CN110749628A - Acetone-sensitive cobaltosic oxide/zinc oxide nano-meter rice heterojunction thin film - Google Patents
Acetone-sensitive cobaltosic oxide/zinc oxide nano-meter rice heterojunction thin film Download PDFInfo
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- 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
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- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention provides a preparation method of a cobaltosic oxide/zinc oxide nanoflower heterojunction film for low-concentration acetone detection, and belongs to the technical field of gas sensors. Firstly, a ZIF-67/ZIF-8 precursor is synthesized by taking a cobalt source, a zinc source and imidazole as reactants under the solvothermal condition and methanol as a solvent, then the mixture is calcined in a tube furnace to obtain a cobaltosic oxide/zinc oxide nano flower compound, finally, a cobaltosic oxide/zinc oxide device is prepared by using a dripping coating method, and the sensitivity of pure cobaltosic oxide nano flowers and the sensitivity of the compound cobaltosic oxide/zinc oxide nano flowers to acetone are compared. The sample still had a higher response value (298%) and shorter response/recovery time (16 sec/25 sec) at 10ppm acetone. The sensor film has the advantages of simple preparation method, low raw material cost, excellent material film performance and good application value and prospect.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to preparation of a cobaltosic oxide/zinc oxide nanoflower heterojunction film derived from MOF (metal organic framework) and research on gas-sensitive performance of the film on acetone.
Background
Acetone is an organic solvent for manufacturing materials such as explosives, rubber, plastics, fibers and the like, is also a raw material for synthesizing organic matters such as ketene, polyisoprene rubber, epoxy resin and the like, and has wide application in the fields of military affairs, chemical engineering, medical treatment and the like (Sens. activators B: chem.,2015,209, 368-376). However, acetone gas, as a colorless toxic gas, causes irreversible damage to the human body and the environment. The human body is exposed in the acetone atmosphere for a long time, even trace (less than or equal to 1ppm) of acetone can cause chronic poisoning phenomena such as inflammation of the nose, throat and lung, headache, dizziness, regurgitation and the like of the human body, and the heart, the kidney and the nervous system of the human body can be damaged more seriously. Although high concentrations of acetone are perceived by olfaction (human acetone olfactory threshold of about 100ppm), low concentrations of acetone are not perceived by olfaction. In addition, in the medical field, diabetes mellitus (healthy person: 0.3-0.9ppm, diabetic person: higher than 1.8ppm) can be diagnosed by detecting trace acetone concentration in exhaled breath of human body (adv. Mater.,2017,29, 1700737). Therefore, the method has very important scientific significance and application value in the fields of environmental monitoring, disease diagnosis and the like for the real-time monitoring of trace acetone in a specific environment.
Metal oxides are widely used for gas detection due to their advantages of simple structure, low price, convenient operation, high gas responsiveness, etc. Cobaltosic oxide is a common p-type semiconductor, and research shows that the Cobaltosic oxide has better gas sensitivity performance to acetone gas (Sens. activators B: chem.,2017,242, 369-377). Most of the cobaltosic oxide sensors studied so far are composed of nanofibers (Sens. activators B: Chem,2019,297, 126-. Among them, cobaltosic oxide derived from ZIF-67 (zeolitic imidazolate framework-67) has been widely studied because of its very large specific surface area, abundant pore structure, and good catalytic properties for acetone molecules. However, pure cobaltosic oxide still has some disadvantages, such as being suitable for detecting high concentration acetone (higher than 100ppm), poor detection performance for trace acetone, and too long response time and recovery time.
In recent years, novel two-dimensional graphene-like materials have been widely used in the fields of tribology, electrochemistry, optics, and the like due to their special structures and excellent properties. Among them, cobaltosic oxide/zinc oxide nanoflower derived from ZIF-67 (zeolitic imidazolate framework-67)/ZIF-8 (zeolitic imidazolate framework-8) is used as a derivative of MOF, and thus has a relatively large specific surface area, and a rich surface pore structure, and thus has a significant gas adsorption capacity, and thus can play a certain role in the field of gas sensing. However, the ZIF-67/ZIF-8 derived cobaltosic oxide/zinc oxide nanoflowers are reported in the literature to be detected by applying acetone gas.
In order to realize high-sensitivity and rapid detection of low-concentration acetone, a ZIF-67/ZIF-8 precursor is synthesized by taking a cobalt source, a zinc source and imidazole as reactants under a solvothermal condition and taking methanol as a solvent, then the mixture is calcined in a tube furnace to obtain a cobaltosic oxide/zinc oxide nanoflower compound, finally a cobaltosic oxide/zinc oxide device is prepared by a dripping method, and the sensitivity of pure cobaltosic oxide and the compounded cobaltosic oxide/zinc oxide nanoflower to acetone is compared. The cobaltosic oxide/zinc oxide nanoflower can be prepared only under the condition of heat of solution, the method is simple, the response recovery time to low-concentration acetone is short, the stability is high, and the work has important guiding significance for developing low-concentration acetone sensors.
Disclosure of Invention
The invention aims to provide a preparation method of a sensor film capable of detecting low-concentration acetone. Firstly, preparing a cobaltosic oxide/zinc oxide nano-meter rice composite structure, and then preparing a film by a dripping coating method. The preparation method has the characteristics of low cost, simple operation, convenience, rapidness and the like.
The implementation of the invention is briefly described below by taking cobalt nitrate hexahydrate as an example. Firstly, preparing ZIF-67/ZIF-8 nanometer flower composite structure powder, and then calcining to obtain cobaltosic oxide/zinc oxide nanometer flower black powder. And ultrasonically stirring and uniformly mixing a proper amount of powder and deionized water, dripping the mixture on a platinum interdigital electrode, drying the membrane, placing the membrane in an oven, drying the membrane for 2 hours at 60 ℃, and taking out the membrane to obtain the test substrate. The cobaltosic oxide/zinc oxide device can be realized by the following specific steps:
(1) dissolving a certain amount of cobalt nitrate hexahydrate and zinc nitrate hexahydrate in a certain amount of methanol solution, and stirring for 15 minutes;
(2) dissolving a certain amount of dimethyl imidazole in a certain amount of methanol solution, and stirring for 15 minutes;
(3) quickly injecting the dimethyl imidazole solution in the step (2) into the zinc-cobalt source solution in the step (1), and stirring for 15 minutes;
(4) pouring the solution in the step (3) into a 100 ml reaction kettle, and carrying out hydrothermal reaction for 1.5 hours at 120 ℃;
(5) centrifuging and washing the product obtained in the step (4) for multiple times by using a methanol solution, and drying the centrifuged product at 70 ℃ in vacuum to obtain brown yellow ZIF-67/ZIF-8 nano flower powder;
(6) putting the ZIF-67/ZIF-8 nanometer flower powder obtained in the step (5) into a tube furnace, calcining for 2 hours in an air atmosphere at 400 ℃, wherein the heating rate is 2 ℃ per minute, and calcining to obtain cobaltosic oxide/zinc oxide nanometer flower black powder;
(7) taking a proper amount of cobaltosic oxide/zinc oxide nano-flower powder, dispersing the powder by using deionized water, then dripping the powder on a ceramic chip printed with a platinum interdigital electrode, putting the dripped film in an oven for 2 hours after the dripped film is completely dried, and setting the temperature in the oven to be 60 ℃, and finally obtaining the test substrate.
The cobaltosic oxide/zinc oxide device can be obtained by the process. When zinc nitrate hexahydrate is not added, the ZIF-67 nano flowers are directly calcined to obtain pure cobaltosic oxide nano flowers. Comparing the response of pure cobaltosic oxide nanoflower and cobaltosic oxide/zinc oxide nanoflower to 10ppm acetone at 300 ℃, the gas-sensitive performance of the cobaltosic oxide/zinc oxide nanoflower to the acetone is found to be best, the response value is 298%, and the response/recovery time is only 16 seconds/25 seconds. At the same time, we also tested the response of cobaltosic oxide/zinc oxide nanoflower to 500ppb-10ppm acetone and found that it still has a good characteristic curve. And 10ppm acetone is subjected to cycle test, so that the product has good stability and can meet the requirements of practical application.
The preparation method of the cobaltosic oxide/zinc oxide nanoflower heterojunction film provided by the invention can realize detection of low-concentration acetone, and response/recovery time is short. The method has the advantages of simple preparation, low raw material cost, good repeatability, and good application value and prospect.
Drawings
FIG. 1 is a scanning electron microscope photograph of ZIF-67 nanoflower, ZIF-67/ZIF-8 nanoflower, and cobaltosic oxide/zinc oxide nanoflower composites.
FIG. 2 is a graph showing the response of pure cobaltosic oxide, cobaltosic oxide/zinc oxide nanoflower composite material to 500ppb-10ppm acetone on-off gas at 300 ℃.
FIG. 3 is a graph of resistance cycling test of cobaltosic oxide/zinc oxide nanoflowers against 10ppm acetone at 300 ℃.
Detailed Description
The present invention is described in detail below with reference to the drawings and examples.
In example 1, 0.8294 g of cobalt nitrate hexahydrate and 0.0446 g of zinc nitrate hexahydrate were dissolved in 25 ml of methanol solution and stirred for 15 minutes as solution A. 0.328 g of dimethylimidazole was dissolved in 25 ml of methanol and stirred for 15 minutes, which was designated as solution B. Solution B was quickly poured into solution a and stirred for 15 minutes, as solution C. The solution C was poured into a 100 ml reaction vessel and reacted at 120 ℃ for 1.5 hours. And centrifuging and washing the obtained product for multiple times by using a methanol solution, and then putting the product into a vacuum drying oven at 70 ℃ for drying overnight to obtain a ZIF-67/ZIF-8 nanometer flower yellow product. And (3) placing the ZIF-67ZIF-8 nanoflower powder in a tube furnace, carrying out heat treatment for 2 hours at 400 ℃ in an air atmosphere, wherein the heating rate is 2 ℃ per minute, and finally obtaining the cobaltosic oxide/zinc oxide nanoflower compound black powder. And when no zinc nitrate hexahydrate is added into the solution A, carrying out hydro-thermal synthesis to obtain ZIF-67 nano-flower powder, putting the ZIF-67 nano-flower powder into a tubular furnace, carrying out heat treatment for 2 hours at 400 ℃ in an air atmosphere, and carrying out heating rate of 2 ℃ per minute to obtain pure cobaltosic oxide nano-flower powder. Respectively taking a proper amount of pure cobaltosic oxide nanoflowers and composite cobaltosic oxide/zinc oxide nanoflower powder, dispersing the powders by using deionized water, then dripping the powders on a ceramic chip printed with a platinum interdigital electrode, putting the dripped film in an oven for 2 hours after the dripped film is completely dried, and setting the temperature in the oven to be 60 ℃ to finally obtain a test substrate. Scanning electron microscopy of test samples as shown in FIG. 1, from FIG. 1(a) it can be seen that ZIF-67 is a typical flower-like structure, approximately 2 microns in size and only a few nanometers in thickness; from FIG. 1(b), it can be seen that ZIF-67/ZIF-8 are still typical flower-like structures; it is apparent from fig. 1(c) that the flower-like structure of the obtained cobaltosic oxide/zinc oxide composite material is still intact after heat treatment, and the structure is not damaged.
Sensor sensitivity (%) calculation method: for p-type oxide semiconductors, S ═ Rg-Ra)/RaX 100; for n-type oxide semiconductors, S ═ R (R)a-Rg)/RaX 100. Wherein R isgIs the resistance of the sensor in an acetone atmosphere, RaIs the resistance of the sensor under air. The response time of the sensor is defined as: the time from the contact of the measured gas with a certain concentration to the time when the resistance value reaches 90% of the steady-state resistance value under the concentration; the recovery time is defined as: from the time of disengagement with the measured gas of a certain concentration to the time required for the resistance value to recover 90% of the changed resistance value. To investigate the response of different materials to acetone and to explore better acetone performance, the responses of pure tricobalt tetraoxide nanoflower and the tricobalt tetraoxide/zinc oxide nanoflower compound to 500ppb to 10ppm acetone at 300 ℃ were compared, as shown in fig. 2. It is known that pure cobaltosic oxide responds very little to low concentrations of acetone and cannot be fully recovered. The zinc oxide/cobaltosic oxide has better response to low-concentration acetone, the response value of the zinc oxide/cobaltosic oxide to 10ppm acetone reaches 298%, the improvement is obvious compared with that of pure cobaltosic oxide, and the response/recovery speed is greatly improved (16 seconds/25 seconds).
Figure 3 shows a graph of the response cycle test of cobaltosic oxide/zinc oxide nanoflowers to 10ppm acetone at 300 c. Therefore, the cobaltosic oxide/zinc oxide nano-meter rice still has a good response curve under a lower concentration, has good stability and can meet the detection requirement of low-concentration acetone.
Claims (1)
1. A method of preparing an acetone-sensitive cobaltosic oxide/zinc oxide nanocomposite film, comprising:
(1) dissolving a certain amount of cobalt nitrate hexahydrate and zinc nitrate hexahydrate in a certain amount of methanol solution, and stirring for 15 minutes;
(2) dissolving a certain amount of dimethyl imidazole in a certain amount of methanol solution, and stirring for 15 minutes;
(3) quickly injecting the dimethyl imidazole solution in the step (2) into the zinc-cobalt source solution in the step (1), and stirring for 15 minutes;
(4) pouring the solution in the step (3) into a 100 ml reaction kettle, and carrying out hydrothermal reaction for 1.5 hours at 120 ℃;
(5) centrifuging and washing the product obtained in the step (4) for multiple times by using a methanol solution, and drying the centrifuged product in a vacuum drying oven at 70 ℃ to obtain brown yellow ZIF-67/ZIF-8 nano flower powder;
(6) putting the ZIF-67/ZIF-8 nanometer flower powder obtained in the step (5) into a tube furnace, calcining for 2 hours in an air atmosphere at 400 ℃, wherein the heating rate is 2 ℃ per minute, and calcining to obtain cobaltosic oxide/zinc oxide nanometer flower black powder;
(7) taking a proper amount of cobaltosic oxide/zinc oxide nano-flower powder, dispersing the powder by using deionized water, then dripping the powder on a ceramic chip printed with a platinum interdigital electrode, putting the dripped film in an oven for 2 hours after the dripped film is completely dried, and setting the temperature in the oven to be 60 ℃, and finally obtaining the test substrate.
The cobaltosic oxide/zinc oxide nano-crystalline rice obtained by the process also has high response to low-concentration acetone, and has high response/recovery speed and good stability.
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Cited By (4)
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| CN111269431A (en) * | 2020-03-09 | 2020-06-12 | 广东石油化工学院 | Preparation method of ZIF-67 nanoflower |
| CN112642433A (en) * | 2020-12-29 | 2021-04-13 | 西安交通大学 | Preparation method of two-dimensional flaky porous composite oxide and application of two-dimensional flaky porous composite oxide in control of chlorine-containing volatile organic pollutants |
| 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 |
| CN114797928A (en) * | 2021-01-27 | 2022-07-29 | 中国科学院大连化学物理研究所 | Core-shell ZIFs pyrolysis derived porous carbon material cobalt catalyst and preparation method thereof |
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