CN104749225A - ZnO/ZnFe2O4 composite sensitive material, preparation method thereof and application of ZnO/ZnFe2O4 composite sensitive material in acetone gas sensor - Google Patents

ZnO/ZnFe2O4 composite sensitive material, preparation method thereof and application of ZnO/ZnFe2O4 composite sensitive material in acetone gas sensor Download PDF

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CN104749225A
CN104749225A CN201510193771.1A CN201510193771A CN104749225A CN 104749225 A CN104749225 A CN 104749225A CN 201510193771 A CN201510193771 A CN 201510193771A CN 104749225 A CN104749225 A CN 104749225A
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sensitive material
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CN104749225B (en
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卢革宇
李晓伟
孙鹏
刘凤敏
孙彦峰
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Jilin University
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Abstract

The invention belongs to the technical field of metal-oxide gas sensors, and particularly relates to design and synthesis of a composite sensitive material ZnO/ZnFe2O4, and an application of the composite sensitive material ZnO/ZnFe2O4 in an acetone gas sensor. In the preparation and preparation processes of the sensitive material, ZnO hollow microspheres are successfully synthesized first by adopting a microwave heating technology, and then a layer of ZnFe2O4 nanosheets grow on the surfaces of the ZnO hollow microspheres by adopting an epitaxial growth method. The whole synthesis process is simple, highly-efficient, energy-saving and suitable for large-scale production. Compared with ZnO hollow microspheres with a single component, the ZnO gas sensor modified by the ZnFe2O4 nanosheets shows more excellent gas sensitivity to acetone. In addition, the gas sensor of this type is small in size, and low in cost, so that the gas sensor based on the ZnO/ZnFe2O4 heterostructure is more applicable to monitoring acetone gas.

Description

ZnO/ZnFe 2o 4composite sensitive material, preparation method and the application in acetone gas sensor
Technical field
The invention belongs to metal-oxide gas transducer technical field, be specifically related to ZnO/ZnFe 2o 4composite sensitive material, preparation method and the application in acetone gas sensor.
Background technology
Along with constantly weeding out the old and bring forth the new of sensitive material, various gas sensitive material is successively developed.In numerous gas sensitive material, due to metal-oxide semiconductor (MOS) have highly sensitive, preparation cost is low, asepsis environment-protecting, be easy to the advantage such as integrated, is considered to a kind of gas sensitive having application prospect most.Therefore, in the last few years, metal oxide received and paid close attention to widely and the development obtained energetically.According to the kind of majority carrier, metal-oxide semiconductor (MOS) can be divided into N-shaped sensitive material (as In 2o 3, SnO 2, ZnO, Fe 2o 3, WO 3deng) and p-type sensitive material (as NiO, Co 3o 4, CuO etc.).Although the gas sensor based on above-mentioned metal oxide obtains some application, due to the physicochemical property that himself is limited, the metal-oxide semiconductor (MOS) of these one-components is relied on to be difficult to obtain the further raising of gas-sensitive property.In this case, sensitive material is expanded to multi-component heterojunction structure from the metal oxide of one-component and seem particularly important.Synergy between the chemical composition adjustable due to it and heterogeneity, heterojunction structure often can show outstanding gas sensitization characteristic.
Especially, zinc paste (ZnO) is widely used in detecting CO, NH as one typical N-shaped oxide semiconductor sensitive material 3, in NOx and various poisonous and hazardous escaping gas.But, exactly because ZnO is more responsive to a lot of gas, so the selectivity of ZnO is poor, be difficult to distinguish different types of gas exactly.In recent years, spinel-type ternary metal oxide zinc ferrite (ZnFe is reported 2o 4) extraordinary selectivity and susceptibility can be shown to some specific gas.If can by ZnO and ZnFe 2o 4combine, perhaps can improve the selectivity of ZnO to gas to be measured.Realize above-mentioned guess to verify, what first needed is prepare homogeneous ZnO/ZnFe 2o 4heterojunction structure.
At present, the preparation method of heterojunction structure has a lot, mainly contains sol-gal process, chemical vapour deposition technique (CVD), supersonic spraying, water/solvent-thermal method and method of electrostatic spinning etc.But these synthetic methods above-mentioned all exist much serious deficiency in actual applications, such as, the experiment condition of loaded down with trivial details running program, tediously long course of reaction, a large amount of energy resource consumptions and harshness.These deficiencies greatly govern their application and development.Therefore, in order to explore the relation between material structure and gas-sensitive property, the preparation method finding a kind of simple and effective heterojunction structure still tool is of great significance.
Summary of the invention
The object of this invention is to provide a kind of composite sensitive material ZnO/ZnFe that can be used in acetone gas sensor 2o 4.
ZnO/ZnFe of the present invention 2o 4composite sensitive material is a kind of by ZnO hollow microsphere with at its epontic ZnFe 2o 4the heterojunction structure that nanometer sheet is formed; The external diameter of ZnO hollow microsphere is 2 ~ 4 μm, and internal diameter is 1 ~ 2.5 μm; Single ZnFe 2o 4the thickness of nanometer sheet is 8 ~ 15nm, at the epontic ZnFe of ZnO hollow microsphere 2o 4the thickness of nanoscale twins is 80 ~ 150nm.
The present invention, first using zinc acetate, trisodium citrate and ammoniacal liquor as raw material, utilizes Microwave-assisted synthesis method successfully to prepare ZnO hollow microsphere in 30 ~ 40min; Then at room temperature, by ZnFe 2o 4the surface that nanometer sheet grows into ZnO hollow microsphere forms ZnO/ZnFe 2o 4composite sensitive material; Finally, above-mentioned ZnO/ZnFe is utilized 2o 4composite sensitive material constructs acetone gas sensor.ZnO/ZnFe of the present invention 2o 4the concrete preparation method of composite sensitive material is as follows:
The preparation of 1.ZnO hollow microsphere
1. 0.8 ~ 1.2g Zinc diacetate dihydrate (Zn (CH is taken successively 3cOO) 22H 2o) and 0.03 ~ 0.08g bis-citric acid monohydrate trisodium (Na 3c 6h 5o 72H 2o) join in 150 ~ 220mL deionized water, be stirred to dissolve completely, form clear transparent solutions, then measure 4 ~ 6mL ammoniacal liquor (30wt%) and join in above-mentioned solution, stir 5 ~ 10min;
2. utilize microwave that reaction solution is heated to 75 ~ 95 DEG C, then keep 10 ~ 60min, microwave heating power is 200 ~ 500W;
3., after question response terminates, the white precipitate deionized water of gained and ethanol alternating centrifugal are washed 5 ~ 8 times, washes the survivor ion in reaction solution off, the product after washing is dry under 60 ~ 80 DEG C of conditions, thus obtain ZnO hollow microsphere;
2.ZnO/ZnFe 2o 4the preparation of composite sensitive material
1. getting 40 ~ 60mg ZnO hollow microsphere joins in 40 ~ 50mL deionized water, and ultrasonic 1 ~ 5min makes ZnO hollow microsphere disperse completely;
2. by the FeSO of 2 ~ 6mL, 0.3 ~ 0.8M 4solution is slowly added drop-wise in above-mentioned dispersion liquid, stirred at ambient temperature 5 ~ 10min, the product deionized water obtained and ethanol alternating centrifugal is washed 5 ~ 8 times; Then dry at 60 ~ 80 DEG C, finally calcine 2 ~ 5 hours under 400 ~ 500 DEG C of conditions, thus obtain ZnO/ZnFe 2o 4composite sensitive material;
3. the making of acetone gas sensor
1. with Al 2o 3ceramic pipe is substrate, ceramic pipe range 2 ~ 6mm, internal diameter 0.6 ~ 0.9mm, external diameter 1 ~ 1.2mm, and every one end of ceramic pipe outside surface is respectively with a ring-type gold electrode, and the width of gold electrode is 0.5 ~ 0.8mm, each gold electrode is all connected with two Pt silks and makes pin;
2. by 15 ~ 40mg ZnO/ZnFe 2o 4composite sensitive material mixes with 100 ~ 500 μ L deionized waters, and grinding obtains the slurry of modest viscosity gently, then with fine, soft fur brush, above-mentioned slurry is coated in Al 2o 3the outside surface of ceramic pipe substrate, coating thickness is 10 ~ 30 μm, the Al after coating 2o 3the outside surface of ceramic pipe substrate and ring-type gold electrode are completely by ZnO/ZnFe 2o 4composite sensitive material covers, and only reserves pin;
3. under ceramic pipe being placed on infrared lamp, baking 20 ~ 30min carries out post bake, then calcine 2 ~ 4 hours under placing it in 400 ~ 500 DEG C of conditions, until naturally after cooling, the nickel-chrome heater strip being 30 ~ 50 Ω resistance penetrates from ceramic tube inside, temperature required when providing acetone gas normal operation of sensor with this, finally pin is welded on device base, just obtains acetone gas sensor through encapsulation.
The principle of work of acetone gas sensor:
When gas sensor exposes in atmosphere, the oxygen molecule in air can be adsorbed on composite sensitive material surface, and therefrom can capture electronics, thus forms O at material surface 2 -, O -or O 2-deng adion.Along with the orientation transfer of electronics from composite sensitive material to gas molecule, depleted of electrons layer will appear in the surface of composite sensitive material.If when now having acetone gas molecule to occur in air, first acetone molecules can be diffused into the surface of composite sensitive material, then, react with the oxygen desorption ion on composite sensitive material surface at a certain temperature.In course of reaction, be again released in composite sensitive material by the electronics of oxygen desorption ion binding.Correspondingly, the depleted of electrons layer width on composite sensitive material surface reduces, and material electric conductivity increases.Therefore, the change of ambient gas kind and concentration just can be monitored by the change of the resistance of survey sensor before and after contact measured gas.Here, the sensitivity definition of sensor is S=R a/ R g, wherein R aand R gbe respectively sensor in atmosphere with the resistance value in gas to be measured.
Beneficial effect of the present invention:
Composite sensitive material ZnO/ZnFe of the present invention 2o 4synthesize on the basis of ZnO hollow microsphere.Compared with the ZnO of one-component, ZnO/ZnFe 2o 4there is larger specific surface area (53.8m 2/ g).Therefore, through ZnFe 2o 4znO after modification can provide more avtive spot for gas reaction.In addition, in the interface of heterojunction structure, contact berrier forms the initial resistance adding sensor.The acting in conjunction of these factors imparts ZnO/ZnFe 2o 4the gas-sensitive property that heterojunction structure is more excellent.Whole building-up process is simple, efficient, energy-conservation, is suitable for large-scale production.To compare the ZnO hollow microsphere of one-component, through ZnFe 2o 4znO gas sensor after nanometer sheet modification can show more excellent gas-sensitive property to acetone.In addition, the gas sensor volume of this type is little, cost is low, makes this based on ZnO/ZnFe 2o 4the gas sensor of heterojunction structure is more applicable for the monitoring of acetone gas.
Accompanying drawing explanation
Fig. 1: the ZnO/ZnFe of preparation in embodiment 1 2o 4the XRD spectra of composite sensitive material;
Fig. 2: the ZnO/ZnFe of preparation in embodiment 1 2o 4electron scanning (SEM) photo of heterojunction structure under (a) low enlargement ratio and under (b) high magnification; Figure (c) is its corresponding transmission electron microscope (TEM) photo;
Fig. 3: (a) is based on ZnO/ZnFe 2o 4the structural representation of the acetone gas sensor of heterojunction structure; (b) base schematic diagram;
Fig. 4: embodiment 1 and the sensor in comparative example 1 at different operating temperature to the sensitivity curve of 100ppm acetone gas;
Fig. 5: embodiment 1 and the response curve of the sensor in comparative example 1 under different acetone concentration;
Fig. 6: the sensor in embodiment 1 at 250 DEG C to the dynamic response curve of 100ppm acetone.
As shown in Figure 1, the product obtained in embodiment 1 is a kind of ZnO and ZnFe 2o 4compound substance, and to exist without other dephasigns.
From Fig. 2 (a) and 2 (b), in embodiment 1, obtain ZnO/ZnFe 2o 4heterojunction structure particle dispersion is better, surface porosity porous, ZnFe 2o 4nanometer sheet thickness is about 10nm.From figure (c) known products therefrom be a kind of nucleocapsid structure.This nucleocapsid structure is by the ZnO hollow microsphere of internal layer and outer field ZnFe 2o 4nanometer sheet composition, the internal diameter of ZnO hollow microsphere is about 1 μm, external diameter is about 2.5 μm, ZnFe 2o 4layer thickness is about 100nm.
As shown in Figure 3, the acetone sensor in embodiment 1 is decomposed into six ingredient: Al 2o 3ceramic pipe substrate 401, annular gold electrode 402, ZnO/ZnFe 2o 4composite sensitive material 403, Pt silk 404, nichrome coils 405 and device base 406; 1,2,3,4,5,6 six pins connecing device base respectively.
As shown in Figure 4, the optimum working temperature of the sensor in comparative example 1 and embodiment 1 is respectively 250 DEG C and 350 DEG C, and sensitivity is respectively 16.8 and 5.4.Be not difficult to find, the sensor in embodiment 1 shows outstanding in sensitivity characteristic.
As shown in Figure 5, under the acetone of variable concentrations (5 ~ 700ppm), the sensor in embodiment 1 all will be far superior to the sensor in comparative example 1 in sensitivity.
As shown in Figure 6, when the working sensor in embodiment 1 is under optimum working temperature (250 DEG C), it is respectively 1s and 33s to the response recovery time of the acetone of 100ppm.As is shown in said inset, the sensor in embodiment 1 also has extraordinary stability and repeatability.
Embodiment
Comparative example 1:
With ZnO hollow microsphere for sensitive material makes acetone gas sensor, its concrete grammar is as follows:
1. by 1.1g Zn (CH 3cOO) 22H 2o and 0.0588g Na 3c 6h 5o 72H 2o joins in 200mL deionized water successively, keeps constantly stirring making it fully dissolve, and then measures 6mL ammoniacal liquor (30wt%) and joins in above-mentioned solution, continues to keep stirring 5min;
2. transferred in three-neck flask by gained settled solution, and place the devices such as thermometric, stirring and backflow, utilize microwave reaction solution to be heated to 90 DEG C, the heat time is set to 40min, and heating power is set to 300W;
3. after reaction terminates, microwave heating system stops heating automatically, after question response system naturally cools to room temperature, take out three-neck flask, the white precipitate deionized water of gained and ethanol alternating centrifugal are washed 6 times, washes the survivor ion in reaction solution off, the product after washing is dry under 70 DEG C of conditions, thus obtaining ZnO hollow microsphere, product quality is about 200mg;
4. the ZnO hollow microsphere getting 20mg obtained mixes with 200 μ L deionized waters, and grinding obtains the slurry of modest viscosity gently, then with fine, soft fur brush, above-mentioned slurry is coated in Al 2o 3the outside surface of ceramic pipe substrate, coating thickness is about 20 μm, the Al after coating 2o 3outside surface and the gold electrode of ceramic pipe substrate are covered by sensitive material completely, only reserve pin stand-by;
5. ceramic pipe is placed on below infrared lamp and toasts 25min post bake, then 2h is calcined under placing it in 450 DEG C of conditions, until naturally after cooling, the nickel-chrome heater strip being about 35 Ω a resistance penetrates from ceramic tube inside, temperature required when providing normal operation of sensor with this, finally all external pins are welded on device base, just obtain acetone gas sensor through encapsulation.
Embodiment 1:
With ZnO/ZnFe 2o 4heterojunction structure is that sensitive material makes acetone gas sensor, and its concrete grammar is as follows:
1. by 1.1g Zn (CH 3cOO) 22H 2o and 0.0588g Na 3c 6h 5o 72H 2o joins in 200mL deionized water successively, keeps constantly stirring making it fully dissolve, and then measures 6mL ammoniacal liquor (30wt%) and joins in above-mentioned solution, continues to keep stirring 5min;
2. transfer in three-neck flask by gained settled solution, utilize microwave that reaction solution is heated to 90 DEG C, the heat time is set to 40min, and heating power is set to 300W;
3. after reaction terminates, microwave heating system stops heating automatically, after question response system naturally cools to room temperature, take out three-neck flask, the white precipitate deionized water of gained and ethanol alternating centrifugal are washed 6 times, washes the survivor ion in reaction solution off, the product after washing is dry under 70 DEG C of conditions, thus obtaining ZnO hollow microsphere, product quality is about 200mg;
4. the ZnO hollow microsphere getting 50mg obtained joins in 47mL deionized water, and ultrasonic 2min makes in the complete aqueous dispersion of ZnO hollow microsphere;
5. by FeSO pre-configured for 3mL 4solution (0.5M, 10mmol FeSO 4be dissolved in 20mL deionized water) be slowly added drop-wise in above-mentioned mixed solution, after stirred at ambient temperature 5min, afterproduct deionized water and ethanol alternating centrifugal washing washing 6 times will be obtained, and dry under 70 DEG C of conditions, then under 450 DEG C of conditions, calcine 3h, finally obtain ZnO/ZnFe 2o 4composite sensitive material, product quality is about 60mg;
6. the ZnO/ZnFe that 20mg is obtained is got 2o 4composite sensitive material mixes with 200 μ L deionized waters, and grinding obtains the slurry of modest viscosity gently, then with fine, soft fur brush, above-mentioned slurry is coated in Al 2o 3the outside surface of ceramic pipe substrate, coating thickness is about 20 μm, the Al after coating 2o 3outside surface and the gold electrode of ceramic pipe substrate are covered by composite sensitive material completely, only reserve pin stand-by;
7. ceramic pipe is placed on below infrared lamp and toasts 25min post bake, then 2h is calcined under placing it in 450 DEG C of conditions, until naturally after cooling, the nickel-chrome heater strip being about 35 Ω a resistance penetrates from ceramic tube inside, temperature required when providing normal operation of sensor with this, finally all external pins are welded on device base, just obtain acetone gas sensor through encapsulation.

Claims (5)

1. the composite sensitive material ZnO/ZnFe for acetone sensor 2o 4, it is characterized in that: be by ZnO hollow microsphere with at its epontic ZnFe 2o 4the heterojunction structure that nanometer sheet is formed; The external diameter of ZnO hollow microsphere is 2 ~ 4 μm, and internal diameter is 1 ~ 2.5 μm; Single ZnFe 2o 4the thickness of nanometer sheet is 8 ~ 15nm, at the epontic ZnFe of ZnO hollow microsphere 2o 4the thickness of nanoscale twins is 80 ~ 150nm.
2. a ZnO/ZnFe according to claim 1 2o 4the preparation method of composite sensitive material, its step is as follows:
(1) preparation of ZnO hollow microsphere
1. 0.8 ~ 1.2g Zinc diacetate dihydrate is taken successively and 0.03 ~ 0.08g bis-citric acid monohydrate trisodium joins in 150 ~ 220mL deionized water, stirring makes it dissolve completely, form clear transparent solutions, then measure 4 ~ 6mL ammoniacal liquor and join in above-mentioned solution, continue stirring 5 ~ 10min;
2. utilize microwave that reaction solution is heated to 75 ~ 95 DEG C, then keep 10 ~ 60min, microwave heating power is 200 ~ 500W;
3., after question response terminates, the white precipitate deionized water of gained and ethanol alternating centrifugal are washed 5 ~ 8 times, washes the survivor ion in reaction solution off, the product after washing is dry under 60 ~ 80 DEG C of conditions, thus obtain ZnO hollow microsphere;
(2) ZnO/ZnFe 2o 4the preparation of composite sensitive material
1. getting 40 ~ 60mg ZnO hollow microsphere joins in 40 ~ 50mL deionized water, and ultrasonic 1 ~ 5min makes ZnO hollow microsphere disperse completely;
2. by the FeSO of 2 ~ 6mL, 0.3 ~ 0.8M 4solution is slowly added drop-wise in above-mentioned dispersion liquid, stirred at ambient temperature 5 ~ 10min, the product deionized water obtained and ethanol alternating centrifugal is washed 5 ~ 8 times; Then dry at 60 ~ 80 DEG C, finally calcine 2 ~ 5 hours under 400 ~ 500 DEG C of conditions, thus obtain ZnO/ZnFe 2o 4composite sensitive material.
3. ZnO/ZnFe as claimed in claim 1 2o 4composite sensitive material is preparing the application in acetone gas sensor.
4. ZnO/ZnFe as claimed in claim 3 2o 4composite sensitive material is preparing the application in acetone gas sensor, it is characterized in that the step preparing acetone gas sensor is as follows:
1. with Al 2o 3ceramic pipe is substrate, and every one end of ceramic pipe outside surface, respectively with a ring-type gold electrode, each gold electrode is all connected with two Pt silks and makes pin;
2. by ZnO/ZnFe obtained for 15 ~ 40mg 2o 4composite sensitive material mixes with 100 ~ 500 μ L deionized waters, and grinding obtains the slurry of modest viscosity gently, then with fine, soft fur brush, above-mentioned slurry is coated in Al 2o 3the outside surface of ceramic pipe substrate, coating thickness is 10 ~ 30 μm, the Al after coating 2o 3the outside surface of ceramic pipe substrate and ring-type gold electrode are completely by ZnO/ZnFe 2o 4sensitive material covers, and only reserves pin;
3. under ceramic pipe being placed on infrared lamp, baking 20 ~ 30min carries out post bake, then calcine 2 ~ 4 hours under placing it in 400 ~ 500 DEG C of conditions, until naturally after cooling, the nickel-chrome heater strip being 30 ~ 50 Ω resistance penetrates from ceramic tube inside, finally pin is welded on device base, just obtains acetone gas sensor through encapsulation.
5. ZnO/ZnFe as claimed in claim 4 2o 4composite sensitive material is preparing the application in acetone gas sensor, it is characterized in that: ceramic pipe range 2 ~ 6mm, internal diameter 0.6 ~ 0.9mm, external diameter 1 ~ 1.2mm, and the width of gold electrode is 0.5 ~ 0.8mm.
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CN106896146A (en) * 2017-01-05 2017-06-27 扬州大学 A kind of coating production of zinc ferrite acetone gas sensing layer
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