CN104213098B - A kind of nanometer wall construction being made up of sheet tin oxide and preparation method thereof - Google Patents
A kind of nanometer wall construction being made up of sheet tin oxide and preparation method thereof Download PDFInfo
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- CN104213098B CN104213098B CN201310217839.6A CN201310217839A CN104213098B CN 104213098 B CN104213098 B CN 104213098B CN 201310217839 A CN201310217839 A CN 201310217839A CN 104213098 B CN104213098 B CN 104213098B
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Abstract
Present invention relates particularly to a kind of nanometer wall construction being made up of sheet tin oxide and preparation method thereof.Its method is, using stannous oxide powder and toner mixture as source material material, to be grown using thermal evaporation method.The edge of made nanometer wall construction is simultaneously irregular, and the side of each wall is also rough, and its diameter is about in 100 1000nm, and thickness is about 30nm.The present invention can in silicon chip substrate this structure of the growth of large area, its unique construction and anti-oxidant, high temperature resistant, Flied emission current density is high, threshold electric field is relatively low, it is prevented effectively from Field shielding effect, the features such as launch stability is good can realize its application in feds, the structure specific surface area is big, sensitivity characteristic of the stannic oxide materials to various chemical gas will be remarkably reinforced, micro-nano sensor field can be applied to as gas sensitized material, therefore the structure has huge scientific research value and wide commercial application prospect.
Description
Technical field
The invention belongs to photoelectron material, semiconductor materials and devices technical field, and in particular to one kind is aoxidized by sheet
The nanometer wall construction of tin composition and the thermal evaporation method used, under the conditions of atmospheric pressure, argon gas atmosphere, in silicon chip substrate
Obtain the preparation method of this structure of large area.
Technical background
SnO2As a kind of important feature semiconductor material with wide forbidden band, due to excellent optics, electrology characteristic,
There is wide potential application foreground in various fields such as gas sensor, transparent conductive material, solar cell, transistors.
Application due to special physical attribute and in nanoscale devices, in recent years nanostructured caused strong emerging of people
Interest.SnO2The research of nanostructured also achieves great progress, and in recent years, people utilize solwution method, molecular beam epitaxy, pulse
Laser deposition, a variety of methods such as metal-organic chemical vapor deposition equipment have prepared the abundant SnO of pattern2Nanostructured, for example
Nano wire, nanobelt, herring-bone form, in a zigzag etc. nanostructured all it has been reported that however, but also few by sheet SnO2Composition
Nanometer wall construction is reported.Develop some simple and effective SnO2Preparation method of nano material, the SnO of complex functionality2Nano junction
The architecture that structure is assembled is still a very big challenge.
The content of the invention
It is an object of the invention to provide a kind of nanometer wall construction being made up of sheet tin oxide and preparation method thereof.
The nanometer wall construction provided by the present invention being made up of sheet tin oxide, is to report first in the world.This knot
Structure is by sheet tin oxide nano structure composition, and the edge of nm wall is irregular, and the side of each wall is also rough, and its diameter about exists
100-1000nm, thickness is about 30nm.
A kind of method for preparing the nanometer wall construction being made up of sheet tin oxide, its concrete technology is as follows：
1. stannous oxide powder and carbon dust in mass ratio 1~3: 1 is matched, plus absolute ethyl alcohol, it is sufficiently mixed by ultrasound
After dry as source material；
2. the tubular type growth furnace of horizontal positioned is heated to 650~850 DEG C with 15 DEG C/min speed；
3. source material is laid in a quartz boat, a silicon chip is put under source material at air port as substrate transverse,
The distance of substrate and source material about 0.5~1cm, is put into the quartz boat in the source that is loaded with and substrate the horizontal pipe furnace heated in advance
Middle part；
4. being passed through high-purity argon gas that flow is 0.3L/min~0.5L/min as protection gas, the gas outlet of high-temperature smelting pot is protected
Semi-closed state is held, turns off stove after reacting 60~90min under atmospheric pressure, it is naturally cooled to room temperature, in this process
In remain that argon flow amount is constant；
5. taking out quartz boat, the uniform white flock material of a layer thickness is deposited on a silicon substrate.
The quartzy length of tube for the horizontal pipe furnace mentioned in the process step of the invention 2 is 110cm, a diameter of 8cm.
By changing the proportioning of source material, and the control to some parameters in thermal evaporation process, synthesize by sheet
SnO2The nanometer wall construction of composition.Relative to the synthetic method of other tin oxide nano structures, outstanding feature of the invention is：
(1) reaction pressure environment is only required to be normal pressure, and reaction temperature is low, reduces the requirement to equipment；(2) it is not related to chemical solution,
Reduce environmental pollution；(3) a large amount of carrier gas are not needed, it is only necessary to which a small amount of high-purity argon gas is made in protective gas, diluting reaction environment
Oxygen content；(4) method is simple, and low cost is reproducible, and can raised growth.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrum of sample.
Fig. 2 be sample ESEM (SEM) picture, wherein (a) (b) for sample low power and in times scanning electron microscope (SEM) photograph
Picture, (c) is the image of its partial enlargement.
Embodiment
The technical characterstic of the present invention is further illustrated with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1：
1. stannous oxide powder and carbon dust are matched by 2.5: 1 mass ratio, plus absolute ethyl alcohol, it is sufficiently mixed by ultrasound
After dry as source material；
2. the tubular type growth furnace of horizontal positioned is heated to 650 DEG C with 15 DEG C/min speed；
3. source material is laid in a quartz boat, a silicon chip is put under source material at air port as substrate transverse,
The distance of substrate and source material about 0.5cm, is put into the quartz boat in the source that is loaded with and substrate the horizontal pipe furnace that heats in advance
Middle part；
4. being passed through high-purity argon gas that flow is 0.5L/min as protection gas, the gas outlet of high-temperature smelting pot keeps semiclosed shape
State, turns off stove after reacting 90min under atmospheric pressure, it is naturally cooled to room temperature, argon gas is remained in the process
Flow is constant；
5. taking out quartz boat, the uniform white flock material of a layer thickness is deposited on a silicon substrate.
Embodiment 2：
1. stannous oxide powder and carbon dust are matched by 1: 1 mass ratio, plus absolute ethyl alcohol, after being sufficiently mixed by ultrasound
Drying is used as source material；
2. the tubular type growth furnace of horizontal positioned is heated to 750 DEG C with 15 DEG C/min speed；
3. source material is laid in a quartz boat, a silicon chip is put under source material at air port as substrate transverse,
The distance of substrate and source material about 0.5cm, is put into the quartz boat in the source that is loaded with and substrate the horizontal pipe furnace that heats in advance
Middle part；
4. being passed through high-purity argon gas that flow is 0.4L/min as protection gas, the gas outlet of high-temperature smelting pot keeps semiclosed shape
State, turns off stove after reacting 70min under atmospheric pressure, it is naturally cooled to room temperature, argon gas is remained in the process
Flow is constant；
5. taking out quartz boat, the uniform white flock material of a layer thickness is deposited on a silicon substrate.
Embodiment 3：
1. stannous oxide powder and carbon dust are matched by 3: 1 mass ratio, plus absolute ethyl alcohol, after being sufficiently mixed by ultrasound
Drying is used as source material；
2. the tubular type growth furnace of horizontal positioned is heated to 850 DEG C with 15 DEG C/min speed；
3. source material is laid in a quartz boat, a silicon chip is put under source material at air port as substrate transverse,
The distance of substrate and source material about 0.5cm, is put into the quartz boat in the source that is loaded with and substrate the horizontal pipe furnace that heats in advance
Middle part；
4. being passed through high-purity argon gas that flow is 0.3L/min as protection gas, the gas outlet of high-temperature smelting pot keeps semiclosed shape
State, turns off stove after reacting 60min under atmospheric pressure, it is naturally cooled to room temperature, argon gas is remained in the process
Flow is constant；
5. taking out quartz boat, the uniform white flock material of a layer thickness is deposited on a silicon substrate.
The X-ray diffractogram of above-described embodiment products therefrom is as shown in figure 1, as can be seen that most three strong diffraction in figure
Peak is the diffraction maximum of tin oxide.Illustrate the rutile structure tin oxide that the sample obtained by us is Tetragonal, lattice constant is a
The diffraction maximum data fit of the dated relevant tin oxide of=b=0.4739nm, c=0.3186nm, with JCPDS file it is fine
(Powder Diffraction File Compiled by the Joint Committee on Powder
Diffraction, 1985, Card No.77-0448).In addition other oxides or other impurities peak without tin are present, can be with
It is pure tin oxide structure to illustrate our made samples.
The SEM photograph of products therefrom as shown in Fig. 2 wherein (a) (b) for sample low power and in times scanning electron microscope image,
There it can be seen that substrate is by substantial amounts of sheet tin oxide film uniform fold, (c) is to learn in the image of its partial enlargement, figure,
Products therefrom is the nanometer wall construction that is made up of sheet tin oxide, and the edge of the structure is simultaneously irregular, and the side of each wall is also not only
Sliding, its diameter is about in 100-1000nm, and thickness is about 30nm.
Claims (1)
1. a kind of preparation technology for the nanometer wall construction being made up of sheet tin oxide, it is characterised in that the nanometer wall construction
Edge is irregular, and the side of each wall is rough, its a diameter of 100~1000nm, and thickness is 30nm, the step of the preparation technology
It is as follows：
1) it is in mass ratio 2.5: 1 proportionings, plus absolute ethyl alcohol by stannous oxide powder and carbon dust, is dried after being sufficiently mixed by ultrasound
It is dry to be used as source material；
2) the tubular type growth furnace of horizontal positioned is heated to 650 DEG C with 15 DEG C/min speed；The quartz of the tubular type growth furnace
Length of tube is 110cm, a diameter of 8cm；
3) source material is laid in a quartz boat, a silicon chip is put in the leeward of the source material as substrate transverse
At mouthful, the distance of the substrate and the source material is 0.5cm, and the quartz boat for being loaded with the source material and the substrate is put into
The middle part of the tubular type growth furnace heated in advance；
4) be passed through into the tubular type growth furnace flow be 0.5L/min high-purity argon gas as protection gas, the tubular type growth furnace
Gas outlet keep semi-closed state, turn off the tubular type growth furnace after reacting 90min under atmospheric pressure, give birth to the tubular type
Long stove naturally cools to room temperature, remains that argon flow amount is constant in the process；
5) quartz boat is taken out, the uniform white flock material of a layer thickness is deposited over the substrate.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107619065A (en) * | 2017-08-02 | 2018-01-23 | 上海纳米技术及应用国家工程研究中心有限公司 | One kind improves SnO2The method of nano material air-sensitive performance |
| CN108842142B (en) * | 2018-07-03 | 2021-03-26 | 河北工业大学 | Film composed of micron-sized pentagonal stannous oxide and preparation method thereof |
| CN109553126B (en) * | 2019-01-02 | 2021-08-10 | 华南理工大学 | Method for preparing stannic oxide crystal by thermal evaporation |
| CN111965324A (en) * | 2020-08-24 | 2020-11-20 | 深圳市美克森电子有限公司 | Preparation method of silicon-resistant gas-sensitive detection body of methane gas sensor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306835A (en) * | 2008-04-22 | 2008-11-19 | 华东师范大学 | SnO2 complex three-dimensional nanostructure and method for preparing same |
| CN101823703A (en) * | 2009-03-06 | 2010-09-08 | 中国科学院宁波材料技术与工程研究所 | Controllable preparation method for petaliform tin oxide nano powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306835A (en) * | 2008-04-22 | 2008-11-19 | 华东师范大学 | SnO2 complex three-dimensional nanostructure and method for preparing same |
| CN101823703A (en) * | 2009-03-06 | 2010-09-08 | 中国科学院宁波材料技术与工程研究所 | Controllable preparation method for petaliform tin oxide nano powder |
Non-Patent Citations (6)
| Title |
|---|
| Growth and characterization of single crystalline tin oxide (SnO2) nanowires;S. Budak et al.;《Journal of Crystal Growth》;20060601;第291卷(第2期);第405-411期 * |
| Metal oxide and hydroxide nanoarrays: Hydrothermal synthesis and applications as supercapacitors and nanocatalysts;Qiu Yang et al.;《Chinese Materials Research Society》;20130722;第23卷(第4期);第351-366页 * |
| SnO2 nanowall-arrays coated with rutile-TiO2 nanoneedles for high performance dye-sensitized solar cells;Dipak V. Shinde et al;《Dalton Trans.》;20120717;第41卷(第34期);第10161-10163页 * |
| SnO2和SnO2基纳米材料的制备、表征和磁性研究;张莉;《中国优秀博硕士学位论文全文数据库 (博士) 工程科技Ⅰ辑 （月刊 ） 》;20101015(第10期);正文第35页 * |
| Synthesis, photoluminescence and dielectric properties of O-deficient SnO2 nanowires;P.G.Li et al.;《Journal of Alloys and Compounds》;20090129;第479卷(第1-2期);第74-77页 * |
| 碳热还原法制备SnO2纳米带及其表征分析;倪自丰等;《无机材料学报》;20070731;第22卷(第4期);第609-612页 * |
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