CN101613206A - A kind of preparation method of alumina hollow structure - Google Patents
A kind of preparation method of alumina hollow structure Download PDFInfo
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- CN101613206A CN101613206A CN200910160767A CN200910160767A CN101613206A CN 101613206 A CN101613206 A CN 101613206A CN 200910160767 A CN200910160767 A CN 200910160767A CN 200910160767 A CN200910160767 A CN 200910160767A CN 101613206 A CN101613206 A CN 101613206A
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- pyrolysis
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Abstract
The auxiliary two step pyrolysis methods of a kind of activated carbon powder phantom plate prepare the method for alumina ceramic hollow structure, and it comprises following concrete steps: (1) mixes aluminum isopropylate and two kinds of raw material dry method of activated carbon powder planetary ball mill; (2) powder that mixes is placed crucible; (3) N
2Pyrolysis 10～30min under the atmosphere protection; (4) pyrolysis 1.5～3.5 hours under air ambient; (5) stove is chilled to room temperature.Compared with prior art, advantage equipment of the present invention and technology are simple, with short production cycle, can exempt and remove the problems such as material contamination that template is brought in the traditional technology.This hollow structure particularly hollow network structure has the potential widespread use in fields such as lightweight structural material, filtration and purification separation and catalysis.
Description
Technical field
The present invention relates to a kind of preparation method of alumina hollow structure, belong to technical field of material.
Background technology
Hollow ceramic has internal space that volume density is little, specific surface area is big, thermostability is high and bigger etc., thereby presents the not available specific function of conventional material as a kind of novel stupalith.The hollow ceramic material has pottery itself distinctive high temperature resistant, corrosion-resistant, high chemical stability and dimensional stability simultaneously, it is used widely in filtration, purification separation, chemical industry catalytic carrier, many-sides such as sound absorption damping, senior lagging material and lightweight structural material, is subjected to increasing concern of people and research.
At present, the method for preparing the hollow ceramic structure mainly contains spray reaction method, template, microemulsion polymerization method and self-assembly method etc.Wherein, adopting template to embody certain advantage on the control hollow structure, is one of the method for hollow structure for preparing commonly used at present.Yet, generally needing the added pattern material utilizing template to prepare in the process of hollow material, some used in the process of removing template solution toxicity is bigger, may pollute prepared material.
Aluminum oxide (Al
2O
3) pottery has high hardness, good wear resistance, corrosion-resistant, high good characteristics such as physical strength are one of stupaliths of being most widely used of ceramic industry.The present invention relates to a kind of new preparation Al
2O
3The method of hollow structure can tentatively realize the regulation and control to hollow structure, and can directly exempt the problems such as pollution that follow-up removal mould material is brought.
Summary of the invention
Technical problem to be solved by this invention provides a kind of novel method for preparing alumina hollow structure, and equipment and technology are very simple, and is with short production cycle, and can exempt the problems such as pollution that follow-up removal mould material is brought.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: this prepares the method for alumina hollow structure, and it comprises following concrete steps:
(1) polymer precursor and two kinds of raw material dry method of activated carbon powder planetary ball mill are mixed;
(2) powder that mixes is placed crucible;
(3) N
2Pyrolysis 10～30min under the atmosphere protection;
(4) pyrolysis 1.5～3.5 hours under air ambient;
(5) stove is chilled to room temperature.
In the described step (1), the raw material that uses is aluminum isopropylate (Al[OCH (CH
3)
2]
3); Use the template of amorphous activated carbon powder, median size～100nm as the preparation hollow structure; Aluminum isopropylate and activated carbon weight ratio are 10: 1 and 20: 1; Use nylon resin ball grinder and zirconium oxide balls, 12 hours ball milling time.
In the described step (2), use alumina crucible, add a cover, prevent that product is evaporated in the external environment in the heat tracing process.
In the described step (3), the sintering oven that uses is resistive heating tubular type atmosphere sintering furnace.
In the described step (4), at first at N
2Sintering 30min under the atmosphere protection also can adopt other protective atmospheres, makes the activated carbon template do not calcined, for gaseous oxidation aluminium at its surface deposition; Sintering 1.5～3.5 hours under air ambient then, this moment, template will be calcined in air, decomposed the gaseous oxidation aluminium that obtains by aluminum isopropylate and continued to continue deposition on sedimentary aluminum oxide, at high temperature carried out atomic diffusion simultaneously, formed hollow structure.
Compared with prior art, the invention has the advantages that:
1. technology of the present invention and equipment are simple;
2. the preparation method of alumina hollow structure of the present invention, in theory by regulating and control the chemical ingredients of presoma, can be extended to according to identical technology in the middle of the hollow structure preparation of other materials system, be expected to become a kind of universal method of preparation ceramic hollow structure;
3. the present invention uses activated carbon as template, can directly calcine in air, has exempted the problems such as material contamination that follow-up removal template is brought.
Description of drawings
Fig. 1 is scanning electron microscope (SEM) figure of the embodiment of the invention one prepared alumina hollow structure;
Fig. 2 is X-ray diffraction (XRD) spectrum of the embodiment of the invention one prepared alumina hollow structure;
Fig. 3 is transmission electron microscope (TEM) figure of the embodiment of the invention one prepared alumina hollow structure;
Fig. 4 is transmission electron microscope (TEM) figure of the embodiment of the invention two prepared alumina hollow structures;
Fig. 5 is transmission electron microscope (TEM) figure of the embodiment of the invention three prepared alumina hollow structures.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment one
By weight 10: 1 (aluminum isopropylates: activated carbon) take by weighing aluminum isopropylate (Al[OCH (CH
3)
2]
3) and the common 5g (median size 200nm) of activated carbon, place nylon ball grinder, use the zirconium oxide balls planetary ball mill to mix in 12 hours.The gained powder is placed 99 alumina-ceramic crucibles, add a cover, place resistive heating tubular type atmosphere sintering furnace then to prevent the pyrolysis product volatilization.At first, charge into N then with atmosphere sintering stove evacuation 10Pa
2To a normal atmosphere (～0.11MPa).Atmosphere sintering furnace is warmed up to 1350 ℃ with 10 ℃/min, behind insulation 30min under 1350 ℃, the sealed at both ends lid of tube furnace is opened, and continues insulation 2.5 hours, free then cool to room temperature under air ambient.The SEM of prepared typical hollow network structure and TEM photo and XRD figure spectrum are respectively shown in Fig. 1～3.SEM and TEM photo show that prepared material is a hollow network structure, and XRD result shows that hollow network structure is α-Al
2O
3
Embodiment two
By weight 10: 1 (aluminum isopropylates: activated carbon) take by weighing aluminum isopropylate (Al[OCH (CH
3)
2]
3) and the common 5g (median size 200nm) of activated carbon, place nylon ball grinder, use the zirconium oxide balls planetary ball mill to mix in 12 hours.The gained powder is placed 99 alumina-ceramic crucibles, add a cover, place resistive heating tubular type atmosphere sintering furnace then to prevent the pyrolysis product volatilization.At first, charge into N then with atmosphere sintering stove evacuation 10Pa
2To a normal atmosphere (～0.11MPa).Atmosphere sintering furnace is warmed up to 1350 ℃ with 10 ℃/min, behind insulation 30min under 1350 ℃, the sealed at both ends lid of tube furnace is opened, and continues insulation 1.5 hours, free then cool to room temperature under air ambient.The TEM photo of prepared typical hollow structure as shown in Figure 4.Compare with embodiment one, illustrate that prolongation pyrolysis soaking time has the gathering between atomic diffusion utilized and adjacent particle, thereby promote the formation of hollow network structure.
Embodiment three
By weight 20: 1 (aluminum isopropylates: activated carbon) take by weighing aluminum isopropylate (Al[OCH (CH
3)
2]
3) and the common 5g (median size 50nm) of activated carbon, place nylon ball grinder, use the zirconium oxide balls planetary ball mill to mix in 12 hours.The gained powder is placed 99 alumina-ceramic crucibles, add a cover, place resistive heating tubular type atmosphere sintering furnace then to prevent the pyrolysis product volatilization.At first, charge into N then with atmosphere sintering stove evacuation 10Pa
2To a normal atmosphere (～0.11MPa).Atmosphere sintering furnace is warmed up to 1350 ℃ with 10 ℃/min, behind insulation 10min under 1350 ℃, the sealed at both ends lid of tube furnace is opened, and continues insulation 3.5 hours, free then cool to room temperature under air ambient.The TEM photo of prepared typical hollow structure as shown in Figure 5.Compare with embodiment one, show that the size that changes activated carbon powder phantom plate can realize the regulation and control to hollow structure.
The present invention proposes and a kind ofly simply prepare alumina hollow structure with forerunner's body new method. Method of the present invention and biography The system method is compared, and has equipment and synthesis technique is simple, and can exempt and remove the material dirt that template is brought in the traditional handicraft The problem such as dye. By prolonging the aerial pyrolysis time, can promote gathering between atom diffusion and adjacent particle and shape Become hollow network structure. The novel ceramic hollow structure of this kind will and be urged in lightweight structural material, filtration and purification separation Have potential in the fields such as change and application prospect widely.
Claims (3)
1, a kind of novel method for preparing alumina hollow structure, it comprises following concrete steps:
(1) aluminum isopropylate and two kinds of raw material dry method of activated carbon powder planetary ball mill are mixed;
(2) powder that mixes is placed crucible;
(3) N
2Pyrolysis 10～30min under the atmosphere protection;
(4) pyrolysis 1.5～3.5 hours under air ambient;
(5) stove is chilled to room temperature.
2, the method for preparing alumina hollow structure according to claim 1 is characterized in that: adopt the template of activated carbon powder as the preparation hollow structure in the described step (1) to (4).
3, the method for preparing alumina hollow structure according to claim 2; it is characterized in that: in described step (3) and (4), pyrolysis in two steps, at first pyrolysis is not oxidized with protection carbon template under protective atmosphere; the calcining of carbon template is removed in pyrolysis under air ambient then.
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| CN200910160767A CN101613206A (en) | 2009-07-17 | 2009-07-17 | A kind of preparation method of alumina hollow structure |
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| CN200910160767A CN101613206A (en) | 2009-07-17 | 2009-07-17 | A kind of preparation method of alumina hollow structure |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092305A (en) * | 2006-06-19 | 2007-12-26 | 郑州大学 | Method for preparing Sialon hollow ball |
| CN101214984A (en) * | 2007-01-05 | 2008-07-09 | 宁波工程学院 | Method for preparing aluminum oxide micro-sphere |
| CN101327454A (en) * | 2008-07-29 | 2008-12-24 | 华东理工大学 | Modified carbon-coated alumina supporter with nucleocapsid structure and preparation method thereof |
-
2009
- 2009-07-17 CN CN200910160767A patent/CN101613206A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092305A (en) * | 2006-06-19 | 2007-12-26 | 郑州大学 | Method for preparing Sialon hollow ball |
| CN101214984A (en) * | 2007-01-05 | 2008-07-09 | 宁波工程学院 | Method for preparing aluminum oxide micro-sphere |
| CN101327454A (en) * | 2008-07-29 | 2008-12-24 | 华东理工大学 | Modified carbon-coated alumina supporter with nucleocapsid structure and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| WEIYOU YANG ET AL.: "Hollow Alumina Microsphere Chain Networks", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
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Application publication date: 20091230 |