CN106153689A - The application in detection nitrogen dioxide of the tungsten oxide vanadium oxide heterojunction nano-wire array - Google Patents
The application in detection nitrogen dioxide of the tungsten oxide vanadium oxide heterojunction nano-wire array Download PDFInfo
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Abstract
The present invention provides the application in detection nitrogen dioxide of the tungsten oxide/vanadium oxide heterojunction nano-wire array, the annealing heat treatment including the tungsten oxide nano plated surface vanadium after deposits tungsten film material plies, the crystalline growth of tungsten oxide nano, the annealing of tungsten oxide nano, annealing, carrying out vanadium and the making of electrode.The invention has the beneficial effects as follows that appearance structure is one-dimensional nano line array, there is the highest specific surface area, can give full play to the superiority of hetero-junctions, the direct special band structure of hetero-junctions can effectively reduce the operating temperature of gas sensor, the sensitivity improving sensor and response speed.Processing technology is ripe, easy to use, cheap, and be expected to put it in gas sensor field application.
Description
Technical field
The present invention relates to oxides of nitrogen gas detection technique field, more specifically to tungsten oxide vanadium oxide hetero-junctions nanometer
Linear array application in detection nitrogen dioxide.
Background technology
Entering 21 century, industrialized level is fast-developing, but the natural environment that the mankind depend on for existence suffers seriously with ecology
Destroy, air also exists a large amount of toxic and harmful (such as NO2, NO, H2S, CO, SO2 etc.).NOx class is poisonous
Gas, it is possible to form acid rain corrosion building and skin, also can produce chemical fumes, sucks and causes cough, makes what is more
Become respiratory tract disease.Therefore efficient and accurately detection and prevention toxic and harmful sensor is made very urgent.Obtain
Obtain high performance nano-sensor, first will prepare and the nano material of these high-performance probabilities can be provided.
MOS type gas sensor has low cost, high sensitivity, it is easy to control and the advantage of operation, thus
Paid close attention to by the most widely, but study at present more ripe gas sensitive metal-oxide semiconductor (MOS) have ZnO, SnO2,
TiO2 etc., but they all cannot be used for efficient detection NOx class gas.Along with research deeply, Akiyama M in 1991
It is the high sensitive material detecting NOx in the environment of 300 degree etc. reporting WO3 pottery.Since then, numerous scientific research work is caused
Author's research to WO3.
WO3 is a kind of metal-oxide semiconductor (MOS), is a kind of surface conductance (resistance) control type gas sensitive.WO3 crystal
The atomic property on surface is enlivened, easy adsorption gas molecule, and when gas molecule absorption is at plane of crystal, in being made it
There is corresponding change in portion's carrier concentration, shows as the resistance variations of sensor.In view of the atom that enlivens of tungsten oxide is positioned at
Plane of crystal expands the contact area of plane of crystal and gas the most greatly, it is possible to effectively improve air-sensitive performance.One-dimensional
The tungsten oxide of nano thread structure has attracted the research of numerous researcher because of its huge specific surface area.Through in recent years
Research can have been passed through hydro-thermal method, vapor phase method, sol-gel etc. and prepare.The results show, 1-dimention nano line structure
Tungsten oxide really improve the sensitivity of detected gas, but this still can not reach the requirement of the marketization and integra-tion application.
In order to obtain high selectivity, high sensitivity, low operating temperature, the gas sensor of high stability, can be heterogeneous by structure
Structurally-modified.Heterojunction structure is currently mainly applied to the scientific domains such as semiconductor laser, luminescent device, solar cell.
Summary of the invention
It is an object of the invention to overcome conventional gas sensitive element device operating temperature high, the shortcoming of the low grade of sensitivity, by gas phase side
Method prepares the good tungsten oxide of pattern/vanadium oxide heterojunction nano-wire array structure materials, and one-dimensional nano line array is huge
Specific surface area makes it have very in response speed in the sensitivity improving gas sensor with the heterojunction structure performance of its excellence
Important researching value.
The purpose of the present invention is achieved by following technical proposals.
The preparation method of a kind of tungsten oxide/vanadium oxide heterojunction nano-wire array sensing element, is carried out as steps described below:
Step 1, utilizes facing-target magnetron sputtering system deposits tungsten film material plies in substrate, using tungsten as target, with inertia
Gas is sputter gas, and sputtering operating air pressure is 1 2.0Pa, and sputtering power is 80-110W, and sputtering time is 15-20min；
Preferably noble gas is argon, helium or nitrogen, and sputtering operating air pressure is 2.0Pa, and sputtering power is 90-100W,
Sputtering time is 15-20min；
Step 2, the W film prepared step 1 at vacuum high-temperature tube furnace equipment carries out crystalline growth tungsten oxide nano,
Ambiance is the mixed gas of oxygen and argon, in tungsten oxide nano growth course, controls oxygen and argon flow amount
Being respectively 0.1sccm and 35-50sccm, in control stove, growth pressure is 140 160Pa, and tube furnace is from room temperature 20 25
Degree Celsius it is raised to 600-700 DEG C, 5 DEG C/min of heating rate, it is incubated 12 hours at 600-700 DEG C, then lowers the temperature 1
Hour to 300-400 DEG C, finally naturally cool to room temperature 20 25 degrees Celsius；
Preferably in growth course, control oxygen and argon flow amount is respectively 0.1sccm and 35sccm, control growth in stove
Pressure is 150Pa；Tube furnace is raised to 700 DEG C from room temperature 20 25 degrees Celsius, 5 DEG C/min of heating rate, at 700 DEG C
Being incubated 1 hour, then cooling 1 hour to 400 DEG C, finally naturally cools to room temperature 20 25 degrees Celsius.
Step 3, the annealing of tungsten oxide nano, tungsten oxide nano step 2 prepared is at 300-500 DEG C and sky
Anneal 1-2 hour under gas atmosphere, to stablize crystal orientation further；
Step 4, utilizes and deposits vanadium on the tungsten oxide nano layer of the substrate that facing-target magnetron sputtering system processes through step 3 preparation
Film, using vanadium metal as target, using noble gas as sputter gas, inert gas flow is 30-50sccm, sputters work
Being 2.0Pa as air pressure, sputtering power is 80-110W, and sputtering time is 2-5min；
Preferably noble gas is argon, helium or nitrogen, and sputtering operating air pressure is 2.0Pa, and sputtering power is 90-100W,
Sputtering time is 2 5min；
Step 5, carries out the annealing heat treatment of vanadium, the substrate processing the deposition vanadium metal film obtained through step 4 is existed
Anneal 12 hours under 300-500 DEG C and air atmosphere environment；
Preferably anneal 1 1.5 hours under 300-400 DEG C and air atmosphere environment；
Step 6, the making of electrode: the tungsten oxide/vanadium oxide heterojunction nano-wire array platinum plating that will prepare in step 5
Electrode, forming two spacing on tungsten oxide/vanadium oxide heterojunction nano-wire array by template is 0.5-2.5cm, size
For the electrode of 1mm*1mm-3mm*3mm, using argon as working gas, background vacuum 3-9 × 10-4Pa, uses radio frequency
Prepared by magnetron sputtering method, sputter 1-5min, film thickness 60-150nm,
Preferably two spacing are 1-2cm, and size is the electrode of 2mm*2mm, background vacuum 4-6 × 10-4Pa, employing is penetrated
Frequently prepared by magnetron sputtering method, sputters 2min, film thickness 80-120nm.
In step 1, the quality purity of target tungsten is 99.999%.
In step 4, the quality purity of target vanadium metal is 99.999%.
The quality purity of the noble gas used is 99.999%.
Described substrate is single-sided polishing silicon chip, or alumina ceramic plate.
In described step 6, target metal platinum is quality purity 99.95%, and the quality purity of the argon of use is 99.999%.
Hitachi scanning electron microscope Hitachi-S4800FESEM and NEC JEM-2100F Flied emission transmitted electron is used to show
Tungsten oxide/vanadium oxide heterojunction nano-wire array is analyzed understanding by micro mirror, tungsten oxide/vanadium oxide heterojunction nano-wire battle array
Row are made up of tungsten oxide/vanadium oxide heterojunction nano-wire, a length of 300 800nm of tungsten oxide/vanadium oxide heterojunction nano-wire,
A diameter of 10-20nm of described tungsten oxide nano, wraps up vanadium oxide, institute equably in the periphery of described tungsten oxide nano
The thickness stating vanadium oxide is that 20-30nm, tungsten oxide and vanadium oxide define coaxial nucleocapsid heterojunction structure, and this structure is optimum
Different heterojunction structure form, contrast mixing decentralized and laminate-type structure, coaxial nucleocapsid hetero-junctions has the most different of maximum
Matter junction area, has important function to playing hetero-junctions superiority.
Fig. 3 is prepared tungsten oxide/vanadium oxide heterojunction nano-wire array transmission electron micrograph and elementary analysis line
Scanning, line scanning result surface nuclear structure is mainly wolfram element, and shell is v element, absolutely proves that its structure is that nucleocapsid is different
Matter structure.Kernel is tungsten oxide nano, and diameter is about 20nm, and shell is the shell structurre of vanadium oxide, about 5-10nm.
Scale is 20nm；Transmission electron microscope is NEC JEM-2100F Flied emission transmission electron microscope；Fig. 4 is in embodiment
The structural representation of tungsten oxide/vanadium oxide heterojunction nano-wire array structure gas sensor；(1) represent silica-basedly；(2)
Represent the tungsten oxide nuclear structure formed；(3) the vanadium oxide shell formed is represented；(4) represent in preparation process (7) and receiving
The platinum electrode that nanowire surface makes, forms good contacting with nano wire, convenient connection with external measurement devices measures resistance
Value；(5) it is UT70D resistance detection equipment, detects the change of resistance in real time, and transmission is shown on computer；(6)
For gas sensor is placed in nitrogen dioxide atmosphere.
Fig. 5 is that gas responds detection platform schematic diagram, as follows.1 is air inlet, enters test by trace injectant
The tested gas of amount；2 is gas sensor element as shown in Figure 4, is connected with platinum electrode by probe, with external detection
Equipment connects；3 for can heat and keep to the platform needing temperature；4 seal container for taking the test made, and hold for 30L
Amount；5 is mini fan, helps gas diffusion, makes gas be dispersed in cube container；6 is gas outlet；7 is can
The electronic control equipment of control regulation temperature；8 is the UT70D resistance detection equipment of excellent Leadd B.V, and display probe connects in real time
The resistance value at place, and export to computer equipment；9 for being recorded as table the computer terminal shown by the resistance variations recorded；Logical
Cross and seal the air inlet that container head arranges and inject tested gas to sealing trace in container, by mini fan and give vent to anger
The common effect of mouth so that tested gas spreads in sealing container further, makes tested gas diffuse to be placed on heating
On gas sensor element on platform, electronic control equipment controls the temperature of heating platform in real time by temperature pilot,
Gas sensor element is connected, in order in real time with the UT70D resistance detection equipment of excellent Leadd B.V by sensing element wire
The resistance value of display probe junction, and by corresponding resistance test data transfer to computer terminal, will by computer terminal
All resistance test numerical value summary record becomes form.
Fig. 8 is the gas response detection platform shown in application drawing 5, contrasts this practicality tungsten oxide/vanadium oxide nucleocapsid heterojunction structure
The selectivity of nanowire array structure gas sensor at room temperature gas with various.Response intensity is defined as the electricity under tested gas
Resistance value in resistance value ratio air.By figure it is concluded that tungsten oxide/vanadium oxide nucleocapsid heterogeneous structural nano linear array structure
Gas sensor can the most effectively detect nitrogen dioxide, and the minimal detectable concentration of nitrogen dioxide is 5ppm.
The invention have the benefit that the invention provides a kind of method with low cost uses vapor phase method to prepare one-dimensional knot
The tungsten oxide of structure/vanadium oxide heterojunction nano-wire, has equipment simple compared with the method such as existing thermal evaporation, electro-deposition,
Easy to operate, the advantages such as technological parameter is easily controllable, with low cost.Single tungsten oxide nano gas under 100 degree is anti-
Under Ying Yuben hetero-junctions sensor at room temperature (25 degree), the gas-dynamic to 5ppm～1ppm responds such as Fig. 6, shown in 7,
Wherein single tungsten oxide nano under 100 degree to 5ppm, the sensitivity (sensitivity of 4ppm, 3ppm, 2ppm, 1ppmNO2 gas
Gas sensitive device resistance value in resistance value/air under=detected gas) respectively: 4.2,2.8,2.1,1.6,1.3.Prepare
Tungsten oxide/vanadium oxide heterojunction nano-wire array (the plating vanadium 5min) gas sensitive device at room temperature (25 degree) of one-dimentional structure
Under the gas sensitivity of 5ppm～1ppm reacted be respectively as follows: 23,20,17,9.5,6.5.Its response time is about 5s
Left and right, contrasts other gas sensitive device speed higher.Appearance structure is one-dimensional nano line array, has the highest specific surface area,
Can give full play to the superiority of hetero-junctions, the direct special band structure of hetero-junctions can effectively reduce gas sensor
Operating temperature, the sensitivity improving sensor and response speed.Processing technology is ripe, easy to use, cheap, has
Hope the application that puts it in gas sensor field.By to different types of gas detecting, obtain result shown in Fig. 7,
This gas sensitive device of surface can have good selectivity to nitrogen oxygen class oxidizing gas.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of prepared tungsten oxide nano, and section and plane photograph, scale is 500nm；
Scanning electron microscope is Hitachi scanning electron microscope Hitachi-S4800FESEM；
Fig. 2 is prepared tungsten oxide/vanadium oxide heterojunction nano-wire array scanning electron micrograph, section and plane
According to, the sputtering time of vanadium is 5min, and scale is 500nm；
Fig. 3 is prepared tungsten oxide/vanadium oxide heterojunction nano-wire array transmission electron micrograph and elementary analysis line
Scanning, absolutely proves that its structure is nucleocapsid structure always.Kernel is tungsten oxide nano, and shell is vanadium oxide.Scale is
20nm；Transmission electron microscope is NEC JEM-2100F Flied emission transmission electron microscope；
Fig. 4 is the structural representation of tungsten oxide in embodiment/vanadium oxide heterojunction nano-wire array structure gas sensor；
Fig. 5 is that gas responds detection platform structural representation；
Fig. 6 is that single tungsten oxide nano gas sensor is at room temperature to 5ppm-1ppm NO2The dynamic continuous response of gas is bent
Line；
Fig. 7 is that this practicality tungsten oxide/vanadium oxide nucleocapsid heterogeneous structural nano linear array structure gas sensor is the most right
The dynamic continuous response curve of 5ppm-1ppm NO2 gas；
Fig. 8 is this practicality tungsten oxide/vanadium oxide nucleocapsid heterogeneous structural nano linear array structure gas sensor at room temperature different gas
The selectivity of body.
Detailed description of the invention
The present invention is raw materials used all uses commercially available chemically pure reagent, makees the present invention the most in detail below in conjunction with specific embodiment
Thin explanation.
Single-sided polishing silicon chip: buy in Hedong District, Tianjin Jing Yifang electronic product business department, model: p-type, resistivity:
10-15Ω·cm.Crystal orientation:<100>± 0.5 °.Thickness: 400 μm.Alumina ceramic plate: buy in north, Guangzhou
Dragon Electronics Co., Ltd., thickness: 0.6mm, specification: 20*25mm.Superhigh vacuum magnetron sputtering manufacturer: Shenyang science instrument
Device development center company limited, model: DPS type III ultrahigh vacuum facing-target magnetron sputtering system coater；Vacuum high-temperature tubular type
Stove: GSL-1400X mono-warm area horizontal vacuum tube furnace that Hefei Ke Jing Materials Technology Ltd. produces.
First single-sided polishing silicon chip and alumina ceramic plate are carried out: by single-sided polishing silicon chip or alumina ceramic plate
Ultrasonic cleaning 10min in hydrogen peroxide and the concentrated sulphuric acid of volume ratio 4:1, be then successively placed in acetone solvent, dehydrated alcohol,
The ultrasonic 5-10min that is respectively washed in deionized water, removes surface and oil contaminant and organic impurities, is placed in infrared baking oven thoroughly
Dry.
Embodiment 1
Step 1, utilizes facing-target magnetron sputtering system deposits tungsten film material plies on substrate single-sided polishing silicon chip, using tungsten as
Target, with argon as sputter gas, sputtering operating air pressure is 2.0Pa, and sputtering power is 80W, and sputtering time is 20min；
Step 2, the W film prepared step 1 at vacuum high-temperature tube furnace equipment carries out crystalline growth tungsten oxide nano,
Ambiance is the mixed gas of oxygen and argon, in tungsten oxide nano growth course, controls oxygen and argon flow amount
Being respectively 0.1sccm and 35sccm, in control stove, growth pressure is 140Pa, and tube furnace is raised to from room temperature 25 degrees Celsius
700 DEG C, 5 DEG C/min of heating rate, it is incubated 1 hour at 700 DEG C, then cooling 1 hour to 400 DEG C, the coldest
But room temperature 25 degrees Celsius is arrived；
Step 3, the annealing of tungsten oxide nano, tungsten oxide nano step 2 prepared is at 500 DEG C and air gas
Anneal 1 hour under atmosphere environment, to stablize crystal orientation further；
Step 4, utilizes and deposits vanadium on the tungsten oxide nano layer of the substrate that facing-target magnetron sputtering system processes through step 3 preparation
Film, using vanadium metal as target, using argon as sputter gas, inert gas flow is 50sccm, sputters operating air pressure
For 2.0Pa, sputtering power is 110W, and sputtering time is 5min；
Step 5, carries out the annealing heat treatment of vanadium, will process the substrate of the deposition vanadium metal film obtained through step 4 at 500 DEG C
And anneal 1 hour under air atmosphere environment；
Step 6, the making of electrode: the tungsten oxide/vanadium oxide heterojunction nano-wire array platinum plating that will prepare in step 5
Electrode, forming two spacing on tungsten oxide/vanadium oxide heterojunction nano-wire array by template is 0.5cm, and size is
The electrode of 1mm*1mm, using argon as working gas, background vacuum 3 × 10-4Pa, uses radio-frequency magnetron sputter method system
Standby, sputter 5min, film thickness 60nm.
Embodiment 2
Step 1, utilizes facing-target magnetron sputtering system deposits tungsten film material plies on substrate single-sided polishing silicon chip, using tungsten as
Target, with argon as sputter gas, sputtering operating air pressure is 1.0Pa, and sputtering power is 80W, and sputtering time is 20min；
Step 2, the W film prepared step 1 at vacuum high-temperature tube furnace equipment carries out crystalline growth tungsten oxide nano,
Ambiance is the mixed gas of oxygen and argon, in tungsten oxide nano growth course, controls oxygen and argon flow amount
Being respectively 0.1sccm and 50sccm, in control stove, growth pressure is 150Pa, and tube furnace is raised to from room temperature 25 degrees Celsius
600 DEG C, 5 DEG C/min of heating rate, it is incubated 1.5 hours at 600 DEG C, then cooling 1 hour to 350 DEG C, finally natural
It is cooled to room temperature 25 degrees Celsius；
Step 3, the annealing of tungsten oxide nano, tungsten oxide nano step 2 prepared is at 400 DEG C and air gas
Anneal 2 hours under atmosphere environment, to stablize crystal orientation further；
Step 4, utilizes and deposits vanadium on the tungsten oxide nano layer of the substrate that facing-target magnetron sputtering system processes through step 3 preparation
Film, using vanadium metal as target, using argon as sputter gas, inert gas flow is 40sccm, sputters operating air pressure
For 2.0Pa, sputtering power is 80W, and sputtering time is 2min；
Step 5, carries out the annealing heat treatment of vanadium, will process the substrate of the deposition vanadium metal film obtained through step 4 at 300 DEG C
And anneal 2 hours under air atmosphere environment；
Step 6, the making of electrode: the tungsten oxide/vanadium oxide heterojunction nano-wire array platinum plating that will prepare in step 5
Electrode, forming two spacing on tungsten oxide/vanadium oxide heterojunction nano-wire array by template is 2.5cm, and size is
The electrode of 3mm*3mm, using argon as working gas, background vacuum 9 × 10-4Pa, uses radio-frequency magnetron sputter method system
Standby, sputter 1min, film thickness 150nm.
Embodiment 3
Step 1, utilizes facing-target magnetron sputtering system deposits tungsten film material plies on substrate alumina potsherd, using tungsten as
Target, with argon as sputter gas, sputtering operating air pressure is 2.0Pa, and sputtering power is 80W, and sputtering time is 20min；
Step 2, the W film prepared step 1 at vacuum high-temperature tube furnace equipment carries out crystalline growth tungsten oxide nano,
Ambiance is the mixed gas of oxygen and argon, in tungsten oxide nano growth course, controls oxygen and argon flow amount
Being respectively 0.1sccm and 40sccm, in control stove, growth pressure is 160Pa, and tube furnace is raised to from room temperature 20 degrees Celsius
650 DEG C, 5 DEG C/min of heating rate, it is incubated 2 hours at 650 DEG C, then cooling 1 hour to 300 DEG C, the coldest
But room temperature 20 degrees Celsius is arrived；
Step 3, the annealing of tungsten oxide nano, tungsten oxide nano step 2 prepared is at 300 DEG C and air gas
Anneal 1.5 hours under atmosphere environment, to stablize crystal orientation further；
Step 4, utilizes and deposits vanadium on the tungsten oxide nano layer of the substrate that facing-target magnetron sputtering system processes through step 3 preparation
Film, using vanadium metal as target, using argon as sputter gas, inert gas flow is 30sccm, sputters operating air pressure
For 2Pa, sputtering power is 100W, and sputtering time is 3min；
Step 5, carries out the annealing heat treatment of vanadium, will process the substrate of the deposition vanadium metal film obtained through step 4 at 400 DEG C
And anneal 1.5 hours under air atmosphere environment；
Step 6, the making of electrode: the tungsten oxide/vanadium oxide heterojunction nano-wire array platinum plating that will prepare in step 5
Electrode, forming two spacing on tungsten oxide/vanadium oxide heterojunction nano-wire array by template is 2cm, and size is
The electrode of 2mm*2mm, using argon as working gas, background vacuum 4 × 10-4Pa, uses radio-frequency magnetron sputter method system
Standby, sputter 2min, film thickness 80nm.
Embodiment 4
Step 1, utilizes facing-target magnetron sputtering system deposits tungsten film material plies on substrate single-sided polishing silicon chip, using tungsten as
Target, with argon as sputter gas, sputtering operating air pressure is 2.0Pa, and sputtering power is 80W, and sputtering time is 20min；
Step 2, the W film prepared step 1 at vacuum high-temperature tube furnace equipment carries out crystalline growth tungsten oxide nano,
Ambiance is the mixed gas of oxygen and argon, in tungsten oxide nano growth course, controls oxygen and argon flow amount
Being respectively 0.1sccm and 35sccm, in control stove, growth pressure is 140Pa, and tube furnace is raised to from room temperature 25 degrees Celsius
700 DEG C, 5 DEG C/min of heating rate, it is incubated 1 hour at 700 DEG C, then cooling 1 hour to 400 DEG C, the coldest
But room temperature 25 degrees Celsius is arrived；
Step 3, the annealing of tungsten oxide nano, tungsten oxide nano step 2 prepared is at 500 DEG C and air gas
Anneal 1 hour under atmosphere environment, to stablize crystal orientation further；
Step 4, utilizes and deposits vanadium on the tungsten oxide nano layer of the substrate that facing-target magnetron sputtering system processes through step 3 preparation
Film, using vanadium metal as target, using argon as sputter gas, inert gas flow is 50sccm, sputters operating air pressure
For 2.0Pa, sputtering power is 110W, and sputtering time is 5min；
Step 5, carries out the annealing heat treatment of vanadium, will process the substrate of the deposition vanadium metal film obtained through step 4 at 500 DEG C
And anneal 1 hour under air atmosphere environment；
Step 6, the making of electrode: the tungsten oxide/vanadium oxide heterojunction nano-wire array platinum plating that will prepare in step 5
Electrode, forming two spacing on tungsten oxide/vanadium oxide heterojunction nano-wire array by template is 1cm, and size is
The electrode of 2mm*2mm, using argon as working gas, background vacuum 6 × 10-4Pa, uses radio-frequency magnetron sputter method system
Standby, sputter 6min, film thickness 120nm.
Embodiment 5
Step 1, utilizes facing-target magnetron sputtering system deposits tungsten film material plies on substrate alumina potsherd, using tungsten as
Target, with argon as sputter gas, sputtering operating air pressure is 2.0Pa, and sputtering power is 80W, and sputtering time is 20min；
Step 2, the W film prepared step 1 at vacuum high-temperature tube furnace equipment carries out crystalline growth tungsten oxide nano,
Ambiance is the mixed gas of oxygen and argon, in tungsten oxide nano growth course, controls oxygen and argon flow amount
Being respectively 0.1sccm and 40sccm, in control stove, growth pressure is 160Pa, and tube furnace is raised to from room temperature 20 degrees Celsius
650 DEG C, 5 DEG C/min of heating rate, it is incubated 2 hours at 650 DEG C, then cooling 1 hour to 300 DEG C, the coldest
But room temperature 20 degrees Celsius is arrived；
Step 3, the annealing of tungsten oxide nano, tungsten oxide nano step 2 prepared is at 300 DEG C and air gas
Anneal 1.5 hours under atmosphere environment, to stablize crystal orientation further；
Step 4, utilizes and deposits vanadium on the tungsten oxide nano layer of the substrate that facing-target magnetron sputtering system processes through step 3 preparation
Film, using vanadium metal as target, using argon as sputter gas, inert gas flow is 30sccm, sputters operating air pressure
For 2Pa, sputtering power is 100W, and sputtering time is 3min；
Step 5, carries out the annealing heat treatment of vanadium, will process the substrate of the deposition vanadium metal film obtained through step 4 at 400 DEG C
And anneal 1.5 hours under air atmosphere environment；
Step 6, the making of electrode: the tungsten oxide/vanadium oxide heterojunction nano-wire array platinum plating that will prepare in step 5
Electrode, forming two spacing on tungsten oxide/vanadium oxide heterojunction nano-wire array by template is 1.5cm, and size is
The electrode of 2mm*2mm, using argon as working gas, background vacuum 5 × 10-4Pa, uses radio-frequency magnetron sputter method system
Standby, sputter 2min, film thickness 100nm.
Above the present invention is done exemplary description, it should explanation, in the case of without departing from the core of the present invention,
Any simple deformation, amendment or other those skilled in the art can not spend the equivalent of creative work all to fall
Enter protection scope of the present invention.
Claims (2)
1. tungsten oxide vanadium oxide heterojunction nano-wire array application in detection nitrogen dioxide, it is characterised in that tungsten oxide
Vanadium oxide heterojunction nano-wire array is made up of tungsten oxide/vanadium oxide heterojunction nano-wire, tungsten oxide vanadium oxide hetero-junctions nanometer
Line length is 300 800nm, and a diameter of 10-20nm of described tungsten oxide nano, outside described tungsten oxide nano
Enclosing and wrap up vanadium oxide equably, it is different that the thickness of described vanadium oxide is that 20-30nm, tungsten oxide and vanadium oxide define coaxial nucleocapsid
Matter structure, tungsten oxide vanadium oxide heterojunction nano-wire array detects answering on nitrogen dioxide gas under the conditions of room temperature 25-30 DEG C
With.
2. the tungsten oxide vanadium oxide heterojunction nano-wire array as claimed in claim 1 application in detection nitrogen dioxide,
It is characterized in that: the minimal detectable concentration of described nitrogen dioxide gas is 5ppm.
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