, drying time 48 at 50 DEG C Hour；Porous cordierite ceramic surface after drying forms one layer of thin layer containing aluminium dihydrogen phosphate and aluminum nitrate；（4）Dry Product heats to 300 DEG C under air atmosphere with the speed of 20 DEG C/min, then with the speed heat temperature raising of 5 DEG C/min To 700 DEG C and 2 hours are kept the temperature, then heat to 1150 DEG C with the speed of 5 DEG C/min and keeps the temperature 2 hours, then with 5 DEG C/the speed cooling down of min to 800 DEG C and keeps the temperature 2 hours, finally naturally cools to room temperature with stove, it obtains height and holds one's breath hole The cordierite of rate-aluminum phosphate ceramics, open pore rate are not higher than 10 %, and porosity of holding one's breath highest reaches 39%.
The operation principle of this technology invention：
The mixed solution that the solubility of aluminium dihydrogen phosphate is 0.05 M, aluminum nitrate solubility is 0.1 M as low as porous cordierite surface And it can be inhaled into porous cordierite.In 50 DEG C of drying processes, as moisture is from the hole inside porous cordierite ceramic It is diffused into the surface of porous ceramics, aluminium dihydrogen phosphate and aluminum nitrate can also be diffused into the surface of porous ceramics, form one layer and contain The thin layer of aluminium dihydrogen phosphate and aluminum nitrate；In sintering process, the purpose kept the temperature at 700 DEG C is to form aluminium metaphosphate, metaphosphoric acid The fusing point of aluminium is low, and compared with that will form liquid phase under low temperature, liquid phase has higher surface tension, can the outer end of open pore with And the outside of porous ceramic surface forms one layer of continuous whole liquid film, and open pore is closed；Then as temperature It quickly reduces, fine and close glass phase will be formed；During heat preservation two hours at 800 DEG C, glass phase and be wrapped in the inside The reaction was continued for the unreacted aluminium oxide in part, generates aluminum phosphate, and will not form more open pore.
The advantages of this technology is invented:
1. the present invention prepares the open pore rate of cordierite-aluminum phosphate 10% or so, minimum to can reach 5.0%；
2. the porosity of holding one's breath that can significantly improve porous ceramics prepared by this technology, the porous violet for being such as 60% using open pore rate Cordierite prepared by cordierite ceramic-aluminum phosphate ceramics, porosity of holding one's breath can be increased to 35% or more from original 5% or so, open gas Porosity is then reduced to 10% or so；
3. this technology invention can significantly improve the heat-insulating property of porous ceramics, for example using open pore rate it is 60%, hole of holding one's breath Cordierite prepared by the porous cordierite ceramic that rate is 5% or so-aluminum phosphate ceramics, room temperature thermal coefficient is from 1.7W/ (m.K) Left and right is reduced to 0.5 W/（m.K）Left and right.
Specific implementation mode
Embodiment 1
Aluminium dihydrogen phosphate, aluminum nitrate according to molar ratio 1：2 ratio is dissolved into water, is configured to the solubility of aluminium dihydrogen phosphate For 0.05 M, the mixed solution that aluminum nitrate solubility is 0.1 M；The solution prepared is dripped to porous cordierite ceramic at room temperature Surface, until porous cordierite ceramic reaches adsorption saturation, the open pore rate 60% of wherein porous cordierite ceramic is left The right side, porosity of holding one's breath are 5% or so；The dry porous cordierite ceramic for having adsorbed mixed solution at 50 DEG C, drying time are 48 small When；Porous cordierite ceramic surface after drying forms one layer of thin layer containing aluminium dihydrogen phosphate and aluminum nitrate；Desciccate 300 DEG C are heated to the speed of 20 DEG C/min under air atmosphere, then 700 are heated to the speed of 5 DEG C/min DEG C and keep the temperature 2 hours, then with the speed of 5 DEG C/min heat to 1150 DEG C and keep the temperature 2 hours, then with 5 DEG C/ The speed cooling down of min is to 800 DEG C and keeps the temperature 2 hours, finally naturally cools to room temperature with stove.It is prepared by this technology invention The open pore rate of cordierite-aluminum phosphate ceramics is not higher than 10.0%, and porosity of holding one's breath is up to 39 % or more, room temperature thermal coefficient from 1.7 W/ (m.K) are reduced to about 0.5 W/（m.K）.The principal crystalline phase that the ceramics are measured with XRD analysis is cordierite and aluminum phosphate.
Embodiment 2
Aluminium dihydrogen phosphate, aluminum nitrate according to molar ratio 1：2 ratio is dissolved into water, and the solubility for being configured to aluminium dihydrogen phosphate is 0.05 M, the mixed solution that aluminum nitrate solubility is 0.1 M；The solution prepared is dripped to porous cordierite ceramic at room temperature Surface, until porous cordierite ceramic reaches adsorption saturation, the wherein open pore rate of porous cordierite ceramic about 50% is closed The porosity about 7%；The dry porous cordierite ceramic for having adsorbed mixed solution at 50 DEG C, drying time are 48 hours；After drying Porous cordierite ceramic surface formed one layer of thin layer containing aluminium dihydrogen phosphate and aluminum nitrate；Desciccate in air atmosphere Under with the speed of 20 DEG C/min heat to 300 DEG C, then heat to 700 DEG C with the speed of 5 DEG C/min and keep the temperature 2 Hour, then 1150 DEG C are heated to the speed of 5 DEG C/min and keep the temperature 2 hours, then with the speed of 5 DEG C/min Cooling down is to 800 DEG C and keeps the temperature 2 hours, finally naturally cools to room temperature with stove.Cordierite-phosphorus prepared by this technology invention The open pore rate of sour aluminium ceramics is not higher than 8.0%, and porosity of holding one's breath is up to 33% or more, and room temperature thermal coefficient is from 1.9 W/ (m.K) Left and right is reduced to 0.8 W/（m.K）Left and right.The principal crystalline phase that the ceramics are measured with XRD analysis is cordierite and aluminum phosphate.
Embodiment 3
Aluminium dihydrogen phosphate, aluminum nitrate according to molar ratio 1：2 ratio is dissolved into water, is configured to aluminium dihydrogen phosphate solubility and is 0.05 M, the mixed solution that aluminum nitrate solubility is 0.1 M；The solution prepared is dripped to porous cordierite ceramic at room temperature Surface, until porous cordierite ceramic reaches adsorption saturation, the wherein open pore rate of porous cordierite ceramic about 40% is closed The porosity is about 8%；The dry porous cordierite ceramic for having adsorbed mixed solution at 50 DEG C, drying time are 48 hours；It is dry Porous cordierite ceramic surface afterwards forms one layer of coating containing aluminium dihydrogen phosphate and aluminum nitrate；Desciccate in air gas 300 DEG C are heated to the speed of 20 DEG C/min under atmosphere, then heats to 700 DEG C with the speed of 5 DEG C/min and keeps the temperature 2 hours, then 1150 DEG C are heated to the speed of 5 DEG C/min and keep the temperature 2 hours, then with the speed of 5 DEG C/min Cooling down is to 800 DEG C and keeps the temperature 2 hours, finally naturally cools to room temperature with stove, obtains cordierite-aluminum phosphate ceramics.This The open pore rate of cordierite-aluminum phosphate ceramics prepared by technological invention is not higher than 5.0%, and porosity of holding one's breath is up to 30% or more, room Warm thermal coefficient is reduced to 1.1 W/ from the left and right 2.3 W/ (m.K)（m.K）Left and right.The principal crystalline phase of the ceramics is measured with XRD analysis For cordierite and aluminum phosphate.

Claims (1)

1. a kind of method preparing high porosity cordierite-aluminum phosphate ceramics of holding one's breath, it is characterised in that use following steps：（1） Aluminium dihydrogen phosphate, aluminum nitrate are according to molar ratio 1：2 ratio is dissolved into water, and the solubility for being configured to aluminium dihydrogen phosphate is 0.05 M, aluminum nitrate solubility is the mixed solution of 0.1 M；（2）The solution prepared is dripped at room temperature the table of porous cordierite ceramic It the wherein open pore rate 40-60% of porous cordierite ceramic, holds one's breath until porous cordierite ceramic reaches adsorption saturation in face Porosity is in the range of 8-5%；（3）The dry porous cordierite ceramic for having adsorbed mixed solution, drying time 48 at 50 DEG C Hour；Porous cordierite ceramic surface after drying forms one layer of thin layer containing aluminium dihydrogen phosphate and aluminum nitrate；（4）Dry Product heats to 300 DEG C under air atmosphere with the speed of 20 DEG C/min, then with the speed heat temperature raising of 5 DEG C/min To 700 DEG C and 2 hours are kept the temperature, then heat to 1150 DEG C with the speed of 5 DEG C/min and keeps the temperature 2 hours, then with 5 DEG C/the speed cooling down of min to 800 DEG C and keeps the temperature 2 hours, finally naturally cools to room temperature with stove, it obtains height and holds one's breath hole The cordierite of rate-aluminum phosphate ceramics, porosity of holding one's breath are up to 39%.
CN201810342744.XA 2018-04-17 2018-04-17 A method of preparing high porosity cordierite of holding one's breath-aluminum phosphate ceramics Withdrawn CN108298975A (en)

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Application publication date: 20180720