CN104749225B - ZnO/ZnFe2O4Composite sensitive material, preparation method and the application in acetone gas sensor - Google Patents
ZnO/ZnFe2O4Composite sensitive material, preparation method and the application in acetone gas sensor Download PDFInfo
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Abstract
The invention belongs to metal-oxide gas transducer technical field, and in particular to a kind of composite sensitive material ZnO/ZnFe2O4Design, synthesis and its application in acetone gas sensor.The present invention successfully synthesizes ZnO hollow microspheres, then using the method for epitaxial growth in one layer of ZnFe of ZnO hollow microspheres superficial growth using microwave heating technique first in the design and preparation process of sensitive material2O4Nanometer sheet.Whole building-up process is simple, efficient, energy-conservation, suitable for large-scale production.Compare for the ZnO hollow microspheres of one-component, by ZnFe2O4ZnO gas sensors after nanometer sheet modification can show more excellent gas-sensitive property to acetone.In addition, the gas sensor small volume of this type, low cost so that this to be based on ZnO/ZnFe2O4The gas sensor of heterojunction structure is more applicable for the monitoring of acetone gas.
Description
Technical field
The invention belongs to metal-oxide gas transducer technical field, and in particular to ZnO/ZnFe2O4Composite sensing material
Material, preparation method and the application in acetone gas sensor.
Background technology
With constantly weeding out the old and bring forth the new for sensitive material, various gas sensitive materials are successively developed.In numerous gases
In sensitive material, have that sensitivity is high due to metal-oxide semiconductor (MOS), prepare low cost, asepsis environment-protecting, being easily integrated etc. and be excellent
A kind of point, it is considered to be gas sensitive for most having an application prospect.Therefore, in the last few years, metal oxide receives extensive pass
Note and obtained development energetically.According to the species of majority carrier, metal-oxide semiconductor (MOS) can be divided into N-shaped sensitive material
(such as In2O3、SnO2、ZnO、Fe2O3、WO3Deng) and p-type sensitive material (such as NiO, Co3O4, CuO etc.).Although based on above-mentioned metal
The gas sensor of oxide obtains some applications, but is due to its own limited physicochemical properties, by these lists
The metal-oxide semiconductor (MOS) of one component is difficult the further raising for obtaining gas-sensitive property.In this case, by sensitive material
Multi-component heterojunction structure is expanded to from the metal oxide of one-component to be particularly important.Due to its adjustable chemical composition
Synergy between heterogeneity, heterojunction structure tends to show outstanding gas sensitization characteristic.
Especially, zinc oxide (ZnO) is widely used in inspection as a kind of typical N-shaped oxide semiconductor sensitive material
Survey CO, NH3, in NOx and various poisonous and hazardous escaping gases.However, exactly because ZnO is quicker to many gases
Sense, so ZnO selectivity is poor, it is difficult to distinguish different types of gas exactly.In recent years, it has been reported that spinel-type three
First metal oxide zinc ferrite (ZnFe2O4) extraordinary selectivity and sensitiveness can be shown to some specific gas.If
Can be by ZnO and ZnFe2O4It is combined together, perhaps can improves selectivity of the ZnO under test gas.In order to verify realize it is above-mentioned
Guess, it is necessary first to which completion is to prepare homogeneous ZnO/ZnFe2O4Heterojunction structure.
At present, the preparation method of heterojunction structure has a lot, mainly has sol-gal process, chemical vapour deposition technique (CVD), surpasses
Sound spray-on process, water/solvent-thermal method and method of electrostatic spinning etc..However, these above-mentioned synthetic methods all exist very in actual applications
More serious deficiency, for example, cumbersome operation sequence, tediously long course of reaction, substantial amounts of energy resource consumption and harsh experiment bar
Part.These deficiencies greatly govern their application and development.Therefore, in order to explore between material structure and gas-sensitive property
Relation, a kind of preparation method of simple and effective heterojunction structure of searching, which still has, to be of great significance.
The content of the invention
It is an object of the invention to provide a kind of composite sensitive material ZnO/ZnFe that can be used in acetone gas sensor2O4。
ZnO/ZnFe of the present invention2O4Composite sensitive material is one kind by ZnO hollow microspheres and in its superficial growth
ZnFe2O4The heterojunction structure that nanometer sheet is constituted；The external diameter of ZnO hollow microspheres is 2~4 μm, and internal diameter is 1~2.5 μm；It is single
ZnFe2O4The thickness of nanometer sheet is 8~15nm, in the ZnFe of ZnO hollow microsphere superficial growths2O4The thickness of nanoscale twins is 80
~150nm.
The present invention first using zinc acetate, trisodium citrate and ammoniacal liquor as raw material, using Microwave-assisted synthesis method 30~
ZnO hollow microspheres are successfully prepared in 40min；Then at room temperature, by ZnFe2O4Nanometer sheet grows into ZnO hollow microspheres
Surface forms ZnO/ZnFe2O4Composite sensitive material；Finally, above-mentioned ZnO/ZnFe is utilized2O4Composite sensitive material constructs acetone gas
Body sensor.ZnO/ZnFe of the present invention2O4The specific preparation method of composite sensitive material is as follows：
The preparation of 1.ZnO hollow microspheres
1. 0.8~1.2g Zinc diacetate dihydrates (Zn (CH are weighed successively3COO)2·2H2O) it is hydrated with 0.03~0.08g bis-
Trisodium citrate (Na3C6H5O7·2H2O) it is added in 150~220mL deionized waters, is stirred to dissolve completely, forms clarification saturating
Bright solution, then measures 4~6mL ammoniacal liquor (30wt%) and is added in above-mentioned solution, stirs 5~10min；
2. reaction solution is heated to 75~95 DEG C using microwave, then keeps 10~60min, heating using microwave power is
200~500W；
3. after question response terminates, the white precipitate of gained is washed 5~8 times with deionized water and ethanol alternating centrifugal, washed
Fall the survivor ion in reaction solution, the product after washing is dried under the conditions of 60~80 DEG C, so that it is hollow micro- to obtain ZnO
Ball；
2.ZnO/ZnFe2O4The preparation of composite sensitive material
1. 40~60mg ZnO hollow microspheres are taken to be added in 40~50mL deionized waters, 1~5min of ultrasound makes ZnO hollow
Microballoon is scattered complete；
2. by 2~6mL, 0.3~0.8M FeSO4Solution is slowly dropped in above-mentioned dispersion liquid, at room temperature stir 5~
10min, obtained product is washed 5~8 times with deionized water and ethanol alternating centrifugal；Then dried at 60~80 DEG C, most
Calcined 2~5 hours under the conditions of 400~500 DEG C afterwards, so as to obtain ZnO/ZnFe2O4Composite sensitive material；
3. the making of acetone gas sensor
1. with Al2O3Earthenware is substrate, ceramic 2~6mm of pipe range, 0.6~0.9mm of internal diameter, 1~1.2mm of external diameter, ceramics
Every one end of tube outer surface is respectively with a ring-type gold electrode, and the width of gold electrode is equal on 0.5~0.8 mm, each gold electrode
It is connected with two Pt and makees pin；
2. by 15~40mg ZnO/ZnFe2O4Composite sensitive material is mixed with 100~500 μ L deionized waters, is lightly ground
The slurry of modest viscosity is obtained, above-mentioned slurry is then coated in Al with fine, soft fur brush2O3The outer surface of earthenware substrate, applies thickness
Spend for 10~30 μm, the Al after coating2O3The outer surface of earthenware substrate and ring-type gold electrode are completely by ZnO/ZnFe2O4It is compound
Sensitive material is covered, and only reserves pin；
3. earthenware is placed under infrared lamp and toasts 20~30min progress post bakes, be then placed on 400~500 DEG C of bars
Calcined 2~4 hours under part, until after natural cooling, resistance for 30~50 Ω nichrome heater strip from ceramic tube inside
Penetrate, pin is finally welded on device base by required temperature when providing acetone gas sensor normal work with this, pass through
Encapsulation has just obtained acetone gas sensor.
The operation principle of acetone gas sensor：
When gas sensor exposes in atmosphere, the oxygen molecule in air can be adsorbed on composite sensitive material surface, and
Electronics can therefrom be captured, so that in material surface formation O2 -、O-Or O2-Deng adion.As electronics is from composite sensitive material
Orientation to gas molecule is shifted, and depleted of electrons layer will appear in the surface of composite sensitive material.If now had in air
When acetone gas molecule occurs, acetone molecules can be diffused into the surface of composite sensitive material first, then, at a certain temperature with
The oxygen adion on composite sensitive material surface reacts.In course of reaction, the electronics fettered by oxygen adion again by
It is discharged into composite sensitive material.Correspondingly, the depleted of electrons slice width degree on composite sensitive material surface reduces, and material electric conductivity increases
Plus.Therefore, the change of the resistance by measurement sensor before and after contact measured gas can just monitor ambient gas species and
The change of concentration.Herein, the sensitivity definition of sensor is S=Ra/Rg, wherein RaAnd RgRespectively sensor is in atmosphere
With the resistance value under test gas.
Beneficial effects of the present invention：
Composite sensitive material ZnO/ZnFe of the present invention2O4Synthesized on the basis of ZnO hollow microspheres.With list
The ZnO of one component is compared, ZnO/ZnFe2O4With bigger specific surface area (53.8m2/g).Therefore, by ZnFe2O4After modification
ZnO more avtive spots can be provided for gas reaction.In addition, in the interface of heterojunction structure, contact berrier formation increases
The initial resistance of sensor is added.The collective effect of these factors imparts ZnO/ZnFe2O4The more excellent air-sensitive of heterojunction structure
Characteristic.Whole building-up process is simple, efficient, energy-conservation, suitable for large-scale production.Compare one-component ZnO hollow microspheres and
Speech, by ZnFe2O4ZnO gas sensors after nanometer sheet modification can show more excellent gas-sensitive property to acetone.Plus
It, the gas sensor small volume of this type, low cost so that this to be based on ZnO/ZnFe2O4The gas sensing of heterojunction structure
Device is more applicable for the monitoring of acetone gas.
Brief description of the drawings
Fig. 1：The ZnO/ZnFe prepared in embodiment 12O4The XRD spectra of composite sensitive material；
Fig. 2：The ZnO/ZnFe prepared in embodiment 12O4Heterojunction structure is under (a) low enlargement ratio and (b) high magnification
Under electron scanning (SEM) photo；It is its corresponding transmission electron microscope (TEM) photo to scheme (c)；
Fig. 3：(a) it is based on ZnO/ZnFe2O4The structural representation of the acetone gas sensor of heterojunction structure；(b) base is illustrated
Figure；
Fig. 4：Embodiment 1 and the sensor in comparative example 1 are at a temperature of different operating to the sensitive of 100ppm acetone gas
Write music line；
Fig. 5：Response curve of the embodiment 1 from the sensor in comparative example 1 under different acetone concentrations；
Fig. 6：Dynamic response curve of the sensor at 250 DEG C to 100ppm acetone in embodiment 1.
As shown in figure 1, the product obtained in embodiment 1 is a kind of ZnO and ZnFe2O4Composite, and without other dephasigns
In the presence of.
From Fig. 2 (a) and 2 (b), ZnO/ZnFe is obtained in embodiment 12O4Heterojunction structure particle dispersion is preferable, surface
It is loose porous, ZnFe2O4Nanometer sheet thickness is about 10nm.Understand that products therefrom is a kind of core shell structure from figure (c).This nucleocapsid
Structure is the ZnO hollow microspheres and the ZnFe of outer layer by internal layer2O4Nanometer sheet composition, the internal diameters of ZnO hollow microspheres is about 1 μm,
External diameter is about 2.5 μm, ZnFe2O4Thickness degree is about 100nm.
As shown in figure 3, the acetone sensor in embodiment 1 is decomposed into six parts：Al2O3Earthenware substrate
401st, annular gold electrode 402, ZnO/ZnFe2O4Composite sensitive material 403, Pt silks 404, nichrome coils 405 and device base 406；
1st, 2,3,4,5,6 six pins for connecing device base respectively.
As shown in Figure 4, comparative example 1 and the optimum working temperature of the sensor in embodiment 1 are respectively 250 DEG C and 350 DEG C,
Sensitivity is respectively 16.8 and 5.4.It is seen that, the sensor in embodiment 1 shows outstanding in sensitivity characteristic.
As shown in figure 5, under the acetone of various concentrations (5~700ppm), the sensor in embodiment 1 is in sensitivity
The sensor that aspect will be far superior in comparative example 1.
As shown in fig. 6, when the working sensor in embodiment 1 is under optimum working temperature (250 DEG C), it is to 100ppm
The response recovery time of acetone be respectively 1s and 33s.As is shown in said inset, the sensor in embodiment 1 also has extraordinary
Stability and repeatability.
Embodiment
Comparative example 1：
Acetone gas sensor is made by sensitive material of ZnO hollow microspheres, its specific method is as follows：
1. by 1.1g Zn (CH3COO)2·2H2O and 0.0588g Na3C6H5O7·2H2O is added sequentially to 200mL deionizations
In water, holding, which is stirred continuously, makes it fully dissolve, and then measures 6mL ammoniacal liquor (30wt%) and is added in above-mentioned solution, continues to protect
Hold stirring 5min；
2. gained settled solution is transferred in three-neck flask, and places the devices such as thermometric, stirring and backflow, using micro-
Reaction solution is heated to 90 DEG C by ripple, and the heat time is set to 40min, and heating power is set to 300W；
3. after reaction terminates, microwave heating system is automatically stopped heating, and question response system is naturally cooled to after room temperature, takes out
Three-neck flask, the white precipitate of gained is washed 6 times with deionized water and ethanol alternating centrifugal, the remnants in reaction solution are washed off
Ion, the product after washing is dried under the conditions of 70 DEG C, so that ZnO hollow microspheres are obtained, product quality about 200mg；
4. take ZnO hollow microspheres made from 20mg to be mixed with 200 μ L deionized waters, be lightly ground the slurry for obtaining modest viscosity
Material, is then coated in Al with fine, soft fur brush by above-mentioned slurry2O3The outer surface of earthenware substrate, coating layer thickness is about 20 μm, after coating
Al2O3The outer surface of earthenware substrate and gold electrode are sensitive material by covering completely, only reserve pin stand-by；
5. earthenware is placed on baking 25min post bakes below infrared lamp, 2h is calcined under the conditions of being then placed on 450 DEG C,
Until after natural cooling, the nichrome heater strip that a resistance is 35 Ω or so is penetrated from ceramic tube inside, provided with this
All external pins, are finally welded on device base by required temperature during normal operation of sensor, are just obtained by encapsulation
Acetone gas sensor.
Embodiment 1：
With ZnO/ZnFe2O4Heterojunction structure is that sensitive material makes acetone gas sensor, and its specific method is as follows：
1. by 1.1g Zn (CH3COO)2·2H2O and 0.0588g Na3C6H5O7·2H2O is added sequentially to 200mL deionizations
In water, holding, which is stirred continuously, makes it fully dissolve, and then measures 6mL ammoniacal liquor (30wt%) and is added in above-mentioned solution, continues to protect
Hold stirring 5min；
2. gained settled solution is transferred in three-neck flask, reaction solution is heated to 90 DEG C, during heating using microwave
Between be set to 40min, heating power is set to 300W；
3. after reaction terminates, microwave heating system is automatically stopped heating, and question response system is naturally cooled to after room temperature, takes out
Three-neck flask, the white precipitate of gained is washed 6 times with deionized water and ethanol alternating centrifugal, the remnants in reaction solution are washed off
Ion, the product after washing is dried under the conditions of 70 DEG C, so that ZnO hollow microspheres are obtained, product quality about 200mg；
4. ZnO hollow microspheres made from 50mg are taken to be added in 47mL deionized waters, ultrasonic 2min makes ZnO hollow microspheres complete
In full aqueous dispersion；
5. by FeSO pre-configured 3mL4Solution (0.5M, 10mmol FeSO4It is dissolved in 20mL deionized waters) it is slow
Slowly it is added drop-wise in above-mentioned mixed solution, stirs at room temperature after 5min, rear product deionized water will be obtained and ethanol alternating centrifugal is washed
It is washed out 6 times, and is dried under the conditions of 70 DEG C, then calcines 3h under the conditions of 450 DEG C, finally give ZnO/ZnFe2O4It is compound quick
Feel material, product quality is about 60mg；
6. ZnO/ZnFe made from 20mg is taken2O4Composite sensitive material is mixed with 200 μ L deionized waters, is lightly ground and is obtained
The slurry of modest viscosity, is then coated in Al with fine, soft fur brush by above-mentioned slurry2O3The outer surface of earthenware substrate, coating layer thickness is about
For 20 μm, the Al after coating2O3The outer surface of earthenware substrate and gold electrode are covered by composite sensitive material completely, are only reserved and are drawn
Pin is stand-by；
7. earthenware is placed on baking 25min post bakes below infrared lamp, 2h is calcined under the conditions of being then placed on 450 DEG C,
Until after natural cooling, the nichrome heater strip that a resistance is 35 Ω or so is penetrated from ceramic tube inside, provided with this
All external pins, are finally welded on device base by required temperature during normal operation of sensor, are just obtained by encapsulation
Acetone gas sensor.
Claims (4)
1. a kind of composite sensitive material ZnO/ZnFe for acetone sensor2O4, it is characterised in that：Be by ZnO hollow microspheres and
In the ZnFe of its superficial growth2O4The heterojunction structure that nanometer sheet is constituted；The external diameter of ZnO hollow microspheres be 2~4 μm, internal diameter be 1~
2.5μm；Single ZnFe2O4The thickness of nanometer sheet is 8~15nm, in the ZnFe of ZnO hollow microsphere superficial growths2O4Nanoscale twins
Thickness be 80~150nm；And the composite sensitive material is prepared by following steps,
(1) preparation of ZnO hollow microspheres
1. weigh 0.8~1.2g Zinc diacetate dihydrates successively and 0.03~0.08g two citric acid monohydrate trisodiums be added to 150~
In 220mL deionized waters, stirring makes its dissolving complete, forms clear transparent solutions, then measures 4~6mL ammoniacal liquor and be added to
State in solution, continue to stir 5~10min；
2. reaction solution is heated to 75~95 DEG C using microwave, then keep 10~60min, heating using microwave power be 200~
500W；
3. after question response terminates, the white precipitate of gained is washed 5~8 times with deionized water and ethanol alternating centrifugal, washed off anti-
The survivor ion in solution is answered, the product after washing is dried under the conditions of 60~80 DEG C, so as to obtain ZnO hollow microspheres；
(2)ZnO/ZnFe2O4The preparation of composite sensitive material
1. 40~60mg ZnO hollow microspheres are taken to be added in 40~50mL deionized waters, 1~5min of ultrasound makes ZnO hollow microspheres
It is scattered complete；
2. by 2~6mL, 0.3~0.8M FeSO4Solution is slowly dropped in above-mentioned dispersion liquid, and 5~10min is stirred at room temperature,
Obtained product is washed 5~8 times with deionized water and ethanol alternating centrifugal；Then dried at 60~80 DEG C, finally 400
Calcined 2~5 hours under the conditions of~500 DEG C, so as to obtain ZnO/ZnFe2O4Composite sensitive material.
2. the ZnO/ZnFe described in claim 12O4Application of the composite sensitive material in acetone gas sensor is prepared.
3. ZnO/ZnFe as claimed in claim 22O4Application of the composite sensitive material in acetone gas sensor is prepared, its
The step of being characterised by preparing acetone gas sensor is as follows：
1. with Al2O3Earthenware is substrate, and every one end of ceramic tube outer surface is respectively with a ring-type gold electrode, each gold electrode
On be respectively connected with two Pt and make pin；
2. by ZnO/ZnFe made from 15~40mg2O4Composite sensitive material is mixed with 100~500 μ L deionized waters, is lightly ground
The slurry of modest viscosity is obtained, above-mentioned slurry is then coated in Al with fine, soft fur brush2O3The outer surface of earthenware substrate, applies thickness
Spend for 10~30 μm, the Al after coating2O3The outer surface of earthenware substrate and ring-type gold electrode are completely by ZnO/ZnFe2O4It is sensitive
Material is covered, and only reserves pin；
3. earthenware is placed under infrared lamp and toasts 20~30min progress post bakes, be then placed under the conditions of 400~500 DEG C
Calcining 2~4 hours, until after natural cooling, resistance is penetrated for 30~50 Ω nichrome heater strip from ceramic tube inside,
Finally pin is welded on device base, acetone gas sensor has just been obtained by encapsulation.
4. ZnO/ZnFe as claimed in claim 32O4Application of the composite sensitive material in acetone gas sensor is prepared, its
It is characterised by：Ceramic 2~6mm of pipe range, 0.6~0.9mm of internal diameter, 1~1.2mm of external diameter, the width of gold electrode is 0.5~0.8mm.
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| WO2017145915A1 (en) * | 2016-02-25 | 2017-08-31 | 株式会社豊田中央研究所 | Metal oxide film and method for producing same |
| CN105655477A (en) * | 2016-04-08 | 2016-06-08 | 大连理工大学 | Flexible nanogenerator with heterogeneous junction structure as well as manufacturing method and application thereof |
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| CN106896146B (en) * | 2017-01-05 | 2019-03-01 | 扬州大学 | A kind of coating production of zinc ferrite acetone gas sensing layer |
| CN109399725B (en) * | 2017-08-15 | 2021-04-13 | 中国石油化工股份有限公司 | Preparation method and application of zinc ferrite-containing nano-structure array |
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| CN108802116A (en) * | 2018-06-19 | 2018-11-13 | 扬州睿德石油机械有限公司 | A kind of preparation method of acetone gas sensitive material |
| CN109115843B (en) * | 2018-09-20 | 2020-12-25 | 东北大学 | Cu-doped ZnFe2O4Nanoparticles, and preparation method and application thereof |
| CN109342534B (en) * | 2018-11-08 | 2020-09-08 | 吉林大学 | Oxygen vacancy dominated CuO/ZnFe based2O4Xylene gas sensor of core-shell structure microsphere and preparation method thereof |
| CN110006958B (en) * | 2019-04-10 | 2022-03-08 | 河北工业大学 | Co3O4Preparation method of-ZnO nano material acetone thick film gas sensor |
| CN111766282B (en) * | 2020-06-05 | 2023-01-17 | 济南大学 | Preparation method and application of competitive photoelectrochemical immunosensor based on spinel type zinc ferrite |
| CN111610234B (en) * | 2020-07-07 | 2021-09-07 | 上海大学 | Acetone gas sensor of field effect transistor and preparation method thereof |
| CN113155924B (en) * | 2021-03-19 | 2022-02-15 | 云南大学 | Detection method of norovirus |
| CN113899790A (en) * | 2021-08-30 | 2022-01-07 | 西安电子科技大学 | Acetone sensor, preparation method and application |
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