CN111533161A - Preparation method and application of indium-doped zinc oxide gas-sensitive material - Google Patents
Preparation method and application of indium-doped zinc oxide gas-sensitive material Download PDFInfo
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- CN111533161A CN111533161A CN202010446709.XA CN202010446709A CN111533161A CN 111533161 A CN111533161 A CN 111533161A CN 202010446709 A CN202010446709 A CN 202010446709A CN 111533161 A CN111533161 A CN 111533161A
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- C—CHEMISTRY; METALLURGY
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- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a preparation method and application of an indium-doped zinc oxide gas-sensitive material, wherein zinc nitrate and indium acetylacetonate are used as raw materials, methanol is used as a solvent, 2-methylimidazole is used as an organic linking agent, standing is carried out for 24 hours at the temperature of 25-27 ℃, and in (acac) is obtained after methanol centrifugal washing3And @ ZIF-8, drying the obtained compound in a drying oven at 60 ℃, and annealing to obtain the indium-doped zinc oxide gas-sensitive material. The preparation method is simple in preparation process and low in cost, and the prepared indium-doped zinc oxide gas-sensitive material has a porous hollow cage-shaped structure, can realize detection of ppb level nitrogen dioxide gas and has the potential of detecting hydrogen sulfide gas.
Description
Technical Field
The invention relates to a preparation method and application of an indium-doped zinc oxide gas-sensitive material, which are used for preparing a nitrogen dioxide gas sensor, can realize the detection of ppb level nitrogen dioxide, have the potential of detecting hydrogen sulfide gas and belong to the technical field of gas-sensitive material preparation.
Background
Nitrogen dioxide is mainly derived from the combustion of fossil fuels and industrial production activities, and is of great concern due to its potential hazards to environmental safety and human health. Excessive emissions of nitrogen dioxide can lead to various environmental problems such as acid rain, photochemical smog, and PM2.5 (particulate matter less than 2.5 μm). People are most likely to suffer from upper respiratory and heart diseases when exposed to an environment containing nitrogen dioxide gas for a long period of time. Chinese character' shiThe national health organization requires that the concentration of nitrogen dioxide in cities within 1 hour should be lower than 200 mu g/m3(106ppb) and should be less than 40. mu.g/m throughout the year3(21 ppb). At the same time, nitrogen dioxide produced by human metabolic activity is an important biomarker. The diagnosis of various human diseases including chronic obstructive pulmonary diseases can be effectively assisted by detecting the content of nitrogen dioxide in the exhaled air. Therefore, the realization of the high-sensitivity detection of the trace nitrogen dioxide has important significance on environmental protection and personal safety.
Based on ZnO and In2O3、SnO2、Fe2O3And WO3The metal oxide semiconductor gas sensors have a dominant role in gas detection equipment for domestic, laboratory and commercial applications due to the characteristics of high sensitivity, fast response speed, low cost, portability and the like. As a typical metal oxide semiconductor sensing material, ZnO has been widely studied for detecting various gases including nitrogen dioxide. However, for most ZnO-based sensors, the lower limit of detection is still high and the sensitivity is not sufficient to accurately monitor changes in low concentrations of nitrogen dioxide. In order to obtain higher gas sensing performance, the use of porous micro-nano structures has proven to be one of the most effective methods. On the other hand, the gas-sensitive performance can be further improved by selective doping. It has been found that an increase in sensitivity, better selectivity to the target gas or a reduction in response/recovery time can be achieved based on doping with a metal element such as indium. However, achieving uniform dispersion of the doping elements while maintaining a porous hollow structure remains challenging.
As a sub-class of the well-known Metal Organic Frameworks (MOFs), the Zeolitic Imidazolate Frameworks (ZIFs) are an emerging class of porous materials. Among all ZIFs, ZIF-8 consisting of zinc and 2-methylimidazole has been most widely studied due to its stable synthetic route, excellent thermal/chemical stability and definite pore characteristics. These unique advantages of ZIF-8 greatly facilitate its use in gas separation, gas storage and catalysis. Among them, ZIF-8 has been extensively studied to encapsulate noble metal nanoparticles (e.g., Pd and Pt) within its micropores. Technically, the in-situ packaging strategy can wrap precursors with specific molecular diameters in ZIF-8 micropores, and the problem of agglomeration of doped metal in the annealing process can be solved. Furthermore, to our knowledge, there has been no study on the use of this strategy for the preparation of metal doped ZnO as a high performance gas sensitive material.
Disclosure of Invention
The invention aims to provide a preparation method and application of an indium-doped zinc oxide gas-sensitive material. The invention fully utilizes the ZIF-8 aperture as
And a cage diameter of
In (acac) in the crystallization process3The molecules were encapsulated in situ in the micropores of ZIF-8. After annealing treatment, the indium doping element is uniformly and dispersedly doped into the crystal lattice of the zinc dioxide, so that the agglomeration problem of the doping element is effectively avoided, and the preparation of the high-performance sensitive material is realized.
The invention relates to a method for preparing indium-doped zinc oxide gas-sensitive material, which is prepared from zinc nitrate and indium acetylacetonate (in (acac)3) Taking methanol as a solvent and 2-methylimidazole as an organic linking agent as raw materials, standing for 24 hours at 25-27 ℃, and centrifugally washing by using methanol to obtain in (acac)3And @ ZIF-8, drying the obtained compound in a drying oven at 60 ℃, and annealing to obtain the indium-doped zinc oxide gas-sensitive material. The method specifically comprises the following steps:
step 1: dissolving a proper amount of zinc nitrate hexahydrate in methanol, and continuously stirring by magnetic force to form a transparent solution A;
step 2: adding a proper amount of acetylacetone indium into the obtained transparent solution A, and continuously magnetically stirring to form a transparent solution B;
and step 3: dissolving a proper amount of 2-methylimidazole in methanol, and continuously stirring by magnetic force to form a solution C;
and 4, step 4: adding the solution C obtained in the step (3) into the transparent solution B obtained in the step (2), magnetically stirring, and standing at 25-27 ℃;
and 5: the precipitate obtained in step 4, i.e. in (acac)3The @ ZIF-8 compound is centrifugally washed by absolute methanol and then is dried in a drying oven;
step 6: and (5) annealing the compound obtained In the step (5) to obtain the indium-mixed zinc oxide gas-sensitive material, namely In/ZnO.
In step 1, the amount of zinc nitrate hexahydrate was 810mg and the volume of methanol was 40 mL.
In the step 2, the molar weight of the acetylacetone indium is 2 to 10 percent of the molar weight of zinc nitrate hexahydrate.
In step 3, the amount of 2-methylimidazole added was 721.6mg, and the volume of methanol was 40 mL.
In the step 4, the magnetic stirring time is 15-20 minutes, and the standing time is 24 hours.
In the step 5, the drying temperature is 60 ℃, and the drying time is 12-24 hours.
In step 6, the annealing temperature is 500 ℃, the annealing time is 2 hours, and the temperature rise and reduction rate is 1 ℃/min.
The indium-doped zinc oxide obtained by the method has the particle size of 0.3-2 mu m and has a porous hollow cage-shaped structure.
The indium-doped zinc oxide gas-sensitive material prepared by the invention is used as a sensor film material, can realize the detection of ppb level nitrogen dioxide gas and has the potential of detecting hydrogen sulfide gas.
Compared with the prior art, the invention has the beneficial effects that:
the invention fully utilizes the ZIF-8 aperture as
And a cage diameter of
In (acac) in the crystallization process3The molecules are wrapped in the micropores of the ZIF-8 in situ; after annealing treatment, the indium doping element is uniformly and dispersedly doped with the indiumThe crystal lattice of the zinc oxide effectively avoids the agglomeration problem of the doping elements.
The indium-doped zinc oxide gas sensor prepared based on the method can realize the detection of ppb level nitrogen dioxide gas, and shows higher response value and excellent sensitivity.
The preparation process is simple and low in cost.
Drawings
FIG. 1 shows in (acac) in example 1 of the present invention3@ ZIF-8 complex.
FIG. 2 is an X-ray diffraction pattern of In/ZnO In example 1 of the present invention.
FIG. 3 is a scanning electron micrograph of In/ZnO In example 1 of the present invention.
FIG. 4 is a transmission electron micrograph and elemental distribution of In/ZnO of example 1 of the present invention. The scale in the figure is 400 nm.
FIG. 5 is a graph of the dynamic response of In/ZnO at optimum operating conditions for 10, 25, 50 and 100ppb nitrogen dioxide In example 1 of the present invention.
FIG. 6 is a graph showing the response of In/ZnO with respect to the concentration of nitrogen dioxide In the optimum operating condition In example 1 of the present invention.
FIG. 7 is a graph showing the response of In/ZnO In example 1 of the present invention to 10ppm of nitrogen dioxide and hydrogen sulfide, 100ppm of ethanol and acetone under optimum operating conditions.
FIG. 8 is an X-ray diffraction pattern of In/ZnO-2 In example 2 of the present invention.
FIG. 9 is a scanning electron micrograph of In/ZnO-2 In example 2 of the present invention.
FIG. 10 is a graph showing the dynamic response to 0.2 to 10ppm nitrogen dioxide In the optimum operating conditions of In/ZnO-2 In example 2 of the present invention.
FIG. 11 is a graph of the optimum In/ZnO-2 operation of example 2 of the present invention for 5 cycles of 200ppn nitrogen dioxide.
FIG. 12 is a graph showing the response of In/ZnO-2 In example 2 of the present invention to 10ppm of nitrogen dioxide and hydrogen sulfide, 100ppm of ethanol and acetone under optimum operating conditions.
In fig. 1, 2 and 8: a.u. denotes intensity units; in fig. 6, 7 and 12: response denotes the Response value, defineIs Response ═ Rg/Ra(Nitrogen dioxide) or Ra/Rg(remaining reducing gas) in which RaAnd RgThe resistance value of the sensor when in dry air and the resistance value of the sensor in the target gas, respectively; the Sensitivity is defined as Sensitivity ═ Δ R/Δ C, i.e., the slope of the change in sensor response value (Δ R) versus the change in gas concentration (Δ C).
Detailed Description
To further illustrate the technical solutions and advantages of the present invention, the following detailed description of the embodiments of the present invention is provided with reference to the accompanying drawings.
Example 1:
1. dissolving 810mg of zinc nitrate hexahydrate in 40mL of methanol, and continuously magnetically stirring to form a transparent solution A;
2. 114.5mg of acetylacetone indium (the molar ratio of the acetylacetone indium to zinc nitrate hexahydrate is 10%) is added into the solution A, and magnetic stirring is continued to form a transparent solution B;
3. 721.6mg of 2-methylimidazole is dissolved in 40mL of methanol, and magnetic stirring is continuously carried out to form a solution C;
4. adding the transparent solution C prepared in the step 3 into the transparent solution B, magnetically stirring for 20 minutes, and standing for 24 hours at room temperature (27 ℃);
5. the precipitate obtained in step 4, in (acac)3The @ ZIF-8 compound is centrifugally washed for three times by absolute methanol and then is dried for 24 hours in a drying oven at the temperature of 60 ℃;
6. and (3) annealing the compound obtained In the step (5) at 500 ℃ for 2 hours at the heating and cooling rate of 1 ℃/min to obtain the indium hybrid zinc oxide gas-sensitive material, namely In/ZnO.
FIG. 1 shows in (acac) in example 1 of the present invention3@ ZIF-8 complex. The measured compound peaks all correspond to the peaks of ZIF-8 one by one, and no other miscellaneous peaks exist. FIG. 2 is an X-ray diffraction pattern of In/ZnO In example 1 of the present invention. The measured peaks all correspond to the peaks of ZnO one by one, and no other miscellaneous peaks exist. FIG. 3 is a scanning electron micrograph of In/ZnO In example 1 of the present invention. The average size of the cage particles was measured to be around 1.5 μm. FIG. 4 is a transmission electron micrograph of In/ZnO In example 1 of the present inventionAnd an element distribution map. The porous and hollow structure is confirmed, the indium element is uniformly distributed, and no obvious agglomeration phenomenon exists. FIG. 5 is a graph of the dynamic response of In/ZnO at optimum operating temperatures for 10, 25, 50 and 100ppb nitrogen dioxide In example 1 of the present invention. The In/ZnO can realize the detection of ppb level nitrogen dioxide gas, and the response value of the In/ZnO to 10ppb nitrogen dioxide is as high as 3.7. FIG. 6 is a graph showing the response of In/ZnO with respect to the concentration of nitrogen dioxide at the optimum operating temperature In example 1 of the present invention. Under 1ppm, the response value and the nitrogen dioxide concentration have good linear relation, and the sensitivity is calculated to be up to 187.9ppm-1. FIG. 7 is a graph showing the response of In/ZnO In example 1 of the present invention to 10ppm of nitrogen dioxide and hydrogen sulfide, 100ppm of ethanol and acetone under optimum operation conditions. Besides high response to nitrogen dioxide, In/ZnO has good response to hydrogen sulfide, and low response to ethanol and acetone gases.
Example 2:
1. dissolving 810mg of zinc nitrate hexahydrate in 40mL of methanol, and continuously magnetically stirring to form a transparent solution A;
2. adding 22.9mg of acetylacetone indium (the molar ratio of acetylacetone indium to zinc nitrate hexahydrate is 2%) into the solution A, and continuously stirring by magnetic force to form a transparent solution B;
3. 721.6mg of 2-methylimidazole is dissolved in 40mL of methanol, and magnetic stirring is continuously carried out to form a solution C;
4. adding the transparent solution C prepared in the step 3 into the transparent solution B, magnetically stirring for 15 minutes, and standing for 24 hours at room temperature (25 ℃);
5. the precipitate obtained in step 4, in (acac)3The @ ZIF-8 compound is centrifugally washed for three times by absolute methanol and then is dried for 18 hours in a drying oven at the temperature of 60 ℃;
6. and (3) annealing the compound obtained In the step (5) at 500 ℃ for 2 hours at the heating and cooling rate of 1 ℃/min to obtain the indium hybrid zinc oxide gas-sensitive material, namely In/ZnO-2.
FIG. 8 is an X-ray diffraction pattern of In/ZnO-2 In example 2 of the present invention. The measured peaks all correspond to the peaks of ZnO one by one, and no other miscellaneous peaks exist. FIG. 9 is a scanning electron micrograph of In/ZnO-2 In example 2 of the present invention. The average size of the cage particles was measured to be around 0.4 μm. FIG. 10 is a graph showing the dynamic response to 0.2 to 10ppm nitrogen dioxide In the optimum operating conditions of In/ZnO-2 In example 2 of the present invention. The In/ZnO resistance gradually increases with increasing nitrogen dioxide concentration. The calculated response value for 200ppb nitrogen dioxide was 6.7. FIG. 11 is a graph of the optimum operation of In/ZnO-2 for 5 cycles of 200ppb nitrogen dioxide In example 2 of the present invention. The response behavior of In/ZnO-2 to 200ppb nitrogen dioxide can be repeated well. FIG. 12 is a graph showing the response of In/ZnO-2 In example 2 of the present invention to 10ppm of nitrogen dioxide and hydrogen sulfide, 100ppm of ethanol and acetone under optimum operating conditions. Besides high response to nitrogen dioxide, In/ZnO has good response to hydrogen sulfide, and low response to ethanol and acetone gases.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. A preparation method of an indium-doped zinc oxide gas-sensitive material is characterized by comprising the following steps:
zinc nitrate and indium acetylacetonate as raw materials, methanol as a solvent, 2-methylimidazole as an organic linking agent, standing for 24 hours at 25-27 ℃, and centrifugally washing by methanol to obtain in (acac)3And @ ZIF-8, drying the obtained compound in a drying oven at 60 ℃, and annealing to obtain the indium-doped zinc oxide gas-sensitive material.
2. The method of claim 1, comprising the steps of:
step 1: dissolving a proper amount of zinc nitrate hexahydrate in methanol, and continuously stirring by magnetic force to form a transparent solution A;
step 2: adding a proper amount of acetylacetone indium into the obtained transparent solution A, and continuously magnetically stirring to form a transparent solution B;
and step 3: dissolving a proper amount of 2-methylimidazole in methanol, and continuously stirring by magnetic force to form a solution C;
and 4, step 4: adding the solution C obtained in the step (3) into the transparent solution B obtained in the step (2), magnetically stirring, and standing at 25-27 ℃;
and 5: centrifuging and washing the precipitate, namely in (acac)3@ ZIF-8 compound obtained in the step 4 by using anhydrous methanol, and then drying the compound in a drying box;
step 6: and (5) annealing the compound obtained In the step (5) to obtain the indium-mixed zinc oxide gas-sensitive material, namely In/ZnO.
3. The method of claim 2, wherein:
in step 1, the amount of zinc nitrate hexahydrate was 810mg and the volume of methanol was 40 mL.
4. The method of claim 2, wherein:
in the step 2, the molar weight of the acetylacetone indium is 2 to 10 percent of the molar weight of zinc nitrate hexahydrate.
5. The method of claim 2, wherein:
in step 3, the amount of 2-methylimidazole added was 721.6mg, and the volume of methanol was 40 mL.
6. The method of claim 2, wherein:
in the step 4, the magnetic stirring time is 15-20 minutes, and the standing time is 24 hours.
7. The method of claim 2, wherein:
in the step 5, the drying temperature is 60 ℃, and the drying time is 12-24 hours.
8. The method of claim 2, wherein:
in step 6, the annealing temperature is 500 ℃, the annealing time is 2 hours, and the temperature rise and reduction rate is 1 ℃/min.
9. The method of claim 2, wherein:
the obtained indium-doped zinc oxide has a particle size of 0.3-2 μm and a porous hollow cage structure.
10. Use of an indium-doped zinc oxide gas-sensitive material prepared according to any one of the preparation methods described in claims 1 to 9, characterized in that: and the indium-doped zinc oxide gas-sensitive material is used as a sensor thin film material to detect nitrogen dioxide gas or hydrogen sulfide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112899722A (en) * | 2021-01-27 | 2021-06-04 | 同济大学 | Metal organic framework derived In/ZnO @ C hollow nanocage electrocatalytic material and preparation and application thereof |
| CN113680311A (en) * | 2021-08-19 | 2021-11-23 | 上海应用技术大学 | Preparation method of zinc-based composite metal oxide |
| CN114988457A (en) * | 2022-06-27 | 2022-09-02 | 上海复纯环保科技有限公司 | Based on alpha-Fe 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial, and preparation process and application thereof |
-
2020
- 2020-05-25 CN CN202010446709.XA patent/CN111533161A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| YI JIANXIN ET AL.: "IMCS03-2065-Indium-Doped zno porous cages derived from ZIF-8 for Ppb-level NO2 detection", 《237TH ECS MEETING》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112899722A (en) * | 2021-01-27 | 2021-06-04 | 同济大学 | Metal organic framework derived In/ZnO @ C hollow nanocage electrocatalytic material and preparation and application thereof |
| CN112899722B (en) * | 2021-01-27 | 2022-02-18 | 同济大学 | Metal organic framework derived In/ZnO @ C hollow nanocage electrocatalytic material and preparation and application thereof |
| CN113680311A (en) * | 2021-08-19 | 2021-11-23 | 上海应用技术大学 | Preparation method of zinc-based composite metal oxide |
| CN113680311B (en) * | 2021-08-19 | 2023-07-21 | 上海应用技术大学 | Preparation method of zinc-based composite metal oxide |
| CN114988457A (en) * | 2022-06-27 | 2022-09-02 | 上海复纯环保科技有限公司 | Based on alpha-Fe 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial, and preparation process and application thereof |
| CN114988457B (en) * | 2022-06-27 | 2023-06-23 | 上海复纯环保科技有限公司 | Based on alpha-Fe 2 O 3 Microporous nanomaterial of nano wire heteroepitaxy ZnO@ZIF-8, preparation process and application |
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Application publication date: 20200814 |