CN113670993A - Composite gas-sensitive material with hierarchical structure and preparation method and application thereof - Google Patents
Composite gas-sensitive material with hierarchical structure and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a composite gas-sensitive material with a hierarchical structure, a preparation method and application thereof, and belongs to the technical field of gas-sensitive materials. The method comprises the following steps: (1) preparing a zinc source solution, a cobalt source solution and an organic ligand solution; (2) dropwise adding the organic ligand solution into the cobalt salt solution, stirring, and performing ultrasonic dispersion to obtain a uniform solution; (3) dropwise adding a zinc salt solution into the solution, stirring, and performing ultrasonic dispersion to obtain a mixed solution; (4) standing the mixed solution for 24 hours, centrifuging, cleaning and drying; (5) and calcining the dried powder to obtain the composite gas-sensitive material taking the zinc oxide as a shell and the cobaltosic oxide as a core. According to the invention, the multilayer composite metal oxide is obtained by further calcining the MOF directly as a template, so that the characteristics of the nano material and the pore structure are fully utilized, and the influence of the structure and components of the gas-sensitive material on the gas-sensitive characteristics is effectively exerted. The gas sensor prepared from the material has high sensitivity to acetone reaction and low detection limit.
Description
Technical Field
The invention belongs to the field of gas sensors, and particularly relates to application research of inorganic metal oxides in the field of sensors, in particular to multi-element compounding of various inorganic nano particles, and response characteristics of harmful gases are detected.
Background
Metal Oxide Semiconductors (MOSs) have the characteristics of low cost and abundant resources. The sensor taking the nano-silver as the gas sensitive material has the characteristics of high sensitivity, quick response/recovery and the like. The microstructure and composition of the metal oxide has an important influence on the sensitive properties. The composite material with a hierarchical structure combines structural advantages and compositional advantages. From the viewpoint of material structure, on the one hand, the graded structure generally has a high specific surface area, and can provide sufficient surface adsorption sites for gas molecules. From the aspect of material components, the design of the junction material can bring special electronic effect, chemical effect and geometric effect to the composite material, thereby enhancing the sensitivity.
The properties, application, preparation cost and the like of the metal oxide matrix composite depend on the preparation technology to a large extent. The invention can realize double regulation of the structure and the components of the composite material in the preparation process, and has simple and convenient operation and controllable reaction conditions.
Disclosure of Invention
In order to overcome the problems of low sensitivity and poor selectivity of a single metal oxide gas sensor, two (or more) metal oxides are compounded and a hierarchical structure is constructed, so that the gas-sensitive property can be improved. According to the invention, the Metal Organic Framework (MOF) is used as a template, and the zinc oxide and cobaltosic oxide composite hierarchical structure material is obtained after calcination, compared with a pure-phase material, the reactivity of the material is greatly improved, so that the sensitivity and selectivity of the gas sensitive material can be improved, the response/recovery time is shortened, and the method has practical application value for further promoting the development of semiconductor gas sensitive devices.
Aiming at the defects of the prior art, the invention provides a graded composite gas-sensitive material and a preparation method thereof; specifically, the invention adopts a composite organic metal frame material as a template, combines with a calcination method, and prepares the graded composite gas-sensitive material by controlling the calcination temperature, time and gradient. The structure and components of the sensitive material are regulated and controlled simultaneously, and the influence of the morphology and composition of the gas sensitive material on the gas sensitive property is effectively exerted.
Yet another object of the present invention is to: provides a zinc oxide and cobaltosic oxide composite nano material product prepared by the method and application thereof.
The invention solves the technical problems by the following technical means:
a preparation method of a composite gas-sensitive material with a hierarchical structure comprises the following steps of preparing a composite gas-sensitive material with the hierarchical structure, wherein the composite gas-sensitive material comprises zinc oxide and cobaltosic oxide; the method comprises the following steps:
step 1, preparing a zinc source solution, a cobalt source solution and an organic ligand solution:
respectively dissolving zinc salt, cobalt salt and an organic ligand in an organic solution to obtain a zinc source solution, a cobalt source solution and an organic ligand solution with the concentration ratio of (2-4) to (1.5-3) to (6-12), and then performing ultrasonic dispersion to obtain a uniform solution;
dropwise adding an organic ligand solution into a cobalt source solution, and performing ultrasonic treatment; then, dropwise adding a zinc source solution into the mixed solution, and performing ultrasonic treatment; thereafter, the mixed solution was allowed to stand;
step 3 washing
Centrifugally cleaning the mixed solution after standing to obtain a precipitate;
step 4, drying
Drying the precipitate to obtain metal organic framework precursor powder;
step 5, calcining
And placing the dried metal organic frame precursor powder into a muffle furnace for calcination, wherein the calcination temperature is 300-600 ℃, the calcination gradient is 1-10 ℃/min, and the calcination time is 2-4 h, so as to obtain the composite gas-sensitive material with the hierarchical structure.
Further, in the above technical solution, the zinc salt is any one of zinc nitrate hexahydrate, zinc acetate dihydrate, zinc chloride and zinc sulfate heptahydrate, the cobalt salt includes any one of cobalt nitrate hexahydrate, cobalt acetate tetrahydrate, cobalt chloride hexahydrate and cobalt sulfate heptahydrate, and the organic ligand includes 2-methylimidazole; the organic solution comprises methanol.
Further, in the technical scheme, the ultrasonic dispersion time in the step 1 is 10-30 min.
Further, in the technical scheme, in the step 2, the organic ligand solution is dropwise added into the cobalt source solution at a dropping speed of 0.5-2 mL/s, and ultrasonic treatment is carried out for 10-30 min; dropwise adding a zinc source solution into the mixed solution at a dropping speed of 0.5-2 mL/s, and performing ultrasonic treatment for 30-60 min
Further, in the above technical scheme, in the step 2, the standing time of the mixed solution is 20-30 hours.
Further, in the technical scheme, the rotating speed of centrifugal cleaning in the step 3 is 7000-11000 r/min; the cleaning solution comprises methanol or absolute ethanol.
Further, in the technical scheme, in the step 4, the drying temperature is 50-70 ℃, and the drying time is 12-30 hours.
The composite gas-sensitive material with the hierarchical structure is prepared by the method.
An application of a composite gas-sensitive material with a hierarchical structure in preparing a semiconductor gas-sensitive device.
Further, in the above technical scheme, the composite gas sensitive material is coated on the surface of an electrode of the gas sensor to manufacture the indirectly heated gas sensor.
According to the invention, the multilayer composite metal oxide is obtained by further calcining the MOF directly as a template, so that the characteristics of the nano material and the pore structure are fully utilized, and the influence of the structure and components of the gas-sensitive material on the gas-sensitive characteristics is effectively exerted. The gas sensor prepared from the material has high sensitivity to acetone reaction and low detection limit.
Drawings
FIG. 1 is a scanning electron microscope image of the composite nanomaterial in example 1 of the present invention.
Fig. 2 is an XRD spectrum of the composite nanomaterial of example 2 of the present invention.
FIG. 3 is a scanning electron microscope image of the composite nanomaterial in example 3 of the present invention.
FIG. 4 is a flow chart of a preparation process of the graded composite gas-sensitive material according to embodiments 1 to 4 of the present invention.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
The preparation process flow of the ternary composite gas-sensitive material of the embodiments 1 to 4 is shown in fig. 4.
Example 1
Step 1. preparation of zinc source solution, cobalt source solution and organic ligand solution
Respectively dissolving 4.75mmol of zinc acetate dihydrate, 3.75mmol of cobalt acetate hexahydrate and 15mmol of 2-methylimidazole in 15mL, 15mL and 30mL of methanol solutions, and performing ultrasonic dispersion for 10min to obtain a uniform solution;
Dropwise adding the solution dissolved with 2-methylimidazole into the cobalt source solution at the dropping speed of 0.5mL/s, and then carrying out ultrasonic treatment for 10 min; then, dropwise adding a zinc source solution into the mixed solution at the dropping speed of 0.5mL/s, and then carrying out ultrasonic treatment for 30 min; after that, the mixed solution was left standing for 20 hours;
and step 3: washing machine
Centrifugally cleaning the mixed solution after standing at 7000r/min to obtain a precipitate;
and 4, step 4: drying
Placing the centrifuged sample in a vacuum drying oven for drying for 12h at 60 ℃ to obtain MOF precursor powder;
and 5: calcination of
Placing the dried MOF precursor powder in a muffle furnace, calcining for 2h at 6000 ℃ with the gradient of 2 ℃/min to obtain the composite gas-sensitive material with the hierarchical structure;
the obtained graded composite gas-sensitive material comprises zinc oxide and cobaltosic oxide, the obtained composite gas-sensitive material is coated on the surface of an electrode of a gas sensor to prepare an indirectly heated gas sensor, the lower limit of the detection of acetone gas at the optimal working temperature of 260 ℃ is as low as 1ppm, and the sensitivity is 2.5.
An SEM picture of the MOF precursor template in this example 1 is shown in fig. 1. In fig. 1, the samples are micron rhombohedral particles. The structure is consistent with the microstructure of ZIF-8 and ZIF-67 reported in the literature, and the successful preparation of the MOF precursor is demonstrated.
Example 2
Step 1. preparation of zinc source solution, cobalt source solution and organic ligand solution
Respectively dissolving 4.75mmol of zinc nitrate hexahydrate, 3.75mmol of cobalt nitrate hexahydrate and 15mmol of 2-methylimidazole in 15mL of methanol solution, 30mL of methanol solution and 15mL of methanol solution, and performing ultrasonic dispersion for 20min to obtain uniform solution;
Dropwise adding the solution dissolved with 2-methylimidazole into the cobalt source solution at the dropping speed of 0.5mL/s, and then carrying out ultrasonic treatment for 10 min; then, dropwise adding a zinc source solution into the mixed solution at the dropping speed of 0.5mL/s, and then carrying out ultrasonic treatment for 30 min; then, the mixed solution is kept still for 30 hours;
and step 3: washing machine
Centrifuging and cleaning the mixed solution after standing at 8000r/min to obtain a precipitate;
and 4, step 4: drying
Drying the centrifuged sample in a vacuum drying oven at 60 ℃ for 15h to obtain MOF precursor powder;
and 5: calcination of
Placing the dried MOF precursor powder in a muffle furnace, calcining for 2h at 400 ℃, and obtaining the composite gas-sensitive material with the hierarchical structure, wherein the gradient is 5 ℃/min;
the obtained graded composite gas-sensitive material comprises zinc oxide and cobaltosic oxide, the obtained composite gas-sensitive material is coated on the surface of an electrode of a gas sensor to prepare an indirectly heated gas sensor, the lower limit of the detection of acetone gas at the optimal working temperature of 260 ℃ is as low as 1ppm, and the sensitivity is 2.
An XRD detection pattern of the composite gas-sensitive material obtained in this example 2 is shown in fig. 2. In the figure, the characteristic diffraction peaks of zinc oxide and cobaltosic oxide appear on the curve, which shows that the zinc oxide and cobaltosic oxide composite material is successfully prepared.
Example 3
Step 1. preparation of zinc source solution, cobalt source solution and organic ligand solution
Respectively dissolving 4.75mmol of zinc nitrate hexahydrate, 3.75mmol of cobalt nitrate hexahydrate and 15mmol of 2-methylimidazole in 15mL, 20mL and 25mL of methanol solutions, and performing ultrasonic dispersion for 30min to obtain uniform solutions;
Dropwise adding the solution dissolved with 2-methylimidazole into the cobalt source solution at the dropping speed of 1mL/s, and then carrying out ultrasonic treatment for 20 min; then, dropwise adding a zinc source solution into the mixed solution at the dropping speed of 1mL/s, and then carrying out ultrasonic treatment for 20 min; after that, the mixed solution was left standing for 24 hours;
step 3 washing
Centrifuging and cleaning the mixed solution after standing at 10000r/min to obtain a precipitate;
step 4, drying
Drying the centrifuged sample in a vacuum drying oven at 60 ℃ for 20h to obtain MOF precursor powder;
step 5, calcining
Placing the dried MOF precursor powder in a muffle furnace, calcining for 3h at 300 ℃, wherein the gradient is 10 ℃/min, and obtaining the composite gas-sensitive material with the hierarchical structure;
the obtained graded composite gas-sensitive material comprises zinc oxide and cobaltosic oxide, the obtained composite gas-sensitive material is coated on the surface of an electrode of a gas sensor to prepare an indirectly heated gas sensor, the lower limit of the detection of acetone gas at the optimal working temperature of 260 ℃ is as low as 0.5ppm, and the sensitivity is 4.
A TEM image of the composite gas-sensitive material prepared in this example 3 is shown in fig. 3. As can be seen from the figure, the composite material core-shell structure has obvious gaps between the core and the shell, and the structure is loose and porous. Indicating that the graded composite material has been successfully prepared.
Example 4
Step 1. preparation of zinc source solution, cobalt source solution and organic ligand solution
Respectively dissolving 4.75mmol of zinc chloride, 3.75mmol of cobalt chloride hexahydrate and 15mmol of 2-methylimidazole in 30mL of methanol solution, 15mL of methanol solution and 15mL of methanol solution, and performing ultrasonic dispersion for 25min to obtain uniform solution;
Dropwise adding the solution dissolved with 2-methylimidazole into the cobalt source solution at the dropping speed of 0.5mL/s, and then carrying out ultrasonic treatment for 20 min; then, dropwise adding a zinc source solution into the mixed solution at the dropping speed of 1mL/s, and then carrying out ultrasonic treatment for 40 min;
and step 3: washing machine
Centrifugally cleaning the mixed solution after standing at 9000r/min to obtain a precipitate;
and 4, step 4: drying
Placing the centrifuged sample in a vacuum drying oven for drying for 14h at 70 ℃ to obtain MOF precursor powder;
and 5: calcination of
Placing the dried MOF precursor powder in a muffle furnace, calcining for 3h at 300 ℃, wherein the gradient is 10 ℃/min, and obtaining the composite gas-sensitive material with the hierarchical structure;
the obtained graded composite gas-sensitive material comprises zinc oxide and cobaltosic oxide, the obtained composite gas-sensitive material is coated on the surface of an electrode of a gas sensor to prepare an indirectly heated gas sensor, the lower limit of the detection of acetone gas at the optimal working temperature of 260 ℃ is as low as 1ppm, and the sensitivity is 2.2.
Claims (10)
1. The preparation method of the composite gas-sensitive material with the hierarchical structure is characterized in that the composite gas-sensitive material with the hierarchical structure comprises zinc oxide and cobaltosic oxide; the method comprises the following steps:
step 1, preparing a zinc source solution, a cobalt source solution and an organic ligand solution:
respectively dissolving zinc salt, cobalt salt and an organic ligand in an organic solution to obtain a zinc source solution, a cobalt source solution and an organic ligand solution with the concentration ratio of (2-4) to (1.5-3) to (6-12), and then performing ultrasonic dispersion to obtain a uniform solution;
step 2, preparing a metal organic framework precursor solution:
dropwise adding an organic ligand solution into a cobalt source solution, and performing ultrasonic treatment; then, dropwise adding a zinc source solution into the mixed solution, and performing ultrasonic treatment; thereafter, the mixed solution was allowed to stand;
step 3 washing
Centrifugally cleaning the mixed solution after standing to obtain a precipitate;
step 4, drying
Drying the precipitate to obtain metal organic framework precursor powder;
step 5, calcining
And placing the dried metal organic frame precursor powder into a muffle furnace for calcination, wherein the calcination temperature is 300-600 ℃, the calcination gradient is 1-10 ℃/min, and the calcination time is 2-4 h, so as to obtain the composite gas-sensitive material with the hierarchical structure.
2. The method for preparing the composite gas-sensitive material with the hierarchical structure according to claim 1, wherein the zinc salt is any one of zinc nitrate hexahydrate, zinc acetate dihydrate, zinc chloride and zinc sulfate heptahydrate, the cobalt salt comprises any one of cobalt nitrate hexahydrate, cobalt acetate tetrahydrate, cobalt chloride hexahydrate and cobalt sulfate heptahydrate, and the organic ligand comprises 2-methylimidazole; the organic solution comprises methanol.
3. The preparation method of the composite gas-sensitive material with the hierarchical structure according to claim 1, wherein the time for ultrasonic dispersion in the step 1 is 10-30 min.
4. The preparation method of the composite gas-sensitive material with the hierarchical structure according to claim 1, wherein in the step 2, the organic ligand solution is dropwise added into the cobalt source solution at a dropping speed of 0.5-2 mL/s for 10-30 min by ultrasound; and dropwise adding the zinc source solution into the mixed solution at the dropping speed of 0.5-2 mL/s, and carrying out ultrasonic treatment for 30-60 min.
5. The method for preparing the composite gas-sensitive material with the hierarchical structure according to claim 1, wherein in the step 2, the standing time of the mixed solution is 20-30 h.
6. The preparation method of the composite gas-sensitive material with the hierarchical structure according to claim 1, wherein the rotation speed of centrifugal cleaning in the step 3 is 7000-11000 r/min; the cleaning solution comprises methanol or absolute ethanol.
7. The preparation method of the composite gas-sensitive material with the hierarchical structure according to claim 1, wherein in the step 4, the drying temperature is 50-70 ℃ and the drying time is 12-30 h.
8. The composite gas-sensitive material with a graded structure prepared by the preparation method of any one of claims 1 to 7.
9. Use of the composite gas-sensitive material having a graded structure according to claim 8 in the preparation of a semiconductor gas-sensitive device.
10. The application of claim 9, wherein the composite gas-sensitive material is coated on the surface of an electrode of a gas sensor to form an indirectly heated gas sensor.
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