CN104897726A - High-sensitivity gas sensor prepared by utilizing sol-gel method - Google Patents
High-sensitivity gas sensor prepared by utilizing sol-gel method Download PDFInfo
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- CN104897726A CN104897726A CN201510264908.8A CN201510264908A CN104897726A CN 104897726 A CN104897726 A CN 104897726A CN 201510264908 A CN201510264908 A CN 201510264908A CN 104897726 A CN104897726 A CN 104897726A
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Abstract
The invention discloses a high-sensitivity gas sensor prepared by utilizing a sol-gel method. The gas sensor takes nanometer copper oxide as a gas-sensitive material, and is characterized in that the nanometer copper oxide is prepared by virtue of a sol-gel method. The method comprises the following steps: (1) preparing a sol-gel solution, namely taking isopropanol as a solvent, taking copper acetate monohydrate as a solute, taking ethanol amine as a stabilizer, mixing, stirring and heating the isopropanol, copper acetate and ethanol amine, cooling and standing; and (2) drying the sol-gel solution, heating to the temperature of 450-550 DEG C, preserving the temperature for 1-3 hours, and cooling. Compared with the conventional gas sensor taking nanometer copper oxide as the gas-sensitive material, the gas sensor disclosed by the invention has the advantages that the sensitivity for low-concentration gases such as methanol, ethanol, acetone and formaldehyde can be obviously improved, particularly the sensitivity for the gases with the concentration of 20ppm or below can be improved.
Description
Technical field
The invention belongs to sensor field, be specifically related to a kind of high sensitivity gas sensor utilizing sol-gel process to prepare.
Background technology
Along with the raising of industrial expansion, living standards of the people and to environmental protection pay attention to day by day, the detection of people to the monitoring of atmospheric pollution, industrial gaseous waste and human settlement's air quality is proposed higher requirement.Metal oxide nano-material can be applicable to sensor manufacture because it has gas-sensitive property, day by day comes into one's own.
Gas sensor divides from structure, heater-type and directly-heated type can be divided into, due to heater-type gas sensor have power consumption little, have explosion-protection equipment, the feature such as safe and reliable, therefore it utilization and development more and more wider, its structure as shown in Figure 1, comprises insulation course, gas sensing layer, electrode and heater strip.
The document [1] be published in Dec, 2014 on Journal of Colloid and Interface Science has been reported and has been utilized chemical precipitation method, with polyglycol, copper sulphate, urea and NaOH etc. for CuO nanocrystal prepared by raw material, and with it for gas sensitive, the gas sensitive device of preparation has good sensitivity (response(R when gas concentration reaches hundreds of ppm
gas/ R
air)), but when concentration is down to ten about ppm, sensitivity obviously declines, the sensitivity as the alcohol gas to 10ppm is only about 2.0.
Be published in January, 2015 in the pertinent literature [2] on J Mater Sci:Mater Electron publication, author utilizes chemical precipitation method equally, with thiocarbamide, copper sulphate and sodium peroxide etc. for CuO nano flake prepared by raw material, and with it for gas sensitive, the alcohol gas of 20ppm level of the sensitivity gas sensitive device of preparation is low to moderate to(for) concentration is also only about 2.0.
Be published in August, 2014 in the pertinent literature [3] on Scientific Reports publication, to expose, { the CuO nano material of 001} crystal face is that gas sensitive prepares gas sensitive device, when although CuO pattern is nano-plates (nanoplatelets), gas sensitive device for concentration be several acetone to tens ppm, alcohol gas can reach sensitivity close to 3, but when CuO pattern is nano particle (nanoparticles), the sensitivity of gas sensitive device to the acetone under this concentration, alcohol gas significantly declines, only less than 1-1.5.
Although several gas sensor be made up of copper oxide nano material has good sensitivity to the gas that concentration reaches hundreds of ppm above, the concentration of detected gas drop to tens ppm even lower time, sensitivity obviously reduces, and limits its application.
Be published in November, 2014 in the pertinent literature [4] on Sensors and Acturtors B:Chemical publication, author utilizes chemical precipitation method, with Schweinfurt green, 1,5-pentanediol, tygon pyrrole network alkane ketone and acetone are that CuO nano cubic structure prepared by raw material, and with it for gas sensitive, the gas sensitive device prepared is for the formaldehyde gas of concentration 3ppm ~ 50ppb, and its sensitivity is all less than 1.2, and the sensitivity for other gas is then lower.
List of references:
[1] Yang Chao, Xiao Feng, Wang Jide etc., " Synthesis and microwave modification of CuO nanoparticles:Crystallinity and morphological variations, catalysis, and gas sensing ", JOURNAL OF COLLOID AND INTERFACE SCIENCE, volume: 435, page: 34-42, imp d: DEC 2014.
[2] Yan Huiying, Tian Xianqing, Sun Jie etc., " Enhanced sensing properties of CuO nanosheets for volatile organic compounds detection ", JOURNAL OF MATERIALS SCIENCE:MATERIALS IN ELECTRONICS, volume: 26, phase: 1, page: 280-287, imp d: JAN 2015.
[3] Su Dawei, Xie Xiuqiang, Dou Shixue etc., " CuO single crystal with exposed 001}facets-A highly efficient material foe gas sensing and Li-ion battery applications ", SCIENTIFIC REPORTS, volume: 4, document number: 5753, imp d: AUG 29 2014.
[4] Park Hyung Ju, Choi Nak-Jin, Kang Hyuntae etc., " A ppb-level formaldehyde gas sensor based on CuO nanocubes prepared using a polyol process ", SENSORS AND ACTUATORS B:CHEMICAL, volume: 203, page: 282-288, imp d: NOV 2014.
Summary of the invention
The object of the invention is to overcome the existing gas sensor using nano cupric oxide as gas sensitive for the high defect of the insufficient sensitivity of low concentration particularly below 20ppm gas, provide a kind of, for light concentration gas, still there is highly sensitive gas sensor.
It is as follows that the present invention realizes the technical scheme that above-mentioned purpose adopts:
The high sensitivity gas sensor utilizing sol-gel process to prepare, described gas sensor take nano cupric oxide as gas sensitive, it is characterized in that, described nano cupric oxide is prepared by sol-gel process, comprises the steps:
(1) preparation of sol gel solution: take isopropyl alcohol as solvent, a hydration Schweinfurt green is solute, and monoethanolamine is stabilizing agent, heats isopropyl alcohol, Schweinfurt green and monoethanolamine mix and blend, and cooling leaves standstill;
(2) after sol gel solution is dried, be heated to 450 ~ 550 DEG C, be incubated 1 ~ 3 hour, cooling.
Further, in step (1), the amount ratio of a described hydration Schweinfurt green and isopropyl alcohol is 1g:(10-20) mL.
Further, in step (1), the mass ratio of a described hydration Schweinfurt green and monoethanolamine is 1:(1-2).
Further, in step (1), isopropyl alcohol, Schweinfurt green and monoethanolamine are mixed and heated to 70-80 DEG C, insulation 1-3 hour.
Further, step (2), is incubated in air atmosphere.
Further, step (2) is with heating rate to 450 ~ 550 DEG C of 4-6 DEG C/min.
Further, step (2) cools with the speed of 2-4 DEG C/min.
Described highly sensitive gas sensor is for detecting alcohols, aldehydes, ketone, benzene hydrocarbon gase.
Further, described alcohols gas is methyl alcohol, ethanol, propyl alcohol etc.; Described gaseous aldehyde is formaldehyde, acetaldehyde etc.; Described ketone gas is acetone etc.; Described benzene hydrocarbon gase is benzene,toluene,xylene.
Beneficial effect of the present invention:
Compared with the existing gas sensor using nano cupric oxide as gas sensitive, gas sensor of the present invention can significantly improve the sensitivity sensitivity, particularly concentration of light concentration gas (as methyl alcohol, ethanol, acetone, formaldehyde etc.) being low to moderate to below 20ppm.
Present invention process is simple, and cost is low, and product conversion capability is high, is easy to batch production, low in energy consumption, pollution-free, with environmental friendliness.
Accompanying drawing explanation
Fig. 1 is the structural representation of heater-type gas sensor.
Fig. 2 is the x-ray diffraction pattern (XRD) of gas sensor gas sensing layer of the present invention.
Fig. 3 is scanning electron microscope (SEM) photo of gas sensor gas sensing layer of the present invention.
Fig. 4 is the air-sensitive response diagram of gas sensor of the present invention to gas with various.
Fig. 5-6 is the air-sensitive response diagram of gas sensor of the present invention to the alcohol gas of variable concentrations.
Fig. 7-8 is the air-sensitive response diagram of gas sensor of the present invention to the formaldehyde gas of variable concentrations.
Fig. 9-10 is the air-sensitive response diagram of gas sensor of the present invention to the acetone gas of variable concentrations.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Embodiment 1
(1) measure isopropyl alcohol with graduated cylinder, volume is 30mL; Draw monoethanolamine with the disposable plastic dropper of cleaning, volume is 2mL; With electronic balance weighing one hydration Schweinfurt green, quality is 2g;
The hydration Schweinfurt green taken is poured in isopropyl alcohol, adds monoethanolamine subsequently as stabilizing agent;
Carry out temperature constant magnetic stirring to potpourri, temperature controls at 80 DEG C, and stirring the duration is 2 hours;
The potpourri stirred at room temperature is left standstill 24 hours, forms navy blue sol-gel liquid, for subsequent use.
(2) making of gas sensor:
Pass ceramic pipe center pit with fixing ceramic pipe with copper wire, launch four pin electrodes of ceramic pipe outer wall, to carry out pin welding;
Draw the sol-gel liquid left standstill with dropper, drip sol-gel liquid gently in the ceramic pipe outer wall of horizontal positioned;
The ceramic pipe of slow circumvolve horizontal positioned, the sol-gel liquid that outer wall is suspended gradually uniform fold in outer wall, until form the blue rete of one deck not easily deformation;
Be fixed in metal frame by ceramic pipe together with copper wire, put into baking oven, and toast half an hour with 85 DEG C, the solvent in sol-gel liquid is fully evaporated, and after taking-up, ceramic pipe outer wall adheres to blue rete;
After baking, ceramic pipe is put into tubular furnace together with metal frame, is warming up to 500 DEG C with the programming rate of 5 DEG C/min, in air ambient, be incubated 2 hours, then be cooled to room temperature with the speed of 3 DEG C/min;
Take out cooled ceramic pipe, ceramic pipe outer wall forms one deck silvery white rete, namely obtains heater-type gas sensor.
The XRD of gas sensing layer as shown in Figure 2, coincide good with the CuO standard peak shape of numbering 80-0076, can judge that gas sensing layer is CuO thus by XRD peak shape.
As shown in Figure 3, CuO forms nanocrystalline granulosa at ceramic pipe outer wall to the SEM of gas sensing layer, and the mean diameter of nanocrystal is about 100nm.
Working temperature of the present invention is usually between 180 DEG C to 220 DEG C.Fig. 4 is the air-sensitive response diagram of gas sensor of the present invention to gas with various (5ppm).As seen from the figure, gas sensor of the present invention to concentration be the methyl alcohol of 5ppm, the sensitivity of ethanol, acetone is all not less than 2.8, also reaches 1.7 to the sensitivity of toluene.
Fig. 5-6 is gas sensor of the present invention air-sensitive response diagrams to the alcohol gas of variable concentrations.As seen from the figure, the present invention is the alcohol gas of 10ppm for concentration, and its sensitivity is 3.1; Concentration is the alcohol gas of 5ppm, and its sensitivity is 2.8; 0.1ppm(and 100ppb is low to moderate for concentration) alcohol gas, its sensitivity also can reach 1.4.
Fig. 7-8 is gas sensor of the present invention air-sensitive response diagrams to the formaldehyde gas of variable concentrations.As seen from the figure, the present invention is the formaldehyde gas of 400ppb, 200ppb, 100ppb and 50ppb for concentration, and sensitivity is respectively 2.15,1.85,1.63 and 1.55.
Fig. 9-10 be gas sensor of the present invention to the air-sensitive response diagram of the acetone gas of variable concentrations as seen from the figure, the present invention is the acetone gas of 1ppm, 2ppm, 5ppm and 10ppm for concentration, and sensitivity is respectively 1.52,3.78,4.2 and 5.5.
Embodiment 2
Be different from embodiment 1, in step (1), the consumption of isopropyl alcohol, monoethanolamine and a hydration Schweinfurt green is respectively 30mL, 2mL, 1.5g.Step (2), is warming up to 550 DEG C with the programming rate of 6 DEG C/min, is down to room temperature with the cooling rate of 2 DEG C/min.
The structure of gas sensor of the present invention is not limited to above-mentioned heater-type, is suitable for too for directly-heated type structure.
Claims (10)
1. utilize a high sensitivity gas sensor prepared by sol-gel process, described gas sensor is gas sensitive with nano cupric oxide, and it is characterized in that, described nano cupric oxide is prepared by sol-gel process, comprises the steps:
(1) preparation of sol gel solution: take isopropyl alcohol as solvent, a hydration Schweinfurt green is solute, and monoethanolamine is stabilizing agent, heats isopropyl alcohol, Schweinfurt green and monoethanolamine mix and blend, and cooling leaves standstill;
(2) after sol gel solution is dried, be heated to 450 ~ 550 DEG C, be incubated 1 ~ 3 hour, cooling.
2. gas sensor according to claim 1, is characterized in that, in step (1), the amount ratio of a described hydration Schweinfurt green and isopropyl alcohol is 1g:(10-20) mL.
3. gas sensor according to claim 1, is characterized in that, in step (1), the mass ratio of a described hydration Schweinfurt green and monoethanolamine is 1:(1-2).
4. gas sensor according to claim 1, is characterized in that, in step (1), isopropyl alcohol, Schweinfurt green and monoethanolamine are mixed and heated to 70-80 DEG C, insulation 1-3 hour.
5. gas sensor according to claim 1, is characterized in that, step (2), is incubated in air atmosphere.
6. gas sensor according to claim 1, is characterized in that, step (2) is with heating rate to 450 ~ 550 DEG C of 4-6 DEG C/min.
7. gas sensor according to claim 1, is characterized in that, step (2) cools with the speed of 2-4 DEG C/min.
8. gas sensor according to claim 1, is characterized in that: described gas sensor is heater-type gas sensor.
9. gas sensor according to claim 1 is for detecting alcohols, aldehydes, ketone, benzene hydrocarbon gase.
10. purposes according to claim 9, is characterized in that, described alcohols gas is methyl alcohol, ethanol, propyl alcohol; Described gaseous aldehyde is formaldehyde, acetaldehyde; Described ketone gas is acetone; Described benzene hydrocarbon gase is benzene,toluene,xylene.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1443228A (en) * | 2001-05-21 | 2003-09-17 | 日本油漆株式会社 | Colloidal alcohol solution of noble metal or copper, process for producing same, and coating composition |
| CN102331443A (en) * | 2011-07-13 | 2012-01-25 | 东华大学 | Acetone gas sensor and manufacturing method thereof |
| CN102581294A (en) * | 2012-03-26 | 2012-07-18 | 沈阳化工大学 | Method for preparing nano-metallic copper powder |
| US9011778B2 (en) * | 2006-10-12 | 2015-04-21 | Nextech Materials, Ltd. | Hydrogen sensitive composite material, hydrogen gas sensor, and sensor for detecting hydrogen and other gases with improved baseline resistance |
-
2015
- 2015-05-22 CN CN201510264908.8A patent/CN104897726A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1443228A (en) * | 2001-05-21 | 2003-09-17 | 日本油漆株式会社 | Colloidal alcohol solution of noble metal or copper, process for producing same, and coating composition |
| US9011778B2 (en) * | 2006-10-12 | 2015-04-21 | Nextech Materials, Ltd. | Hydrogen sensitive composite material, hydrogen gas sensor, and sensor for detecting hydrogen and other gases with improved baseline resistance |
| CN102331443A (en) * | 2011-07-13 | 2012-01-25 | 东华大学 | Acetone gas sensor and manufacturing method thereof |
| CN102581294A (en) * | 2012-03-26 | 2012-07-18 | 沈阳化工大学 | Method for preparing nano-metallic copper powder |
Non-Patent Citations (3)
| Title |
|---|
| IQBAL SINGH等: ""Influence of pH on the synthesis and characterization of CuO powder for thick film room-temperature NH3 gas sensor"", 《JOURNAL OF MATERIALS SCIENCE》 * |
| 谭伟石: "《近代物理实验》", 30 September 2013 * |
| 贾瑜等: ""多孔不锈钢基体表面CuO薄膜的制备"", 《材料热处理技术》 * |
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