CN107894448B - Photo-assisted gas sensitive element of boron-doped titanium dioxide, preparation method and application - Google Patents
Photo-assisted gas sensitive element of boron-doped titanium dioxide, preparation method and application Download PDFInfo
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Abstract
The invention discloses a boron-doped titanium dioxide photo-assisted gas sensor, a preparation method and application thereof, wherein the method is used for treating TiO by a boron-doped mode2The modified gas-sensitive element is used for preparing a light-assisted gas-sensitive element, and the method has mild condition and easy operationPrepared B/TiO2The gas sensitive element shows better H under the action of ultraviolet light2And CO, and shows good stability and repeatability, thereby being beneficial to promoting the practical application of the semiconductor photo-assisted gas sensor.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to a boron-doped titanium dioxide photo-assisted gas sensor, and a preparation method and application thereof.
Background
With the development of industry, environmental problems are becoming more serious, and thus monitoring of toxic, harmful, flammable and the like gases in the air is becoming more important. Gas sensors have been widely used in the fields of industrial production, home security, environmental monitoring, medical care, petrochemical industry, and the like. The semiconductor metal oxide has the advantages of high sensitivity, short response time, lower cost, simple and convenient processing, no toxicity, environmental protection and the like, so the semiconductor metal oxide is most widely applied. Currently, the most widely used gas-sensitive materials are mainly n-or p-type metal oxides, such as: TiO 22，ZnO，SnO2，WO3And the like. But there are some problems in the use: the stability is poor, the selectivity is low, the working temperature is high, the energy consumption is high, the safety problem exists, the service life is short, the intellectualization is low, and the like. Therefore, it is required to develop a novel gas sensor. Because the semiconductor material has the characteristics of light absorption and photoconduction, and photoresponse can occur under the illumination condition of a certain wavelength to generate photo-generated electrons, the improvement of the sensitivity of the metal oxide gas sensor by light excitation is a new idea. TiO 22Not only has good ultraviolet light catalytic activity, but also has good gas-sensitive characteristic for specific gas, so that the catalyst has good ultraviolet light catalytic activity and good gas-sensitive characteristic for TiO2The research of modifying the material and improving the sensitivity, the repeatability and the stability has certain practical significance.
H2As a clean energy source, it has flammable and explosive propertiesThe production, storage and use have great safety problems; CO is not only flammable and explosive, but also easily causes great harm to human bodies in industrial and indoor environments. H2And CO are both colorless, odorless gases and thus are directed to H2And CO monitoring is of paramount importance. By doping the TiO with elements2The introduction of impurity energy level can effectively improve the H pair2Gas sensitive response, repeatability and stability of CO.
Disclosure of Invention
Aiming at the defects of the existing gas sensitive material, the invention aims to provide a preparation method and application of a boron-doped titanium dioxide photo-assisted gas sensitive element, which is simple in preparation method, mild in reaction condition, rapid and easy to implement.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a boron-doped titanium dioxide photo-assisted gas sensor comprises the following steps: under stirring, adding H3BO3Dropwise adding the solution into isopropyl titanate, uniformly stirring, drying, and calcining the obtained material to obtain B/TiO2Powder, then dropping the B/TiO by the drop coating method2And coating the powder on the surface of the gold interdigital electrode plate, and then roasting to obtain the boron-doped titanium dioxide photo-assisted gas sensitive element.
Said H3BO3The dosage ratio of the titanium acid isopropyl ester is 1 g: 5-6.5 mL, and the preferred dosage ratio is 1 g: 5.83 mL.
The stirring condition is that stirring is carried out for 8-12 h at room temperature, and the drying condition is 90-110 ℃.
The temperature for calcining the material is 400-600 ℃.
The invention is prepared from B/TiO2The method for preparing the photo-assisted gas sensor of the boron-doped titanium dioxide by the powder comprises the following specific steps: ultrasonic washing the gold interdigital electrode plate for 20-30min by using deionized water and ethanol in sequence, and drying for later use; weighing B/TiO2Putting the powder into a medicine bottle, dripping ethylene glycol, and performing ultrasonic dispersion to obtain a gas-sensitive material, wherein B/TiO2The ratio of the powder to the ethylene glycol was 30And mg: 1mL, then using a liquid transfer gun to transfer 45-50 mu L of gas sensitive material drops on the surface of the gold interdigital electrode plate, drying at 70-80 ℃ after the gold interdigital electrode plate is uniformly spread, finally placing the gold interdigital electrode plate in a muffle furnace, heating to 400-600 ℃, roasting for 1-1.5h, naturally cooling, and then taking out to obtain the boron-doped titanium dioxide photo-assisted gas sensitive element.
Further, the temperature rise rate is 1 ℃/min.
The invention also provides application of the boron-doped titanium dioxide photo-assisted gas sensor, and the gas sensor can be used for H at room temperature under ultraviolet illumination2And CO shows better gas-sensitive response.
The invention has the following effects and advantages: with pure TiO2Compared with a gas sensor, the B/TiO of the invention2The photo-assisted gas sensitive element has better gas sensitive response under the irradiation of ultraviolet light and room temperature, and has stable photo-assisted gas sensitive performance and good repeatability. The invention dopes TiO by the element B2The modification is carried out, the preparation method is simple, the condition is mild, the operation is easy, and especially for H2Gas sensitive response of the invention, boron doped TiO2Electrons are more readily available. The invention is beneficial to the preparation and application of the actual photo-assisted gas sensor and provides a new idea and direction for the preparation of other gas sensitive materials.
Drawings
FIG. 1 shows TiO prepared in example 12、B/TiO2XRD spectrum of the material;
FIG. 2 shows TiO prepared in example 12、B/TiO2DRS profile of material;
FIG. 3 shows TiO prepared in example 12、B/TiO2A TEM spectrum of the material;
FIG. 4 shows TiO prepared in example 12Gas sensor and B/TiO2Gas sensor is aligned to H in nitrogen atmosphere at room temperature2The ultraviolet light assisted gas sensitive response performance is compared;
FIG. 5 shows TiO obtained in example 12Gas sensor and B/TiO2And the gas sensor compares the ultraviolet assisted gas-sensitive response performance of the gas sensor to CO in nitrogen atmosphere at room temperature.
Detailed Description
In order to make the aforementioned features and advantages of the present invention more comprehensible, the present invention is described in further detail below with reference to the accompanying drawings and the embodiments, but the present invention is not limited thereto.
Preparation method of photo-assisted gas sensor of boron-doped titanium dioxide
1) Under stirring, adding H3BO3The solution is added dropwise to isopropyl titanate, H3BO3The dosage ratio of the titanium acid to the isopropyl titanate is 1 g: 5-6.5 mL, the mixture is stirred for 8-12 h at room temperature and then dried at 90-110 ℃, and the obtained material is calcined at 400-600 ℃ to obtain B/TiO2Powder;
2) ultrasonic washing the gold interdigital electrode plate for 20-30min by using deionized water and ethanol in sequence, and drying for later use;
3) 30mg of B/TiO are weighed2And putting the powder into a medicine bottle, dropping 1mL of ethylene glycol, performing ultrasonic dispersion to obtain a gas-sensitive material, then transferring 50 mu L of the gas-sensitive material to the surface of the gold interdigital electrode plate by using a liquid transfer gun, drying at 70-80 ℃ after the gold interdigital electrode plate is uniformly spread, finally placing the gold interdigital electrode plate in a muffle furnace, heating to 400-600 ℃, roasting for 1-1.5h at the heating rate of 1 ℃/min, naturally cooling, and taking out to obtain the boron-doped titanium dioxide photo-assisted gas-sensitive element.
Example 1
TiO2And B/TiO2Preparation of gas sensor
Preparation of B/TiO2Materials: 1.24g of H are taken3BO3Adding 50ml of deionized water into a 100ml beaker for dissolution, dropwise adding 7ml of isopropyl titanate under continuous stirring, stirring at room temperature for 12h, baking at 100 ℃ for 12h, and baking at 500 ℃ for 1 h.
Preparation of TiO2Materials: 50ml of deionized water is taken to be put into a 100ml beaker, 7ml of isopropyl titanate is added dropwise under the condition of continuous stirring, the mixture is baked for 12 hours at the temperature of 100 ℃ and baked for 1 hour at the temperature of 500 ℃.
And (3) firstly, washing the gold interdigital electrode plate by using deionized water and ethanol through ultrasonic treatment for 20min respectively, and drying for later use.
30mg of TiO are weighed out separately2、B/TiO2And (2) respectively dripping 1ml of glycol into two 1.5ml medicine bottles, ultrasonically dispersing for 1h, transferring 50 mu L of the powder onto a cleaned electrode piece by using a liquid transfer gun, uniformly spreading the powder, drying at 80 ℃, finally, putting the electrode piece into a muffle furnace, heating (the heating rate is 1 ℃/min) to 500 ℃, calcining for 1h, naturally cooling to room temperature, and taking out to obtain the required gas sensitive element.
Measurement of gas sensitivity
Example 1 preparation of TiO2、B/TiO2The light-assisted gas-sensitive response test of the gas-sensitive element is carried out by combining a JF02E type gas-sensitive test system (Kunming noble research King-Pong scientific and technological company) with a self-designed device. The gas sensor was placed in a sealed gas cell (with a quartz window) made of stainless steel and having a capacity of 100ml, and light was supplied from four 365nm UV fluorescent lamps (4W, Philips TL/05). With high purity N2And (3) as background gas, introducing gas to be detected with different concentrations into the gas chamber, and controlling the total flow to be 250 ml/min. The response of the gas sensor to various gases is represented by resistance change, the resistance of the gas sensor is tested by a JF02E type gas sensitive test system (Kunming noble research King-Pond technologies Co.), and the working voltage is 8.5V. After the gas sensitive element is arranged in a gas chamber, pretreatment is carried out, firstly, the gas sensitive element is heated to 200 ℃, and is swept in a background atmosphere for a certain time to remove water and other gases adsorbed on the surface, and then, the gas sensitive element is cooled to room temperature to switch gas testing.
According to this method, the gas sensor pair H prepared in example 1 was evaluated separately2And the light assisted gas sensing performance of CO, the results of which are shown in fig. 4-5.
As can be seen from FIG. 1, TiO synthesized according to example 12And B/TiO2XRD spectrum was analyzed by X' Pert HighScore software: TiO 22The diffraction peak at 30.81 degrees (121) is a characteristic peak of brookite, and other peaks are all characteristic peaks of anatase and indicate that the prepared TiO is2Mainly in anatase form with a small content of brookite, and B/TiO2Two B's appear at 14.56 deg., 27.77 deg. (310)2O3And the brookite (121) diffraction peak substantially disappeared, indicating that the B-doped TiO2The crystal form of (a) is changed.
As can be seen from the UV-visible diffuse reflectance spectrum of FIG. 2, B/TiO2The absorption wavelength of (2) is shifted slightly in the long wavelength direction, so that a red shift occurs, and the band gap width does not change greatly.
The TEM image analysis result of FIG. 3 is consistent with the XRD analysis result, with a small amount of B during doping2O3Are present.
As can be seen from the gas-sensitive result chart of FIG. 4, H was introduced2Of TiO 22Resistance rise of gas sensor, H2Exhibit electron-donating behavior, while B/TiO2The resistance of the gas sensor is in a downward trend, H2Shows electron donating behavior and higher response value, which indicates that the TiO doped with B2Is favorable to H2Giving electrons when adsorbed on its surface.
As can be seen from FIG. 5, B/TiO2The response sensitivity to CO is obviously improved, and the repeatability and the stability are better. This illustrates the doping of TiO by way of element B2The modification can effectively improve the room temperature to H under the action of ultraviolet light2And CO, and the preparation method is simple and easy to implement, thereby being beneficial to the preparation aspect of the actual photo-assisted gas sensor and providing a new idea and direction for the preparation of other gas-sensitive materials.
Example 2
Preparation method of photo-assisted gas sensor of boron-doped titanium dioxide
1) Under stirring, adding H3BO3The solution is added dropwise to isopropyl titanate, H3BO3The dosage ratio of the titanium acid to isopropyl titanate is 1 g: 6 mL, the mixture is stirred for 12h at room temperature and then dried at 100 ℃, and the obtained material is calcined at 500 ℃ to obtain B/TiO2Powder;
2) ultrasonic washing the gold interdigital electrode plate for 25min by using deionized water and ethanol in sequence, and drying for later use;
3) 30mg of B/TiO are weighed2Putting the powder into a medicine bottle, dripping 1mL of ethylene glycol, performing ultrasonic dispersion to obtain a gas-sensitive material, and then transferring 50 mu L of the gas-sensitive material to the gold interdigital electrode by using a liquid transfer gunAnd (3) drying the surface of the sheet at 80 ℃ after the sheet is uniformly spread, finally placing the gold interdigital electrode sheet in a muffle furnace, heating to 500 ℃ (the heating rate is 1 ℃/min), roasting for 1h, naturally cooling, and taking out to obtain the boron-doped titanium dioxide photo-assisted gas sensitive element.
Example 3
Preparation method of photo-assisted gas sensor of boron-doped titanium dioxide
1) Under stirring, adding H3BO3The solution is added dropwise to isopropyl titanate, H3BO3The dosage ratio of the titanium acid to isopropyl titanate is 1 g: 5mL, the mixture is stirred for 8 hours at room temperature and then dried at 110 ℃, and the obtained material is calcined at 400 ℃ to obtain B/TiO2Powder;
2) ultrasonic washing the gold interdigital electrode plate for 20min by using deionized water and ethanol in sequence, and drying for later use;
3) 30mg of B/TiO are weighed2And putting the powder into a medicine bottle, dropping 1mL of ethylene glycol, performing ultrasonic dispersion to obtain a gas-sensitive material, then using a liquid-transferring gun to transfer 50 muL of the gas-sensitive material to drop on the surface of the gold interdigital electrode plate, drying at 70 ℃ after the gold interdigital electrode plate is uniformly spread, finally placing the gold interdigital electrode plate into a muffle furnace, heating to 400 ℃ (the heating rate is 1 ℃/min), roasting for 1.5h, naturally cooling, and taking out to obtain the boron-doped titanium dioxide photo-assisted gas-sensitive element.
Example 4
Preparation method of photo-assisted gas sensor of boron-doped titanium dioxide
1) Under stirring, adding H3BO3The solution is added dropwise to isopropyl titanate, H3BO3The dosage ratio of the titanium acid to isopropyl ester is 1 g: 6.5 mL, the mixture is stirred for 10 hours at room temperature and then dried at 90 ℃, and the obtained material is calcined at 600 ℃ to obtain B/TiO2Powder;
2) ultrasonic washing the gold interdigital electrode plate for 30min by using deionized water and ethanol in sequence, and drying for later use;
3) 30mg of B/TiO are weighed2Putting the powder into a medicine bottle, dripping 1mL of ethylene glycol, performing ultrasonic dispersion to obtain a gas-sensitive material, and then transferring 50 mu L of the gas-sensitive material to a gold interdigital electrode by using a liquid-transferring gunAnd (3) drying the surface of the pole piece at 75 ℃ after the pole piece is uniformly spread, finally placing the gold interdigital electrode plate in a muffle furnace, heating to 600 ℃ (the heating rate is 1 ℃/min), roasting for 1.5h, naturally cooling, and taking out to obtain the boron-doped titanium dioxide photo-assisted gas sensitive element.
Claims (4)
1. The application of the light-assisted gas sensor of boron-doped titanium dioxide is characterized in that: the preparation method of the photo-assisted gas sensor comprises the following steps: (1) under stirring, adding H3BO3The solution is added dropwise to isopropyl titanate, H3BO3The dosage ratio of the titanium acid to the isopropyl titanate is 1 g: 5-6.5 mL, the mixture is stirred for 8-12 h at room temperature and then dried at 90-110 ℃, and the obtained material is calcined to obtain B/TiO2Powder; (2) ultrasonic washing the gold interdigital electrode plate for 20-30min by using deionized water and ethanol in sequence, and drying for later use; weighing B/TiO2Putting the powder into a vessel, dripping ethylene glycol, and performing ultrasonic dispersion to obtain the gas-sensitive material, wherein B/TiO2The dosage ratio of the powder to the ethylene glycol is 30 mg: 1mL, then a liquid-transferring gun is used for transferring 45-50 muL of gas-sensitive material to drop on the surface of the gold interdigital electrode plate, the gold interdigital electrode plate is dried at 70-80 ℃ after being uniformly spread, finally, the gold interdigital electrode plate is placed in a muffle furnace, is heated to 400-600 ℃, is roasted for 1-1.5h, and is taken out after natural cooling, so that the boron-doped titanium dioxide photo-assisted gas-sensitive element is obtained;
the light-assisted gas sensor is used for H-gas at room temperature under ultraviolet light conditions2Or CO produces a gas sensitive response.
2. The use of the photo-assisted gas sensor of boron-doped titanium dioxide as claimed in claim 1, wherein: said H3BO3The dosage ratio of the titanium acid isopropyl ester and the titanium acid isopropyl ester is 1 g: 5.83 mL.
3. The use of the photo-assisted gas sensor of boron-doped titanium dioxide as claimed in claim 1, wherein: the temperature for calcining the material is 400-600 ℃.
4. The use of the photo-assisted gas sensor of boron-doped titanium dioxide as claimed in claim 1, wherein: during roasting, the heating rate is 1 ℃/min.
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