CN106970116B - The sensitive polyhedral cobaltosic oxide of a kind of pair of acetone-three-dimensional porous Graphene gel composite material film - Google Patents
The sensitive polyhedral cobaltosic oxide of a kind of pair of acetone-three-dimensional porous Graphene gel composite material film Download PDFInfo
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Abstract
The present invention provides a kind of polyhedral cobaltosic oxide that can be used for detecting acetone-three-dimensional porous Graphene gel composite material sensor film preparation methods, belong to gas sensor technology field.We pass through the three-dimensional porous Graphene gel of hydrothermal synthesis first, then that the metal-organic framework material of the three-dimensional porous Graphene gel of preparation and cobalt-based is compound, are finally heat-treated composite material under air and obtain polyhedral CO3O4With the composite material of three-dimensional porous Graphene gel, cladding process preparation film forming is recycled, acetone sensing detection is used for.The composite material film can detect the acetone of various concentration, 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, and favorable repeatability, material membrane is had excellent performance, and has good application value and prospect.
Description
Technical field
The invention belongs to gas sensor technology fields, and in particular to a kind of polyhedron-shaped cobaltosic oxide and three-dimensional
Porous graphene gel complex material film preparing and its studying the air-sensitive performance of acetone.
Background technique
With the continuous development of human society, the continuous discharge of toxic and harmful gas is so that atmospheric environment receives 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 for the detection of environmental quality and personal security protection play an important role.Acetone (CH3COCH3) it is organic
One kind of gas, it is closely bound up with the life of the mankind.On the one hand, acetone is laboratory and industrial production workshop is most-often used has
One of machine reagent.Sucking a large amount of acetone can be to inhibition, the anesthetic effect that human central nervous system generates, high concentration contact
The liver of people, kidney and pancreas can be damaged.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 for detecting acetone in the expiratory air of people is diagnosis diabetes patient again
A kind of important references standard.
Currently, the sensing material for detecting acetone gas concentration is many kinds of.And the metal oxide materials of semiconductor
Because it has many advantages, such as that low in cost, high sensitivity, response reply are very fast, and the preparation process of its product is simple, operation side
Just, have become one of current acetone sensitive material widely used in the world.Cobaltosic oxide (Co3O4) it is a kind of non-
Normal typical P-type semiconductor, forbidden bandwidth 1.6-2.2eV.Co3O4Have very strong oxygen adsorption capacity, and existing research
Show it with excellent acetone sensitive property.And use single Co3O4Some shortcomings, such as work are still had for acetone detection
Make temperature height, sensitivity is low, and response restores slow etc..These problems can mainly be solved by two schemes: 1) shape of controlled material
Looks and micro-structure 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
The sensitive property (Sens.Actuators B:2011,157,681) of gas.The water that Wang et al. is assisted using surfactant
Hot preparation method has synthesized Co3O4Hollow nanospheres, the experimental results showed that, the Co with semiconductor property3O4Hollow nanometer is micro-
Ball has biggish promoted (Sens.Actuators B:2009,136,494) to the sensitive property of acetone.2) by with other
Semiconductors coupling forms p-n heterojunction.And it is this it is compound often have at low cost, chemical stability is good, be easy to adulterate etc. it is excellent
Point, compound gas sensitive easy to form.For example, Luo et al. is prepared for SnO using the method for electrostatic spinning2Adulterate Co3O4In
Empty nanotube structure.Itself the experimental results showed that, with intrinsic Co3O4It compares, this structure shows higher sensitivity to acetone
Characteristic, lower detection temperature and faster response (RSC.Adv.2014,108,62862).Ji et al. is prepared using two-step method
Co3O4-WO3Hetero-junctions nanostructure, and its sensitive property to acetone is had studied, find the heterojunction structure than pure WO3
Sensor shows better sensitivity characteristic to acetone.
In addition, because it has extremely excellent electrical properties, having had been used for widely answering since graphene is found
For every field.Therefore, the design of acetone sensor is in addition to constructing oxide heterojunction, by graphene and the compound use of oxide
The concern of more and more researchers is also resulted in the detection of acetone.For example, Il-Doo Kim et al. two-step thermal processing
Method is prepared for one-dimensional more sky WO with needle-shaped branch3Fiber, it is then further that it is compound with graphene nanometer sheet, and grind
The composite construction has been studied carefully to the sensitivity characteristic of acetone.The experimental results showed that the structure is to the sensitive property of acetone with biggish
It is promoted (RSC.Adv.2014,10,7584).
In order to realize highly sensitive, the quick detection to acetone gas, we use thermally decomposable metal organic frame (MOFs)
Polyhedral CO is prepared with three-dimensional porous Graphene gel for the composite material of presoma3O4With three-dimensional porous Graphene gel
Then composite material is prepared for Sensitive Apparatus using cladding process, and system research operating temperature is quick to the acetone of various concentration
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
To acetone high sensitivity and response recovery time it is short, have good application value and prospect.
Summary of the invention
The object of the present invention is to provide one kind different temperatures test scope, using air as background gas under detect it is different dense
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 material, polyhedral CO is then prepared by thermal decomposition MOFs3O4With the composite wood of three-dimensional porous Graphene gel
Material is prepared by cladding process and is formed a film.The preparation method has the characteristics that low in cost, convenient and simple for operation quick.
Below with cobalt nitrate hexahydrate (Co (NO3)2·6H2Realization process of the invention is briefly explained for O.First using letter
The three-dimensional more empty graphene hydrogels of single ground hydrothermal method preparation, then prepare polyhedral using self assembly and heat treatment method
CO3O4With the composite material of three-dimensional porous Graphene gel, suitable composite material is coated in after mixing with dehydrated alcohol
In interdigital electrode, drying several minutes later obtains one layer of uniform film.Above-mentioned sample is placed in drying box, at 80 DEG C
Reason is taken out after 2 hours, obtains test substrate, and test substrate is put into clean environment and is saved, subsequent electrical properties is waited to test.
Polyhedral CO3O4It can be realized by step in detail below with the composite material film of three-dimensional porous Graphene gel:
(1) a certain amount of graphene oxide is added in a certain amount of deionized water, first ultrasound several minutes, is added
A certain amount of hydroquinone and under ceaselessly magnetic agitation, makes it be uniformly dispersed；
(2) graphene oxide dispersion in (1) is added to the poly- of autoclave that volume is 50 milliliters of stainless steels
It in tetrafluoroethene liner, and is sealed against, liner is fitted into stainless steel casing seals later；
(3) autoclave being sealed is put into air dry oven, suitable reaction time and reaction temperature is set
Degree, when after reaction, allowing its cooled to room temperature；
(4) reaction product is collected by centrifugation, is washed several times with deionized water and dehydrated alcohol respectively, by the product after centrifugation
It is freeze-dried in freeze drier, collecting product later is three-dimensional porous Graphene gel；
(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, make it completely dissolved；
(6) the three-dimensional porous Graphene gel prepared in a certain amount of (4) is added in the lysate of cobalt nitrate, magnetic force stirs
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 several times with deionized water and dehydrated alcohol respectively, by the product after centrifugation
80 DEG C drying 24 hours in drying box；
(9) product obtained after drying is put into quartz boat, is heat-treated under certain temperature in airtight tube type furnace several
Hour；
(10) it coated in interdigital electrode after taking appropriate heat treatment gained sample and dehydrated alcohol grinding uniform, obtains most
Test substrate is put into clean environment and saves, subsequent electrical properties is waited to test by whole sample to be tested.
Polyhedral structure CO can get by the above 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.It is background gas to the acetone table of 1-50ppm using air at 250 DEG C
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 detection of the acetone of low concentration to high concentration.The preparation method is simple, low raw-material cost, can weigh
Renaturation is good, and practicability is high, has good application value and prospect.
Detailed description of the invention
Fig. 1 is that test sample prepares schematic diagram.
Fig. 2 is to vary with temperature curve graph to the sensitivity of 25ppm acetone under different temperatures under air background gas.
Fig. 3 is the sensitivity response return curve figure at lower 250 DEG C of air background gas to 25ppm acetone.
Fig. 4 is at 250 DEG C of air background, to 1-50ppm acetone change of sensitivity curve and response return curve figure.
Specific embodiment
Carry out the present invention is described in detail with reference to the accompanying drawings and examples.
A certain amount of graphene oxide is added in a certain amount of deionized water by embodiment 1, first ultrasound several minutes,
It adds a certain amount of hydroquinone and under ceaselessly magnetic agitation, keeps its evenly dispersed；By graphene oxide dispersion
It is added in the polytetrafluoroethyllining lining for the autoclave that volume is 50 milliliters of stainless steels, and is sealed against；By what is be sealed
Autoclave is put into air dry oven, and suitable reaction time and reaction temperature is arranged, when after reaction, allow its from
So it is cooled to room temperature；Reaction product is collected by centrifugation, is washed several times with deionized water and dehydrated alcohol respectively, by the production after centrifugation
Object is freeze-dried in freeze drier, and collecting product later is three-dimensional porous Graphene gel；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 made it 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 several times respectively with deionized water and dehydrated alcohol, by the product after centrifugation 80 DEG C in drying box
It is 24 hours dry；The product obtained after drying is put into quartz boat, is heat-treated under certain temperature in airtight tube type furnace several
Hour；It is final to be measured coated in obtaining in interdigital electrode after taking appropriate heat treatment gained sample and dehydrated alcohol grinding uniform
Test substrate is put into clean environment and saves, subsequent electrical properties is waited to test by sample.Its process is as shown in Figure 1.
It is to vary with temperature curve to the sensitivity of 25ppm acetone under background gas, different temperatures that Fig. 2, which gives air,
Figure.It can be seen that within the scope of measured temperature, sensitivity highest of the composite material film to 25ppm at 250 DEG C.
It is background gas that Fig. 3, which gives air, 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 be background gas, at 250 DEG C the composite membrane to 25ppm acetone all have it is good,
Stable response recovery cycles curve is passed through on acetone material resistance that is, in air background after the resistance baseline balance of material
It rises, material can be restored to initial resistance quickly after stopping is passed through acetone.
Fig. 4 gives in air at 250 DEG C, to 1-50ppm acetone dynamic response return curve and sensitivity number.From
In figure it is found that when background gas is air at 250 DEG C, material has well stable circulation to the acetone of various concentration, with
The increase of acetone concentration, sensitivity be consequently increased.Material resistance rises after being passed through the acetone of low concentration, and stopping is passed through third
Material can be restored 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 acetone after, material resistance can finally return to initial resistance value.
Claims (1)
1. the sensitive polyhedral cobaltosic oxide of a kind of pair of acetone-three-dimensional porous Graphene gel composite material film preparation side
Method, preparation step include:
(1) a certain amount of graphene oxide is added in a certain amount of deionized water, first ultrasound several minutes, is added certain
The hydroquinone of amount and under ceaselessly magnetic agitation, keeps its evenly dispersed；
(2) graphene oxide dispersion in (1) is added to the polytetrafluoro for the autoclave that volume is 50 milliliters of stainless steels
In ethylene liner, and it is sealed against；Liner is fitted into stainless steel casing later and is sealed；
(3) autoclave being sealed is put into air dry oven, suitable reaction time and reaction temperature is set, when anti-
After answering, its cooled to room temperature is allowed；
(4) reaction product is collected by centrifugation, is washed several times with deionized water and dehydrated alcohol respectively, by the product after centrifugation in cold
It is freeze-dried in lyophilizer, collecting product later is three-dimensional porous Graphene gel；
(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, make it completely dissolved；
(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, is held under magnetic stirring
It is six hours continuous；
(8) reaction product is collected by centrifugation, is washed several times with deionized water and dehydrated alcohol respectively, by the product after centrifugation in dry
80 DEG C drying 24 hours in dry case；
(9) product obtained after drying is put into quartz boat, is heat-treated several hours under certain temperature in airtight tube type furnace；
(10) final to be measured coated in obtaining in interdigital electrode after taking appropriate heat treatment gained sample and dehydrated alcohol grinding uniform
Test substrate is put into clean environment and saves, subsequent electrical properties is waited to test by sample.
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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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