CN101318677A - Method for preparing aluminum oxide nano-stick - Google Patents
Method for preparing aluminum oxide nano-stick Download PDFInfo
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- CN101318677A CN101318677A CNA2008100404616A CN200810040461A CN101318677A CN 101318677 A CN101318677 A CN 101318677A CN A2008100404616 A CNA2008100404616 A CN A2008100404616A CN 200810040461 A CN200810040461 A CN 200810040461A CN 101318677 A CN101318677 A CN 101318677A
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Abstract
The invention relates to a method for preparing an alumina nano-rod, belonging to the nanotechnical field. The method comprises the following steps: firstly, an aluminum salt water solution and a NaOH water solution are prepared, and the NaOH water solution is dripped into the aluminum salt water solution to make the pH value be 5; secondly, suspension is transferred into a high-pressure kiln autoclave, heated up to between 200 and 220 DEG C for heat insulation, and cooled to the room temperature along with a furnace, and a boehmite precursor nano-rod can be prepared; and thirdly, the boehmite precursor nano-rod is heated up to between 500 and 800 DEG C for heat insulation and then converted into the alumina nano-rod. The boehmite precursor nano-rod and the alumina nano-rod prepared by the method are monocrystals, a diameter is between 10 and 20 nanometers, a length is between 100 and 300 nanometers and a slenderness ratio is between 5 and 15; and the boehmite precursor nano-rod and the alumina nano-rod have regular shapes and smooth surfaces, and can be used for ceramic composite material reinforce.
Description
Technical field
The present invention relates to a kind of preparation method of field of nanometer technology, specifically, that relate to is a kind of preparation method of Nano bars of alumina.
Background technology
One dimension Nano structure is to have bidimensional to be in the nanostructure of nanoscale scope in the three-dimensional space.The modal method of preparation crystal aluminum oxide one dimension Nano structure is a vapor phase process.The signle crystal alumina fiber at first is produced out in U.S. Lao Lunsi Berkeley laboratory, grows the signle crystal alumina nanofiber by the VLS method on the monocrystalline sapphire substrate.In this preparation process, at first, the Pt fusing is formed drop be deposited on the sapphire substrate, the Pt drop absorbs aluminum oxide from gas phase, grow sapphire whisker then.
Find that through literature search people such as Valcarcel deliver in " Advanced Materials " (Vol.10, No.2,1998) and are entitled as " Development of singl e-crystal α-Al to prior art
2O
3Fibers by vapor-liquid-solid deposition (VLS) from aluminum and powderedsilica " research paper; the mixture of aluminium powder and silica flour is heated to 1300-1500 ℃ can prepares diameter Distribution wide (0.1-10 μ m), the signle crystal alumina nano wire that length is hundreds of microns under vacuum condition.
It is very harsh that the employing vapor phase process prepares the preparation condition of aluminum oxide one dimension Nano structure, needs specific installation usually, and reaction needed is carried out under high temperature, vacuum or protective atmosphere, catalyzer condition, therefore limited the preparation of aluminum oxide one dimension Nano structure.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of Nano bars of alumina, prepare boehmite presoma nanometer rod, and change the similar Nano bars of alumina of pattern into by calcining with liquid phase method at the shortcomings and deficiencies that exist in the prior art.This method is utilized the laminate structure of boehmite, is under 5 the condition at reacting solution pH value, forms the boehmite nanometer rod by the mechanism of curling, and changes Nano bars of alumina into 500-800 ℃ of following thermolysis.
The present invention is achieved by the following technical solutions, the present invention includes following steps:
The first step, compound concentration are the aluminum saline solution and the NaOH aqueous solution of 1M-3M, and the NaOH aqueous solution is added dropwise to aluminum saline solution, and the pH value that makes reaction soln is 5.
Used aluminium salt is a kind of in Tai-Ace S 150, aluminum nitrate and the aluminum chloride.
With the NaOH aqueous solution is precipitation agent, and at the boehmite early growth period, the boehmite of formation is the boehmite nanometer layer that is of a size of 50-100nm, shorter by the boehmite one dimension Nano structure length that the mechanism of curling forms, and is 50-100nm.
Second step, the suspension that the first step generates is transferred in the autoclave, be heated to 200-220 ℃ of insulation, cool to room temperature with the furnace.
Described insulation, its time is 24-72 hour.
In the 3rd step, reacted product is realized solid-liquid separation after filtration, and throw out is with pure water rinsing repeatedly, dry then, obtains boehmite presoma nanometer rod.
Described drying, its temperature are 100 ℃.
Described drying, its time is 12-24 hour.
The 4th step was heated to 500 ℃ of-800 ℃ of insulations with boehmite presoma nanometer rod, changed the similar Nano bars of alumina of pattern into.
Described insulation, its time is 2-6 hour.
The present invention utilize boehmite (laminate structure of γ-AlOOH) prepare boehmite (nano wire of γ-AlOOH), boehmite (in the laminate structure of γ-AlOOH), in one deck, each Al
3+Six O around ion is collaborative
2-Ion constitutes an AlO
6Octahedra unit, layer with layer between be connected by hydrogen bond by hydroxyl.Under acidic conditions, contain excessive hydrogen ion in the reaction soln, it can make boehmite, and (γ-AlOOH) hydroxyl of interlayer-oxygen lone electron pair is protonated, forms the ligand of water, and (γ-AlOOH) laminate structure is separated to make boehmite.(γ-AlOOH) laminar surface is full of unsettled hydroxyl, and (layer of γ-AlOOH) can curl into the boehmite (one dimension Nano structure of γ-AlOOH) by curling growth mechanism (rolling growth) to boehmite subsequently because the boehmite that is separated from each other.
Because with the NaOH aqueous solution is precipitation agent, (γ-AlOOH) layer is of a size of 50-100nm to the boehmite of preparing, (γ-AlOOH) length-to-diameter ratio of one dimension Nano structure is less to curl into boehmite by the growth mechanism (rolling growth) that curls, therefore be 5-15, the product of preparation is the boehmite (nanometer rod (length-to-diameter ratio is greater than 50) of γ-AlOOH).
Compared with prior art, the present invention is a raw material with aluminium salt and NaOH, and adopting hydro-thermal reaction to prepare diameter is 10-20nm, and length is 100-300nm, and length-to-diameter ratio is 5-15, regular shape, ganoid boehmite presoma nanometer rod and Nano bars of alumina.Because the Nano bars of alumina of preparation has unique one-dimentional structure, can be used for the fabric reinforcement of ceramic composite.
Description of drawings
Fig. 1 is the inventive method schema;
Fig. 2 is an embodiment of the invention gained alumina nanowires shape appearance figure.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Below the concrete implementation step of each embodiment, as shown in Figure 1.
Embodiment 1:
Compound concentration is the aluminum sulfate aqueous solution of 1M and the NaOH aqueous solution of 1M, and the NaOH aqueous solution is added dropwise to aluminum sulfate aqueous solution, and the pH value that makes reaction soln is 5.The suspension that generates is transferred in the autoclave, be heated to 220 ℃ of insulations 24 hours, cool to room temperature with the furnace.Reacted product is realized solid-liquid separation after filtration, and throw out with pure water rinsing repeatedly, was descended dry 12 hours at 100 ℃ then, obtains boehmite presoma nanometer rod.Boehmite presoma nanometer rod is heated to 800 ℃ of insulations 2 hours, changes Nano bars of alumina into.As shown in Figure 2, the boehmite presoma nanometer rod and the Nano bars of alumina of preparation are monocrystalline, its diameter 10-20nm, and length 100-300nm, length-to-diameter ratio 5-15, regular shape, the surface is straight smooth.
Embodiment 2:
Compound concentration is the aluminum nitrate aqueous solution of 2M and the NaOH aqueous solution of 2M, and the NaOH aqueous solution is added dropwise to aluminum nitrate aqueous solution, and the pH value that makes reaction soln is 5.The suspension that generates is transferred in the autoclave, be heated to 210 ℃ of insulations 48 hours, cool to room temperature with the furnace.Reacted product is realized solid-liquid separation after filtration, and throw out with pure water rinsing repeatedly, was descended dry 18 hours at 100 ℃ then, obtains boehmite presoma nanometer rod.Boehmite presoma nanometer rod is heated to 600 ℃ of insulations 4 hours, changes Nano bars of alumina into.The boehmite presoma nanometer rod and the Nano bars of alumina of preparation are monocrystalline, its diameter 10-20nm, and length 100-300nm, length-to-diameter ratio 5-15, regular shape, the surface is straight smooth.
Embodiment 3:
Compound concentration is the aluminum chloride aqueous solution of 3M and the NaOH aqueous solution of 3M, and the NaOH aqueous solution is added dropwise to aluminum chloride aqueous solution, and the pH value that makes reaction soln is 5.The suspension that generates is transferred in the autoclave, be heated to 200 ℃ of insulations 72 hours, cool to room temperature with the furnace.Reacted product is realized solid-liquid separation after filtration, and throw out with pure water rinsing repeatedly, was descended dry 24 hours at 100 ℃ then, obtains boehmite presoma nanometer rod.Boehmite presoma nanometer rod is heated to 500 ℃ of insulations 6 hours, changes Nano bars of alumina into.The boehmite presoma nanometer rod and the Nano bars of alumina of preparation are monocrystalline, its diameter 10-20nm, and length 100-300nm, length-to-diameter ratio 5-15, regular shape, the surface is straight smooth.
Claims (7)
1, a kind of preparation method of Nano bars of alumina is characterized in that, may further comprise the steps:
The first step, compound concentration are the aluminum saline solution and the NaOH aqueous solution of 1M-3M, and the NaOH aqueous solution is added dropwise to aluminum saline solution, and the pH value that makes reaction soln is 5;
Second step, the suspension that the first step generates is transferred in the autoclave, be heated to 200-220 ℃ of insulation, cool to room temperature with the furnace;
In the 3rd step, reacted product is realized solid-liquid separation after filtration, and throw out is with pure water rinsing repeatedly, dry then, obtains boehmite presoma nanometer rod;
The 4th step was heated to 500 ℃ of-800 ℃ of insulations with boehmite presoma nanometer rod, changed the similar Nano bars of alumina of pattern into.
2, the preparation method of Nano bars of alumina according to claim 1 is characterized in that, in the first step, used aluminium salt is a kind of in Tai-Ace S 150, aluminum nitrate and the aluminum chloride.
3, the preparation method of Nano bars of alumina according to claim 1 is characterized in that, in second step, and described insulation, its time is 24-72 hour.
4, the preparation method of Nano bars of alumina according to claim 1 is characterized in that, in the 3rd step, described drying, its temperature are 100 ℃.
5, according to the preparation method of claim 1 or 4 described Nano bars of alumina, it is characterized in that, in the 3rd step, described drying, its time is 12-24 hour.
6, the preparation method of Nano bars of alumina according to claim 1 is characterized in that, in the 4th step, and described insulation, its time is 2-6 hour.
7, the preparation method of Nano bars of alumina according to claim 1 is characterized in that, described Nano bars of alumina is a monocrystalline, and its diameter is 10-20nm, and length is 100-300nm, and length-to-diameter ratio is 5-15.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102372298A (en) * | 2010-08-24 | 2012-03-14 | 中国石油化工股份有限公司 | Alumina nanobelt and production method thereof |
| CN101885501B (en) * | 2009-05-13 | 2012-06-27 | 中国石油化工股份有限公司 | Preparation method of one-dimensional alumina nanowire/nano rod |
| CN102557092A (en) * | 2012-01-06 | 2012-07-11 | 重庆理工大学 | Preparation method of alumina nanometer rod with short length-diameter ratio |
| CN101774533B (en) * | 2009-09-28 | 2014-02-19 | 南京大学 | Preparation method for gamma-alumina nanotube with prior exposure of (111) face |
| CN105174293A (en) * | 2015-09-10 | 2015-12-23 | 中国海洋石油总公司 | Preparation method of pseudo-boehmite with centralized pore size distribution |
| CN105643480A (en) * | 2016-01-14 | 2016-06-08 | 洛阳三睿宝纳米科技有限公司 | Nano fiber oilstone |
| CN106115754A (en) * | 2016-06-29 | 2016-11-16 | 北京化工大学 | A kind of method preparing transparent aluminium hydroxide liquid dispersion |
| CN106242625A (en) * | 2016-08-02 | 2016-12-21 | 西安电子科技大学 | The low temperature preparation method of gas sensor sensitive layer ultrathin alumina protecting film |
| CN106268969A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of catalyst carrier and preparation method thereof and Hydrodemetalation catalyst |
| CN107879368A (en) * | 2017-12-06 | 2018-04-06 | 宁波爱克创威新材料科技有限公司 | Nano aluminium oxide and preparation method thereof |
| CN107959053A (en) * | 2017-11-28 | 2018-04-24 | 南开大学 | Improve the feature electrolyte and preparation method of nickelic positive electrode cyclical stability |
-
2008
- 2008-07-10 CN CNA2008100404616A patent/CN101318677A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885501B (en) * | 2009-05-13 | 2012-06-27 | 中国石油化工股份有限公司 | Preparation method of one-dimensional alumina nanowire/nano rod |
| CN101774533B (en) * | 2009-09-28 | 2014-02-19 | 南京大学 | Preparation method for gamma-alumina nanotube with prior exposure of (111) face |
| CN102372298A (en) * | 2010-08-24 | 2012-03-14 | 中国石油化工股份有限公司 | Alumina nanobelt and production method thereof |
| CN102372298B (en) * | 2010-08-24 | 2013-10-09 | 中国石油化工股份有限公司 | Alumina nanobelt and production method thereof |
| CN102557092A (en) * | 2012-01-06 | 2012-07-11 | 重庆理工大学 | Preparation method of alumina nanometer rod with short length-diameter ratio |
| CN106268969A (en) * | 2015-06-12 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of catalyst carrier and preparation method thereof and Hydrodemetalation catalyst |
| CN105174293A (en) * | 2015-09-10 | 2015-12-23 | 中国海洋石油总公司 | Preparation method of pseudo-boehmite with centralized pore size distribution |
| CN105643480A (en) * | 2016-01-14 | 2016-06-08 | 洛阳三睿宝纳米科技有限公司 | Nano fiber oilstone |
| CN106115754A (en) * | 2016-06-29 | 2016-11-16 | 北京化工大学 | A kind of method preparing transparent aluminium hydroxide liquid dispersion |
| CN106242625A (en) * | 2016-08-02 | 2016-12-21 | 西安电子科技大学 | The low temperature preparation method of gas sensor sensitive layer ultrathin alumina protecting film |
| CN107959053A (en) * | 2017-11-28 | 2018-04-24 | 南开大学 | Improve the feature electrolyte and preparation method of nickelic positive electrode cyclical stability |
| CN107879368A (en) * | 2017-12-06 | 2018-04-06 | 宁波爱克创威新材料科技有限公司 | Nano aluminium oxide and preparation method thereof |
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