CN106841326B - The zinc oxide of a kind of pair of alcohol sensible-cobalt oxide hollow nano polyhedron film - Google Patents
The zinc oxide of a kind of pair of alcohol sensible-cobalt oxide hollow nano polyhedron film Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- 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
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention provides a kind of zinc oxide that can be used for detecting ethyl alcohol-cobalt oxide hollow nano polyhedron film preparation methods, belong to gas sensor technology field.Zinc nitrate hexahydrate and cobalt nitrate hexahydrate are mixed in a certain proportion by we, are prepared for zinc oxide-oxidation cobalt precursor by template, subsequently heat-treated to obtain zinc oxide-cobalt oxide hollow polyhedron, then are prepared into membrane module by silk screen print method.In adulterated range (molar ratio of zinc oxide and cobalt oxide is respectively 0,0.5mol%, 2mol% and 4mol%), 2mol% is optimum doping.Within the scope of measured temperature (100-300 DEG C), for 2mol%ZnO-Co3O4And 4mol%ZnO-Co3O4, optimum working temperature is reduced to 200 DEG C.2mol%ZnO-Co3O4To the high sensitivity of 1000ppm ethyl alcohol up to 106 at 200 DEG C, response/recovery time is 7/236 second.This sensor film preparation method is simple, and cost of material is low, and material membrane is had excellent performance, favorable repeatability, has good application value and prospect.
Description
Technical field
The invention belongs to gas sensor technology fields, and in particular to a kind of Zinc oxide doped cobalt oxide (ZnO-Co3O4) receive
Rice hollow polyhedron film preparing and its studying the air-sensitive performance of ethyl alcohol.
Background technique
Ethyl alcohol (ethanol) is a kind of colourless volatile liquid, a kind of excellent organic solvent.As a kind of important work
Industry raw material and disinfectant, ethyl alcohol are not only widely used in the fields such as food industry, daily-use chemical industry and health care, and in petroleum
Alternative aspect has good development prospect.Since ethyl alcohol smell is fragrant and sweet, the drink and food containing ethyl alcohol is more and more at present,
China is especially in the majority with drinks.The illegal accident driven when intoxicated increases increasingly, this proposes the dynamics and level of traffic administration
New requirement.Although ethyl alcohol itself is to human body and non-hazardous, if people will go out in the environment containing alcohol vapour for a long time
The symptoms such as now headache, sleepy, eye pain, expiratory dyspnea.Therefore the concentration for quick and precisely detecting ethyl alcohol has very important reality
Meaning and practical value.
Solid state resistance type metal oxide semiconductor gas sensor is widely used in medical diagnosis, air quality prison
The fields such as survey, the detection of Food processing, toxic gas.Cobalt oxide (Co3O4) it is a kind of very typical p-type semiconductor, prohibit
Bandwidth is 1.6-2.2eV.Co3O4Have very strong oxygen adsorption capacity, is primarily due to divalent Co2+It is higher for being oxidized easily
The Co ion of valence state, this property make Co3O4A kind of gas sensitive as great potential.Regrettably, using single
Co3O4Some shortcomings are still had for gas detection, such as operating temperature height, sensitivity is low, and response restores slow etc..These problems master
Want to solve by two schemes: 1) pattern and micro-structure of controlled material such as prepares hollow structure, and three-dimensional structure etc. is to enhance
The specific surface area of material；2) by being compounded to form p-n heterojunction.Due to having at low cost, chemical stability is good, is easy to adulterate etc.
Advantage, zinc oxide (ZnO) is often used to and Co3O4In conjunction with formation composite air-sensitive material.For example, Lee seminar uses thermal evaporation
By Co3O4On particle modification to ZnO nano-wire, and have studied its to the response of nitrogen dioxide and ethyl alcohol (Chem.Commun,
2011,47,5148).Liu et al. people is prepared for ZnO/Co3O4Complex microsphere structure, and compared this composite construction and single-phase ZnO
Structure is to the response of ethyl alcohol (Sens.Actuators B:Chem., 2015,221,1492).Yuan et al. uses wet-chemical route
It is prepared for the Co of ZnO modification3O4Composite construction, research shows that the structure is substantially better than pure ZnO to the air-sensitive performance of ethyl alcohol and formaldehyde
(Appl.Surf.Sci.,2013,265,379).Two step plasma enhanced chemical vapor depositions of Gasparotto seminar
Method (PECVD) is prepared for Co3O4/ ZnO composite construction, and have studied its air-sensitive performance to acetone, ethyl alcohol and nitrogen dioxide
(ACS Appl.Mater.Inter.,2012,4,928).Therefore, for theoretically, by by ZnO and Co3O4It is compound, it can be significant
Promote the air-sensitive performance of sensor.
Hollow structure can be prepared by various templates, and template is removed by subsequent chemistry corrosion or calcination method again
It goes.Common template mainly has: colloidal particle, carbon ball, emulsion micelles, bubble etc..In recent years, due to having high specific surface area
And porosity, metallorganic frame (MOFs) are considered as the ideal template for preparing hollow structure.On the one hand, using MOFs mould
The hollow structure of plate preparation remains the pattern of presoma；On the other hand, the hollow structure distribution of pores prepared with MOFs template
It is highly uniform.More importantly being typically all spherical shape using the hollow structure of conventional template method preparation, it is very easy to reunite.
And aspherical hollow structure can be prepared using MOFs template, effectively prevent particle agglomeration.So far, using MOFs mould
Plate has had been successfully prepared the number of other, non-spherical shapes such as micro- cell type, nanometer cage modle, nanometer spill cubic block, nanometer dodecahedron.
As far as we know, when constructing hetero-junctions, most documents are all reported using n-type semiconductor as main material, are used
P-type semiconductor carrys out doping vario-property, because studies have shown that, typically the gas sensing property of n-type semiconductor is greater than p-type semiconductor.But
It is that the potential value of p-type semiconductor can not be ignored, most of p-type semiconductor all has very strong catalytic capability, to very much
The oxidation rate of gas especially volatile organic matter (VOCs) is quickly.Therefore, with Co3O4Based on material, study different proportion
Influence of the ZnO doping to its air-sensitive performance be highly desirable.
To realize highly sensitive, the quick detection to ethyl alcohol, we use MOFs to be prepared for pure Co for template3O4It is mixed with difference
The ZnO-Co of miscellaneous ratio3O4Then hollow nano polyhedral structure prepares membrane module, and system research using silk screen print method
The influence to alcohol sensible performance such as operating temperature, doping ratio.The hollow polyhedron structure preparation method is simple, cost of material
Low, favorable repeatability can be right based on the sensor of the structure is to ethyl alcohol high sensitivity and response recovery time is short, selectivity is high
The concentration of alcohol (1-1000ppm) of larger atmosphere is detected, and has good application value and prospect.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of sensor film for detecting ethyl alcohol.It is prepared by template pure
Co3O4And ZnO-Co3O4Hollow nano polyhedral structure, then prepared and formed a film by silk screen print method.The preparation method have at
The features such as this is cheap, simple, convenient quick.
Below with cobalt nitrate hexahydrate (Co (NO3)2·6H2O realization process of the invention is briefly explained for).It uses first
Template and heat treating process prepare ZnO-Co3O4Hollow nano polyhedral structure by suitable hollow nano polyhedron powder and is gone
Ionized water is screen printed onto after mixing on the potsherd for being printed on platinum electrode, is placed it in drying box after waiting films dry,
It is taken out after being handled 2 hours at 100 DEG C, obtains test substrate.The ZnO-Co3O4Hollow nano polyhedron film can be by detail below
Step is realized:
(1) a certain amount of 2-methylimidazole is dissolved in suitable methanol, persistently stirred 5 minutes；
(2) it is dissolved in proper amount of methanol after mixing a certain amount of zinc nitrate hexahydrate with certain proportion and cobalt nitrate hexahydrate, will be walked
Suddenly the mixed liquor of (1) and the mixed liquor of step (2) are mixed and stirred for 10 minutes；
(3) above-mentioned mixed liquor is stood 20 hours at room temperature, is then carried out respectively with deionized water and dehydrated alcohol more
Secondary centrifuge washing, will be dry at the purple sample after centrifuge washing in a vacuum drying oven 80 DEG C, obtains ZnO-Co3O4Presoma；
(4) above-mentioned precursor powder is placed in tube furnace and is handled 3 hours at 300 DEG C, the heating rate of tube furnace
It is 2 DEG C/min, finally obtains ZnO-Co3O4Hollow nano polyhedron powder；
(5) it takes appropriate above-mentioned powder to be dissolved in deionized water and stir, forms it into uniform dope, then use screen printing
Brush technology prints to the dope on the potsherd of platinum electrode, after waiting films to be completely dried, places it in drying box 2 hours,
Drying box temperature setting is 100 DEG C, finally obtains test substrate.
It can be obtained the ZnO-Co of different doping ratios by the above process3O4(ZnO and Co3O4Molar ratio be respectively 0,
0.5%, 2% and 4%, it is denoted as 0,0.5mol%, 2mol% and 4mol%).Comparison 100 DEG C, 150 DEG C, 200 DEG C, 250 DEG C,
300 DEG C of operating conditions are found for pure Co3O4And 0.5mol%ZnO-Co3O4, 250 DEG C are optimum working temperature, and for
2mol%ZnO-Co3O4And 4mol%ZnO-Co3O4, optimum working temperature is reduced to 200 DEG C.In addition to this, all material pair
The response recovery time of 1000ppm ethanol is reduced with the increase of operating temperature.Meanwhile research shows that difference is mixed
The ZnO-Co of miscellaneous ratio3O4, no matter for which kind of temperature (100-150 DEG C), optimum doping amount is 2mol%.Pass through research 200
2mol%ZnO-Co at DEG C3O4Response to different ethanol concentration (1-1000ppm), increase of the discovery with concentration of alcohol, sensing
Device is in exponential increase to the sensitivity of ethyl alcohol, is not saturated in surveyed concentration range.2mol% is repeatedly tested at 200 DEG C
ZnO-Co3O4Response to 1000ppm ethyl alcohol finds the repeatability of material and has good stability.
ZnO-Co provided by the present invention3O4The preparation method of hollow nano polyhedron film, it can be achieved that ethyl alcohol it is quick,
Accurate detection.This method preparation is simple, and cost of material is low, favorable repeatability, has good application value and prospect.
Detailed description of the invention
Fig. 1 is ZnO-Co3O4The preparation flow figure of hollow nano polyhedron membrane module.
Fig. 2 (a) is pure Co3O4And 0.5mol%, 2mol% and 4mol%ZnO-Co3O4Spirit to 1000ppm ethanol
Sensitivity varies with temperature curve graph, and Fig. 2 (b) is 2mol%ZnO-Co3O4To response/recovery time of 1000ppm ethanol with
Temperature changing curve diagram.
Fig. 3 (a) and 3 (b) is respectively 2mol%ZnO-Co at 200 DEG C3O4The resistance of hollow nano polyhedron film and sensitive
Degree is with various concentration ethanol on-off gas change curve (illustration 2mol%ZnO-Co3O4Resistance with 1ppm ethanol
On-off gas change curve).
Fig. 4 is 2mol%ZnO-Co at 200 DEG C3O4Repeatability of the hollow nano polyhedron film to 1000ppm ethanol
Test curve figure.
Specific embodiment
Carry out the present invention is described in detail with reference to the accompanying drawings and examples.
1.97 grams of 2-methylimidazoles are dissolved in 40 ml methanols by embodiment 1, are persistently stirred 5 minutes.By 1.746 gram of six water
Cobalt nitrate and 0.036 gram of zinc nitrate hexahydrate (ZnO and Co3O4Molar ratio be 2mol%) mixing after be dissolved in 20 ml methanols, by this
Mixed liquor and above-mentioned 2-methylimidazole mixed liquor are mixed and stirred for 10 minutes, it is finally stood 20 hours at room temperature.It stands
After mixed liquor is subjected to multiple centrifuge washing with deionized water and dehydrated alcohol respectively, the purple sample after centrifugation is in vacuum
It is dry at 80 DEG C in drying box, obtain ZnO-Co3O4Presoma.Above-mentioned precursor powder is placed in tube furnace at 300 DEG C and is handled
3 hours, the heating rate of tube furnace was 2 DEG C/min, obtained ZnO-Co3O4Hollow nano polyhedron powder.Take appropriate above-mentioned powder
End is dissolved in deionized water and stirs, and forms it into uniform dope, and then the dope has been printed to screen printing technique
On the potsherd of platinum electrode, after waiting films to be completely dried, placing it in drying box 2 hours, drying box temperature setting is 100 DEG C,
Test substrate is finally obtained, the preparation flow of the thin-film device is as shown in Figure 1.
Transducer sensitivity calculation method: S=Ra/Rg.Wherein, RaFor resistance of the sensor under specific concentration of alcohol, Rg
For the resistance of sensor in air atmosphere.It, respectively will at 100-300 DEG C for research optimum working temperature and optimum doping amount
Pure Co3O4With the ZnO-Co of different proportion doping3O4The sound of (0.5mol%, 2mol%, 4mol%) to 1000ppm ethanol
It should be compared, as shown in Fig. 2 (a).It is found that for pure Co3O4And 0.5mol%ZnO-Co3O4, 250 DEG C are best effort
Temperature, and for 2mol%ZnO-Co3O4And 4mol%ZnO-Co3O4, optimum working temperature is reduced to 200 DEG C.It is also known by figure,
Optimum doping ratio is 2mol%.2mol%ZnO-Co3O4Pure Co is compared to the sensitivity of 1000ppm ethanol3O4It improves
Nearly 18.7 times.The response time of sensor is defined as: since when contacting with certain density tested gas, reach this to resistance value
Under concentration the time required to the 90% of stable state resistance value；Recovery time is defined as: since when being detached from certain density tested gas,
The time required to restored variation resistance value to resistance value 90%.Fig. 2 (b) is 2mol%ZnO-Co3O4To 1000ppm ethanol's
Response/recovery time varies with temperature curve graph.As shown, the response recovery time of sensor is held as the temperature increases
Continuous decline.At 200 DEG C, 2mol%ZnO-Co3O4Response/recovery time be 7/236 second.It is rung in general, operating temperature increases
It answers resume speed to increase, but certain sensitivity can be sacrificed.When comprehensively considering energy consumption, transducer sensitivity, response recovery
Between, the factors such as stability, we select 200 DEG C as optimum controlling condition, and follow-up test all carries out at this temperature.
Fig. 3 (a) is 2mol%ZnO-Co3O4The resistance of hollow polyhedron film changes bent with various concentration ethanol on-off gas
Line chart, illustration 2mol%ZnO-Co3O4Resistance with 1ppm ethanol on-off gas change curve, as seen from the figure, sensor
Preferable response recovery curve is also showed that 1ppm ethanol, sensitivity is about 1.57.Fig. 3 (b) is 2mol% ZnO-
Co3O4To the sensitivity of ethanol with ethanol concentration curve figure, as seen from the figure, within the scope of 1-1000ppm, with
The increase of ethanol concentration, 2mol%ZnO-Co3O4Sensitivity it is in exponential increase.
Fig. 4 is 2mol%ZnO-Co at 200 DEG C3O4Reperformance test of the hollow polyhedron film to 1000ppm ethanol
Curve graph.As seen from the figure, in 6 circulations surveyed, the sensitivity of material does not change substantially, and every time can after test
It is restored to baseline state, illustrates that the repeatability of material and consistency are good.
Claims (1)
1. the ZnO-Co of a kind of pair of alcohol sensible3O4The preparation method of hollow nano polyhedron film, preparation step include:
(1) a certain amount of 2-methylimidazole is dissolved in suitable methanol, persistently stirred 5 minutes；
(2) it is dissolved in proper amount of methanol after mixing a certain amount of zinc nitrate hexahydrate with certain proportion and cobalt nitrate hexahydrate, by step (1)
Mixed liquor and the mixed liquor of step (2) be mixed and stirred for 10 minutes；
(3) above-mentioned mixed liquor is stood 20 hours at room temperature, then respectively with deionized water and dehydrated alcohol carry out repeatedly from
Heart washing, will be dry at the purple sample after centrifuge washing in a vacuum drying oven 80 DEG C, obtains ZnO-Co3O4Presoma；
(4) above-mentioned precursor powder being placed in tube furnace and is handled 3 hours at 300 DEG C, the heating rate of tube furnace is 2 DEG C/
Minute, finally obtain ZnO-Co3O4Hollow polyhedron powder；
(5) it takes appropriate above-mentioned powder to be dissolved in deionized water and stir, forms it into uniform dope, then use silk-screen printing skill
Art prints to the dope on the potsherd of platinum electrode, after waiting films to be completely dried, places it in drying box 2 hours, dry
Box temperature degree is set as 100 DEG C, finally obtains test substrate.
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| CN107610940A (en) * | 2017-09-20 | 2018-01-19 | 安阳师范学院 | Hollow polyhedral cobaltosic oxide ceria composite oxide material and its preparation method and application |
| CN108107085A (en) * | 2017-12-11 | 2018-06-01 | 何旭连 | A kind of portable ethyl alcohol detection device |
| JP6337193B1 (en) | 2017-12-14 | 2018-06-06 | 株式会社ドワンゴ | Server and program |
| CN109459470A (en) * | 2018-11-27 | 2019-03-12 | 中国石油大学(华东) | Palladium/cobaltosic oxide-the graphene film sensitive to extremely low concentration acetone under a kind of lower temperature |
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| CN109678214B (en) * | 2019-01-11 | 2021-03-09 | 中国石油大学(华东) | Acetone-sensitive cobaltosic oxide/indium oxide nanotube composite film |
| CN110323425B (en) * | 2019-06-24 | 2021-04-06 | 华南师范大学 | Hollow flaky zinc oxide/cobaltosic oxide heterojunction, electrode, lithium ion battery and preparation method thereof |
| CN110749628A (en) * | 2019-10-25 | 2020-02-04 | 中国石油大学(华东) | Acetone-sensitive cobaltosic oxide/zinc oxide nano-meter rice heterojunction thin film |
| CN110736771B (en) * | 2019-10-25 | 2022-10-11 | 中国石油大学(华东) | Zinc oxide/cobaltosic oxide heterojunction film sensitive to low-concentration acetone |
| CN113125521B (en) * | 2021-04-26 | 2022-05-27 | 中国石油大学(华东) | Preparation method of molybdenum disulfide/cerium oxide composite gas-sensitive structure and application of molybdenum disulfide/cerium oxide composite gas-sensitive structure in gas-sensitive coating, element and sensor |
| CN113713725B (en) * | 2021-09-03 | 2023-11-21 | 杭州恒毅智创科技有限公司 | Preparation method of hollow core-shell cube zinc oxide/cobaltosic oxide/zinc oxide nanocomposite |
| CN113670993B (en) * | 2021-09-08 | 2023-03-17 | 大连理工大学 | Composite gas-sensitive material with hierarchical structure and preparation method and application thereof |
| CN113740391B (en) * | 2021-09-26 | 2023-12-05 | 河北工业大学 | MOF-derived NiO-Co 3 O 4 Preparation method of acetone gas sensor |
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