CN102383105A - Method for preparing quasi-one-dimensional metallic oxide nano material - Google Patents
Method for preparing quasi-one-dimensional metallic oxide nano material Download PDFInfo
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- CN102383105A CN102383105A CN2011103542304A CN201110354230A CN102383105A CN 102383105 A CN102383105 A CN 102383105A CN 2011103542304 A CN2011103542304 A CN 2011103542304A CN 201110354230 A CN201110354230 A CN 201110354230A CN 102383105 A CN102383105 A CN 102383105A
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Abstract
The invention discloses a method for preparing a quasi-one-dimensional metallic oxide nano material. The nano material is a nano wire of a metallic oxide; the length of the nano material is in a micron level, and the width and the height of the nano material are only in a nano level; and the material is in an amorphous structure state. In the method, two reactants are fed into a reaction cavity in batches by adopting an atomic layer deposition technology; the reactants adsorbed on the surface of a substrate generate chemical reaction so as to produce the metallic oxide nano wire; aluminum oxide nano wires are parallel to one another, so a growth characteristic with certain preferred orientation is represented; meanwhile, the method is easy to operate and low in cost; control can be realized by programming; and the method is easy to implement and popularize industrially.
Description
Technical field
The present invention relates to accurate one-dimensional nano line preparation methods, a kind of method that adopts technique for atomic layer deposition to prepare metal oxide nano-wire is provided especially.The metal oxide nano-wire that this method is prepared shows certain preferred orientation growth characteristics, and can be easy to carry out the control of nanowire height and width, thereby for preparing different size metal nano wire material a kind of possibility is provided.
Background technology
The grain-size of material reach 100nm when following or a certain dimension of material reached nano level, we are defined as nano material this kind material.Nano material is the totally different performance of a series of and conventional coarse grain material because of its particular structure has, and has obtained paying close attention to widely and studying all the time.
Nanometer material science is carried out deep research, at first need prepare suitable nano material.At present, there are many scientists just being devoted to the research preparation work of nano material in the world wide, and obtained many breakthrough achievements in research.In present experiment and the research, the method that obtains the distribution of different size crystal grain has usually: the control ball milling time; Recrystallize and secondary recrystallization; And stress induced grain growth etc.Obtaining many significant achievements in research aspect the control material dimension too; Your Clotho doctor of Englishize scholar Harold water in 1985 and U.S. scientist Richard Si Moli have prepared first kind of soccerballene in the Rice University, this soccerballene is the nano material that zero dimension is only arranged; Japan in 1991 builds the breadboard physicist's Sumio Iijima of ripple NEC and under high-resolution electron microscopy, has found a kind of unidimensional tubulose carbon nanomaterial that only has, Here it is carbon nanotube; The scientist An Deliehaimu of the University of Manchester of Britain in 2004 etc. has prepared the accurate two-dimensional material that several atomic layer level thickness are only arranged through " micromechanics is peeled off " method, i.e. Graphene.
After a certain dimension of macroscopic block materials got into Nano grade, huge variation can take place in its performance.Accurate two-dimensional material Graphene is the maximum material of present known hardness, and macroscopic carbon material graphite is a kind of soft material with lubricant effect.This shows that the change of dimension can make material obtain some very particular performances, more and more, more and more deep to the research of the nano material of preparation different dimensions in recent years.
Summary of the invention
The object of the present invention is to provide a kind of material preparation method of novel metal oxide nano wire.The characteristic of this material is: the length of metal oxide nano-wire can reach micron level, and width and nano level is highly only arranged is typical 1-dimention nano wire material, and presents non-crystal structure.The nano wire of preparing under this technology has certain preferred orientation growth characteristics, can be easy to through control growing time, depositing temperature the metal oxide nano-wire form controlled.Simultaneously, operation is simple for this method, and cost is lower, is easy in industry, realize and promote.
The method that the present invention adopted; Cardinal principle is: in the ald process of growth; Adopt high pure nitrogen that precursor trimethylaluminium, the ydrogen peroxide 50 of reaction needed are blown in the reaction chamber in batches, the saturated precursor that is adsorbed on substrate surface reacts to each other, and generates aluminum oxide.Under specific growth temperature, depositing time, (Highly Oriented Pyrolytic Graphite HOPG) will grow the aluminum oxide (Al of linear structure (Wire-like structure) to employed highly oriented pyrolytic graphite in the experiment on the substrate surface
2O
3).
This method specifically comprises the following steps:
1) adopts the normal transparent adhesive tape that highly oriented pyrolytic graphite is carried out placing it in the growth chamber of atomic layer deposition apparatus after micromechanics peels off, prepare to carry out nanowire growth;
2) starting material trimethylaluminium, the ydrogen peroxide 50 that needs is reacted packed in the reaction source, and temperature of reaction is set at 150 ℃, be evacuated to 8mTorr after start-up routine control reaction process automatically; Adopt high-purity N
2As the auxiliary atmosphere of reaction, the phenomenon of the thing oxidation that guarantees in reaction chamber, can not react;
3) in the nanowire growth process; The temperature-stable that makes reaction chamber through the wire spiral type of heating is in predefined temperature of reaction; The reaction and the flush time of reaction source trimethylaluminium are respectively: 4s, 20s; The reaction of ydrogen peroxide 50 and flush time are respectively 0.2s, 45s, through the program of setting reaction are repeated;
4) height of alumina nanowires and width are controlled through control reaction cycle.
This method adopts technique for atomic layer deposition, and two kinds of reactants are passed in the reaction chamber in batches, and the reactant generation chemical reaction that is adsorbed on substrate surface generates metal oxide nano-wire.Be parallel to each other between the alumina nanowires, show the growth characteristics of certain preferred orientation; Simultaneously, this method is simple to operate, and cost is lower, can control through coding, is easy in industry, realize and promote.
Description of drawings
Fig. 1 is the surface topography SEM figure of the aluminum oxide film of 150 ℃ of growth temperatures, deposition 120 cycles.
Fig. 2 is the surface topography SEM figure of the alumina nanowires of 150 ℃ of growth temperatures, deposition 150 cycles.
Fig. 3 is for being the surface topography SEM figure of the alumina nanowires of 50 ℃ of growth temperatures, deposition 120 cycles.
Fig. 4 is an alumina nanowires transmission electron microscope microstructure synoptic diagram.
Fig. 5 is the diffraction spot point diagram of aluminum oxide.
Table 1 is the component concentration of alumina nanowires.
The embodiment that provides below in conjunction with accompanying drawing and contriver does further detailed description to the present invention.
Embodiment
The invention provides a kind of technique for atomic layer deposition that utilizes, thereby deposition is prepared a kind of method of metal oxide nano-wire.Present embodiment adopts trimethylaluminium and ydrogen peroxide 50 as growth source, and high pure nitrogen is prepared aluminum oxide (Al as the auxiliary atmosphere of reaction
2O
3) nano wire.
Aluminum oxide (Al
2O
3) the concrete technological process of nano wire:
1) peel off with the extexine of common scotch tape with the highly oriented pyrolytic graphite of A grade, the substrate after will peeling off is rapidly put into the growth chamber of atomic layer deposition apparatus, closes chamber.
2) in the reaction source with trimethylaluminium and ydrogen peroxide 50 load facility, after the inspection gas circuit, the equipment growth chamber is vacuumized processing.
3) temperature with reaction chamber is set to temperature of reaction, and starting switch heats, temperature control software the most at last temperature-stable at 150 ℃.
4) base vacuum of reaction chamber reaches back 8mTorr, and the gas cylinder top hole pressure of high pure nitrogen is set in about 0.3MPa, and the line program of going forward side by side is set: warm up time: 20min; Trimethylaluminium be blown into the time and flush time is respectively: 4s, 20s; Ydrogen peroxide 50 be blown into the time and flush time is respectively: 0.2s, 45s; Reaction cycle: 120 or 150 etc.
5) start setting program, carry out aluminum oxide (Al
2O
3) deposition growing.
In order to compare, accompanying drawing 3 is the surface topography SEM figure of 50 ℃ of growth temperatures, the aluminum oxide of deposition cycle under 120 weeks.On scheming, can find out that the aluminum oxide under this technology is a kind of form of wire too.Can draw such conclusion by Fig. 2, the correlated result of Fig. 3:, can control to the form of aluminum oxide through changing growth temperature, depositing time.
Accompanying drawing 4, accompanying drawing 5 are respectively high resolution microstructure, the diffraction spot point diagram of aluminum oxide, can know that for dizzy shape the aluminum oxide of preparation is a non-crystalline state from diffraction spot.
Table 1
More than these, explain that method of the present invention can prepare amorphous alumina nanowires, and can control the form of nano wire through changing depositing operation (growth temperature, depositing time).Simultaneously, because growth temperature and sedimentation rate relative fixed,, be convenient to realize suitability for industrialized production and popularization through the writing and setting of related computer program.
Claims (2)
1. the preparation method of a quasi-one-dimensional metal oxide nano-material is characterized in that, this method comprises the following steps:
1) adopts the normal transparent adhesive tape that highly oriented pyrolytic graphite is carried out placing it in the growth chamber of atomic layer deposition apparatus after micromechanics peels off, prepare to carry out nanowire growth;
2) starting material trimethylaluminium, the ydrogen peroxide 50 that needs is reacted packed in the reaction source, and temperature of reaction is set at 150 ℃, be evacuated to 8mTorr after start-up routine control reaction process automatically; Adopt high-purity N
2As the auxiliary atmosphere of reaction, the phenomenon of the thing oxidation that guarantees in reaction chamber, can not react;
3) in the nanowire growth process; The temperature-stable that makes reaction chamber through the wire spiral type of heating is in predefined temperature of reaction; The reaction and the flush time of reaction source trimethylaluminium are respectively: 4s, 20s; The reaction of ydrogen peroxide 50 and flush time are respectively 0.2s, 45s, through the program of setting reaction are repeated;
4) height of alumina nanowires and width are controlled through control reaction cycle.
2. method according to claim 1 is characterized in that, described micromechanics is peeled off adhesive tape is adhered on the surface of highly oriented pyrolytic graphite, evenly firmly the pyrolytic graphite outermost layer is torn, and exposes its unsalted surface.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110042365A (en) * | 2019-03-04 | 2019-07-23 | 中国科学院物理研究所 | A kind of Atomic layer deposition method in two-dimensional material surface growth aluminium oxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143708A (en) * | 2007-08-17 | 2008-03-19 | 中国科学技术大学 | Method for preparing ultra-thin two-dimension graphite sheet |
| CN101688300A (en) * | 2007-07-03 | 2010-03-31 | Beneq有限公司 | Method in depositing metal oxide materials |
| CN101974734A (en) * | 2010-11-30 | 2011-02-16 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing substrate material with multilayer composite protective film |
-
2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101688300A (en) * | 2007-07-03 | 2010-03-31 | Beneq有限公司 | Method in depositing metal oxide materials |
| CN101143708A (en) * | 2007-08-17 | 2008-03-19 | 中国科学技术大学 | Method for preparing ultra-thin two-dimension graphite sheet |
| CN101974734A (en) * | 2010-11-30 | 2011-02-16 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing substrate material with multilayer composite protective film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110042365A (en) * | 2019-03-04 | 2019-07-23 | 中国科学院物理研究所 | A kind of Atomic layer deposition method in two-dimensional material surface growth aluminium oxide |
| CN110042365B (en) * | 2019-03-04 | 2020-09-22 | 中国科学院物理研究所 | Atomic layer deposition method for growing aluminum oxide on surface of two-dimensional material |
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Application publication date: 20120321 |