CN112624202A - Preparation method of lanthanum ferrite gas-sensitive material with high specific surface area - Google Patents
Preparation method of lanthanum ferrite gas-sensitive material with high specific surface area Download PDFInfo
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Abstract
The invention discloses a preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area, which comprises the following steps: lanthanum nitrate hexahydrate and ferric nitrate nonahydrate in a certain atomic ratio are used as precursors, and a lanthanum ferrite composite material with a flocculent microstructure is obtained by a sol-gel method through the technologies of high-specific-surface-area dispersant addition, solution evaporation, high-temperature sintering and the like. The lanthanum ferrite prepared by the invention is a p-type semiconductor material and is suitable for early warning of low-concentration ethanol gas. The lanthanum ferrite nano material has high specific surface area, and shows good sensitivity and response recovery characteristics to ethanol gas.
Description
Technical Field
The invention relates to a preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area, which can be used for preparing a semiconductor gas sensor and effectively detecting and monitoring low-concentration dangerous gas.
Background
The gas sensor is a device capable of detecting the type and concentration of external gas, and the mechanism of the gas sensor is that the resistance value of the sensor is changed and correspondingly converted into an electric signal by carrying out physical adsorption or chemical adsorption with the external gas. The sensor can be used for safely and effectively detecting explosive, inflammable and toxic gases and waste gases.
At present, metal semiconductor oxide gas sensors are widely researched due to low preparation cost, low power consumption, wide application and the like of metal semiconductor oxides, such as SnO2、ZnO、In2O3、CuO、Co3O4NiO, etc. Wherein LaFeO3The P-type semiconductor oxide with a narrower forbidden band width has a wide application prospect in the fields of photocatalysis, gas sensitivity, magnetic performance and the like.
The semiconductor metal oxide gas sensor realizes qualitative and quantitative detection of special gas mainly through different changes of resistance values caused by adsorption and desorption of atoms on the surface of a material in different gas atmospheres. When the P-type semiconductor gas-sensitive material is placed in the air, oxygen molecules in the air and atoms on the surface of the material are adsorbed and desorbed, wherein atomic valence bands on the surface lose electrons and are combined with the adsorbed oxygen molecules to be converted into O2-、O-、O2-. The loss of the valence band electrons on the surface of the material reduces the electron concentration on the surface layer of the material, and a hole accumulation layer is formed, so that the resistance of the surface layer of the material is reduced. When the material is in the reducing gas atmosphere, electrons provided by the reducing gas are counteracted with holes on the surface layer of the material, the carrier concentration is reduced, and the resistance value of the semiconductor oxide is increased.
The semiconductor gas-sensitive material is mainly affected by two factors, namely, the change of the shape, the size and the structure of the material and the doping of other elements. The gas-sensitive materials with different shapes and sizes are prepared by different synthesis methods, and the active stable points on the surface of the material are increased by increasing the specific surface area of the material, so that the performance of the gas-sensitive material is improved. By doping high-price elements, the hole concentration of the P-type semiconductor material can be increased, the carrier concentration of the material can be increased, and the resistance of the surface of the material can be reduced.
Disclosure of Invention
The invention designs a preparation process of a lanthanum ferrite gas-sensitive material with high specific surface area aiming at the defects of sensitivity and response recovery time of a P-type semiconductor oxide gas-sensitive material, can be used as a low-concentration gas sensor material, and has higher sensitivity and lower response recovery time to ethanol.
LaFeO3The nano material is a typical P-type metal oxide semiconductor material, the forbidden bandwidth is between 2.0eV at room temperature, the low forbidden bandwidth can improve the electron transition rate and reduce the response recovery time, and the nano material has high thermal stability, so the nano material can be used as an excellent gas sensitive material.
The experiment adopts a sol-gel method to prepare the lanthanum ferrite nano flocculent particles. LaFeO prepared by sol-gel method3The sensor has high specific surface area and low forbidden band width, can increase the surface defects of materials, and improves the oxygen adsorption capacity and rate, thereby increasing the sensitivity of the sensor and improving the recovery rate.
A preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area is characterized in that the preparation method adopts a sol-gel method, a proper amount of activated carbon dispersing agent with high specific surface area is added, and flocculent lanthanum ferrite nano material with high specific surface area is obtained by adjusting the pH value of a solution. The method comprises the following specific steps: firstly, stirring 2.165g of lanthanum nitrate nonahydrate, 2.02g of ferric nitrate hexahydrate and 100 mL of deionized water for 0.5-1 h. After the nitrate is completely dissolved, adding 3-9 g of citric acid, and continuously stirring for 0.5-1 h; secondly, the activated high specific surface area activated carbon is prepared by the following steps of: 1: 2-3, continuously stirring for 4-8 h, and then titrating by ammonia water to slowly adjust the pH of the solution to 5-7; pouring the mixed solution into a constant-temperature water bath cup at 67-75 ℃, after the volume of the solution is reduced by about 40-60%, transferring the collected sol into a drying oven, and drying and foaming for 7 hours at 150-240 ℃ to obtain a brown fluffy sample. And fourthly, after fully grinding, placing the brown powder into a muffle furnace to be sintered for 2-6 hours at 400-650 ℃ to obtain the high-surface-area lanthanum ferrite nano material.
The invention has the advantages that: LaFeO prepared by sol-gel method3The sensitivity of the gas sensor is higher, and LaFeO prepared by a sol-gel method at the working temperature of 240 DEG C3The response value to 100ppm ethanol reached 224.87, the response time was 110s, and the recovery time was 100 s.
Drawings
FIG. 1 is an XRD (X-ray diffraction) graph of a lanthanum ferrite nano material prepared by the first embodiment; FIG. 2 is a scanning electron microscope image of a lanthanum ferrite nanomaterial prepared in accordance with one embodiment; FIG. 3 is a graph showing a relationship between a temperature and a sensitivity of a gas-sensitive property of a lanthanum ferrite nanomaterial prepared in accordance with the first embodiment with respect to 100ppm ethanol; FIG. 4 is a graph showing the response recovery of the lanthanum ferrite nanomaterial prepared according to the first embodiment to 100ppm ethanol at 240 ℃.
The first embodiment is as follows: a preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area comprises the following specific steps: firstly, 2.165g of lanthanum nitrate nonahydrate, 2.02g of ferric nitrate hexahydrate and 100 mL of deionized water are stirred for 0.5 h. After the nitrate is completely dissolved, adding 5g of citric acid, and continuously stirring for 0.5 h; secondly, the activated high specific surface area activated carbon is prepared by the following steps of: 1:2.5, continuously stirring for 4 hours, and then titrating by ammonia water to slowly adjust the pH value of the solution to 6; and thirdly, pouring the mixed solution into a constant-temperature water bath cup at 70 ℃, after the volume of the solution is reduced by about 50%, transferring the collected sol into a drying oven, and drying and foaming the sol for 7 hours at 180 ℃ to obtain a brown fluffy sample. And fourthly, after fully grinding, placing the brown powder into a muffle furnace for sintering for 6 hours at 400 ℃ (the heating rate is 1 ℃/min), and obtaining the high-surface-area lanthanum ferrite nano material.
The second embodiment is as follows: a preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area comprises the following specific steps: first, 2.165g of lanthanum nitrate nonahydrate, 2.02g of ferric nitrate hexahydrate and 100 mL of deionized water were stirred for 1 h. After the nitrate is completely dissolved, adding 7 g of citric acid, and continuously stirring for 1 h; secondly, the activated high specific surface area activated carbon is prepared by the following steps of: 1:2, after continuously stirring for 6 hours, titrating by ammonia water to slowly adjust the pH value of the solution to 5; and thirdly, pouring the mixed solution into a constant-temperature water bath cup at 67 ℃, after the volume of the solution is reduced by about 40%, transferring the collected sol into a drying oven, and drying and foaming the sol for 7 hours at 150 ℃ to obtain a brown fluffy sample. And fourthly, after fully grinding, placing the brown powder into a muffle furnace for sintering for 4 hours at 500 ℃ (the heating rate is 3 ℃/min), and obtaining the high-surface-area lanthanum ferrite nano material.
The third concrete implementation mode: a preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area comprises the following specific steps: first, 2.165g of lanthanum nitrate nonahydrate, 2.02g of ferric nitrate hexahydrate and 100 mL of deionized water were stirred for 1 h. After the nitrate is completely dissolved, adding 3 g of citric acid, and continuously stirring for 0.5 h; secondly, the activated high specific surface area activated carbon is prepared by the following steps of: 1:3, after continuously stirring for 8 hours, titrating by ammonia water to slowly adjust the pH value of the solution to 7; and thirdly, pouring the mixed solution into a constant-temperature water bath cup at 75 ℃, transferring the collected sol into a drying oven after the volume of the solution is reduced by about 60%, and drying and foaming the sol for 7 hours at 200 ℃ to obtain a brown fluffy sample. And fourthly, after fully grinding, placing the brown powder into a muffle furnace for 550 ℃ (the heating rate is 5 ℃/min) to be sintered for 3 hours, and obtaining the high-surface-area lanthanum ferrite nano material.
The fourth concrete implementation mode: a preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area comprises the following specific steps: firstly, 2.165g of lanthanum nitrate nonahydrate, 2.02g of ferric nitrate hexahydrate and 100 mL of deionized water are stirred for 0.5 h. After the nitrate is completely dissolved, 9 g of citric acid is added, and the mixture is continuously stirred for 1; secondly, the activated high specific surface area activated carbon is prepared by the following steps of: 1:2, after continuously stirring for 4 hours, titrating by ammonia water to slowly adjust the pH value of the solution to 6; and thirdly, pouring the mixed solution into a constant-temperature water bath cup at 70 ℃, after the volume of the solution is reduced by about 60%, transferring the collected sol into a drying oven, and drying and foaming the sol for 7 hours at 240 ℃ to obtain a brown fluffy sample. And fourthly, after fully grinding, placing the brown powder into a muffle furnace for 650 ℃ (the heating rate is 3 ℃/min) to be sintered for 2 hours, and obtaining the high-surface-area lanthanum ferrite nano material.
The fifth concrete implementation mode: a preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area comprises the following specific steps: firstly, 2.165g of lanthanum nitrate nonahydrate, 2.02g of ferric nitrate hexahydrate and 100 mL of deionized water are stirred for 0.5 h. After the nitrate is completely dissolved, adding 7 g of citric acid, and continuously stirring for 1 h; secondly, the activated high specific surface area activated carbon is prepared by the following steps of: 1:2.5, continuously stirring for 8 h, and then titrating by ammonia water to slowly adjust the pH value of the solution to 7; and thirdly, pouring the mixed solution into a constant-temperature water bath cup at 75 ℃, transferring the collected sol into a drying oven after the volume of the solution is reduced by about 50%, and drying and foaming the sol for 7 hours at 240 ℃ to obtain a brown fluffy sample. And fourthly, after fully grinding, placing the brown powder into a muffle furnace for sintering for 4 hours at 500 ℃ (the heating rate is 1 ℃/min), and obtaining the high-surface-area lanthanum ferrite nano material.
The sixth specific implementation mode: a preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area comprises the following specific steps: first, 2.165g of lanthanum nitrate nonahydrate, 2.02g of ferric nitrate hexahydrate and 100 mL of deionized water were stirred for 1 h. After the nitrate is completely dissolved, adding 5g of citric acid, and continuously stirring for 0.5 h; secondly, the activated high specific surface area activated carbon is prepared by the following steps of: 1:3, continuously stirring for 6 hours, and then titrating by ammonia water to slowly adjust the pH value of the solution to 5; and thirdly, pouring the mixed solution into a constant-temperature water bath cup at 67 ℃, after the volume of the solution is reduced by about 40%, transferring the collected sol into a drying oven, and drying and foaming the sol for 7 hours at 150 ℃ to obtain a brown fluffy sample. And fourthly, after fully grinding, placing the brown powder into a muffle furnace for 550 ℃ (the heating rate is 5 ℃/min) to be sintered for 2 hours, and obtaining the high-surface-area lanthanum ferrite nano material.
FIG. 1 is an XRD pattern of the lanthanum ferrite nano-material prepared by the first embodiment, and it can be seen from the XRD pattern that all the obtained nano-materials are crystalline phases, and the peak positions of the diffraction peaks in the obtained spectrum are completely consistent with the peak positions of the standard PDF card PDF # 37-1493.
Fig. 2 is a scanning electron microscope image of the lanthanum ferrite nanomaterial prepared in the first embodiment, and it can be known from the image that the prepared lanthanum ferrite particles are flocculent.
Fig. 3 is a graph showing the relationship between the gas-sensitive characteristic temperature and the sensitivity of the lanthanum ferrite nanomaterial prepared according to the first embodiment to 100ppm ethanol at a test time of 180s, and it can be seen from the graph that the optimal working temperature of the lanthanum ferrite nanomaterial is 240 ℃ and the sensitivity is as high as 224.87.
FIG. 4 is a graph of the response recovery time of the lanthanum ferrite nanomaterial prepared according to the first embodiment when the test time is 180s and the test temperature is 240 ℃ versus 100ppm ethanol, and it can be seen that the response recovery time of the lanthanum ferrite nanomaterial is 110s and 100s, respectively.
Claims (4)
1. A preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area is characterized in that the preparation method adopts a sol-gel-self-propagating combustion method, and a proper amount of activated carbon dispersing agent and pore-forming agent with high specific surface area are added to obtain flocculent lanthanum ferrite nano-material with high specific surface area.
2. A preparation method of a lanthanum ferrite gas-sensitive material with high specific surface area is characterized by comprising the following specific steps: firstly, stirring 2.165g of lanthanum nitrate nonahydrate, 2.02g of ferric nitrate hexahydrate and 100-200 mL of deionized water for 0.5-1 h, adding 3-9 g of citric acid after nitrate is completely dissolved, and continuing stirring for 0.5-1 h; secondly, the activated high specific surface area activated carbon is prepared by the following steps of: 1: 2-3, continuously stirring for 4-8 h, and then titrating by ammonia water to slowly adjust the pH of the solution to 5-7; pouring the mixed solution into a constant-temperature water bath cup at 67-75 ℃, after the volume of the solution is reduced by about 40-60%, transferring the collected sol into a drying oven, drying and foaming for 7 h at 150-240 ℃ to obtain a brown fluffy sample, and after fully grinding, putting brown powder into a muffle furnace for sintering for 2-6 h at 400-650 ℃ (the heating rate is 0.5-1 ℃/min) to obtain the high-surface-area lanthanum ferrite nano material.
3. The method for preparing the lanthanum ferrite gas-sensitive material with high specific surface area as claimed in claim 2, wherein the specific surface area of the activated carbon is 1800-2500 m2The lanthanum ferrite/g is activated for 2-4 h at 60-80 ℃ by 4-6M KOH before use, the high-specific-surface-area activated carbon can inhibit the growth of lanthanum ferrite particles, and a porous lanthanum ferrite material can be generated after the activated carbon is burnt at high temperature, so that the specific surface of the lanthanum ferrite gas-sensitive material can be improvedThe activated carbon is decomposed at high temperature to release heat, so that the sintering temperature of the lanthanum ferrite can be effectively reduced, and the method is energy-saving and environment-friendly.
4. The method for preparing the lanthanum ferrite gas-sensitive material as claimed in claim 1, wherein the lanthanum ferrite nano-particles prepared by the sol-gel method are porous and flocculent, the grain size is 30-35 nm, the specific surface area of the material is large, the oxygen adsorption capacity is improved, and the sensitivity of the sensor is improved.
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Cited By (3)
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CN115893501A (en) * | 2022-10-27 | 2023-04-04 | 齐鲁工业大学 | Preparation method of lanthanum ferrite and application of lanthanum ferrite in anaerobic digestion of organic wastewater under stress of carbamazepine |
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