CN111830089A - Based on two shell shape Cu2N-propanol gas sensor of O-grade structure micron sphere sensitive material and preparation method thereof - Google Patents
Based on two shell shape Cu2N-propanol gas sensor of O-grade structure micron sphere sensitive material and preparation method thereof Download PDFInfo
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- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
Based on two shell shape Cu2An n-propanol gas sensor of O graded structure micron sphere sensitive material and a preparation method thereof belong to the technical field of semiconductor oxide gas sensors. The sensor is commercially available Al with two parallel, annular and mutually separated gold electrodes on the outer surface2O3Ceramic tube, coating on annular gold electrode and Al2O3Double-shell Cu on insulating ceramic tube2O-sensitive material, and through-Al2O3Nickel-cadmium heating coil of insulating ceramic tube. The invention prepares double-shell Cu by a simple solvothermal method and using a glutamic acid weak reducing agent2The O semiconductor sensitive material realizes a great leap of gas sensitive property. The prepared sensor shows excellent selectivity and sensitivity (11-100ppm) to n-propanol, and has good long-term stability and repeatability. In addition, the device has simple process and small volume, is suitable for mass production, and has wide application range in detecting n-propanol pollutantsAnd the application prospect is good.
Description
Technical Field
The invention belongs to the technical field of semiconductor oxide gas sensors, and particularly relates to a Cu sensor based on a double-shell shape2An n-propanol gas sensor of a micron sphere sensitive material with an O hierarchical structure and a preparation method thereof.
Background
N-propanol is a colorless transparent liquid, has an odor similar to ethanol, and is one of chemical raw materials commonly used in industrial production, such as solvents, medicines, paints, cosmetics, and the like. However, n-propanol is a toxic Volatile Organic Compound (VOCs) that presents a significant health hazard to humans and can cause skin dryness and cracking over prolonged skin contact. Headache, lethargy, and irritation of the eye, nose, and throat can occur when exposed to high concentrations (-400 ppm) of n-propanol vapor, but are still used in industry as intermediates to produce other chemicals and as solvents in research laboratories. Therefore, the development of the n-propanol gas sensor with good selectivity and high sensitivity to realize the efficient detection of the n-propanol gas in the microenvironment is of great significance.
Among a variety of gas sensors, a resistance type gas sensor using a semiconductor oxide as a sensitive material has the advantages of high sensitivity, high stability, good selectivity, fast response and recovery speed, simple manufacturing method, low cost and the like, and is one of the most widely used gas sensors at present. With the development of nano science and technology, the gas-sensitive material is regulated into a hierarchical structure with a novel morphology, so that the specific surface area of the material can be greatly increased, active sites can be increased, the gas-sensitive property can be improved, and the better gas-sensitive property can be obtained.
Cuprous oxide (Cu)2O) is an important P-type metal oxide semiconductor, which is widely used in the fields of solar energy, photocatalysis, gas sensors, etc. due to its stable chemical and electrical properties. For Cu2Studies of the sensing properties of O-material structures have shown that cuprous oxide has excellent catalytic activity for the oxidation of Volatile Organic Compounds (VOCs), which makes Cu accessible, although its sensitivity is relatively low compared to certain N-type metal oxide semiconductors2Modification of O-sensitive materials becomes significant. The invention synthesizes double-shell Cu by using a solvothermal method2The O-grade structure microspheres are used for improving the gas-sensitive property, and the grade structure can improve the gas-sensitive property of the gas sensor.
Disclosure of Invention
The invention aims to provide Cu based on double shell2A gas sensor of a micron sphere sensitive material with an O-grade structure and a preparation method thereof. The invention relates to double-shell Cu prepared by a solvothermal one-step synthesis method2The micron ball with O-grade structure is used as a sensitive material, on one hand, Cu2The O microsphere has stronger oxidability, has better catalytic oxidation activity on various VOC gases, and can cause more oxygen molecules to participate in the reaction; moreover, the double-shell structure in the form of concentric circles greatly improves the Cu content2The specific surface area of the grading structure of the O microspheres enhances the oxygen adsorption capacity, so that the Cu2The carrier hole concentration in the O material increases, resulting in an increase in the chemisorbed oxygen component, resulting in a more pronounced change in the resistance of the sensitive material. The combined action of the two aspects greatly improves the reaction efficiency of the gas and the sensitive material, and further improves the sensitivity of the sensor. 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 Cu based on double shell2The gas sensor of the O-grade structure microsphere sensitive material consists of a ceramic tube substrate, sensitive materials and a nickel-cadmium heating coil, wherein the ceramic tube substrate is provided with two parallel annular gold electrodes which are separated from each other on the outer surface; the method is characterized in that: the sensitive material is double-shell Cu2The micron ball with the O-grade structure is prepared by the following steps:
(1) weighing 20-30 mL of absolute ethyl alcohol, and adding 0.2-0.3 g of Cu (NO)3)2·3H2Adding O into absolute ethyl alcohol, continuously stirring until the O is completely dissolved, and adding 0.1-0.2 g of glutamic acid (C)5H9NO4) Stirring for 20-40 minutes;
(2) transferring the solution obtained in the step (1) into a hydrothermal kettle, keeping the solution at 160-200 ℃ for 10-15 hours, taking out the solution, naturally cooling the solution to room temperature, centrifugally cleaning the generated precipitate for multiple times by using deionized water and absolute ethyl alcohol, and drying the precipitate for 10-15 hours at 70-90 ℃ to obtain the double-shell Cu2O-grade structured microsphere powder.
The invention relates to Cu based on double shell2The preparation method of the n-propanol gas sensor of the O-grade structure micron ball sensitive material is a indirectly heated structure, and comprises the following steps:
(1) taking double-shell Cu2Mixing the O-grade structure micro-sphere powder with deionized water to form pasty slurry, dipping a small amount of the slurry by a brush, and uniformly coating the slurry on Al with two parallel, annular and mutually separated gold electrodes on the outer surface2O3Forming a sensitive material film with the thickness of 15-25 mu m on the surface of the ceramic tube, and completely covering the Al with the sensitive material2O3The outer surface of the ceramic tube and the annular gold electrode; al (Al)2O3The inner diameter and the outer diameter of the ceramic tube are respectively 0.6-0.8 mm and 1.0-1.5 mm, and the length is 4-5 mm; the width of the single annular gold electrode is 0.4-0.5 mm, and the distance between the two gold electrodes is 0.5-0.6 mm; a platinum wire lead is led out of the gold electrode, and the length of the platinum wire lead is 4-6 mm;
(2) baking the device obtained in the step (1) under an infrared lamp for 10-15min to be sensitizedDrying the sensitive material, and adding Al2O3Calcining the ceramic tube at 90-100 ℃ for 1.5-3 hours; then, penetrating a nickel-cadmium heating coil with a resistance value of 30-40 omega through Al2O3The interior of the ceramic tube is used as a heating wire, and finally the device is welded and packaged according to an indirectly heated gas sensitive element, so that the Cu based on the double-shell shape is obtained2An n-propanol gas sensor of a micron sphere sensitive material with an O graded structure.
Cu prepared by the invention based on double shell2The n-propanol gas sensor of the O-graded structure micron ball sensitive material has the following advantages:
1. successfully preparing double-shell Cu by using one-step simple solvothermal method2The O-grade structure microsphere has simple synthesis method and low cost;
2. preparation of double-shell Cu by using glutamic acid as reducing agent2The O-grade structure microsphere improves the selectivity and sensitivity (11-100ppm) of the microsphere to n-propanol gas, has good repeatability and stability, and has a wide application prospect in the aspect of detecting n-propanol pollution in a microenvironment;
3. the tube sensor is commercially available, and the device has simple process and small volume and is suitable for mass production.
Drawings
FIG. 1a, FIG. 1b, and FIG. 1c are each a double-shell Cu2O-micron sphere and hollow sphere Cu2O and solid sphere Cu2An SEM topography of O;
FIG. 2a1FIG. 2a2FIG. 2a3Are respectively double-shell shaped Cu2SEM, TEM, HRTEM images of O microspheres;
FIG. 2b1FIG. 2b2FIG. 2b3Are respectively hollow ball Cu2SEM, TEM, HRTEM image of O; FIG. 2c1、
FIG. 2c2FIG. 2c3Are respectively solid sphere Cu2SEM, TEM, HRTEM image of O;
FIG. 3: double-shell Cu2O-micron sphere and hollow sphere Cu2O and solid sphere Cu2XRD pattern of O;
FIG. 4 a: sensitivity curves of the sensors in comparative examples and examples for 100ppm n-propanol gas at different operating temperatures; FIG. 4 b: the selectivity curves of the sensors in the comparative examples and examples at 187 ℃ for 8 gases to be measured at 100 ppm;
FIG. 5: sensitivity vs. n-propanol concentration characteristic curves for the sensors in the comparative examples and examples at the optimum operating temperature (225 ℃);
FIGS. 6a, 6b, and 6c are response recovery curves of the sensors at the optimum operating temperature (187 ℃) for the n-propanol concentration gradient in the examples and comparative examples, respectively;
FIG. 7: the recovery curve of the response of the sensor at the optimum operating temperature (187 ℃) for 100ppm of n-propanol gas in the examples;
FIG. 8: long-term stability curves of the resistance in air and the corresponding sensitivity in 100ppm n-propanol gas for the sensor operating at the optimum operating temperature in the examples;
as shown in FIG. 1, double-shelled Cu2O-micron sphere and hollow sphere Cu2O and solid sphere Cu2The topography at low power of O, from FIG. 1a, can be seen the double shell Cu2The O-micron sphere is composed of a plurality of nano-particles, and Cu is in a double shell shape2The diameter of O is about 5 to 5.2 μm. Hollow sphere Cu of FIG. 1b2O has a diameter of about 1 μm, solid sphere Cu of FIG. 1c2O has a diameter of about 0.9 to 1um
As shown in fig. 2, double-shelled Cu2The morphology shown in the O-microsphere TEM image and the SEM image is uniform, the O-microsphere TEM image is a hierarchical structure formed by self-assembly of a plurality of nano particles, and the high-resolution TEM image shows a lattice spacing of 0.24 width and Cu2The (111) crystal face of O is inosculated, and the hollow sphere Cu is2O and solid sphere Cu2The appearance of the O is uniform with that of the SEM image, and the high-resolution TEM image shows that the lattice spacing is 0.21nm wide and pure Cu2The (200) crystal face of O coincides.
As shown in FIG. 3, double-shelled Cu2O-micron sphere and hollow sphere Cu2O and solid sphere Cu2XRD spectrum of O, no impurity peak of other phase and Cu2The O standard cards are matched.
As shown in fig. 4, the optimum operating temperature of the sensors in the comparative example and the example was 187 ℃, and the sensitivity of the device to 100ppm of n-propanol gas was 11, 6 and 5, respectively, and the selectivity to n-propanol gas was the best, and the gas sensing performance of the sensor in the example was improved more and the selectivity to n-propanol gas was the best, compared with the sensor in the comparative example.
As shown in fig. 5, the sensor in the example showed a significant increase in sensitivity with increasing n-propanol gas concentration, and showed a better linear increase in sensitivity and concentration relative to the sensor in the comparative example.
As shown in fig. 6, for the example sensor exposed to n-propanol, the resistance of the semiconductor became large, which is consistent with the gas sensing characteristics of the P-type oxide semiconductor, and the sensor exhibited excellent response and recovery characteristics to different concentrations of n-propanol. When the working temperature of the device of the embodiment is 187 ℃, the sensitivity of the device is increased along with the increase of the concentration of the n-propanol, the sensitivity of the sensor of the embodiment to 10, 20, 40, 60, 80 and 100ppm of the n-propanol is respectively 3.3, 5.2, 7.0, 7.5, 9.1 and 11, while the sensitivity of the device of the comparative example 2 to 10 to 100ppm of the n-propanol is only 1.5 to 5.2.
As shown in fig. 7, the sensor in the example has no significant fluctuation in the response recovery curve for 100ppm of n-propanol gas at the operating temperature of 187 ℃, response recovery times of 50s and 40s, respectively, and high sensitivity.
As shown in fig. 8, the initial resistance in air and its corresponding sensitivity curve in 100ppm xylene gas for the sensor in the example operating at a temperature of 187 ℃ fluctuated less over one month of the continuous test, indicating its good long term stability.
Note: the sensitivity of the device (P-type semiconductor) is defined in the test reducing atmosphere as the ratio of the resistance in the tested atmosphere to the resistance in air, i.e. S-Rg/Ra. During the test, a static test system is used for testing. Placing the device in a 50-80L gas box, injecting a certain amount of organic gas to be detected inwards, observing and recording the resistance change of the organic gas, and calculating to obtain corresponding sensitivityAnd (4) degree value.
Detailed Description
Comparative example 1:
with hollow spheres Cu2The specific manufacturing process of the n-propanol sensor with O as a sensitive material comprises the following steps:
(1) firstly, measuring 25mL of absolute ethyl alcohol, pouring the absolute ethyl alcohol into a beaker, and continuously stirring;
(2) 0.25g of Cu (NO)3)2·3H2Adding O into a beaker filled with absolute ethyl alcohol, continuously stirring until the O is completely dissolved, adding 0.15g of glycine into the beaker, and stirring for 30 minutes;
(3) transferring the solution into a 50mL hydrothermal kettle, keeping the temperature at 180 ℃ for 10 hours, taking out the solution, naturally cooling the solution to room temperature, centrifugally cleaning the generated precipitate for multiple times by using deionized water and ethanol, and drying the precipitate in a drying oven at 80 ℃ for 12 hours to obtain hollow sphere Cu2And (4) O powder.
(4) Taking a proper amount of hollow sphere Cu prepared by a solvothermal method2Mixing O powder with deionized water, grinding to form paste slurry, dipping a small amount of slurry, and uniformly coating Al with 2 annular gold electrodes on the outer surface2O3Forming a sensitive material film with the thickness of 15-25 um on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
(5) baking under infrared lamp for 10-15min, drying the sensitive material, and adding Al2O3Calcining the ceramic tube at 90-100 ℃ for 2 hours; then, penetrating a nickel-cadmium heating coil with a resistance value of 30-40 omega through Al2O3The inside of the ceramic tube is used as a heating wire, and finally the device is welded and packaged according to a general indirectly heated gas sensitive element, so that the hollow ball Cu is obtained2An n-propanol gas sensor of O sensitive material.
Comparative example 2:
with solid spheres Cu2The specific manufacturing process of the n-propanol sensor with O as a sensitive material comprises the following steps:
(1) firstly, measuring 25mL of absolute ethyl alcohol, pouring the absolute ethyl alcohol into a beaker, and continuously stirring;
(2) 0.25g of Cu (NO)3)2·3H2Adding O into a beaker filled with absolute ethyl alcohol, continuously stirring until the O is completely dissolved, adding 0.15g of phenylalanine into the beaker, and stirring for 30 minutes;
(3) transferring the solution into a 50mL hydrothermal kettle, keeping the temperature at 180 ℃ for 10 hours, taking out the solution, naturally cooling the solution to room temperature, centrifugally cleaning the generated precipitate for multiple times by using deionized water and ethanol, and drying the precipitate in a drying oven at 80 ℃ for 12 hours to obtain the solid Cu balls2And (4) O powder.
(4) Taking a proper amount of solid sphere Cu prepared by a solvothermal method2Mixing O powder with deionized water, grinding to form paste slurry, dipping a small amount of slurry, and uniformly coating Al with 2 annular gold electrodes on the outer surface2O3Forming a sensitive material film with the thickness of 15-25 um on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
(5) baking under infrared lamp for 10-15min, drying the sensitive material, and adding Al2O3Calcining the ceramic tube at 90-100 ℃ for 2 hours; then, penetrating a nickel-cadmium heating coil with a resistance value of 30-40 omega through Al2O3The inside of the ceramic tube is used as a heating wire, and finally the device is welded and packaged according to a general indirectly heated gas sensitive element, so that a solid ball Cu is obtained2An n-propanol gas sensor of O sensitive material.
Example 1:
with double-shelled Cu2The n-propanol gas sensor of the O-graded structure micron ball sensitive material comprises the following specific manufacturing processes:
(1) firstly, measuring 25mL of absolute ethyl alcohol, pouring the absolute ethyl alcohol into a beaker, and continuously stirring;
(2) 0.25g of Cu (NO)3)2·3H2Adding O into a beaker filled with absolute ethyl alcohol, continuously stirring until the O is completely dissolved, adding 0.15g of glutamic acid into the beaker, and stirring for 30 minutes;
(3) transferring the solution into a 50mL hydrothermal kettle, keeping the temperature at 180 ℃ for 10 hours, taking out the hydrothermal kettle, naturally cooling to room temperature to obtain the productThe precipitate was centrifugally washed with deionized water and ethanol several times, and then dried in a drying oven at 80 ℃ for 12 hours, thereby obtaining double-shelled Cu2And (4) O powder.
(4) Taking a proper amount of double-shell Cu prepared by a solvothermal method2Mixing O powder with deionized water, grinding to form paste slurry, dipping a small amount of slurry, and uniformly coating Al with 2 annular gold electrodes on the outer surface2O3Forming a sensitive material film with the thickness of 15-25 um on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
(5) baking under infrared lamp for 10-15min, drying the sensitive material, and adding Al2O3Calcining the ceramic tube at 90-100 ℃ for 2 hours; then, penetrating a nickel-cadmium heating coil with a resistance value of 30-40 omega through Al2O3The interior of the ceramic tube is used as a heating wire, and finally the device is welded and packaged according to a general indirectly heated gas sensitive element, so that double-shell Cu is obtained2An n-propanol gas sensor of a micron sphere sensitive material with an O graded structure.
Claims (3)
1. Based on two shell shape Cu2The n-propanol gas sensor of the O-graded structure micron ball sensitive material consists of a ceramic tube substrate, sensitive materials and a nickel-cadmium heating coil, wherein the ceramic tube substrate is provided with two parallel annular gold electrodes which are separated from each other on the outer surface; the method is characterized in that: the sensitive material is double-shell Cu2O-grade structure microspheres, and is prepared by the following steps,
(1) weighing 20-30 mL of absolute ethyl alcohol, and adding 0.2-0.3 g of Cu (NO)3)2·3H2Adding O into absolute ethyl alcohol, continuously stirring until the O is completely dissolved, and adding 0.1-0.2 g of glutamic acid (C)5H9NO4) Stirring for 20-40 minutes;
(2) transferring the solution obtained in the step (1) into a hydrothermal kettle, keeping the solution at 160-200 ℃ for 10-15 hours, taking out the solution, naturally cooling the solution to room temperature, centrifugally cleaning the generated precipitate for multiple times by using deionized water and absolute ethyl alcohol, and then centrifuging the precipitate for 70-9 timesDrying for 10-15 hours at 0 ℃ to obtain the double-shell Cu2O-grade structured microsphere powder.
2. The Cu of claim 1 based on a double shell2The preparation method of the n-propanol gas sensor of the O-grade structure micron ball sensitive material comprises the following steps:
(1) taking double-shell Cu2Mixing the O-grade structure micro-sphere powder with deionized water to form pasty slurry, dipping a small amount of the slurry by a brush, and uniformly coating the slurry on Al with two parallel, annular and mutually separated gold electrodes on the outer surface2O3Forming a sensitive material film with the thickness of 15-25 mu m on the surface of the ceramic tube, and completely covering the Al with the sensitive material2O3The outer surface of the ceramic tube and the annular gold electrode;
(2) baking the device obtained in the step (1) for 10-15min under an infrared lamp, and drying the sensitive material, and then, adding Al2O3Calcining the ceramic tube at 90-100 ℃ for 1.5-3 hours; then, penetrating a nickel-cadmium heating coil with a resistance value of 30-40 omega through Al2O3The interior of the ceramic tube is used as a heating wire, and finally the device is welded and packaged according to an indirectly heated gas sensitive element, so that the Cu based on the double-shell shape is obtained2An n-propanol gas sensor of a micron sphere sensitive material with an O graded structure.
3. The Cu based on double shell as claimed in claim 22The preparation method of the n-propanol gas sensor of the O-grade structure micron ball sensitive material is characterized by comprising the following steps of: al (Al)2O3The inner diameter and the outer diameter of the ceramic tube are respectively 0.6-0.8 mm and 1.0-1.5 mm, and the length is 4-5 mm; the width of the single annular gold electrode is 0.4-0.5 mm, and the distance between the two gold electrodes is 0.5-0.6 mm; and a platinum wire lead is led out of the gold electrode, and the length of the platinum wire lead is 4-6 mm.
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Cited By (4)
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| CN113533453A (en) * | 2021-07-19 | 2021-10-22 | 吉林大学 | Based on CdSnO3Acetone gas sensor and preparation method thereof |
| CN113916946A (en) * | 2021-10-09 | 2022-01-11 | 吉林大学 | N-amyl alcohol gas sensor based on ZnO nano sensitive material and preparation method thereof |
| CN114264703A (en) * | 2021-12-27 | 2022-04-01 | 吉林大学 | Cubic/hexagonal phase CdS composite nanomaterial-based n-propanol sensor and preparation method thereof |
| CN115583668A (en) * | 2022-11-09 | 2023-01-10 | 吉林大学 | Heterogeneous three-layer hollow structure gas sensitive material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113533453A (en) * | 2021-07-19 | 2021-10-22 | 吉林大学 | Based on CdSnO3Acetone gas sensor and preparation method thereof |
| CN113916946A (en) * | 2021-10-09 | 2022-01-11 | 吉林大学 | N-amyl alcohol gas sensor based on ZnO nano sensitive material and preparation method thereof |
| CN114264703A (en) * | 2021-12-27 | 2022-04-01 | 吉林大学 | Cubic/hexagonal phase CdS composite nanomaterial-based n-propanol sensor and preparation method thereof |
| CN114264703B (en) * | 2021-12-27 | 2023-08-18 | 吉林大学 | N-propanol sensor based on cubic/hexagonal phase CdS composite nano material and preparation method thereof |
| CN115583668A (en) * | 2022-11-09 | 2023-01-10 | 吉林大学 | Heterogeneous three-layer hollow structure gas sensitive material and preparation method thereof |
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