CN106006756A - Method for manufacturing Fe2O3 nanometer film curled tubes - Google Patents
Method for manufacturing Fe2O3 nanometer film curled tubes Download PDFInfo
- Publication number
- CN106006756A CN106006756A CN201610334581.1A CN201610334581A CN106006756A CN 106006756 A CN106006756 A CN 106006756A CN 201610334581 A CN201610334581 A CN 201610334581A CN 106006756 A CN106006756 A CN 106006756A
- Authority
- CN
- China
- Prior art keywords
- film
- nanometer film
- nanometer
- crimp tube
- nano thin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 24
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title abstract 5
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000010409 thin film Substances 0.000 claims description 20
- 239000005030 aluminium foil Substances 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 9
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- 238000005566 electron beam evaporation Methods 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 5
- 238000000352 supercritical drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000002788 crimping Methods 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 238000007747 plating Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 238000000313 electron-beam-induced deposition Methods 0.000 abstract description 3
- 239000007888 film coating Substances 0.000 abstract 1
- 238000009501 film coating Methods 0.000 abstract 1
- 239000002071 nanotube Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000002120 nanofilm Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
-
- 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]
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention belongs to the field of technologies for manufacturing nanometer film materials, and relates to a method for manufacturing Fe2O3 nanometer film curled tubes. The method includes manufacturing elementary Fe nanometer film curled tube structures by the aid of electron beam deposition film coating technologies and nanometer film curling technologies; annealing the elementary Fe nanometer film curled tube structures in atmosphere of air to obtain the Fe2O3 nanometer film curled tubes. The method has the advantages that processes for manufacturing the Fe2O3 nanometer film curled tubes are simple, the method is convenient to implement, scientific in principle and free of pollution and is environmentally friendly, the tube wall thicknesses of the Fe2O3 nanometer film curled tubes can be effectively controlled, and the lengths of the Fe2O3 nanometer film curled tubes manufactured by the aid of the method can reach several hundreds of micrometers.
Description
Technical field:
The invention belongs to nano film material preparing technical field, relate to a kind of Fe2O3Micro-nano
The preparation method of structural material, particularly a kind of Fe2O3The preparation method of nano thin-film crimp tube.
Background technology:
Ferrum oxide is a kind of important transition metal oxide semi-conducting material, has nontoxic, storage
The advantages such as amount is abundant, physical and chemical performance is stable, are widely used in gas sensor, photocatalysis
The research fields such as agent, lithium ion battery, magnetic material.Fe2O3Nano film material is partly being led
Body device has important application prospect, the two-dimensional structure of its uniqueness and current semiconductor machining
Technical compatibility, and be especially suitable for for making scrolled tubular structure, is used for preparing integrated micro-
Type electronic device.
At present, Fe2O3The preparation of tubular structure material mainly uses chemical method, document " J.
Chen, L.Xu, W.Li, X.Gou, Advanced Materials, 2005,17,582 586 "
Report and utilize porous anodic aluminium oxide to prepare Fe as template2O3The method of nanotube；Document
" Z.Sun, H.Yuan, Z.Liu, B.Han, X.Zhang, Advanced Materials, 2005,
17,2,993 2997 " report and utilize CNT as template to prepare Fe2O3Nanotube
Method；Document " Jinping Liu, Yuanyuan Li, Hongjin Fan, Zhihong Zhu,
Jian Jiang, Ruimin Ding, Yingying Hu, Xintang Huang, Chem.Mater.,
2010,22,212 217 " report and utilize ZnO nano-rod array to prepare Fe as template2O3
The method of nanotube；Document " Zhiyu Wang, Deyan Luan, Srinivasan Madhavi,
Chang Ming Li,Xiong Wen Lou,Chem.Commun.,2011,47,
8061-8063 " report and utilize Cu nano wire to prepare Fe (OH) x nanotube as template, so
After obtain Fe 300 DEG C of roastings2O3The method of nanotube；Said method needs to use template to make
For the medium of hollow structure, complex steps is complicated, exists to remove because of template and does not thoroughly pollute material
The risk of material.
Summary of the invention:
It is an object of the invention to the shortcoming overcoming prior art to exist, seeking design provides one
Electron beam deposition technique is utilized to prepare quasiconductor Fe2O3The method of nanometer film scrolled tubular structure.
The method is mutually compatible with existing semiconductor processing technology, is suitable for the big of quasiconductor crimp tube structure
Prepared by scale.
In order to realize foregoing invention purpose, the present invention utilizes electron beam deposition coating technique and nanometer
Film crimping techniques, first prepares the nanometer film crimp tube structure of simple substance Fe, then at air atmosphere
Lower annealing obtains Fe2O3Nanometer film crimp tube, specifically includes following steps:
(1) electron beam evaporation deposition instrument is utilized successively to deposit one in the streaky one side of aluminium foil
The Al of layer 50-100nm thickness2O3Ti nanometer film that nanometer film, one layer of 10-20nm are thick and
One layer of Fe nano thin-film thick for 20-50nm, obtaining deposition has Al2O3, Ti, Fe nanometer thin
The aluminium foil of film；
(2) deposition there is Al2O3, to put into concentration be 1M's to the aluminium foil of Ti, Fe nano thin-film
NaOH solution is soaked 3h, in immersion process, aluminium foil and Al2O3, Ti nanometer film quilt
NaOH solution erodes, and Fe nano thin-film curling under the stress effect of release simultaneously is pipe
Shape structure；
(3) the product deionized water that step (2) obtains repeatedly is filtered, washs 2-5 time
After, then filter successively with ethanol and isopropanol, wash 2-5 time respectively, then by curling for managing
The Fe nano thin-film of shape structure is through CO2Supercritical drying 12h, obtains Fe crimp tube；
(4) Fe crimp tube is put into the 2h that anneals at 450 DEG C in tube furnace, prepares
Fe2O3Nanometer film crimp tube.
Compared with prior art, its preparation technology is simple, easy to operate, scientific in principle for the present invention,
Pollution-free, environmental friendliness, it is possible to effectively control the pipe thickness of crimp tube, the nanometer film of preparation
Crimp tube length can reach hundreds of micron.
Accompanying drawing illustrates:
Fig. 1 is the Fe of the embodiment of the present invention 1 preparation2O3The scanning electron microscope of nano thin-film crimp tube
Photo.
Fig. 2 is the Fe of the embodiment of the present invention 2 preparation2O3The scanning electron microscope of nano thin-film crimp tube
Photo.
Fig. 3 is the Fe of the embodiment of the present invention 3 preparation2O3The scanning electron microscope of nano thin-film crimp tube
Photo.
Detailed description of the invention:
Below by specific embodiment and combine accompanying drawing and be described further.
Embodiment 1:
The present embodiment prepares Fe2O3The detailed process of nanometer film crimp tube is: first with electron beam
Evaporation coating instrument successively deposits the Al of one layer of 50nm thickness in the streaky one side of aluminium foil2O3
Nanometer film, one layer of Ti nanometer film thick for 10nm, one layer of Fe nano thin-film thick for 50nm；
Aluminium foil is put into immersion 3h in the NaOH solution that concentration is 1M again, is gone by chemical attack
Fall Al2O3With Ti nanometer film, meanwhile, the curling under the stress effect of release of Fe nanometer film is
Tubular structure, by products therefrom with deionized water filter, washing 3 times, more respectively with ethanol,
Isopropanol filters successively, washs 3 times, and the product after then filtering, wash is through CO2
Supercritical drying 12h, obtains Fe crimp tube, finally by Fe crimp tube in tube furnace 450 DEG C
Lower annealing 2h, prepares Fe2O3Nanometer film crimp tube.
The present embodiment Fe to preparation2O3Nanometer film crimp tube carries out SEM sign, and result is such as
Shown in Fig. 1, sample major part presents two-dimensional film structure, can clearly observe a small amount of two
Dimension thin 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 coating instrument successively deposits the Al of one layer of 50nm thickness in the streaky one side of aluminium foil2O3
Nanometer film, one layer of Ti nanometer film thick for 20nm, one layer of Fe nano thin-film thick for 20nm；
Aluminium foil is put into immersion 3h in the NaOH solution that concentration is 1M again, is gone by chemical attack
Fall Al2O3With Ti nanometer film, meanwhile, the curling under the stress effect of release of Fe nanometer film is
Tubular structure, by products therefrom with deionized water filter, washing 3 times, more respectively with ethanol,
Isopropanol filters successively, washs 3 times, and the product after then filtering, wash is through CO2
Supercritical drying 12h, obtains Fe crimp tube, finally by Fe crimp tube in tube furnace 450 DEG C
Lower annealing 2h, i.e. prepares Fe2O3Nanometer film crimp tube.
The present embodiment Fe to preparation2O3Nano thin-film crimp tube carries out SEM sign, result
As in figure 2 it is shown, sample presents two-dimensional film wrapped configuration, form hollow tubular structure, from portion
The two-port of bundling curved tube is it is apparent that opening, and the length of crimp tube arrives hundreds of micro-tens
Rice, a diameter of 5-10 micron.
Embodiment 3:
The present embodiment prepares Fe2O3The detailed process of nanometer film crimp tube is: first with electron beam
Evaporation coating instrument successively deposits the Al of one layer of 50nm thickness in the streaky one side of aluminium foil2O3
Nanometer film, one layer of Ti nanometer film thick for 20nm, one layer of Fe nano thin-film thick for 35nm；
Aluminium foil is put into immersion 3h in the NaOH solution that concentration is 1M again, is gone by chemical attack
Fall Al2O3With Ti nanometer film, meanwhile, the curling under the stress effect of release of Fe nanometer film is
Tubular structure, by products therefrom with deionized water filter, washing 3 times, more respectively with ethanol,
Isopropanol filters successively, washs 3 times, and the product after then filtering, wash is through CO2
Supercritical drying 12h, obtains Fe crimp tube；Finally by Fe crimp tube in tube furnace 450 DEG C
Lower annealing 2h, prepares Fe2O3Nanometer film crimp tube.
The present embodiment Fe to preparation2O3Nano thin-film crimp tube carries out SEM sign, result
As it is shown on figure 3, sample presents two-dimensional film wrapped configuration, form hollow tubular structure, from portion
The two-port of bundling curved tube is it is apparent that opening, and the length of crimp tube arrives hundreds of micro-tens
Rice, a diameter of 10-15 micron.
Claims (1)
1. a Fe2O3The preparation method of nano thin-film crimp tube, it is characterised in that utilize electricity
Son bundle deposition plating technology and nanometer film crimping techniques, first prepare the nanometer film curling of simple substance Fe
Tubular construction, annealing obtains Fe the most in air atmosphere2O3Nanometer film crimp tube, specifically includes
Following steps:
(1) electron beam evaporation deposition instrument is utilized successively to deposit one in the streaky one side of aluminium foil
The Al of layer 50-100nm thickness2O3Ti nanometer film that nanometer film, one layer of 10-20nm are thick and
One layer of Fe nano thin-film thick for 20-50nm, obtaining deposition has Al2O3, Ti, Fe nanometer thin
The aluminium foil of film；
(2) deposition there is Al2O3, to put into concentration be 1M's to the aluminium foil of Ti, Fe nano thin-film
NaOH solution is soaked 3h, in immersion process, aluminium foil and Al2O3, Ti nanometer film quilt
NaOH solution erodes, and Fe nano thin-film curling under the stress effect of release simultaneously is pipe
Shape structure；
(3) the product deionized water that step (2) obtains repeatedly is filtered, washs 2-5 time
After, then filter successively with ethanol and isopropanol, wash 2-5 time respectively, then by curling for managing
The Fe nano thin-film of shape structure is through CO2Supercritical drying 12h, obtains Fe crimp tube；
(4) Fe crimp tube is put into the 2h that anneals at 450 DEG C in tube furnace, prepares
Fe2O3Nanometer film crimp tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610334581.1A CN106006756B (en) | 2016-05-19 | 2016-05-19 | A kind of Fe2O3The preparation method of nano thin-film crimp tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610334581.1A CN106006756B (en) | 2016-05-19 | 2016-05-19 | A kind of Fe2O3The preparation method of nano thin-film crimp tube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106006756A true CN106006756A (en) | 2016-10-12 |
| CN106006756B CN106006756B (en) | 2017-07-04 |
Family
ID=57095906
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610334581.1A Expired - Fee Related CN106006756B (en) | 2016-05-19 | 2016-05-19 | A kind of Fe2O3The preparation method of nano thin-film crimp tube |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106006756B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431966A (en) * | 2011-12-27 | 2012-05-02 | 复旦大学 | Tubular multi-pore micron motor and preparation method and application thereof |
| CN103160900A (en) * | 2013-02-26 | 2013-06-19 | 中国科学院理化技术研究所 | Method for preparing Fe2O3 nanotube array on conductive substrate |
| CN103872186A (en) * | 2014-03-19 | 2014-06-18 | 浙江大学 | FeS2 thin film and preparation method thereof |
| CN104692466A (en) * | 2015-01-29 | 2015-06-10 | 青岛大学 | Non-template method for preparing alpha-Fe2O3 hollow tubular nano film |
-
2016
- 2016-05-19 CN CN201610334581.1A patent/CN106006756B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102431966A (en) * | 2011-12-27 | 2012-05-02 | 复旦大学 | Tubular multi-pore micron motor and preparation method and application thereof |
| CN103160900A (en) * | 2013-02-26 | 2013-06-19 | 中国科学院理化技术研究所 | Method for preparing Fe2O3 nanotube array on conductive substrate |
| CN103872186A (en) * | 2014-03-19 | 2014-06-18 | 浙江大学 | FeS2 thin film and preparation method thereof |
| CN104692466A (en) * | 2015-01-29 | 2015-06-10 | 青岛大学 | Non-template method for preparing alpha-Fe2O3 hollow tubular nano film |
Non-Patent Citations (1)
| Title |
|---|
| ZHENYU SUN ET AL.: "A Highly Efficient Chemical Sensor Material for H2S: a-Fe2O3 Nanotubes Fabricated Using Carbon Nanotube Templates", 《ADVANCED MATERIALS》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106006756B (en) | 2017-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yang et al. | Electrophoresis coating of titanium dioxide on aligned carbon nanotubes for controlled syntheses of photoelectronic nanomaterials | |
| CN104310372B (en) | A kind of method of direct growth carbon nano pipe array in fibrous substrate | |
| CN100436008C (en) | Chemical production of metal nickel nano-line | |
| CN105603469B (en) | A kind of CuO/Ni core-shell nanos line and preparation method thereof | |
| TW201122396A (en) | ive micro-structure thereof. | |
| CN101302118A (en) | Preparation of silicon nanowire array | |
| CN109052453B (en) | ZnCo2O4/ZnO heterostructure composite gas sensitive material and preparation method thereof | |
| Ahmad et al. | A review on hematite α-Fe 2 O 3 focusing on nanostructures, synthesis methods and applications | |
| CN107385372A (en) | A kind of preparation method of nano-structural transition metal film | |
| KR101916588B1 (en) | Metal Nano-spring And Manufacturing Method Of The Same | |
| CN102345149B (en) | Preparation method of aluminium foil bionic nanostructured super-hydrophobic anti-condensation functional surface | |
| CN103936054B (en) | A kind of synthetic method with the cupric sulfide powder of co-continuous nano-porous structure | |
| Wang et al. | Preparation of lotus-like hierarchical microstructures on zinc substrate and study of its wettability | |
| Bai et al. | Wafer-scale fabrication of uniform Si nanowire arrays using the Si wafer with UV/Ozone pretreatment | |
| CN106917071B (en) | Graphene-nano-noble metal multiple tube preparation method | |
| CN106006756A (en) | Method for manufacturing Fe2O3 nanometer film curled tubes | |
| CN105761943A (en) | Nickel tin alloy nano-pore array and preparation method thereof | |
| CN107739869B (en) | Nano porous copper composite material and preparation method | |
| CN105645376A (en) | Method for direct growth of porous carbon nanotube graphene hybrid on nano-porous copper | |
| KR101711888B1 (en) | Metallic nanotube and preparation method thereof | |
| CN103526299A (en) | Method for preparing silicon nanostructured material | |
| CN105692692A (en) | Synthesis technology for petal-shaped SnO2 nano-arrays | |
| Zhang et al. | Facile synthesis of rose-like nio nanoparticles and their ethanol gas-sensing property | |
| CN108281288B (en) | A kind of quantum dot sensitized solar battery is to electrode and its preparation method and application | |
| CN103646651B (en) | A kind of nano silver/silver bromide polyimide composite film and preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170704 Termination date: 20190519 |