CN108226233A - Hierarchical Z nO@ZnO nano composite air-sensitive materials and preparation method thereof - Google Patents
Hierarchical Z nO@ZnO nano composite air-sensitive materials and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of hierarchical Z nO@ZnO nano composite air-sensitive materials, it is that 2 methylimidazoles are dissolved in N, in the mixed solution of N dimethylformamides and water, is ultrasonically treated, prepares precursor solution；Weigh a certain amount of zinc oxide nano-powder, it is added in prepared precursor solution, all solution are fitted into reaction kettle, it is reacted 12 48 hours at 70 100 DEG C, then reactant is taken out, it filters, is dried after ethyl alcohol repeatedly washs, obtain hierarchical Z nO@ZnO precursor materials；Gained precursor material is placed in tube furnace, calcines 1h in air atmosphere, is obtained with hierarchical Z nO@ZnO nano composite air-sensitive materials.The present invention does not generate poisonous and harmful substance, is conducive to environmental protection；Gas sensitive obtained shows ethyl alcohol higher sensitivity and selectivity.
Description
Technical field
The present invention relates to a kind of gas sensitives and preparation method thereof, and in particular to a kind of hierarchical Z nO@ZnO nanos are answered
Gas sensitive and preparation method thereof is closed, belongs to gas sensitive technical field.
Background technology
Zinc oxide is II-VI race's semiconductor optoelectronic material of a kind of exciton bind energy (60meV) height, broad stopband (3.37eV)
Material, is stabilized with single hexagonal wurtzite structure, it is in kinescope, scanning electron microscope, HIGH-POWERED MICROWAVES device, hair
All various aspects such as optical device, laser have broad application prospects.Zinc oxide is also gas-sensitive metal oxidation studied earliest
One of object material.It can be to H as nano-electrode2、H2S, the gases such as ethyl alcohol and methanol have good response and higher sensitive
Degree.Zinc oxide can prepare the nano material as different morphologies at present, such as nano particle, nanometer rods, nano flower or nano wire,
Meanwhile the electrical properties of the ZnO material of different-shape are different, therefore, selectivity and sensitivity to gas also have larger difference.
Quantum size zinc oxide is influenced since size reduces with quantum effect, and band gap broadens, meanwhile, surface atom
Proportion increases in the material, and the influence to material energy level variations after atomic adsorption on surface gas molecule becomes apparent from, to it
The influence of electric property is more notable.Again since specific surface area greatly increases, it is easier to capture rare detected gas point
Son, therefore can realize higher detection sensitivity.But since under the conditions of high fever, quantum size zinc oxide is easily grown up, very
To being grown to serve as big aggregate, therefore quantum size zinc oxide can't maturely be applied to gas sensing as sensor material
Device field.
Invention content
It, should it is an object of the invention to propose a kind of preparation method of hierarchical Z nO@ZnO nano composite air-sensitive materials
Material can have ethyl alcohol good response characteristic.
To achieve the above object, the technical scheme is that：
The preparation method of hierarchical Z nO@ZnO nano composite air-sensitive materials, is that 2-methylimidazole is dissolved in N, N- diformazans
In base formamide (DMF) and the mixed solution of water, it is ultrasonically treated, prepares precursor solution；Weigh a certain amount of zinc oxide
Nano-powder is added in the precursor solution prepared by step (1), all solution is fitted into reaction kettle, anti-at 70 DEG C
It answers 24 hours, then takes out reactant, filter, be dried after ethyl alcohol repeatedly washs, before obtaining hierarchical Z nO@ZnO
Drive object material；Gained precursor material is placed in tube furnace, calcines 1h in air atmosphere, is obtained with hierarchical Z nO@
ZnO nano composite air-sensitive material；
It is as follows：
(1) 2-methylimidazole is dissolved in NN- dimethylformamides (DMF) and the mixed solution of water, be ultrasonically treated, prepared
Obtain precursor solution；
(2) a certain amount of zinc oxide nano-powder is weighed, is added in the precursor solution prepared by step (1), by institute
There is solution to be fitted into reaction kettle, react 12-48 hours at 70-100 DEG C, then take out reactant, filter, it is multiple through ethyl alcohol
It is dried after washing, obtains hierarchical Z nO@ZnO precursor materials；
(3) precursor material obtained by step (2) is placed in tube furnace, calcines 1h in air atmosphere at a certain temperature,
It obtains with hierarchical Z nO@ZnO nano composite air-sensitive materials；
The weight ratio of 2-methylimidazole and zinc oxide nano-powder described in step (1) is 0.233：1 to 2.330：1, root
It is adjusted accordingly according to synthesis different proportion ZnO.
The mixed liquor volume ratio of N,N-dimethylformamide (DMF) and water described in step (1) is 3:1；
Sonication treatment time described in step (1) is 5 minutes；
Drying described in step (2) refers to dry in the baking oven for being 80-100 DEG C in temperature；
Calcination temperature described in step (3) is 400-600 DEG C；
Control calcining heating rate in step (3) is for 2-10 DEG C/min until reaching set temperature.
The preparation according to hierarchical Z nO@ZnO nano composite air-sensitive materials provided by the invention is also claimed in the present invention
The hierarchical Z nO@ZnO nano composite air-sensitive materials that method is prepared.
The present invention has the advantages that：
(1) present invention obtains the ZnO of different-grain diameter, the ZnO materials by controlling precursor solution concentration, calcination temperature
Material has quantum size, and even particle distribution can obtain different specific surface areas by size regulation and control, increase spatial activity position
Point is conducive to the adsorption and de-adsorption of gas, can improve sensitivity, increases stability；
(2) ZnO@ZnO materials produced by the present invention show ethyl alcohol higher sensitivity and quick response is restored, detection
Low, high selectivity is limited, a kind of effective sensitive material is provided for ethyl alcohol detection；
(3) gas sensitive structure and preparation process produced by the present invention are simple, and one step of preparation process is completed, and effectively improves material
Expect preparation efficiency, each step in preparation process does not generate poisonous and harmful substance, is conducive to environmental protection.
Description of the drawings
Fig. 1 is hierarchical Z nO@ZnO nano composite air-sensitive materials SEM figures prepared by embodiment 1；
Fig. 2 is ethyl alcohol of the hierarchical Z nO@ZnO nano composite air-sensitive materials to a concentration of 50ppm of the preparation of embodiment 1
The dynamic response recovery curve of gas；
Fig. 3 is the hierarchical Z nO@ZnO nano composite air-sensitive materials of the preparation of embodiment 1 to different concentration ethanol gas
Dynamic response recovery curve；
Fig. 4 is other gases of the hierarchical Z nO@ZnO nano composite air-sensitive materials to 50ppm of the preparation of embodiment 1
Remolding sensitivity compared with.
Specific embodiment
The present invention is described further below in conjunction with the accompanying drawings.
Embodiment 1
61.5mg 2-methylimidazoles are dissolved in 60mL n,N-Dimethylformamide (DMF) and the mixed solution of water,
Middle DMF：H2O=3:1, it is ultrasonically treated 5 minutes, prepares precursor solution；The zinc oxide nano-powder of 132mg is weighed, is added
Enter into prepared precursor solution, all solution are fitted into 100mL reaction kettles, react 24 hours at 70 DEG C, then
Reactant is taken out, filters, is dried after ethyl alcohol repeatedly washs, obtains hierarchical Z nO@ZnO precursor materials；By institute
It obtaining precursor material to be placed in tube furnace, in air atmosphere 500 DEG C of calcinings, heating rate is 2 DEG C/min, keeps temperature 1h,
Room temperature is naturally cooling to, is obtained with hierarchical Z nO@ZnO nano composite air-sensitive materials.
The hierarchical Z nO@ZnO nano composite air-sensitive materials SEM figures being prepared as shown in Figure 1, can be seen by Fig. 1
Go out and loaded Zinc oxide quantum dot in zinc oxide particle surfaces；Hierarchical Z nO@ZnO nano composite air-sensitive materials are to a concentration of
The dynamic response recovery curve of the alcohol gas of 50ppm is as shown in Figure 2.
Embodiment 2
61.5mg 2-methylimidazoles are dissolved in 60mL n,N-Dimethylformamide (DMF) and the mixed solution of water,
Middle DMF：H2O=3:1, it is ultrasonically treated 5 minutes, prepares precursor solution；The zinc oxide nano-powder of 132mg is weighed, is added
Enter into prepared precursor solution, all solution are fitted into 100mL reaction kettles, react 24 hours at 70 DEG C, then
Reactant is taken out, filters, is dried after ethyl alcohol repeatedly washs, obtains hierarchical Z nO@ZnO precursor materials；By institute
It obtaining precursor material to be placed in tube furnace, in air atmosphere 400 DEG C of calcinings, heating rate is 2 DEG C/min, keeps temperature 1h,
Room temperature is naturally cooling to, is obtained with hierarchical Z nO@ZnO nano composite air-sensitive materials, at 375 DEG C, to a concentration of
The ethyl alcohol electrical response rate of 50ppm is 36.8.
Embodiment 3
30.75mg 2-methylimidazoles are dissolved in 60mL n,N-Dimethylformamide (DMF) and the mixed solution of water,
Middle DMF：H2O=3:1, it is ultrasonically treated 5 minutes, prepares precursor solution；The zinc oxide nano-powder of 132mg is weighed, is added
Enter into prepared precursor solution, all solution are fitted into 100mL reaction kettles, react 24 hours at 70 DEG C, then
Reactant is taken out, filters, is dried after ethyl alcohol repeatedly washs, obtains hierarchical Z nO@ZnO precursor materials；By institute
It obtaining precursor material to be placed in tube furnace, in air atmosphere 600 DEG C of calcinings, heating rate is 2 DEG C/min, keeps temperature 1h,
Room temperature is naturally cooling to, is obtained with hierarchical Z nO@ZnO nano composite air-sensitive materials, at 375 DEG C, to a concentration of
The ethyl alcohol electrical response rate of 50ppm is 17.
Embodiment 4
The measure of ethyl alcohol：By adjusting heating voltage, the operating temperature of gas sensitive is controlled at 375 DEG C, using constant potential
Method sets loop voltage as 1V, and resistance change of the gas sensitive in air and under test gas is obtained by recording change in electric
Change；The sensitivity response value of gas sensitive is defined as：S=Ra/Rg, wherein RaFor the aerial resistance of gas sensitive, RgFor gas
Resistance of the quick material under test gas；
Using Devince By Dynamic Gas Ration Method, use quality flow controller prepares 1-250ppm ethyl alcohol calibrating gas, is passed through gas survey
Platform is tried, gas sensitive is exposed under test gas, measures its response, obtains ethanol concentration gradient curve, such as Fig. 3 institutes
Show.Using same procedure, 50ppm ethyl alcohol, acetone, CO, H are prepared2、CH4、NH3、NO2Calibrating gas, obtain the gas sensitive
To the selectivity of alcohol gas, the results are shown in Figure 4, which has ethyl alcohol a good response sensitivity, and with compared with
Strong jamming ability.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modifications and embodiment, these modifications and embodiment will be fallen in principle disclosed in the present application
Within scope and spirit.
Claims (8)
1. a kind of preparation method of hierarchical Z nO@ZnO nano composite air-sensitive materials, it is characterised in that include the following steps：
(1) 2-methylimidazole is dissolved in the mixed solution of n,N-Dimethylformamide and water, is ultrasonically treated, prepares preceding body
Liquid solution；
(2) a certain amount of zinc oxide nano-powder is weighed, is added in the precursor solution prepared by step (1), by all solution
It is fitted into reaction kettle, reacts 12-48 hours at 70-100 DEG C, then take out reactant, filter, after ethyl alcohol repeatedly washs
It is dried, obtains hierarchical Z nO@ZnO precursor materials；
(3) precursor material obtained by step (2) is placed in tube furnace, keeps certain temperature calcining 1h in air atmosphere, obtain
To with hierarchical Z nO@ZnO nano composite air-sensitive materials.
2. the preparation method of hierarchical Z nO@ZnO nanos composite air-sensitive material according to claim 1, it is characterised in that：
The weight ratio of 2-methylimidazole and zinc oxide nano-powder described in step (1) is 0.233：1 to 2.330：1, according to synthesis not
ZnO is adjusted accordingly in proportion.
3. the preparation method of hierarchical Z nO@ZnO nanos composite air-sensitive material according to claim 1, it is characterised in that：
N,N-Dimethylformamide described in step (1) and in the mixed solution of water, the volume ratio of n,N-Dimethylformamide and water is
3:1。
4. the preparation method of hierarchical Z nO@ZnO nanos composite air-sensitive material according to claim 1, it is characterised in that：
Sonication treatment time described in step (1) is 5 minutes.
5. the preparation method of hierarchical Z nO@ZnO nanos composite air-sensitive material according to claim 1, it is characterised in that：
Drying described in step (2) refers to dry in the baking oven for being 80-100 DEG C in temperature.
6. the preparation method of hierarchical Z nO@ZnO nanos composite air-sensitive material according to claim 1, it is characterised in that：
The temperature calcined in step (3) is 400-600 DEG C.
7. the preparation method of hierarchical Z nO@ZnO nanos composite air-sensitive material according to claim 6, it is characterised in that：
Control calcining heating rate in step (3) is for 2-10 DEG C/min until reaching the temperature of the calcining of setting.
8. a kind of hierarchical Z nO@ZnO nano composite air-sensitive materials, it is characterised in that the hierarchical Z nO@ZnO nanos are answered
Gas sensitive is closed to be prepared by preparation method described in claim 1 to 7 any claim.
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Cited By (2)
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| CN111610227A (en) * | 2019-02-25 | 2020-09-01 | 天津理工大学 | 2D ZnO @3D CF nano composite material and preparation method and application thereof |
| CN113670993A (en) * | 2021-09-08 | 2021-11-19 | 大连理工大学 | Composite gas-sensitive material with hierarchical structure and preparation method and application thereof |
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| CN111610227B (en) * | 2019-02-25 | 2023-01-31 | 天津理工大学 | 2D ZnO @3D CF nano composite material and preparation method and application thereof |
| CN113670993A (en) * | 2021-09-08 | 2021-11-19 | 大连理工大学 | Composite gas-sensitive material with hierarchical structure and preparation method and application thereof |
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