CN105548275A - Acetone sensor based on NiO/ZnO heterostructure nanoflower sensitive material and preparation method of acetone sensor - Google Patents
Acetone sensor based on NiO/ZnO heterostructure nanoflower sensitive material and preparation method of acetone sensor Download PDFInfo
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Abstract
The invention provides an acetone sensor based on a NiO/ZnO heterostructure nanoflower sensitive material and a preparation method of the acetone sensor, and belongs to the technical field of semiconductor oxide gas sensors. The NiO/ZnO heterostructure nanoflower sensitive material which is used is a NiO-ZnO heterostructure nanoflower sensitive material prepared through a water-bath method and a dipping method. The sensitivity of the sensor to acetone is effectively improved through the catalysis effect of NiO nanoparticles on organic gas and the heterostructure of NiO and ZnO. In addition, The sensor is structurally composed of an Al2O3 insulating ceramic pipe which is sold on the market and comprising two annular cold electrodes, a semiconductor sensitive material with which the annular gold electrodes and the Al2O3 insulating ceramic pipe are coated, and a nichrome alloy heating coil penetrating through the Al2O3 insulating ceramic pipe. The device is simple in process, small in size and suitable for mass production, and therefore the acetone sensor has wide application prospects on the aspect of the acetone content in detection microenvironments.
Description
Technical field
The invention belongs to conductor oxidate gas sensor technical field, be specifically related to a kind of acetone gas sensor based on NiO/ZnO heterogeneous structural nano flower sensitive material and preparation method thereof.
Background technology
Acetone industrially not only as the important solvent of producing explosive, plastics, rubber, or can be used as the important source material of the materials such as synthesis ketenes, iodoform, epoxy resin.But be similar to other organic solvents, it has inflammable, volatile feature, meet naked light, high thermoae easy firing blast.And acetone not only has larger fire risk, also to the central nervous system of people, there is anesthetic action, people even can be caused during high concentration to go into a coma and death.Therefore, the detection tool for acetone gas is of great significance.
In the gas sensor of huge number, with conductor oxidate be the resistor-type gas sensor of sensitive material have highly sensitive, Monitoring lower-cut is low, selectivity good, response and the advantage such as resume speed is fast, method for making simple, cost is lower, is one of current most widely used gas sensor.Along with the development of nanometer science and technology, gas sensitive is regulated and controled the specific surface area that formation of nanostructured greatly can improve material, increase avtive spot, gas-sensitive property can be made to improve.In addition, by making two kinds of gas sensitives combine, utilizing the cooperative effect between them that gas sensitive can be made to obtain further modification, thus obtaining better gas-sensitive property.
ZnO is a kind of n-type semiconductor of broad stopband, and because it is nontoxic, method for making is simple etc. is widely used in gas sensing aspect.But, although many different-shapes, the ZnO material with Large ratio surface sum avtive spot density are developed out, but most of ZnO, when detecting VOC (volatile organic compounds) gas, shows lower sensitivity and higher detected temperatures.Therefore, utilize the catalytic oxidation ability of NiO, for the further modification of ZnO material, thus it is most important to promote its air-sensitive performance.
Summary of the invention
The object of this invention is to provide a kind of acetone gas sensor based on NiO/ZnO heterogeneous structural nano flower sensitive material and preparation method thereof.
Utilize NiO/ZnO heterogeneous structural nano flower as sensitive material, on the one hand the three-dimensional structure of ZnO makes that material is loose, good dispersion, and the matrix pattern that the modification for NiO provides, is conducive to transmission and the detection of gas; NiO nano particle has stronger oxidisability on the other hand, and all has the ability of catalytic oxidation to multiple VOC gas, so more oxygen molecule can be caused to participate in reaction; In addition, because the difference of Fermi level can form a large amount of heterojunction between NiO and ZnO, the appearance of these heterojunction can provide more reactivity site.The acting in conjunction of this three aspect significantly improves the reaction efficiency of gas and sensitive material, and then improves the sensitivity of sensor.Commercially available tubular structure sensor manufacturing process of the present invention is simple, and volume is little, is beneficial to industrial batch production, therefore has important using value.
Acetone gas sensor based on NiO/ZnO heterogeneous structural nano flower sensitive material of the present invention, by outside surface with two parallel, ring-types and the ceramic pipe substrate of gold electrode separate, the sensitive material be coated on ceramic pipe outside surface and gold electrode, the nickel-chrome heater strip be placed in ceramic pipe form; It is characterized in that: sensitive material is NiO/ZnO heterogeneous structural nano flower, and is prepared by following steps:
(1) preparation of ZnO nano flower
1. first by the Zn (CH of 1 ~ 3g
3cOO)
22H
2o is dissolved in the middle of the deionized water of 100 ~ 150mL, and keeps constantly stirring until it all dissolves; Again slowly to its ammoniacal liquor adding 3 ~ 5mL until solution clarification;
2. above-mentioned solution is transferred in thermostat water bath, keep taking out after 30 ~ 90 minutes at 60 ~ 90 DEG C, naturally cool to the precipitate with deionized water that generates and ethanol repeatedly eccentric cleaning after room temperature, then calcine 1 ~ 2 hour at 400 ~ 500 DEG C again after at room temperature drying, thus obtain the ZnO nano pollen end assembled by ZnO nano particle;
(2) preparation of NiO/ZnO heterogeneous structural nano flower
1. getting 30 ~ 50mg above-mentioned ZnO nano pollen end joins in 5 ~ 10mL ethanol, ultrasonic and stir and within 10 ~ 30 minutes, make ZnO nano pollen end disperse completely in ethanol; And then add 8 ~ 10mgNi (NO
3)
26H
2o, is at room temperature stirred to ethanol and is substantially evaporated completely complete;
2. above-mentioned dried powder collected and calcining 2 ~ 4 hours at 500 ~ 550 DEG C, thus obtain with ZnO nano flower be trunk, NiO nano particle is evenly attached to the NiO/ZnO heterogeneous structural nano pollen end on ZnO surface;
The preparation method of a kind of acetone gas sensor based on NiO/ZnO heterogeneous structural nano flower sensitive material of the present invention, its step is as follows:
1. by NiO/ZnO heterogeneous structural nano pollen end with deionized water in mass ratio 3 ~ 5:1 mix, and grind formation pasty slurry, then dip a small amount of slurry and be coated in the Al that commercially available outside surface carries 2 annular gold electrodes equably
2o
3ceramic pipe surface, form 10 ~ 30 μm of thick sensitive material films, the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, and internal diameter is 0.8 ~ 1.0mm, and makes sensitive material cover annular gold electrode completely;
2. toast 30 ~ 45 minutes under infrared lamp, after sensitive material drying, Al
2o
3ceramic pipe is calcined 2 ~ 3 hours at 400 ~ 450 DEG C; Then be that the NI-G heater coil of 30 ~ 40 Ω is through Al by resistance value
2o
3above-mentioned device, as heater strip, finally carries out welding and encapsulating according to general heater-type gas sensor by ceramic tube inside, thus obtains NiO/ZnO oxide semiconductor acetone sensor.
Acetone gas sensor based on NiO/ZnO heterogeneous structural nano flower sensitive material prepared by the present invention has the following advantages:
1. utilize simple immersion method and infusion process just can prepare the composite structure of graduation nano material at low temperatures, synthetic method is simple, with low cost;
2. by taking growth NiO at ZnO nano, bi-material is combined, improves the sensitivity to acetone, reduce the optimum working temperature of material, and there is response resume speed and good repeatability fast, have broad application prospects in detection content of acetone;
3. adopt commercially available tubular type sensor, device technology is simple, and volume is little, is suitable for producing in enormous quantities.
Accompanying drawing explanation
The SEM shape appearance figure of Fig. 1: NiO/ZnO heterogeneous structural nano flower, wherein the enlargement factor of (a) figure is 5000 times, and the enlargement factor of (b) figure is 30000 times;
Fig. 2: the XRD figure of ZnO nano flower and NiO/ZnO heterogeneous structural nano flower;
Fig. 3: based on the acetone sensor structural representation of NiO/ZnO heterogeneous structural nano flower sensitive material;
Fig. 4: in comparative example and embodiment sensor at different operating temperature to the sensitivity curve of 100ppm acetone gas;
Fig. 5: in comparative example and embodiment sensor under respective optimum working temperature to the response recovery curve of 100ppm acetone gas;
Fig. 6: the sensor sensitivity under respective optimum working temperature-acetone concentration family curve in comparative example and embodiment.
As shown in Figure 1, can find out in (a) figure that NiO/ZnO heterojunction structure is flower-like nanostructure, favorable dispersibility; B find out NiO/ZnO heterogeneous structural nano flower in () figure with ZnO nano flower for trunk, NiO nano particle is evenly distributed on nano flower.The diameter of nano flower is about 2 ~ 3 μm;
As shown in Figure 2, there is the characteristic peak of NiO and ZnO in the XRD spectra of NiO/ZnO heterogeneous structural nano flower, interpret sample comprises NiO and ZnO crystal; ZnO nano flower is then pure phase ZnO structure;
As shown in Figure 3, device is by Al
2o
3ceramic pipe 1, semiconductor sensitive material 2, nickel-cadmium coil 3, annular gold electrode 4 and platinum line 5 form;
As shown in Figure 4, the optimum working temperature of comparative example and embodiment is respectively 350 DEG C and 300 DEG C, and the now sensitivity of device to 100ppm acetone is respectively 5.1 and 23.5;
As shown in Figure 5, when device be operated in optimum working temperature separately, under acetone gas concentration is 100ppm, comparative example and embodiment all have good repeatability;
As shown in Figure 6, when embodiment device is at working temperature is 300 DEG C, the sensitivity of device increases along with the increase of acetone concentration, the sensitivity of embodiment to 10,20,40,60,80,100 and 200ppm acetone is respectively 3.61,6.55,12.7,16.62,20.5,23.5 and 38.8, and the sensitivity of comparative example to 10 ~ 200ppm acetone is only 1.45 ~ 7.7.
Note: the sensitivity (n-type semiconductor) of device is defined as its resistance value and ratio of resistance value size in tested gas in atmosphere in test reducibility gas, is S=R
a/ R
g.In test process, static test system is used to test.Be placed in by device in the gas tank of 50 ~ 80L, inwardly a certain amount of organic gas to be measured of injection, observes and records its change in resistance, by calculating corresponding sensitivity number.
Embodiment
Comparative example 1:
Heater-type acetone sensor is made, its concrete manufacturing process using ZnO nano flower as sensitive material:
1. first by the Zn (CH of 1.0g
3cOO)
22H
2o is dissolved in the middle of the deionized water of 100mL, and keeps constantly stirring until it all dissolves; Again slowly to its ammoniacal liquor adding 3.4mL until solution clarification;
2. above-mentioned solution is transferred in thermostat water bath, keep taking out after 60 minutes at 80 DEG C, naturally cool to the precipitate with deionized water that generates and ethanol repeatedly eccentric cleaning after room temperature, then calcine 1.5 hours at 450 DEG C again after at room temperature drying, thus obtain the ZnO nano flower assembled by ZnO nano particle;
3. the ZnO nano flower sensitive material powder taking a morsel obtained, 5:1 instills deionized water in mass ratio, grinds to form pasty slurry.Then dip a small amount of slurry with brush and be coated in the Al that commercially available outside surface carries 2 annular gold electrodes equably
2o
3ceramic pipe surface, form 30 μm of thick sensitive material films, the length of ceramic pipe is 4mm, and external diameter is 1.2mm, and internal diameter is 0.8mm, and makes sensitive material cover annular gold electrode completely;
4. toast 30 minutes under infrared lamp, after sensitive material drying, Al
2o
3ceramic pipe is calcined 2 hours at 400 DEG C; Then be that the nickel-cadmium coil of 30 Ω is through Al by resistance value
2o
3above-mentioned device, as heater strip, finally carries out welding and encapsulating according to general heater-type gas sensor by ceramic tube inside, thus obtains ZnO nano flower acetone sensor.
Embodiment 1:
Acetone sensor is made as sensitive material, its concrete manufacturing process with NiO/ZnO heterogeneous structural nano flower:
1. first by the Zn (CH of 1.0g
3cOO)
22H
2o is dissolved in the middle of the deionized water of 100mL, and keeps constantly stirring until it all dissolves; Again slowly to its ammoniacal liquor adding 3.4mL until solution clarification;
2. above-mentioned solution is transferred in thermostat water bath, keep taking out after 60 minutes at 80 DEG C, naturally cool to the precipitate with deionized water that generates and ethanol repeatedly eccentric cleaning after room temperature, then calcine 1.5 hours at 450 DEG C again after at room temperature drying, thus obtain the ZnO nano flower assembled by ZnO nano particle;
3. getting 35mg above-mentioned ZnO nano pollen end joins in 6mL ethanol, ultrasonic and stir and within 20 minutes, make ZnO nano pollen end disperse completely in ethanol.And then add 10.0mgNi (NO3) 26H2O, be at room temperature stirred to ethanol and be substantially evaporated completely complete; Above-mentioned dried powder is collected and moves to muffle furnace, calcine 3 hours at 550 DEG C, thus obtain with ZnO nano flower be trunk, NiO nano particle be evenly attached to ZnO surface for the colored sensitive material powder of NiO/ZnO heterogeneous structural nano;
4. by the NiO/ZnO heterogeneous structural nano obtained flower sensitive material powder and deionized water in mass ratio 5:1 mix, and grinding forms pasty slurry, then dip a small amount of slurry with brush and be coated in the Al2O3 ceramic pipe surface that commercially available outside surface carries 2 annular gold electrodes equably, form 30 μm of thick sensitive material films, the length of ceramic pipe is 4mm, external diameter is 1.2mm, and internal diameter is 0.8mm, and makes sensitive material cover annular gold electrode completely;
5. toast 3 minutes under infrared lamp, after sensitive material drying, Al
2o
3ceramic pipe is calcined 2 hours at 400 DEG C; Then be that the nickel-cadmium coil of 30 Ω is through Al by resistance value
2o
3above-mentioned device, as heater strip, finally carries out welding and encapsulating according to general heater-type gas sensor by ceramic tube inside, thus obtains the acetone gas sensor of NiO/ZnO heterogeneous structural nano flower sensitive material.
Claims (3)
1. based on an acetone gas sensor for NiO/ZnO heterogeneous structural nano flower sensitive material, by outside surface with two parallel, ring-types and the ceramic pipe substrate of gold electrode separate, the sensitive material be coated on ceramic pipe outside surface and gold electrode, the nickel-chrome heater strip be placed in ceramic pipe form; It is characterized in that: sensitive material is NiO/ZnO heterogeneous structural nano pollen end, and is prepared by following steps:
(1) preparation of ZnO nano flower
1. first by the Zn (CH of 1 ~ 3g
3cOO)
22H
2o is dissolved in the middle of the deionized water of 100 ~ 150mL, and keeps constantly stirring until it all dissolves; Again slowly to its ammoniacal liquor adding 3 ~ 5mL until solution clarification;
2. above-mentioned solution is transferred in thermostat water bath, keep taking out after 30 ~ 90 minutes at 60 ~ 90 DEG C, naturally cool to the precipitate with deionized water that generates and ethanol repeatedly eccentric cleaning after room temperature, then calcine 1 ~ 2 hour at 400 ~ 500 DEG C again after at room temperature drying, thus obtain the ZnO nano pollen end assembled by ZnO nano particle;
(2) preparation of NiO/ZnO heterogeneous structural nano flower
1. getting 30 ~ 50mg above-mentioned ZnO nano pollen end joins in 5 ~ 10mL ethanol, ultrasonic and stir and within 10 ~ 30 minutes, make ZnO nano pollen end disperse completely in ethanol; And then add 8 ~ 10mgNi (NO
3)
26H
2o, is at room temperature stirred to ethanol and is substantially evaporated completely complete;
2. above-mentioned dried powder collected and calcining 2 ~ 4 hours at 500 ~ 550 DEG C, thus obtain with ZnO nano flower be trunk, NiO nano particle is evenly attached to the NiO/ZnO heterogeneous structural nano pollen end on ZnO surface.
2. the preparation method of a kind of acetone gas sensor based on NiO/ZnO heterogeneous structural nano flower sensitive material according to claim 1, its step is as follows:
1. by NiO/ZnO heterogeneous structural nano pollen end with deionized water in mass ratio 3 ~ 5:1 mix, and grind formation pasty slurry, then dip a small amount of slurry and be coated in the Al that outside surface carries 2 annular gold electrodes equably
2o
3ceramic pipe surface, forms 10 ~ 30 μm of thick sensitive material films, and makes sensitive material cover annular gold electrode completely;
2. toast 30 ~ 45 minutes under infrared lamp, after sensitive material drying, Al
2o
3ceramic pipe is calcined 2 ~ 3 hours at 400 ~ 450 DEG C; Then be that the NI-G heater coil of 30 ~ 40 Ω is through Al by resistance value
2o
3above-mentioned device, as heater strip, finally carries out welding and encapsulating according to general heater-type gas sensor by ceramic tube inside, thus obtains the acetone gas sensor based on NiO/ZnO heterogeneous structural nano flower sensitive material.
3. a kind of preparation method of acetone gas sensor based on NiO/ZnO heterogeneous structural nano flower sensitive material as claimed in claim 2, is characterized in that: the length of ceramic pipe is 4 ~ 4.5mm, and external diameter is 1.2 ~ 1.5mm, and internal diameter is 0.8 ~ 1.0mm.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124573A (en) * | 2016-06-20 | 2016-11-16 | 吉林大学 | A kind of acetone gas sensor based on NiO/ZnO heterojunction structure hollow ball sensitive material and preparation method thereof |
| CN106814113A (en) * | 2017-03-02 | 2017-06-09 | 吉林大学 | A kind of H based on ZnO/CuO heterojunction structure nano materials2Sensor and preparation method thereof |
| CN108152338A (en) * | 2017-12-26 | 2018-06-12 | 吉林大学 | Based on Sn of equal value2+Dimethylbenzene gas sensor of NiO nano flower-like microballoons of gap doping and preparation method thereof |
| CN108828025A (en) * | 2018-06-22 | 2018-11-16 | 吉林大学 | One kind being based on hollow CdFe2O4The acetone gas sensor and preparation method thereof of nanocages sensitive material |
| CN108855103A (en) * | 2018-06-01 | 2018-11-23 | 安徽建筑大学 | A kind of compound and preparation method thereof of ZnO rose bouquet load nano NiO |
| CN108872324A (en) * | 2018-05-16 | 2018-11-23 | 吉林大学 | One kind being based on NiO/NiCr2O4Dimethylbenzene gas sensor of nano combined sensitive material and preparation method thereof |
| CN109001264A (en) * | 2018-06-22 | 2018-12-14 | 吉林大学 | One kind being based on porous C uFe2O4The acetone gas sensor and preparation method thereof of microballoon sensitive material |
| CN110596196A (en) * | 2019-09-16 | 2019-12-20 | 山东大学 | Semiconductor heterojunction gas sensitive material and preparation method and application thereof |
| CN111551592A (en) * | 2020-06-18 | 2020-08-18 | 吉林大学 | NiO/Zn based on octahedral structure2SnO4Acetone gas sensor of composite sensitive material and preparation method thereof |
| CN111579600A (en) * | 2020-06-28 | 2020-08-25 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO2Composite material and preparation method and application thereof |
| CN111610234A (en) * | 2020-07-07 | 2020-09-01 | 上海大学 | Acetone gas sensor of field effect transistor and preparation method thereof |
| CN112129823A (en) * | 2020-09-13 | 2020-12-25 | 中国海洋大学 | Ni @ NiO @ ZnO @ CS composite metal wire for copper ion detection and preparation method and application thereof |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
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| CN109001264A (en) * | 2018-06-22 | 2018-12-14 | 吉林大学 | One kind being based on porous C uFe2O4The acetone gas sensor and preparation method thereof of microballoon sensitive material |
| CN110596196A (en) * | 2019-09-16 | 2019-12-20 | 山东大学 | Semiconductor heterojunction gas sensitive material and preparation method and application thereof |
| CN111551592A (en) * | 2020-06-18 | 2020-08-18 | 吉林大学 | NiO/Zn based on octahedral structure2SnO4Acetone gas sensor of composite sensitive material and preparation method thereof |
| CN111579600A (en) * | 2020-06-28 | 2020-08-25 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO2Composite material and preparation method and application thereof |
| CN111579600B (en) * | 2020-06-28 | 2022-11-22 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO 2 Composite material and preparation method and application thereof |
| CN111610234A (en) * | 2020-07-07 | 2020-09-01 | 上海大学 | Acetone gas sensor of field effect transistor and preparation method thereof |
| CN111610234B (en) * | 2020-07-07 | 2021-09-07 | 上海大学 | Acetone gas sensor of field effect transistor and preparation method thereof |
| CN112129823A (en) * | 2020-09-13 | 2020-12-25 | 中国海洋大学 | Ni @ NiO @ ZnO @ CS composite metal wire for copper ion detection and preparation method and application thereof |
| CN112129823B (en) * | 2020-09-13 | 2022-04-08 | 中国海洋大学 | Preparation method of Ni @ NiO @ ZnO @ CS composite metal wire for copper ion detection |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
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Application publication date: 20160504 |