CN108918631B - Preparation method of MOFs/ZnO composite gas-sensitive film responding to CO through ultra-fast in-situ synthesis - Google Patents
Preparation method of MOFs/ZnO composite gas-sensitive film responding to CO through ultra-fast in-situ synthesis Download PDFInfo
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Abstract
The invention relates to the technical field of gas-sensitive materials, in particular to a preparation method of an ultra-fast in-situ synthesis metal organic framework MOFs/ZnO composite gas-sensitive film. The composite gas-sensitive film is obtained by preparing a ZnO nanoparticle film layer on an aluminum oxide planar electrode, sintering the ZnO nanoparticle film layer in a muffle furnace at a high temperature, and then growing MOFs on the ZnO nanoparticle film layer by a dipping ion exchange method. The composite gas-sensitive film is ZnO covered with a layer of MOFs film, and the gas-sensitive film with the composite structure constructs a gas channel, increases gas adsorption sites and is beneficial to greatly improving the gas sensitivity and selectivity. The preparation method of the composite gas-sensitive membrane has the advantages of simple and convenient operation, easy realization and low cost.
Description
Technical Field
The invention belongs to the technical field of gas-sensitive materials, and particularly relates to a preparation method of an ultra-fast in-situ synthesis MOFs/ZnO composite gas-sensitive film.
Background
The sensing technology, one of the three core technologies of information technology, has been the highest point of high-tech competition in various countries. The gas sensor is used as an important branch in the field of sensors, and can convert the information of the outside gas into an electric signal and transmit the electric signal to a control center, thereby realizing the functions of detection, automatic control, alarm and the like. The types of the gas sensors are quite rich, wherein the metal oxide semiconductor gas-sensitive device has the advantages of good stability, high reliability, short adsorption and desorption time and the like, and great research interest of researchers is aroused.
ZnO is an environment-friendly n-type semiconductor, has the electron binding energy of 60meV at room temperature, the forbidden band width of 3.37eV, high electron mobility and good chemical and thermal stability, and has wide application in the fields of sensors, photoelectric devices, photon detectors and the like. According to the report, the humidity sensors with ZnO nanostructures (including nanofibers, nanorods, nanosheets and the like) with different shapes all show good gas-sensitive response. However, the ZnO gas sensor has high working temperature (above 300 ℃) and poor selectivity.
MOFs have many excellent characteristics necessary for sensing. The pore structure of the MOFs can enhance the selective adsorption of the sensor, has large specific surface area and wide pore space, and can greatly improve the sensitivity and accuracy of the sensor by combining with the selective adsorption; in addition, the MOFs also have high stability, including thermal stability and chemical stability, and can greatly improve the stability of the sensor. MOFs, however, are generally poorly conductive, which limits their use as electrochemical-type sensors.
Disclosure of Invention
The invention provides a composite gas-sensitive material formed by growing MOFs on a ZnO film, which takes the advantages of ZnO and MOFs as gas-sensitive materials into consideration and realizes the functions of 1+1 > 2. The novel gas sensitive material lays a foundation for the research of the gas sensitive sensor.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an ultra-fast in-situ synthesis MOFs/ZnO composite gas-sensitive film is characterized in that a layer of ZnO nanoparticle film layer is prepared on an aluminum oxide planar motor by adopting a thick film process, then the ZnO nanoparticle film layer is annealed at a high temperature in a muffle furnace to serve as a growth substrate, and then the MOFs/ZnO composite gas-sensitive film grows on the growth substrate by adopting a dipping ion exchange method, and specifically comprises the following steps:
(1) pretreatment of aluminum oxide planar electrodes
Ultrasonically cleaning an aluminum oxide planar electrode by using acetone, absolute ethyl alcohol and deionized water sequentially and then drying the aluminum oxide planar electrode in an oven for later use;
(2) preparation of ZnO slurry
Mixing ZnO nanoparticles with a proper amount of terpineol, and grinding in an agate mortar to obtain uniformly dispersed ZnO slurry;
(3) preparation of ZnO growth substrate
Coating the ZnO slurry on the pretreated aluminum oxide planar electrode by a spin-coating method to prepare a gas-sensitive element, and drying in an oven;
(4) annealing
Placing the ZnO gas-sensitive element obtained in the step (3) in a muffle furnace for annealing and then naturally cooling to room temperature;
(5) growth of MOFs
Placing the annealed ZnO gas-sensitive element obtained in the step (4) in Cu (NO) with a certain concentration3)2Keeping the solution at room temperature for a certain time, taking out the solution and drying the solution to prepare (Zn, Cu) (OH) NO3a/ZnO film; reacting said (Zn, Cu) (OH) NO3the/ZnO film is placed in an organic ligand solution with a certain concentration, and the organic ligand solution is selected from 1,3, 5-trimesic acid (H)3BTC) and 1, 4-terephthalic acid solution (H)2BDC), keeping for a certain time at room temperature, taking out and drying to prepare the MOFs/ZnO composite gas-sensitive film.
In the preparation method of the ultra-fast in-situ synthesis MOFs/ZnO composite gas-sensitive film, the cleaning time required by ultrasonic cleaning with acetone, absolute ethyl alcohol and deionized water in the step (1) is at least 10min respectively.
In the preparation method of the ultra-fast in-situ synthesis MOFs/ZnO composite gas-sensitive film, the size of the ZnO nanoparticles in the step (2) is 20-40 nm, and the grinding time is 30-60 min.
In the preparation method of the ultra-fast in-situ synthesis MOFs/ZnO composite gas-sensitive film, the annealing temperature in the step (4) is 600 ℃, and the constant temperature holding time is 2 hours.
In the step (5) of the preparation method of the ultra-fast in-situ synthesis MOFs/ZnO composite gas-sensitive film, the Cu (NO) is3)2The concentration of the solution is 0.45mol/L, and the ZnO gas sensor is arranged in Cu (NO)3)2The reaction time in the solution was 1 min.
In the step (5) of the preparation method of the ultra-fast in-situ synthesis MOFs/ZnO composite gas-sensitive film, the concentration of the organic ligand solution is 0.25mol/L, and the (Zn, Cu) (OH) NO is3The reaction time of the/ZnO film in the organic ligand solution was 30 s.
Compared with the prior art, the invention has at least the following beneficial effects: according to the preparation method of the ultra-fast in-situ synthesis MOFs/ZnO composite gas-sensitive film, the MOFs can be HKUST-1 or Cu-BDC, and the composite gas-sensitive film has good response characteristic to low-concentration CO. The invention lays a certain foundation for the development of the gas sensor.
Drawings
Fig. 1 is an SEM image of a ZnO nanoparticle film layer;
FIG. 2 is a low-magnification SEM image of the MOFs/ZnO composite gas-sensitive film of example 1;
FIG. 3 is a high power SEM image of the MOFs/ZnO composite gas-sensitive film of example 1;
FIG. 4 is a dynamic response recovery curve of the MOFs/ZnO composite gas-sensitive film prepared in example 1 for CO gases with different concentrations.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
1) Pretreatment of an aluminum oxide planar electrode: ultrasonically cleaning the aluminum oxide planar electrode by acetone, absolute ethyl alcohol and deionized water for 10min, and drying in an oven for later use;
2) preparing ZnO slurry: weighing 4mg of ZnO nanoparticles with the particle size of 20-40 nm, mixing the ZnO nanoparticles with 0.2mL of terpineol, and grinding the mixture in an agate mortar for 60min to obtain uniformly dispersed ZnO slurry;
3) preparing a ZnO growth substrate: coating the ZnO slurry on the pretreated aluminum oxide planar electrode by a spin-coating method to prepare a gas-sensitive element, and drying in an oven;
4) annealing: placing the ZnO gas-sensitive element obtained in the step 3) in a muffle furnace, setting the annealing temperature to be 600 ℃, keeping the constant temperature for 2 hours, and then naturally cooling to room temperature; the SEM image of the ZnO nanoparticle film layer is shown in fig. 1.
5) Growing MOFs: prepared by the step 4)The annealed ZnO gas sensor is placed in 0.45mol/L Cu (NO)3)2Keeping the solution at room temperature for 1min, taking out, oven drying to obtain (Zn, Cu) (OH) NO3a/ZnO film; reacting said (Zn, Cu) (OH) NO3the/ZnO film is placed at 0.25mol/L H3BTC solution (solvent composition H)2O:CH3CH2And (3) keeping the mixture in DMF (1: 1:1) at room temperature for 30s, taking out the mixture and drying the mixture to prepare the HKUST-1/ZnO composite gas-sensitive film, wherein the microstructure of the HKUST-1/ZnO composite gas-sensitive film is shown in figures 2 and 3.
Example 2
1) Pretreatment of an aluminum oxide planar electrode: ultrasonically cleaning the aluminum oxide planar electrode by acetone, absolute ethyl alcohol and deionized water for 10min, and drying in an oven for later use;
2) preparing ZnO slurry: weighing 4mg of ZnO nanoparticles with the particle size of 20-40 nm, mixing the ZnO nanoparticles with 0.4mL of terpineol, and grinding the mixture in an agate mortar for 30min to obtain uniformly dispersed ZnO slurry;
3) preparing a ZnO growth substrate: coating the ZnO slurry on the pretreated aluminum oxide planar electrode by a spin-coating method to prepare a gas-sensitive element, and drying in an oven;
4) annealing: placing the ZnO gas-sensitive element obtained in the step 3) in a muffle furnace, setting the annealing temperature to be 600 ℃, keeping the constant temperature for 2 hours, and then naturally cooling to room temperature;
5) growing MOFs: placing the annealed ZnO gas-sensitive element prepared in the step 4) in 0.045mol/L Cu (NO)3)2Keeping the solution at room temperature for 1min, taking out, oven drying to obtain (Zn, Cu) (OH) NO3a/ZnO film; reacting said (Zn, Cu) (OH) NO3the/ZnO film is placed at 0.025mol/L H3BTC solution (solvent composition H)2O:CH3CH2And (3) keeping the mixture in an OH (ratio of DMF) to DMF (ratio of DMF) to 1:1:1) at room temperature for 30s, taking out and drying the mixture to prepare the HKUST-1/ZnO composite gas-sensitive film.
Example 3
1) Pretreatment of an aluminum oxide planar electrode: ultrasonically cleaning the aluminum oxide planar electrode by acetone, absolute ethyl alcohol and deionized water for 10min, and drying in an oven for later use;
2) preparing ZnO slurry: weighing 4mg of ZnO nanoparticles with the particle size of 20-40 nm, mixing the ZnO nanoparticles with 0.2mL of terpineol, and grinding the mixture in an agate mortar for 60min to obtain uniformly dispersed ZnO slurry;
3) preparing a ZnO growth substrate: coating the ZnO slurry on the pretreated aluminum oxide planar electrode by a spin-coating method to prepare a gas-sensitive element, and drying in an oven;
4) annealing: placing the ZnO gas-sensitive element obtained in the step 3) in a muffle furnace, setting the annealing temperature to be 600 ℃, keeping the constant temperature for 2 hours, and then naturally cooling to room temperature;
5) growing MOFs: placing the annealed ZnO gas sensor in the step 4) in 0.45mol/L Cu (NO)3)2Keeping the solution at room temperature for 1min, taking out, oven drying to obtain (Zn, Cu) (OH) NO3a/ZnO film; reacting said (Zn, Cu) (OH) NO3the/ZnO film is placed at 0.25mol/L H2BDC solution (solvent composition H)2O:CH3CH2And (3) keeping the solution in an OH and DMF (1: 1:1) at room temperature for 30s, taking out and drying to prepare the Cu-BDC/ZnO composite gas-sensitive film.
Example 4
1) Determination of CO: controlling the temperature of the gas-sensitive reaction cavity to be 50 ℃, controlling the working temperature of the sensor to be 250 ℃, and obtaining the resistance change of the sensor in air and CO standard gas by recording the electric signal change of the gas-sensitive element by adopting a potentiostatic method under the condition of unchanging loop voltage;
2) introducing CO standard gas (with the concentration of 500ppm) into the gas-sensitive reaction cavity by adopting a dynamic gas distribution method, exposing the gas sensor device in the gas to be detected, preparing the CO standard gas with the concentration gradients of 5, 10, 20, 25, 50, 100,200,250 and 500ppm, and measuring the response value of the CO standard gas to obtain a CO concentration standard gradient curve, wherein the CO concentration standard gradient curve is shown in figure 4.
The MOFs grows on the ZnO film finally by applying the invention, and the composite gas-sensitive film with the new structure not only increases the specific surface area, but also increases more channels for gas adsorption and transportation, and the gas-sensitive property is obviously enhanced.
Although the invention has been described herein with reference to illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More specifically, various variations and modifications may be made to the component parts and/or arrangements of the subject combination arrangement within the scope of the disclosure herein. In addition to variations and modifications in the component parts and/or arrangements, other uses will also be apparent to those skilled in the art.
Claims (6)
1. A preparation method of an MOFs/ZnO composite gas-sensitive film responding to CO by ultra-fast in-situ synthesis is characterized in that a layer of ZnO nanoparticle film is prepared on an aluminum oxide planar electrode by adopting a thick film process, then the ZnO nanoparticle film is annealed at a high temperature in a muffle furnace to serve as a growth substrate, and then the MOFs/ZnO composite gas-sensitive film is grown on the growth substrate by adopting a dipping ion exchange method, and specifically comprises the following steps:
(1) pretreatment of aluminum oxide planar electrodes
Ultrasonically cleaning an aluminum oxide planar electrode by using acetone, absolute ethyl alcohol and deionized water sequentially and respectively, and drying in an oven for later use;
(2) preparation of ZnO slurry
Mixing ZnO nanoparticles with a proper amount of terpineol, and grinding in an agate mortar to obtain uniformly dispersed ZnO slurry;
(3) preparation of ZnO growth substrate
Coating the ZnO slurry on the pretreated aluminum oxide planar electrode by a spin-coating method to prepare a gas-sensitive element, and drying in an oven;
(4) annealing
Placing the ZnO gas-sensitive element obtained in the step (3) in a muffle furnace for annealing and then naturally cooling to room temperature;
(5) growth of MOFs
Placing the annealed ZnO gas-sensitive element obtained in the step (4) in Cu (NO) with a certain concentration3)2Keeping the solution at room temperature for a certain time, taking out the solution and drying the solution to prepare (Zn, Cu) (OH) NO3a/ZnO film; reacting said (Zn, Cu) (OH) NO3the/ZnO film is placed in an organic ligand solution with a certain concentration, and the organic ligand solution is selected from 1,3, 5-homozygoteBenzene tricarboxylic acid (H)3BTC) and 1, 4-terephthalic acid solution (H)2BDC), keeping for a certain time at room temperature, taking out and drying to prepare the MOFs/ZnO composite gas-sensitive film.
2. The method for preparing the MOFs/ZnO composite gas-sensitive film responding to CO by the ultra-fast in-situ synthesis method according to claim 1, wherein the cleaning time required by the ultrasonic cleaning respectively with acetone, absolute ethyl alcohol and deionized water in the step (1) is at least 10min respectively.
3. The preparation method of the MOFs/ZnO composite gas-sensitive film responding to CO through the ultra-fast in-situ synthesis according to claim 1, wherein the size of the ZnO nanoparticles in the step (2) is 20-40 nm, and the grinding time is 30-60 min.
4. The method for preparing the MOFs/ZnO composite gas-sensitive film responding to CO by ultra-fast in-situ synthesis according to claim 1, wherein the annealing temperature in the step (4) is 600 ℃, and the constant temperature holding time is 2 h.
5. The method for preparing the MOFs/ZnO composite gas-sensitive film responding to CO through the ultra-fast in-situ synthesis according to claim 1, wherein in the step (5), the Cu (NO) is3)2The concentration of the solution is 0.45mol/L, and the ZnO gas sensor is arranged in Cu (NO)3)2The reaction time in the solution was 1 min.
6. The method for preparing the MOFs/ZnO composite gas-sensitive film responding to CO through the ultra-fast in-situ synthesis according to claim 1, wherein in the step (5), the concentration of the organic ligand solution is 0.25mol/L, and the (Zn, Cu) (OH) NO is3The reaction time of the/ZnO film in the organic ligand solution was 30 s.
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| CN114369252A (en) * | 2020-10-14 | 2022-04-19 | 中国科学院福建物质结构研究所 | Method for preparing metal-organic framework film based on self-sacrifice metal oxide film template |
| CN113218984B (en) * | 2021-05-07 | 2022-07-05 | 河北工业大学 | Method for preparing sensitive element of humidity sensor |
| CN113447532B (en) * | 2021-06-25 | 2023-06-30 | 杭州电子科技大学 | Fe (Fe) 3 O 4 Preparation method of air sensor with@UiO-66 structure |
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