CN101372358B - Method for preparing tin oxide nano-wire by normal atmosphere vapor deposition - Google Patents
Method for preparing tin oxide nano-wire by normal atmosphere vapor deposition Download PDFInfo
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- CN101372358B CN101372358B CN2008102245915A CN200810224591A CN101372358B CN 101372358 B CN101372358 B CN 101372358B CN 2008102245915 A CN2008102245915 A CN 2008102245915A CN 200810224591 A CN200810224591 A CN 200810224591A CN 101372358 B CN101372358 B CN 101372358B
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Abstract
The invention provides a method for preparing a tin oxide nanowire by the method of normal-pressure vapor deposition, which belongs to the field of oxide semiconductor nano materials. The method comprises the following steps: Sn powder and Fe powder are evenly mixed and put in a corundum boat as an evaporator source; the washed blank silicon wafer is taken as a receiving substrate and put over theevaporator source; argon is introduced into a horizontal tube furnace at the flow rate of 70-90ml/min, and then the horizontal tube furnace is heated until the temperature reaches 880-910 DEG C; whenthe setting temperature is reached, the boat with the evaporator source and the silicon wafer is put in the tube furnace for 20-30min heat preservation, and when the temperature of the tube furnace decreases to room temperature, the silicon wafer is taken out with the surface deposited with a layer of white SnO2 nanowire film, wherein, the diameter of the nanowire is 25-160nm and the length of the nanowire is 10-30Mum. The method has the advantages of simple equipment, easy operations, low cost and easy application in industrial production.
Description
Technical field
The invention belongs to the oxide semiconductor field of nanometer material technology, relate to the preparation method of stannic oxide nano material.
Background technology
Stannic oxide (SnO
2) be a kind of n type oxide semiconductor material of excellent property, it has wide band gap (3.16eV), low resistivity (10
-4～10
-6Ω cm) rare high light transmittance and in other semi-conductor is ideal electrode of solar battery and gas sensor material.One dimension SnO
2Nano material has big specific surface area and higher activity, makes aspects such as it is led at air-sensitive, electricity, photosensitive absorption have a wide range of applications; In addition, one dimension Nano structure also makes up nano-device easily to form suitability for industrialized production.At present, with SnO
2The thread field-effect transistor of nanometer, highly sensitive chemical sensor, high power lithium battery and sun power dye cell etc. have caused international concern.The preparation one dimension SnO that has reported
2The method of nano material is a lot, as vapour deposition process [V.V.Sysoev, B.K.Button, K.Wepsiec, S.Dmitriev, A.Kolmakov, Toward the nanoscopic " electronic nose ": Hydrogen vs carbon monoxide discrimination with an array ofindividual metal oxide nano-and mesowire sensors, Nano Letters 6 (2006) 1584-8], AAO template [P.X.Yan, D.M.Qu, J.B.Chang, D.Yan, J.Z.Liu, G.H.Yue, R.F.Zhuo, H.T.Feng, Nanowires and nanowire-nanosheet junctions of SnO
2Nanostructures, Mater.Lett.61 (2007) 2255-8], sol-gel method [Liu Chunming, Zu Xiaotao, a kind of method for preparing one-dimensional nano tin dioxide material, 200510021119.8], hydrothermal method [Y.J.Chen, L.Nie, X.Y.Xue, Y.G.Wang, T.H.Wang, Linear ethanol sensing of SnO
2Nanorods with extremely high sensitivity, Appl.Phys.Lett.88 (2006) 083105-7], burning synthetic gunite [Li Chunzhong, Hu Yanjie, Gu Feng, Jiang Haibo, a kind of preparation method of nanometer tin dioxide rod, 200610029008.6], solution method [Qin Lipeng, Xu Jiaqiang, Dong Xiaowen, Pan Qingyi, the preparation method of four prism type tin oxide nano-wire, 200710047105.2].Wherein, adopt the nano material of CVD (Chemical Vapor Deposition) method preparation to have advantages such as purity height, crystalline quality are good, but the SnO that the vapor phase process of having reported prepares
2Nano wire generally needs vacuum apparatus, and needs catalyzer [H.S.Jang, S.O.Kang, Y.I.Kim, Enhancement of field emission of SnO
2Nanowires film by exposure of hydrogen gas, Sol.Stat.Com.140 (2006) 495-9; Y.J.Chen, X.Y.Xue, Y.G.Wang, T.H.Wang, Synthesis and ethanol sensing characteristics of single crystalline SnO
2Nanorods, Appl.Phys.Lett.87 (2005) 233503], the technology more complicated, production cost is than higher, and introduces the purity that tramp material reduces product easily.
Summary of the invention
The purpose of this invention is to provide a kind of simple for process, with low cost, help large-scale industrial and produce SnO
2The synthetic method of nano wire.Mixed uniformly Sn powder and Fe powder are evaporated in argon gas atmosphere, and deposition obtains the SnO of tetragonal on silicon chip
2Nano wire.About 25～the 160nm of the diameter of nano wire, length reaches 10～30 μ m.The equipment that this method adopts is simple, and easy handling is with low cost, is easy to suitability for industrialized production.
Purpose of the present invention can realize by following technical measures:
1, blank (not plating catalyst film) silicon chip is cleaned the back airing with alcohol and acetone respectively;
2, will put into the corundum boat as evaporation source behind Sn powder and the Fe powder uniform mixing, the blank silicon chip after the cleaning as receive substrate be placed on evaporation source directly over;
3, feeding flow in horizontal pipe furnace is the argon gas of 70～90ml/min, tube furnace is warming up to 880～910 ℃ then, behind the arrival design temperature, the boat that is placed with evaporation source and silicon chip is put into tube furnace, and soaking time is 20～30min.After reducing to room temperature, the temperature of stove takes out silicon chip, deposition one deck white SnO on the silicon chip
2Nano wire film.
The present invention has the following advantages:
1, SnO provided by the invention
2Nano wire prepares under condition of normal pressure, does not adopt complicated vacuum apparatus, has saved production cost greatly.
2, SnO
2Do not adopt catalyzer in the process of growth of nano wire, do not introduce tramp material, thereby guaranteed the high purity of product.
3, after the present invention adopts tube furnace to arrive design temperature, the boat of evaporation source and silicon chip is put into tube furnace, can avoid the oxidation of Sn evaporation source effectively.Because if the Sn powder is put into tube furnace and then intensification earlier, Sn is very easy to oxidizing reaction takes place and causes evaporation source obviously oxidized, does not also just have the product deposition on silicon chip.
4, the present invention have that equipment is simple, easy and simple to handle, fast growth, low, the output advantages of higher of cost, have application prospect at aspects such as highly sensitive gas sensor, transparency electrodes.
Description of drawings
The scanning electron microscope collection of illustrative plates of sample on Fig. 1 silicon substrate.
The X ray diffracting spectrum of Fig. 2 sample.
Embodiment
Embodiment 1
1, blank (not plating catalyst film) silicon chip is cleaned the back airing with alcohol and acetone respectively;
2, will put into the corundum boat as evaporation source behind Sn powder and the Fe powder uniform mixing, the blank silicon chip after the cleaning as receive substrate be placed on evaporation source directly over;
3, feeding flow in horizontal pipe furnace is the argon gas of 80ml/min, tube furnace is warming up to 900 ℃ then, behind the arrival design temperature, the boat that is placed with evaporation source and silicon chip is put into tube furnace, and soaking time is 30min.After the temperature of stove is reduced to room temperature, take out silicon chip, find deposition one deck white SnO on the silicon chip
2Nano wire film.
Fig. 1 is the sem photograph of product, deposits a large amount of SnO as can be seen on silicon substrate
2Nano wire.
Fig. 2 is SnO
2The X-ray diffraction result of nano wire, all diffraction peaks all can be by the SnO of tetragonal
2Explain, illustrate that product is by pure SnO
2Nano wire is formed, the about 25～160nm of nanowire diameter, and length reaches 10～30 μ m.
Embodiment 2
1, blank (not plating catalyst film) silicon chip is cleaned the back airing with alcohol and acetone respectively;
2, will put into the corundum boat as evaporation source behind Sn powder and the Fe powder uniform mixing, the blank silicon chip after the cleaning as receive substrate be placed on evaporation source directly over;
3, feeding flow in horizontal pipe furnace is the argon gas of 90ml/min, tube furnace is warming up to 910 ℃ then, behind the arrival design temperature, the boat that is placed with evaporation source and silicon chip is put into tube furnace, and soaking time is 20min.After the temperature of stove is reduced to room temperature, take out silicon chip, find deposition one deck white SnO on the silicon chip
2Nano wire film.
Embodiment 3
1, blank (not plating catalyst film) silicon chip is cleaned the back airing with alcohol and acetone respectively;
2, will put into the corundum boat as evaporation source behind Sn powder and the Fe powder uniform mixing, the blank silicon chip after the cleaning as receive substrate be placed on evaporation source directly over;
3, feeding flow in horizontal pipe furnace is the argon gas of 70ml/min, tube furnace is warming up to 880 ℃ then, behind the arrival design temperature, the boat that is placed with evaporation source and silicon chip is put into tube furnace, and soaking time is 30min.After the temperature of stove is reduced to room temperature, take out silicon chip, find deposition one deck white SnO on the silicon chip
2Nano wire film.
Claims (1)
1. the method for a preparing tin oxide nano-wire by normal atmosphere vapor deposition, blank silicon chip is cleaned the back airing with alcohol and acetone respectively, it is characterized in that, the Sn powder and the Fe powder that mix are put into the corundum boat as evaporation source, blank silicon chip after the cleaning is placed on the corundum boat as receiving substrate, be positioned at evaporation source directly over; Feeding flow in horizontal pipe furnace is the argon gas of 70～90ml/min, tube furnace is warming up to 880～910 ℃ then, after arriving design temperature, the corundum boat that is placed with evaporation source and silicon chip is put into tube furnace, soaking time is 20～30min, the temperature of stove is taken out silicon chip after reducing to room temperature, deposition one deck white SnO on the silicon chip
2Nano wire film.
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| CN2008102245915A CN101372358B (en) | 2008-10-21 | 2008-10-21 | Method for preparing tin oxide nano-wire by normal atmosphere vapor deposition |
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| CN2008102245915A CN101372358B (en) | 2008-10-21 | 2008-10-21 | Method for preparing tin oxide nano-wire by normal atmosphere vapor deposition |
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|---|---|
| CN101372358A CN101372358A (en) | 2009-02-25 |
| CN101372358B true CN101372358B (en) | 2010-06-02 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030362B (en) * | 2010-10-08 | 2012-08-29 | 四川大学 | Method for preparing SnO2 nanomaterial by hydride deposition |
| CN108043382B (en) * | 2017-12-18 | 2021-04-20 | 中国矿业大学 | Preparation method of high-activity trace transition metal catalyst based on asphaltene |
| CN110040767B (en) * | 2019-04-29 | 2022-03-01 | 吉林大学 | Controllable preparation method of tin dioxide nanowire |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6533966B1 (en) * | 1998-09-06 | 2003-03-18 | Institut Für Neue Materialien Gem. Gmbh | Method for preparing suspensions and powders based in indium tin oxide and the use thereof |
| CN1667856A (en) * | 2005-04-08 | 2005-09-14 | 中国科学院上海微系统与信息技术研究所 | High-capacity lithium ion cell anode material and process for preparing same |
| CN101172644A (en) * | 2007-10-16 | 2008-05-07 | 上海大学 | Method of producing quadrangular shaped tin oxide nano wire |
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2008
- 2008-10-21 CN CN2008102245915A patent/CN101372358B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6533966B1 (en) * | 1998-09-06 | 2003-03-18 | Institut Für Neue Materialien Gem. Gmbh | Method for preparing suspensions and powders based in indium tin oxide and the use thereof |
| CN1667856A (en) * | 2005-04-08 | 2005-09-14 | 中国科学院上海微系统与信息技术研究所 | High-capacity lithium ion cell anode material and process for preparing same |
| CN101172644A (en) * | 2007-10-16 | 2008-05-07 | 上海大学 | Method of producing quadrangular shaped tin oxide nano wire |
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