CN104034757B - A kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof - Google Patents
A kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the gas sensor technical field of one dimension semiconductor oxide, be specifically related to a kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof.The alcohols gas sensor air-sensitive coating composition of the present invention is TeO2Nano wire, TeO2Nano wire has single Tetragonal crystal structure, smooth surface, and diameter is 70～200nm, and length is 500 μm～2mm, and draw ratio is maximum reaches 29000；The preparation method of gas sensor is first to prepare TeO2Nano wire, by TeO2Nano wire mixes with adhesive, is modulated into slip and is applied to ceramic base plate surface, becomes air-sensitive coating, then through heat treatment, finally obtains based on TeO2The alcohols gas sensor of nano wire.The present invention prepare first with thermal evaporation there is advantages of good crystallization, draw ratio is high, yield big, the TeO of high surface2Nano wire, then by TeO2Nano wire prepares into gas sensor, has the advantages such as low operating temperature, high sensitivity, low energy consumption.
Description
Technical field
The invention belongs to the gas sensor technical field of one dimension semiconductor oxide, be specifically related to a kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof.
Background technology
Along with the fast development of economic construction and the continuous of process of industrialization are accelerated, in the processes such as Mining Market, transportation and energy, manufacture processing, constantly give off multiple toxic and harmful.In these gases, some is inflammable and explosive, and some is poisonous and hazardous, if they leak in air will seriously contaminated environment, and have the potential danger causing blast, fire or making people poisoning.In order to effectively prevent and treat the generation of harmful gas, leakage and pollution, it is carried out quick, accurate, portable detection very necessary.Therefore, develop high performance gas sensor imperative, be possible not only to be effectively prevented from the generation of potential security incident, also process for follow-up harmful gas simultaneously and provide the monitoring guarantee of reliable early stage.
In the gas sensor of huge number, by conductor oxidate be the gas sensor that gas sensitive is prepared from have highly sensitive, respond/recover the advantages such as quick and cheap, its gas-sensitive reaction mechanism mainly belongs to sheet resistance control type, i.e. reaction between absorption oxonium ion and the detected gas of based semiconductor oxide surface, and utilize the resistance variations of the conductor oxidate produced therefrom to measure the response condition to detected gas.That presently commercially available alcohols gas sensor adopts is traditional SnO2、ZnO、TiO2、WO3Nanoparticle is gas sensitive, but owing to the agglomeration between particle makes the specific surface area of gas sensitive reduce, thus causing that sensitivity decrease and response/recovery time are longer.Therefore, current research worker focuses on more attention in synthesis and the application of one-dimentional structure nano material, such as nanotube, nano wire, nano belt etc..The features such as single structure, high-specific surface area and surface activity that these monodimension nanometer materials have, make it the potential gas sensitive with high sensitivity and high efficiency gas sensor.
TeO2As a kind of wide band gap semiconducter oxide material, there is the characteristics such as the photoelectricity of excellence, thermoelectricity and catalysis, thus have in the coloring agent etc. of infrared remote sensing, solaode, the catalyst of cracking of oil, pottery and glass and have been widely used.But, to TeO2The investigation of material gas-sensitive property is then still in the starting stage, and correlational study achievement is considerably less, and its corresponding gas sensitive is mainly based on thin-film material.Compared with thin-film material, nano wire has bigger specific surface area and surface activity, thus the air-sensitive performance shown also will be more superior.Additionally, good gas-sensitive property just can be obtained under current most of conductor oxidate gas sensor all operating temperatures more than 200 DEG C, result in that detection energy consumption is high and the complexity of sensor integration.Therefore, improving the sensitivity of gas sensor under cryogenic conditions further is current study hotspot.
Summary of the invention
For current TeO2The blank that material exists in gas-sensitive property application aspect, the present invention provides a kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof, it is therefore an objective to prepared by thermal evaporation there is advantages of good crystallization, draw ratio is high, yield is big TeO2Nano wire, and utilize these TeO2Nano wire is fabricated to the alcohols gas sensor of highly sensitive, good reversibility, response/the recover advantages such as quick, low operating temperature, to overcome response/resume speed that existing alcohols gas sensor exists slow and the problem such as high energy consumption that operating temperature height brings.
Realize the object of the invention based on TeO2The alcohols gas sensor of nano wire, being made up of ceramic substrate, heating resistor, interdigital gold electrode and air-sensitive coating, wherein heating resistor overlays on the ceramic substrate back side, and interdigital gold electrode overlays on ceramic base plate surface, air-sensitive coating is coated in interdigital gold electrode surfaces, and air-sensitive coating composition is TeO2Nano wire, described TeO2Nano wire has single Tetragonal crystal structure, smooth surface, and diameter is 70～200nm, and length is 500 μm～2mm, and draw ratio is maximum reaches 29000.
A kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof, carries out according to following steps:
(1) quartz ampoule is placed in open-type electric tube furnace, the metallic tellurium powder that quality purity is 99.999% is placed on Al2O3Porcelain boat central authorities, are placed on gold-plated glass substrate above metallic tellurium powder that 1～5mm place is in order to collect product, subsequently by Al2O3Porcelain boat sends into the quartz ampoule central authorities thermal treatment zone in electric tube furnace；
(2) fixing quartz ampoule with flange, adjustment air velocity is 0～300ml/min, and intensification electric tube furnace is to 400～500 DEG C and keeps 1～4h, closes electric tube furnace, treats that electric tube furnace naturally cools to room temperature, takes out Al from quartz ampoule2O3Porcelain boat, the milky deposit on gold-plated glass substrate is the TeO of preparation2Nano wire；
(3) TeO that will prepare2Nano wire and adhesive terpineol (90～99) in mass ratio: (10～1) mix, wet grinding 10～30min in agate mortar, are modulated into slip；
(4) above-mentioned slip is applied on ceramic base plate surface, becomes air-sensitive coating；
(5) after the ceramic substrate scribbling air-sensitive coating being placed on air drying 30～60min, in 200～300 DEG C of heat treatment 2～24h on agingtable, finally obtain by TeO2The alcohols gas sensor of nano wire composition.
On described gold-plated glass substrate thickness be 5～10nm golden membranous layer by ion sputtering process deposition form.
The described heat treatment on agingtable, removes adhesive terpineol from air-sensitive coating, is maintained with the structure of air-sensitive coating and stablizing of performance.
Compared with prior art, the feature of the present invention and providing the benefit that:
The invention provides a kind of TeO2Nano wire and consisting of alcohols gas sensor and preparation method thereof, this alcohols gas sensor has the advantages such as low operating temperature, high sensitivity, low energy consumption.
Preparation method, the present invention prepare first with thermal evaporation there is advantages of good crystallization, draw ratio is high, yield big, the TeO of high surface2Nano wire, then by TeO2Nano wire prepares into gas sensor, this gas sensor obtains the peak response to methanol and alcohol gas when room temperature 22 DEG C, the peak response to propanol gas is obtained when 50 DEG C, response and recovery time are short, reversibility and favorable reproducibility, efficiently solve tradition alcohols gas sensor in the poor deficiency of low-temperature region gas-sensitive property, be the alcohols gas sensor with good development prospect.
Accompanying drawing explanation
Fig. 1 be the present invention based on TeO2The alcohols gas sensor configuration schematic diagram of nano wire；
Wherein: 1: ceramic substrate；2: heating resistor；3: air-sensitive coating；4: interdigital gold electrode；
Fig. 2 is that the present invention prepares TeO2The device schematic diagram of nano wire；
Wherein, 5: tellurium powder；6: gold-plated glass substrate；7:Al2O3Porcelain boat；8: open-type electric tube furnace；9: quartz ampoule；10: air；11: flange；
Fig. 3 is TeO prepared by the present invention2The X ray diffracting spectrum of nano wire；
Fig. 4 is TeO prepared by the present invention2(a) low range of nano wire and (b) high magnification electron scanning micrograph；
Fig. 5 is TeO prepared by the present invention2The transmission electron microscope photo of nano wire；
Fig. 6 is the gas sensor of present invention dynamic response curve figure to 500ppm alcohol gas when (a) room temperature 22 DEG C, (b) 50 DEG C, (c) 75 DEG C, (d) 100 DEG C；
Fig. 7 is that the gas sensor of the present invention is to the graph of a relation between sensitivity and the operating temperature of 500ppm alcohol gas；
Fig. 8 is the gas sensor of present invention dynamic response curve figure to different concentration ethanol gas when room temperature 22 DEG C；
Fig. 9 is the gas sensor of present invention graph of a relation between sensitivity and ethanol gas concentration when room temperature 22 DEG C；
Figure 10 is the gas sensor of present invention gas sensitivity to 1000ppm methanol, ethanol and propanol when room temperature 22 DEG C.
Detailed description of the invention
Embodiment 1
Based on TeO2The alcohols gas sensor of nano wire, as shown in Figure 1, it is made up of ceramic substrate, heating resistor, interdigital gold electrode and air-sensitive coating, wherein heating resistor overlays on the ceramic substrate back side, interdigital gold electrode overlays on ceramic base plate surface, air-sensitive coating is coated in interdigital gold electrode surfaces, and described air-sensitive coating composition is TeO2Nano wire, TeO2Nano wire has single Tetragonal crystal structure, smooth surface, and diameter is 70～200nm, and length is 500 μm～2mm, and draw ratio is maximum reaches 29000.
Its X ray diffracting spectrum is as shown in Figure 3, it was shown that generation product is single TeO2Tetragonal crystal structure, without any other impurity diffraction maximum, crystalline condition is excellent.TeO2The electron scanning micrograph of nano wire as shown in Figure 4, from fig. 4, it can be seen that TeO2The yield of nano wire is big and smooth surface, and diameter is 70～200nm, and length is 500 μm～2mm, and draw ratio is maximum up to 29000；TeO2The transmission electron microscope photo of nano wire is as it is shown in figure 5, from figure 5 it can be seen that TeO2The smooth surface of nano wire is smooth, and diameter is about 85nm, is consistent with the result of electron scanning micrograph.
A kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof, carries out according to following steps:
(1) quartz ampoule is placed in open-type electric tube furnace, the metallic tellurium powder that 0.5g quality purity is 99.999% is placed on Al2O3Porcelain boat central authorities, are placed on gold-plated glass substrate above metallic tellurium powder that 2mm place is in order to collect product, subsequently by Al2O3Porcelain boat sends into the quartz ampoule central authorities thermal treatment zone in electric tube furnace；
(2) fixing quartz ampoule with flange, adjustment air velocity is 0ml/min, and intensification electric tube furnace is to 450 DEG C and keeps 2h, closes electric tube furnace, treats that electric tube furnace naturally cools to room temperature, takes out Al from quartz ampoule2O3Porcelain boat, the milky deposit on gold-plated glass substrate is the TeO of preparation2Nano wire；
(3) TeO that will prepare2Nano wire mixes with adhesive terpineol 95:5 in mass ratio, and wet grinding 10min in agate mortar is modulated into slip；
(4) above-mentioned slip is applied on ceramic base plate surface, becomes air-sensitive coating；
(5) after the ceramic substrate scribbling air-sensitive coating being placed on air drying 30min, in 300 DEG C of heat treatment 2h on agingtable, finally obtain by TeO2The alcohols gas sensor of nano wire composition.
In 22 DEG C to 100 DEG C operating temperature ranges of room temperature, TeO2Nano wire gas sensor is to the dynamic response curve figure of 500ppm alcohol gas as shown in Figure 6, as can be seen from Figure 6, the gas sensor of the present invention has response/recovery time, good reversibility faster, and resistance variations tapers into along with the rising of operating temperature；
Fig. 7 is that the gas sensor of the present invention is to the graph of a relation between sensitivity and the operating temperature of 500ppm alcohol gas, as can be seen from Figure 7, gas sensitivity is on a declining curve along with the rising of operating temperature, maximum gas sensitivity can be obtained room temperature 22 DEG C, this is the sharpest edges place of gas sensor of the present invention, it is possible to effectively reduce the energy consumption of gas sensor.
TeO2Nano wire gas sensor when room temperature 22 DEG C to the dynamic response curve figure of different concentration ethanol gas as shown in Figure 8, as can be seen from Figure 8, alcohol gas is had comparatively quickly response/recovery time by gas sensor when room temperature 22 DEG C, in 5 reaction times of continuous print, the alcohol gas of 100～1000ppm had good reversibility, resistance variations presents incremental trend along with the increase of ethanol gas concentration, showing that sensitivity increases along with the increase of ethanol gas concentration, the graph of a relation between its sensitivity and ethanol gas concentration is as shown in Figure 9.
TeO2Nano wire gas sensor when room temperature 22 DEG C to the gas sensitivity of 1000ppm methanol, ethanol and propanol as shown in Figure 10, it can be seen from fig. 10 that TeO2The level of sensitivity order of three kinds of alcohols gases is methanol by nano wire gas sensor > ethanol > propanol, the gas-selectively of methanol is best, and the gas-selectively of propanol is worst.
Embodiment 2
Based on TeO2The alcohols gas sensor of nano wire, as shown in Figure 1, it is made up of ceramic substrate, heating resistor, interdigital gold electrode and air-sensitive coating, wherein heating resistor overlays on the ceramic substrate back side, interdigital gold electrode overlays on ceramic base plate surface, air-sensitive coating is coated in interdigital gold electrode surfaces, and described air-sensitive coating composition is TeO2Nano wire, TeO2Nano wire has single Tetragonal crystal structure, smooth surface, and diameter is 70～200nm, and length is 500 μm～2mm, and draw ratio is maximum reaches 29000.
A kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof, carries out according to following steps:
(1) quartz ampoule is placed in open-type electric tube furnace, the metallic tellurium powder that 2g quality purity is 99.999% is placed on Al2O3Porcelain boat central authorities, are placed on gold-plated glass substrate above metallic tellurium powder that 5mm place is in order to collect product, subsequently by Al2O3Porcelain boat sends into the quartz ampoule central authorities thermal treatment zone in electric tube furnace；
(2) fixing quartz ampoule with flange, adjustment air velocity is 50ml/min, and intensification electric tube furnace is to 400 DEG C and keeps 4h, closes electric tube furnace, treats that electric tube furnace naturally cools to room temperature, takes out Al from quartz ampoule2O3Porcelain boat, the milky deposit on gold-plated glass substrate is the TeO of preparation2Nano wire；
(3) TeO that will prepare2Nano wire mixes with adhesive terpineol 90:10 in mass ratio, and wet grinding 20min in agate mortar is modulated into slip；
(4) above-mentioned slip is applied on ceramic base plate surface, becomes air-sensitive coating；
(5) after the ceramic substrate scribbling air-sensitive coating being placed on air drying 60min, in 200 DEG C of heat treatment 24h on agingtable, finally obtain by TeO2The alcohols gas sensor of nano wire composition.
After testing, the TeO that prepared by the present embodiment2Alcohols gas is had under 22～100 DEG C of conditions of room temperature and well responds effect by nano wire gas sensor.
Embodiment 3
Based on TeO2The alcohols gas sensor of nano wire, as shown in Figure 1, it is made up of ceramic substrate, heating resistor, interdigital gold electrode and air-sensitive coating, wherein heating resistor overlays on the ceramic substrate back side, interdigital gold electrode overlays on ceramic base plate surface, air-sensitive coating is coated in interdigital gold electrode surfaces, and described air-sensitive coating composition is TeO2Nano wire, TeO2Nano wire has single Tetragonal crystal structure, smooth surface, and diameter is 70～200nm, and length is 500 μm～2mm, and draw ratio is maximum reaches 29000.
A kind of based on TeO2Alcohols gas sensor of nano wire and preparation method thereof, carries out according to following steps:
(1) quartz ampoule is placed in open-type electric tube furnace, the metallic tellurium powder that 0.2g quality purity is 99.999% is placed on Al2O3Porcelain boat central authorities, are placed on gold-plated glass substrate above metallic tellurium powder that 1mm place is in order to collect product, subsequently by Al2O3Porcelain boat sends into the quartz ampoule central authorities thermal treatment zone in electric tube furnace；
(2) fixing quartz ampoule with flange, adjustment air velocity is 300ml/min, and intensification electric tube furnace is to 500 DEG C and keeps 1h, closes electric tube furnace, treats that electric tube furnace naturally cools to room temperature, takes out Al from quartz ampoule2O3Porcelain boat, the milky deposit on gold-plated glass substrate is the TeO of preparation2Nano wire.
(3) TeO that will prepare2Nano wire mixes with adhesive terpineol 99:1 in mass ratio, and wet grinding 30min in agate mortar is modulated into slip；
(4) above-mentioned slip is applied on ceramic base plate surface, becomes air-sensitive coating；
(5) after the ceramic substrate scribbling air-sensitive coating being placed on air drying 40min, in 250 DEG C of heat treatment 12h on agingtable, finally obtain by TeO2The alcohols gas sensor of nano wire composition.
After testing, the TeO that prepared by the present embodiment2Alcohols gas is had under 22～100 DEG C of conditions of room temperature and well responds effect by nano wire gas sensor.
Claims (1)
1. one kind based on TeO2The preparation method of the alcohols gas sensor of nano wire, it is characterised in that carry out according to following steps:
(1) quartz ampoule is placed in open-type electric tube furnace, the metallic tellurium powder that quality purity is 99.999% is placed on Al2O3Porcelain boat central authorities, are placed on gold-plated glass substrate above metallic tellurium powder that 1～5mm place is in order to collect product, subsequently by Al2O3Porcelain boat sends into the quartz ampoule central authorities thermal treatment zone in electric tube furnace；On described gold-plated glass substrate, golden membranous layer thickness is 5～10nm, ion sputtering process deposition form；
(2) fixing quartz ampoule with flange, adjustment air velocity is 0～300ml/min, and intensification electric tube furnace is to 400～500 DEG C and keeps 1～4h, closes electric tube furnace, treats that electric tube furnace naturally cools to room temperature, takes out Al from quartz ampoule2O3Porcelain boat, the milky deposit on gold-plated glass substrate is the TeO of preparation2Nano wire；
(3) TeO that will prepare2Nano wire and adhesive terpineol (90～99) in mass ratio: (10 ~ 1) mix, wet grinding 10～30min in agate mortar, are modulated into slip；
(4) above-mentioned slip is applied on ceramic base plate surface, becomes air-sensitive coating；
(5) after the ceramic substrate scribbling air-sensitive coating being placed on air drying 30～60min, in 200～300 DEG C of heat treatment 2～24h on agingtable, finally obtain by TeO2The alcohols gas sensor of nano wire composition.
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