CN106970116A - A kind of polyhedral cobaltosic oxide three-dimensional porous Graphene gel composite material film sensitive to acetone - Google Patents
A kind of polyhedral cobaltosic oxide three-dimensional porous Graphene gel composite material film sensitive to acetone 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
Abstract
The invention provides a kind of preparation method that can be used for detecting the three-dimensional porous Graphene gel composite sensor film of polyhedral cobaltosic oxide of acetone, belong to gas sensor technology field.The metal-organic framework material of the three-dimensional porous Graphene gel of preparation and cobalt-based by the three-dimensional porous Graphene gel of Hydrothermal Synthesiss, is then combined first, composite is finally thermally treated resulting in polyhedral CO under air by we3O4With the composite of three-dimensional porous Graphene gel, cladding process is recycled to prepare film forming, for acetone sensing detection.The composite material film can detect the acetone of various concentrations, in air atmosphere to 50ppm CO2Factor of merit be up to 81.2 (Rgas/R0).This preparation method is simple, and the cost of raw material is cheap, favorable repeatability, material membrane excellent performance, with good application value and prospect.
Description
Technical field
The invention belongs to gas sensor technology field, and in particular to a kind of polyhedron-shaped cobaltosic oxide and three-dimensional
The preparation of porous graphene gel complex material film and its air-sensitive performance research to acetone.
Background technology
With continuing to develop for human society, the continuous discharge of toxic and harmful gas causes atmospheric environment to receive different journeys
The pollution of degree, and the presence of this toxic and harmful gas seriously threatens the health of human body.Therefore, to toxic and harmful gas
Detection of the detection for environmental quality and personal security's protection play an important role.Acetone (CH3COCH3) it is organic
One kind of gas, the life with the mankind is closely bound up.On the one hand, acetone is laboratory and industrial production workshop is most-often used has
One of machine reagent.Suck suppression, anesthetic effect that substantial amounts of acetone can be produced to human central nervous system, high concentration contact
The liver of people, kidney and pancreas can be caused damage.On the other hand, the concentration of acetone will significantly larger than just in the expiratory air of diabetes patient
Acetone concentration in ordinary person's expiratory air.Therefore, the concentration acetone of acetone is diagnosis diabetes patient again in the expiratory air of detection people
A kind of important references standard.
It is presently used for detecting that the sensing material species of acetone gas concentration is various.And the metal oxide materials of semiconductor
Because it has the advantages that with low cost, sensitivity is high, response replys very fast, and the preparation technology of its product is simple, operation side
Just, one of current acetone sensitive material widely used in the world is had become.Cobaltosic oxide (Co3O4) it is a kind of non-
Normal typical P-type semiconductor, its energy gap is 1.6-2.2eV.Co3O4Possess very strong oxygen adsorption capacity, and studied
Show that it has excellent acetone sensitive property.And use single Co3O4Still come with some shortcomings for acetone detection, such as work
Make temperature high, sensitivity is low, response recovers slow etc..These problems can mainly be solved by two schemes:1) shape of controlled material
Looks and micro-structural, such as prepare hollow structure, and three-dimensional structure etc. is with the specific surface area of reinforcing material.For example, Xu et al. utilizes microwave
Assisting alcohol-hydrothermal method is prepared for intimate monodispersed Co3O4Nanocube structure, and have studied multiple organic including acetone
Sensitive property (the Sens.Actuators B of gas:2011,157,681).The water that Wang et al. is aided in using surfactant
Hot preparation method has synthesized Co3O4Hollow nanospheres, test result indicates that, the Co with semiconductor property3O4Hollow nanometer is micro-
Ball has larger lifting (Sens.Actuators B to the sensitive property of acetone:2009,136,494).2) by with other
Semiconductors coupling formation p-n heterojunction.And this compound often possess that cost is low, chemical stability is good, it is excellent to be easy to doping etc.
Point, easily forms compound gas sensitive.For example, Luo et al. is prepared for SnO using the method for electrostatic spinning2Adulterate Co3O4In
Empty nanotube structure.Itself test result indicates that, with intrinsic Co3O4Compare, this structure shows higher sensitivity to acetone
Characteristic, lower detection temperature and response (RSC.Adv.2014,108,62862) faster.Ji et al. is prepared using two-step method
Co3O4-WO3Hetero-junctions nanostructured, and its sensitive property to acetone is have studied, find the heterojunction structure than pure WO3
Sensor shows more preferable sensitivity characteristic to acetone.
In addition, since being found from graphene, because it has extremely excellent electrical properties, widely should have been used for
For every field.Therefore, the design of acetone sensor is except building oxide heterojunction, by graphene and the compound use of oxide
The concern of increasing researcher is also result in the detection of acetone.For example, Il-Doo Kim et al. two-step thermal processings
Method is prepared for one-dimensional many sky WO with needle-like branch3It, is then further combined by fiber with graphene nanometer sheet, and grinds
Sensitivity characteristic of the composite construction to acetone is studied carefully.Test result indicates that, the structure has larger to the sensitive property of acetone
Lifted (RSC.Adv.2014,10,7584).
In order to realize highly sensitive, quick detection to acetone gas, we use thermally decomposable metal organic frame (MOFs)
With three-dimensional porous Graphene gel polyhedral CO is prepared for the composite of presoma3O4With three-dimensional porous Graphene gel
Composite, be then prepared for Sensitive Apparatus using cladding process, and system research operating temperature is quick to the acetone of various concentrations
The influence of perceptual energy.The composite material and preparation method thereof is simple, and cost of material is low, favorable repeatability, the sensor based on the structure
It is high to acetone sensitivity and response recovery time is short, with good application value and prospect.
The content of the invention
Detect different dense under different temperatures test scope, using air as background gas it is an object of the invention to provide one kind
Spend the preparation method of the sensor film of acetone.MOFs and three-dimensional porous Graphene gel are prepared for using simply self-assembling method
Composite, polyhedral CO is then prepared by thermally decomposing MOFs3O4With the composite wood of three-dimensional porous Graphene gel
Material, film forming is prepared by cladding process.The features such as preparation method has with low cost, convenient and simple for operation quick.
Below with cobalt nitrate hexahydrate (Co (NO3)2·6H2The implementation process of the present invention is briefly explained exemplified by O.First using letter
Single ground hydrothermal method prepares three-dimensional many empty graphene hydrogels, then prepares polyhedral using self assembly and heat treatment method
CO3O4With the composite of three-dimensional porous Graphene gel, it is coated in after appropriate composite is well mixed with absolute ethyl alcohol
In interdigital electrode, afterwards dry some minutes obtain one layer of uniform film.Above-mentioned sample is placed in drying box, located at 80 DEG C
Reason is taken out after 2 hours, obtains testing substrate, and test substrate is put into clean environment and preserved, and waits follow-up electrical properties test.
Polyhedral CO3O4It can be realized with the composite material film of three-dimensional porous Graphene gel by step in detail below：
(1) a certain amount of graphene oxide is added in a certain amount of deionized water, first ultrasonic some minutes, added
A certain amount of hydroquinones and under ceaselessly magnetic agitation, makes it be uniformly dispersed；
(2) it is the poly- of the autoclave of 50 milliliters of stainless steels the graphene oxide dispersion in (1) to be added into volume
In tetrafluoroethene liner, and it is sealed against, liner is fitted into stainless steel casing sealed afterwards；
(3) autoclave of good seal is put into air dry oven, suitable reaction time and reaction temperature is set
Degree, after reaction terminates, allows it to naturally cool to room temperature；
(4) reaction product is collected by centrifugation, is washed respectively with deionized water and absolute ethyl alcohol several times, by the product after centrifugation
It is freeze-dried in freeze drier, it is three-dimensional porous Graphene gel that product is collected afterwards；
(5) a certain amount of cobalt nitrate hexahydrate and 2-methylimidazole are added separately in a certain amount of deionized water, not
Under the magnetic agitation stopped, it is completely dissolved it；
(6) the three-dimensional porous Graphene gel prepared in a certain amount of (4) is added in the lysate of cobalt nitrate, magnetic force is stirred
Mix some time；
(7) mixed liquor of cobalt nitrate and graphene is added rapidly in the lysate of 2-methylimidazole, in magnetic agitation
Under continue six hours；
(8) reaction product is collected by centrifugation, is washed respectively with deionized water and absolute ethyl alcohol several times, by the product after centrifugation
80 DEG C of dryings 24 hours in drying box；
(9) product obtained after drying is put into quartz boat, be heat-treated in airtight tube type stove under certain temperature some
Hour；
(10) it is coated in interdigital electrode, is obtained most after taking appropriate heat treatment gained sample and absolute ethyl alcohol grinding uniform
Whole testing sample, test substrate is put into clean environment and preserved, and waits follow-up electrical properties test.
Polyhedral structure CO can be obtained by said process3O4With the composite material film of three-dimensional porous Graphene gel.In air
The sensitivity of 25ppm acetone at 190-280 DEG C is tested for background gas.Test result shows that the membrane material has at 250 DEG C
Highest sensitivity and stable response recovery curve.At 250 DEG C, by background gas of air to 1-50ppm acetone table
Reveal fabulous stable response characteristic and being continuously increased with acetone concentration, Sensitirity va1ue is consequently increased.
It is provided by the present invention to prepare polyhedral CO3O4With the method for the composite material film of three-dimensional porous Graphene gel,
It may be implemented under air background, the acetone of low concentration to high concentration is detected.The preparation method is simple, and low raw-material cost can be weighed
Renaturation is good, and practicality is high, with good application value and prospect.
Brief description of the drawings
Fig. 1 is that test sample prepares schematic diagram.
Fig. 2 is to vary with temperature curve map to the sensitivity of 25ppm acetone under different temperatures under air background gas.
Fig. 3 is to the sensitivity response return curve figure of 25ppm acetone at lower 250 DEG C of air background gas.
Fig. 4 be 250 DEG C of air background at, to 1-50ppm acetone change of sensitivity curves and response return curve figure.
Embodiment
It is described in detail the present invention with reference to the accompanying drawings and examples.
Embodiment 1, a certain amount of graphene oxide is added in a certain amount of deionized water, first ultrasonic some minutes,
Add a certain amount of hydroquinones and under ceaselessly magnetic agitation, make its dispersed；By graphene oxide dispersion
It is added in polytetrafluoroethyllining lining of the volume for the autoclave of 50 milliliters of stainless steels, and is sealed against；By good seal
Autoclave is put into air dry oven, setting suitable reaction time and reaction temperature, after reaction terminates, and allows it certainly
So it is cooled to room temperature；Reaction product is collected by centrifugation, is washed respectively with deionized water and absolute ethyl alcohol several times, by the production after centrifugation
Thing is freeze-dried in freeze drier, and it is three-dimensional porous Graphene gel that product is collected afterwards；By a certain amount of six water nitric acid
Cobalt and 2-methylimidazole are added separately in a certain amount of deionized water, under ceaselessly magnetic agitation, are completely dissolved it；Will
The three-dimensional porous Graphene gel of a certain amount of preparation is added in the lysate of cobalt nitrate, the magnetic agitation some time；By nitric acid
The mixed liquor of cobalt and graphene is added rapidly in the lysate of 2-methylimidazole, continues six hours under magnetic stirring；Centrifugation
Collecting reaction product, is washed with deionized water and absolute ethyl alcohol several times, by the product after centrifugation 80 DEG C in drying box respectively
Dry 24 hours；The product obtained after drying is put into quartz boat, is heat-treated in airtight tube type stove under certain temperature some
Hour；It is coated in after taking appropriate heat treatment gained sample and absolute ethyl alcohol grinding uniform in interdigital electrode, obtains final to be measured
Sample, test substrate is put into clean environment and preserved, and waits follow-up electrical properties test.Its process is as shown in Figure 1.
Fig. 2 gives air to vary with temperature curve to the sensitivity of 25ppm acetone under background gas, different temperatures
Figure.It can be seen that in the range of measured temperature, sensitivity highest of the composite material film to 25ppm at 250 DEG C.
Fig. 3 gives air for background gas, dynamic response of the composite membrane to the sensitivity of 25ppm acetone at 250 DEG C
Return curve figure.It can be seen that air and for background gas, at 250 DEG C the composite membrane 25ppm acetone is respectively provided with well,
Stable response recovery cycles curve, i.e., in air background after the resistance baseline balance of material, be passed through on acetone material resistance
Rise, stopping, which is passed through material after acetone, can return to initial resistance quickly.
Fig. 4 is given in air at 250 DEG C, to 1-50ppm acetone dynamic response return curves and sensitivity number.From
Understood in figure, when background gas is air at 250 DEG C, material has well stable circulation to the acetone of various concentrations, with
The increase of acetone concentration, sensitivity is consequently increased.It is passed through material resistance after the acetone of low concentration to rise, stopping is passed through third
Material can return to initial resistance quickly after ketone；The resistance ascensional range for being passed through material after the acetone of high concentration again is higher than low concentration
When material resistance ascensional range, stopping be passed through after acetone, material resistance can finally return to initial resistance.
Claims (1)
1. a kind of preparation side of the polyhedron cobaltosic oxide-three-dimensional porous graphene hydrogel composite material film sensitive to acetone
Method, its preparation process includes：
(1) a certain amount of graphene oxide is added in a certain amount of deionized water, first ultrasonic some minutes, added certain
The hydroquinones of amount and under ceaselessly magnetic agitation, makes its dispersed,；
(2) graphene oxide dispersion in (1) is added to polytetrafluoro of the volume for the autoclave of 50 milliliters of stainless steels
In ethene liner, and it is sealed against；Liner is fitted into stainless steel casing afterwards and sealed
(3) autoclave of good seal is put into air dry oven, setting suitable reaction time and reaction temperature, when
After reaction terminates, it is allowed to naturally cool to room temperature；
(4) reaction product is collected by centrifugation, is washed several times with deionized water and absolute ethyl alcohol respectively, by the product after centrifugation in cold
It is freeze-dried in lyophilizer, it is three-dimensional porous Graphene gel that product is collected afterwards；
(5) a certain amount of cobalt nitrate hexahydrate and 2-methylimidazole are added separately in a certain amount of deionized water, ceaselessly
Under magnetic agitation, it is completely dissolved it；
(6) the three-dimensional porous Graphene gel prepared in a certain amount of (4) is added in the lysate of cobalt nitrate, if magnetic agitation
The dry time；
(7) mixed liquor of cobalt nitrate and graphene is added rapidly in the lysate of 2-methylimidazole, held under magnetic stirring
It is continuous six hours；
(8) reaction product is collected by centrifugation, is washed respectively with deionized water and absolute ethyl alcohol several times, by the product after centrifugation in dry
80 DEG C of dryings 24 hours in dry case；
(9) product obtained after drying is put into quartz boat, is heat-treated some hours under certain temperature in airtight tube type stove；
(10) it is coated in interdigital electrode, is finally treated after taking appropriate heat treatment gained sample and absolute ethyl alcohol grinding uniform
Test sample product, test substrate is put into clean environment and preserved, and waits follow-up electrical properties test.
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| CN108752368A (en) * | 2018-07-11 | 2018-11-06 | 郑州工程技术学院 | A kind of zinc-containing metal organic framework materials and its synthetic method and application with fluorescence identifying performance |
| CN109437329A (en) * | 2018-11-09 | 2019-03-08 | 东北大学 | A kind of Co3O4/ graphene composite material and its preparation method and application |
| 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 |
| CN109490379A (en) * | 2018-12-27 | 2019-03-19 | 中山大学 | Gas sensor and its preparation method of application, equipment and gas sensor |
| CN110006958A (en) * | 2019-04-10 | 2019-07-12 | 河北工业大学 | Co3O4The preparation method of ZnO nano material acetone thick film gas-sensitive sensor |
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| CN108752368A (en) * | 2018-07-11 | 2018-11-06 | 郑州工程技术学院 | A kind of zinc-containing metal organic framework materials and its synthetic method and application with fluorescence identifying performance |
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| 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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| CN110006958A (en) * | 2019-04-10 | 2019-07-12 | 河北工业大学 | Co3O4The preparation method of ZnO nano material acetone thick film gas-sensitive sensor |
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| CN113003603B (en) * | 2021-03-09 | 2022-05-31 | 中国石油大学(华东) | CdS/Co3O4Composite material, preparation method and application thereof in acetone gas detection under light excitation |
| CN114864294A (en) * | 2022-05-30 | 2022-08-05 | 武汉大学 | 3D printed metal organic framework derived carbon material, and preparation method and application thereof |
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