CN104445047B - A kind of tungsten oxide/vanadium oxide heterojunction nano-wire array and preparation method thereof - Google Patents
A kind of tungsten oxide/vanadium oxide heterojunction nano-wire array and preparation method thereof Download PDFInfo
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- CN104445047B CN104445047B CN201410619764.9A CN201410619764A CN104445047B CN 104445047 B CN104445047 B CN 104445047B CN 201410619764 A CN201410619764 A CN 201410619764A CN 104445047 B CN104445047 B CN 104445047B
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Abstract
Open a kind of tungsten oxide/vanadium oxide heterojunction nano-wire array of the present invention and preparation method thereof, it is 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, vanadium oxide is wrapped up equably in the periphery of described tungsten oxide nano, the thickness of described vanadium oxide is 20 30nm, tungsten oxide and vanadium oxide define coaxial nucleocapsid heterojunction structure, use the method for facing-target magnetron sputtering system and growth in situ to carry out depositing, growing and heat treatment in substrate.The inventive method prepares the good tungsten oxide of pattern/vanadium oxide heterojunction nano-wire array structure materials, significantly improves the specific surface area of material, effectively make use of hetero-junctions in the superiority of aspect of performance.
Description
Technical field
The invention belongs to functional material preparation field, more particularly, relate to a kind of tungsten oxide/vanadium oxide hetero-junctions nanometer
Linear array and preparation method thereof.
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、SO2Etc.).NOx class
Toxic gas, it is possible to form acid rain corrosion building and skin, also can produce chemical fumes, sucks and causes cough, more very
Person causes respiratory tract disease.Therefore efficient and accurately detection and prevention toxic and harmful sensor is made very urgent.
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、TiO2Deng, but they all cannot be used for efficient detection NOx class gas.Along with research deeply, Akiyama in 1991
M etc. report WO3Pottery is the high sensitive material of detection NOx in the environment of 300 degree.Since then, numerous section is caused
The worker that grinds is to WO3Research.WO3It is a kind of metal-oxide semiconductor (MOS), is that a kind of surface conductance (resistance) controls
Type gas sensitive.WO3The atomic property of plane of crystal is enlivened, easy adsorption gas molecule, and when gas molecule absorption exists
During plane of crystal, can make its internal carrier concentration that corresponding change occurs, show as the resistance variations of sensor.In view of
The atom that enlivens of tungsten oxide is positioned at plane of crystal and expands the contact area of plane of crystal and gas the most greatly, it is possible to effectively
Improvement air-sensitive performance.The tungsten oxide of 1-dimention nano line structure has attracted numerous researcher because of its huge specific surface area
Research.Can pass through hydro-thermal method, vapor phase method, sol-gel etc. through research in recent years to prepare.Experimental result
Proving, the tungsten oxide of 1-dimention nano line structure improves the sensitivity of detected gas really, but this still can not reach market
Change the requirement with integra-tion application.In order to obtain high selectivity, high sensitivity, low operating temperature, the air-sensitive of high stability
Sensor, currently mainly improves air-sensitive performance by gas sensitive modification.
Gas sensitive modification aspect, main path has doped precious metal Pt, Au, Pd or transition metal oxide, additionally may be used
Modified by structure heterojunction structure.Heterojunction structure is currently mainly applied to semiconductor laser, luminescent device, sun electricity
The scientific domains such as pond.Hetero-junctions being applied to air-sensitive field and forms heterojunction material is to improve air-sensitive performance another is great latent
The direction of power.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of tungsten oxide/vanadium oxide heterojunction nano-wire array
And preparation method thereof, prepare the good tungsten oxide of pattern/vanadium oxide heterojunction nano-wire array structure material by gas phase process
Material, the specific surface area that one-dimensional nano line array is huge is improving the sensitive of gas sensor with the heterojunction structure performance of its excellence
In degree and response speed, there is critically important researching value.
The technical purpose of the present invention is achieved by following technical proposals:
A kind of tungsten oxide/vanadium oxide heterojunction nano-wire array and preparation method thereof, is prepared 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, 700 DEG C of guarantors
Temperature 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.
In technique scheme, in step 1, the quality purity of target tungsten is 99.999%.
In technique scheme, in step 4, the quality purity of target vanadium metal is 99.999%.
In technique scheme, the quality purity of the noble gas of use is 99.999%.
In technique scheme, described substrate is single-sided polishing silicon chip, or alumina ceramic plate.
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 array
It is 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.
The invention discloses the preparation method of a kind of tungsten oxide/vanadium oxide heterojunction nano-wire array, it is provided that prepared by one
WO3The method of heterojunction nano-wire structure, significantly improves the specific surface area of material, effectively make use of hetero-junctions to exist
The superiority of aspect of performance.Simultaneous oxidation tungsten/vanadium oxide heterojunction nano-wire structure is also in the low-power consumption, ultrafast of Sensitive Apparatus
Response speed aspect has critically important researching value.
Compared with prior art, the invention provides a kind of method with low cost uses vapor phase method to prepare one-dimentional structure
Tungsten oxide/vanadium oxide heterojunction nano-wire, has equipment simple compared with the method such as existing thermal evaporation, electro-deposition, operation
Convenient, the advantages such as technological parameter is easily controllable, with low cost.Further, appearance structure is one-dimensional nano line array, has
The highest specific surface area, it is possible to give full play to the superiority of hetero-junctions, to by this materials application in reduce gas sensor
Operating temperature, the sensitivity and the response speed aspect that improve sensor have the biggest research space.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the tungsten oxide nano prepared by embodiment 1.
Fig. 2 is the tungsten oxide prepared by embodiment 1/vanadium oxide heterojunction nano-wire array scanning electron micrograph.
Fig. 3 is the electron scanning micrograph of the tungsten oxide nano prepared by embodiment 2.
Fig. 4 is the tungsten oxide prepared by embodiment 2/vanadium oxide heterojunction nano-wire array scanning electron micrograph.
Fig. 5 is the tungsten oxide prepared by embodiment 3/vanadium oxide heterojunction nano-wire array scanning electron micrograph.
Fig. 6 is the transmission electron microscope photo of tungsten oxide/vanadium oxide heterojunction nano-wire prepared by the embodiment of the present invention.
Detailed description of the invention
The present invention is raw materials used all uses commercially available chemically pure reagent, makees the present invention further details of below in conjunction with specific embodiment
Explanation.Single-sided polishing silicon chip: buy in Hedong District, Tianjin Jing Yifang electronic product business department, model: p-type, resistance
Rate: 10-15 Ω 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 tube furnace:
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.
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.
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.
In the inventive solutions, tungsten oxide and vanadium oxide all have good air-sensitive performance, are excellent air-sensitives half
Conductor material.Tungsten oxide/the vanadium oxide nanowires utilizing above-mentioned preparation carries out gas experiment, test result indicate that said method
System the at room temperature NO to 5ppm rank of tungsten oxide/vanadium oxide heterojunction structure2The response sensitivity that gas has is
7-9 times of simple tungsten oxide nanometer line sensitivity, response time is less than 3s.
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 (7)
1. the preparation method of tungsten oxide/vanadium oxide heterojunction nano-wire array, it is characterised in that enter as steps described below
Row preparation:
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；
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；
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；
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.
The preparation method of a kind of tungsten oxide the most according to claim 1/vanadium oxide heterojunction nano-wire array, its feature
Being, described substrate is single-sided polishing silicon chip, or alumina ceramic plate.
The preparation method of a kind of tungsten oxide the most according to claim 1/vanadium oxide heterojunction nano-wire array, its feature
Being, in step 1, noble gas is argon, helium or nitrogen, and sputtering operating air pressure is 2.0Pa, sputtering power
For 90-100W, sputtering time is 15-20min, and the quality purity of target tungsten is 99.999%.
The preparation method of a kind of tungsten oxide the most according to claim 1/vanadium oxide heterojunction nano-wire array, its feature
It is, in step 2, in growth course, controls oxygen and argon flow amount is respectively 0.1sccm and 35sccm, control
In stove processed, growth 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,
Being incubated 1 hour at 700 DEG C, then cooling 1 hour to 400 DEG C, finally naturally cools to room temperature 20 25 degrees Celsius.
The preparation method of a kind of tungsten oxide the most according to claim 1/vanadium oxide heterojunction nano-wire array, its feature
Being, in step 4, noble gas is argon, helium or nitrogen, and sputtering operating air pressure is 2.0Pa, sputtering power
For 90-100W, sputtering time is 2 5min, and the quality purity of target vanadium metal is 99.999%.
The preparation method of a kind of tungsten oxide the most according to claim 1/vanadium oxide heterojunction nano-wire array, its feature
It is, in steps of 5, anneals 1 1.5 hours under 300-400 DEG C and air atmosphere environment.
The preparation method of a kind of tungsten oxide the most according to claim 1/vanadium oxide heterojunction nano-wire array, its feature
Being, the quality purity of the noble gas of use is 99.999%.
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| CN201510776094.6A CN105319242A (en) | 2014-11-05 | 2014-11-05 | Application of tungsten oxide-vanadium oxide heterojunction nanowire array as gas sensitive material |
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| CN104835719B (en) * | 2015-04-01 | 2018-03-16 | 浙江大学 | A kind of porous SiO2The preparation method of nano-wire array |
| CN106145030A (en) * | 2015-04-23 | 2016-11-23 | 天津大学 | A kind of hud typed tungsten oxide cupric oxide heterojunction nano-wire array of vertical orientation and preparation method thereof |
| CN105242334B (en) * | 2015-10-27 | 2018-06-05 | 中国科学院宁波材料技术与工程研究所 | A kind of multi-layer cermet film of wide range ultra-fast nonlinear optical response performance and preparation method thereof |
| CN106770476A (en) * | 2015-11-23 | 2017-05-31 | 天津大学 | Heterogeneous clad structure base gas sensor and its application in nitrogen dioxide is detected in order of cupric oxide/tungsten oxide one-dimensional |
| CN106744667A (en) * | 2015-11-23 | 2017-05-31 | 天津大学 | The tungsten oxide of vertical orientation/cupric oxide heterojunction nano-wire array gas sensor and its application in ethanol is detected |
| CN107402241A (en) * | 2016-05-18 | 2017-11-28 | 天津大学 | Gas sensor based on tungsten oxide/titanium oxide core-shell nano line and preparation method thereof |
| CN107402240A (en) * | 2016-05-18 | 2017-11-28 | 天津大学 | One-dimensional application of the tungsten oxide/titanium oxide core-shell nano line in nitrogen dioxide is detected in order |
| CN108572196A (en) * | 2017-03-08 | 2018-09-25 | 天津大学 | Gas sensor and its preparation method and application based on silicon-tungsten oxide nano heterojunction structure |
| CN109298026A (en) * | 2017-07-24 | 2019-02-01 | 天津大学 | Silicon nanowires-tungsten oxide nano brush multilevel structure and preparation method thereof and the application in detection nitrogen dioxide |
| CN109298027A (en) * | 2017-07-25 | 2019-02-01 | 天津大学 | Gas sensor and preparation method thereof based on the nano-particle modified tungsten oxide nanometer stick of tellurium oxide |
| CN109021962B (en) * | 2018-08-30 | 2021-05-07 | 合肥工业大学 | Crystalline tungsten trioxide/titanium doped amorphous tungsten oxide nanowire array and preparation method thereof |
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| CN100427939C (en) * | 2006-12-21 | 2008-10-22 | 天津大学 | Tungstic acid thin film air-sensitive sensor surface modifying method |
| CN101393939B (en) * | 2007-09-20 | 2010-06-02 | 中国科学院合肥物质科学研究院 | Nano tube hetero-junction constituted by zinc oxide and carbon, preparation thereof |
| KR101282155B1 (en) * | 2008-03-20 | 2013-07-04 | 더 유니버시티 오브 아크론 | Ceramic nanofibers conㄱtaining nanosize metal catalyst particles and medium thereof |
| TW201018742A (en) * | 2008-11-05 | 2010-05-16 | Univ Nat Taipei Technology | Nanomaterial with core-shell structure |
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| CN103469272B (en) * | 2013-09-04 | 2015-11-25 | 浙江大学 | Tungsten trioxide/polyanilinecore-shell core-shell nanowire array radiochromic film and preparation method thereof |
| CN103630572A (en) * | 2013-10-21 | 2014-03-12 | 天津大学 | Preparation method of porous silicon/tungsten oxide nanowire composite structure for gas-sensitive material |
| CN103852496B (en) * | 2014-03-07 | 2016-02-17 | 天津大学 | Based on certainly to the preparation method of the gas sensor element of tungsten oxide nano |
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