CN102505144A - 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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- CN102505144A CN102505144A CN2011103427467A CN201110342746A CN102505144A CN 102505144 A CN102505144 A CN 102505144A CN 2011103427467 A CN2011103427467 A CN 2011103427467A CN 201110342746 A CN201110342746 A CN 201110342746A CN 102505144 A CN102505144 A CN 102505144A
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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 the nanometer physical field, be specifically related to a kind of preparation method of organic micro-nano rice noodles oriented growth of overlength.
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Background technology
Height collimation oriented growth or the micro nano structure of arranging have indispensable effect in nano-device prepares and be integrated.In addition, utilize overlength micro-nano rice noodles, can realize the leap of micro/nano-scale and macro-scale, make things convenient for the preparation, integrated and interconnected of nano-device with big L/D ratio.The research of above-mentioned two aspects has caused people's very big interest.But because the complicacy of the singularity of organic materials self structure and preparation process, the preparation of organic nano line orientation array structure often is difficult to realize.In order to prepare the organic nano linear array, there is report to use template (J. L. Yang, S. Schumann and T. S. Jones*. J. Mater. Chem. 2011; 21; 5812 – 5816), the organic nano linear array poor controllability of this this method preparation, process are comparatively complicated; Also there is report to prepare the inorganic nano linear array through template earlier, then utilizes 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 the organic nano linear array; But this method is confined to the organic materials of minority and inorganic materials lattice match, and the nano-wire array surfaceness is bigger; Also have 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 directed against this specific organic materials, the method expansion is relatively poor, and building-up process is also comparatively complicated.
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Summary of the invention
In order to overcome the deficiency that prior art exists; The present invention provides a kind of preparation method of organic micro-nano structure oriented growth; Utilize physical vaporous deposition; Based on organic micro-nano rice noodles of substrate preparation height collimation oriented growth with surface period optical grating construction, realize control through the control growing condition to micro-nano linear dimension, density and length, obtain overlength micro-nano rice noodles periodic structure.This preparation method technology is simple, with low cost, controllability is good, be fit to characteristics such as large area micro-nano rice structure direction growth, the organic nano preparation of devices and integrated in have the important application prospect.
For reaching the foregoing invention purpose; The technical scheme that the present invention adopted is: through control 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, regulate the sedimentary province grating and place height by the carrier gas air-flow; Under the inducing of grating substrate, be self-assembled into the micro-nano rice noodles of height collimation along the grating raceway groove.Specifically may further comprise the steps:
1), takes by weighing 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 the porcelain boat after mixing with the mass ratio of 1:10-1:100, places the heating zone of physical deposition method (PVD) device, promptly in the silica tube.
2), be fixed on the grating substrate on the slide glass after, place the low temperature depositing district of physical deposition method, and use the porcelain boat bed hedgehopping, grating planar is positioned in the middle of the silica tube.
3), silica tube is evacuated to 3Pa, the argon gas that feeds 60 SCCM subsequently keeps stable air-flow velocity and air pressure as carrier gas, and the air pressure of generally controlling in the 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 between 400 ℃～450 ℃ is incubated for some time after a stable temperature, generally with 420 ℃ of equilibrium temperatures for this reason, this moment, the temperature of grating substrate was about 200
oC.Growth time is 3 hours, takes out sample when treating to be cooled to 30 ℃ after growth finishes, and promptly gets 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 the gained sample purity is high;
2, technology is simple, and is with low cost;
3, be fit to large-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 large-area preparation, has in the machine micro nano structure in the big area beam system to have important application prospects.
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Embodiment
The technical scheme that the present invention adopted is: at first the organic evaporating source is heated, make it reach sublimation temperature, depress at certain saturation steam, sample molecule is brought to sedimentary province under the transporting of carrier gas.Heavy machine district temperature is lower, and the organic molecule regelation is gone forward side by side and nucleating growth, because the special molecular structure of organic molecule, it tends at the specific direction oriented growth, thereby obtains the micro-nano rice noodles of one-dimentional structure.Through introducing the grating substrate, because air-flow is more slow in the grating raceway groove, nucleation site is abundant, and organic micro-nano rice noodles are nucleation in the grating raceway groove preferentially, and because the inducing action of grating makes the micro-nano rice noodles along grating channel height oriented growth.
Concrete steps comprise: take by weighing a certain amount of CuPc powder, with Al
2O
3Powder is poured in the porcelain boat after mixing with the mass ratio of 1:10-1:100, places the heating zone of physical vaporous deposition silica tube.
After being fixed on the grating substrate on the sheet glass, place the sedimentary province of physical vaporous deposition.The program of physical vaporous deposition is set: TRT, soaking time, holding temperature, air-flow velocity etc.
Take out sample when treating to be cooled to 30 ℃ after the EP.
Through some condition of reprogramming, obtain different size, the controlled organic micro-nano structure of density property.
Experimental technique described in the following embodiment like no specified otherwise, is ordinary method; Said sample and material like no specified otherwise, all can obtain from commercial sources.
Embodiment 1
Take by weighing a certain amount of CuPc powder, with Al
2O
3Powder is poured in the porcelain boat after mixing with the certain mass ratio, places the heating zone of physical vaporous deposition silica tube.After being fixed on the grating substrate on the sheet glass, place the sedimentary province of physical vaporous deposition.Set the program of physical vaporous deposition, the TRT is made as 40 min, and soaking time is made as 1 h, and holding temperature is made as 420 ℃, and air-flow is an argon gas, and flow velocity is 40 sccm.Take out sample when treating to be cooled to 30 ℃ after the EP.Can obtain the sparse micro-nano structure product of a kind of orientation.
Embodiment 2
In embodiment 1, soaking time prolongs, and 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, soaking time prolongs, and air-flow velocity increases, and the porcelain boat bed hedgehopping is used in the grating substrate of sedimentary province, and other operation is constant, obtains organic micro-nano rice noodles of another form.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of an organic micro-nano structure oriented growth; It is characterized in that; With organic cpds and sorbent material is organic raw material, utilizes physical vaporous deposition, based on organic micro-nano rice noodles of the substrate preparation directionally aligning growth with surface period optical grating construction; Growth conditions through the organic micro-nano rice noodles of grating pair is controlled, and obtains to be with periodic structure organic micro-nano rice noodles of directionally aligning growth.
2. the preparation method of organic micro-nano structure oriented growth according to claim 1 is characterized in that, said preparation method is specially; Through carrier gas air-flow and the chamber pressure in the control physical vaporous deposition; The organifying compound evaporates under its sublimation temperature, and is transported to sedimentary province by the carrier gas air-flow, regulates the placement height of sedimentary province grating; Under the inducing of grating substrate, be self-assembled into the micro-nano rice noodles of height collimation along the grating raceway groove.
3. the preparation method of organic micro-nano structure oriented growth according to claim 2 is characterized in that, said preparation method specifically comprises the steps:
Pack into after organic cpds and sorbent material mixed with the mass ratio of 1:10-1:100 in the container, place the middle heating zone of physical vapor deposition device;
Then the grating substrate is placed the low temperature depositing district of physical vapor deposition device, carrier gas is introduced in the tube chamber, keep stable air-flow velocity and air pressure, be warming up between 400 ℃～450 ℃ and be incubated for some time after a stable temperature;
After treating that growth finishes, and cavity temperature takes out sample when reducing to room temperature, promptly gets organic micro-nano rice noodles of oriented growth.
4. the preparation method of organic micro-nano structure oriented growth according to claim 3 is characterized in that, described organic cpds is that molecular weight is the phthalein mountain valley with clumps of trees and bamboo copper compound of 576.07 g/mol.
5. the preparation method of organic micro-nano structure oriented growth according to claim 3 is characterized in that, described sorbent material is that molecular weight is that 101.96 g/mol, particle size are 100-200 purpose neutral alumina powder.
6. the preparation method of organic micro-nano structure oriented growth according to claim 3 is characterized in that, said container is a porcelain boat.
7. the preparation method of organic micro-nano structure oriented growth according to claim 3 is characterized in that, grating passes through the method for impression or etching at polymkeric substance, glass, quartz, perhaps makes on the silicon chip, and raster density is 500 to 5000 lines.
8. the preparation method of organic micro-nano structure oriented growth according to claim 3 is characterized in that, said air-flow is argon gas or argon hydrogen, and air pressure is 220 Pa.
9. the preparation method of organic micro-nano structure oriented growth according to claim 3 is characterized in that, a said equilibrium temperature that is warming up to is 420 ℃.
10. the preparation method of organic micro-nano structure oriented growth according to claim 3 is characterized in that, described soaking time is 1-3 hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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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| US20100203454A1 (en) * | 2009-02-10 | 2010-08-12 | Mark Brongersma | Enhanced transparent conductive oxides |
| 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 |
| CN102206863A (en) * | 2011-03-24 | 2011-10-05 | 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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Patent Citations (4)
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| US20100203454A1 (en) * | 2009-02-10 | 2010-08-12 | Mark Brongersma | Enhanced transparent conductive oxides |
| 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 |
| CN102206863A (en) * | 2011-03-24 | 2011-10-05 | 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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| ANA BORRAS，等: "Synthesis of Supported Single-Crystalline Organic Nanowires by Physical Vapor Deposition", 《CHEM. MATER.》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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