CN109052453B - ZnCo2O4/ZnO heterostructure composite gas sensitive material and preparation method thereof - Google Patents
ZnCo2O4/ZnO heterostructure composite gas sensitive material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ZnCo catalyst2O4the/ZnO heterostructure composite gas-sensitive material is formed by compounding flaky zinc oxide and zinc cobaltate, wherein the zinc oxide accounts for 4-13.6% of the mass percentage. The invention changes Zn (CH)3COO)2•2H2O and Co (CH)3COO)2·4H2The addition of O synthesizes ZnCo containing ZnO with different contents2O4the/ZnO heterostructure composite gas-sensitive material. This means that we can synthesize ZnO with different doping ratios by controlling the molar ratio of Zn and Co to prepare ZnCo2O4the/ZnO heterostructure composite gas-sensitive material has good sensitivity to triethylamine and has wide application prospect in the aspect of manufacturing novel efficient gas sensors.
Description
Technical Field
The invention relates to the field of nano composite materials, in particular to ZnCo2O4a/ZnO heterostructure composite gas-sensitive material and a preparation method thereof.
Background
The rapid and accurate detection of toxic and harmful gases in the environment has important significance for environmental protection. The gas sensor based on the metal oxide semiconductor gas sensitive material becomes an important gas detection means due to the advantages of high sensitivity, quick response, simple manufacturing method, small volume, low price and the like. The metal oxide semiconductor gas-sensitive material is a core component of the gas sensor, and the gas-sensitive performance of the metal oxide semiconductor gas-sensitive material directly influences the performance and the application of the gas sensor. Therefore, designing and preparing a novel metal oxide semiconductor material with high-efficiency gas-sensitive performance has important significance for improving the performance of the gas sensor, and becomes one of the key research directions in the field of semiconductor gas sensors.
As a typical p-type metal oxide semiconductor, ZnCo2O4Gas sensors are one of the most extensively studied materials. However, ZnCo is poor in selectivity and low in responsiveness2O4And rarely used alone as a sensing material. To date, there have been many methods for improving the sensing performance of p-type materials, such as doping another oxide to form a composite material to design a p-n heterojunction, which is an effective method for improving the sensing performance. For example, Alali et al devised CeO2/ZnCo2O4Nanotubes and pure CeO2Compared with the nano tube, the response and the selectivity of the nano tube to the ethanol gas at the optimal temperature of 180 ℃ are obviously improved(Rsc Advances, 6 (2016) 101626-101637)Qixu et al reported CuO/ZnOp-n heterojunction nanorods (Sensors & Actuators B Chemical, 225 (2016) 16-23) SnO reported by Shouli Bai et al2/NiO(Applied Surface Science, 437 (2017) 304-313)And the like.
ZnO is a typical n-type metal oxide semiconductor with a wide bandgap energy of 3.37 eV. It is also one of the most deeply studied sensing materials. Previous papers have reported that ZnO typically exhibits effective sensing performance against various toxic gases such as ethanol, TEA and acetone at operating temperatures as high as 260-. Therefore, we have adopted ZnO to modify ZnCo2O4. Currently about ZnO/ZnCo2O4Reports of nanocomposites include: ZnO/ZnCo2O4Hollow core-shell nano cage(Nanoscale, 8 (2016) 16349-16357)Porous ZnO/ZnCo2O4Hollow ball( Journal of Materials Chemistry A, 2 (2014) 17683-17690)Hollow tubular ZnO/ZnCo2O4Nano-structure(RSC Adv, 7 (2017) 11428- 11438)And the like. At present, the ZnO porous nanosheet and ZnCo2O4Three assembled by nano sheetsFlower-like ZnO/ZnCo2O4The p-n heterojunction nano composite material and the preparation method thereof are not reported in the literature at present. Therefore, it is necessary to develop a ZnO/ZnCo-based material2O4A gas sensor of p-n heterojunction nanocomposite material.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides ZnCo2O4Composite gas-sensitive material with/ZnO heterostructure and preparation method thereof, and prepared ZnO/ZnCo2O4The composite gas-sensitive material has good sensitivity to triethylamine, and has wide application prospect in the aspect of manufacturing novel efficient gas sensors.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
ZnCo2O4a/ZnO heterostructure composite gas sensitive material, the ZnCo2O4the/ZnO heterostructure composite gas-sensitive material is formed by compounding flaky zinc oxide and zinc cobaltate, wherein the zinc oxide accounts for 4-13.6% of the mass percentage.
Preferably, the zinc oxide accounts for 5% by mass.
In addition, another object of the present invention is to provide a ZnCo2O4The preparation method of the/ZnO heterostructure composite gas-sensitive material comprises the following steps:
step one, under the condition of electromagnetic stirring, 10 mL of NH with the concentration of 0.38mol/L4HCO3The aqueous solution is slowly dropped with Zn (CH)3COO)2·2H2O and Co (CH)3COO)2·4H2Adding 30 mL of O into the water solution, and continuing to electromagnetically stir for 10-20 minutes after the dropwise adding is finished to prepare a precursor solution, wherein Zn (CH)3COO)2·2H2O content of 0.54-1.7 g, Co (CH)3COO)2·4H2The content of O is 1.5 g;
step two, transferring the obtained precursor solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, sealing the autoclave, preserving the heat for 12-24 hours at the temperature of 180-200 ℃, naturally cooling to room temperature, collecting a product through centrifugation, repeatedly washing the obtained product with deionized water and absolute ethyl alcohol, and drying at the temperature of 60-80 ℃ for 12-24 hours to obtain a sacrificial template;
step three, using the sacrificial template prepared in the step two as a self-sacrificial template, heating the template to 400-600 ℃ in the air at the heating rate of 2-4 ℃/min, and annealing for 2 hours to obtain ZnCo2O4the/ZnO heterostructure composite gas-sensitive material.
Further, in the second step, the product is washed with deionized water and absolute ethyl alcohol respectively for four times.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention changes Zn (CH)3COO)2•2H2O and Co (CH)3COO)2·4H2The addition of O synthesizes ZnCo containing ZnO with different contents2O4the/ZnO heterostructure composite gas-sensitive material. This means that we can synthesize ZnO with different doping ratios by controlling the molar ratio of Zn and Co to prepare ZnCo2O4the/ZnO heterostructure composite gas-sensitive material has good sensitivity to triethylamine and has wide application prospect in the aspect of manufacturing novel efficient gas sensors.
2. The invention adopts a precursor synthesized by hydrothermal method as a sacrificial template, zinc acetate dihydrate as a zinc source and cobalt acetate tetrahydrate as a cobalt source, and can realize ZnCo self-assembly of porous nanosheets by regulating and controlling the amount of zinc and cobalt2O4Controllable preparation of the/ZnO heterostructure composite gas-sensitive material on the appearance and components; the porous nano material with the same shape and characteristics as the sacrificial template can be prepared by utilizing the shape and genetic characteristics of the sacrificial template, and the shape and characteristics of the sacrificial template are completely inherited to ZnO/ZnCo through the heat treatment process2O4The components of the sacrificial template can be controlled by controlling the addition of each reagent, thereby controlling the prepared flower-shaped ZnCo2O4The content of ZnO in the/ZnO heterostructure composite gas-sensitive material.
Drawings
FIG. 1 shows the ZnO contents of different materials in the examples of the present inventionAmount of ZnCo2O4XRD spectrogram of the/ZnO heterostructure composite gas-sensitive material; (a) ZnCo prepared for example 12O4XRD spectrogram of the/ZnO heterostructure composite gas-sensitive material; (b) ZnCo prepared for example 22O4XRD spectrogram of the/ZnO heterostructure composite gas-sensitive material; (c) ZnCo prepared for example 32O4XRD spectrogram of the/ZnO heterostructure composite gas-sensitive material.
FIG. 2 shows ZnCo with ZnO contents of 5% and 13.6% by mass in the example of the present invention2O4Scanning electron microscope photos of the overall micro-morphology of the/ZnO heterostructure composite gas-sensitive material; (a) ZnCo prepared for example 22O4the/ZnO heterostructure composite gas-sensitive material is magnified to a scanning electron microscope picture of 10 mu m; (b) ZnCo prepared for example 22O4A scanning electron microscope photo of the/ZnO heterostructure composite gas-sensitive material amplified to 1 mu m; (c) ZnCo prepared for example 42O4the/ZnO heterostructure composite gas-sensitive material is magnified to a scanning electron microscope picture of 10 mu m; (d) ZnCo prepared in example 42O4And the scanning electron microscope picture of the/ZnO heterostructure composite gas-sensitive material is magnified to 1 mu m.
FIG. 3 (a) shows ZnCo obtained in example 2 of the present invention2O4High resolution of/ZnO heterostructure composite gas sensitive material, 3 (b) ZnCo prepared in example 3 of the present invention2O4High resolution diagram of the/ZnO heterostructure composite gas-sensitive material.
FIG. 4 is a sensitivity curve of the ZnCo2O4/ZnO heterostructure composite gas-sensitive material at 220 ℃ for triethylamine gas with different concentrations in the embodiment of the invention.
FIG. 5 is a relation curve of triethylamine gas concentration and response value at 220 ℃ of the ZnCo2O4/ZnO heterostructure composite gas-sensitive material prepared in example 2 of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and examples. The specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
Under the condition of electromagnetic stirring, 10 mL of NH with the concentration of 0.38mol/L4HCO3The aqueous solution was slowly dropped to a container containing 0.72gZn (CH)3COO)2·2H2O and 1.5 gCo (CH)3COO)2·4H2After the dropwise addition of the O into 30 mL of the aqueous solution, continuing to electromagnetically stir for 10 minutes to prepare a precursor solution; transferring the obtained precursor solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, sealing the autoclave, preserving the heat for 24 hours at 180 ℃, naturally cooling to room temperature, collecting a product by centrifugation, washing the product with deionized water and absolute ethyl alcohol for four times respectively, and drying the product for 12 hours at 60 ℃ to obtain a sacrificial template; heating the sacrificial template prepared in the step two to 500 ℃ in the air by using the sacrificial template as a self-sacrificial template, wherein the heating rate is 2 ℃/min, and annealing for 2 hours to obtain ZnCo2O4Composite gas-sensitive material with/ZnO heterostructure and prepared ZnCo2O4The mass fraction of ZnO in the/ZnO heterostructure composite gas-sensitive material is 4%. ZnCo produced in this example2O4The XRD spectrum of the/ZnO heterostructure composite gas-sensitive material is shown in figure 1 (a).
Example 2
Under the condition of electromagnetic stirring, 10 mL of NH with the concentration of 0.38mol/L4HCO3The aqueous solution was slowly dropped to a container containing 0.78gZn (CH)3COO)2·2H2O and 1.5 gCo (CH)3COO)2·4H2After the dropwise addition of the O into 30 mL of the aqueous solution, continuing to electromagnetically stir for 20 minutes to prepare a precursor solution; transferring the obtained precursor solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, sealing the autoclave, preserving the heat for 24 hours at 180 ℃, naturally cooling to room temperature, collecting a product by centrifugation, washing the product with deionized water and absolute ethyl alcohol for four times respectively, and drying the product for 12 hours at 60 ℃ to obtain a sacrificial template; heating the sacrificial template prepared in the step two to 500 ℃ in the air by using the sacrificial template as a self-sacrificial template, wherein the heating rate is 2 ℃/min, and annealing for 2 hours to obtain ZnCo2O4Composite gas-sensitive material with/ZnO heterostructure and prepared ZnCo2O4The mass fraction of ZnO in the/ZnO heterostructure composite gas-sensitive material is 5%. ZnCo produced in this example2O4The XRD spectrum of the/ZnO heterostructure composite gas-sensitive material is shown in figure 1 (b). FIGS. 2(a) and 2(b) are respectively a ZnCo film obtained in this example2O4The electron microscope scanning photographs of the/ZnO heterostructure composite gas-sensitive material magnified to 10 μm and 1 μm can observe that the nanoflowers are in close contact with each other and have a diameter of about 4 μm, and further, many pores on the nanosheets can be observed. The specific surface area of the powder is 28.829 m2/ g-1FIG. 3 (a) is a transmission diagram of the sample, in which ZnO and ZnCo are clearly shown2O4Presence of heterostructures at the interface.
Taking the appropriate amount of ZnCo prepared in the embodiment2O4the/ZnO heterostructure composite gas sensitive material was mixed with ethanol to form a uniform paste, and then applied on the surface of an Ag-Pd ceramic substrate (13.4 mm. times.7 mm) with a brush, and dried and aged at room temperature to obtain a resistive sensor. The gas sensing test was performed on a CGS-4TPS (beijing elite technologies, ltd, china) intelligent gas sensing analysis system. The gas sensitive test employs a static gas dispensing method, during which a micro-syringe is used to inject the desired amount of target gas into the test chamber. The response of the sensor is defined as Rg/RaWherein R isaAnd RgThe sensor resistances in air and the target gas, respectively.
In the experiment, the gas distribution mode of the detected gas is as follows (the detected gas is liquid at normal temperature, gas is generated by evaporation and dissolution, and the injected detected liquid needs to be converted into gas concentration), and the converted gas concentration can be according to the formula:
where Vx is the volume (mL) of the liquid taken by the gas to be detected, V is the volume (1.8L) of the gas distribution box, C is the concentration (ppm) of the gas to be detected, M is the molecular weight (g/mol) of the liquid, and d is the specific gravity (g/cm) of the liquid3) And ρ represents the liquid purity, TrAt room temperature ofoC)，TbFor the temperature in the gas distribution box (oC) In that respect Thus, the number of milliliters of liquid injected into the test vessel can be calculated based on the corresponding volume of gas (ppm) to be measured. The results are shown in FIG. 4, and the test results show that the dynamic response curve at 220 ℃ and the sensitivity to 100 ppm triethylamine are 5.41, and ZnCo shown in FIG. 52O4The relation curve of triethylamine gas concentration and response value of the/ZnO heterostructure composite gas-sensitive material at 220 ℃ shows that the response value gradually approaches saturation along with the increase of the triethylamine gas concentration.
Example 3
Under the condition of electromagnetic stirring, 10 mL of NH with the concentration of 0.38mol/L4HCO3Slowly adding dropwise water solution containing 1gZn (CH)3COO)2·2H2O and 1.5 gCo (CH)3COO)2·4H2After the dropwise addition of the O into 30 mL of the aqueous solution, continuing to electromagnetically stir for 15 minutes to prepare a precursor solution; transferring the obtained precursor solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, sealing the autoclave, preserving the heat for 20 hours at 190 ℃, naturally cooling the autoclave to room temperature, collecting the product by centrifugation, washing the product with deionized water and absolute ethyl alcohol for four times respectively, and drying the product for 18 hours at 70 ℃ to obtain a sacrificial template; heating the sacrificial template prepared in the step two to 550 ℃ in the air by using the sacrificial template as a self-sacrificial template, wherein the heating rate is 3 ℃/min, and annealing for 2 hours to obtain ZnCo2O4Composite gas-sensitive material with/ZnO heterostructure and prepared ZnCo2O4The mass fraction of ZnO in the/ZnO heterostructure composite gas-sensitive material is 8%. ZnCo produced in this example2O4The XRD spectrum of the/ZnO heterostructure composite gas-sensitive material is shown in figure 1 (c). The transmission of this sample is shown in FIG. 3 (b), in which ZnO and ZnCo are clearly shown2O4The presence of heterostructures at the interface is similar to example 2.
Example 4
Under the condition of electromagnetic stirring, 10 mL of NH with the concentration of 0.38mol/L4HCO3The aqueous solution was slowly dropped to a solution containing 1.7gZn (CH)3COO)2·2H2O and 1.5 gCo (CH)3COO)2·4H2After the dropwise addition of the O into 30 mL of the aqueous solution, continuing to electromagnetically stir for 10 minutes to prepare a precursor solution; transferring the obtained precursor solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, sealing the autoclave, preserving the heat for 24 hours at 180 ℃, naturally cooling to room temperature, collecting a product by centrifugation, washing the product with deionized water and absolute ethyl alcohol for four times respectively, and drying the product for 12 hours at 80 ℃ to obtain a sacrificial template; heating the sacrificial template prepared in the step two to 500 ℃ in the air by using the sacrificial template as a self-sacrificial template, wherein the heating rate is 2 ℃/min, and annealing for 2 hours to obtain ZnCo2O4Composite gas-sensitive material with/ZnO heterostructure and prepared ZnCo2O4The mass fraction of ZnO in the/ZnO heterostructure composite gas-sensitive material is 13.6%. Fig. 2(c) and 2(d) are electron microscope scanning photographs of the sample at different magnifications, respectively, and it can be observed that the nanoflowers are closely contacted with each other as compared to example 1.
In summary, the ZnO/ZnCo prepared by the invention2O4The composite gas-sensitive material has good sensitivity to triethylamine, and has wide application prospect in the aspect of manufacturing novel efficient gas sensors.
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.
Claims (2)
1. ZnCo2O4The preparation method of the/ZnO heterostructure composite gas-sensitive material is characterized in that the ZnCo is prepared by adopting a method of preparing a ZnO heterostructure composite gas-sensitive material2O4the/ZnO heterostructure composite gas-sensitive material is formed by compounding flaky zinc oxide and zinc cobaltate, wherein the zinc oxide accounts for 4-13.6% of the mass percentage; the ZnCo2O4The preparation method of the/ZnO heterostructure composite gas-sensitive material comprises the following steps:
step one, under the condition of electromagnetic stirring, 10 mL of NH with the concentration of 0.38mol/L4HCO3The aqueous solution is slowly dropped with Zn (CH)3COO)2·2H2O and Co (CH)3COO)2·4H2Adding 30 mL of O into the water solution, and continuing to electromagnetically stir for 10-20 minutes after the dropwise adding is finished to prepare a precursor solution, wherein Zn (CH)3COO)2·2H2O content of 0.54-1.7 g, Co (CH)3COO)2·4H2The content of O is 1.5 g;
step two, transferring the obtained precursor solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, sealing the autoclave, preserving the heat for 12-24 hours at the temperature of 180-200 ℃, naturally cooling to room temperature, collecting products through centrifugation, respectively and repeatedly washing the obtained products with deionized water and absolute ethyl alcohol, and drying at the temperature of 60-80 ℃ for 12-24 hours to obtain a sacrificial template;
step three, using the sacrificial template prepared in the step two as a self-sacrificial template, heating the template to 400-600 ℃ in the air at the heating rate of 2-4 ℃/min, and annealing for 2 hours to obtain ZnCo2O4the/ZnO heterostructure composite gas-sensitive material.
2. The ZnCo of claim 12O4The preparation method of the/ZnO heterostructure composite gas-sensitive material is characterized by comprising the following steps: in the second step, the product is washed with deionized water and absolute ethyl alcohol four times respectively.
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| CN110203976A (en) * | 2019-05-16 | 2019-09-06 | 中北大学 | Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material |
| CN110117025B (en) * | 2019-06-05 | 2022-05-27 | 河南理工大学 | ZnO/Zn2SnO4Heterostructure composite gas sensitive material, preparation method and application |
| CN110395761B (en) * | 2019-07-26 | 2020-09-04 | 北京化工大学 | Surface cobalt-doped zinc oxide composite material and preparation method and application thereof |
| CN110988053B (en) * | 2019-12-31 | 2021-03-30 | 吉林大学 | Formaldehyde sensor based on zinc oxide/zinc cobaltate composite material and preparation method thereof |
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