CN106006756B - A kind of Fe2O3The preparation method of nano thin-film crimp tube - Google Patents
A kind of Fe2O3The preparation method of nano thin-film crimp tube Download PDFInfo
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- CN106006756B CN106006756B CN201610334581.1A CN201610334581A CN106006756B CN 106006756 B CN106006756 B CN 106006756B CN 201610334581 A CN201610334581 A CN 201610334581A CN 106006756 B CN106006756 B CN 106006756B
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- nanometer
- film
- crimp tube
- films
- nanometer film
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
Abstract
The invention belongs to nano film material preparing technical field, it is related to a kind of Fe2O3The preparation method of nano thin-film crimp tube, using electron beam deposition coating technique and nanometer film crimping techniques, first prepares the nanometer film curling tubular construction of simple substance Fe, and then annealing obtains Fe in air atmosphere2O3Nanometer film crimp tube；Its preparation process is simple, easy to operate, scientific in principle is pollution-free, environment-friendly, can effectively control the nanometer film curling length of tube of the pipe thickness of crimp tube, preparation and can reach hundreds of microns.
Description
Technical field：
The invention belongs to nano film material preparing technical field, it is related to a kind of Fe2O3The preparation side of micro-nanometer structural material
Method, particularly a kind of Fe2O3The preparation method of nano thin-film crimp tube.
Background technology：
Iron oxide is a kind of important transition metal oxide semi-conducting material, with nontoxic, rich reserves, physical chemistry
Steady performance, is widely used in the research fields such as gas sensor, photochemical catalyst, lithium ion battery, magnetic material.
Fe2O3Nano film material has important application prospect, its unique two-dimensional structure and current semiconductor in the semiconductor device
Process technology is compatible, and is especially suitable for for making scrolled tubular structure, for preparing integrated micro electronic device.
At present, Fe2O3The preparation of tubular structure material mainly use chemical method, document " J.Chen, L.Xu, W.Li,
X.Gou, Advanced Materials, 2005,17,582-586 " is reported and prepared as template by the use of porous anodic aluminium oxide
Fe2O3The method of nanotube；Document " Z.Sun, H.Yuan, Z.Liu, B.Han, X.Zhang, Advanced Materials,
2005,17,2993-2997 " report by the use of CNT as template to prepare Fe2O3The method of nanotube；Document
" Jinping Liu, Yuanyuan Li, Hongjin Fan, Zhihong Zhu, Jian Jiang, Ruimin Ding,
Yingying Hu, Xintang Huang, Chem.Mater., 2010,22,212-217 " is reported and is utilized ZnO nano-rod array
Fe is prepared as template2O3The method of nanotube；Document " Zhiyu Wang, Deyan Luan, Srinivasan Madhavi,
Chang Ming Li, Xiong Wen Lou, Chem.Commun., 2011,47,8061-8063 " is reported using Cu nano wires
Fe (OH) x nanotubes are prepared as template, then Fe is obtained in 300 DEG C of roastings2O3The method of nanotube；The above method needs to adopt
With template as hollow structure medium, complex steps are complicated, exist because of the template removal not thorough risk of contaminated materials.
The content of the invention：
It is an object of the invention to the shortcoming for overcoming prior art to exist, design offer one kind is provided and is sunk using electron beam
Product technology prepares semiconductor Fe2O3The method of nanometer film scrolled tubular structure.The method is mutually simultaneous with existing semiconductor processing technology
Hold, be adapted to the extensive preparation that semiconductor crimps tubular construction.
In order to realize foregoing invention purpose, the present invention utilizes electron beam deposition coating technique and nanometer film crimping techniques, first
The nanometer film curling tubular construction of simple substance Fe is prepared, then annealing obtains Fe in air atmosphere2O3Nanometer film crimp tube, specific bag
Include following steps：
(1) one layer of 50-100nm thickness is successively deposited in the streaky one side of aluminium foil using electron beam evaporation deposition instrument
Al2O3Nanometer film, one layer of 10-20nm thick Ti nanometer films and the thick Fe nano thin-films of one layer of 20-50nm, obtaining deposition has
Al2O3, Ti, Fe nano thin-film aluminium foil；
(2) deposition there is into Al2O3, Ti, Fe nano thin-film aluminium foil be put into concentration be 1M NaOH solution in soak 3h,
In immersion process, aluminium foil and Al2O3, Ti nanometer films eroded by NaOH solution, while Fe nano thin-films release stress
Lower curling is tubular structure；
(3) after filtering the product deionized water that step (2) is obtained repeatedly, wash 2-5 times, then respectively with ethanol and different
Propyl alcohol is filtered, washed 2-5 times successively, then will crimp the Fe nano thin-films for tubular structure by CO2Supercritical drying 12h,
Obtain Fe crimp tubes；
(4) Fe crimp tubes are put into the 2h that annealed at 450 DEG C in tube furnace, prepare Fe2O3Nanometer film crimp tube.
The present invention compared with prior art, its preparation process is simple, easy to operate, scientific in principle is pollution-free, environment friend
Good, can effectively control the nanometer film curling length of tube of the pipe thickness of crimp tube, preparation can reach hundreds of microns.
Brief description of the drawings：
Fig. 1 is Fe prepared by the embodiment of the present invention 12O3The stereoscan photograph of nano thin-film crimp tube.
Fig. 2 is Fe prepared by the embodiment of the present invention 22O3The stereoscan photograph of nano thin-film crimp tube.
Fig. 3 is Fe prepared by the embodiment of the present invention 32O3The stereoscan photograph of nano thin-film crimp tube.
Specific embodiment：
It is described further below by specific embodiment and with reference to accompanying drawing.
Embodiment 1：
The present embodiment prepares Fe2O3The detailed process of nanometer film crimp tube is：First with electron beam evaporation deposition instrument in aluminium foil
One layer of Al of 50nm thickness is successively deposited in streaky one side2O3Nanometer film, one layer of 10nm thick Ti nanometer films, one layer of 50nm
Thick Fe nano thin-films；Aluminium foil is put into the NaOH solution that concentration is 1M again soaks 3h, Al is removed by chemical attack2O3With
Ti nanometer films, meanwhile, the curling under the stress of release of Fe nanometer films is tubular structure, by products therefrom deionized water mistake
Filter, washing 3 times, then filtered successively with ethanol, isopropanol respectively, wash 3 times, then will filter, wash after product by CO2
Supercritical drying 12h, obtains Fe crimp tubes, and finally Fe crimp tubes are annealed in the tube furnace 2h at 450 DEG C, prepares Fe2O3
Nanometer film crimp tube.
Fe of the present embodiment to preparation2O3Nanometer film crimp tube carries out SEM signs, as a result as shown in figure 1, sample is most of
Two-dimensional film structure is presented, can clearly observe that a small amount of two-dimensional film is curled into tubular structure.
Embodiment 2：
The present embodiment prepares Fe2O3The detailed process of nanometer film crimp tube is：First with electron beam evaporation deposition instrument in aluminium foil
One layer of Al of 50nm thickness is successively deposited in streaky one side2O3Nanometer film, one layer of 20nm thick Ti nanometer films, one layer of 20nm
Thick Fe nano thin-films；Aluminium foil is put into the NaOH solution that concentration is 1M again soaks 3h, Al is removed by chemical attack2O3With
Ti nanometer films, meanwhile, the curling under the stress of release of Fe nanometer films is tubular structure, by products therefrom deionized water mistake
Filter, washing 3 times, then filtered successively with ethanol, isopropanol respectively, wash 3 times, then will filter, wash after product by CO2
Supercritical drying 12h, obtains Fe crimp tubes, and finally Fe crimp tubes are annealed in the tube furnace 2h at 450 DEG C, that is, prepare
Fe2O3Nanometer film crimp tube.
Fe of the present embodiment to preparation2O3Nano thin-film crimp tube carries out SEM signs, as a result as shown in Fig. 2 sample is presented
Two-dimensional film wrapped configuration, forms hollow tubular structure, and opening, crimp tube are apparent that from the two-port of part crimp tube
Length at tens to hundreds of microns, it is a diameter of 5-10 microns.
Embodiment 3：
The present embodiment prepares Fe2O3The detailed process of nanometer film crimp tube is：First with electron beam evaporation deposition instrument in aluminium foil
One layer of Al of 50nm thickness is successively deposited in streaky one side2O3Nanometer film, one layer of 20nm thick Ti nanometer films, one layer of 35nm
Thick Fe nano thin-films；Aluminium foil is put into the NaOH solution that concentration is 1M again soaks 3h, Al is removed by chemical attack2O3With
Ti nanometer films, meanwhile, the curling under the stress of release of Fe nanometer films is tubular structure, by products therefrom deionized water mistake
Filter, washing 3 times, then filtered successively with ethanol, isopropanol respectively, wash 3 times, then will filter, wash after product by CO2
Supercritical drying 12h, obtains Fe crimp tubes；Finally Fe crimp tubes are annealed in the tube furnace 2h at 450 DEG C, Fe is prepared2O3
Nanometer film crimp tube.
Fe of the present embodiment to preparation2O3Nano thin-film crimp tube carries out SEM signs, as a result as shown in figure 3, sample is presented
Two-dimensional film wrapped configuration, forms hollow tubular structure, and opening, crimp tube are apparent that from the two-port of part crimp tube
Length at tens to hundreds of microns, it is a diameter of 10-15 microns.
Claims (1)
1. a kind of Fe2O3The preparation method of nano thin-film crimp tube, it is characterised in that utilize electron beam deposition coating technique and nanometer
Film crimping techniques, first prepare the nanometer film curling tubular construction of simple substance Fe, and then annealing obtains Fe in air atmosphere2O3Nanometer film
Crimp tube, specifically includes following steps：First with electron beam evaporation deposition instrument one is successively deposited in the streaky one side of aluminium foil
The Al of layer 50nm thickness2O3Nanometer film, one layer of 20nm thick Ti nanometer films, one layer of 20nm thick Fe nano thin-films；Aluminium foil is put again
Enter concentration to soak 3h in the NaOH solution of 1M, Al is removed by chemical attack2O3With Ti nanometer films, meanwhile, Fe nanometer films are being released
Curling is tubular structure under the stress put, and products therefrom is filtered with deionized water, washing 3 times, then respectively with ethanol, different
Propyl alcohol filters successively, wash 3 times, then will filter, the product after washing is by CO2Supercritical drying 12h, obtains Fe curlings
Pipe, finally anneals 2h Fe crimp tubes in the tube furnace at 450 DEG C, that is, prepare Fe2O3Nanometer film crimp tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610334581.1A CN106006756B (en) | 2016-05-19 | 2016-05-19 | A kind of Fe2O3The preparation method of nano thin-film crimp tube |
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| CN201610334581.1A CN106006756B (en) | 2016-05-19 | 2016-05-19 | A kind of Fe2O3The preparation method of nano thin-film crimp tube |
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| CN106006756B true CN106006756B (en) | 2017-07-04 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102431966B (en) * | 2011-12-27 | 2014-10-29 | 复旦大学 | Tubular multi-pore micron motor and preparation method and application thereof |
| CN103160900B (en) * | 2013-02-26 | 2015-11-04 | 中国科学院理化技术研究所 | One prepares Fe in conductive substrates 2o 3the method of nano-tube array |
| CN103872186B (en) * | 2014-03-19 | 2016-05-11 | 浙江大学 | FeS2The preparation method of film |
| CN104692466B (en) * | 2015-01-29 | 2016-07-20 | 青岛大学 | A kind of non-template prepares α-Fe2o3the method of hollow tubular nano thin-film |
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