CN107764872A - The nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire - Google Patents

The nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire Download PDF

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CN107764872A
CN107764872A CN201710875896.1A CN201710875896A CN107764872A CN 107764872 A CN107764872 A CN 107764872A CN 201710875896 A CN201710875896 A CN 201710875896A CN 107764872 A CN107764872 A CN 107764872A
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vanadium dioxide
dioxide nanowire
gold
nanowire
modification
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梁继然
朱奎龙
杨然
郭津榜
周立伟
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Tianjin University
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    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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    • G01N27/127Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles

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Abstract

The present invention relates to a kind of nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire, this method step mainly includes:The cleaning of quartz plate is not polished;Grow vanadium dioxide nanowire;Gold grain is modified and prepared by platinum electrode:Gold grain modification vanadium dioxide nanowire is placed in the high vacuum magnetron sputtering coaters of JCP 200, platinum electrode is prepared with template.The shortcomings that present invention overcomes conventional Metal Oxide Semiconductor Gas Sensing element manipulation temperature high, by one-dimensional nano structure, with reference to modification of the metal-modified to device, developing the NO of low operating temperature2There is very important researching value and application prospect in terms of sensor.

Description

The nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire
Technical field
The present invention relates to semiconductor gas sensor field, and in particular to a kind of dioxy of gold modification vanadium dioxide nanowire Change nitrogen transducer production method.
Background technology
Modern industry also brings unprecedented destruction while rapid development to natural environment for the survival of mankind. In recent years, it is serious all the more situations such as acid rain, greenhouse effects, not only environment is caused seriously to pollute, has also threatened the life of the mankind Health.NO2It is the important arch-criminal to form acid rain and photochemical fog, while is a kind of inflammable and explosive toxic gas again.Suction Excessive NO2, the various respiratory disorders such as pulmonary edema can be caused, human body is caused greatly to injure.Therefore, it is excellent to develop a performance Good NO2Gas sensor, tool are of great significance.
In various types of gas sensors, Metal Oxide Semiconductor Gas Sensing sensor is because of its high sensitivity, response The advantages such as speed is fast, manufacturing cost is low are widely used.Currently used as NO2The metal oxide of gas sensor is partly led Body sensitive material mainly has ZnO, SnO2、WO3And Cu2O etc., wherein with WO3And SnO2Both materials are most commonly seen.However, this A little sensors are wanted to realize preferable performance, need to work at high temperature.Operating temperature on how to reduce sensor is current still It is the emphasis of research.For vanadium dioxide as a kind of new Metal oxide semiconductor gas-sensitiveness material, being found can be in room temperature Lower detection NO2, gas sensor is made with vanadium dioxide, can be achieved to reduce the purpose of operating temperature.In addition, monodimension nanometer material has There is the features such as specific surface area is big, and avtive spot is more, be advantageous to the diffusion response of gas and recover.In addition, what metal-modified was formed Schottky junction, the absorption and decomposition of gas can be accelerated, so as to greatly improve the gas sensitivity of sensing element.
The content of the invention
The shortcomings that it is an object of the invention to overcome conventional Metal Oxide Semiconductor Gas Sensing element manipulation temperature high, pass through A kind of one-dimensional nano structure, with reference to modification of the metal-modified to device, it is proposed that gold modification with higher sensitivity at room temperature Vanadium dioxide nanowire gas sensor, developing the NO of low operating temperature2There is very important research valency in terms of sensor Value and application prospect.
Technical scheme:The nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire, should Method comprises the following steps:
(1) cleaning does not polish quartz plate;
(2) vanadium dioxide nanowire is grown;
(3) vanadium dioxide nanowire grown in gold grain modification above-mentioned steps (2);
(4) prepared by platinum electrode:The vanadium dioxide nanowire of gold grain modification growth in above-mentioned steps (3) is placed in high vacuum In magnetron sputtering coater, platinum electrode is prepared with template.
The step (1) is specifically:Quartz plate is sequentially placed into acetone solvent (Nong Du≤99.5%) and absolute ethyl alcohol (Nong Du≤99.7%) in be cleaned by ultrasonic 15min, to remove surface and oil contaminant and organic impurities;Then put it into deionized water Middle cleaning, it is placed in thoroughly drying in infrared baking oven.
The step (2) using chemical meteorology deposition method growth vanadium dioxide nanowire, using purity as 99.99% five oxygen It is reaction raw materials to change two vanadium powders, using argon gas as carrier gas, grows vanadium dioxide nanowire at 900 DEG C, during keep 50~100pa intraductal pressure and 90~100sccm gas flow rate, specifically include following steps:
(a) electronic balance weighing 0.2g vanadium pentoxide powders (purity 99.99%), are used first, by its uniform placement In quartz boat;
(b) it is 400mm that the quartz boat equipped with vanadium pentoxide powder, is put into a length, a diameter of 40mm quartz Pipe center;
(c), quartz plate substrate cleaned in step (1) is put into quartz ampoule, away from 4 ± 0.5mm of quartz boat;(d), will This quartz ampoule is put into GSL-1400X type tube furnaces, is evacuated down to below 10pa, leads to argon gas, keeps pressure left in 50~100pa It is right;
(e), heat up:900 DEG C are heated to from room temperature with 5~7 DEG C/min programming rate, is incubated 3~4h;
(f) 300 DEG C, are reduced the temperature to 5~7 DEG C/min speed, stove is closed, room temperature is naturally cooled to, in this process In remain 50~100pa intraductal pressure and 90~100sccm argon gas flow velocity;
(g), after stove is cooled to room temperature, sample is taken out.
The step (3) is specifically:The vanadium dioxide nanowire of growth in above-mentioned steps (2) is put into small ion sputtering The modification of gold particle is carried out in instrument;After sputtering, the sample of gained is put into quick anneal oven and annealed, makes gold grain Good Ohmic contact is formed with vanadium dioxide nanowire surface.
Compared with prior art, the present invention has the advantage that:
(1), the vanadium dioxide nanowire length for preparing of the present invention has big specific surface area, big ratio in micron level Surface area provides more avtive spots, allows gas sensor quick detection NO at room temperature2Gas, so as to lift air-sensitive The sensitivity of sensor.
(2), using Preparation equipment is easy to operate, technological parameter is easily controllable, cost is cheap:The present invention is sunk with chemical vapor Area method prepares vanadium dioxide nanowire, and this method technique is simple compared with the method that other prepare vanadium dioxide nanowire, parameter Less, controllability is high, reproducible.
(3), the present invention has higher sensitivity and selectivity, the gold modification vanadium dioxide nanowire gas of nitrogen dioxide gas Dependent sensor can detect at room temperature, and gold is used as a kind of precious metal material, can be formed with metal oxide semiconductor material surface Schottky junction, schottky junction can form depletion layer on the surface of gas sensor, so as to reduce the conducting channel of gas sensor, lifting Gas sensitivity.
(4), gold particle also has catalytic action to nitrogen dioxide gas, can accelerate nitrogen dioxide in semiconductor surface Decompose, so as to cause the change of the electrical conductivity of whole sensitive material, improve the activity of sensor, reduce its operating temperature.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of vanadium dioxide nanowire:(a) scale is 10 μm;(b) scale is 100nm.
Fig. 2 is gold modification vanadium dioxide nanowire gas-sensitive sensor structure schematic diagram.
Fig. 3 is gold modification vanadium dioxide nanowire gas sensor material XRD characterization results.
Fig. 4 is gold modification vanadium dioxide nanowire gas sensor material EDS characterization results.
Fig. 5 is gold modification vanadium dioxide nanowire gas sensor material phase transformation characteristic present's result.
Fig. 6 is gold modification vanadium dioxide nanowire gas sensor at room temperature to 0.5ppm~5ppm NO2Gas moves State continuous response curve.
Embodiment
Below by specific embodiments and the drawings, the present invention is further illustrated.Embodiments of the invention are in order to more Those skilled in the art is more fully understood the present invention well, any limitation is not made to the present invention.
The technical scheme is that the nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire, should Method comprises the following steps:
(1) the unpolished quartz plate in surface, is cleaned:
This substrate used is the unpolished circular quartz piece (frosted glass plate) in surface, and quartzy chip size is:Diameter 15mm, thickness 2mm.
Substrate is sequentially placed into acetone solvent (Nong Du≤99.5%), absolute ethyl alcohol (Nong Du≤99.7%) in ultrasound it is clear 15min is washed, to remove surface and oil contaminant and organic impurities;Then put it into deionized water and clean, be placed in infrared baking oven In thoroughly dry.
(2) vanadium dioxide nanowire, is grown, this experiment is using vanadic anhydride as reaction raw materials, using chemical vapor Sedimentation, grow vanadium dioxide nanowire in GSL-1400X type tube furnaces:
Electronic balance weighing 0.2g vanadium pentoxide powders (purity 99.99%) are used first, and it is uniformly placed on stone Ying Zhouzhong;
Then, it is 400mm the quartz boat equipped with vanadium pentoxide powder to be put into a length, a diameter of 40mm quartz Pipe center;
Quartz plate substrate cleaned in step (1) is put into quartz ampoule again, away from 4 ± 0.5mm of quartz boat;
This quartz ampoule is put into GSL-1400X type tube furnaces afterwards, is evacuated down to below 10pa, leads to argon gas, keeps pressure By force in 50~100pa;
Heating, 900 DEG C are heated to from room temperature with 5~7 DEG C/min programming rate, is incubated 3~4h;
300 DEG C are reduced the temperature to 5~7 DEG C/min speed, stove is closed, naturally cools to room temperature, in the process, is begun 50~100pa intraductal pressure and 90~100sccm argon gas flow velocity are kept eventually;
After stove is cooled to room temperature, sample is taken out.
(3), gold grain modification vanadium dioxide nanowire:
The vanadium dioxide nanowire of growth in step (2) is put into SBC-12 small ion sputters and carries out gold particle Modification, sputtering time 10s.In sputter procedure, 5~6pa pressure is kept in instrument, sputtering power maintains 2.1~2.3W. After sputtering, the sample of gained is put into quick anneal oven and annealed, annealing temperature is 400 DEG C, time 1min.This Step forms good Ohmic contact to ensure gold grain and vanadium dioxide nanowire surface.
(4) platinum electrode, is prepared:
First, it is 1~2cm to prepare with two spacing, and size is the template of 2mm × 2mm square aperture, by it It is covered in above-mentioned steps (3) on gold grain modification vanadium dioxide nanowire;
Then, the device for covering template is put into JCP-200 high vacuum magnetron sputtering coaters;
Finally, it is argon gas 22~24sccm of flow velocity to set instrument parameter, sputtering pressure 4.0~5.0 × 10-5Pa, sputter work( 95~100W of rate, sputtering time 2min, the Platinum Electrode Thickness prepared are 80~120nm.
Target in JCP-200 high vacuum magnetron sputtering coaters uses purity to be splashed for 99.95% high purity metal platinum During penetrating, substrate remains at room temperature.
Embodiment 1:The technical scheme is that the nitrogen dioxide gas sensor system of gold modification vanadium dioxide nanowire Preparation Method, this method comprise the following steps:
(1) the unpolished quartz plate in surface, is cleaned:
This substrate used is the unpolished circular quartz piece (frosted glass plate) in surface, and quartzy chip size is:Diameter 15mm, thickness 2mm.
Substrate is sequentially placed into acetone solvent (Nong Du≤99.5%), absolute ethyl alcohol (Nong Du≤99.7%) in ultrasound it is clear 15min is washed, to remove surface and oil contaminant and organic impurities;Then put it into deionized water and clean, be placed in infrared baking oven In thoroughly dry.
(2) vanadium dioxide nanowire, is grown, this experiment is using vanadic anhydride as reaction raw materials, using chemical vapor Sedimentation, grow vanadium dioxide nanowire in GSL-1400X type tube furnaces:
Electronic balance weighing 0.2g vanadium pentoxide powders (purity 99.99%) are used first, and it is uniformly placed on stone Ying Zhouzhong;
Then, it is 400mm the quartz boat equipped with vanadium pentoxide powder to be put into a length, a diameter of 40mm quartz Pipe center;
Quartz plate substrate cleaned in step (1) is put into quartz ampoule again, away from quartz boat 4mm;
This quartz ampoule is put into GSL-1400X type tube furnaces afterwards, is evacuated down to below 10pa, leads to argon gas, keeps pressure By force in 50pa;
Heating, 900 DEG C are heated to from room temperature with 5 DEG C/min programming rate, is incubated 4h;
300 DEG C are reduced the temperature to 5 DEG C/min speed, stove is closed, naturally cools to room temperature, in the process, all the time Keep 50pa intraductal pressure and 90sccm argon gas flow velocity;
After stove is cooled to room temperature, sample is taken out.
(3), gold grain modification vanadium dioxide nanowire:
Obtained vanadium dioxide nanowire in step (2) is put into SBC-12 small ion sputters and carries out gold particle Modification, sputtering time 10s.In sputter procedure, 5pa pressure is kept in instrument, sputtering power maintains 2.1w.Sputtering finishes Afterwards, the sample of gained is put into quick anneal oven and annealed, annealing temperature is 400 DEG C, time 1min.This step in order to Ensure that gold grain forms good Ohmic contact with vanadium dioxide nanowire surface.
(4) platinum electrode, is prepared:
First, it is 1cm to prepare with two spacing, and size is the template of 2mm × 2mm square aperture, is covered Cover in above-mentioned steps (3) on gold grain modification vanadium dioxide nanowire;
Then, the device for covering template is put into JCP-200 high vacuum magnetron sputtering coaters;
Finally, it is argon gas flow velocity 22sccm to set instrument parameter, sputtering pressure 4.0 × 10-5Pa, sputtering power 95W, sputtering Time 2min, the Platinum Electrode Thickness prepared are 80~120nm.
Target in JCP-200 high vacuum magnetron sputtering coaters uses purity to be splashed for 99.95% high purity metal platinum During penetrating, substrate remains at room temperature.
Fig. 1 is the electron scanning micrograph of vanadium dioxide nanowire, and a, b icon chi are respectively 10 μm and 100nm.From Fig. 1 can be seen that vanadium dioxide nanowire average diameter is 900nm, and average length is 25 μm.
Fig. 2 is gold modification vanadium dioxide nanowire gas-sensitive sensor structure schematic diagram.
Fig. 3 is gold modification vanadium dioxide nanowire gas sensor material XRD characterization results.PDF card datas storehouse is contrasted, Collection of illustrative plates can be mapped well with JCPDS#72-0514, and the main component for illustrating sample is vanadium dioxide.At the same time, scheme In golden (Au) element also be present and part 13 aoxidizes the peak of six vanadium (V6O13), this is due to vanadic anhydride in growth course Reaction is incomplete, caused by generating six vanadium of oxidation of interphase 13.In this sensor, 13 six vanadium of oxidation are tested air-sensitive Result influence little, can ignore.
Fig. 4 is gold modification vanadium dioxide nanowire gas sensor material EDS characterization results.It can be seen that sensor be by Vanadium (V), oxygen (O) and golden (Au) are formed, and are consistent with XRD results.
Fig. 5 is gold modification vanadium dioxide nanowire gas sensor material phase transformation characteristic present's result.Can from figure Go out its phase time-varying amplitude and reached 3 orders of magnitude, illustrating the vanadium dioxide of generation has good crystallinity.
Fig. 6 is gold modification vanadium dioxide nanowire gas sensor at room temperature to 0.5ppm~5ppm nitrogen dioxide gas Dynamic continuous response curve.It can be seen that when sensor is exposed in nitrogen dioxide gas, the resistance of sensor is at once Increase, and after removing nitrogen dioxide gas, for sensor resistance almost back to original value, this shows that this sensor has good move State responds recovery characteristics.After the nitrogen dioxide test of four various concentrations, the recovery resistance and initial resistance of sensor it Between still without too big change, so as to confirm the stability of this sensor and repeatability.
Embodiment 2:Gold modification vanadium dioxide nanowire nitrogen dioxide gas sensor preparation method, this method include with Lower step:
(1) the unpolished quartz plate in surface, is cleaned:
This substrate used is the unpolished circular quartz piece (frosted glass plate) in surface, and quartzy chip size is:Diameter 15mm, thickness 2mm.
Substrate is sequentially placed into acetone solvent (Nong Du≤99.5%), absolute ethyl alcohol (Nong Du≤99.7%) in ultrasound it is clear 15min is washed, to remove surface and oil contaminant and organic impurities;Then put it into deionized water and clean, be placed in infrared baking oven In thoroughly dry.
(2) vanadium dioxide nanowire, is grown, this experiment is using vanadic anhydride as reaction raw materials, using chemical vapor Sedimentation, grow vanadium dioxide nanowire in GSL-1400X type tube furnaces:
Electronic balance weighing 0.2g vanadium pentoxide powders (purity 99.99%) are used first, and it is uniformly placed on stone Ying Zhouzhong;
Then, it is 400mm the quartz boat equipped with vanadium pentoxide powder to be put into a length, a diameter of 40mm quartz Pipe center;
Quartz plate substrate cleaned in step (1) is put into quartz ampoule again, away from quartz boat 4.5mm;
This quartz ampoule is put into GSL-1400X type tube furnaces afterwards, is evacuated down to below 10pa, leads to argon gas, keeps pressure By force in 100pa;
Heating, 900 DEG C are heated to from room temperature with 7 DEG C/min programming rate, is incubated 3h;
300 DEG C are reduced the temperature to 7 DEG C/min speed, stove is closed, naturally cools to room temperature, in the process, all the time Keep 100pa intraductal pressure and 100sccm argon gas flow velocity;
After stove is cooled to room temperature, sample is taken out.
(3), gold grain modification vanadium dioxide nanowire:
Obtained vanadium dioxide nanowire in step (2) is put into SBC-12 small ion sputters and carries out gold particle Modification, sputtering time 10s.In sputter procedure, 6pa pressure is kept in instrument, sputtering power maintains 2.3w.Sputtering finishes Afterwards, the sample of gained is put into quick anneal oven and annealed, annealing temperature is 400 DEG C, time 1min.This step in order to Ensure that gold grain forms good Ohmic contact with vanadium dioxide nanowire surface.
(4) platinum electrode, is prepared:
First, it is 2cm to prepare with two spacing, and size is the template of 2mm × 2mm square aperture, is covered Cover in above-mentioned steps (3) on gold grain modification vanadium dioxide nanowire;
Then, the device for covering template is put into JCP-200 high vacuum magnetron sputtering coaters;
Finally, it is argon gas flow velocity 24sccm to set instrument parameter, sputtering pressure 5.0 × 10-5Pa, sputtering power 100W, splashes Time 2min is penetrated, the Platinum Electrode Thickness prepared is 80~120nm.
Target in JCP-200 high vacuum magnetron sputtering coaters uses purity to be splashed for 99.95% high purity metal platinum During penetrating, substrate remains at room temperature.
Embodiment 3:Gold modification vanadium dioxide nanowire nitrogen dioxide gas sensor preparation method, this method include with Lower step:
(1) the unpolished quartz plate in surface, is cleaned:
This substrate used is the unpolished circular quartz piece (frosted glass plate) in surface, and quartzy chip size is:Diameter 15mm, thickness 2mm.
Substrate is sequentially placed into acetone solvent (Nong Du≤99.5%), absolute ethyl alcohol (Nong Du≤99.7%) in ultrasound it is clear 15min is washed, to remove surface and oil contaminant and organic impurities;Then put it into deionized water and clean, be placed in infrared baking oven In thoroughly dry.
(2) vanadium dioxide nanowire, is grown, this experiment is using vanadic anhydride as reaction raw materials, using chemical vapor Sedimentation, grow vanadium dioxide nanowire in GSL-1400X type tube furnaces:
Electronic balance weighing 0.2g vanadium pentoxide powders (purity 99.99%) are used first, and it is uniformly placed on stone Ying Zhouzhong;
Then, it is 400mm the quartz boat equipped with vanadium pentoxide powder to be put into a length, a diameter of 40mm quartz Pipe center;
Quartz plate substrate cleaned in step (1) is put into quartz ampoule again, away from quartz boat 3.5mm;
This quartz ampoule is put into GSL-1400X type tube furnaces afterwards, is evacuated down to below 10pa, leads to argon gas, keeps pressure By force in 75pa;
Heating, 900 DEG C are heated to from room temperature with 6 DEG C/min programming rate, is incubated 3h;
300 DEG C are reduced the temperature to 6 DEG C/min speed, stove is closed, naturally cools to room temperature, in the process, all the time Keep 75pa intraductal pressure and 95sccm argon gas flow velocity;
After stove is cooled to room temperature, sample is taken out.
(3), gold grain modification vanadium dioxide nanowire:
Obtained vanadium dioxide nanowire in step (2) is put into SBC-12 small ion sputters and carries out gold particle Modification, sputtering time 10s.In sputter procedure, 6pa pressure is kept in instrument, sputtering power maintains 2.3w.Sputtering finishes Afterwards, the sample of gained is put into quick anneal oven and annealed, annealing temperature is 400 DEG C, time 1min.This step in order to Ensure that gold grain forms good Ohmic contact with vanadium dioxide nanowire surface.
(4) platinum electrode is prepared:
First, it is 2cm to prepare with two spacing, and size is the template of 2mm × 2mm square aperture, is covered Cover in above-mentioned steps (3) on gold grain modification vanadium dioxide nanowire;
Then, the device for covering template is put into JCP-200 high vacuum magnetron sputtering coaters;
Finally, it is argon gas flow velocity 23sccm to set instrument parameter, sputtering pressure 4.5 × 10-5Pa, sputtering power 100W, splashes Time 2min is penetrated, the Platinum Electrode Thickness prepared is 80~120nm.
Target in JCP-200 high vacuum magnetron sputtering coaters uses purity to be splashed for 99.95% high purity metal platinum During penetrating, substrate remains at room temperature.
It should be appreciated that embodiment and example discussed herein simply to illustrate that, to those skilled in the art For, it can be improved or be converted, and all these modifications and variations should all belong to the protection of appended claims of the present invention Scope.

Claims (4)

1. gold medal modifies the nitrogen dioxide gas sensor preparation method of vanadium dioxide nanowire, it is characterised in that this method includes Following steps:
(1) cleaning does not polish quartz plate;
(2) vanadium dioxide nanowire is grown;
(3) vanadium dioxide nanowire grown in gold grain modification above-mentioned steps (2);
(4) prepared by platinum electrode:The vanadium dioxide nanowire of gold grain modification growth in above-mentioned steps (3) is placed in high vacuum magnetic control In sputter coating machine, platinum electrode is prepared with template.
2. preparation method according to claim 1, it is characterised in that the step (1) is specifically:Quartz plate is put successively Enter to acetone solvent (Nong Du≤99.5%) and absolute ethyl alcohol (Nong Du≤99.7%) in be cleaned by ultrasonic 15min, to remove surface Greasy dirt and organic impurities;Then put it into deionized water and clean, be placed in thoroughly drying in infrared baking oven.
3. preparation method according to claim 1, it is characterised in that the step (2) is given birth to using chemical meteorology deposition method Long vanadium dioxide nanowire, using the vanadium pentoxide powder that purity is 99.99% as reaction raw materials, using argon gas as carrier gas, Grow vanadium dioxide nanowire at 900 DEG C, during keep 50~100pa intraductal pressure and 90~100sccm gas Flow velocity, specifically include following steps:
(a) electronic balance weighing 0.2g vanadium pentoxide powders (purity 99.99%), are used first, and it is uniformly placed on stone Ying Zhouzhong;
(b) it is 400mm that the quartz boat equipped with vanadium pentoxide powder, is put into a length, in a diameter of 40mm quartz ampoule Centre;
(c), quartz plate substrate cleaned in step (1) is put into quartz ampoule, away from 4 ± 0.5mm of quartz boat;
(d), this quartz ampoule is put into GSL-1400X type tube furnaces, is evacuated down to below 10pa, leads to argon gas, keeps pressure to exist 50~100pa or so;
(e), heat up:900 DEG C are heated to from room temperature with 5~7 DEG C/min programming rate, is incubated 3~4h;
(f) 300 DEG C, are reduced the temperature to 5~7 DEG C/min speed, stove is closed, naturally cools to room temperature, begin in the process 50~100pa intraductal pressure and 90~100sccm argon gas flow velocity are kept eventually;
(g), after stove is cooled to room temperature, sample is taken out.
4. preparation method according to claim 1, it is characterised in that the step (3) is specifically:By above-mentioned steps (2) The vanadium dioxide nanowire of middle growth is put into the modification that gold particle is carried out in small ion sputter;After sputtering, by gained Sample be put into quick anneal oven and annealed, gold grain is formed good ohm with vanadium dioxide nanowire surface and connect Touch.
CN201710875896.1A 2017-09-25 2017-09-25 The nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire Pending CN107764872A (en)

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D. WANG ET AL.: "Room temperature NO2 gas sensing of Au-loaded tungsten oxide nanowires/porous silicon hybrid structure", 《CHINESE PHYSICS B》 *
J. LIANG ET AL.: "Room temperature NO2 sensing performance of free-standing mesh-structure vanadium dioxide nanorods by a chemical vapour deposition method", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *

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* Cited by examiner, † Cited by third party
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CN109536990A (en) * 2018-10-15 2019-03-29 华南理工大学 A kind of flat thin-film electro catalyst operation electrode and its preparation method and application
CN110806432A (en) * 2019-11-19 2020-02-18 清华大学 Micro-hotplate and method for producing a micro-hotplate
CN113155762A (en) * 2021-04-14 2021-07-23 贵阳海关综合技术中心(贵州国际旅行卫生保健中心、贵阳海关口岸门诊部) Based on V6O13Method for detecting Cd (II) and Pb (II) with nanobelt catalytic activity

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