CN104569081A - Ethanol gas sensor based on In2O3 microflower/SnO2 nanoparticle composite material and preparation method of sensor - Google Patents
Ethanol gas sensor based on In2O3 microflower/SnO2 nanoparticle composite material and preparation method of sensor Download PDFInfo
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- CN104569081A CN104569081A CN201510057920.1A CN201510057920A CN104569081A CN 104569081 A CN104569081 A CN 104569081A CN 201510057920 A CN201510057920 A CN 201510057920A CN 104569081 A CN104569081 A CN 104569081A
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Abstract
The invention discloses an ethanol gas sensor based on an In2O3 microflower/SnO2 nanoparticle composite material and a preparation method of the sensor, belonging to the technical field of gas sensors. The ethanol gas sensor consists of a nickel-cadmium alloy heating coil, an alumina ceramic tube, a platinum wire, a gold electrode and an In2O3 microflower/SnO2 nanoparticle composite material. By utilizing the catalytic activity of SnO2 on In2O3, the oxidative activity of the material is improved, so that the sensitivity of the sensor is greatly improved, materials with morphology are directly mixed at the first time, the large specific surface area of the material is utilized, and the catalytic characteristics between oxides are utilized. According to the material, ethanol gas molecules are transported on the surface and have the characteristics of rapid adsorption and desorption, so that the response and recovery speed of the sensor is increased. Compared with an ethanol sensor manufactured by In2O3 microflowers which are not compounded with SnO2 nanoparticles, the ethanol sensor disclosed by the invention has the advantages that the sensitivity is greatly improved, and the sensitivity of the ethanol sensor disclosed by the invention is about 9.5 times that of the sensitivity of the ethanol sensor manufactured by In2O3 microflowers.
Description
Technical field
The invention belongs to gas sensor technical field, be specifically related to a kind of based on In
2o
3micro-flowers/SnO
2alcohol gas sensor of nano composition and preparation method thereof.
Background technology
Organic steam refers to the gas containing class organic compounds such as aromatic hydrocarbon, nitro hydrocarbon, halogenated hydrocarbons, long chain alkane, alcohol, ether, ketone, fat, hydrazines, is all poisonous, flammable explosive gas substantially.For harm humans existence and healthy gas, namely they can produce harmful effect to human body once exceed safe level.Ethanol is important industrial chemicals and solvent, volatile inflammable, in production and use procedure, if misoperation and cause a large amount of ethanol evaporation or leakage, can cause burning or explosion accident, causes damage to country and individual life and property safety.Most people has the custom of drinking, but if drink beyond one's capacity, the control ability of people can be made to decline, gently then forget oneself, heavy then can cause actual bodily harm, even dead.If driver indulges in excessive drinking and causes traffic hazard, the life security of more people will be injured and cause damage.Therefore, all need easy to carry, cheap, that sensitive property is good alcohol sensitive element in various public place, traffic department, automobile industry, chemical plant, food factory, Soft Drinks Plant etc., development research have high sensitivity and optionally low-concentration ethanol sensor just have very important meaning.
After from the sixties in 20th century, people utilize metal-oxide semiconductor (MOS) to develop combustible gas sensor, oxide gas sensor just obtains and develops rapidly.In recent years, the emphasis of sensor development improves the sensitivity of gas sensor, stability, selectivity enlargement gas sensing range under concentrating on and considering response time, cost of manufacture and the prerequisite in guarantee life-span.Concerning a gas sensor, the key of its excellent performance depends on the quality of gas sensitive, and gas-sensitive reaction is the gas one liquid/solid interface reaction occurring in semiconductor surface, therefore, the modification doping of the composition structure of gas sensitive, microscopic appearance and the surface mass with catalytic activity often becomes the most critical factor determining gas sensor performance.Research shows, modification can be carried out to gas sensor by the adulterate method of another kind of metal oxide of finishing, improve the selectivity of gas sensor, working temperature can be reduced simultaneously, the thermal stability of raising sensitivity, gas sensitive and long-time stability, reduce response time and release time.
Summary of the invention
The object of the invention is to develop high sensitivity and high selectivity based on In
2o
3micro-flowers/SnO
2alcohol gas sensor of nano composition and preparation method thereof, and a kind of novel In is provided
2o
3micro-flowers/SnO
2the formation method of nano composition.
Sensor involved in the present invention adopts heater-type structure, by outside surface with 2 parallel to each other and discrete ring-type gold electrodes insulating oxide aluminium ceramic pipe substrate, be coated in the metal oxide semiconductor gas sensitive material on insulating oxide aluminium ceramic pipe outer substrate surface and gold electrode and the nickel-chrome heater coil be placed in insulating ceramics pipe forms, all with platinum filament wire on each gold electrode; It is characterized in that: metal oxide semiconductor gas sensitive material is In
2o
3micro-flowers/SnO
2nano composition, it is prepared by following steps:
(1) 0.36 ~ 0.40g In (NO is taken
3)
34.5H
2o, 0.14g ~ 0.16g urea, is dissolved in 34 ~ 38mL deionized water, and stirred at ambient temperature is until clarification, moved in water heating kettle by gained solution, water heating kettle capacity is 50mL, 140 ~ 180 DEG C of reaction 2 ~ 5h, after being cooled to room temperature, being precipitated by centrifugal, namely obtaining In
2o
3micro-flowers precursor;
(2) 0.5g ~ 0.6SnCl is taken
45H
2o, 0.5 ~ 0.7g CTAB (cetyl trimethyl ammonium bromide) and 0.150.3g HMT (urotropine), be dissolved in (deionized water mixes with absolute ethyl alcohol, and deionized water and absolute ethyl alcohol are 20mL) in 40mL solvent, stirred at ambient temperature is until clarification, gained solution is moved in water heating kettle, water heating kettle capacity is 50mL, and 160 ~ 200 DEG C of reaction 2 ~ 4h, after being cooled to room temperature, be precipitated by centrifugal, namely obtain SnO
2precursor of Nano Particles;
(3) by gained two kinds of precursors, calcine 2 ~ 4h at 450 ~ 500 DEG C, namely obtain In
2o
3micro-flowers and SnO
2nano particle;
(4) by In
2o
3micro-flowers and SnO
2nano particle according to certain mass than ultrasonic mixing, SnO in potpourri
2massfraction is 30% ~ 45%, namely obtains In
2o
3micro-flowers/SnO
2nano composition, carries out during mixing under ultrasonic environment, with make mixing evenly, more disperse.
Operationally, nickel-chrome heater coil passes to direct current to provide working temperature to sensor, realizes by the resistance measuring direct current resistance between two gold electrodes in different atmosphere the function measuring ethanol vapor concentration (100ppm ~ 1000ppm).Sensitivity be namely by the ratio calculation of the resistance of device in the resistance of device in air and alcohol vapour out.Ethanol gas concentration is larger, and the sensitivity that sensor measurement obtains is higher.Utilize In
2o
3micro-flowers and SnO
2nano particle mass ratio is the In of 2:1 compound
2o
3micro-flowers/SnO
2nano composition, optimum working temperature is about 250 DEG C, and at this temperature, for the ethanol of 100ppm, sensitivity can reach 53.2, compared to not with SnO
2the In of Nanocomposites
2o
3the ethanol sensor sensitivity that micro-flowers makes significantly improves, and the former sensitivity is about 9.5 times of the latter.
Sensitive element each portion major parameter is:
The internal diameter of insulating oxide aluminium ceramic pipe substrate is 1.5 ~ 1.8mm, and external diameter is 2.2 ~ 2.5mm, and length is 4 ~ 5mm; It carries two ring-type gold electrodes be parallel to each other, single electrode width is 0.6 ~ 0.8mm, and two electrode separations are 0.8 ~ 1.2mm; The platinum filament conductor length that gold electrode is drawn is 4 ~ 6mm; The number of turn of nickel-chrome heater coil is 50 ~ 60 circles, and resistance is 30 ~ 40 Ω.
In
2o
3micro-flowers/SnO
2nano composition is as sensitive material, and be attached to the outside surface of insulating oxide aluminium ceramic pipe substrate, its thickness is about 400 ~ 500 μm.
The hydrothermal method adopted in the present invention mainly comprises the following steps, first prepare precursor liquid, subsequently precursor liquid is poured in water heating kettle, under uniform temperature after reaction, to room temperature, also standing a period of time makes product precipitate to cooling water heat still, removes supernatant and namely obtains hydrothermal product.
Based on In in the present invention
2o
3micro-flowers/SnO
2the method for making of the alcohol gas sensor of nano composition is:
(1) by In
2o
3micro-flowers/SnO
2nano composition 10 ~ 15mg mixes with removing absolute ethyl alcohol 0.5 ~ 1mL, even furnishing slurry;
(2) above-mentioned slurry is coated in equably the surface of insulating oxide aluminium ceramic pipe substrate and gold electrode, dry 2 ~ 3h, In after dry under infrared lamp
2o
3micro-flowers/SnO
2the thickness of nano composition film is 400 ~ 500 μm, then at 400 ~ 500 DEG C, sinters 2 ~ 4h;
(3) finally by device in 200 ~ 400 DEG C of air ambients aging 5 ~ 7 days, namely prepare based on In
2o
3micro-flowers/SnO
2the alcohol gas sensor of nano composition.
Principle of work:
Work as In
2o
3micro-flowers/SnO
2when nano composition alcohol gas sensor is placed in air, adsorb oxygen molecules at sensor surface, and by from In
2o
3micro-flowers/SnO
2the electron ionization of nano composition conduction band forms negative oxygen ion (O
2 -, O
-, or O
2-).In this process, oxygen to reduce by instigator's sensor electronic concentration as electronics and resistance raises.When sensor contacts alcohol gas under certain suitable temperature, the negative oxygen ion adsorbed with sensor surface reacts (see formula 1) by alcohol gas molecule, causes the electronics by negative oxygen ion is caught again to be discharged into In
2o
3micro-flowers/SnO
2in nano composition conduction band, thus reduce measuring resistance.The change of resistivity of material is converted into the measured termination of electric signal by sensor and receives, thus reaches the object detecting ethanol.
C
2H
5OH+O
S -→CH
3CHO+H
2O+e
-
Advantage of the present invention:
(1) In for preparing of the present invention
2o
3micro-flowers/SnO
2nano composition has larger BET specific surface area (34.4m
2/ g), homogeneous Size Distribution, for this ethanol sensor provides a kind of effective sensitive material; The preparation method's step adopted is simple, and do not need expensive equipment, cost is low.
(2) the present invention's profit SnO
2nano particle is as bulk gas sensitive material In
2o
3catalyzer, improve the oxidation activity of material, transducer sensitivity is significantly improved, and as described embodiments, sensitivity is promoted to 53.2 by original 5.6, improves multiple and is about 8.5 times.
(3) the present invention utilizes In
2o
3micro-flowers/SnO
2nano composition is conducive to alcohol gas molecule at its surface delivery, can the characteristic of quick adsorption and desorption, makes that sensor responds, resume speed is accelerated.
(4) In of the present invention's making
2o
3micro-flowers/SnO
2nano composition alcohol gas sensor compact conformation, maximally utilizes the heat energy of heater strip all directions, improves heat utilization rate.
(5) In of the present invention's making
2o
3micro-flowers/SnO
2nano composition alcohol gas sensor manufacture craft is simple, cheap and be applicable to industrial batch production.
Accompanying drawing explanation
Fig. 1 is In of the present invention
2o
3micro-flowers/SnO
2nano particle SEM schemes (c figure) and independent SnO
2nano particle, In
2o
3micro-flowers SEM schemes (a figure and b figure).
Fig. 2 is of the present invention based on In
2o
3micro-flowers/SnO
2the structural representation of nano particle alcohol gas sensor.
Fig. 3 is In
2o
3micro-flowers/SnO
2nanocomposites structure alcohol gas sensor (S1 type), SnO
2nano particle alcohol gas sensor (S0 type) and In
2o
3micro-flowers alcohol gas sensor is at the temperature variant histogram of 100ppm alcohol atmosphere medium sensitivity.
Fig. 4 is In
2o
3micro-flowers/SnO
2nanocomposites structure alcohol gas sensor (S1 type) under 250 DEG C of working temperatures, to the acetone gas change of sensitivity curve of variable concentrations.
As In in Fig. 1
2o
3micro-flowers/SnO
2nano composition and independent SnO
2nano particle, In
2o
3shown in micro-flowers SEM figure, at In
2o
3micro-flowers and SnO
2after nano particle bi-material compound, not there is significant change in material surface pattern, but permeability is better, and bi-material defines heterojunction, is conducive to the raising of transducer sensitivity.
As shown in Figure 2, In
2o
3micro-flowers/SnO
2the each component names of Nanocomposites structure alcohol gas sensor is: nickel-cadmium heater coil 1, platinum filament (four) 2, gold electrode (two) 3, insulating oxide aluminium ceramic pipe substrate 4, In
2o
3micro-flowers/SnO2 nano composition 5.
As shown in Figure 3, for the sensitivity of comparative example and embodiment S0, S1, S2 type ethanol sensor is with the change of senor operating temperature, as can be seen from the figure, In2O3 micro-flowers/SnO2 nano composition, compared to SnO
2the sensitivity of nano particle ethanol sensor has and significantly improves, and under device 250 DEG C of working temperatures, the former sensitivity is about 9.5 times of the latter.
As shown in Figure 4, the change curve of sensitivity under the alcohol atmosphere of variable concentrations of S1 type ethanol sensor.As can be seen from the figure along with the concentration detecting gas acetone increases, the sensitivity of sensor increases, and moves closer to saturated at more than 500ppm, and under the alcoholic environment of 100ppm, corresponding sensitivity is 53.2.
Embodiment
Comparative example 1
With In
2o
3micro-flowers, as gas sensitive material, makes S0 type ethanol sensor, its concrete manufacturing process:
1) 0.381g In (NO is taken
3)
34.5H
2o, 0.15g urea, is dissolved in 36mL deionized water, and gained solution, until clarification, moves in water heating kettle by stirred at ambient temperature, and 160 DEG C of reaction 4h, take out precipitation after cooling a period of time, namely obtain In
2o
3micro-flowers precursor.
2) above-mentioned (1) gained precursor is placed in silica crucible, is placed in muffle furnace and sinters 2h with 500 DEG C, obtain In
2o
3micro-flowers.
3) by In in above-mentioned (2)
2o
3micro-flowers and absolute ethyl alcohol 0.25 mix furnishing slurry by volume.Slurry is coated in equably on the alumina ceramic tube with gold electrode, covers whole electrode, be coated with slurry thickness and be about 400 μm, dry 2h under infrared lamp.Drying is placed in muffle furnace with 500 DEG C of sintering 2h.NI-G heater coil resistance being about 40 Ω (number of turn is 60 circles) is interior as well heater through pipe, weld with heater-type hexagonal base by the platinum filament wire on alumina ceramic tube and through the heater strip of tube chamber, encapsulate, at 400 DEG C aging 7 days, obtained S0 type alcohol gas sensor.
Comparative example 2
With SnO
2nano particle, as gas sensitive material, makes S2 type ethanol sensor, its concrete manufacturing process:
1) 0.526g SnCl is taken
45H
2o, 0.6g CTAB (cetyl trimethyl ammonium bromide) and 0.2gHMT (urotropine), be dissolved in (deionized water and each 20mL of absolute ethyl alcohol) in 40mL solvent, stirred at ambient temperature is until clarification, gained solution is moved in water heating kettle, 200 DEG C of reaction 4h, take out precipitation after cooling a period of time, namely obtain SnO
2precursor of Nano Particles.
2) above-mentioned (1) gained precursor is placed in silica crucible, is placed in muffle furnace and sinters 2h with 500 DEG C, obtain SnO
2nano particle.
3) by SnO in above-mentioned (2)
2nano particle and absolute ethyl alcohol 0.25 mix furnishing slurry by volume.Slurry is coated in equably on the alumina ceramic tube with gold electrode, covers whole electrode, be coated with slurry thickness and be about 400 μm, dry 2h under infrared lamp.Drying is placed in muffle furnace with 500 DEG C of sintering 2h.NI-G heater coil resistance being about 40 Ω (number of turn is 60 circles) through in pipe as well heater, weld with base by the platinum filament wire on alumina ceramic tube and through the heater strip of tube chamber, encapsulate, at 400 DEG C aging 7 days, obtain S2 type SnO
2nanofiber semiconductor acetone gas sensor.
Embodiment 1
With In
2o
3micro-flowers and SnO
2nano particle mass ratio is the In of 2:1 compound
2o
3micro-flowers/SnO
2nano composition is as gas sensitive material, and make S1 type acetone sensor, its manufacturing process is:
(1) 0.526g SnCl is taken
45H
2o, 0.6g CTAB (cetyl trimethyl ammonium bromide) and 0.2gHMT (urotropine), be dissolved in (deionized water and each 20mL of absolute ethyl alcohol) in 40mL solvent, stirred at ambient temperature is until clarification, gained solution is moved in water heating kettle, 200 DEG C of reaction 4h, take out precipitation after cooling a period of time, namely obtain SnO
2precursor of Nano Particles.
(2) 0.381g In (NO is taken
3)
34.5H
2o, 0.15g urea, is dissolved in 36mL deionized water, and gained solution, until clarification, moves in water heating kettle by stirred at ambient temperature, and 160 DEG C of reaction 4h, take out precipitation after cooling a period of time, namely obtain In
2o
3micro-flowers precursor.
(3) by above-mentioned (1), (2) gained precursor under ultrasound environments with In
2o
3micro-flowers and SnO
2nano particle mass ratio is 2:1 dry mixed, obtains In
2o
3micro-flowers/SnO
2nano composition.
(4) by In in above-mentioned (3)
2o
3micro-flowers/SnO
2nano composition and absolute ethyl alcohol 0.25 mix furnishing slurry by volume.Slurry is coated in equably on the alumina ceramic tube with gold electrode, covers whole electrode, be coated with slurry thickness and be about 400 μm, dry 2h under infrared lamp.Drying is placed in muffle furnace with 500 DEG C of sintering 2h.NI-G heater coil resistance being about 40 Ω (number of turn is 60 circles) is interior as well heater through pipe, weld with base by the platinum filament wire on alumina ceramic tube and through the heater strip of tube chamber, encapsulate, at 400 DEG C aging 7 days, obtained S1 type alcohol gas sensor.
List with In in table 1
2o
3micro-flowers and SnO
2nano particle mass ratio is the In of 2:1 compound
2o
3micro-flowers/SnO
2nano composition as the S1 type alcohol gas sensor of gas sensitive material, not with SnO
2the In of Nanocomposites
2o
3micro-flowers as the S0 type ethanol sensor of sensitive material, and not with In
2o
3the SnO of micro-flowers compound
2nano particle as the S2 type ethanol sensor of gas sensitive material in 100ppm alcohol atmosphere, sensitivity variation with temperature value.
Table 1. three kinds of ethanol sensors are in 100ppm alcohol atmosphere, and sensitivity is with the change of senor operating temperature
Claims (5)
1. one kind based on In
2o
3micro-flowers/SnO
2the alcohol gas sensor of nano composition, by outside surface with 2 parallel to each other and discrete ring-type gold electrodes insulating oxide aluminium ceramic pipe substrate, be coated in the metal oxide semiconductor gas sensitive material on insulating oxide aluminium ceramic pipe outer substrate surface and gold electrode and the nickel-chrome heater coil be placed in insulating ceramics pipe forms, all with platinum filament wire on each gold electrode; It is characterized in that: metal oxide semiconductor gas sensitive material is In
2o
3micro-flowers/SnO
2nano composition, it is prepared by following steps:
(1) 0.36 ~ 0.40g In (NO is taken
3)
34.5H
2o, 0.14g ~ 0.16g urea, is dissolved in 34 ~ 38mL deionized water, and gained solution, until clarification, moves in water heating kettle by stirred at ambient temperature, and 140 ~ 180 DEG C of reaction 2 ~ 5h, after being cooled to room temperature, being precipitated by centrifugal, namely obtaining In
2o
3micro-flowers precursor;
(2) 0.5g ~ 0.6SnCl is taken
45H
2o, 0.5 ~ 0.7g CTAB (cetyl trimethyl ammonium bromide) and 0.150.3g HMT (urotropine), being dissolved in 40mL volume ratio is in the deionized water of 1:1 and the mixed solvent of absolute ethyl alcohol, stirred at ambient temperature is until clarification, moved into by gained solution in water heating kettle, 160 ~ 200 DEG C of reaction 2 ~ 4h, after being cooled to room temperature, be precipitated by centrifugal, namely obtain SnO
2precursor of Nano Particles;
(3) calcine 2 ~ 4h by gained two kinds of precursors 450 ~ 500 DEG C, namely obtain In
2o
3micro-flowers and SnO
2nano particle;
(4) by In
2o
3micro-flowers and SnO
2nano particle according to certain mass than ultrasonic mixing, SnO in potpourri
2massfraction is 30% ~ 45%, namely obtains In
2o
3micro-flowers/SnO
2nano composition.
2. as claimed in claim 1 a kind of based on In
2o
3micro-flowers/SnO
2the alcohol gas sensor of nano composition, is characterized in that: the internal diameter of tubular ceramic substrate is 1.5 ~ 1.8mm, and external diameter is 2.2 ~ 2.5mm, and length is 4 ~ 5mm; The single electrode width of ring-type gold electrode is 0.6 ~ 0.8mm, and two electrode separations are 0.8 ~ 1.2mm; The platinum filament conductor length that gold electrode is drawn is 4 ~ 6mm.
3. as claimed in claim 1 a kind of based on In
2o
3micro-flowers/SnO
2the alcohol gas sensor of nano composition, is characterized in that: the number of turn of nickel-chrome heater coil is 50 ~ 60 circles, and resistance is 30 ~ 40 Ω.
4. as claimed in claim 1 a kind of based on In
2o
3micro-flowers/SnO
2the alcohol gas sensor of nano composition, is characterized in that: In
2o
3micro-flowers/SnO
2the thickness of nano composition is 400 ~ 500 μm.
5. one according to claim 1 is based on In
2o
3micro-flowers/SnO
2the preparation method of the alcohol gas sensor of nano composition, its step is as follows:
1) by In
2o
3micro-flowers/SnO
2nano composition 10 ~ 15mg mixes with removing absolute ethyl alcohol 0.5 ~ 1mL, even furnishing slurry;
2) above-mentioned slurry is coated in equably the surface of insulating oxide aluminium ceramic pipe substrate and gold electrode, under infrared lamp, dry 2 ~ 3h, then sinters 2 ~ 4h at 400 ~ 500 DEG C;
3) finally by device in 200 ~ 400 DEG C of air ambients aging 5 ~ 7 days, namely prepare based on In
2o
3micro-flowers/SnO
2the alcohol gas sensor of nano composition.
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| CN113281383B (en) * | 2021-05-24 | 2024-04-12 | 安徽大学绿色产业创新研究院 | Ethanol gas sensor of heterojunction composite material and preparation method thereof |
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| CN108508062A (en) * | 2018-03-27 | 2018-09-07 | 吉林大学 | One kind being based on MoO3The triethylamine sensor of nano sensitive material, preparation method and applications |
| CN109781800A (en) * | 2019-01-25 | 2019-05-21 | 青岛大学 | A kind of gas sensor and preparation method thereof based on metal molybdate nanocomposite |
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| CN109799270A (en) * | 2019-02-18 | 2019-05-24 | 蔡涛 | Sensitive membrane capable of effectively improving response performance to ethanol gas |
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