CN104502418B - Based on ZnO/ α-Fe2o3acetone gas sensor of composite oxide semiconductor and preparation method thereof - Google Patents
Based on ZnO/ α-Fe2o3acetone gas sensor of composite oxide semiconductor and preparation method thereof Download PDFInfo
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Abstract
A kind of based on ZnO/ α Fe2O3Acetone gas sensor of composite oxide semiconductor and preparation method thereof, belongs to gas sensor technical field.The present invention uses two step solvent-thermal methods to prepare ZnO/ α Fe2O3Heterojunction structure sensitive material, utilizes ZnO and α Fe2O3Between formed a large amount of hetero-junctions and the two collaborative sensitization to acetone, drastically increase sensitive material and to the sensitivity of acetone and accelerate the response speed to acetone.Senser element made in the present invention is by the Al with two annular gold electrodes2O3Insulating ceramics pipe, the Ni Cr alloy through ceramic tube inside heats coil and is coated in Al2O3Sensitive material three part of earthenware outer surface is constituted.Device architecture is simple, cheap, small volume, it is easy to integrated and production in enormous quantities, and acetone is revealed in the industrial production detection and warning aspect have important application prospect.
Description
Technical field
The invention belongs to gas sensor technical field, be specifically related to a kind of based on ZnO/ α-Fe2O3Acetone gas sensor of composite oxide semiconductor and preparation method thereof.
Background technology
Gas sensor can be defined as a kind of when being exposed in gas with various atmosphere, its intrinsic physical quantity, the device that can be measured by specific instrument such as the variable quantity of quality, resistance value, dielectric property etc. and quantify.Compared with numerous traditional gas detecting means, gas sensor is considered as to detect poisonous, harmful, inflammable, a kind of simple in construction of explosion hazard gases, instrument with low cost.Therefore, gas sensor is widely used in all many-sides such as commercial production safety, environmental monitoring, indoor and public safety and automobile emission gas analyzer etc..
Although conductor oxidate is (such as α-Fe2O3,SnO2, ZnO, In2O3, NiO etc.) and cheap due to it, low energy consumption, the advantage such as easy preparation is widely used in gas sensor domain.But, the problems such as it still suffers from poor selectivity, and sensitivity is the highest.Therefore, the methods such as many scientists attempt to be supported by noble metal, doped transition metal ions improve the air-sensitive performance of sensitive material, thus meet people to having high sensitivity, fast-response speed, the needs that good selective gas sensor is growing.In addition, two kinds of metal-oxides are combined, construct hetero-junctions and utilize the two cooperative effect to be also a kind of extremely effective mode improving sensitive property simultaneously.
Acetone is a kind of important organic synthesis raw material, is widely used in pesticide, medicine, coating and the commercial production such as spray paint.Although acetone is the most essential, but owing to it has inflammable, volatile and has strong impulse, so, if people are chronically exposed in acetone there will be dizziness, pharyngitis, bronchitis, the ill symptoms such as weak, healthy to people brings harm greatly.Therefore, it is particularly important for detecting the acetone gas in commercial production fast and accurately ensureing commercial production safety and the unnecessary property loss of minimizing.This is accomplished by by means of high sensitivity, the acetone gas sensor of fast response time.
At present, seldom it is related to liquid phase method and prepares ZnO/ α-Fe2O3Composite materials, and it is applied to the document report of field of gas detection.We are prepared for ZnO/ α-Fe first2O3Complex, finds, single α-Fe compared by this composite subsequently when studying its gas-sensitive property2O3Acetone is shown higher sensitivity and faster response speed so that it exists great application prospect at acetone detection field.
Summary of the invention
It is an object of the invention to use a kind of simple effective and that productivity is big liquid phase method to prepare ZnO/ α-Fe2O3Composite oxides sensitive material, and for making gas sensor to verify its application in terms of acetone gas Leak Detection and warning in the industrial production.The present invention, by the way of semi-conducting material is compound, drastically increases the sensitivity of sensor and accelerates the response speed of sensor, further promoting the sensors with auxiliary electrode application at field of industrial production.
Sensor obtained by the present invention is in addition to having high sensitivity, fast response speed, and has good selectivity and repeatability.This sensor is about 30 to the sensitivity of 100ppm acetone, is less than the response time of 20ppm acetone 1 second.Therefore, it can the leakage to acetone quickly detect and report to the police.
ZnO/ α-Fe of the present invention2O3The structure of oxide semiconductor acetone sensor is as it is shown in figure 1, it is with the Al of 2 annular gold electrodes 4 by outer surface2O3Insulating ceramics pipe 1, through Al2O3Ni-Cr alloy heater strip 2 within insulating ceramics pipe 1 and the sensitive material 3 being coated on insulating ceramics pipe 1 outer surface and annular gold electrode 4 are constituted；And each annular gold electrode 4 on be connected to a pair platinum filament 5.Gas sensor is S=R to the definition of reducibility gas sensitivitya/Rg, wherein RaAnd RgIt is respectively sensor two interelectrode resistance value when air atmosphere and atmosphere to be measured.It is characterized in that: sensitive material 3 is ZnO/ α-Fe2O3Composite oxide semiconductor sensitive material, it prepares by following steps,
(1)α-Fe2O3Preparation
First by 12.5～17.5mmol FeCl3·6H2The cetyl trimethylammonium bromide of O, 2.3～4.1mmol and 3.5～5.3mmol hexamethylenetetramines are added sequentially in the mixed solvent of deionized water and ethanol that (solvent volume is 30mL, the volume ratio of deionized water and ethanol is 1:2～1:1), ultrasonic make dissolving；
2. above-mentioned solution is transferred in reactor, the airtight baking oven being placed on 140～160 DEG C reacts 12～14 hours, make reactor naturally cool to room temperature subsequently, then gained precipitation is cleaned with ethanol and deionized water respectively, after being finally dried at room temperature for, obtain α-Fe2O3Powder, it is fillet hexahedron structure；
(2) the ZnO/ α-Fe of heterojunction structure2O3The preparation of composite semiconductor oxide
1. α-the Fe of 35～55mg is taken2O3Fillet hexahedron powder joins in 10～15mL ethylene glycol, ultrasonic makes α-Fe2O3It is completely dispersed, is subsequently adding the Zn (NO of 50～70mg3)2·6H2O, stirring makes Zn (NO3)2·6H2O is completely dissolved；
2. above-mentioned mixing liquid is poured in reactor, react 12～14 hours at 180～200 DEG C, be cooled to the precipitate with deionized water generated and ethanol eccentric cleaning after room temperature, under room temperature, obtain ZnO nano particle modification α-Fe after drying2O3The ZnO/ α-Fe of heterojunction structure2O3Composite semiconductor oxide powder.
Of the present invention is a kind of based on ZnO/ α-Fe2O3The acetone gas sensor of composite semiconductor oxide, its concrete manufacturing process is as follows:
1. by ZnO/ α-Fe2O3Composite semiconductor oxide powder is sufficiently mixed with mass ratio 4:1～6:1 with deionized water, forms pasty slurry, then slurry is uniformly coated on the commercially available outer surface Al with 2 annular gold electrodes 42O3Earthenware 1 surface, forms the sensitive material 3 that thickness is 10～30 μm, and makes sensitive material that annular gold electrode 4 is completely covered；A length of the 4 of earthenware 1～4.5mm, external diameter is 1.2～1.5mm, and internal diameter is 0.8～1.0mm；
2. by the Al of coated sensitive material2O3Earthenware 1 is placed under infrared lamp (power is 100～150W) baking 30～45 minutes, treats that sensitive material is dried, Al2O3Earthenware 1 is calcined 2～3 hours at 400～450 DEG C；Then the Ni-Cr alloy heating coil that resistance value is 30～40 Ω is passed Al2O3Above-mentioned device, as heater strip, is finally welded according to general heater-type gas sensor and encapsulates by ceramic tube inside, thus obtains based on ZnO/ α-Fe2O3The acetone gas sensor of composite oxide semiconductor.
Utilize ZnO/ α-Fe2O3Composite oxide semiconductor is as sensitive material, on the one hand, ZnO and α-Fe2O3It is all conventional sensitive material, ZnO/ α-Fe can be made under the effect of the two cooperative effect2O3The sensitive property of composite oxide semiconductor is further enhanced；On the other hand, α-Fe it is grown in2O3The ZnO nano granule on fillet hexahedron surface makes to form therebetween substantial amounts of hetero-junctions, and these are heterogeneous becomes surface reaction and provide more avtive spot, equally improves the air-sensitive performance of sensitive material.Thus, the common effect of these two aspects can be greatly improved the reaction efficiency between sensitive material and gas and speed, and then improves sensitivity and the response speed of sensor greatly.Meanwhile, the present invention use liquid phase method that productivity is big to prepare sensitive material, and with commercially available cheap Al2O3Sensor construction constructed by earthenware, and its technique is simple, and volume is little, it is easy to integrated, thus is beneficial to batch production, has relatively broad application prospect.
Advantages of the present invention:
(1) utilizing two step solvent structure sensitive materials, synthetic method is simple, and instrument and equipment requires low, low cost, it is easy to industrialized mass production；
(2) common and ZnO and the α-Fe of rich content is used2O3As basic sensitive material, by the way of semiconductors coupling, synthesize the ZnO/ α-Fe of heterojunction structure2O3Sensitive material, improves the sensitivity to acetone, and has response speed and preferably repeatability faster, have broad application prospects in detection commercial production in terms of content of acetone；
(3) using commercially available tubular type sensor construction, device technology is simple, and volume is little, it is easy to integrated, is suitable to produce in enormous quantities.
Accompanying drawing explanation
Fig. 1: based on ZnO/ α-Fe2O3The acetone gas sensor construction schematic diagram of composite oxide semiconductor；
ZnO/ α-the Fe of Fig. 2: heterojunction structure2O3The SEM photograph of fillet hexahedron sensitive material, wherein the amplification of figure (a) is 8000 times, and the amplification of figure (b) is 50000 times；
ZnO/ α-the Fe of Fig. 3: heterojunction structure2O3The XRD spectra of fillet hexahedron sensitive material；
Sensor Sensitivity comparison figure to 100ppm acetone at a temperature of different operating in Fig. 4: comparative example and embodiment；Concrete method of testing is as follows: first put in gas tank by sensor, is carried out the operating temperature of adjusting device by the electric current of Ni-Cr alloy heater strip by regulation, the most available sensor i.e. R of aerial resistance value after it is stablea；Subsequently, with microsyringe, 100ppm acetone is injected in gas tank, treat that its resistance stablizes postscript lower sensor resistance R in acetoneg.Defined formula S=R according to sensitivity Sa/Rg, just obtained the sensor sensitivity at such a temperature to 100ppm acetone by calculating.Similarly, repeat said process, just can get the device sensitivity to 100ppm acetone at a temperature of different operating by the electric current of regulation Ni-Cr alloy heater strip.Subsequently, the data recorded are processed, so that it may comparative example and embodiment sensor to the sensitivity of 100ppm acetone with the change curve of operating temperature；
In Fig. 5: comparative example and embodiment sensor respectively operating temperature be 237.5 DEG C and 287.5 DEG C, acetone concentration be under 20ppm, the response recovery curve of device；Concrete operations are as follows: for embodiment sensor, first sensor is put in gas tank, regulate under the operating temperature making device be operated in 287.5 DEG C by the electric current of Ni-Cr alloy heater strip, after its resistance is stable, 20ppm acetone is injected in gas tank, after resistance is stable, device is transferred in the gas tank of another full air so that it is slowly recover, thus obtained the embodiment sensor response recovery curve to 20ppm acetone under the operating temperature of 287.5 DEG C.Same method of testing is taked for comparative example sensor, under the operating temperature of 237.5 DEG C, simply records its response recovery curve.
The standard working curve of the acetone concentration-sensitivity of sensor in Fig. 6: comparative example and embodiment.Sensitivity test method: first put in gas tank by sensor, treats that its resistance the most i.e. obtains the sensor i.e. R of aerial resistance valuea；Then use microsyringe to be implanted sequentially the acetone of 5～100ppm in gas cabinet, obtain the sensor i.e. R of the resistance value in variable concentrations acetone by measurementg, according to the defined formula S=R of sensitivity Sa/Rg, by being calculated the sensitivity of variable concentrations lower sensor, finally give the standard working curve of acetone concentration-sensitivity.R can be recorded by above-mentioned way during actual measurementa、Rg, after obtaining Sensitirity va1ue, the standard working curve with acetone concentration-sensitivity contrasts, thus obtains the content of acetone in environment.It addition, as shown in the figure when acetone concentration is in the range of 100ppm, transducer sensitivity linear preferably, these features make this kind of acetone sensor can be good at being applied to the detection of acetone gas in commercial production.
As it is shown in figure 1, each component names of gas sensor is: Al2O3Insulating ceramics pipe 1, Ni-Cr alloy heater strip 2, sensitive material 3, annular gold electrode 4, platinum filament 5；
As in figure 2 it is shown, (a) figure can be seen that ZnO/ α-Fe2O3Complex is fillet hexahedron structure, and the hexahedral particle diameter of fillet is about 1～1.2 μm, finds out ZnO/ α-Fe in (b) figure2O3Heterojunction structure is by being grown in α-Fe2O3The erose ZnO nano granule that has on fillet hexahedron surface is constituted；
As it is shown on figure 3, the XRD spectra of products therefrom occurs in that α-Fe after two step solvent thermal reactions2O3With the characteristic peak of ZnO, illustrate that sample comprises α-Fe2O3And ZnO crystal；
As shown in Figure 4, the optimum working temperature of comparative example and embodiment is respectively 237.5 DEG C and 287.5 DEG C, and now device is respectively 6.4 and 29.9 to the sensitivity of 100ppm acetone；
As it is shown in figure 5, when acetone gas concentration is 20ppm, the response time of comparative example is 8s, the response time of embodiment is then less than 1s.Comparatively speaking, the response speed of embodiment relatively comparative example is greatly improved；
As shown in Figure 6, when comparative example and embodiment are at operating temperature is respectively 237.5 DEG C and 287.5 DEG C, the sensitivity of two class devices-acetone concentration standard working curve.Can significantly find out from figure, the sensitivity of device all increases along with the increase of acetone concentration, wherein embodiment is respectively 4.7,6.5,9.7,14.9,16.9,20.5,21.6,23.1,25.9,27.2 and 29.9 to the sensitivity of 5,10,20,30,40,50,60,70,80,90 and 100ppm acetone, and comparative example is then respectively 1.1,1.4,2.1,2.4,2.9,4.4,4.8,5.4,6.2,6.9 and 7.2 to the sensitivity of 5～100ppm acetone.Comparatively speaking, the sensitivity relatively comparative example of acetone is greatly improved by embodiment.
Detailed description of the invention
Comparative example 1:
With α-Fe2O3Fillet hexahedron makes heater-type acetone sensor as sensitive material, and its concrete manufacturing process is as follows:
First by the FeCl of 15.0mmol3·6H2In the mixed solvent that the cetyl trimethylammonium bromide of O, 3.3mmol and 4.3mmol hexamethylenetetramine are added sequentially to 15mL deionized water and 15mL ethanol is prepared, after ultrasonic 30 minutes, the experimental drug of addition is made all to dissolve.
2. above-mentioned solution is transferred in the reactor that volume is 40mL, until reactor is tightened airtight after be placed in the electrical heating baking oven of 160 DEG C reaction 12 hours, make reactor naturally cool to room temperature and gained precipitation be cleaned 5 times with ethanol and deionized water respectively subsequently, after being dried at room temperature for, just obtain α-Fe2O3Fillet hexahedron powder.
3. by the α-Fe of above-mentioned preparation2O3Powder is sufficiently mixed with mass ratio 5:1 with deionized water, thus forms pasty slurry.Then with hairbrush, slurry is uniformly coated on the commercially available outer surface Al with 2 annular gold electrodes2O3The outer surface of earthenware, forms thickness and is about the sensitive material film of 30 μm, and make sensitive material that two annular gold electrodes are completely covered.
4. by the Al of coated sensitive material2O3Earthenware is placed under infrared lamp baking 40 minutes, treats that sensitive material is dried, Al2O3Earthenware is calcined 3 hours at 400 DEG C；The Ni-Cr alloy heating coil that then resistance value is about 40 Ω passes Al2O3Above-mentioned device, as heater strip, is finally welded according to general heater-type gas sensor and encapsulates, thus obtain based on α-Fe by ceramic tube inside2O3Fillet hexahedral acetone gas sensor.
Embodiment 1:
With ZnO/ α-Fe2O3Complex heterojunction structure makes acetone sensor as sensitive material, its concrete manufacturing process:
First by the FeCl of 15.0mmol3·6H2In the mixed solvent that the cetyl trimethylammonium bromide of O, 3.3mmol and 4.3mmol hexamethylenetetramine are added sequentially to 15mL ionized water and 15mL ethanol is prepared, after ultrasonic 30 minutes, the experimental drug of addition is made all to dissolve.
2. above-mentioned solution is transferred in the reactor that volume is 40mL, until reactor is tightened airtight after be placed in the electrical heating baking oven of 160 DEG C reaction 12 hours, make reactor naturally cool to room temperature and gained precipitation be cleaned 5 times with ethanol and deionized water respectively subsequently, after being finally dried at room temperature for, just obtain α-Fe2O3Fillet hexahedron powder.
3. take 40mg above-mentioned α-Fe2O3Powder joins in the ethylene glycol solvent of 10mL, within ultrasonic 15 minutes, makes α-Fe2O3Fillet hexahedron powder is thoroughly dispersed in ethylene glycol；It is subsequently adding the Zn (NO of 55mg3)2·6H2O, stirs 20 minutes under room temperature, treats Zn (NO3)2·6H2After O is completely dissolved, the solution configured is transferred in the reactor that volume is 40mL, reacts 12 hours at 180 DEG C, be cooled to by the precipitate with deionized water generated and ethanol repeatedly eccentric cleaning after room temperature, and be dried at room temperature for, thus obtain ZnO/ α-Fe2O3Composite oxide semiconductor；
4. by the ZnO/ α-Fe of above-mentioned preparation2O3Composite powder is sufficiently mixed with mass ratio 5:1 with deionized water, thus forms pasty slurry.Then with hairbrush, slurry is uniformly coated on the commercially available outer surface Al with 2 annular gold electrodes2O3The outer surface of earthenware, forms thickness and is about the sensitive material film of 30 μm, and make sensitive material that two annular gold electrodes are completely covered.
5. by the Al of coated sensitive material2O3Earthenware is placed under infrared lamp baking 40 minutes, treats that sensitive material is dried, Al2O3Earthenware is calcined 3 hours at 400 DEG C；The Ni-Cr alloy heating coil that then resistance value is about 40 Ω passes Al2O3Above-mentioned device, as heater strip, is finally welded according to general heater-type gas sensor and encapsulates by ceramic tube inside, thus obtains base ZnO/ α-Fe2O3The acetone gas sensor of complex heterojunction structure.
Claims (4)
1. one kind based on ZnO/ α-Fe2O3The acetone gas sensor of composite oxide semiconductor, is with the Al of 2 annular gold electrodes (4) by outer surface2O3Insulating ceramics pipe (1), through Al2O3Ni-Cr alloy heater strip (2) that insulating ceramics pipe (1) is internal and be coated in Al2O3Sensitive material (3) on insulating ceramics pipe (1) outer surface and annular gold electrode (4) is constituted, and the most each annular gold electrode (4) is connected to a pair platinum filament (5)；It is characterized in that: sensitive material (3) is ZnO/ α-Fe2O3Composite oxide semiconductor sensitive material, it prepares by following steps,
First by 12.5～17.5mmol FeCl3·6H2The cetyl trimethylammonium bromide of O, 2.3～4.1mmol and 3.5～5.3mmol hexamethylenetetramine be added sequentially in the mixed solvent of deionized water and ethanol, ultrasonic make dissolving；
2. above-mentioned solution is transferred in reactor, the airtight baking oven being placed on 140～160 DEG C reacts 12～14 hours, make reactor naturally cool to room temperature subsequently, then gained precipitation is cleaned with ethanol and deionized water respectively, after being finally dried at room temperature for, obtain α-Fe2O3Powder；
3. α-the Fe of 35～55mg is taken2O3Powder joins in 10～15mL ethylene glycol, ultrasonic makes α-Fe2O3It is completely dispersed, is subsequently adding the Zn (NO of 50～70mg3)2·6H2O, stirring makes Zn (NO3)2·6H2O is completely dissolved；
4. above-mentioned mixing liquid is poured in reactor, react 12～14 hours at 180～200 DEG C, be cooled to the precipitate with deionized water generated and ethanol eccentric cleaning after room temperature, under room temperature, obtain the ZnO/ α-Fe of heterojunction structure after drying2O3Composite semiconductor oxide powder.
2. as claimed in claim 1 a kind of based on ZnO/ α-Fe2O3The acetone gas sensor of composite oxide semiconductor, it is characterised in that: ZnO/ α-Fe2O3Composite oxide semiconductor is fillet hexahedron structure, and the hexahedral particle diameter of fillet is 1～1.2 μm, ZnO/ α-Fe2O3Heterojunction structure is by being grown in α-Fe2O3The erose ZnO nano granule that has on fillet hexahedron surface is constituted, ZnO/ α-Fe2O3The thickness of composite oxide semiconductor sensitive material is 10～30 μm.
3. as claimed in claim 1 a kind of based on ZnO/ α-Fe2O3The acetone gas sensor of composite oxide semiconductor, it is characterised in that: the volume ratio that volume is 30mL, deionized water and ethanol of step 1. middle mixed solvent is 1:2～1:1.
4. the one described in claims 1 to 3 any one is based on ZnO/ α-Fe2O3The preparation method of the acetone gas sensor of composite oxide semiconductor, its step is as follows:
1. by ZnO/ α-Fe2O3Composite semiconductor oxide powder is sufficiently mixed with mass ratio 4:1～6:1 with deionized water, forms pasty slurry, then slurry is uniformly coated on the outer surface Al with 2 annular gold electrodes (4)2O3Insulating ceramics pipe (1) surface, forms the sensitive material (3) that thickness is 10～30 μm, and makes sensitive material that annular gold electrode (4) is completely covered；
2. by the Al of coated sensitive material2O3Insulating ceramics pipe (1) is placed under infrared lamp baking 30～45 minutes, treats that sensitive material is dried, Al2O3Insulating ceramics pipe (1) is calcined 2～3 hours at 400～450 DEG C；Then the Ni-Cr alloy heating coil that resistance value is 30～40 Ω is passed Al2O3Insulating ceramics pipe (1) is internal as heater strip, finally above-mentioned device is welded according to general heater-type gas sensor and is encapsulated, thus obtains based on ZnO/ α-Fe2O3The acetone gas sensor of composite oxide semiconductor.
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| JP2921032B2 (en) * | 1990-05-25 | 1999-07-19 | 東陶機器株式会社 | Ammonia gas sensor |
| JP2000131259A (en) * | 1998-10-23 | 2000-05-12 | Nippon Ceramic Co Ltd | Oxidizing gas sensor |
| CN1955729A (en) * | 2005-10-26 | 2007-05-02 | 井叶之 | Acetone steam gas sensitive sensing element |
| CN103675078B (en) * | 2013-12-11 | 2014-12-10 | 中国人民解放军白求恩医务士官学校 | Preparation method for acetone gas sensor |
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