CN109709184B - In-based2O3NO of carbon dot complexes2Sensor and preparation method thereof - Google Patents
In-based2O3NO of carbon dot complexes2Sensor and preparation method thereof Download PDFInfo
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- CN109709184B CN109709184B CN201910070147.0A CN201910070147A CN109709184B CN 109709184 B CN109709184 B CN 109709184B CN 201910070147 A CN201910070147 A CN 201910070147A CN 109709184 B CN109709184 B CN 109709184B
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Abstract
In-based2O3Room temperature NO of-carbon dot composite2A sensor and a preparation method thereof belong to the technical field of semiconductor metal oxide gas sensors. Al with 2 discrete annular gold electrodes from the outer surface2O3Ceramic tube, uniformly coated on annular gold electrode and Al2O3In of the outer surface of the ceramic tube2O3-a thin film of carbon dot composite sensitive material. The invention utilizes the gas adsorption capacity and shielding effect of carbon dots and In2O3Thereby increasing the surface chemical reaction of the detected gas and forming In2O3And carbon dots, thereby effectively improving NO resistance of the sensor2The sensitivity of the sensor is improved by 5 times; meanwhile, the device has the excellent effects of simple process, small volume and suitability for mass production.
Description
Technical Field
The invention belongs to the technical field of semiconductor metal oxide gas sensors, and particularly relates to an In-based sensor2O3NO of carbon dot (carbon dots) complexes2A sensor and a method for manufacturing the same.
Background
In general, the composition of trace amounts of gases in the atmosphere is negligible. However, in a certain range of atmosphere, there is a possibility that a trace amount of substances which are not originally present may adversely affect or harm human beings, animals, plants, articles, materials, and the like. When the concentration of pollutants in the atmosphere reaches a harmful level, even the ecological system and the conditions for normal survival and development of human beings can be destroyed, and the phenomenon of causing harm to people or objects is called atmospheric pollution. The air pollution is caused by natural factors and artificial factors, and the natural factors comprise smoke, oxysulfide, nitric oxide and the like generated by volcanic eruption, earthquake, forest fire and the like. With the rapid development of human economic activities and production, human factors become more and more dominant, and human beings exhaust a large amount of waste gas, smoke dust and other substances into the atmosphere while consuming energy, thus seriously affecting the quality of the atmospheric environment.
Nitrogen dioxide (NO)2) Is a reddish-brown highly active gaseous substance, also known as nitrogen peroxide. Besides natural sources, nitrogen dioxide mainly comes from combustion of fuel and urban automobile exhaust. In addition, industrial processes may also produce certain amounts of nitrogen dioxide. NO2The damage to health is mainly caused by respiratory tract injury and NO inhalation2The initial stage of the gas has mild eye and upper respiratory tract irritation symptoms, such as pharyngeal discomfort, dry cough, etc. After incubation for several hours or more, delayed pulmonary edema, adult respiratory distress syndrome, chest distress, cough, cyanosis, and other symptoms may develop, with pneumothorax and mediastinal emphysema. Nitrogen dioxide is also one of the causes of acid rain, and the environmental hazards caused by nitrogen dioxide mainly include: influence on competition and composition change between wetland and terrestrial plant species, reduction of atmospheric visibility, acidification of surface water and eutrophication.
Among a wide variety of gas sensors, a resistive gas sensor using a semiconductor metal oxide as a sensitive material has the advantages of high sensitivity, high response and recovery speed, low cost, and the like, and is one of the most widely used gas sensors at present. However, the development of the semiconductor device is severely restricted by the defects of general selectivity, large power consumption, poor interference resistance and the like, so that doping and modification based on the semiconductor metal oxide become a necessary means for solving the problems.
N-type semiconductor In with wider band gap In various gas sensing materials2O3It has been widely studied because of its high conductivity. In2O3For NO2Gas detection has good sensitivity. However, pure In2O3Due to its inherent physical or chemical properties, certain drawbacks such as limited sensitivity, poor selectivity, etc., remain, which undoubtedly hinders further development thereof.
Compared with other nano carbon materials (CNTs, GO and rGO), the carbon dots (carbon dots) have some unique performances and simple and environment-friendly synthesis processes as a novel promising fluorescent probe. The carbon dots are zero in size and typically less than 10nm in diameter. It consists of graphite core or amorphous carbon with great amount of edge/functional groups on its surface, high activity and NO benefiting effect2Adsorption of (3). In addition, since the carbon dots can act as carrier reservoirs in heterojunctions, electron transport can also be modulated
Disclosure of Invention
The object of the present invention is to provide an In-based solution2O3Room temperature NO of-carbon dot composite2A sensor and a method for manufacturing the same.
The present invention utilizes In2O3Carbon dot composites as sensitive materials. On one hand, the carbon dots have high specific surface area and gas adsorption capacity, so that the adsorption quantity of the detected gas is greatly increased, and the sensitivity of the gas is improved; on the other hand, the introduction of carbon dots causes a shielding effect, so that chemisorption of oxygen increases. In addition, carbon dots can be bonded with In2O3A heterojunction is formed between the two electrodes, thereby facilitating the transfer of charges and effectively improving the NO resistance of the sensor2The sensitivity characteristics of (a). In addition, the carbon sites themselves have many defects, such as heteroatoms, functional groups, etc., and the presence of these defects provides more reactive sites, adsorbing more oxygen ions and target gas molecules at the sites. The combined action of the aspects greatly improves the reaction efficiency of the gas and the sensitive material, and further improves the sensitive characteristic of the sensor. Meanwhile, the sensor with the tubular structure is simple in manufacturing process, small in size and beneficial to industrial mass production, and therefore has important application value.
The invention relates to an In-based2O3Room temperature NO of-carbon dot composite2Sensor consisting of Al with 2 discrete annular gold electrodes on its outer surface2O3Ceramic tube, uniformly coated on annular gold electrode and Al2O3Sensitive material film on outer surface of ceramic tube, Al2O3The nickel-cadmium alloy coil In the ceramic tube is characterized In that the sensitive material is In2O3-a carbon dot composite, prepared by the steps of:
firstly, dissolving 0.5-0.7 g of urea into 15-30 ml of deionized water to obtain a solution A; adding 0.2-0.4 g of indium chloride tetrahydrate and 0.3-0.5 g of citric acid into 15-30 ml of deionized water, and forming a solution B for uniform decomposition under continuous stirring; slowly adding the solution B into the solution A, and magnetically stirring for 20-40 minutes to obtain a uniform mixed solution;
secondly, transferring the obtained mixed solution into a polytetrafluoroethylene reaction kettle, and reacting for 10-15 hours at 110-130 ℃; after the reaction kettle is naturally cooled to room temperature, centrifuging the solution, and cleaning the precipitate with deionized water and ethanol; drying at 50-70 ℃, sintering the obtained precipitate for 1.5-3.0 hours at 300-400 ℃ under nitrogen, and heating at a rate of 1.5-3.0 ℃/min to obtain In2O3-carbon dot composite sensitive material powder.
The invention relates to an In-based2O3Room temperature NO of-carbon dot composite2The preparation method of the sensor comprises the following steps:
in2O3The mass ratio of the carbon dot composite sensitive material powder to deionized water is 4-6: 1 mixing and grinding to form paste slurry, then dipping a small amount of the slurry by a brush to uniformly coat the Al with 2 discrete and annular gold electrodes on the outer surface of a market2O3Surface of ceramic tube, Al2O3The length of the ceramic tube is 4-4.5 mm, the outer diameter is 1.2-1.5 mm, the inner diameter is 0.8-1.0 mm, the width of the gold electrode is 0.5-1.0 mm, a sensitive material film with the thickness of 10-30 mu m is formed, and the sensitive material completely covers the annular gold electrode;
② Al obtained in the step I2O3Baking the ceramic tube under an infrared lamp for 30-45 minutes, and drying the sensitive material, and then, adding Al2O3Calcining the ceramic tube at 150-200 ℃ for 2-3 hours; then, enabling the nickel-cadmium alloy coil with the resistance value of 30-40 omega to penetrate through Al2O3Inside the ceramic tube as heatingFinally, welding and packaging the filament according to an indirectly heated gas sensitive element to obtain the In-based gas sensitive element2O3Room temperature NO of-carbon dot composite2A sensor.
In-based prepared by the invention2O3Room temperature NO of-carbon dot composite2The sensor has the following advantages:
1. in production by hydrothermal method2O3The carbon dot composite sensitive material has simple synthesis method and low cost;
2. gas adsorption capacity and shielding effect using carbon dots and In2O3Thereby increasing the surface chemical reaction of the detected gas and forming In2O3And carbon dots, thereby effectively improving NO resistance of the sensor2The sensitivity of the sensor is improved by 5 times;
3. the tube sensor is commercially available, and the device has simple process and small volume and is suitable for mass production.
Drawings
FIG. 1: in2O3And In2O3-XRD pattern of carbon dot composite;
FIG. 2: a. b is pure In2O3The SEM topography of (1), c and d are pure In2O3A TEM topography of;
FIG. 3: a is a TEM photograph of carbon dots, and b, c and d are In2O3-TEM topography of carbon dot composites;
FIG. 4: comparative example and example the sensor is sensitive to 500ppb of NO at different operating temperatures2A sensitivity contrast map of (a);
FIG. 5: comparative example and example the sensor has a device sensitivity-NO at a working temperature of 50 DEG C2Concentration profile.
FIG. 6: long term stability curve of the sensor in the examples.
As shown In FIG. 1, In the XRD spectrum, curve a is In the spectrum library2O3Curve b is comparative example In2O3XRD peak of (1)By comparison, we can find that the peak positions of the two are completely consistent, proving that In2O3Successful synthesis of the compound; curve c is In2O3XRD peaks of the-carbon dot complexes, no significant change occurred in either the position or intensity of the peaks in curve c compared to curve b, demonstrating Co3O4Good crystallinity is maintained in the composite; in addition, there is a weak broad peak between 23 ° and 26 ° of the curve c, which is the 002 characteristic peak of the carbon-based material, and the low peak intensity is due to the small content;
as shown In FIG. 2, it can be seen from the graphs a and b that pure In2O3The gas sample is in a graded spherical shape and consists of a plurality of small balls with smaller sizes, and the diameter of a large ball is about 100nm, so that the adsorption, diffusion and desorption processes of the gas to be detected are facilitated; from the c diagram, we can clearly observe the existence of sparse holes; the high resolution photograph of the d plot shows a lattice match to that of indium oxide.
As shown in FIG. 3, a is a TEM photograph of carbon dots, in which the size distribution of the carbon dots is seen to be around 5nm, and the lattice spacing in the inset is matched with that of the carbon material; b and c are In2O3SEM photograph of-carbon dot composite, In can be found2O3The-carbon dot complex well retains In2O3The morphology of (a); d is In2O3High resolution photograph of-carbon dot composite, In can be seen2O3And the lattice spacing of the carbon dots.
As shown in FIG. 4, the optimum operating temperatures of the comparative example and the example were 50 ℃ and the sensitivity of the gas sensor was defined as the resistance R in airaAnd in NO2Resistance value in gas RgWhen the comparative example and the example are at respective optimum operating temperatures for 500ppb NO2Sensitivity of 30 and 130, respectively;
as shown in FIG. 5, for the example, the sensitivity with NO was measured when the device was operated at 50 deg.C2Increasing the concentration, we can also find that the examples are capable of detecting 50ppb of NO2Gas, which represents its very low detection limit.
As shown in fig. 6, the embodiment has good long-term stability.
Detailed Description
Comparative example 1:
in pure form2O3Production of NO as sensitive material2The sensor comprises the following specific manufacturing processes:
dissolving 0.6g of urea into 20 ml of deionized water to obtain a solution A; 0.3g of indium chloride tetrahydrate and 0.4g of citric acid were added to 20 ml of deionized water with continuous stirring to form a homogeneous solution B. The solution B was slowly added to the solution A, and the mixture was magnetically stirred to form a mixed solution. After stirring for 30 minutes, a mixed solution was synthesized.
② the mixed solution is transferred into a 50 ml polytetrafluoroethylene reaction kettle, and the temperature is maintained at 120 ℃ for reaction for 12 hours. After the reaction kettle is naturally cooled to room temperature, the solution is centrifuged, and the precipitate is washed for 3 times by deionized water and ethanol. Drying In a 60 ℃ oven, putting the white precipitate on a ceramic boat, sintering for 2 hours In an air sintering furnace heated to 350 ℃, and obtaining In after the temperature rise rate is 2 ℃/min2O3。
③ In2O3The mass ratio of the powder to the deionized water is 5: 1 mixing, grinding to form paste slurry, dipping a small amount of the slurry by a brush, and uniformly coating Al with 2 annular gold electrodes on the outer surface of a market2O3Surface of ceramic tube, Al2O3The length of the ceramic tube is 4.2mm, the outer diameter is 1.4mm, the inner diameter is 0.9mm, the width of the gold electrode is 0.6mm, a sensitive material film with the thickness of 20 mu m is formed, and the sensitive material completely covers the annular gold electrode;
fourthly, Al obtained in the step one2O3Baking the ceramic tube under an infrared lamp for 40 minutes, and drying the sensitive material, and then adding Al2O3The ceramic tube is calcined for 2.5 hours at 180 ℃; then, a nickel-cadmium alloy coil with the resistance value of 35 omega is penetrated through Al2O3The interior of the ceramic tube is used as a heating wire, and finally, the obtained device is welded and packaged according to a general indirectly heated gas sensitive element to obtain the gas sensitive elementTo In based on2O3NO of2A sensor.
Example 1:
in is formed by2O3Preparation of room temperature NO by using carbon dot composite as sensitive material2The sensor comprises the following specific manufacturing processes:
dissolving 0.6g of urea into 20 ml of deionized water to obtain a solution A; adding 0.3g of indium chloride tetrahydrate and 0.4g of citric acid into 20 ml of deionized water, and forming a solution B which is uniform in decomposition under continuous stirring; the solution B was slowly added to the solution A, and the mixture was magnetically stirred to form a mixed solution. After stirring for 30 minutes, a mixed solution was synthesized.
② the mixed solution is transferred into a 50 ml polytetrafluoroethylene reaction kettle, and the temperature is maintained at 120 ℃ for reaction for 12 hours. After the reaction kettle is naturally cooled to room temperature, the solution is centrifuged, and the precipitate is washed for 3 times by deionized water and ethanol. Drying In a 60 ℃ oven, putting the white precipitate on a ceramic boat, sintering for 2 hours In a nitrogen sintering furnace heated to 350 ℃, and heating at the rate of 2 ℃/min In the furnace to obtain In2O3-carbon dot composite powder.
③ In2O3-carbon dot composite powder and deionized water in a mass ratio of 5: 1 mixing, grinding to form paste slurry, dipping a small amount of the slurry by a brush, and uniformly coating Al with 2 annular gold electrodes on the outer surface of a market2O3Surface of ceramic tube, Al2O3The length of the ceramic tube is 4.2mm, the outer diameter is 1.4mm, the inner diameter is 0.9mm, the width of the gold electrode is 0.6mm, a sensitive material film with the thickness of 20 mu m is formed, and the sensitive material completely covers the annular gold electrode;
fourthly, Al obtained in the step one2O3Baking the ceramic tube under an infrared lamp for 40 minutes, and drying the sensitive material, and then adding Al2O3The ceramic tube is calcined for 2.5 hours at 180 ℃; then, a nickel-cadmium alloy coil with the resistance value of 35 omega is penetrated through Al2O3The interior of the ceramic tube is used as a heating wire, and finally, the obtained device is welded and packaged according to a general indirectly heated gas sensitive element to obtain the In-based gas sensitive element2O3NO of carbon dot complexes2A sensor.
Claims (3)
1. In-based2O3NO of carbon dot complexes2Sensor consisting of an outer surface of Al with 2 mutually discrete and annular gold electrodes2O3Ceramic tube, uniformly coated on annular gold electrode and Al2O3Sensitive material film on outer surface of ceramic tube, Al2O3The nickel-cadmium alloy coil in the ceramic tube is characterized in that: the sensitive material is In2O3A carbon dot complex, which is prepared by the steps of,
firstly, dissolving 0.5-0.7 g of urea into 15-30 ml of deionized water to obtain a solution A; adding 0.2-0.4 g of indium chloride tetrahydrate and 0.3-0.5 g of citric acid into 15-30 ml of deionized water, and forming a solution B for uniform decomposition under continuous stirring; slowly adding the solution B into the solution A, and magnetically stirring for 20-40 minutes to obtain a uniform mixed solution;
secondly, transferring the mixed solution obtained in the first step into a polytetrafluoroethylene reaction kettle, and reacting for 10-15 hours at 110-130 ℃; after the reaction kettle is naturally cooled to room temperature, centrifuging the solution, and cleaning the precipitate with deionized water and ethanol; drying at 50-70 ℃, sintering the obtained precipitate for 1.5-3.0 hours at 300-400 ℃ under nitrogen, and heating at a rate of 1.5-3.0 ℃/min to obtain In2O3-carbon dot composite sensitive material powder.
2. An In-based composition as claimed In claim 12O3NO of carbon dot complexes2The preparation method of the sensor comprises the following steps:
(1) in is mixed with2O3The mass ratio of the carbon dot composite sensitive material powder to deionized water is 4-6: 1 mixing and grinding to form paste slurry, then dipping a small amount of the slurry by a brush to uniformly coat the Al with 2 discrete and annular gold electrodes on the outer surface of a market2O3Forming a sensitive material film with the thickness of 10-30 mu m on the surface of the ceramic tube and enabling the sensitive material film to be sensitiveThe material completely covers the annular gold electrode;
(2) al obtained in the step (1)2O3Baking the ceramic tube under an infrared lamp for 30-45 minutes, and drying the sensitive material, and then, adding Al2O3Calcining the ceramic tube at 150-200 ℃ for 2-3 hours; then, enabling the nickel-cadmium alloy coil with the resistance value of 30-40 omega to penetrate through Al2O3The ceramic tube is internally used as a heating wire and is finally welded and packaged according to an indirectly heated gas sensitive element, thereby obtaining the In-based gas sensitive element2O3Room temperature NO of-carbon dot composite2A sensor.
3. An In-based composition as claimed In claim 22O3NO of carbon dot complexes2The preparation method of the sensor is characterized by comprising the following steps: al (Al)2O3The ceramic tube has a length of 4-4.5 mm, an outer diameter of 1.2-1.5 mm, an inner diameter of 0.8-1.0 mm, and a width of 0.5-1.0 mm.
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