CN1704330A - Process for preparing low-dimensional aluminium nitride nano materials - Google Patents

Process for preparing low-dimensional aluminium nitride nano materials Download PDF

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Publication number
CN1704330A
CN1704330A CN 200410020610 CN200410020610A CN1704330A CN 1704330 A CN1704330 A CN 1704330A CN 200410020610 CN200410020610 CN 200410020610 CN 200410020610 A CN200410020610 A CN 200410020610A CN 1704330 A CN1704330 A CN 1704330A
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China
Prior art keywords
preparing low
nano wire
dimensional
aln
aluminium nitride
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CN 200410020610
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CN1278927C (en
Inventor
贺连龙
李志杰
沈志奇
王福
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Publication of CN1278927C publication Critical patent/CN1278927C/en
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Abstract

The invention relates to a process for preparing low dimensional nano-materials which comprises, using metallic aluminium as anode, using metal wolfram as cathode, employing direct current arc plasma technique under the condition of mixed hydrogen and nitrogen, wherein the processing parameter include, volumetric ratio of H2:N2=0.2-1.5, overall pressure between the range of 6000-9500Pa, the electric arc current = 150-300A, the gas flow = 5-15l/s, arc ignition time = 0.5-6 hours.

Description

The method for preparing low-dimensional aluminum nitride nanometer material
Technical field
The present invention relates to semiconductor nano material, specifically a kind of low-dimensional aluminium nitride (AlN) preparation of nanomaterials.
Background technology
The conventional semiconductor material is difficult to satisfy the requirement of super large unicircuit, restriction automatization and intelligentized development.The super large unicircuit is badly in need of micro devices, the i.e. device of nanoscale.The AlN nano wire is a kind of semiconductor nano material, can make nano level PN junction.The method that now prepares the AlN nano wire has powder sintering, chemical cracking method, template or the like.The prior art weak point is that purity is low, and purification difficult is because of the remaining residue of chemical reaction is difficult for removing.
Summary of the invention
In order to overcome the deficiency of technology among the existing preparation method, the purpose of this invention is to provide that a kind of purity height, time are short, usefulness DC arc plasma legal system simple to operate is equipped with the method for low-dimensional AlN nano-material.
To achieve these goals, technical solution of the present invention is: with the metallic aluminium be starting material as anode, as negative electrode, under the mixing condition of hydrogen and nitrogen, adopt the DC arc plasma technology to carry out with tungsten, its processing parameter is: H 2: N 2In volume ratio is (to be H under 0.2~1.5 condition 2: N 2Volume ratio be 1: 5~3: 2); The control total pressure is in 6000~95000Pa scope, and flame current is 150~300A, and gas flow is 5~15l/s, and the scratch start time is 0.5 hour~6 hours;
Wherein: the purity of described aluminium is more than or equal to 99%.
Compared with prior art, the present invention has following advantage:
1. purity height.Adopt the high purity of the low-dimensional AlN nano material of the inventive method preparation to show that diameter Distribution is 20~110nm, length reaches 0.5~20 μ m, and the crystalline lattice parameter is a=0.31nm and c=0.49nm.
2. generated time is short.The present invention only is 0.5 hour~6 hours, because purification need not be loaded down with trivial details, that grow is slowly once made, so compared with prior art the time is few, cost is low.
3. simple to operate, be beneficial to enforcement.
Description of drawings
Fig. 1 is the stereoscan photograph of first embodiment of the invention AlN nano wire.
Fig. 2 is the transmission electron microscope photo of first embodiment of the invention nano wire.
Fig. 3 is the selected area electron diffraction spectrum of first embodiment of the invention AlN nano wire.
Fig. 4 is the amplification transmission electron microscope photo of first AlN nano wire among Fig. 2.
The height explanation transmission electron microscope photo of Fig. 5 first embodiment of the invention AlN nano wire.
Fig. 6 is the selected area electron diffraction spectrum of first embodiment of the invention AlN nano wire.
Fig. 7 is the stereoscan photograph (0.5 hour) of second embodiment of the invention AlN nano wire.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1
Present embodiment adopts physical vapor deposition to prepare low-dimension nano material method, i.e. DC arc plasma method.Be specially: with rafifinal (purity equals 99.9%) be starting material as anode, with tungsten as negative electrode, (H under the mixing condition of hydrogen and nitrogen 2: N 2Volume ratio is 1: 3), total pressure is 95000Pa, flame current is 300A, gas flow 5l/s, scratch start 4 hours is prepared a large amount of AlN nano wires.
Get the present embodiment sample and be placed on the specimen holder, send in the JSM6301F scanning electron microscope and observe, find to have a lot of nano wires.As shown in Figure 1, preparing the AlN nano wire is a kind of wide gap belt semiconductor material, and its diameter Distribution is 20~110nm, and length reaches 0.5~20 μ m, and the AlN nano wire is a hexagonal structure.The crystalline lattice parameter is a=0.31nm and c=0.49nm.As shown in Figure 2, in above-mentioned sample, get a part of sample and put alcohol (analytical pure) into, use ultrasonic oscillation 10 minutes, drip to again on the aperture plate, send at last to observe on the JEOL2010 transmission electron microscope and determine that nano wire is the AlN nano wire with the suction pipe sucking-off; Its electron diffraction spectrum analysis is referring to Fig. 3.As Fig. 4 is that AlN nano wire among Fig. 2 amplifies transmission electron microscope photo, and Fig. 5 is the high-resolution-ration transmission electric-lens photo of locating shown in the arrow among Fig. 4, and Fig. 6 is corresponding selected area electron diffraction photo, and their determine that further nano wire is the AlN nano wire.
Present embodiment is equipped with low-dimensional AlN nano-material with the DC arc plasma legal system, the raw material and the working gas that use are highly purified, so the low-dimensional AlN nano material purity height of preparation, and this method is simple to operate, is the preparation method of the high-quality AlN nano wire of a kind of acquisition of economy.
Embodiment 2
Difference from Example 1 is:
With purity be 99.99% aluminium be starting material as anode, as negative electrode, be 2: 5 with tungsten at the mixed volume ratio of hydrogen and nitrogen, total pressure is 6000Pa, flame current is 150A, gas flow 15l/s, scratch start 0.5 hour.
It is 10~30nm that present embodiment is prepared a large amount of AlN wire diameter distribution, and length reaches 0.1~0.5 μ m, and the AlN nano wire is a hexagonal structure, and the crystalline lattice parameter is a=0.31nm and c=0.49nm (referring to Fig. 7).

Claims (2)

1. method for preparing low-dimensional aluminum nitride nanometer material is characterized in that: with the metallic aluminium be starting material as anode, as negative electrode, under the mixing condition of hydrogen and nitrogen, adopt the DC arc plasma technology to carry out with tungsten, its processing parameter is: H 2: N 2In volume ratio is under 0.2~1.5 condition, and the control total pressure is in 6000~95000Pa scope, and flame current is 150~300A, and gas flow is 5~15l/s, and the scratch start time is 0.5 hour~6 hours.
2. according to the described method for preparing low-dimensional aluminum nitride nanometer material of claim 1, it is characterized in that: the purity of described aluminium is more than or equal to 99%.
CN 200410020610 2004-05-26 2004-05-26 Process for preparing low-dimensional aluminium nitride nano materials Expired - Fee Related CN1278927C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200410020610 CN1278927C (en) 2004-05-26 2004-05-26 Process for preparing low-dimensional aluminium nitride nano materials

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200410020610 CN1278927C (en) 2004-05-26 2004-05-26 Process for preparing low-dimensional aluminium nitride nano materials

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CN1704330A true CN1704330A (en) 2005-12-07
CN1278927C CN1278927C (en) 2006-10-11

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100434573C (en) * 2006-04-03 2008-11-19 深圳大学 Method for developing aluminum nitride crystal in large size through flow of plasma flame
CN101880857A (en) * 2010-06-10 2010-11-10 沈阳工业大学 Direct-current arc method for preparing Al nano tadpoles
CN104370278A (en) * 2014-10-23 2015-02-25 西安理工大学 Preparation method of high-purity nano-AlN powder

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100434573C (en) * 2006-04-03 2008-11-19 深圳大学 Method for developing aluminum nitride crystal in large size through flow of plasma flame
CN101880857A (en) * 2010-06-10 2010-11-10 沈阳工业大学 Direct-current arc method for preparing Al nano tadpoles
CN101880857B (en) * 2010-06-10 2012-03-14 沈阳工业大学 Direct-current arc method for preparing Al nano tadpoles
CN104370278A (en) * 2014-10-23 2015-02-25 西安理工大学 Preparation method of high-purity nano-AlN powder
CN104370278B (en) * 2014-10-23 2016-07-06 西安理工大学 A kind of preparation method of high-purity nano AlN powder

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