CN103852496B - Based on certainly to the preparation method of the gas sensor element of tungsten oxide nano - Google Patents
Based on certainly to the preparation method of the gas sensor element of tungsten oxide nano Download PDFInfo
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- CN103852496B CN103852496B CN201410082909.6A CN201410082909A CN103852496B CN 103852496 B CN103852496 B CN 103852496B CN 201410082909 A CN201410082909 A CN 201410082909A CN 103852496 B CN103852496 B CN 103852496B
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Abstract
The invention discloses a kind of based on certainly to the preparation method of the gas sensor element of tungsten oxide nano, by plating interdigital electrode, plated metal W film layer successively in sensor base, so tube type vacuum stove recrystallization be aided with after annealing process obtain have good pattern certainly to tungsten oxide nano.Nano wire is from the upwards recrystallization growth of the tungsten thin layer of electrode surface, and self assembly defines intersected with each other certainly to the responsive rete of tungsten oxide nano.Based on the inventive method certainly to tungsten oxide nano sensor element to NO
2there is high sensitivity, good selectivity and stability.Good air-sensitive performance, owing to certainly to the special construction characteristic of the responsive rete of nano wire gas sensor, shows it at monitoring toxicity NO simultaneously
2the huge applications potentiality in field.
Description
Technical field
The invention relates to gas sensor, particularly relate to a kind of based on certainly to the preparation method of the gas sensor element of tungsten oxide nano.
Background technology
Development of modern industry creates a large amount of inflammable, explosive, poisonous harmful gases, wherein oxides of nitrogen (NO
x) be a kind ofly cause the serious environmental problems such as acid rain, photo-chemical smog and human health brought to the Typical Air Pollution thing of grave danger.Research is used for NO
xthe high-performance gas sensor material of accurate examination and controlling and device to protection of the environment and human health significant.And along with the enhancing of environmental consciousness, the performance of people to oxides of nitrogen gas sensors is had higher requirement.The sensitive material that researchist is also passing through to research and develop new structure and composition always constantly improves the sensitive property of gas sensor.
Large quantity research finds, one dimension tungsten oxide nano is to NO
xgas has very high sensitivity and selectivity, is the NO that there is research and apply prospect a kind of pole
xsensitive material, its gas sensing mechanism belongs to surface resistance control type, is at semiconductor grain adsorption and the modulated process that reacts tungsten oxide semiconductor surface resistance based on oxygen and tested gas to the detection of gas.Due to accurate one dimension tungsten oxide nano-material, to have high specific surface area and its vertical axial size and Debye length comparable thus can obtain higher gas sensitivity, better selectivity and lower working temperature, shows the bright outlook that tungsten oxide nano gas sensitive is applied in high-performance oxides of nitrogen gas sensors.
Up to now, pre-synthesis nano wire is mainly carried out secondary assembling by the manufacture craft based on the sensor element of the oxide nano threads such as one dimension tungsten oxide on device substrate surface, namely utilize the aft-loaded airfoil methods such as silk-screen, spin coating, electrophoresis, AFM to form thick film or the single structure of nano wire on sensor base surface.From the angle of application, single nano-wire air-sensitive performance is poor, mission life is short and the realization of electricity contact is too dependent on the high precision process technologies such as beamwriter lithography expensive consuming time, cause that device fabrication efficiency is low, cost is high, be difficult to walk out use for laboratory in batch production; And when forming thick film sensitive layer by secondary assembling, nano wire thick film is randomly dispersed on two electrodes, complicated rear operation is difficult to reach nano wire and assembles in the high precision of substrate surface, and be difficult to the excellent sensitivity characteristic playing one-dimensional nano line completely, there is not the mechanism that be combined with each other reliably in the nano wire particularly in thick film and the contact between electrode, thus greatly affect sensitivity and the response characteristic of sensor, and cause device stability, reliability to reduce, the device performance problem such as large affected by environment.Say in a sense, the technical limitation existing for the packaging technology of existing nano wire hinders one of major reason of nano wire base microsensor practicalization just.
Summary of the invention
Object of the present invention, be the number of disadvantages overcoming existing secondary assembling nanometer line gas sensor, solve the problem of nano wire in sensor substrate surface-assembled in microsensor manufacture, provide a kind of tungsten metallic film recrystallization that adopts to be aided with after annealing self assembly preparation certainly to the method for tungsten oxide nano base gas sensor element.
The present invention is achieved by following technical solution, and step is as follows:
(1) substrate is cleaned
By aluminium oxide ceramics substrate ultrasonic cleaning 20 minutes in absolute ethyl alcohol, take out substrate, with deionized water rinsing, then continue ultrasonic cleaning 5 ~ 10 minutes in a solution of hydrofluoric acid, with thorough clean surface impurity; Then, continue ultrasonic cleaning 20 minutes with deionized water, substrate is dry, for subsequent use under air atmosphere.
(2) interdigital electrode is sputtered
Alumina sensor substrate after step (1) ultrasonic cleaning also thoroughly being dried is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, using high pure metal platinum as target, using argon gas as working gas, sputtering operating pressure is 2.0Pa, sputtering power 80 ~ 90W, sputtering time 8 ~ 10min, substrate temperature is room temperature, and forming a layer thickness at aluminium oxide ceramics substrate surface is the interdigital platinum electrode of 100-300nm;
(3) plated metal W film:
Ultrahigh vacuum facing-target magnetron sputtering system equipment is utilized to have the aluminium oxide ceramics substrate surface plated metal W film of interdigital Pt electrode at plating.Using tungsten as target, argon gas is as sputter gas, and sputter operating air pressure 2.0Pa, sputtering power is 80-90W, argon flow amount 30-40sccm, and sputtering time is 10-20min, and the tungsten film thickness of sputtering sedimentation is 50-80nm;
(4) film recrystallization growth is certainly to nano wire
Heat-treat tungsten film in vacuum high-temperature tubular furnace equipment, recrystallization realizes certainly to the growth of nano wire; The aluminium oxide ceramics substrate depositing W film is placed on the high-temperature region of tubular furnace, adopts ladder-elevating temperature, controlling heating curve is: room temperature to 500 DEG C, heating rate 5 DEG C/min; By 500 DEG C to 600 ~ 650 DEG C, heating rate 10 DEG C/min; 600 ~ 650 DEG C of insulations 1 ~ 1.5 hour, insulation terminated, and naturally cools to room temperature; The nano wire film goods obtained are mazarine or black;
Nanowire growth atmosphere is oxygen argon gas mixed gas, and controlling argon flow amount by mass flowmeter is 30 ~ 35sccm, and oxygen flow amount is 0.1 ~ 0.2sccm, and in stove, growth pressure is 140 ~ 150Pa;
(5) after annealing process
For stablizing crystalline phase further, improve the air-sensitive performance of element, after annealing process is carried out to the product film of step (4); Annealing temperature is 400 ~ 500 DEG C, and programming rate is at 5 ~ 10 DEG C/min, and temperature retention time 2 ~ 3 hours, annealing atmosphere is air.
The quality purity of the target metal platinum of described step (2) is 99.999%.
The quality purity of the target tungsten of described step (2) is 99.999%.
The quality purity of the sputter gas argon gas of described step (2), step (3) is 99.999%.
The blending ratio of the argon gas oxygen mixed gas of described step (4) is controlled by mass flowmeter, and ratio is 150:1 ~ 350:1.
The invention provides a kind of novel structure, have fast-response can based on the gas sensor element certainly to tungsten oxide nano.By the tungsten thin layer upwards accurate oriented growth of the standby nano wire of tungsten metallic film recrystallization legal system from electrode surface, self assembly intersected with each other defines the responsive rete of tungsten oxide nano of highly porous.Between nano wire and substrate, the existence of binding layer enhances the electrical stability of sensor element, and the accurate directive texture of nano wire gas sensitive is beneficial to the diffusion of gas in layer, ensure that the fast response characteristic of sensor element.
Accompanying drawing explanation
Fig. 1 is that embodiment 1 sensor base surface is certainly schemed to the inclination SEM of tungsten oxide nano amplification 20,000 times;
Fig. 2 is that embodiment 1 sensor base surface is certainly schemed to the inclination SEM of tungsten oxide nano amplification 50,000 times;
Fig. 3 is that embodiment 4 sensor base surface is certainly to the SEM sectional drawing of tungsten oxide nano.
Fig. 4 is at 150 DEG C, based on certainly to the gas sensor element of tungsten oxide nano to 0.25-9ppmNO
2dynamic response curve.
Fig. 5 is at 150 DEG C, based on certainly to the sensitivity-NO of the gas sensor element of tungsten oxide nano
2concentration curve.
Embodiment
The present invention is raw materials used all adopts commercially available chemically pure reagent, is described in more detail the present invention below in conjunction with specific embodiment.
Embodiment 1
(1) substrate is cleaned
First sensor base material carries out thorough ultrasonic cleaning before use, removes surface impurity.By aluminium oxide ceramics substrate ultrasonic cleaning 20 minutes in absolute ethyl alcohol; Take out substrate, with deionized water rinsing, afterwards, continue ultrasonic cleaning 5 minutes in a solution of hydrofluoric acid, with thorough clean surface impurity; Then, ultrasonic cleaning 20 minutes is continued with deionized water; Finally, substrate is dry, for subsequent use under air atmosphere.
(2) interdigital electrode is sputtered
Alumina sensor ceramic bases after step (1) ultrasonic cleaning also thoroughly being dried is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, be that the high pure metal platinum of 99.999% is as target using quality purity, be that the argon gas of 99.999% is as working gas using quality purity, sputtering operating pressure is 2.0Pa, sputtering power 80W, sputtering time 8min, aluminium oxide ceramics substrate temperature is room temperature, and forming a layer thickness at alumina surface is the interdigital platinum electrode of 100nm.
(3) plated metal W film:
Ultrahigh vacuum facing-target magnetron sputtering system equipment is utilized to have the aluminium oxide ceramics substrate surface plated metal W film of interdigital Pt electrode at plating.Using the tungsten of quality purity 99.999% as target, quality purity be the argon gas of 99.999% as sputter gas, sputtering operating air pressure 2.0Pa, sputtering power is 80W, argon flow amount 30sccm, sputtering time is 10min, and the tungsten film thickness of sputtering sedimentation is 50nm.
(4) film recrystallization growth is certainly to nano wire
Heat-treat tungsten film in vacuum high-temperature tubular furnace equipment, recrystallization realizes certainly to the growth of nano wire.The substrate depositing W film is placed on the high-temperature region of tubular furnace, adopts ladder-elevating temperature, controlling heating curve is: room temperature ~ 500 DEG C, heating rate 5 DEG C/min; By 500 DEG C to 600 DEG C, heating rate 10 DEG C/min; 600 DEG C of insulations 1 hour, insulation terminated, and naturally cools to room temperature.The nano wire film goods obtained are mazarine or black.
Nanowire growth atmosphere is oxygen argon gas mixed gas, and controlling argon flow amount by mass flowmeter is 35sccm, and oxygen flow amount is 0.1sccm, and in stove, growth pressure is 150Pa.
(5) after annealing process
The goods taken out from step (4) tubular furnace, in order to stablize crystalline phase further, improving the air-sensitive performance of element, carrying out after annealing process to product film.Annealing conditions is: annealing temperature 400 DEG C, and programming rate is at 5 DEG C/min, and temperature retention time 2 hours, annealing atmosphere is air.Obtain the product morphology change after annealing little, namely 400 DEG C of air atmosphere annealing do not have an impact to product.
The product obtained under above process conditions is analyzed, the upgrowth situation that nanowire is good can be seen by accompanying drawing 1 and accompanying drawing 2, can see the separatrix of silicon chip surface nano wire and silicon chip edge nano wire, silicon chip edge nanowire density is than large at same crystallization condition lower silicon slice nano surface line density.At Fig. 4, Fig. 5 are respectively 150 DEG C, based on certainly to the gas sensor element of tungsten oxide nano to 0.25-9ppmNO
2dynamic response curve and sensitivity-NO
2concentration curve.As can be seen from the figure, the NO of this sensor element to low concentration 150 DEG C time
2gas shows extraordinary response characteristic.At 150 DEG C, this sensor element is to 0.25-9ppmNO
2the sensitivity of gas can reach 2.2-30.2, and this sensor element has good reversibility and demonstrates NO fast
2gas response characteristic, its response time lower than 10s, this show adopt the inventive method prepare can be used for low concentration of NO based on the gas sensor element certainly to tungsten oxide nano
2the high sensitivity detection of gas.
Embodiment 2
The present embodiment step (1) ~ (4) are identical with embodiment 1, and the annealing temperature only changed in step (5) is 450 DEG C, and other condition remains unchanged.Obtain the product nano line after annealing thinning thin, some nano wire bends, and nanowire diameter becomes large, and irregular nano particle appears in substrate surface.Namely nano wire is in annealing process, and substrate has minority nano wire there occurs fusion and become irregular nano particle, nano wire becomes sparse, and the nano wire do not merged, in air anneal process, there occurs bending.
Embodiment 3
The present embodiment step (1) ~ (4) are identical with embodiment 1, and the annealing temperature only changed in step (5) is 500 DEG C, and other condition remains unchanged.Obtain the product nano line after annealing thinning thin, directly discontinuous each other.Namely annealing temperature is 500 DEG C time, and temperature is high, in annealing process, there occurs fusion, become membrane structure, only have minority nano wire not merge at a distance of near nano wire.
Embodiment 4
The present embodiment step (1) ~ (4) are identical with embodiment 1, and the programming rate only changed in the annealing conditions in step (5) is 10 DEG C/min, and other condition remains unchanged.The product obtaining the product after annealing and embodiment 1 changes not quite.Accompanying drawing 3 be obtain under the process conditions of this embodiment certainly to grow nanowire, as can be seen from the figure nano wire is along the accurate oriented growth in same direction, and nanowire diameter is at about 10nm, and length is at about 2 μm.
Embodiment 5
The present embodiment step (1) ~ (4) are identical with embodiment 1, and the temperature retention time only changed in the annealing conditions in step (5) is 3 hours, and other condition remains unchanged.The product obtaining the product after annealing and embodiment 1 changes not quite.
Embodiment 6
The ratio of the argon gas oxygen that the present embodiment changes in embodiment 1 step (4) is 30sccm/0.2sccm, keep other step and condition constant.The film obtaining alumina surface is made up of large particle, cannot form nano thread structure.Namely oxygen flow becomes large, in the tungsten oxide generated under steady state (SS), oxygen element is large containing quantitative change, tungsten oxide molecular chemistry bond structure changes, crystal growth is the process of chemical bond Cheng Jian, this change makes compound have the characteristic of different growth rate not show along different crystalline lattice direction, nano thread structure is can not get in product, but membrane structure.
Embodiment 7
The ratio of the argon gas oxygen that the present embodiment changes in embodiment 1 step (4) is 35sccm/0.2sccm, keep other step and condition constant.The result obtained is similar to Example 6, cannot obtain nano thread structure.
Embodiment 8
It is 140Pa that the present embodiment to change in embodiment 1 step (4) growth pressure in stove, keep other step and condition constant.The product of the product obtained and embodiment 1 changes not quite.
Embodiment 9
The time that the present embodiment changes ultrasonic cleaning in embodiment 1 step (1) is 10 minutes, keep other step and condition constant.Obtain result product similar to embodiment 1.
Embodiment 10
The sputtering power that the present embodiment changes in embodiment 1 step (2) is 90W, keep other step and condition constant.Obtain result product similar to embodiment 1.
Embodiment 11
The sputtering time that the present embodiment changes in embodiment 1 step (2) is 10min, keep other step and condition constant.Obtain result product similar to embodiment 1.
Technological condition and the effect of embodiment 1 ~ 8 refer to table 1.
Table 1
Claims (4)
1., based on certainly to a preparation method for the gas sensor element of tungsten oxide nano, there are following steps:
(1) substrate is cleaned
By aluminium oxide ceramics substrate ultrasonic cleaning 20 minutes in absolute ethyl alcohol, take out substrate, with deionized water rinsing, then continue ultrasonic cleaning 5 ~ 10 minutes in a solution of hydrofluoric acid, with thorough clean surface impurity; Then, continue ultrasonic cleaning 20 minutes with deionized water, substrate is dry, for subsequent use under air atmosphere;
(2) interdigital electrode is sputtered
Aluminium oxide ceramics substrate after step (1) ultrasonic cleaning also thoroughly being dried is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, using high pure metal platinum as target, using argon gas as working gas, sputtering operating pressure is 2.0Pa, sputtering power 80 ~ 90W, sputtering time 8 ~ 10min, substrate temperature is room temperature, and forming a layer thickness at aluminium oxide ceramics substrate surface is the interdigital platinum electrode of 100-300nm;
(3) plated metal W film:
Ultrahigh vacuum facing-target magnetron sputtering system equipment is utilized to have the aluminium oxide ceramics substrate surface plated metal W film of interdigital Pt electrode at plating; Using tungsten as target, argon gas is as sputter gas, and sputter operating air pressure 2.0Pa, sputtering power is 80-90W, argon flow amount 30-40sccm, and sputtering time is 10-20min, and the tungsten film thickness of sputtering sedimentation is 50-80nm;
(4) film recrystallization growth is certainly to nano wire
Heat-treat tungsten film in vacuum high-temperature tubular furnace equipment, recrystallization realizes certainly to the growth of nano wire; The aluminium oxide ceramics substrate depositing W film is placed on the high-temperature region of tubular furnace, adopts ladder-elevating temperature, controlling heating curve is: room temperature to 500 DEG C, heating rate 5 DEG C/min; By 500 DEG C to 600 ~ 650 DEG C, heating rate 10 DEG C/min; 600 ~ 650 DEG C of insulations 1 ~ 1.5 hour, insulation terminated, and naturally cools to room temperature; The nano wire film goods obtained are mazarine or black;
Nanowire growth atmosphere is oxygen argon gas mixed gas, and controlling argon flow amount by mass flowmeter is 30 ~ 35sccm, and oxygen flow amount is 0.1sccm, and in stove, growth pressure is 140 ~ 150Pa;
(5) after annealing process
For stablizing crystalline phase further, improve the air-sensitive performance of element, after annealing process is carried out to the product film of step (4); Annealing temperature is 400 DEG C, and programming rate is at 5 ~ 10 DEG C/min, and temperature retention time 2 ~ 3 hours, annealing atmosphere is air.
2. according to claim 1ly it is characterized in that based on certainly to the preparation method of the gas sensor element of tungsten oxide nano, the quality purity of the target metal platinum of described step (2) is 99.999%.
3. according to claim 1ly it is characterized in that based on certainly to the preparation method of the gas sensor element of tungsten oxide nano, the quality purity of the target tungsten of described step (2) is 99.999%.
4. according to claim 1ly it is characterized in that based on certainly to the preparation method of the gas sensor element of tungsten oxide nano, the quality purity of the sputter gas argon gas of described step (2), step (3) is 99.999%.
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| GB2527340A (en) * | 2014-06-19 | 2015-12-23 | Applied Nanodetectors Ltd | Gas sensors and gas sensor arrays |
| CN104445047B (en) * | 2014-11-05 | 2016-08-17 | 天津大学 | A kind of tungsten oxide/vanadium oxide heterojunction nano-wire array and preparation method thereof |
| CN104698038A (en) * | 2015-01-21 | 2015-06-10 | 济南大学 | Indium oxide nanosheet gas sensor and preparation method thereof |
| CN106153689A (en) * | 2015-04-23 | 2016-11-23 | 天津大学 | The application in detection nitrogen dioxide of the tungsten oxide vanadium oxide heterojunction 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 |
| CN105606659A (en) * | 2015-08-28 | 2016-05-25 | 天津大学 | Preparation method of tungsten oxide nano-rod structure gas sensitive sensor for low temperature work |
| CN105301063A (en) * | 2015-10-29 | 2016-02-03 | 天津大学 | Preparation method for tungsten-oxide-nanosheet-structured gas sensor working at room temperature |
| CN105486723A (en) * | 2015-11-19 | 2016-04-13 | 天津大学 | Preparation method for room temperature NO2 sensor with ceramic-based vanadium oxide nanorod structure |
| CN105628749A (en) * | 2016-01-05 | 2016-06-01 | 天津大学 | Preparing method of high sensitivity nitrogen dioxide gas sensitive material working at low temperature |
| CN105486721A (en) * | 2016-01-05 | 2016-04-13 | 天津大学 | Method for preparing nitrogen oxide sensor element based on tungsten oxide nanometer blocks |
| CN106124575B (en) * | 2016-08-08 | 2019-12-24 | 苏州科技大学 | NO (nitric oxide)2Sensor and preparation method thereof |
| CN107907573A (en) * | 2017-10-27 | 2018-04-13 | 天津大学 | A kind of preparation method of p-type respond style tungsten oxide nano gas sensor |
| CN107907572A (en) * | 2017-10-27 | 2018-04-13 | 天津大学 | A kind of respond style control method of tungsten oxide nano gas sensor |
| CN107978520B (en) * | 2017-11-23 | 2020-01-31 | 长江存储科技有限责任公司 | Metal growth process |
| CN110057869A (en) * | 2018-01-18 | 2019-07-26 | 中国科学院过程工程研究所 | A kind of semiconductor gas sensor and preparation method thereof |
| CN108490038A (en) * | 2018-02-23 | 2018-09-04 | 天津大学 | The preparation method of tungsten oxide nano/porous silicon composite structure gas sensor |
| CN110672671B (en) * | 2019-10-18 | 2022-04-01 | 上海理工大学 | Acetone sensitive material and sensitive element and preparation method thereof |
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| CN101973510B (en) * | 2010-10-24 | 2012-03-07 | 天津大学 | Method for preparing gas-sensitive sensor element based on carbon nano tube microarray/tungsten oxide nano composite structure |
| CN102012386A (en) * | 2010-10-24 | 2011-04-13 | 天津大学 | Preparation method of nitric oxide gas sensor element based on pseudodirected tungsten trioxide nano tape |
| CN103267784A (en) * | 2013-05-11 | 2013-08-28 | 天津大学 | Preparation method of gas sensitive sensor with porous silicon and tungsten oxide nano-rod composite structure |
| CN103512924A (en) * | 2013-10-21 | 2014-01-15 | 天津大学 | Preparation method of gas sensitive element for detecting nitric oxide at low temperature |
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