CN102505144B - Preparation method for directional growth of organic micro/nano structure - Google Patents
Preparation method for directional growth of organic micro/nano structure Download PDFInfo
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- CN102505144B CN102505144B CN201110342746.7A CN201110342746A CN102505144B CN 102505144 B CN102505144 B CN 102505144B CN 201110342746 A CN201110342746 A CN 201110342746A CN 102505144 B CN102505144 B CN 102505144B
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Abstract
The invention discloses a preparation method for the directional growth of an organic micro/nano structure. Organic micro/nano wires are directionally prepared on the basis of a substrate with a surface periodic grating structure by a physical vapor deposition method, the growth size and growth density of the organic micro/nano wires are highly controllable by controlling growth conditions such as air pressure, air flow, temperature, heat preservation time, deposition area position and the like, and a simple and effective preparation method for the highly aligned and directional growth of super-long organic micro/nano wires in a two-dimensional plane is provided. The method is simple and practicable, flexible, high in extensibility and suitable for the directional growth of various organic compound micro/nano wires, and has great significance for preparing nano devices based on the organic micro/nano structure and further integrating the nano devices, and the length of the prepared micro/nano wires is from tens of micrometers to millimeter magnitude.
Description
Technical field
The present invention relates to nanometer physical field, be specifically related to a kind of preparation method of organic micro-nano rice noodles oriented growth of overlength.
Background technology
The micro nano structure that highly collimates oriented growth or arrange has indispensable effect in nano-device is prepared and be integrated.In addition, utilize and there are the overlength micro-nano rice noodles of big L/D ratio, can realize the leap of micro/nano-scale and macro-scale, facilitate the preparation, integrated and interconnected of nano-device.The research of above-mentioned two aspects has caused people's very big interest.But due to the singularity of organic materials self structure and the complicacy of preparation process, the preparation of organic nano line orientation array structure is often difficult to realize.In order to prepare organic nano-wire array, there is report to apply template (J. L. Yang, S. Schumann and T. S. Jones*. J. Mater. Chem. 2011,21,5812 – 5816), organic nano linear array poor controllability prepared by this this method, process is comparatively complicated; Also there is report first by template synthesis inorganic nano linear array, then utilize again sedimentation to be coated with machine material (Mi Ouyang, Ru Bai, Lin Chen, Ligong Yang, Mang Wang, Hongzheng Chen*. J. Phys. Chem. C 2008,112,11250 – 11256) prepare organic nano-wire array, but this method is confined to the organic materials of minority and inorganic materials lattice match, and nano-wire array surfaceness is larger; Also has report (Yong Sheng, Zhao, Peng Zhan, Jaemyung Kim, Cheng Sun, and Jiaxing Huang. Acs. Nano 2010,1630-1636) to specific organic materials based on different base growth of vertical array, but can only be for this specific organic materials, method expansion is poor, and building-up process is also comparatively complicated.
Summary of the invention
The deficiency existing in order to overcome prior art, the invention provides a kind of preparation method of directional growth of organic micro/nano structure, utilize physical vaporous deposition, substrate preparation based on having surface period optical grating construction highly collimates organic micro-nano rice noodles of oriented growth, realize the control to micro-nano linear dimension, density and length by controlling growth conditions, obtain overlength micro-nano rice noodles periodic structure.This preparation method technique is simple, with low cost, controllability is good, be applicable to the feature such as large area micro-nano rice structure direction growth, the preparation of organic nano device and integrated in there is important application prospect.
To achieve the above object of the invention, the technical solution adopted in the present invention is: by controlling carrier gas air-flow, chamber pressure, phthalein mountain valley with clumps of trees and bamboo copper compound (CuPc) is evaporated under its sublimation temperature, and be transported to sedimentary province by carrier gas air-flow, regulate sedimentary province grating placing height, under the induction of grating substrate, be self-assembled into the highly micro-nano rice noodles of collimation along grating raceway groove.Specifically comprise the following steps:
1), take phthalein mountain valley with clumps of trees and bamboo copper compound (CuPc) powder of certain mass, with neutral alumina (Al
2o
3) powder pours in porcelain boat after mixing with the mass ratio of 1:10-1:100, is placed in the heating zone of physical deposition method (PVD) device, in silica tube.
2), grating substrate is fixed on slide glass after, be placed in the low temperature depositing district of physical deposition method, and padded with porcelain boat, grating planar is positioned in the middle of silica tube.
3), silica tube is evacuated to 3Pa, pass into subsequently the argon gas of 60 SCCM as carrier gas, keep stable air-flow velocity and air pressure, the air pressure in general control silica tube tube chamber is 220 Pa.
4), physical deposition method program is set, phthalein mountain valley with clumps of trees and bamboo copper compound powder is heated to after a stable temperature, be incubated for some time between 400 DEG C～450 DEG C, generally, with 420 DEG C of equilibrium temperatures for this reason, the temperature of now grating substrate is about 200
oc.Growth time is 3 hours, while being cooled to 30 DEG C, takes out sample after growth finishes, and obtains organic micro-nano rice noodles of oriented growth.
Compared with prior art, the invention has the advantages that:
The advantage of the inventive method is:
1, preparation process is non-solution method, and gained sample purity is high;
2, technique is simple, with low cost;
3, be applicable to big area preparation;
4, can expand to multiple organic materials.
To sum up, because preparation technology of the present invention is simple, controllability is good, flexibly and can big area preparation, in the organic micro nano structure of big area directional preparation, has important application prospect.
Embodiment
The technical solution adopted in the present invention is: first organic evaporating source is heated, make it reach sublimation temperature, depress at certain saturation steam, sample molecule, under the transporting of carrier gas, is taken to sedimentary province.Chen Ji district temperature is lower, and organic molecule regelation, goes forward side by side and nucleating growth, and due to the special molecular structure of organic molecule, it tends at specific direction oriented growth, thereby obtains the micro-nano rice noodles of one-dimentional structure.By introducing grating substrate, because air-flow in grating raceway groove is more slow, nucleation site is abundant, and organic micro-nano rice noodles are nucleation in grating raceway groove preferentially, and due to the inducing action of grating, makes micro-nano rice noodles along grating channel height oriented growth.
Concrete steps comprise: take a certain amount of CuPc powder, with Al
2o
3powder is poured in porcelain boat after mixing with the mass ratio of 1:10-1:100, is placed in the heating zone of physical vaporous deposition silica tube.
After grating substrate is fixed on sheet glass, be placed in the sedimentary province of physical vaporous deposition.The program of physical vaporous deposition is set: heating-up time, soaking time, holding temperature, air-flow velocity etc.
Be cooled to 30 DEG C after EP (end of program) time, take out sample.
By some condition of reprogramming, obtain different size, the controlled organic micro/nano structure of density.
Experimental technique described in following embodiment, if no special instructions, is ordinary method; Described sample and material, if no special instructions, all can obtain from commercial channels.
Embodiment 1
Take a certain amount of CuPc powder, with Al
2o
3powder is poured in porcelain boat after mixing with certain mass ratio, is placed in the heating zone of physical vaporous deposition silica tube.After grating substrate is fixed on sheet glass, be placed in the sedimentary province of physical vaporous deposition.Set the program of physical vaporous deposition, the heating-up time is made as 40 min, and soaking time is made as 1 h, and holding temperature is made as 420 DEG C, and air-flow is argon gas, and flow velocity is 40 sccm.Be cooled to 30 DEG C after EP (end of program) time, take out sample.Can obtain the sparse micro-nano structure product of a kind of orientation.
Embodiment 2
In embodiment 1, holding time, air-flow velocity increases, and other operation is constant, obtains organic micro-nano rice noodles of another kind of form.
Embodiment 3
In embodiment 1, holding time, air-flow velocity increases, and the grating substrate of sedimentary province is padded with porcelain boat, and other operation is constant, obtains organic micro-nano rice noodles of another form.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (3)
1. a preparation method for CuPc micro-nano structure oriented growth, comprises the following steps:
After CuPc is mixed with the mass ratio of 1:10 with alumina powder, pack porcelain boat into, be placed in the middle heating zone of physical vapor deposition device;
The grating substrate of periodic structure is fixed on to the low temperature depositing district that is placed on physical vapor deposition device on sheet glass, argon hydrogen mixture is introduced in tube chamber, keep stable air-flow velocity and air pressure, be incubated 1-3 hour after being warming up to 420 DEG C;
In the time that cavity temperature is down to room temperature, take out sample, obtain along the periodically CuPc micro wire of growth of grating raceway groove.
2. preparation method according to claim 1, further comprising the steps of: regulate the placing height of sedimentary province grating, under the induction of grating substrate, CuPc is self-assembled into the highly micro wire of collimation along grating raceway groove.
3. preparation method according to claim 1 and 2, wherein grating, by impression or the method for etching at polymkeric substance, glass, quartz, or makes on silicon chip, and raster density is 500 to 5000 lines.
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| CN103255374A (en) * | 2012-09-19 | 2013-08-21 | 苏州大学 | Method for preparing ordered one-dimensional organic nano wire array |
| CN103400760A (en) * | 2013-08-05 | 2013-11-20 | 电子科技大学 | Method and device for growing bismuth selenide single crystal film on silicon substrate |
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| CN101837287A (en) * | 2009-03-21 | 2010-09-22 | 清华大学 | Carbon nano-tube nano-particle composite material and preparation hereof |
| CN101997084A (en) * | 2010-09-10 | 2011-03-30 | 江苏大学 | CuPc/ZnO organic/inorganic compound solar battery and preparation method thereof |
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| US20100203454A1 (en) * | 2009-02-10 | 2010-08-12 | Mark Brongersma | Enhanced transparent conductive oxides |
| CN102206863B (en) * | 2011-03-24 | 2012-07-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of metal phthalocyanine nanowires |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101837287A (en) * | 2009-03-21 | 2010-09-22 | 清华大学 | Carbon nano-tube nano-particle composite material and preparation hereof |
| CN101997084A (en) * | 2010-09-10 | 2011-03-30 | 江苏大学 | CuPc/ZnO organic/inorganic compound solar battery and preparation method thereof |
Non-Patent Citations (4)
| Title |
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| 2,4,5-Triphenylimidazole Nanowires with Fluorescence Narrowing Spectra Prepared through the Adsorbent-Assisted Physical Vapor Deposition Method;Yong Sheng Zhao，等;《Chem. Mater.》;20060328;第18卷(第9期);2302-2306 * |
| Patterned Growth of Vertically Aligned Organic Nanowire Waveguide Arrays;Yong Sheng Zhao，等;《Acs. Nano》;20100208;第4卷(第3期);1630-1636 * |
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