CN103852496A - Preparation method of gas sensor element based on quasi-directed tungsten oxide nanowires - Google Patents
Preparation method of gas sensor element based on quasi-directed tungsten oxide nanowires Download PDFInfo
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Abstract
The invention discloses a preparation method of a gas sensor based on quasi-directed tungsten oxide nanowires. An interdigital electrode and a deposited metal tungsten thin layer are plated on the substrate of the sensor in sequence, and futher the quasi-directed tungsten oxide nanowire with good appearance is obtained through annealing treatment in an assisted manner after recrystallization in a tubular vacuum oven. The nanowires are self-assembled to form a sensitive film layer with crossed quasi-directed tungsten oxide nanowires through upward recrystallization growth on the metal tungsten thin layer on the surface of the electrode. The sensor for the quasi-directed tungsten oxide nanowires based on the method disclosed by the invention has higher sensitivity for NO2 and good selectivity and stability. Good gas-sensitive property attributes to the special structural property of the sensitive film layer of the gas sensor element of the quasi-directed tungsten oxide nanowires, and great application potential is shown in the field of monitoring of poisonous NO2.
Description
Technical field
The invention relates to gas sensor, relate in particular to a kind of based on the preparation method to the gas sensor element of tungsten oxide nano certainly.
Background technology
Development of modern industry has produced a large amount of inflammable, explosive, poisonous harmful gases, wherein oxides of nitrogen (NO
x) be a kind of Typical Air Pollution thing that causes the serious environmental problems such as acid rain, photo-chemical smog and human health is brought to grave danger.Research is for NO
xhigh-performance gas sensor material and the device of accurate examination and controlling significant to protection of the environment and human health.And along with the enhancing of environmental consciousness, people have higher requirement to the performance of oxides of nitrogen gas sensors.Researchist is also always in the sensitive property of constantly improving gas sensor by the sensitive material of research and development new structure and composition.
Large quantity research discovery, one dimension tungsten oxide nano is to NO
xgas has very high sensitivity and selectivity, is the NO that a kind of utmost point has research and application prospect
xsensitive material, its gas sensing mechanism belongs to surface resistance control type, is at semiconductor grain adsorption with react the modulated process to tungsten oxide semiconductor surface resistance based on oxygen and tested gas to the detection of gas.Thereby due to accurate one dimension tungsten oxide nano-material have high specific surface area with and vertical axial size and Debye length is comparable can obtain higher gas sensitivity, better selectivity and lower working temperature, shown the bright outlook that tungsten oxide nano gas sensitive is applied in high-performance oxides of nitrogen gas sensors.
Up to now, the manufacture craft of the sensor element based on oxide nano threads such as one dimension tungsten oxides is mainly pre-synthesis nano wire to be carried out to secondary assembling on device substrate surface, namely utilizes the rear job operations 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 in the situation that 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 the high precision assembling of nano wire at substrate surface, and the very difficult excellent sensitivity characteristic of bringing into play one-dimensional nano line completely, there is not the mechanism that mutually combines reliably in contacting between the nano wire in thick film and electrode particularly, thereby 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 existing technical limitation of 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 to overcome the serial shortcoming of existing secondary assembling nanometer line gas sensor, solve microsensor manufacture in the problem of nano wire in sensor substrate surface-assembled, 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) clean substrate
By aluminium oxide ceramics substrate ultrasonic cleaning 20 minutes in absolute ethyl alcohol, take out substrate, with deionized water rinsing, then in hydrofluoric acid solution, continue ultrasonic cleaning 5～10 minutes, with thorough clean surface impurity; Then, with deionized water continuation ultrasonic cleaning 20 minutes, substrate is dry, for subsequent use under air atmosphere.
(2) sputter interdigital electrode
Aluminium oxide sensor base by step (1) ultrasonic cleaning and after thoroughly drying 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, sputter operating pressure is 2.0Pa, sputtering power 80～90W, sputtering time 8～10min, substrate temperature is room temperature, forming a layer thickness at aluminium oxide ceramics substrate surface is the interdigital platinum electrode of 100-300nm;
(3) plated metal W film:
Utilize ultrahigh vacuum facing-target magnetron sputtering system equipment 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, sputter operating air pressure 2.0Pa, and sputtering power is 80-90W, argon flow amount 30-40sccm, sputtering time is 10-20min, the tungsten film thickness of sputtering sedimentation is 50-80nm;
(4) film recrystallization is grown certainly to nano wire
In vacuum high-temperature tubular furnace equipment, tungsten film is heat-treated, recrystallization realizes the certainly growth to nano wire; The aluminium oxide ceramics substrate that deposits W film is placed on to the high-temperature region of tubular furnace, adopts ladder-elevating temperature, control heating curve is: room temperature to 500 DEG C, 5 DEG C/min of heating rate; By 500 DEG C to 600～650 DEG C, 10 DEG C/min of heating rate; 600～650 DEG C of insulations 1～1.5 hour, insulation finished, and naturally cools to room temperature; The nano wire film goods that obtain are mazarine or black;
Nanowire growth atmosphere is oxygen argon gas mixed gas, is 30～35sccm by mass flowmeter control argon flow amount, and oxygen flow amount is 0.1～0.2sccm, and in stove, growth pressure is 140～150Pa;
(5) after annealing processing
For further stablizing crystalline phase, improve the air-sensitive performance of element, the product film of step (4) is carried out to after annealing processing; Annealing temperature is 400～500 DEG C, and programming rate is at 5～10 DEG C/min, temperature retention time 2～3 hours, and 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 by mass flowmeter control, 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 to tungsten oxide nano certainly.Upwards accurate oriented growth of tungsten thin layer by the standby nano wire of tungsten metallic film recrystallization legal system from electrode surface, self assembly intersected with each other has formed the responsive rete of tungsten oxide nano of highly porous.Between nano wire and substrate, the existence of binding layer has strengthened 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, has ensured the fast response characteristic of sensor element.
Brief description of the drawings
Fig. 1 is that certainly scheme at the inclination SEM that amplifies 20,000 times to tungsten oxide nano on embodiment 1 sensor base surface;
Fig. 2 is that certainly scheme at the inclination SEM that amplifies 50,000 times to tungsten oxide nano on embodiment 1 sensor base surface;
Fig. 3 is that embodiment 4 sensor base surfaces are 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 0.25-9ppm NO
2dynamic response curve.
Fig. 5 is at 150 DEG C, based on the sensitivity-NO to the gas sensor element of tungsten oxide nano certainly
2concentration curve.
Embodiment
The present invention is raw materials used all adopts commercially available chemically pure reagent, below in conjunction with specific embodiment, the present invention is described in more detail.
Embodiment 1
(1) clean substrate
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, in hydrofluoric acid solution, continue ultrasonic cleaning 5 minutes, with thorough clean surface impurity; Then, continue ultrasonic cleaning 20 minutes with deionized water; Finally, substrate is dry, for subsequent use under air atmosphere.
(2) sputter interdigital electrode
Aluminium oxide sensor ceramic bases by step (1) ultrasonic cleaning and after thoroughly drying is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, high pure metal platinum using quality purity as 99.999% is as target, argon gas using quality purity as 99.999% is as working gas, sputter operating pressure is 2.0Pa, sputtering power 80W, sputtering time 8min, aluminium oxide ceramics substrate temperature is room temperature, forming a layer thickness at alumina surface is the interdigital platinum electrode of 100nm.
(3) plated metal W film:
Utilize ultrahigh vacuum facing-target magnetron sputtering system equipment 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, the argon gas that quality purity is 99.999% is as sputter gas, sputter operating air pressure 2.0Pa, sputtering power is 80W, argon flow amount 30sccm, sputtering time is 10min, the tungsten film thickness of sputtering sedimentation is 50nm.
(4) film recrystallization is grown certainly to nano wire
In vacuum high-temperature tubular furnace equipment, tungsten film is heat-treated, recrystallization realizes the certainly growth to nano wire.The substrate that deposits W film is placed on to the high-temperature region of tubular furnace, adopts ladder-elevating temperature, control heating curve is: room temperature～500 DEG C, 5 DEG C/min of heating rate; By 500 DEG C to 600 DEG C, 10 DEG C/min of heating rate; 600 DEG C of insulations 1 hour, insulation finished, and naturally cools to room temperature.The nano wire film goods that obtain are mazarine or black.
Nanowire growth atmosphere is oxygen argon gas mixed gas, is 35sccm by mass flowmeter control argon flow amount, and oxygen flow amount is 0.1sccm, and in stove, growth pressure is 150Pa.
(5) after annealing processing
The goods that take out from step (4) tubular furnace, in order further to stablize crystalline phase, improve the air-sensitive performance of element, and product film is carried out to after annealing processing.Annealing conditions is: 400 DEG C of annealing temperatures, and programming rate is at 5 DEG C/min, temperature retention time 2 hours, annealing atmosphere is air.The product pattern obtaining after annealing changes not quite, i.e. 400 DEG C of air atmospheres annealing do not exert an influence to product.
The product obtaining under above process conditions is analyzed, can find out by accompanying drawing 1 and accompanying drawing 2 upgrowth situation that nano wire is good, 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.Fig. 4, Fig. 5 are respectively at 150 DEG C, based on certainly to the gas sensor element of tungsten oxide nano to 0.25-9ppm NO
2dynamic response curve and sensitivity-NO
2concentration curve.As can be seen from the figure, this sensor element NO to low concentration in the time of 150 DEG C
2gas has demonstrated extraordinary response characteristic.At 150 DEG C, this sensor element is to 0.25-9ppm NO
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 is lower than 10s, and this shows to adopt, and prepared by the inventive method can be used for low concentration of NO based on the gas sensor element to tungsten oxide nano certainly
2the high sensitivity detection of gas.
Embodiment 2
The present embodiment step (1)～(4) are identical with embodiment 1, and the annealing temperature only changing in step (5) is 450 DEG C, and other condition remains unchanged.Obtain thinning the dredging of product nano wire after annealing, some nano wire bends, and it is large that nanowire diameter becomes, and irregular nano particle appears in substrate surface.Be nano wire in annealing process, in substrate, have minority nano wire occurred merge become irregular nano particle, it is sparse that nano wire becomes, do not merge nano wire in air annealing process, there is bending.
Embodiment 3
The present embodiment step (1)～(4) are identical with embodiment 1, and the annealing temperature only changing in step (5) is 500 DEG C, and other condition remains unchanged.Obtain thinning the dredging of product nano wire after annealing, directly discontinuous each other.Be annealing temperature in the time of 500 DEG C, temperature is high, in annealing process, fusion has occurred at a distance of near nano wire, has become membrane structure, only has minority nano wire not merge.
The present embodiment step (1)～(4) are identical with embodiment 1, and the programming rate only changing in the annealing conditions in step (5) is 10 DEG C/min, and other condition remains unchanged.The product that obtains product and embodiment 1 after annealing changes not quite.Accompanying drawing 3 under the process conditions of this embodiment, obtain certainly to grow nanowire, as can be seen from the figure nano wire is along the accurate oriented growth of same direction, nanowire diameter is in 10nm left and right, length is in 2 μ m left and right.
Embodiment 5
The present embodiment step (1)～(4) are identical with embodiment 1, and the temperature retention time only changing in the annealing conditions in step (5) is 3 hours, and other condition remains unchanged.The product that obtains product and embodiment 1 after annealing changes not quite.
The ratio that the present embodiment changes the argon gas oxygen in embodiment 1 step (4) is 30sccm/0.2sccm, keeps other step and condition constant.The film that obtains alumina surface is made up of large particle, cannot form nano thread structure.Be that Oxygen Flow quantitative change is large, in the tungsten oxide generating 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 variation makes compound have the characteristic of different growth rates not show along different crystalline lattice direction, in product, can not get nano thread structure, but membrane structure.
Embodiment 7
The ratio that the present embodiment changes the argon gas oxygen in embodiment 1 step (4) is 35sccm/0.2sccm, keeps other step and condition constant.The result obtaining is similar to Example 6, cannot obtain nano thread structure.
It is 140Pa that the present embodiment changes the interior growth pressure of stove in embodiment 1 step (4), keeps other step and condition constant.The product of the product obtaining and embodiment 1 changes little.
Embodiment 9
The time that the present embodiment changes ultrasonic cleaning in embodiment 1 step (1) is 10 minutes, keeps 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, keeps 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, keeps 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 (5)
1. based on the preparation method to the gas sensor element of tungsten oxide nano certainly, there are following steps:
(1) clean substrate
By aluminium oxide ceramics substrate ultrasonic cleaning 20 minutes in absolute ethyl alcohol, take out substrate, with deionized water rinsing, then in hydrofluoric acid solution, continue ultrasonic cleaning 5～10 minutes, with thorough clean surface impurity; Then, with deionized water continuation ultrasonic cleaning 20 minutes, substrate is dry, for subsequent use under air atmosphere.
(2) sputter interdigital electrode
Aluminium oxide sensor base by step (1) ultrasonic cleaning and after thoroughly drying 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, sputter operating pressure is 2.0Pa, sputtering power 80～90W, sputtering time 8～10min, substrate temperature is room temperature, forming a layer thickness at aluminium oxide ceramics substrate surface is the interdigital platinum electrode of 100-300nm;
(3) plated metal W film:
Utilize ultrahigh vacuum facing-target magnetron sputtering system equipment 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, sputter operating air pressure 2.0Pa, and sputtering power is 80-90W, argon flow amount 30-40sccm, sputtering time is 10-20min, the tungsten film thickness of sputtering sedimentation is 50-80nm;
(4) film recrystallization is grown certainly to nano wire
In vacuum high-temperature tubular furnace equipment, tungsten film is heat-treated, recrystallization realizes the certainly growth to nano wire; The aluminium oxide ceramics substrate that deposits W film is placed on to the high-temperature region of tubular furnace, adopts ladder-elevating temperature, control heating curve is: room temperature to 500 DEG C, 5 DEG C/min of heating rate; By 500 DEG C to 600～650 DEG C, 10 DEG C/min of heating rate; 600～650 DEG C of insulations 1～1.5 hour, insulation finished, and naturally cools to room temperature; The nano wire film goods that obtain are mazarine or black;
Nanowire growth atmosphere is oxygen argon gas mixed gas, is 30～35sccm by mass flowmeter control argon flow amount, and oxygen flow amount is 0.1～0.2sccm, and in stove, growth pressure is 140～150Pa;
(5) after annealing processing
For further stablizing crystalline phase, improve the air-sensitive performance of element, the product film of step (4) is carried out to after annealing processing; Annealing temperature is 400～500 DEG C, and programming rate is at 5～10 DEG C/min, temperature retention time 2～3 hours, and annealing atmosphere is air.
2. according to claim 1ly it is characterized in that based on the preparation method to the gas sensor element of tungsten oxide nano certainly, 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 the preparation method to the gas sensor element of tungsten oxide nano certainly, 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 the preparation method to the gas sensor element of tungsten oxide nano certainly, the quality purity of the sputter gas argon gas of described step (2), step (3) is 99.999%.
5. according to claim 1 based on the preparation method to the gas sensor element of tungsten oxide nano certainly, it is characterized in that, the blending ratio of the argon gas oxygen mixed gas of described step (4) is by mass flowmeter control, and ratio is 150:1～350:1.
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