CN114993972A - ZnO nanowire and NO 2 Gas sensor, its preparation and application - Google Patents

ZnO nanowire and NO 2 Gas sensor, its preparation and application Download PDF

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CN114993972A
CN114993972A CN202210590696.2A CN202210590696A CN114993972A CN 114993972 A CN114993972 A CN 114993972A CN 202210590696 A CN202210590696 A CN 202210590696A CN 114993972 A CN114993972 A CN 114993972A
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zno
gas sensor
anionic surfactant
mixed solution
nanowire
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CN114993972B (en
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张博
张帅
倪屹
王靖
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Jiangnan University
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

The invention belongs to the technical field of gas sensors, and particularly relates to a ZnO nanowire and NO 2 Gas sensor and its preparation and application. According to the invention, the ZnO nanowire prepared by a hydrothermal method is used as a sensitive material, and due to the addition of the anionic surfactant, the microstructure and the internal characteristics of ZnO are changed, so that the prepared ZnO nanowire has high length-diameter ratio, oxygen vacancy and adsorbed oxygen ratio; in addition, anionic surfactant molecules are attached to the surface of the ZnO nanowire, which can be used as a photosensitizer for ultraviolet irradiation. NO based on ZnO nanowires 2 The gas sensor has high sensitivity at room temperature and in the dark, shows higher response and faster response/recovery speed under ultraviolet irradiation, and detects NO in the environment 2 Has wide application prospect in the aspect of content.

Description

ZnO nanowire and NO 2 Gas sensor, its preparation and application
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to a ZnO nanowire and NO 2 Gas sensor and its preparation and application.
Background
Nitrogen dioxide (NO) 2 ) Is a typical poisonous and harmful gas, is one of common atmospheric pollutants, and has excessive NO 2 Can directly damage the respiratory system of the human body and seriously harm the health of the human bodyKang (health recovery). In addition, NO 2 But also can be dissolved in water vapor to form acid rain which causes secondary damage to the environment. Therefore, development of timely and accurate detection of NO 2 The sensor is a work with great practical significance.
Metal oxide semiconductor based gas sensors are widely used due to their advantages of excellent performance, simple fabrication, low cost, etc. ZnO is a typical n-type metal oxide semiconductor, has excellent thermal/chemical stability, and is one of the most commonly used gas sensitive materials. However, the existing sensor based on the ZnO nano material generally has the problems of low sensitivity, long response/recovery time, high working temperature and the like, and the practical application range of the ZnO-based gas sensor is greatly limited. Therefore, further improvement of ZnO nanomaterial in terms of material synthesis method, morphology, etc. is needed to improve its sensing performance.
Disclosure of Invention
The invention aims to provide ZnO nanowires and NO 2 The gas sensor and the preparation and the application thereof change the microstructure of ZnO by adding the anionic surfactant, so that the prepared ZnO nanowire has high length-diameter ratio. The change of the shape of the ZnO gas-sensitive material increases the ratio of reactive active sites and oxygen vacancies on the surface of the ZnO gas-sensitive material to adsorbed oxygen, and improves the NO response of the sensor in the dark 2 The sensitivity of (2). Anionic surfactant molecules adsorbed on the surface of ZnO can be used as a photosensitizer, the utilization rate of the material to ultraviolet light is improved, and finally, better room-temperature NO is obtained under the excitation of the ultraviolet light 2 The sensing performance has wide application prospect in practical application.
According to the technical scheme of the invention, the method for synthesizing the ZnO nanowire by the aid of the anionic surfactant comprises the following steps,
a 1: adding alkali into the zinc salt solution, and stirring for reaction to obtain a mixed solution I;
a 2: adding an anionic surfactant into the mixed solution I, stirring and standing to obtain a mixed solution II, wherein the anionic surfactant is sodium alkyl sulfonate;
a 3: and carrying out hydrothermal treatment on the mixed solution II to obtain the ZnO nanowire.
Further, the zinc salt is zinc chloride or zinc acetate and is used for providing a Zn source. The concentration of the zinc salt solution is 0.5-1.0 mol/L; taking zinc acetate as an example, a zinc salt solution is prepared as follows: adding zinc acetate into water (such as deionized water), and stirring in ice bath for 30-40 min.
Further, the alkali is sodium hydroxide or potassium hydroxide, and the alkali can be added in the form of an alkali solution, such as a sodium hydroxide solution with a concentration of 10 mol/L.
Further, the molar ratio of the zinc salt to the base is 1: 20-30.
Further, in the step a1, the stirring reaction (stirring aging) is carried out under ice bath conditions, and the reaction time is 3-4 h.
Further, the molar ratio of the anionic surfactant to the zinc salt is 1-2: 10.
specifically, the molecular formula of the sodium alkylsulfonate is RSO 3 Na, R ═ C10-C22 alkyl, preferably sodium decyl sulfonate (C) 10 H 21 SO 3 Na), sodium dodecyl sulfate (C) 12 H 25 SO 3 Na), sodium tetradecylsulfonate (C) 14 H 29 SO 3 Na) or sodium hexadecylsulfonate (C) 16 H 33 SO 3 Na). The length of the C chain is different, the content of the surfactant adsorbed on the surface of ZnO is different, the length of the C chain is long, the adsorption quantity is large, the space effect is strong, the diameter of the nanowire is small, and the doping is deeper.
The anionic surfactant may be added in the form of a solution, such as a solution of sodium hexadecylsulfonate with a concentration of 0.0375 mol/L.
Further, in the step a2, stirring for 20-30min and standing for 1-2 h.
Furthermore, in the step a3, the heating treatment is performed by adopting a hydrothermal method, the temperature is 140-160 ℃, and the time is 1-1.5 h.
Furthermore, in the step a3, a separation operation is also included after the heating treatment,
specifically, the separation operation is as follows: and cooling the heated mixed solution II to room temperature, transferring the milky white precipitate into a beaker filled with absolute ethyl alcohol, fully stirring for 10-15min, filtering, alternately washing the obtained product with deionized water and absolute ethyl alcohol for 3-5 times, putting the product into a constant-temperature drying oven, continuously drying for 8-12h at 60-80 ℃, and naturally cooling at the temperature to obtain a ZnO powder sample, namely the ZnO nanowire.
The second aspect of the present invention provides the ZnO nanowires prepared by the above method. The length-diameter ratio of the ZnO nanowire is 25-250. Specifically, the method comprises the following steps:
the anionic surfactant is sodium decyl sulfonate, the length-diameter ratio is 25-35, and the diameter is 800-1600 nm;
the anion surfactant is sodium dodecyl sulfate, the length-diameter ratio is 60-70, and the diameter is 400-600 nm;
the anion surfactant is sodium tetradecyl sulfonate, the length-diameter ratio is 130-145, and the diameter is 150-250 nm;
the anionic surfactant is sodium hexadecyl sulfonate with the length-diameter ratio of 235-250 and the diameter of 70-90 nm. In a third aspect of the invention there is provided a NO 2 A method of making a gas sensor comprising the steps of, b 1: dispersing the ZnO nanowire in absolute ethyl alcohol or water to obtain pasty mixed solution;
b 2: coating the pasty mixed solution on the surface of an electrode of a gas sensor carrier to form a sensitive material film, and drying to obtain the NO 2 A gas sensor.
Further, the volume ratio of the ZnO nanowire to the absolute ethyl alcohol is 2-5: 1.
further, the thickness of the sensitive material film is 10-30 μm.
Furthermore, the gas sensor carrier comprises a monocrystalline silicon piece substrate, a silicon dioxide insulating layer covering the surface of the monocrystalline silicon piece substrate, and interdigital electrodes integrated on the surface of the silicon dioxide insulating layer.
Specifically, the preparation method of the gas sensor carrier comprises the following steps: growing a silicon dioxide insulating layer on a monocrystalline silicon substrate, and integrating Cr/Au interdigital electrodes on the monocrystalline silicon substrate covered with the silicon dioxide insulating layer through a photoetching process, a radio frequency sputtering process and a stripping process.
The size of the single crystal silicon wafer substrate is 6 x 4 x 0.5mm, the thickness of a silicon dioxide insulating layer is 300nm, the interdigital electrodes are provided with 25 pairs of interdigital fingers, the width of each interdigital finger is 20 mu m, the length of each interdigital finger is 1.5mm, the gap between every two adjacent interdigital fingers is 20 mu m, each electrode is composed of Cr/Au, and the thickness of each electrode is 10nm/100 nm.
Furthermore, the surface of the carrier of the gas sensor is uniformly covered with a sensitive material film formed by the ZnO nanowires except the interdigital electrodes.
Furthermore, in the step b2, the drying temperature is 80-100 ℃ and the drying time is 8-12 h.
In a fourth aspect of the present invention, there is provided NO obtained by the above-mentioned production method 2 A gas sensor.
Further, the device also comprises an illumination module, wherein the illumination module is used for carrying out UV (ultraviolet) light irradiation on the sensitive material film.
The fifth aspect of the present invention provides the above ZnO nanowire, or NO 2 Gas sensor for detecting NO at room temperature (25 +/-5℃) 2 The use of (1).
Compared with the prior art, the technical scheme of the invention has the following advantages:
the preparation method of the ZnO nanowire based on the anionic surfactant assisted synthesis can prepare the ZnO nanowire with the high length-diameter ratio of 50-120nm in diameter, and the ZnO nanowire is covered on the outer surface of a sensor carrier to prepare NO 2 The prepared ZnO nanowire has high length-diameter ratio, and the ZnO nanowire is doped by surfactant ions, so that the proportion of reactive active sites and oxygen vacancies on the surface of the gas-sensitive material to adsorbed oxygen is increased, and more NO is favorably generated 2 The gas-sensitive material is adsorbed on the surface to participate in the reaction, so that the sensing performance of the sensor is further improved;
NO of the invention 2 The gas sensor also comprises an illumination module, and as the anionic surfactant serving as a soft template can form bonding with the precursor in the hydrothermal solution, the prepared ZnO nanowire is subjected to in-situ functionalization, so that the prepared ZnO nanowire-based NO is 2 The performance of the gas sensor can be further obtained under the UV irradiation at room temperatureTo realize high sensitivity and fast response/recovery speed of NO at room temperature 2 A gas sensor;
the sensor in the technical scheme of the invention can be manufactured by taking the planar gas sensor as a carrier, and the device has simple process and small volume, is suitable for mass production and is applied to practical application.
Drawings
Fig. 1 is an SEM topography based on ZnO nanowires prepared in the present invention, wherein (a) is an SEM topography of pure ZnO nanorods, and (b) - (e) are SEM topography of ZnO nanowires prepared based on examples 1-4.
Fig. 2 is an XRD pattern based on ZnO nanowires prepared in the present invention, wherein (a) the pattern is a full-angle diffraction pattern of a prepared sample, and (b) the pattern is an enlarged view of an XRD pattern of the prepared sample at 30 ° -39 °.
Fig. 3 is an FT-IR diagram based on ZnO nanowires prepared in the present invention.
FIG. 4 is an XPS graph based on ZnO nanowires prepared in the present invention, wherein (a) the graph is a comparison of S2 p nuclear-scale spectra of ZnO nanowires prepared based on examples 1-4, (b) the XPS peak area ratio of Zn2p to S2 p prepared based on examples 1-4, and (c) the graph is an oxygen vacancy (O) in pure ZnO nanorods prepared and ZnO nanowires prepared based on examples 1-4 V ) Adsorption of oxygen (O) C ) And the total content (O) V +O C ) The trend of change of (c).
FIG. 5 shows NO prepared according to examples 1-4 of the present invention 2 Sensor for NO under dark conditions at room temperature 2 Wherein (a) is a dynamic response-recovery curve and (b) is a response-concentration fitted curve.
FIG. 6 shows NO prepared in the present invention based on examples 1 to 4 2 The sensor can measure 10ppmNO under the irradiation of UV light with different light intensities at room temperature 2 The response curve of (c).
FIG. 7 shows NO prepared according to example 4 in the present invention 2 The sensor is used for detecting 10ppmNO under the conditions of room-temperature UV illumination and room-temperature darkness 2 Response-recovery curve of (a).
FIG. 8 shows NO prepared according to example 4 of the present invention 2 Sensor for measuring 10ppmNO under room temperature UV illumination condition 2 Continuous cyclic response-recovery curve.
Detailed Description
The present invention is further described below in conjunction with the drawings and the embodiments so that those skilled in the art can better understand the present invention and can carry out the present invention, but the embodiments are not to be construed as limiting the present invention.
Example 1
1. Anionic surfactant assisted synthesis of ZnO nanowire
a 1: weighing zinc acetate, adding the zinc acetate into deionized water to prepare a mixed solution with the concentration of 0.5mol/L, and stirring for 30min in an ice bath;
a 2: weighing sodium hydroxide solution (10mol/L) according to the molar ratio of 20/1 and taking the zinc acetate in the step a1 as a reference, adding the sodium hydroxide solution into the uniformly stirred mixed solution in the step a1, and stirring and aging the obtained mixed solution in ice bath for 3 hours;
a 3: weighing a surfactant solution (0.0375mol/L) containing sodium decyl sulfonate into the mixed solution obtained in the step a2 according to a molar ratio of 1/10 by taking the zinc acetate in the step a1 as a reference at room temperature, slightly stirring for 20min, and then standing for 2 h;
a 4: transferring the solution obtained in the step a3 into a polytetrafluoroethylene-lined high-pressure reaction kettle, and heating to 140 ℃ under a hydrothermal condition to react for 1 h;
a 5: and c, after the reaction kettle in the step a4 is cooled to room temperature, transferring the milky white precipitate into a beaker filled with absolute ethyl alcohol, fully stirring for 10min, filtering, alternately washing the obtained product with deionized water and absolute ethyl alcohol for 3 times, putting the product into a constant-temperature drying oven, continuously drying the product at 60 ℃ for 12h, and naturally cooling the product at the temperature to obtain a ZnO powdery sample.
2. NO based on ZnO nanowires 2 Preparation of the sensor
b 1: growing a silicon dioxide insulating layer on a monocrystalline silicon substrate, and integrating Cr/Au interdigital electrodes on the monocrystalline silicon substrate covered with the silicon dioxide insulating layer through a photoetching technology, a radio frequency sputtering technology and a stripping process to obtain a sensor carrier with a gas sensor function; wherein, the size of the single crystal silicon wafer substrate is 6 x 4 x 0.5mm, the thickness of the silicon dioxide insulating layer is 300nm, the interdigital electrode has 25 pairs of interdigital, the width of a single interdigital is 20 μm, the length is 1.5mm, the gap between adjacent interdigital is 20 μm, the electrode is composed of Cr/Au, and the thickness is 10nm/100 nm;
b 2: mixing the ZnO powder sample obtained in the step a5 and absolute ethyl alcohol according to the weight ratio of 3: 1, and performing ultrasonic treatment for 5min to uniformly disperse the mixture to prepare paste mixed solution containing the ZnO nanowires;
b 3: uniformly and completely covering the mixed solution obtained in the step b2 on the outer surface of the sensor carrier by spin coating, ensuring that the mixed solution completely covers the electrode, and forming a sensitive material film with the thickness of about 20 microns;
b 4: drying the sensor carrier coated with the sensitive material film for 12 hours in a drying oven at 80 ℃ to obtain NO based on the ZnO nanowire 2 A sensor.
Examples 2 to 4
Sodium decyl sulfonate was replaced with sodium dodecyl sulfonate, sodium tetradecyl sulfonate, and sodium hexadecyl sulfonate, respectively, on the basis of example 1.
Comparative example NO based on pure ZnO nanorods 2 Sensor and its preparation
1. The preparation method of the pure ZnO nano-rod comprises the following steps:
a 1: weighing zinc acetate, adding the zinc acetate into deionized water to prepare a mixed solution with the concentration of 0.5mol/L, and stirring for 30min in an ice bath;
a 2: weighing sodium hydroxide solution (10mol/L) according to the molar ratio of 20/1 and taking the zinc acetate in the step a1 as a reference, adding the sodium hydroxide solution into the uniformly stirred mixed solution in the step a1, and stirring and aging the obtained mixed solution in ice bath for 3 hours;
a 3: transferring the solution obtained in the step a2 into a polytetrafluoroethylene-lined high-pressure reaction kettle, and heating to 140 ℃ under a hydrothermal condition to react for 1 h;
a 4: and c, after the reaction kettle in the step a3 is cooled to room temperature, transferring the precipitate into a beaker filled with absolute ethyl alcohol, fully stirring for 10min, filtering, alternately washing the obtained product with deionized water and absolute ethyl alcohol for 3 times, putting the product into a constant-temperature drying oven, continuously drying the product at 60 ℃ for 12h, and naturally cooling the reaction kettle to obtain a pure ZnO powder sample.
2. Based on pure ZnO nano-rod NO 2 The preparation method of the sensor comprises the following steps:
b 1: preparing a sensor carrier having a gas sensor function;
b 2: the ZnO powder sample obtained in comparative example a4 and absolute ethanol were mixed according to a ratio of 3: 1, and carrying out ultrasonic treatment for 5min to uniformly disperse the mixture to prepare a paste mixed solution containing pure ZnO nanorods;
b 3: uniformly and completely covering the mixed solution obtained in the step b2 on the outer surface of the sensor carrier through spin coating, ensuring that the mixed solution completely covers the electrode, and forming a sensitive material film with the thickness of about 20 mu m;
b 4: drying the sensor carrier coated with the sensitive material film for 12 hours in a drying oven at the temperature of 80 ℃ to obtain the NO based on the pure ZnO nano-rod 2 A sensor.
Analysis of results
Pure ZnO is a nanorod structure with a larger diameter as shown in FIG. 1(a), while ZnO prepared based on examples 1-4 is a nanowire structure with a smaller diameter as shown in FIGS. 1(b) - (e), and as the C chain length of the added surfactant increases, the ZnO nanowires shown in FIGS. b) - (e) have a decreasing diameter and an increasing aspect ratio;
as shown in fig. 2(a), all peak positions of the pure ZnO nanorods (comparative example) and the ZnO nanowires prepared in examples 1 to 4 were consistent with the standard peak, indicating successful preparation of the pure ZnO nanorods and the ZnO nanowires of examples 1 to 4, but the peak positions of the ZnO nanowires prepared in examples 1 to 4 were shifted to a small angle and the shift angles of examples 1 to 4 were gradually increased as compared with the pure ZnO, as shown in fig. 2(b), indicating that the adsorption amount of the surfactant adsorbed on the ZnO is increased, resulting in an increase in lattice constant and deeper doping of the prepared ZnO nanowires, as shown in fig. 2 (a).
As shown in FIG. 3, pure ZnO does not have any characteristic peak due to no addition of surfactant, and ZnO nanowire synthesized with the aid of anionic surfactant has characteristic peaks due to-CH respectively 2 Asymmetric stretching vibration of radicals(2906cm -1 ) And symmetric telescopic vibration (2838 cm) -1 ),-SO 3 Asymmetric stretching vibration of S ═ O bond in group (1170 cm) -1 ) And symmetric telescopic vibration (1056 cm) -1 ) and-CH 2 Asymmetric in-plane bending vibration (1421 cm) of the radical -1 ) The resulting characteristic peaks, the ZnO peaks prepared in examples 1 to 4, increased in intensity gradually, indicating that anionic surfactant molecules interacted with and finally adsorbed on the ZnO crystal surface, and the adsorption amount of the surfactant increased gradually with the increase in the C chain length. In addition, during the growth of ZnO crystals, the anionic surfactant forms micelles and is gathered on the surfaces of ZnO crystal grains, and the inhibition of the radial growth of the ZnO crystals by the steric effect is considered as a potential cause for the formation of high aspect ratio of the ZnO crystals;
as shown in FIG. 4(a), the peak area of S2 p gradually increased, and the sharp decrease in the peak area ratio of Z2 p to S2 p shown in FIG. 4(b) all indicated that the content of the anionic surfactant adsorbed on the surface of ZnO sharply increased, and as shown in FIG. 4(c), the oxygen vacancies (O) of the ZnO nanowires prepared in examples 1 to 4 V ) And adsorbing oxygen (O) C ) The total content is gradually increased, which proves that ZnO synthesized by the aid of the anionic surfactant has rich defects and is beneficial to enhancing gas sensing response;
as shown in FIG. 5(a), the sensors prepared according to examples 1-4 respond with NO in dark ambient at room temperature 2 The response values of the sensors prepared in examples 1 to 4 increased gradually with increasing concentration, and in fig. 5(b), the response of the sensors prepared in examples 1 to 4 was linear with concentration and the slope of the fitted curve increased gradually with increasing concentration, indicating that the prepared sensors had NO 2 The discrimination ability of the gas concentration gradually increases.
As shown in FIG. 6, the sensors prepared based on the comparative example and examples 1 to 4 were sensitive to 10ppmNO at different light intensities when the sensors were exposed to UV light at room temperature 2 Increased and then decreased in response, the sensors prepared in comparative example and example 1 were at 0.42mW/cm 2 The maximum response was obtained at 0.68mW/cm for the sensors prepared in examples 2-4 2 Maximum response was obtained, and whether in the dark or under UV light, prepared in examples 1-4The response of the sensor is far higher than that of a comparative example sensor, and the ZnO nanowire synthesized by the aid of the anionic surfactant is proved to have excellent NO 2 Sensing performance.
As shown in FIG. 7, the sensor prepared based on example 4 was exposed to UV light (0.68 mW/cm) at room temperature 2 ) For 10ppmNO in an irradiation environment 2 The response time of (2) is 602%, the response time is 58s, the recovery time is 91s, and the response time is 10ppmNO under the dark environment at room temperature 2 The response of the ZnO nanowire is 271%, the response time is 393s, and the recovery time is 953s, which proves that the response and the response/recovery time of the ZnO nanowire synthesized by the aid of the anionic surfactant under the UV illumination are further enhanced, and the ZnO nanowire has better NO under the UV illumination 2 Sensing performance. Besides the activation effect of ultraviolet light on ZnO semiconductors, surfactant molecules adsorbed on the surface of ZnO with high length-diameter ratio can be used as photosensitizers to promote the absorption efficiency of ultraviolet light, and finally better photoexcited NO is caused 2 Gas-sensitive performance.
As shown in FIG. 8, the sensor prepared in example 4 can measure 10ppm NO in the environment of UV light irradiation at room temperature 2 The characteristic curve of the sensor is almost unchanged under the continuous cycle test, which shows the good stability of the sensor of the embodiment.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.

Claims (10)

1. A method for synthesizing ZnO nano-wire with the assistance of anionic surfactant is characterized by comprising the following steps,
a 1: adding alkali into the zinc salt solution, and stirring for reaction to obtain a mixed solution I;
a 2: adding an anionic surfactant into the mixed solution I, stirring and standing to obtain a mixed solution II, wherein the anionic surfactant is sodium alkyl sulfonate;
a 3: and carrying out hydrothermal treatment on the mixed solution II to obtain the ZnO nanowire.
2. The method for synthesizing the ZnO nanowires with the assistance of the anionic surfactant according to claim 1, wherein the molar ratio of the zinc salt to the alkali is 1: 20-30.
3. The method for synthesizing the ZnO nanowire with the assistance of the anionic surfactant as claimed in claim 1, wherein the molar ratio of the anionic surfactant to the zinc salt is 1-2: 10.
4. the method for synthesizing ZnO nanowires with the assistance of anionic surfactant as claimed in claim 1, wherein the temperature of the heat treatment in step a3 is 140-160 ℃ and the time is 1-1.5 h.
5. ZnO nanowires produced by the method of any one of claims 1 to 4.
6. NO (nitric oxide) 2 The preparation method of the gas sensor is characterized by comprising the following steps,
b 1: dispersing the ZnO nanowire of claim 5 in absolute ethyl alcohol or water to obtain a paste-like mixed solution;
b 2: coating the pasty mixed solution on the surface of an electrode of a gas sensor carrier to form a sensitive material film, and drying to obtain the NO 2 A gas sensor.
7. The NO of claim 6 2 The preparation method of the gas sensor is characterized in that the thickness of the sensitive material film is 10-30 μm.
8. NO produced by the production method according to claim 6 or 7 2 A gas sensor.
9. Such as rightNO according to claim 8 2 Gas sensor, characterized in that said NO 2 The gas sensor also comprises an illumination module, and the illumination module is used for carrying out UV light irradiation on the sensitive material film.
10. ZnO nanowires as defined in claim 4, or NO as defined in claim 8 or 9 2 Gas sensor for detecting NO at room temperature 2 The use of (1).
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Citations (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004091300A (en) * 2002-09-04 2004-03-25 National Institute Of Advanced Industrial & Technology Zinc oxide polycrystalline tube
US20070261959A1 (en) * 2005-12-23 2007-11-15 Korea Institute Of Science And Technology Ultra-sensitive metal oxide gas sensor and fabrication method thereof
KR20090093096A (en) * 2008-02-28 2009-09-02 재단법인서울대학교산학협력재단 ZnO Quantum Dots with Monodisperse and High Quality Photoluminescence and Process for Preparing Same
US20120091451A1 (en) * 2009-04-14 2012-04-19 John Vedamuthu Kennedy Zinc Oxide Nanostructures and Sensors Using Zinc Oxide Nanostructures
CN102795658A (en) * 2012-07-30 2012-11-28 西安理工大学 Method for regulating zinc oxide crystal microstructure by using hydrogen peroxide
KR20130104173A (en) * 2012-03-13 2013-09-25 인하대학교 산학협력단 Znsno3 nanorods coated with palladium particles, a preparation method thereof, and gas sensor using the same
US20150279669A1 (en) * 2014-03-28 2015-10-01 Samsung Electronics Co., Ltd. METHOD OF PREPARING ZnO NANOWIRE AND ZnO NANOWIRE PREPARED THEREBY
CN106290482A (en) * 2016-07-15 2017-01-04 西安工业大学 A kind of NO2the preparation method of Photo-electric gas-sensitivity sensor
RU2613488C1 (en) * 2015-10-06 2017-03-16 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Пензенский государственный университет" (ФГБОУ ВПО "Пензенский государственный университет") Method of producing gas sensor based on thermovoltaic effect in zinc oxide
CN106970117A (en) * 2017-03-27 2017-07-21 东北大学 A kind of NO based on electrode surface growth in situ nano-ZnO2Sensor
CN107727700A (en) * 2017-10-10 2018-02-23 重庆大学 NO2Gas sensor and preparation method thereof, application method and desorption method
CN108128798A (en) * 2017-12-22 2018-06-08 江南大学 A kind of simple method for preparing of flaky nanometer zinc oxide sun-screening agent
CN108318544A (en) * 2018-03-22 2018-07-24 吉林大学 Based on In2O3The NO of-ZnO compound nano sensitive materials2Gas sensor and preparation method thereof
CN109725039A (en) * 2019-01-10 2019-05-07 沈阳化工大学 A kind of preparation and its application of Pd modification ZnO nano-rod array
CN110879245A (en) * 2019-12-12 2020-03-13 淮北师范大学 Preparation method of heavy metal ion nano sensitive material
CN111289580A (en) * 2018-06-27 2020-06-16 成都新柯力化工科技有限公司 Film sensing material for detecting atmosphere hydrogen sulfide gas and preparation method thereof
CN112557458A (en) * 2020-12-04 2021-03-26 江南大学 Preparation method of indium oxide nanowire and NO containing indium oxide nanowire2Method for manufacturing sensor and sensor
CN113125519A (en) * 2021-04-19 2021-07-16 江南大学 In2O3/α-Fe2O3Nanowire, triethylamine sensor and preparation method thereof
CN113308680A (en) * 2021-04-16 2021-08-27 沈阳化工大学 Preparation method and application of ZnO nanowire sensitive material
CN113670989A (en) * 2021-08-27 2021-11-19 河南理工大学 Pd/In2O3Gas sensitive material, preparation method thereof and gas sensor
CN114199951A (en) * 2021-12-10 2022-03-18 吉林大学 NO based on ZnO/ZnS heterostructure nanowire sensitive material2Sensor and preparation method thereof

Patent Citations (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004091300A (en) * 2002-09-04 2004-03-25 National Institute Of Advanced Industrial & Technology Zinc oxide polycrystalline tube
US20070261959A1 (en) * 2005-12-23 2007-11-15 Korea Institute Of Science And Technology Ultra-sensitive metal oxide gas sensor and fabrication method thereof
KR20090093096A (en) * 2008-02-28 2009-09-02 재단법인서울대학교산학협력재단 ZnO Quantum Dots with Monodisperse and High Quality Photoluminescence and Process for Preparing Same
US20120091451A1 (en) * 2009-04-14 2012-04-19 John Vedamuthu Kennedy Zinc Oxide Nanostructures and Sensors Using Zinc Oxide Nanostructures
KR20130104173A (en) * 2012-03-13 2013-09-25 인하대학교 산학협력단 Znsno3 nanorods coated with palladium particles, a preparation method thereof, and gas sensor using the same
CN102795658A (en) * 2012-07-30 2012-11-28 西安理工大学 Method for regulating zinc oxide crystal microstructure by using hydrogen peroxide
US20150279669A1 (en) * 2014-03-28 2015-10-01 Samsung Electronics Co., Ltd. METHOD OF PREPARING ZnO NANOWIRE AND ZnO NANOWIRE PREPARED THEREBY
RU2613488C1 (en) * 2015-10-06 2017-03-16 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Пензенский государственный университет" (ФГБОУ ВПО "Пензенский государственный университет") Method of producing gas sensor based on thermovoltaic effect in zinc oxide
CN106290482A (en) * 2016-07-15 2017-01-04 西安工业大学 A kind of NO2the preparation method of Photo-electric gas-sensitivity sensor
CN106970117A (en) * 2017-03-27 2017-07-21 东北大学 A kind of NO based on electrode surface growth in situ nano-ZnO2Sensor
CN107727700A (en) * 2017-10-10 2018-02-23 重庆大学 NO2Gas sensor and preparation method thereof, application method and desorption method
CN108128798A (en) * 2017-12-22 2018-06-08 江南大学 A kind of simple method for preparing of flaky nanometer zinc oxide sun-screening agent
CN108318544A (en) * 2018-03-22 2018-07-24 吉林大学 Based on In2O3The NO of-ZnO compound nano sensitive materials2Gas sensor and preparation method thereof
CN111289580A (en) * 2018-06-27 2020-06-16 成都新柯力化工科技有限公司 Film sensing material for detecting atmosphere hydrogen sulfide gas and preparation method thereof
CN109725039A (en) * 2019-01-10 2019-05-07 沈阳化工大学 A kind of preparation and its application of Pd modification ZnO nano-rod array
CN110879245A (en) * 2019-12-12 2020-03-13 淮北师范大学 Preparation method of heavy metal ion nano sensitive material
CN112557458A (en) * 2020-12-04 2021-03-26 江南大学 Preparation method of indium oxide nanowire and NO containing indium oxide nanowire2Method for manufacturing sensor and sensor
CN113308680A (en) * 2021-04-16 2021-08-27 沈阳化工大学 Preparation method and application of ZnO nanowire sensitive material
CN113125519A (en) * 2021-04-19 2021-07-16 江南大学 In2O3/α-Fe2O3Nanowire, triethylamine sensor and preparation method thereof
CN113670989A (en) * 2021-08-27 2021-11-19 河南理工大学 Pd/In2O3Gas sensitive material, preparation method thereof and gas sensor
CN114199951A (en) * 2021-12-10 2022-03-18 吉林大学 NO based on ZnO/ZnS heterostructure nanowire sensitive material2Sensor and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
BO ZHANG ETAL.: "ZnO Nanowires with Increasing Aspect Ratios for Room-Temperature NO2 Gas Sensing", 《APPLIED NANO MATERIALS》, pages 10603 - 10616 *
SOU-HUI HSIAO ETAL.: "High-selectivity NOx sensors based on an Au/InGaP Schottky diode functionalized with self-assembled monolayer of alkanedithiols", 《SENSORS AND ACTUATORS B: CHEMICAL》, pages 1 - 10 *

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