CN104502418A - Acetone-gas sensor based on ZnO/alpha-Fe2O3 compound oxide semiconductor and preparation method of acetone-gas sensor - Google Patents

Acetone-gas sensor based on ZnO/alpha-Fe2O3 compound oxide semiconductor and preparation method of acetone-gas sensor Download PDF

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CN104502418A
CN104502418A CN201510012903.6A CN201510012903A CN104502418A CN 104502418 A CN104502418 A CN 104502418A CN 201510012903 A CN201510012903 A CN 201510012903A CN 104502418 A CN104502418 A CN 104502418A
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acetone
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oxide semiconductor
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卢革宇
周鑫
孙鹏
刘凤敏
李晓伟
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Jilin University
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Abstract

The invention discloses an acetone-gas sensor based on a ZnO/alpha-Fe2O3 compound oxide semiconductor and a preparation method of the acetone-gas sensor and belongs to the technical field of the gas sensor. The acetone-gas sensor and the preparation method have the advantages that a two-step solvothermal method is adopted for preparing a ZnO/alpha-Fe2O3 heterostructure sensitive material, a great amount of heterojunctions formed between ZnO and alpha-Fe2O3 and the collaborative sensitization of ZnO and alpha-Fe2O3 for the acetone are utilized, so that the sensitivity of the sensitive material for acetone is greatly improved and the response speed for the acetone is accelerated. The sensing device prepared in the invention is formed by an Al2O3 insulated ceramic tube with two ring-shaped gold electrodes, a Ni-Cr alloy heating coil penetrating through the inner part of the ceramic tube and a sensitive material coating the outer surface of the Al2O3 ceramic tube. The sensor is simple in structure, low in price, small in volume and easy in integration and large-batch production, and has an important application prospect in the aspects of detection and alarming for acetone leakage in industrial production.

Description

Based on ZnO/ α-Fe 2o 3acetone gas sensor of composite oxide semiconductor and preparation method thereof
Technical field
The invention belongs to gas sensor technical field, be specifically related to a kind of based on ZnO/ α-Fe 2o 3acetone 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, and the variable quantity as quality, resistance value, dielectric property etc. can carry out by specific instrument the device measuring and quantize.Compared with numerous traditional gas detect means, gas sensor is considered to detect a kind of structure that is poisonous, harmful, inflammable, explosion hazard gases instrument simple, 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 (as α-Fe 2o 3, SnO 2, ZnO, In 2o 3, NiO etc.) and cheap due to it, low energy consumption, the advantages such as easy preparation are widely used in gas sensor domain.But still there is poor selectivity in it, the problems such as sensitivity is not high.Therefore, many scientific workers attempt to be supported by noble metal, and the methods such as doped transition metal ions improve the air-sensitive performance of sensitive material, thus meet people to having high sensitivity, fast-response speed, the good needs that optionally gas sensor is growing.In addition, two kinds of metal oxides are carried out compound, construct heterojunction and utilize the cooperative effect of the two to be also a kind of very effective mode improving sensitive property simultaneously.
Acetone is a kind of important organic synthesis raw material, in the commercial production such as be widely used in agricultural chemicals, medicine, coating and spray paint.Although acetone is essential in the industrial production, but have inflammable, volatile due to it and there is strong impulse, so, if people are chronically exposed in acetone there will be dizzy, pharyngitis, bronchitis, the ill symptoms such as weak, great harm is brought to the healthy of people.Therefore, it is very important for detecting guarantee commercial production safety and the unnecessary property loss of minimizing fast and accurately to the acetone gas in commercial production.This just needs the acetone gas sensor by means of high sensitivity, fast response time.
At present, seldom have both at home and abroad about Liquid preparation methods ZnO/ α-Fe 2o 3composite materials, and the bibliographical information being applied to field of gas detection.We have prepared ZnO/ α-Fe first 2o 3compound, find when studying its gas-sensitive property subsequently, single α-Fe compared by this compound substance 2o 3higher sensitivity and response speed are faster shown to acetone, makes it there is great application prospect at acetone detection field.
Summary of the invention
The object of the invention is to adopt a kind of simple effectively and the large liquid phase method of productive rate carrys out making ZnO/α-Fe 2o 3composite oxides sensitive material, and for making gas sensor to verify the application of its acetone gas Leak Detection and warning aspect in the industrial production.The present invention, by the mode of semiconductor material compound, drastically increases the sensitivity of sensor and accelerates the response speed of sensor, further promoting the application of sensors with auxiliary electrode at field of industrial production.
The sensor that the present invention obtains except having high sensitivity, fast response speed, and has good selectivity and repeatability.The sensitivity of this sensor to 100ppm acetone is about 30, is less than 1 second to the response time of 20ppm acetone.Therefore, can detect fast the leakage of acetone and report to the police.
ZnO/ α-Fe of the present invention 2o 3as shown in Figure 1, it is by the Al of outside surface with 2 annular gold electrodes 4 to the structure of oxide semiconductor acetone sensor 2o 3insulating ceramics pipe 1, through Al 2o 3ni-Cr alloy heater strip 2 and the sensitive material 3 be coated on insulating ceramics pipe 1 outside surface and annular gold electrode 4 of insulating ceramics pipe 1 inside are formed; And each annular gold electrode 4 is connected to a pair platinum filament 5.Gas sensor is defined as S=R to reducibility gas sensitivity a/ R g, wherein R aand R gbe respectively sensor two interelectrode resistance values when air atmosphere and atmosphere to be measured.It is characterized in that: sensitive material 3 is ZnO/ α-Fe 2o 3composite oxide semiconductor sensitive material, it is prepared by following steps,
(1) α-Fe 2o 3preparation
1. first by the FeCl of 12.5 ~ 17.5mmol 36H 2the cetyl trimethyl ammonium bromide of O, 2.3 ~ 4.1mmol and 3.5 ~ 5.3mmol hexamethylenetetramine join in the mixed solvent of deionized water and ethanol that (solvent volume is 30mL successively, the volume ratio of deionized water and ethanol is 1:2 ~ 1:1), ultrasonicly make dissolving;
2. above-mentioned solution is transferred in reactor, airtight being placed in the baking oven of 140 ~ 160 DEG C is reacted 12 ~ 14 hours, make reactor naturally cool to room temperature subsequently, then gained precipitation is used ethanol and washed with de-ionized water respectively, finally obtain α-Fe after at room temperature drying 2o 3powder, it is fillet hexahedron structure;
(2) the ZnO/ α-Fe of heterojunction structure 2o 3the preparation of composite semiconductor oxide
1. α-the Fe of 35 ~ 55mg is got 2o 3fillet hexahedron powder joins in 10 ~ 15mL ethylene glycol, ultrasonicly makes α-Fe 2o 3disperse completely, then add the Zn (NO of 50 ~ 70mg 3) 26H 2o, stirs and makes Zn (NO 3) 26H 2o dissolves completely;
2. above-mentioned mixing material is poured in reactor, react 12 ~ 14 hours at 180 ~ 200 DEG C, to be cooled to the precipitate with deionized water that generates and ethanol eccentric cleaning after room temperature, under room temperature, after drying, to obtain ZnO nano particle modification α-Fe 2o 3the ZnO/ α-Fe of heterojunction structure 2o 3composite semiconductor oxide powder.
Of the present invention is a kind of based on ZnO/ α-Fe 2o 3the acetone gas sensor of composite semiconductor oxide, its concrete manufacturing process is as follows:
1. by ZnO/ α-Fe 2o 3composite semiconductor oxide powder fully mixes with mass ratio 4:1 ~ 6:1 with deionized water, forms pasty slurry, then slurry is coated in equably the Al of commercially available outside surface with 2 annular gold electrodes 4 2o 3ceramic pipe 1 surface, forms the sensitive material 3 that thickness is 10 ~ 30 μm, and makes sensitive material cover annular gold electrode 4 completely; The length of ceramic pipe 1 is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, and internal diameter is 0.8 ~ 1.0mm;
2. by the Al of coated sensitive material 2o 3ceramic pipe 1 toasts 30 ~ 45 minutes, after sensitive material drying, Al under being placed in infrared lamp (power is 100 ~ 150W) 2o 3ceramic pipe 1 is calcined 2 ~ 3 hours at 400 ~ 450 DEG C; Then be that the Ni-Cr alloy heater coil of 30 ~ 40 Ω is through Al by resistance value 2o 3above-mentioned device, as heater strip, finally carries out welding and encapsulating according to general heater-type gas sensor by ceramic tube inside, thus obtains based on ZnO/ α-Fe 2o 3the acetone gas sensor of composite oxide semiconductor.
Utilize ZnO/ α-Fe 2o 3composite oxide semiconductor as sensitive material, on the one hand, ZnO and α-Fe 2o 3be all conventional sensitive material, ZnO/ α-Fe can be made under the effect of the two cooperative effect 2o 3the sensitive property of composite oxide semiconductor is further enhanced; On the other hand, grow at α-Fe 2o 3the ZnO nano particle on fillet hexahedron surface makes to form a large amount of heterojunction therebetween, and these are heterogeneous becomes surface reaction and provide more avtive spot, can improve the air-sensitive performance of sensitive material equally.Thus, the acting in conjunction of these two aspects can improve reaction efficiency between sensitive material and gas and speed greatly, and then improves sensitivity and the response speed of sensor greatly.Meanwhile, the liquid phase method that the present invention adopts productive rate large to prepare sensitive material, and with commercially available cheap Al 2o 3sensor construction constructed by ceramic pipe, and its technique is simple, and volume is little, is easy to integrated, is thus beneficial to batch production, has application prospect comparatively widely.
Advantage of the present invention:
(1) utilize two step solvent structure sensitive materials, synthetic method is simple, and instrument and equipment requires low, and cost is low, is easy to industrialized mass production;
(2) common and ZnO and the α-Fe of rich content is adopted 2o 3as basic sensitive material, synthesized the ZnO/ α-Fe of heterojunction structure by the mode of semiconductors coupling 2o 3sensitive material, improves the sensitivity to acetone, and has response speed and preferably repeatability faster, has broad application prospects in detection commercial production in content of acetone;
(3) adopt commercially available tubular type sensor construction, device technology is simple, and volume is little, is easy to integrated, is suitable for producing in enormous quantities.
Accompanying drawing explanation
Fig. 1: based on ZnO/ α-Fe 2o 3the acetone gas sensor construction schematic diagram of composite oxide semiconductor;
Fig. 2: the ZnO/ α-Fe of heterojunction structure 2o 3the SEM photo of fillet hexahedron sensitive material, the enlargement factor wherein scheming (a) is 8000 times, and the enlargement factor of figure (b) is 50000 times;
Fig. 3: the ZnO/ α-Fe of heterojunction structure 2o 3the XRD spectra of fillet hexahedron sensitive material;
Fig. 4: in comparative example and embodiment sensor at different operating temperature to the Sensitivity comparison figure of 100ppm acetone; Concrete method of testing is as follows: first sensor is put into gas tank, by regulating the working temperature being carried out adjusting device by the electric current of Ni-Cr alloy heater strip, after it is stable, just can obtain the aerial resistance value of sensor and R a; Subsequently, with microsyringe by 100ppm acetone inject gas tank, treat that its resistance stablizes postscript lower sensor resistance R in acetone g.According to the defined formula S=R of sensitivity S a/ R g, just obtain sensor at such a temperature to the sensitivity of 100ppm acetone by calculating.Similarly, repeating said process, just can obtain device sensitivity to 100ppm acetone at different operating temperature by regulating the electric current of Ni-Cr alloy heater strip.Subsequently, the data recorded are processed, just can obtain comparative example and embodiment sensor to the change curve of the sensitivity of 100ppm acetone with working temperature;
Fig. 5: in comparative example and embodiment sensor respectively working temperature be 237.5 DEG C and 287.5 DEG C, under acetone concentration is 20ppm, the response recovery curve of device; Concrete operations are as follows: for embodiment sensor, first sensor is put into gas tank, regulating makes devices function under the working temperature of 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 stablized, device being transferred to another is full of in the gas tank of air, makes it slowly recover, and so just obtains embodiment sensor response recovery curve to 20ppm acetone under the working temperature of 287.5 DEG C.Same method of testing is taked for comparative example sensor, under the working temperature of 237.5 DEG C, just records its response recovery curve.
Fig. 6: the standard working curve of the acetone concentration-sensitivity of sensor in comparative example and embodiment.Sensitivity test method: first sensor is put into gas tank, treats that its resistance is stable and namely obtains the aerial resistance value of sensor and R a; Then using microsyringe in gas cabinet, inject the acetone of 5 ~ 100ppm successively, obtaining the resistance value of sensor in variable concentrations acetone and R by measuring g, according to the defined formula S=R of sensitivity S a/ R g, by calculating the sensitivity of variable concentrations lower sensor, finally obtain the standard working curve of acetone concentration-sensitivity.R is recorded by above-mentioned way during actual measurement a, R g, contrast with the standard working curve of acetone concentration-sensitivity after obtaining Sensitirity va1ue, thus obtain the content of acetone in environment.In addition, as shown in the figure when acetone concentration is within the scope of 100ppm, transducer sensitivity linear better, these features make this kind of acetone sensor can be good at being applied to the detection of acetone gas in commercial production.
As shown in Figure 1, each component names of gas sensor is: Al 2o 3insulating ceramics pipe 1, Ni-Cr alloy heater strip 2, sensitive material 3, annular gold electrode 4, platinum filament 5;
As shown in Figure 2, ZnO/ α-Fe can be found out in (a) figure 2o 3compound is fillet hexahedron structure, and the hexahedral particle diameter of fillet is about 1 ~ 1.2 μm, finds out ZnO/ α-Fe in (b) figure 2o 3heterojunction structure is at α-Fe by growth 2o 3the erose ZnO nano particle that has on fillet hexahedron surface is formed;
As shown in Figure 3, after two step solvent thermal reactions products therefrom XRD spectra in there is α-Fe 2o 3with the characteristic peak of ZnO, interpret sample comprises α-Fe 2o 3and 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 the now sensitivity of device to 100ppm acetone is respectively 6.4 and 29.9;
As shown in Figure 5, when acetone gas concentration is 20ppm, the response time of comparative example is 8s, and the response time of embodiment is then less than 1s.Comparatively speaking, the response speed of embodiment comparatively comparative example be greatly improved;
As shown in Figure 6, when comparative example and embodiment are at working temperature is respectively 237.5 DEG C and 287.5 DEG C, the sensitivity-acetone concentration standard working curve of two class devices.Can significantly find out from figure, the sensitivity of device all increases along with the increase of acetone concentration, wherein the sensitivity of embodiment to 5,10,20,30,40,50,60,70,80,90 and 100ppm acetone 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, 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, embodiment to the sensitivity of acetone comparatively comparative example be greatly improved.
Embodiment
Comparative example 1:
With α-Fe 2o 3fillet hexahedron makes heater-type acetone sensor as sensitive material, and its concrete manufacturing process is as follows:
1. first by the FeCl of 15.0mmol 36H 2the cetyl trimethyl ammonium bromide of O, 3.3mmol and 4.3mmol hexamethylenetetramine join in the mixed solvent that 15mL deionized water and 15mL ethanol prepares successively, after ultrasonic 30 minutes, the experimental drug added all are dissolved.
2. above-mentioned solution being transferred to volume is in the reactor of 40mL, until reactor is tightened airtight after be placed in the electrical heating baking oven of 160 DEG C react 12 hours, make reactor naturally cool to room temperature subsequently and gained precipitation is used ethanol and washed with de-ionized water 5 times respectively, at room temperature just obtaining α-Fe after drying 2o 3fillet hexahedron powder.
3. by the α-Fe of above-mentioned preparation 2o 3powder fully mixes with mass ratio 5:1 with deionized water, thus forms pasty slurry.Then with hairbrush, slurry is coated in the Al of commercially available outside surface with 2 annular gold electrodes equably 2o 3the outside surface of ceramic pipe, forms the sensitive material film that thickness is about 30 μm, and makes sensitive material cover two annular gold electrodes completely.
4. by the Al of coated sensitive material 2o 3ceramic pipe toasts 40 minutes, after sensitive material drying, Al under being placed in infrared lamp 2o 3ceramic pipe is calcined 3 hours at 400 DEG C; Then resistance value is about the Ni-Cr alloy heater coil of 40 Ω through Al 2o 3above-mentioned device, as heater strip, finally carries out welding and encapsulating according to general heater-type gas sensor, thus obtains based on α-Fe by ceramic tube inside 2o 3the hexahedral acetone gas sensor of fillet.
Embodiment 1:
With ZnO/ α-Fe 2o 3compound heterojunction structure makes acetone sensor as sensitive material, its concrete manufacturing process:
1. first by the FeCl of 15.0mmol 36H 2the cetyl trimethyl ammonium bromide of O, 3.3mmol and 4.3mmol hexamethylenetetramine join in the mixed solvent that 15mL ionized water and 15mL ethanol prepares successively, after ultrasonic 30 minutes, the experimental drug added all are dissolved.
2. above-mentioned solution being transferred to volume is in the reactor of 40mL, until reactor is tightened airtight after be placed in the electrical heating baking oven of 160 DEG C react 12 hours, make reactor naturally cool to room temperature subsequently and gained precipitation is used ethanol and washed with de-ionized water 5 times respectively, finally just obtaining α-Fe after at room temperature drying 2o 3fillet hexahedron powder.
3. get the above-mentioned α of 40mg-Fe 2o 3powder joins in the ethylene glycol solvent of 10mL, within ultrasonic 15 minutes, makes α-Fe 2o 3fillet hexahedron powder is dispersed in ethylene glycol completely; Then Zn (the NO of 55mg is added 3) 26H 2o, stirred at ambient temperature 20 minutes, treats Zn (NO 3) 26H 2after O dissolves completely, configured solution being transferred to volume is in the reactor of 40mL, reacts 12 hours at 180 DEG C, is cooled to by the precipitate with deionized water that generates and ethanol repeatedly eccentric cleaning after room temperature, and at room temperature dry, thus obtains ZnO/ α-Fe 2o 3composite oxide semiconductor;
4. by the ZnO/ α-Fe of above-mentioned preparation 2o 3composite powder fully mixes with mass ratio 5:1 with deionized water, thus forms pasty slurry.Then with hairbrush, slurry is coated in the Al of commercially available outside surface with 2 annular gold electrodes equably 2o 3the outside surface of ceramic pipe, forms the sensitive material film that thickness is about 30 μm, and makes sensitive material cover two annular gold electrodes completely.
5. by the Al of coated sensitive material 2o 3ceramic pipe toasts 40 minutes, after sensitive material drying, Al under being placed in infrared lamp 2o 3ceramic pipe is calcined 3 hours at 400 DEG C; Then resistance value is about the Ni-Cr alloy heater coil of 40 Ω through Al 2o 3above-mentioned device, as heater strip, finally carries out welding and encapsulating according to general heater-type gas sensor by ceramic tube inside, thus obtains base ZnO/ α-Fe 2o 3the acetone gas sensor of compound heterojunction structure.

Claims (4)

1. one kind based on ZnO/ α-Fe 2o 3the acetone gas sensor of composite oxide semiconductor is by the Al of outside surface with 2 annular gold electrodes (4) 2o 3insulating ceramics pipe (1), through Al 2o 3the Ni-Cr alloy heater strip (2) that insulating ceramics pipe (1) is inner and the sensitive material (3) be coated on insulating ceramics pipe (1) outside surface and annular gold electrode (4) are formed, and each annular gold electrode (4) are connected to a pair platinum filament (5) simultaneously; It is characterized in that: sensitive material (3) is ZnO/ α-Fe 2o 3composite oxide semiconductor sensitive material, it is prepared by following steps,
1. first by the FeCl of 12.5 ~ 17.5mmol 36H 2the cetyl trimethyl ammonium bromide of O, 2.3 ~ 4.1mmol and the hexamethylenetetramine of 3.5 ~ 5.3mmol join in the mixed solvent of deionized water and ethanol successively, ultrasonicly make dissolving;
2. above-mentioned solution is transferred in reactor, airtight being placed in the baking oven of 140 ~ 160 DEG C is reacted 12 ~ 14 hours, make reactor naturally cool to room temperature subsequently, then gained precipitation is used ethanol and washed with de-ionized water respectively, finally obtain α-Fe after at room temperature drying 2o 3powder;
3. α-the Fe of 35 ~ 55mg is got 2o 3powder joins in 10 ~ 15mL ethylene glycol, ultrasonicly makes α-Fe 2o 3disperse completely, then add the Zn (NO of 50 ~ 70mg 3) 26H 2o, stirs and makes Zn (NO 3) 26H 2o dissolves completely;
4. above-mentioned mixing material is poured in reactor, react 12 ~ 14 hours at 180 ~ 200 DEG C, to be cooled to the precipitate with deionized water that generates and ethanol eccentric cleaning after room temperature, under room temperature, after drying, to obtain the ZnO/ α-Fe of heterojunction structure 2o 3composite semiconductor oxide powder.
2. as claimed in claim 1 a kind of based on ZnO/ α-Fe 2o 3the acetone gas sensor of composite oxide semiconductor, is characterized in that: ZnO/ α-Fe 2o 3composite oxide semiconductor is fillet hexahedron structure, and the hexahedral particle diameter of fillet is 1 ~ 1.2 μm, ZnO/ α-Fe 2o 3heterojunction structure is at α-Fe by growth 2o 3the erose ZnO nano particle that has on fillet hexahedron surface is formed, ZnO/ α-Fe 2o 3the thickness of composite oxide semiconductor sensitive material is 10 ~ 30 μm.
3. as claimed in claim 1 a kind of based on ZnO/ α-Fe 2o 3the acetone gas sensor of composite oxide semiconductor, is characterized in that: step 1. in the volume of mixed solvent be 30mL, the volume ratio of deionized water and ethanol is 1:2 ~ 1:1.
4. the one of claims 1 to 3 described in any one is based on ZnO/ α-Fe 2o 3the preparation method of the acetone gas sensor of composite oxide semiconductor, its step is as follows:
1. by ZnO/ α-Fe 2o 3composite semiconductor oxide powder fully mixes with mass ratio 4:1 ~ 6:1 with deionized water, forms pasty slurry, then slurry is coated in equably the Al of outside surface with 2 annular gold electrodes (4) 2o 3ceramic pipe (1) surface, forms the sensitive material (3) that thickness is 10 ~ 30 μm, and makes sensitive material cover annular gold electrode (4) completely;
2. by the Al of coated sensitive material 2o 3ceramic pipe (1) toasts 30 ~ 45 minutes, after sensitive material drying, Al under being placed in infrared lamp 2o 3ceramic pipe (1) is calcined 2 ~ 3 hours at 400 ~ 450 DEG C; Then be that the Ni-Cr alloy heater coil of 30 ~ 40 Ω is through Al by resistance value 2o 3ceramic pipe (1) is inner as heater strip, is finally carried out welding and encapsulating according to general heater-type gas sensor by above-mentioned device, thus obtains based on ZnO/ α-Fe 2o 3the acetone gas sensor of composite oxide semiconductor.
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CN106745315A (en) * 2017-02-22 2017-05-31 济南大学 A kind of method of the growth in situ Fe2O3 nanoneedles on earthenware
CN106745315B (en) * 2017-02-22 2018-06-26 济南大学 A kind of method of the growth in situ Fe2O3 nanoneedles on ceramic tube
CN109975367A (en) * 2019-03-11 2019-07-05 陕西科技大学 The WO less than 60nm based on the modification of Ag quantum dot3-SnO2Solid nanospheres acetone sensor and preparation method
CN109781797A (en) * 2019-03-13 2019-05-21 珠海格力电器股份有限公司 TVOC gas sensing devices, air processor

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