CN111252816A - Nb-NiO nano material and preparation method and application thereof - Google Patents
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Abstract
The invention relates to the technical field of gas sensor sensitive materials, and particularly discloses an Nb-NiO nano material and a preparation method and application thereof. The Nb-NiO nano material is a two-dimensional nano flaky crystal with the maximum diagonal length of 480-550nm obtained by doping Nb in a NiO lattice. The preparation method of the Nb-NiO nano material comprises the steps of adding soluble nickel salt and niobium salt into a mixed solution consisting of ethylene glycol and deionized water, adding urea, carrying out hydrothermal reaction, and sintering the generated solid to obtain the Nb-NiO nano material. The Nb-NiO nano material is used as a sensitive material of a gas sensor, and has the excellent characteristics of high response speed, high response value and good selectivity to xylene gas.
Description
Technical Field
The invention relates to the technical field of gas sensor sensitive materials, in particular to a Nb-NiO nano material and a preparation method and application thereof.
Background
In recent decades, with the rapid development of economy and industrialization, the emission of organic volatile compounds such as benzene, toluene, xylene, formaldehyde, acetone has attracted much attention. Xylene, a toxic gaseous pollutant, is widely used and released in the industrial production field, including as a chemical intermediate in the synthesis of polyesters, paints, rubbers and solvents in the leather industry, and also in gasoline, cigarettes, smoke, building and decorative materials, etc. The emission of xylene gas can cause air pollution and harm to human health, and long term exposure to 14ppm xylene and short term inhalation of as low as 50ppm xylene can damage the respiratory system, central nervous system, liver, kidneys, eyes and skin of a human. Therefore, it is also crucial to effectively detect the content of xylene gas in the environment.
Among various gas sensors, the metal oxide semiconductor type gas sensor is one of the most widely used gas sensors at present because of its advantages of high sensitivity, good selectivity, fast response recovery, low cost, convenient carrying and the like. The metal oxide semiconductor gas sensor can directly adsorb gas to be detected by using a sensitive material, so that the characteristics of the material, such as electrical property and the like, are changed, and the concentration of the gas to be detected is detected by detecting the change of an output signal of a peripheral circuit to a sensitive element. Nickel oxide, a typical p-type metal oxide semiconductor, has an adjustable band gap, excellent electrical properties and excellent chemical stability, and has outstanding oxidation catalytic activity on organic volatile compounds, which makes it a good candidate for designing and manufacturing high-performance gas sensors for detecting organic volatile compounds, however, due to its special parallel conduction paths (resistive particle cores and semiconductor near-surface regions), the p-type metal oxide semiconductor has a certain response to benzene, toluene, xylene, formaldehyde and acetone, but the response value and selectivity are low, which limits the application field of the p-type metal oxide semiconductor type gas sensors.
Disclosure of Invention
Aiming at the problems of low response value and poor selectivity of the gas sensor sensitive material made of the existing p-type metal oxide, the invention provides an Nb-NiO nano material and a preparation method and application thereof.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
an Nb-NiO nano material is a two-dimensional nano flaky crystal with the maximum diagonal length of 480-550nm, which is obtained by doping Nb element into NiO crystal lattice.
Compared with the prior art, the Nb-NiO nanomaterial provided by the invention has the advantages that the Nb element is doped in the NiO lattice to obtain the two-dimensional nano flaky crystal with the maximum diagonal length of 480-550nm, the two-dimensional nano flaky crystal has extremely high specific surface area, meanwhile, a uniform nano-pore structure is formed on the flaky crystal, the active sites of the two-dimensional nano flaky crystal are obviously increased, and the transmission of gas in the two-dimensional nano flaky crystal is promoted, so that the sensitivity and the selectivity of the two-dimensional nano flaky crystal on gas detection are obviously improved, particularly, the Nb-NiO nanomaterial has the excellent characteristics of high response speed, high response value and high sensitivity on xylene gas, the gas sensitivity is improved by about 110 times and the selectivity is improved by at least 2-16.1 times compared with the conventional.
The invention also provides a preparation method of the Nb-NiO nano material. The preparation method specifically comprises the following steps: adding soluble nickel salt and niobium salt into a mixed solution consisting of ethylene glycol and deionized water, dissolving, adding urea, carrying out hydrothermal reaction at 80-150 ℃ for 3-8h, cooling to obtain a suspension, carrying out solid-liquid separation, and sintering the solid at 400-600 ℃ for 1-5h to obtain the Nb-NiO nano material.
Compared with the prior art, the preparation method of the Nb-NiO nano material provided by the invention adopts a rapid hydrothermal synthesis method, adds soluble nickel salt and niobium salt into a mixed solution consisting of ethylene glycol and deionized water, adds urea, then reacts at a specific temperature, and sinters a reaction product, so that Nb is uniformly doped in a NiO lattice in the obtained Nb-NiO two-dimensional nano flaky crystal, thereby not only improving the specific surface area and pore volume of the Nb-NiO nano material, but also adjusting the carrier concentration of the formed Nb-NiO nano material, realizing electronic sensitization, and further improving the sensitivity and selectivity of gas detection.
The preparation method is simple, low in cost and high in preparation efficiency, and can be used for mass production, and the obtained Nb-NiO nano material has excellent gas sensitivity.
Preferably, the nickel salt is nickel nitrate, and the niobium salt is niobium pentachloride; the mass ratio of the nickel nitrate to the niobium pentachloride is 3.5-15: 1.
Preferably, the volume ratio of the ethylene glycol to the deionized water is 1-1.5: 1.
Preferably, the concentration of the nickel nitrate added into the mixed solution of glycol and deionized water is 0.02-0.04 g/ml.
Preferably, the mass ratio of the added urea to the nickel nitrate is 1: 0.8-2.3.
The preferable addition amounts of the ethylene glycol, the water and the urea can improve the uniformity of the thickness of the formed Nb-NiO flaky crystals, further control the maximum diagonal length of the formed flaky crystals to be about 500nm and the thickness to be between 5 and 20nm, increase the uniformity of the size and the thickness of the formed two-dimensional nano flaky crystals and improve the stability of the performance of the formed Nb-NiO nano material.
Preferably, the solid-liquid separation process is as follows: after centrifuging the suspension, the separated solid was washed with water, washed with alcohol and dried.
Preferably, the water washing process is to repeatedly wash the solid for 3 to 5 times by using deionized water; the alcohol washing process is to wash the solid with isopropanol; the drying process is drying the solid at 55-65 ℃.
The invention provides application of the Nb-NiO nano material in volatile gas detection
Preferably, the volatile gas is xylene.
The invention provides a gas sensor using the Nb-NiO nano material as a sensitive material, which comprises a sensitive element, wherein the Nb-NiO nano material is coated on the sensitive element, and the coating thickness is 20-40 mu m.
Compared with the prior art, the gas sensor disclosed by the invention can be used for rapidly and accurately detecting dimethylbenzene in the air by coating the Nb-NiO nano material on the sensitive element, and compared with a pure nickel oxide nano sheet, the sensitivity of the gas sensor to the dimethylbenzene in the air is improved by about 110 times, the gas sensor is sensitive in reaction and high in detection accuracy, and the gas sensor is simple in structure, convenient to manufacture, small in size, convenient to carry, suitable for mass production, capable of detecting the content of harmful volatile gas in multiple occasions and extremely high in application value.
The gas sensor also comprises a base and a protective cover; the sensitive element is fixed above the base, and the protective cover is arranged above the sensitive element. Wherein the base is a six-pin tube seat; the sensitive element is formed by taking Ni-Cr alloy with the resistance value of 35-40 omega as a heating wire to penetrate through Al with a ring-shaped Au electrode2O3The Nb-NiO nano material is coated on Al2O3The surface of the ceramic tube;
the method for coating the Nb-NiO nano material on the surface of the sensitive element comprises the following steps: putting the Nb-NiO nano material into a mortar, grinding for 20-30 minutes, then dripping water into the mortar, and uniformly stirring, wherein the mass ratio of the Nb-NiO nano material to the water is 5:1-3, so as to obtain viscous slurry; and (3) coating the obtained sticky slurry on the surface of a sensitive element, and drying for 1-3h at the temperature of 60-80 ℃.
Drawings
FIG. 1 is an X-ray diffraction pattern of Nb-NiO nanomaterials and NiO crystals obtained in example 1 of the present invention, wherein 1 is the X-ray diffraction pattern of Nb-NiO nanomaterials, and 2 is the X-ray diffraction pattern of NiO crystals;
FIG. 2 is a scanning electron microscope image of the Nb-NiO nanomaterial obtained in example 1 of the present invention;
FIG. 3 is a schematic view showing the structure of a gas sensor in example 1 of the present invention; the device comprises a base, a protective cover 1, a sensitive element 2, a sensitive element 3 and a base;
FIG. 4 is a graph showing the detection of response values of the gas sensor to various volatile gases in example 1 of the present invention;
FIG. 5 is a graph showing selective detection of paraxylene in the gas sensor of example 1 of the present invention with other gases of the same concentration as the interfering gas.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of Nb-NiO nano material comprises the following steps:
a. adding 1.5g of nickel nitrate and 0.1g of niobium pentachloride into 40ml of mixed solution consisting of ethylene glycol and deionized water, wherein the volume ratio of the ethylene glycol to the deionized water is 1:1, performing ultrasonic dispersion to form uniform solution, adding 1.875g of urea, continuing performing ultrasonic dispersion to form uniform solution, transferring the solution into a Teflon reaction kettle, performing hydrothermal reaction at 80 ℃ for 3 hours, and cooling to room temperature to obtain suspension;
b. and centrifuging the obtained suspension, separating solids, repeatedly washing the separated solids for 3 times by using deionized water, then washing the solids by using isopropanol, drying the washed solids in a 55-DEG C drying oven, placing the dried solids in a muffle furnace, and sintering for 5 hours at 400 ℃ to obtain the Nb-NiO nano material.
Performing X-ray diffraction analysis on the Nb-NiO nanomaterial obtained in the example 1 and a traditional NiO nano sheet to obtain an X-ray diffraction spectrum as shown in figure 1, wherein only characteristic peaks of NiO appear in the X-ray diffraction spectrum of the Nb-NiO nanomaterial to show that the Nb element is successfully doped into a NiO lattice of the obtained Nb-NiO nanomaterial and only shows the crystal form of NiO;
scanning electron microscope observation is carried out on the Nb-NiO nano material obtained in the example 1, and the observation result is shown in figure 2, so that the obtained Nb-NiO nano material is in a two-dimensional nano flaky structure with uniform thickness, and the thickness of the Nb-NiO nano material is 10-15 nm; the maximum diagonal length is 480-520 nm;
the gas sensor using the obtained Nb-NiO nanomaterial as a sensitive material, as shown in fig. 3, includes a base 3, a sensitive element 2, and a shield 1; the sensitive element 2 is fixed above the base 3, and the surface of the sensitive element is coated with the Nb-NiO nano material; the protective cover 1 is arranged above the sensitive element 2; thickness of the Nb-NiO nanomaterial coating20 μm; wherein, the base 3 is a six-pin tube seat; the sensing element 2 is formed by passing Ni-Cr alloy with a resistance value of 35 omega as a heating wire through Al with a ring-shaped Au electrode2O3Obtaining a ceramic tube, coating the Nb-NiO nano material on Al2O3The surface of the ceramic tube;
the method for coating the Nb-NiO nano material on the surface of the sensitive element 2 comprises the following steps: putting the Nb-NiO nano material into a mortar, grinding for 20 minutes, then dripping water into the mortar, and uniformly stirring, wherein the mass ratio of the Nb-NiO nano material to the water is 5:1, so as to obtain viscous slurry; the obtained viscous paste was coated on the surface of the sensor 2 and then dried at 60 ℃ for 1 hour.
The response values of the gas sensor obtained in this example to methanol, ethanol, acetone, benzene, toluene, and xylene gases were measured, and as shown in fig. 4, when the temperature was 370 ℃ and the gas concentration was 100ppm, the response value of the gas sensor to xylene reached 335 (the response value of the gas sensor with NiO as a sensitive material to xylene was 3), the response value to methanol was 30, the response value to ethanol was 45, the response value to acetone was 55, the response value to benzene was 5, and the response value to toluene was 110. Compared with a gas sensor with NiO as a sensitive material, the response value of the gas sensor in the embodiment to xylene is improved by 111 times, so that the gas sensor in the embodiment has excellent detection performance to xylene, and can be used for detecting toluene, methanol, ethanol and acetone in the air when necessary.
Detecting the selectivity of the gas sensor by taking the response value of the sensor to xylene as a reference, taking other gases with the same concentration as interference gases, and detecting the response value of the gas sensor to the xylene as a multiple of the response value of the gas sensor to the interference gases, wherein the response values are the selectivity values of the sensor, and the interference gases are methanol, ethanol, acetone, benzene and toluene respectively; the detection result is shown in fig. 5, when the sensitive material of the gas sensor is nickel oxide and the interference gases are methanol, ethanol, acetone, benzene and toluene, the selectivity values of the gas sensor to xylene are 2.6, 2.7, 2.5, 3 and 1.5 respectively; the sensitive material of the body sensor is the Nb-NiO nano material in the embodiment, and when the interference gases are methanol, ethanol, acetone, benzene and toluene, the selectivity values of the gas sensor to xylene are 12, 7.5, 6, 42.5 and 2.5 respectively; the gas sensor using the Nb-NiO nano material obtained in the embodiment as a sensitive material has higher selectivity to xylene.
Example 2
A preparation method of Nb-NiO nano material comprises the following steps:
a. adding 2g of nickel nitrate and 0.2g of niobium pentachloride into 70ml of mixed solution consisting of ethylene glycol and deionized water, wherein the volume ratio of the ethylene glycol to the deionized water is 1.2:1, performing ultrasonic dispersion to form uniform solution, adding 1g of urea, continuing to perform ultrasonic dispersion to form uniform solution, transferring the solution into a Teflon reaction kettle, performing hydrothermal reaction at 120 ℃ for 5 hours, and cooling to room temperature to obtain suspension;
b. and centrifuging the obtained suspension, separating solids, repeatedly washing the separated solids for 4 times by using deionized water, then washing the solids by using isopropanol, drying the washed solids in a 60 ℃ drying oven, and sintering the dried solids in a muffle furnace at 500 ℃ for 3 hours to obtain the Nb-NiO nano material.
Performing X-ray diffraction analysis on the Nb-NiO nano material obtained in the example 2 and the traditional NiO nano sheet, wherein only a characteristic peak of NiO appears in an X-ray diffraction pattern of the Nb-NiO nano material, which indicates that Nb element is successfully doped into a NiO lattice and only shows a NiO crystal form;
scanning electron microscope observation is carried out on the Nb-NiO nano material obtained in the embodiment 2, and the obtained Nb-NiO nano material is in a two-dimensional nano flaky structure with uniform thickness, and the thickness of the Nb-NiO nano material is 10-15 nm; the maximum diagonal length is 495-525 nm;
the structure of the gas sensor using the obtained Nb-NiO nanomaterial as a sensing material was the same as in example 1, wherein the Nb-NiO nanomaterial was coated to a thickness of 30 μm, and the coating method was the same as in example 1.
The response values of the gas sensor obtained in this example to methanol, ethanol, acetone, benzene, toluene, and xylene gases were measured, and when the temperature was 370 ℃ and the gas concentration was 100ppm, the response value of the gas sensor to xylene reached 341, the response value to methanol was 32, the response value to ethanol was 50, the response value to acetone was 53, the response value to benzene was 6, and the response value to toluene was 117.
The selectivity of the gas sensor is detected, the sensitive material of the gas sensor is the Nb-NiO nano material in the embodiment, and when the interference gas is methanol, ethanol, acetone, benzene and toluene, the selectivity values of the gas sensor to xylene are 15, 7.9, 6.5, 45 and 2.8 respectively.
Example 3
A preparation method of Nb-NiO nano material comprises the following steps:
a. adding 2.12g of nickel nitrate and 0.6g of niobium pentachloride into 100ml of mixed solution consisting of ethylene glycol and deionized water, wherein the volume ratio of the ethylene glycol to the deionized water is 1.5:1, performing ultrasonic dispersion to form uniform solution, adding 0.92g of urea, continuing performing ultrasonic dispersion to form uniform solution, transferring the solution into a Teflon reaction kettle, performing hydrothermal reaction at 150 ℃ for 8 hours, and cooling to room temperature to obtain suspension;
b. and centrifuging the obtained suspension, separating solids, repeatedly washing the separated solids for 5 times by using deionized water, then washing the solids by using isopropanol, drying the washed solids in a 65 ℃ drying oven, placing the dried solids in a muffle furnace, and sintering for 1h at 600 ℃ to obtain the Nb-NiO nano material.
Performing X-ray diffraction analysis on the Nb-NiO nano material obtained in the embodiment 3 and the traditional NiO nano sheet, wherein only a characteristic peak of NiO appears in an X-ray diffraction pattern of the Nb-NiO nano material, which indicates that Nb is successfully doped into a NiO lattice and only shows a NiO crystal form;
scanning electron microscope observation is carried out on the Nb-NiO nano material obtained in the embodiment 3, the obtained Nb-NiO nano material is in a two-dimensional nano flaky structure with uniform thickness, the thickness is between 10 and 20nm, and the maximum diagonal length is 480-550 nm;
the structure of the gas sensor using the obtained Nb-NiO nanomaterial as a sensitive material is the same as that of example 1, wherein the Nb-NiO nanomaterial is coated to a thickness of 40 μm, and the coating method is the same as that of example 1.
The response values of the gas sensor obtained in this example to methanol, ethanol, acetone, benzene, toluene, and xylene gases were measured, and when the temperature was 370 ℃ and the gas concentration was 100ppm, the response value of the gas sensor to xylene reached 343, the response value to methanol was 36, the response value to ethanol was 51, the response value to acetone was 55, the response value to benzene was 5, and the response value to toluene was 110.
The selectivity of the gas sensor is detected, the sensitive material of the gas sensor is the Nb-NiO nanomaterial in this embodiment, and when the interfering gases are methanol, ethanol, acetone, benzene, and toluene, the selectivity values of the gas sensor to xylene are 15.5, 8.2, 7, 49, and 3.2, respectively.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. An Nb-NiO nano material, which is characterized in that: nb is doped in NiO crystal lattice to obtain two-dimensional nano sheet crystal with maximum diagonal length of 480-550 nm.
2. The method for preparing the Nb-NiO nano material of claim 1, wherein: adding soluble nickel salt and niobium salt into a mixed solution consisting of ethylene glycol and deionized water, dissolving, adding urea, carrying out hydrothermal reaction at 80-150 ℃ for 3-8h, cooling to obtain a suspension, carrying out solid-liquid separation, and sintering the solid at 400-600 ℃ for 1-5h to obtain the Nb-NiO nano material.
3. The method of producing Nb-NiO nanomaterials of claim 2 wherein: the nickel salt is nickel nitrate, and the niobium salt is niobium pentachloride; the mass ratio of the nickel nitrate to the niobium pentachloride is 3.5-15: 1.
4. The method of producing Nb-NiO nanomaterials of claim 2 wherein: the volume ratio of the ethylene glycol to the deionized water is 1-1.5: 1.
5. The method of producing Nb-NiO nanomaterials of claim 2 wherein: the concentration of the nickel nitrate added into a mixed solution consisting of glycol and deionized water is 0.02-0.04 g/ml; and/or
The mass ratio of the added urea to the nickel nitrate is 1: 0.8-2.3.
6. The method of producing Nb-NiO nanomaterials of claim 2 wherein: the solid-liquid separation process comprises the following steps: after centrifuging the suspension, the separated solid was washed with water, washed with alcohol and dried.
7. The method of producing Nb-NiO nanomaterials of claim 6 wherein: the water washing process is to repeatedly wash the solid for 3-5 times by using deionized water; the alcohol washing process is to wash the solid with isopropanol; the drying process is drying the solid at 55-65 ℃.
8. Use of the Nb-NiO nanomaterials of claim 1 to detect volatile gases.
9. The use of claim 8, wherein: the volatile gas is xylene.
10. A gas sensor using the Nb-NiO nanomaterial of claim 1 as a sensing material, characterized in that: the sensor comprises a sensing element, wherein the Nb-NiO nano material is coated on the sensing element, and the coating thickness is 20-40 mu m.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111892715B (en) * | 2020-08-13 | 2021-04-16 | 广东泰金智能包装有限公司 | Metal organic framework material and preparation method and application thereof |
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| Title |
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| LEI QIU等: "Highly selective and sensitive xylene sensors based on Nb-doped NiO nanosheets", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111892715B (en) * | 2020-08-13 | 2021-04-16 | 广东泰金智能包装有限公司 | Metal organic framework material and preparation method and application thereof |
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Application publication date: 20200609 |