CN111056846A - Directional porous aluminum nitride honeycomb ceramic rapidly prepared by adopting freeze drying and combustion synthesis method and method thereof - Google Patents
Directional porous aluminum nitride honeycomb ceramic rapidly prepared by adopting freeze drying and combustion synthesis method and method thereof Download PDFInfo
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Abstract
The invention discloses a directional porous aluminum nitride honeycomb ceramic prepared rapidly by adopting a freeze drying and combustion synthesis method and a method thereof. The method for preparing the directional porous aluminum nitride ceramic has the characteristics of simple process, short period, good repeatability, low cost and the like. The prepared directional porous aluminum nitride ceramic has wide application prospect in the fields of metal filtration, catalyst carriers, polymer reinforced phases, automobile industry, solar power generation and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic non-metallic materials, and relates to directional porous aluminum nitride honeycomb ceramic rapidly prepared by adopting a freeze drying and combustion synthesis method and a method thereof.
Background
The AlN honeycomb ceramic has a series of excellent characteristics of high thermal conductivity, high resistivity, low thermal expansion coefficient, excellent mechanical property, high chemical stability and the like, and has wide application prospects in the aspects of molten metal filtration, catalyst carriers, polymer reinforced phases, heat exchange components and the like. Since the properties of the honeycomb ceramic are closely related to the porosity and pore structure thereof, the design of the structure thereof has become a hot point of research in recent years.
At present, many honeycomb ceramics with controllable structures, such as cordierite, silicon carbide, alumina, mullite and the like, are prepared by an extrusion forming method and a template method, but the methods have the problems of high temperature, high energy consumption, long preparation period and the like. For example, in the invention patent with the publication number of CN110194441A, namely a preparation method of a hollow spherical aluminum nitride powder material and an aluminum nitride porous ceramic, a two-step method is adopted to prepare the porous AlN ceramic, the preparation process involves a plurality of complex physical and chemical reactions and sintering processes with high energy consumption, the preparation period is long, and the purity of the product is difficult to ensure.
Disclosure of Invention
The invention aims to provide a method for rapidly preparing directional porous aluminum nitride honeycomb ceramics by adopting a freeze drying and combustion synthesis method, which can overcome the defects of long preparation period, low production efficiency, difficult control of pore structure and the like of porous AlN ceramics prepared by the traditional method.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a method for rapidly preparing directional porous aluminum nitride honeycomb ceramics by adopting a freeze drying and combustion synthesis method, which comprises the following steps:
1) taking aluminum powder, aluminum nitride powder and citric acid as raw materials, taking tert-butyl alcohol as a solvent, and fully mixing to prepare slurry;
2) freezing the slurry, and then carrying out vacuum freeze drying on the frozen sample to obtain a green body;
3) placing the green body into a porous graphite crucible of a combustion synthesis reaction chamber, vacuumizing the reaction chamber until the air pressure is less than 10Pa, charging nitrogen with the pressure of 0.2-2.0MPa and the purity of 99.99%, igniting the graphite paper tape from the bottom of a block by the graphite paper tape, electrifying the graphite paper tape for 10 seconds under the conditions of the voltage of 20V and the current of 60A to perform combustion reaction, placing the block which is a cylindrical sample after freeze drying on the graphite paper, electrifying two ends of the graphite paper, igniting the bottom of the block after heating, and then spontaneously combusting from bottom to top; and after the combustion reaction is finished, obtaining a white block in the porous graphite crucible, namely the directional porous aluminum nitride honeycomb ceramic.
Preferably, in step 1), the aluminum powder, the aluminum nitride powder and the tert-butyl alcohol are mixed according to the following volume percentages: 5% -35%: 5% -35%: 60-90 percent of aluminum powder and 1-5 percent of citric acid in the total mass of the aluminum powder and the aluminum nitride powder.
Preferably, in the step 1), aluminum powder, aluminum nitride powder, citric acid and tert-butyl alcohol are placed into a ball milling tank for mixing, the ball milling time is 2-12 hours, the material-ball ratio is 4:1, and the rotating speed is 400 r/min.
Preferably, in the step 2), the freezing temperature is-100 to-25 ℃, and the vacuum freeze-drying temperature is-100 to-20 ℃.
Preferably, in step 2), the slurry is poured into a cylindrical silicon rubber mold for freezing, and the bottom of the silicon rubber mold is a copper column partially immersed in liquid nitrogen. And (3) placing the copper column into liquid nitrogen for keeping the temperature constant, placing a mold on the copper column after the temperature is stable, pouring the slurry, and spontaneously freezing from bottom to top.
The invention also discloses the directional porous aluminum nitride honeycomb ceramic prepared by the method, which is characterized in that the honeycomb pore diameter of the directional porous aluminum nitride honeycomb ceramic is 10-50 mu m, the wall thickness is 10-25 mu m, and the porosity is 45-88%.
Compared with the prior art, the invention has the following beneficial effects:
the method adopts tert-butyl alcohol as a freeze-drying solvent, citric acid as a dispersing agent, aluminum powder and AlN powder as an aluminum source and a diluent for combustion synthesis respectively, slurry after ball milling and uniform mixing is subjected to freeze drying, a dried sample is placed in a combustion synthesis chamber, and combustion synthesis is performed under a lower nitrogen pressure, so that the directional porous AlN honeycomb ceramic is prepared. The method utilizes the self-heat release of the combustion reaction to sinter the sample, the combustion time is only 10s, and the sintering furnace is not required to be utilized to carry out high-temperature long-time heat preservation sintering in the prior art, so the method has the advantages of simple process, good repeatability, low cost, low energy consumption, short period and the like.
The directional porous AlN honeycomb ceramic prepared by the method has the advantages of uniform internal pore structure, high shape repeatability, high yield, high porosity and controllable pore structure, thereby having wide application prospect in the fields of metal filtration, catalyst carriers, polymer reinforced phases, heat exchange parts, automobile industry, solar power generation and the like.
Drawings
FIG. 1 is a schematic view of a combustion synthesis apparatus;
FIG. 2 is an XRD pattern of an oriented porous AlN honeycomb ceramic;
FIG. 3 is an SEM image of an oriented porous AlN honeycomb ceramic; wherein, (a) is an SEM image parallel to the freezing direction, and (b) is an SEM image perpendicular to the freezing direction.
Wherein: 1-observation window; 2-an air inlet valve; 3-a vacuum valve; 4-a graphite paper tape; 5-sample; 6-graphite crucible; 7-barometer; 8, power supply.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings: example 1
Mixing 11.34g of aluminum powder, 25.43g of AlN powder, 1.84g of citric acid and 48mL of tert-butyl alcohol, putting the mixture into a sealed alumina ball milling pot, and ball-milling for 2 hours, wherein the ball-material ratio is 4:1, the rotating speed is 400 r/min. Then, the slurry after ball milling is poured into a silicon rubber mold for freezing, the bottom of the mold is a copper column precooled in liquid nitrogen, the freezing temperature is controlled at minus 50 ℃, and the frozen sample is placed in a freeze dryer for vacuum freeze drying at minus 20 ℃. Finally, the dried green body is placed into a combustion synthesis reaction chamber, and a schematic diagram of the combustion synthesis apparatus is shown in fig. 1. Vacuumizing the reaction chamber until the air pressure is less than 10Pa, charging nitrogen with the purity of 99.99 percent at 0.5Mpa, igniting the graphite paper tape from the bottom of the block body through the graphite paper tape, and electrifying the graphite paper tape under the conditions that the voltage is 20V and the current is 60A for 10 seconds to generate combustion reaction. After the reaction, the sample is taken out from the combustion synthesis device, and the directional porous AlN honeycomb ceramic can be obtained.
The resulting product was characterized by X-ray diffractometer (XRD), Field Emission Scanning Electron Microscope (FESEM). Fig. 2 is an XRD pattern of the product, all the peaks corresponding to the hexagonal AlN phase, and no peaks of any impurity phase appeared. FIG. 3 is an FESEM photograph of the product, and it can be found that the inside of the oriented porous AlN honeycomb ceramic is vertically arranged with a porosity of 77%, a honeycomb pore diameter of 28 μm and a wall thickness of 15 μm.
Example 2
Mixing 5.67g of aluminum powder, 12.71g of AlN powder, 0.74g of citric acid and 54mL of tert-butyl alcohol, putting the mixture into a sealed alumina ball milling tank, and ball milling for 4 hours, wherein the ball-material ratio is 4:1, the rotating speed is 400 r/min. Then, the slurry after ball milling is poured into a silicon rubber mold for freezing, the bottom of the mold is a copper column precooled in liquid nitrogen, the freezing temperature is controlled at minus 50 ℃, and the frozen sample is placed in a freeze dryer for vacuum freeze drying at minus 20 ℃. And finally, placing the dried green body into a combustion synthesis reaction chamber, vacuumizing the reaction chamber until the air pressure is less than 10Pa, filling nitrogen with the purity of 99.99 percent at 0.8Mpa, igniting the graphite paper tape from the bottom of the block body through the graphite paper tape, and electrifying the graphite paper tape for 10 seconds under the conditions that the voltage is 20V and the current is 60A to generate combustion reaction. After the reaction, the sample is taken out from the combustion synthesis device, and the directional porous AlN honeycomb ceramic can be obtained.
The resulting product was characterized by X-ray diffractometer (XRD), Field Emission Scanning Electron Microscope (FESEM). It can be found that the oriented porous AlN honeycomb ceramic has oriented pores vertically arranged inside, porosity of 88%, honeycomb pore diameter of 50 μm and wall thickness of 10 μm. Other results were the same as in example 1.
Example 3
Mixing 8.51g of aluminum powder, 19.07g of AlN powder, 0.83g of citric acid and 51mL of tert-butyl alcohol, putting the mixture into a sealed alumina ball milling tank, and ball milling for 6 hours, wherein the ball-material ratio is 4:1, the rotating speed is 400 r/min. Then, the slurry after ball milling is poured into a silicon rubber mold for freezing, the bottom of the mold is a copper column precooled in liquid nitrogen, the freezing temperature is controlled at-25 ℃, and the frozen sample is placed in a freeze dryer for vacuum freeze drying at-40 ℃. And finally, placing the dried green body into a combustion synthesis reaction chamber, vacuumizing the reaction chamber until the air pressure is less than 10Pa, filling nitrogen with the purity of 99.99 percent under the pressure of 1.2Mpa, igniting the graphite paper tape from the bottom of the block body through the graphite paper tape, and electrifying the graphite paper tape for 10 seconds under the conditions that the voltage is 20V and the current is 60A to generate combustion reaction. After the reaction, the sample is taken out from the combustion synthesis device, and the directional porous AlN honeycomb ceramic can be obtained.
The resulting product was characterized by X-ray diffractometer (XRD), Field Emission Scanning Electron Microscope (FESEM). It was found that the inside of the oriented porous AlN honeycomb ceramic was oriented vertically, the porosity was 81%, the pore diameter of the honeycomb was 38 μm, and the wall thickness was 13 μm. Other results were the same as in example 1.
Example 4
Mixing 14.18g of aluminum powder, 31.79g of AlN powder, 0.92g of citric acid and 45mL of tert-butyl alcohol, putting the mixture into a sealed alumina ball milling pot, and ball-milling for 8 hours, wherein the ball-material ratio is 4:1, the rotating speed is 400 r/min. Then, the slurry after ball milling is poured into a silicon rubber mold for freezing, the bottom of the mold is a copper column precooled in liquid nitrogen, the freezing temperature is controlled to be-75 ℃, and the frozen sample is placed in a freeze dryer for vacuum freeze drying at-60 ℃. And finally, placing the dried green body into a combustion synthesis reaction chamber, vacuumizing the reaction chamber until the air pressure is less than 10Pa, filling nitrogen with the purity of 99.99 percent under the pressure of 1.5Mpa, igniting the graphite paper tape from the bottom of the block body through the graphite paper tape, and electrifying the graphite paper tape for 10 seconds under the conditions that the voltage is 20V and the current is 60A to generate combustion reaction. After the reaction, the sample is taken out from the combustion synthesis device, and the directional porous AlN honeycomb ceramic can be obtained.
The resulting product was characterized by X-ray diffractometer (XRD), Field Emission Scanning Electron Microscope (FESEM). It can be found that the oriented porous AlN honeycomb ceramic has oriented pores vertically arranged inside, the porosity is 69%, the pore diameter of the honeycomb is 20 μm, and the wall thickness is 18 μm. Other results were the same as in example 1.
Example 5
Mixing 17.01g of aluminum powder, 38.14g of AlN powder, 0.55g of citric acid and 42mL of tert-butyl alcohol, putting the mixture into a sealed alumina ball milling pot, and ball-milling for 10 hours, wherein the ball-material ratio is 4:1, the rotating speed is 400 r/min. Then, the slurry after ball milling is poured into a silicon rubber mold for freezing, the bottom of the mold is a copper column precooled in liquid nitrogen, the freezing temperature is controlled at-100 ℃, and the frozen sample is placed in a freeze dryer for vacuum freeze drying at-80 ℃. And finally, placing the dried green body into a combustion synthesis reaction chamber, vacuumizing the reaction chamber until the air pressure is less than 10Pa, filling nitrogen with the purity of 99.99 percent at 1.8Mpa, igniting the graphite paper tape from the bottom of the block body through the graphite paper tape, and electrifying the graphite paper tape for 10 seconds under the conditions that the voltage is 20V and the current is 60A to generate combustion reaction. After the reaction, the sample is taken out from the combustion synthesis device, and the directional porous AlN honeycomb ceramic can be obtained.
The resulting product was characterized by X-ray diffractometer (XRD), Field Emission Scanning Electron Microscope (FESEM). It was found that the inside of the oriented porous AlN honeycomb ceramic was vertically arranged oriented pores, the porosity was 59%, the pore diameter of the honeycomb was 16 μm, and the wall thickness was 21 μm. Other results were the same as in example 1.
Example 6
Mixing 22.68g of aluminum powder, 50.86g of AlN powder, 0.74g of citric acid and 36mL of tert-butyl alcohol, putting the mixture into a sealed alumina ball milling pot, and ball-milling for 12 hours, wherein the ball-material ratio is 4:1, the rotating speed is 400 r/min. Then, the slurry after ball milling is poured into a silicon rubber mold for freezing, the bottom of the mold is a copper column precooled in liquid nitrogen, the freezing temperature is controlled at-50 ℃, and the frozen sample is placed in a freeze dryer for vacuum freeze drying at-100 ℃. And finally, placing the dried green body into a combustion synthesis reaction chamber, vacuumizing the reaction chamber until the air pressure is less than 10Pa, filling nitrogen with the purity of 99.99% at 2Mpa, igniting the graphite paper tape from the bottom of the block body through the graphite paper tape, and electrifying the graphite paper tape for 10 seconds under the conditions that the voltage is 20V and the current is 60A to perform combustion reaction. After the reaction, the sample is taken out from the combustion synthesis device, and the directional porous AlN honeycomb ceramic can be obtained.
The resulting product was characterized by X-ray diffractometer (XRD), Field Emission Scanning Electron Microscope (FESEM). It can be found that the oriented porous AlN honeycomb ceramic has vertically arranged oriented pores inside, the porosity is 45%, the pore diameter of the honeycomb is 10 μm, and the wall thickness is 25 μm. Other results were the same as in example 1.
In conclusion, the method adopts tert-butyl alcohol as a solvent and citric acid as a dispersing agent to freeze-dry the aluminum powder and the aluminum nitride powder, and burns and synthesizes the dried green body in a low nitrogen pressure atmosphere to obtain the directional porous aluminum nitride honeycomb ceramic with high porosity and controllable pore structure. The method for preparing the directional porous aluminum nitride honeycomb ceramic by combining freeze drying and combustion synthesis for the first time utilizes the self-heat release of combustion reaction to sinter the sample, does not need to utilize a sintering furnace to carry out high-temperature long-time heat preservation sintering, and has the characteristics of simple process, good repeatability, low cost and the like. The directional porous aluminum nitride honeycomb ceramic prepared by the invention has wide application prospect in the fields of metal filtration, catalyst carriers, polymer reinforced phases, heat exchange parts, automobile industry, solar power generation and the like.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (6)
1. A method for rapidly preparing directional porous aluminum nitride honeycomb ceramics by adopting a freeze drying and combustion synthesis method is characterized by comprising the following steps:
1) taking aluminum powder, aluminum nitride powder and citric acid as raw materials, taking tert-butyl alcohol as a solvent, and fully mixing to prepare slurry;
2) freezing the slurry, and then carrying out vacuum freeze drying on the frozen sample to obtain a green body;
3) placing the green body into a porous graphite crucible of a combustion synthesis reaction chamber, vacuumizing the reaction chamber until the air pressure is less than 10Pa, charging nitrogen with the pressure of 0.2-2.0MPa and the purity of 99.99%, igniting the green body from the bottom of the green body through a graphite paper tape, electrifying the graphite paper tape for 10 seconds under the conditions of the voltage of 20V and the current of 60A to perform combustion reaction, wherein a white block body obtained in the porous graphite crucible is the directional porous aluminum nitride honeycomb ceramic.
2. The method for rapidly preparing the oriented porous aluminum nitride honeycomb ceramic by adopting the freeze drying and combustion synthesis method according to claim 1, wherein in the step 1), the aluminum powder, the aluminum nitride powder and the tertiary butanol are mixed according to the following volume percentages: 5% -35%: 5% -35%: 60-90 percent of aluminum powder and 1-5 percent of citric acid in the total mass of the aluminum powder and the aluminum nitride powder.
3. The method for rapidly preparing the oriented porous aluminum nitride honeycomb ceramic by adopting the freeze drying and combustion synthesis method according to claim 1, wherein in the step 1), aluminum powder, aluminum nitride powder, citric acid and tert-butyl alcohol are put into a ball milling tank for mixing, the ball milling time is 2-12 hours, the material-ball ratio is 4:1, and the rotating speed is 400 r/min.
4. The method for rapidly preparing the directional porous aluminum nitride honeycomb ceramic by adopting the freeze-drying and combustion synthesis method according to claim 1, wherein the freezing temperature in the step 2) is-100 to-25 ℃, and the vacuum freeze-drying temperature is-100 to-20 ℃.
5. The method for rapidly preparing the directional porous aluminum nitride honeycomb ceramic by using the freeze-drying and combustion synthesis method according to claim 1 or 4, wherein the slurry is poured into a cylindrical silicon rubber mold for freezing in the step 2), and the bottom of the silicon rubber mold is a copper column partially immersed in liquid nitrogen.
6. The oriented porous aluminum nitride honeycomb ceramic prepared by the method of any one of claims 1 to 5, wherein the oriented porous aluminum nitride honeycomb ceramic has a honeycomb pore size of 10 to 50 μm, a wall thickness of 10 to 25 μm, and a porosity of 45 to 88%.
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| CN201911243324.7A CN111056846B (en) | 2019-12-06 | 2019-12-06 | Directional porous aluminum nitride honeycomb ceramic rapidly prepared by adopting freeze drying and combustion synthesis method and method thereof |
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| CN111056846B CN111056846B (en) | 2021-04-20 |
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