CN109828009B - H based on metal oxide semiconductor thin film material2S gas sensor and preparation method thereof - Google Patents
H based on metal oxide semiconductor thin film material2S gas sensor and preparation method thereof Download PDFInfo
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Abstract
H based on metal oxide semiconductor film nano material2An S gas sensor and a preparation method thereof belong to the technical field of semiconductor oxide gas sensors. Firstly, a seed layer is prepared on a gold interdigital electrode of an alumina ceramic substrate, a metal material is deposited on the electrode by adopting an electrochemical deposition method on the basis of the seed layer, and the metal oxide semiconductor thin film material is obtained after thermal annealing. Taking the prepared NiO/CuO film nano material as an example, the method is used for low-concentration H2S gas shows higher response in detecting H2Has good application prospect in the aspect of S content. The preparation method has the advantages of mild conditions, simple synthesis method, low cost, short experimental period and good reproducibility, and therefore, the preparation method has important application value.
Description
Technical Field
The invention belongs to the technical field of semiconductor oxide gas sensors, and particularly relates to a metal oxide semiconductor film nano material-based H2S gas sensor and its preparation method.
Background
The development of social industrialization and human activities have led to an increase in the concentration of various toxic gases in the air, resulting in depletion of the ozone layer, global warming and climate change. Therefore, controlling air pollution is becoming more and more important. Prolonged exposure to low levels of harmful gases can lead to paresthesia, headache, fatigue and even obstruction of oxygen transfer to blood cells. Early detection of toxic gases in the environment has received a great deal of attention in order to protect human health and environmental safety. Metal oxide nanomaterials due to their small size effect and special surfaceThe properties, which represent novel optical, electrical and chemical properties, are the mainstream and hot spots in the chemical sensor field and have been used in important fields such as industrial/home safety. Many semiconductor nanostructured materials such as SnO2，TiO2ZnO, etc. have been widely used as excellent sensing materials.
The traditional gas sensor adopts a tubular structure, and needs to prepare a powder material, coat the powder material on a ceramic tube and finally obtain a sensing device in ways of sintering and the like. The preparation process of the device structure is complex and time-consuming, and the porosity of the prepared sensitive film is difficult to control and the consistency is poor. This problem can be overcome if the sensitive material is grown directly on the substrate.
Various methods have been used to prepare metal oxide nanomaterials, such as sputtering, chemical vapour deposition, sol-gel methods, hydrothermal growth. Electrochemical deposition is a liquid phase process used to produce various polycrystalline thin films and nanostructures, and has been successful in producing materials such as metals, ceramic materials, semiconductors, superlattices, and superconductor films. With the continuous development and deepening of scientific technology, the research field of electrochemical deposition is continuously widened and expanded, and the electrochemical deposition is rapidly developed into a technology with great industrial significance. Electrochemical deposition processes, by their very nature, are typically performed at or slightly above room temperature and are therefore well suited for the preparation of nanostructures. The thickness, chemical composition and structure of the deposited layer can be precisely controlled by controlling the process conditions (e.g., current, potential, solution pH, temperature, concentration, composition, etc.). Therefore, the electrochemical deposition method has the advantages of less equipment investment, simple process, easy operation, safe environment and flexible production mode, is suitable for industrial production and is an economic preparation method.
Disclosure of Invention
Aiming at the advantages of electrochemical deposition in the background technology, the invention provides a preparation method for depositing an oxide semiconductor film on a ceramic substrate and a method for preparing the material in H2S gas sensing field.
The gas sensor is composed of a three-electrode system consisting of a platinum sheet serving as a counter electrode, a saturated calomel electrode serving as a reference electrode and a gold interdigital electrode serving as a working electrode and taking an alumina ceramic sheet as a substrate. And preparing the oxide semiconductor film on the working electrode by using an electrochemical workstation and adopting a constant potential electrodeposition method.
The preparation method of the electrodeposition can obtain nano materials of various substances, can obtain nano materials of various grain sizes, and has low cost and high efficiency. The conditions of the electrosynthesis reaction are mild, and high temperature and high pressure are not generally required. And has the advantages of high reproducibility, simple operation and the like, thereby having important application value. The oxide semiconductor film of the invention is carried out according to a cathodic electrodeposition mechanism, namely: reducing agent (e.g. H) in electrolyte solution when electrodeposition is carried out in prepared electrolyte solution2O，NO3 -Etc.) are first reduced at the electrode surface and OH is formed-(ii) a Subsequently, the metal ions or complexes in the solution react with OH adsorbed on the surface of the electrode-Reacting to generate metal hydroxide; finally, annealing treatment is carried out, and the metal hydroxide is further dehydrated to generate a metal oxide film.
The invention relates to H based on a metal oxide semiconductor film nano material2The preparation method of the S gas sensor takes the preparation of NiO/CuO and noble metal Pt doped NiO nano film material as an example, and comprises the following steps:
(1) immersing a gold interdigital electrode which is purchased and takes an aluminum oxide ceramic chip as a substrate into acetone, and ultrasonically cleaning for 20-40 min; taking out, washing the fabric by using deionized water, then putting the fabric into ethanol for ultrasonic cleaning for 10-20 min, finally putting the fabric into deionized water for ultrasonic cleaning for 10-20 min, and drying the fabric for 1-3 h at the temperature of 30-60 ℃ for later use;
(2) weighing 0.4-1.2 g of nickel nitrate, adding the nickel nitrate into a mixed solution of 5-10 mL of deionized water and 5-10 mL of ethanol, and stirring for 10-20 min until the nickel nitrate is completely dissolved to obtain a nickel nitrate solution; spin-coating a nickel nitrate solution on the gold interdigital electrode obtained in the step (1) for 50-90 s at the speed of 2000-5000 r/min, and finally performing heat treatment in air at the temperature of 200-400 ℃ for 20-60 min, so as to prepare a NiO seed layer with the thickness of 0.1-0.3 mu m on the gold interdigital electrode;
(3) weighing 0.6-1.2 g of nickel nitrate, 0.1-0.5 g of copper nitrate or 0.3-1.0 mL of chloroplatinic acid, adding into a mixed solution of 15-30 mL of deionized water and 15-30 mL of ethanol, and stirring for 30-60 min until the nickel nitrate, the copper nitrate or the chloroplatinic acid are completely dissolved to obtain a mixed solution;
(4) a three-electrode system is adopted, a platinum sheet is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and an aluminum oxide ceramic sheet is used as a gold interdigital electrode with a NiO seed layer of a substrate and used as a working electrode; taking the mixed solution prepared in the step (3) as a deposition solution for electrochemical deposition;
(5) a cathode constant potential electrodeposition method is adopted, a working electrode is used as a cathode, a counter electrode is used as an anode, a constant voltage of-2.0 to-0.5 v is applied to the working electrode, and the deposition time is 200-400 s; annealing the gold interdigital electrode at 400-600 ℃ for 1.5-5.0 hours after deposition, thereby obtaining a metal oxide semiconductor film serving as a nano sensitive material and uniformly growing on the gold interdigital electrode;
(6) and (3) placing the gold interdigital electrode which is obtained in the step (5) and takes the aluminum oxide ceramic wafer as the substrate on a ceramic tube heating sheet (the working temperature of the material can be changed by changing the heating current of the ceramic tube), welding the gold interdigital electrode on a tube seat through a platinum wire lead, and finally welding and packaging the device according to an indirect-heating gas sensitive element to obtain the gas sensor of the metal oxide semiconductor film. The gas sensor based on the oxide semiconductor film nano material prepared by the invention has the following advantages:
1. the nano material of various substances can be prepared by utilizing a simple electrochemical deposition method, the synthesis method is simple, the cost is low, and the experimental period is short;
2. the conditions of the electrochemical deposition method are mild, and high temperature and high pressure are not generally required. And has the advantages of high reproducibility, simple operation and the like, thereby having important application value.
3. By electrochemical deposition of the prepared metal oxide semiconductor thin film material, the H pair is improved2S sensitivity, higher response characteristic, in detecting H2Has wide application in S contentApplication prospect
4. The obtained material can be directly used as a device for gas-sensitive test, does not need further coating, is sintered and is convenient to use.
Drawings
FIG. 1: SEM topography of the NiO/CuO film nano material prepared in example 1; wherein, the magnification of the picture (a) is 3000 times, and the magnification of the insets is 15000 times; (b) the magnification of the figure is 15000 times, and the magnification of the insets is 50000 times; as shown in FIG. 1, the pattern (a) is the morphology of the material prepared on the ceramic substrate, and it can be clearly seen that the material is composed of a large number of cracked small NiO films, and the size of the small NiO films is about 2-10 μm. FIG. b shows the morphology of the material prepared on the gold electrode, which shows the string-like structure composed of particles;
FIG. 2: XRD pattern of NiO/CuO thin film nanomaterial prepared in example 1; NiO and NiO are observed2Indicating that the sample contains NiO and NiO2And in the crystal, because the copper doping amount is less, the corresponding characteristic peak of copper is not detected. Detected Al2O3Because the main component of the ceramic substrate is Al2O3The result is;
FIG. 3: a schematic of the selectivity of the sensor in example 1 to 1ppm of different gases at an operating temperature of 140 ℃; it can be seen that the sensor in the embodiment is opposite to other harmful gases, for H2S has higher sensitivity;
FIG. 4: sensitivity of the sensor in example 1 at optimum operating temperature is dependent on H2S concentration profile. In the embodiment, the sensitivity of the sensor is along with H at the optimum working temperature2The S concentration increases.
FIG. 5: the selectivity of the sensor in example 2 for 1ppm of different gases at a working temperature of 110 ℃; it can be seen that the sensor in the embodiment is opposite to other harmful gases, for H2S has higher sensitivity;
FIG. 6: sensitivity of the sensor in example 2 at optimum operating temperature as a function of H2S concentration profile. In the embodiment, the sensitivity of the sensor is along with H at the optimum working temperature2The S concentration increases.
Note: when no metal oxide thin film material exists on the gold interdigital electrode, the two comb-shaped electrodes are not connected, and the resistance at the two ends of the interdigital electrode is infinite. After the metal oxide film material is deposited on the interdigital electrode, the two non-contact comb-shaped electrodes are conducted due to the existence of the film material, a certain resistance is arranged at the two ends of the measuring electrode, and the resistance is determined by the type of the metal oxide film material, the thickness of the film and other factors.
The sensitivity of the device is defined as the resistance value (R) of the interdigital electrode in the gas to be measuredg) And resistance value (R) in aira) The ratio is S ═ Rg/Ra. During the test, a static test system is used for testing. The device is placed in a 1L gas cylinder, a certain amount of gas to be detected is injected inwards, resistance value change of the gas to be detected is observed and recorded, and a corresponding sensitivity value is obtained through calculation.
Detailed Description
Example 1:
1. placing gold interdigital electrode with aluminum oxide as substrate in beaker, pouring acetone solution to immerse the electrode in acetone completely, and ultrasonic cleaning for 30 min. And then washing with deionized water, putting into ethanol for ultrasonic cleaning for 10min, and finally putting into deionized water for ultrasonic cleaning for 10 min. And placing the mixture in an oven at 40 ℃ for 2h to dry for later use.
2. Weighing 0.4362g of nickel nitrate, adding the nickel nitrate into a mixed solution of 5mL of deionized water and 5mL of ethanol, and stirring for 10 min; and (3) performing spin coating on the prepared nickel nitrate solution on the gold interdigital electrode for 60s at 3000r/min by using a spin coater. Finally, heat-treating in the air at 300 ℃ for 30min to prepare a NiO seed layer on the gold interdigital electrode, wherein the thickness of the seed layer is about 0.25 mu m;
3. weighing 1.0469g of nickel nitrate and 0.0966g of copper nitrate, adding the nickel nitrate and the 0.0966g of copper nitrate into a mixed solution of 20mL of deionized water and 20mL of ethanol, and stirring for 30min to obtain a deposition solution for electrochemical deposition;
4. cathodic potentiostatic electrodeposition is achieved using an electrochemical workstation. And (3) constructing a three-electrode system, wherein a platinum sheet is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and a gold interdigital electrode with a NiO seed layer and an aluminum oxide substrate is used as a working electrode. And (3) adopting a cathode constant potential electrodeposition method, taking a working electrode as a cathode and a counter electrode as an anode, applying a constant voltage of-1 v to the working electrode for 300s, and depositing the product on the interdigital electrode. And finally sintering for 2 hours at 500 ℃ to obtain the NiO/CuO metal oxide semiconductor film material uniformly grown on the interdigital electrode, wherein the film thickness is about 1.1 mu m.
5. Placing the prepared interdigital electrode on a ceramic tube heating sheet, changing the working temperature of the material by changing the heating current of the ceramic tube, welding the interdigital electrode on a tube seat by a platinum wire lead, and finally welding and packaging the device to obtain the H prepared based on the NiO/CuO composite film material2And (S) a gas sensor.
Table 1: gas-sensitive response data of NiO/CuO film nano material at different working temperatures
Table 2: data of variation of gas-sensitive response of NiO/CuO sensitive film material sensor along with concentration of hydrogen sulfide gas
Connecting the sensor to Rigol signal tester, and respectively placing the above sensitive film gas sensor in air and 1ppm H2Testing in the atmosphere of S, and recording the resistance change conditions in different atmospheres; the sensors with NiO/CuO sensitive film material were placed in air at 0.5ppm, 1ppm, 5ppm and 10ppm H2And carrying out gas-sensitive test in the atmosphere of S.
Table 1 shows that the prepared NiO/CuO sensitive film material can react to 1ppm H at different working temperatures2Gas sensitive response of S, as can be seen from the table, the device is sensitive to H at different operating temperatures2S gas response has an "increase-maxThe trend of-decrease ", the response value being maximal at 140 ℃, 19.3. This variation is because the response of the gas sensor depends on the chemical reaction between the oxygen adsorbed on its surface and the gas molecules to be measured. H to be tested at relatively low temperatures2The S gas molecules do not have sufficient thermal energy to react with the adsorbed oxygen on the membrane surface and therefore the response is relatively low. With increasing operating temperature, H2The S gas molecules become active and are able to overcome the activation energy barrier of the reaction on the membrane surface, which results in a significant increase in response. But with further increase in operating temperature due to H2The adsorption of S gas molecules is difficult, the utilization rate of the NiO film surface is low, and the response of the gas sensor begins to be reduced. The response of the sensor therefore exhibits a tendency to "rise". According to the results of table 1, the device exhibited the best gas sensing characteristics at 140 ℃. Therefore, the optimum working temperature of the NiO/CuO sensitive film material is 140 ℃.
Meanwhile, Table 2 shows that the prepared NiO/CuO sensitive film material has different concentrations of H at the working temperature of 140 DEG C2Gas-sensitive response of S gas. It can be seen that the gas sensitive response value varies with H2The increasing concentration of S gas shows high sensitivity and low H concentration2S also has an acceptable response value. As the two results show, the sensitivity of the device can be effectively improved by changing the working temperature of the device, and the metal oxide sensitive film material has low H concentration2S gas has good response, and the metal oxide sensitive film material is hopeful to be used for manufacturing high-performance H2Promising materials for S-sensors.
Example 2:
1. placing gold interdigital electrode with aluminum oxide as substrate in beaker, pouring acetone solution to immerse the electrode in acetone completely, and ultrasonic cleaning for 30 min. And then washing with deionized water, putting into ethanol for ultrasonic cleaning for 10min, and finally putting into deionized water for ultrasonic cleaning for 10 min. And placing the mixture in an oven at 40 ℃ for 2h to dry for later use.
2. Weighing 0.4362g of nickel nitrate, adding the nickel nitrate into a mixed solution of 5mL of deionized water and 5mL of ethanol, and stirring for 10 min; and (3) performing spin coating on the prepared nickel nitrate solution on the gold interdigital electrode for 60s at 3000r/min by using a spin coater. Finally, heat-treating in the air at 300 ℃ for 30min to prepare a NiO seed layer on the gold interdigital electrode, wherein the thickness of the seed layer is about 0.25 mu m;
3. weighing 1.0469g of nickel nitrate and 0.402mL of chloroplatinic acid, adding the nickel nitrate and the chloroplatinic acid into a mixed solution of 20mL of deionized water and 20mL of ethanol, and stirring for 30min to obtain a deposition solution for electrochemical deposition;
4. cathodic potentiostatic electrodeposition is achieved using an electrochemical workstation. And (3) constructing a three-electrode system, wherein a platinum sheet is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and a gold interdigital electrode with a NiO seed layer and an aluminum oxide substrate is used as a working electrode. And (3) adopting a cathode constant potential electrodeposition method, taking a working electrode as a cathode and a counter electrode as an anode, applying a constant voltage of-1 v to the working electrode for 300s, and depositing the product on the interdigital electrode. And finally sintering the film at 500 ℃ for 2 hours to obtain the Pt-supported NiO semiconductor film material which uniformly grows on the interdigital electrode, wherein the film thickness is about 1.1 mu m.
5. Placing the prepared interdigital electrode on a ceramic tube heating sheet, changing the working temperature of the material by changing the heating current of the ceramic tube, welding the interdigital electrode on a tube seat by a platinum wire lead, and finally welding and packaging the device to obtain the H prepared from the Pt-supported NiO sensitive film material2And (S) a gas sensor.
Table 3: gas-sensitive response data of Pt-supported NiO sensitive film nano material at different working temperatures
Table 4: gas-sensitive response of sensor made of Pt-supported NiO sensitive thin film material along with change of concentration of hydrogen sulfide gas
Connecting the sensor to Rigol signal tester, and respectively placing the above sensitive film gas sensor in air and 1ppm H2Testing in the atmosphere of S, and recording the resistance change conditions in different atmospheres; the sensors with NiO/CuO sensitive film material were placed in air at 0.1ppm, 0.2ppm, 0.5ppm, 1ppm, 2ppm and 5ppm H2And carrying out gas-sensitive test in the atmosphere of S.
Table 3 shows that the prepared Pt-supported NiO sensitive film material can react to 1ppm H at different working temperatures2Gas sensitive response of S, as can be seen from the table, the device is sensitive to H at different operating temperatures2The response of S gas had a tendency of "increase-max-decrease", with a maximum response value of 14.9 at 110 ℃. This variation is because the response of the gas sensor depends on the chemical reaction between the oxygen adsorbed on its surface and the gas molecules to be measured. According to the results of table 1, the device exhibited the best gas sensing characteristics at 110 ℃. Therefore, the optimal working temperature of the prepared Pt supported NiO sensitive film material is 110 ℃.
Meanwhile, Table 4 lists that the prepared Pt supported NiO sensitive film material has different concentrations H at the optimal working temperature of 110 DEG C2Gas-sensitive response of S gas. It can be seen that the gas sensitive response value varies with H2The increasing concentration of S gas shows high sensitivity and low H concentration2S also has an acceptable response value. As can be seen from the above two results, the change of the working temperature of the device can effectively improve the sensitivity of the device, and the noble metal supported metal oxide sensitive film material has low H concentration2S gas has good response, and the metal oxide sensitive film material is hopeful to be used for manufacturing high-performance H2Promising materials for S-sensors.
Claims (2)
1. H based on metal oxide semiconductor film nano material2The preparation method of the S gas sensor comprises the following steps:
(1) immersing a gold interdigital electrode taking an aluminum oxide ceramic wafer as a substrate into acetone, and ultrasonically cleaning for 20-40 min; taking out, washing the fabric by using deionized water, then putting the fabric into ethanol for ultrasonic cleaning for 10-20 min, finally putting the fabric into deionized water for ultrasonic cleaning for 10-20 min, and drying the fabric for 1-3 h at the temperature of 30-60 ℃ for later use;
(2) weighing 0.4-1.2 g of nickel nitrate, adding the nickel nitrate into a mixed solution of 5-10 mL of deionized water and 5-10 mL of ethanol, and stirring for 10-20 min until the nickel nitrate is completely dissolved to obtain a nickel nitrate solution; spin-coating a nickel nitrate solution on the gold interdigital electrode obtained in the step (1) for 50-90 s at the speed of 2000-5000 r/min, and finally performing heat treatment in air at the temperature of 200-400 ℃ for 20-60 min, so as to prepare a NiO seed layer with the thickness of 0.1-0.3 mu m on the gold interdigital electrode;
(3) weighing 0.6-1.2 g of nickel nitrate and 0.1-0.5 g of copper nitrate, or adding 0.6-1.2 g of nickel nitrate and 0.3-1.0 mL of chloroplatinic acid into a mixed solution of 15-30 mL of deionized water and 15-30 mL of ethanol, and stirring for 30-60 min until the nickel nitrate and the copper nitrate are completely dissolved to obtain a mixed solution;
(4) a three-electrode system is adopted, a platinum sheet is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, and an aluminum oxide ceramic sheet is used as a gold interdigital electrode with a NiO seed layer of a substrate and used as a working electrode; taking the mixed solution prepared in the step (3) as a deposition solution for electrochemical deposition;
(5) a cathode constant potential electrodeposition method is adopted, a working electrode is used as a cathode, a counter electrode is used as an anode, a constant voltage of-2.0 to-0.5 v is applied to the working electrode, and the deposition time is 200 to 400 s; annealing the gold interdigital electrode at 400-600 ℃ for 1.5-5.0 hours after deposition, thereby obtaining a metal oxide semiconductor film serving as a nano sensitive material and uniformly growing on the gold interdigital electrode;
(6) placing the gold interdigital electrode which is obtained in the step (5) and takes the aluminum oxide ceramic wafer as the substrate on a ceramic tube heating plate, welding the gold interdigital electrode on a tube seat through a platinum wire lead, and finally welding and packaging the device according to an indirectly heated gas sensitive element to obtain the H based on the metal oxide semiconductor film nano material2And (S) a gas sensor.
2. A kind ofH based on metal oxide semiconductor film nano material2S gas sensor, its characterized in that: is prepared by the method of claim 1.
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| CN110844948A (en) * | 2019-10-22 | 2020-02-28 | 刘沛源 | Cobalt-doped porous nickel oxide gas-sensitive material, gas-sensitive element, preparation method and application |
| CN113049646B (en) * | 2021-03-16 | 2022-02-08 | 吉林大学 | Based on Cu7S4Hydrogen sulfide sensor made of-CuO graded structure micro-flower sensitive material and preparation method thereof |
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