CN103267779A - Preparation method for ethanol gas sensor based on vanadium pentoxide multilevel nanometer network structure - Google Patents
Preparation method for ethanol gas sensor based on vanadium pentoxide multilevel nanometer network structure Download PDFInfo
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Abstract
The present invention discloses a preparation method for an ethanol gas sensor based on a vanadium pentoxide multilevel nanometer network structure, wherein a seed layer induction growth approach is adopted to achieve direct in-situ assembly of a multilevel vanadium oxide nanometer network structure on the surface of a sensor substrate to form a high performance vanadium oxide base ethanol gas sensor element with a double work temperature characteristic so as to avoid a secondary transfer process of a gas sensitive material, the multilevel nanometer structure formed on the substrate in the in-situ manner presents a continuous, porous and loose-like micro-structure characteristic and has a significantly high specific surface area, and reliable electric contact is formed between a gas sensitive film and an electrode. The sensor element prepared by the preparation method provides double work temperature and dual response characteristics at a room temperature and a temperature of 250 DEG C for ethanol gas, and has advantages of simple equipment, easy operation, easy process parameter control, low cost and the like.
Description
Technical field
The invention relates to gas sensor, relate in particular to the preparation method that a kind of duplex based on vanadium pentoxide multi-stage nano network structure is made temperature alcohol gas sensor element.
Background technology
The development of modern society; security issues become increasingly urgent; therefore it is more and more higher reliability gas to be detected requirement; at the alcohol gas sensor that biology, chemical industry, medical science and food service industry all need to have features such as high sensitivity, stability, selectivity and portability, this is all significant to environmental protection and health.At present, many metal oxide semiconductors comprise SnO
2, ZnO, TiO
2And Fe
2O
3Deng the detection that is widely used in alcohol gas, its sensitive mechanism belongs to the surface resistance control type, and the detection of alcohol gas is based on airborne oxygen and detected alcohol gas at the absorption of metal oxide semiconductor surface and the reaction resistance modulated process to semiconductor material.But higher, the gas-sensitive property problems such as sensitivity is lower, gas-selectively difference of this class alcohol gas sensor ubiquity working temperature have increased many complicacy and instability to the microminiaturization of gas sensing technology, integrated, low-power consumption development.
Has more high performance alcohol gas sensor in order to research and develop, researchist one is straight through the structure of studying new material and form the sensitive property of constantly improving gas sensor, for example surface modification, formation composite oxides synthesize the nano material of high activity surface etc.Particularly in recent years people to the broad research of metal-oxide semiconductor (MOS) vanadium pentoxide, find that it has good sensitivity characteristic to ethanol, especially based on monodimension nano stick, nanotube, nano wire and the multi-stage oxidizing vanadium nanostructured that forms with the self-organization of two-dimensional nano sheet, present porous, loose shape microstructure features, thereby has a higher specific surface area, thereby the low-dimensional size of its constituent element structure and Debye length is comparable can obtain higher sensitivity simultaneously, better choice and lower working temperature are for its application at the high-performance alcohol gas sensor provides more wide stage.Yet, discover that based on previous researcher its optimum working temperature is higher, usually about 200 ℃, be unfavorable for the research of low energy-consumption electronic device, and most gas sensors adopt secondary transferring technology, be the synthetic of gas sensitive, disperse, and transfer to the gas sensor substrate, form gas sensor by thermal treatment at last, such secondary transferring technology is difficult to make the sensitive property of nanostructured gas sensitive to be not fully exerted, and the reliability that electricity contacts between the air-sensitive film that is formed by secondary transferring and the electrode is difficult to guarantee, thereby influence stability and the reliability of gas sensor, in addition, Fu Za technological process also is unfavorable for miniaturization of devices, integrated.
Summary of the invention
Purpose of the present invention, it is higher to be to overcome present vanadium oxide base alcohol gas sensor working temperature, the secondary transferring preparation technology of sensor is to the adverse effect of device air-sensitive performance, a kind of direct in-situ assembling with Seed Layer induced growth approach realization sensor base surface multi-stage oxidizing vanadium nanometer network structure is provided, and formation has the preparation method that duplex is made the high-performance vanadium oxide base alcohol gas sensor element of temperature characterisitic.
The present invention is achieved by following technical solution.
A kind of preparation method based on vanadium pentoxide multi-stage nano network structure alcohol gas sensor element has following steps:
(1) preparation of the interdigital platinum electrode of sensor
The aluminium oxide sensor base is successively cleaned also thoroughly oven dry in acetone solvent, absolute ethyl alcohol, deionized water for ultrasonic to be placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, with high pure metal platinum as target, be that 99.999% argon gas is as working gas with quality purity, the sputter operating pressure is 2.0Pa, sputtering power 80～90W, sputtering time 8～10min, substrate temperature are room temperature, form interdigital platinum electrode at alumina surface;
(2) preparation of seed solution
Ammonium metavanadate is dissolved in the 20ml deionized water, and magnetic agitation becomes light yellowly up to solution, add an amount of rare nitric acid, makes the pH control of solution about 2.1～2.5, and forming concentration is the seed solution of 0.05M～0.2M transparent salmon;
(3) preparation of Seed Layer
The ammonium metavanadate seed solution of preparation in the step (2) is coated to step (1) to be covered on the alumina substrate that interdigital electrode is arranged, place annealing furnace air atmosphere annealing in process then, 500～650 ℃ of annealing temperatures, temperature retention time 1～2h is about 2～3 ℃/min of heating rate;
(4) preparation of hydro-thermal reaction solution
The ammonium metavanadate solution of preparation 0.04M～0.08M is dissolved in ammonium metavanadate in the deionized water magnetic agitation, become light yellow up to solution, add an amount of rare nitric acid, make the pH control of solution about 2.1～2.5, form the ammonium metavanadate solution of transparent salmon;
(5) preparation of vanadium pentoxide multi-stage nano network structure
To place liner be the stainless steel hydrothermal reaction kettle of teflon with covering the alumina substrate that the ammonium metavanadate Seed Layer is arranged in the step (3), also transfer to the ammonium metavanadate solution of step (4) preparation in the reactor simultaneously, sealing, under 180～200 ℃ of temperature, adopt the synthetic vanadium pentoxide mesh nanometer structure of hydro-thermal method in alumina substrate then, the hydro-thermal reaction time is 9～15 hours, and reactor naturally cools to room temperature;
(6) alumina substrate after the rinse water thermal response
With the alumina substrate after the hydro-thermal reaction in the step (5), clean through deionized water and soaked in absolute ethyl alcohol repeatedly, dry in 60～80 ℃ vacuum drying chamber, make the gas sensor element based on vanadium pentoxide nanometer network structure.
The quality purity of the high pure metal platinum target of described step (1) is 99.95% metal platinum.
The platinum electrode thickness of the employing radio-frequency magnetron sputter method preparation of described step (1) is 80～120nm.
The seed solution of described step (3) adopts spin-coating method, dipping, spraying or drips and method such as is coated with and is coated on the alumina substrate that is covered with interdigital electrode.
After the Seed Layer annealing of described step (3), can form equally distributed diameter at alumina substrate is 100nm～1 μ m, and length is the little crystal grain of 1～5 μ m.
The invention has the beneficial effects as follows:
(1) provides a kind of direct in-situ assembling that realizes sensor base surface multi-stage oxidizing vanadium nanometer network structure with Seed Layer induced growth approach, formation has the preparation method that duplex is made the high-performance vanadium oxide base alcohol gas sensor element of temperature characterisitic, has avoided the secondary transferring technological process of gas sensitive; The multi-level nano-structure that original position forms on substrate presents continuously, porous, loose shape microstructure features, has obvious high specific surface area; Having formed reliable electricity between air-sensitive film and the electrode contacts.
(2) have duplex based on the ethanol gas dependent sensor of multi-stage oxidizing vanadium nanometer network structure and make temperature characterisitic, sensor shows the double-response characteristic room temperature and 250 ℃ to alcohol gas, particularly when room temperature (20 ℃), alcohol gas has been represented gas-sensitive properties such as good response-recovery characteristic, gas-selectively, high sensitivity.This summary of the invention has vital role to high-performance low-power-consumption ethanol development of Gas-sensitive Sensor, can further improve range of application and the application of ethanol gas dependent sensor.
Advantages such as it is simple, easy to operate (3) to have equipment, and technological parameter is easy to control, and is with low cost.
Description of drawings
Fig. 1 is the electron scanning micrograph of the prepared Seed Layer of embodiment 1;
Fig. 2 is the electron scanning micrograph of the prepared vanadium oxide multi-stage nano network structure of embodiment 1;
Fig. 3 is the electron scanning micrograph of the prepared vanadium oxide multi-stage nano network structure of embodiment 2;
Fig. 4 is the electron scanning micrograph of the prepared vanadium oxide multi-stage nano network structure of embodiment 3;
Fig. 5 is the sensitivity to the 250ppm alcohol gas under the different operating temperature of the prepared vanadium oxide multi-stage nano network structure sensor element of embodiment 2;
Fig. 6 is the prepared vanadium oxide multi-stage nano network structure sensor element of embodiment 2 dynamic response curve to alcohol gas under room temperature (20 ℃);
Fig. 7 is the prepared vanadium oxide multi-stage nano network structure sensor element of embodiment 2 dynamic response curve to alcohol gas under 250 ℃;
Fig. 8 is the prepared vanadium oxide multi-stage nano network structure sensor element of embodiment 2 under room temperature and 250 ℃ to gas with various selectivity synoptic diagram;
Embodiment
The present invention is raw materials used all to adopt commercially available chemically pure reagent, and the present invention is further detailed explanation below in conjunction with specific embodiment.
Embodiment 1
(1) preparation of the interdigital platinum electrode of aluminium oxide
The aluminium oxide sensor base is successively cleaned also thoroughly oven dry in acetone solvent, absolute ethyl alcohol, deionized water for ultrasonic to be placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, with high pure metal platinum as target, be that 99.999% argon gas is as working gas with quality purity, the sputter operating pressure is 2.0Pa, sputtering power 80～90W, sputtering time 8～10min, substrate temperature are room temperature, form interdigital platinum electrode at alumina surface;
(2) preparation of seed solution
An amount of ammonium metavanadate is dissolved in the deionized water, and magnetic agitation becomes light yellowly up to solution, add an amount of rare nitric acid, makes the pH control of solution about 2.1～2.5, and forming concentration is the seed solution of 0.05M～0.2M transparent salmon;
(3) preparation of Seed Layer
The ammonium metavanadate seed solution of preparation in the step (2) is coated to step (1) to be covered on the alumina substrate that interdigital electrode is arranged, place annealing furnace to anneal then, atmosphere is air, 500～650 ℃ of annealing temperatures, temperature retention time 1～2h is about 2.5 ℃/min of heating rate;
(4) preparation of hydro-thermal reaction solution
The ammonium metavanadate solution of preparation 0.04M is dissolved in an amount of ammonium metavanadate in the 80mml deionized water magnetic agitation, become light yellow up to solution, add an amount of rare nitric acid, make the pH control of solution about 2.1～2.5, form the ammonium metavanadate solution of transparent salmon;
(5) preparation of vanadium pentoxide multi-stage nano network structure
Be the stainless steel hydrothermal reaction kettle of teflon with covering the liner that the alumina substrate that the ammonium metavanadate Seed Layer is arranged places 100ml in the step (3), also transfer to the ammonium metavanadate solution of step (4) preparation in the reactor simultaneously, sealing, under 180 ℃ of temperature, adopt the synthetic vanadium pentoxide mesh nanometer structure of hydro-thermal method in alumina substrate then, the hydro-thermal reaction time is 12 hours, and reactor naturally cools to room temperature;
(6) alumina substrate after the rinse water thermal response
With the alumina substrate after the hydro-thermal reaction in the step (5), clean through deionized water and soaked in absolute ethyl alcohol repeatedly, dry in 60～80 ℃ vacuum drying chamber, make the gas sensor element based on vanadium pentoxide nanometer network structure.The electron microscopic analysis result of the surface topography in embodiment 1 step (3) after the annealing of ammonium metavanadate Seed Layer as shown in Figure 1, can form equally distributed diameter at alumina substrate is 100nm～1 μ m, length is the little crystal grain of 1～5 μ m, for next step provides the growth in situ point in alumina substrate preparation vanadium oxide multi-stage nano network structure, it is the indispensable experimental section of the present invention.
The electron microscopic analysis result of the surface topography of the vanadium oxide multi-stage nano network structure of embodiment 1 preparation form the evenly vanadium oxide reticulated film of the loose shape of distribution at alumina substrate, and these mesh is to be made of nano wire, nanometer band as shown in Figure 2.
Embodiment 2
The difference of present embodiment and embodiment 1 is: the ammonium metavanadate concentration in the step (5) in the hydro-thermal reaction solution becomes 0.06M, makes vanadium oxide multi-stage nano network gas sensitive.The scanning electron microscope analysis result of surface topography as shown in Figure 3, nanometer is colored dispersedly in a large number in existence, present cell texture, and superimposed nano wire is closely connected with the nanometer band and is in the same place, and the radial structure that the nanometer flower is made up of nanoneedle, nano wire, have bigger specific surface area, can make alcohol gas freely " turnover ", thereby make it have higher sensitivity, dynamic response faster.Fig. 5-8 is its dual working temperature to alcohol gas of reaction further, and response/recovery characteristics and selectivity characteristic faster.
Embodiment 3
The difference of present embodiment and embodiment 1 is: the concentration of the ammonium metavanadate in the step (5) in the hydro-thermal reaction solution becomes 0.08M, makes vanadium oxide multi-stage nano network gas sensitive.The scanning electron microscope analysis result of surface topography exists spherical cellular nanometer to spend closely and contacts as shown in Figure 4, and mean diameter is about 3-5 μ m, also presents cell texture simultaneously.
The present invention adopts static distribution method to measure vanadium pentoxide multi-stage nano network structure sensor element to the sensitivity characteristic of alcohol gas in room temperature to 300 ℃ temperature range, sensitivity S=the Rg/Ra of definition gas sensor, wherein Rg, Ra are respectively the resistance value of element in detecting gas and dry air.
Claims (5)
1. preparation method based on vanadium pentoxide multi-stage nano network structure alcohol gas sensor element has following steps:
(1) preparation of the interdigital platinum electrode of sensor
The aluminium oxide sensor base is successively cleaned also thoroughly oven dry in acetone solvent, absolute ethyl alcohol, deionized water for ultrasonic to be placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, with high pure metal platinum as target, be that 99.999% argon gas is as working gas with quality purity, the sputter operating pressure is 2.0Pa, sputtering power 80～90W, sputtering time 8～10min, substrate temperature are room temperature, form interdigital platinum electrode at alumina surface;
(2) preparation of seed solution
Ammonium metavanadate is dissolved in the deionized water of 20ml, magnetic agitation becomes light yellowly up to solution, add an amount of rare nitric acid, makes the pH control of solution about 2.1～2.5, and forming concentration is the seed solution of 0.05M～0.2M transparent salmon;
(3) preparation of Seed Layer
The ammonium metavanadate seed solution of preparation in the step (2) is coated on the alumina substrate that is covered with interdigital electrode of step (1) preparation, place annealing furnace air atmosphere annealing in process then, 500～650 ℃ of annealing temperatures, temperature retention time 1～2h, heating rate 2-3 ℃/min;
(4) preparation of hydro-thermal reaction solution
The ammonium metavanadate solution of preparation 0.04M～0.08M is dissolved in ammonium metavanadate in the deionized water, and magnetic agitation becomes light yellowly up to solution, adds an amount of rare nitric acid, makes the pH control of solution 2.1～2.5, the ammonium metavanadate solution of formation transparent salmon;
(5) preparation of vanadium pentoxide multi-stage nano network structure
To place liner be the stainless steel hydrothermal reaction kettle of teflon with covering the alumina substrate that the ammonium metavanadate Seed Layer is arranged in the step (3), also transfer to the ammonium metavanadate solution of step (4) preparation in the reactor simultaneously, sealing, adopt hydro-thermal method directly to synthesize vanadium pentoxide nanometer network structure on the alumina substrate surface down 180～200 ℃ of temperature then, the hydro-thermal reaction time is 9～15 hours, reaction finishes, and makes reactor naturally cool to room temperature;
(6) cleaning of change aluminium substrate after the hydro-thermal reaction
With the alumina substrate after the hydro-thermal reaction in the step (5), clean through deionized water and soaked in absolute ethyl alcohol repeatedly, dry in 60～80 ℃ vacuum drying chamber, make the gas sensor element based on vanadium pentoxide nanometer network structure.
2. according to the preparation method based on vanadium pentoxide nanometer network structure alcohol gas sensor element of claim 1, it is characterized in that the quality purity of the high pure metal platinum target of described step (1) is 99.95% metal platinum.
3. according to the preparation method based on vanadium pentoxide nanometer network structure alcohol gas sensor element of claim 1, it is characterized in that the platinum electrode thickness of the employing radio-frequency magnetron sputter method preparation of described step (1) is 80～120nm.
4. according to the preparation method based on vanadium pentoxide nanometer network structure alcohol gas sensor element of claim 1, it is characterized in that the seed solution of described step (3) adopts spin-coating method, dipping, spraying or drips and method such as is coated with and is coated on the alumina substrate that is covered with interdigital electrode.
5. according to the preparation method based on vanadium pentoxide nanometer network structure alcohol gas sensor element of claim 1, it is characterized in that, after the Seed Layer annealing of described step (3), can form equally distributed diameter at alumina substrate is 100nm～1 μ m, and length is the little crystal grain of 1～5 μ m.
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