CN113740389B - Zinc oxide nanorod-based field emission hydrogen sensor and preparation method and application thereof - Google Patents
Zinc oxide nanorod-based field emission hydrogen sensor and preparation method and application thereof Download PDFInfo
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Abstract
The application discloses a field emission hydrogen sensor based on zinc oxide nano rod, a preparation method and application thereof, the technical proposal is that the field emission hydrogen sensor comprises a field emission cathode and a field emission anode, wherein the field emission cathode comprises a substrate, a ZnO seed crystal layer arranged on the substrate in a spin coating way, and a ZnO nano rod array growing on the ZnO seed crystal layer on the substrate, and the field emission cathode is arranged at a position of 10 ‑7 ‑10 ‑3 Under Pa hydrogen partial pressure, the absorption of hydrogen on the surface of the field emission cathode can enhance the emission current under the same field intensity, so that the hydrogen sensor has hydrogen sensing characteristics. The application has the advantages that: the method has the advantages of stability, microminiature, simple structure, quick recovery and the like, and in addition, compared with the traditional carbon nano tube preparation technology (chemical vapor deposition method), the zinc oxide nano rod is prepared by adopting a hydrothermal method, a transition metal catalyst is not required to be used, the temperature is low (70-95 ℃), the cost is low, and the large-area growth can be realized.
Description
Technical Field
The application relates to a hydrogen sensor, in particular to a field emission hydrogen sensor based on zinc oxide nanorods, and a preparation method and application thereof.
Background
Zinc oxide is a semiconductor material with a wide forbidden band (-3.37 eV), and the zinc oxide nano material can be widely applied to the fields of gas sensing, energy sources, piezoelectricity, field emission and the like. The zinc oxide nano material has obvious sensing performance on various gases, and in addition, the zinc oxide has simple growth condition, easy preparation, no toxicity and no harm, and is an environment-friendly material. By detecting the change in resistance, the zinc oxide sensor can be used to detect various gases such as methane, acetylene, ammonia, nitrogen dioxide, and the like.
Hydrogen sensing plays an important role in many scientific and industrial fields, and at present, research and development based on hydrogen sensing technology is mainly focused on the atmospheric pressure environment, however, low-pressure hydrogen detection also plays an important role in many fields including oil gas transmission, space mission, low-emission fuel cell, high-vacuum processing equipment, vacuum electronic devices and the like. The hydrogen sensor based on the nano mechanical resonance technology and the technology of directly growing the carbon nano tube on the metal substrate can be applied to 10 -5 In a gas environment of Torr or more, low-pressure hydrogen sensor technology is not very diverse. However, the low-pressure hydrogen detection sensing technology related to zinc oxide nano rods has not been reported yet.
Disclosure of Invention
The application aims to overcome the defects and the shortcomings of the prior art and provides a field emission hydrogen sensor based on zinc oxide nanorods, and a preparation method and application thereof. According to the field emission hydrogen sensor based on the zinc oxide nanorods, the hydrogen partial pressure in a low-pressure environment is detected by detecting the change of field emission current of the ZnO nanorod array.
To achieve the above object, a first aspect of the present application provides a field emission hydrogen sensor based on zinc oxide nanorods, comprising a field emission cathode and a field emission anode, wherein the field emission cathode comprises a substrate, a ZnO seed layer spin-coated on the substrate, and a ZnO nanorod array grown on the ZnO seed layer on the substrate by a hydrothermal method, and the field emission cathode has a hydrogen partial pressure of 10 -7 -10 -3 Under Pa, the absorption of hydrogen on the surface of the field emission cathode can enhance the emission current under the same field intensity, so that the hydrogen-emitting cathode has hydrogen sensing characteristics.
Further provided is that the field emission anode is planar or pointed in shape.
The substrate is a silicon wafer substrate or a metal substrate or conductive glass, the metal substrate is made of stainless steel, alloy, nickel sheet and the like, and the conductive glass is made of ITO, FTO and the like.
In addition, the application also provides a field emission cathode of the field emission hydrogen sensor based on the zinc oxide nano rod, which comprises a substrate, a ZnO seed crystal layer which is arranged on the substrate in a spin coating way, and a ZnO nano rod array which grows on the ZnO seed crystal layer on the substrate through a hydrothermal method.
The application provides a method for detecting hydrogen in a low-pressure hydrogen environment by using a field emission hydrogen sensor, which comprises the following steps:
(1) Determining hydrogen sensing current and pressure curves:
10 under partial pressure of hydrogen -7 -10 -3 The specific steps are as follows:
i) At each measuring point, the field emission cathode is subjected to Joule heating degassing by using an increased emission current, and the intrinsic emission I is measured 0 ;
ii) applying a field emission voltage V and obtaining an initial emission current I 0 And detecting a change in current during a time t;
iii) Dividing t time into N equal intervals according to the requirement, and recording the current I at the end of each interval i I=0, …, N); vi) passing the current I at the end of each interval i Accumulating, and taking an average value to obtain a current I, wherein the current I is used as a gas-sensitive sensing current of the measuring point;
v) after the measurement is finished, the sensor is enabled to emit pulses for one to several times under a higher current, and the purposes of cleaning the surface and recovering the detection function of the sensor are achieved;
drawing a hydrogen sensing current and pressure curve after multi-point testing according to the gas sensing current of the measuring point and the hydrogen partial pressure of the corresponding test;
(2) And detecting the gas-sensitive sensing current in the hydrogen partial pressure environment to be detected, and determining the hydrogen partial pressure value according to the hydrogen sensing current and the pressure curve.
The application has the advantages that: the method has the advantages of stability, microminiature, simple structure, quick recovery and the like, and in addition, compared with the traditional carbon nano tube preparation technology (chemical vapor deposition method), the zinc oxide nano rod is prepared by adopting a hydrothermal method, a transition metal catalyst is not required to be used, the temperature is low (70-95 ℃), the cost is low, and the large-area growth can be realized.
Drawings
In order to more clearly illustrate the embodiments of the application or the technical solutions of the prior art, the drawings which are required in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the application, and that it is within the scope of the application to one skilled in the art to obtain other drawings from these drawings without inventive faculty.
FIG. 1 is a photograph of a zinc oxide nanorod cathode material, (a) SEM and (b) TEM;
FIG. 2 is a graph of field emission of zinc oxide nanorods, (a) J-E, (b) F-N;
FIG. 3 is a graph showing that zinc oxide (400 ℃ annealing) has a small current emission which increases gradually with time, and the effect is stronger with the increase of pressure under different hydrogen pressure environments;
FIG. 4 shows a novel low-pressure hydrogen sensing characteristic curve based on the zinc oxide nanorod (400 ℃ annealing) field emission principle.
Detailed Description
The present application will be described in further detail with reference to the accompanying drawings, for the purpose of making the objects, technical solutions and advantages of the present application more apparent.
As shown in fig. 1 to fig. 4, in the embodiment of the present application, the ZnO nanorod array is prepared by a two-step method, first, a ZnO seed layer is spin-coated on a substrate, and then, the ZnO nanorod array is obtained on the substrate by a hydrothermal method. The ZnO nano rod array can also grow through a chemical vapor deposition method, and the sensor adopts a diode structure and adopts the working principle of field electron emission. The cathode A is a ZnO nano rod array, and the anode B can be a plane, a tip or other shapes. At low air pressure (pressure less than or equal to 10 -2 Pa) applying a specific cathode voltage V to the anode 1 High voltage V 2 When the electric field intensity E of the cathode surface 1 After reaching a certain value, the ZnO surface emits electrons and the current I generated by the ZnO surface is measured 1 A field emission current-voltage curve is obtained. For a field emission cathode of a ZnO nano rod with hydrogen sensing characteristics, the adsorption of hydrogen on the surface of the nano cathode can influence the field emission performance, wherein one influence is the enhancement of emission current under the same field intensity; also, different hydrogen partial pressures have different effects on field emission performance, e.g., the higher the hydrogen partial pressure, the more pronounced the effect of field emission enhancement. When hydrogen sensing measurement is carried out, the change of field electron emission current is measured under certain fixed electric field intensity, the measurement time can be different according to different sensors and measurement environments, and before the field emission current measurement, the surface of the zinc oxide nanorod can be cleaned and degassed by using Joule heat generated by large-current field emission. In order to enhance the sensing effect, improve the sensing performance such as measurement stability and reliability, and the like, the testing method can be properly adjusted and improved on the premise of ensuring the time required by the sensing test: 1) In the measurement of the current change along with time, parameters such as sensitivity, response time and the like can be synthesized, and the measurement time can be properly adjusted; 2) Repeated and multi-point measurements may be used. Repeated measurement is carried out for a plurality of times under the same field emission voltage; the multipoint measurement is to select different voltages and measure the field emission current. The repeated and multi-point measurements may be used alone or in combination, with the data weighted averaged using appropriate mathematical methods.
In the embodiment, a zinc oxide nano rod (shown in figure 1) is grown on a silicon wafer substrate by adopting a two-step method, and is subjected to field emission test, and the field emission current enhancement effect is obvious under the conditions of low-pressure hydrogen and low current; at the same time at 10 -7 -10 -3 Under Pa, the higher the hydrogen partial pressure, the more obvious the field emission enhancement effect. Based on this, the inventors developed a hydrogen sensor based on ZnO nanorod field emission as a mechanism. In the field emission test, the current-voltage curve and the corresponding F-N curve of the field emission of fig. 2 show that the electron emission deviates from the intrinsic emission characteristic of Fowler-Nordheim theory in the small current emission state. Further experiments confirm that: the emission effect of the field emission assistance with the hydrogen molecules acting in a determining way causes the deviation, and lays the technical foundation of hydrogen-sensitive field emission sensing. Compared with the carbon nano tube preparation technology (chemical vapor deposition method), the zinc oxide nano rod adopts a hydrothermal methodThe preparation method does not need to use a transition metal catalyst, has lower temperature (70-95 ℃), lower cost and can grow in a large area. Compared with the carbon nano Guan Qingmin field emission sensing technology, the hydrogen-sensitive field emission current of the zinc oxide nano rod is related to the concentration of oxygen defects in the zinc oxide nano rod, and the higher the concentration of oxygen defects is, the higher the field emission current is. The mechanism is mainly that after hydrogen molecules or hydrogen atoms are adsorbed on the surface of the zinc oxide nano rod, the hydrogen molecules or the hydrogen atoms interact with oxygen defects in zinc oxide to cause the change of zinc oxide work function, so that the change of field emission current is initiated. In addition, compared with the carbon nano tube, the zinc oxide has better emission stability under the condition of small current emission. FIG. 3 shows the gradual increase of emission current at different partial pressures of hydrogen in a hydrogen atmosphere at a field emission initiation current of about 1. Mu.A. Based on this, the inventors tested that at different hydrogen partial pressures (10 -7 -10 -3 Pa). And the data acquisition is carried out by adopting an accumulation method, and the specific steps are as follows: i) At each measurement point, the zinc oxide cathode is subjected to Joule heating degassing by using an increased emission current, and the intrinsic emission (or near-intrinsic emission) I is measured 0 The method comprises the steps of carrying out a first treatment on the surface of the ii) applying a field emission voltage V and obtaining an initial emission current I 0 And detecting a change in current during a time t; iii) Dividing t time into N equal intervals according to the requirement, and recording the current I at the end of each interval i . (i=0, …, N); vi) passing the current I at the end of each interval i Accumulating, and taking an average value to obtain a current I, wherein the current I is used as a gas-sensitive sensing current of the measuring point; v) after the measurement is finished, the sensor can pulse and emit one to several times under a higher current, so as to achieve the purposes of cleaning the surface and recovering the detection function of the sensor.
The method has the advantages of stability, miniature size, simple structure, quick recovery and the like.
The foregoing disclosure is illustrative of the present application and is not to be construed as limiting the scope of the application, which is defined by the appended claims.
Claims (3)
1. Field emission hydrogen based on zinc oxide nano rodA sensor is characterized by comprising a field emission cathode and a field emission anode, wherein the field emission cathode comprises a substrate, a ZnO seed layer which is arranged on the substrate in a spin coating way, and a ZnO nano-rod array which is grown on the ZnO seed layer on the substrate, and the field emission cathode is under the pressure of 10 parts of hydrogen -7 -10 -3 Under Pa, the absorption of hydrogen on the surface of the field emission cathode can enhance the emission current under the same field intensity, so that the hydrogen sensor has hydrogen sensing characteristics;
the field emission anode is in a plane or tip shape;
the substrate is a silicon wafer substrate or a metal substrate or conductive glass.
2. A method of manufacturing a field emission cathode for a field emission hydrogen sensor as defined in claim 1, wherein: firstly, spin-coating a ZnO seed crystal layer on a substrate, and then obtaining a ZnO nano rod array on the substrate by adopting a hydrothermal method, wherein the temperature of the hydrothermal method is 70-95 ℃, and a transition metal catalyst is not needed.
3. A method of detecting hydrogen in a low pressure hydrogen environment using a field emission hydrogen sensor as claimed in claim 1, comprising:
(1) Determining hydrogen sensing current and pressure curves:
10 under partial pressure of hydrogen -7 -10 -3 The specific steps are as follows:
i) At each measuring point, the field emission cathode is subjected to Joule heating degassing by using an increased emission current, and the intrinsic emission I is measured 0 ;
ii) applying a field emission voltage V and obtaining an initial emission current I 0 And detecting a change in current during a time t;
iii) Dividing t time into N equal intervals according to the requirement, and recording the current I at the end of each interval i ,i=0,…,N;
iv) passing the current I at the end of each interval i Accumulating, and taking an average value to obtain a current I, wherein the current I is used as a gas-sensitive sensing current of the measuring point;
v) after the measurement is finished, the sensor is enabled to emit pulses for one to several times under a higher current, and the purposes of cleaning the surface and recovering the detection function of the sensor are achieved;
drawing a hydrogen sensing current and pressure curve after multi-point testing according to the gas sensing current of the measuring point and the hydrogen partial pressure of the corresponding test;
(2) And detecting the gas-sensitive sensing current in the hydrogen partial pressure environment to be detected, and determining the hydrogen partial pressure value according to the hydrogen sensing current and the pressure curve.
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