CN103926278B - graphene-based ternary composite film gas sensor and preparation method thereof - Google Patents
graphene-based ternary composite film gas sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene-based ternary composite film gas sensor and a preparation method thereof. The graphene-based ternary composite film gas sensor consists of a ternary composite film and a substrate, wherein the ternary composite film is formed by compounding graphene, metal or metal oxide nanoparticles and conducting polymers. The high specific surface area and excellent electric and physicochemical characteristics of the graphene and the nanoparticles and the specific gas-sensitive response characteristic of the conducting polymers are fully utilized, a gain complementary mechanism is formed between different materials due to ternary compounding, and the gas-sensitive characteristic and stability of the system are enhanced. Meanwhile, the preparation method is combined with a self-assembling process with high ordering property and can be used for preparing the high-sensitivity room temperature detection gas sensor.
Description
Technical field
The present invention relates to nano composite material and gas sensor technical field are and in particular to a kind of graphene-based ternary is multiple
Close thin film gas sensor and preparation method thereof.
Background technology
Graphene is a kind of new material of the monolayer laminated structure being made up of carbon atom, is with sp by carbon atom2Hydridization rail
It is in the flat film of honeycomb lattice, the two-dimensional material of only one of which carbon atom thickness that road forms hexangle type.The occurring in of Graphene
Scientific circles have evoked huge great waves, and the characteristic such as its unusual electric conductivity, excellent machinery and optical property makes graphite
Alkene has caused new round revolution in hyundai electronicses scientific domain.Graphene has very big advantage as gas sensor, first
First Graphene is two-dimensional material, and all carbon atoms are all exposed in adsorption gas molecule it is meant that can provide in unitary space
Maximum sensitive area；Secondly, the thickness of Graphene atom level is the diffusion of gas molecule and electric charge transfer provides new way
Footpath；3rd, Johnson's noise of Graphene is very little so that the sensitivity of graphene sensor is very high；4th, sonde method
Measurement can be realized on Graphene crystal, and forms Ohmic contact, and resistance is very little.Additionally, Graphene is in gas sensing
Device field also has the advantage of practical application, such as the favorable compatibility of film build method and Conventional printing process and good stablizing
Performance etc..As a kind of new gas sensitive, Graphene gas sensor is used for thering is good electricity when gas molecule detects
Characteristic, higher sensitivity and relatively low detectable limit, but select poor-performing；Meanwhile, the excellent chemical property of sensitive membrane
Depend on the dispersibility that Graphene is good, and single Graphene is then because effect and high surface are easy to reunite.
Metal nano material has excellent mechanical performance, physical property and chemical property, using platinum, gold, silver etc. to leading
Electric polymer carries out modification and can effectively strengthen electrology characteristic and chemism；And metal-oxide has higher chemistry surely
Qualitative and different characteristic of semiconductor, can form heterojunction structure with conducting polymer, change barrier height, improve composite
Characteristic of semiconductor.Metal or metal oxide nano-material are strengthened Graphene electrology characteristic and machinery with Graphene recombination energy
Characteristic, there are some researches show, the tin ash that will be provided with positive tetrahedron Rutile structure is uniformly attached to graphenic surface composition
Composite, can significantly improve the performances such as hardness, conductivity and the electrochemistry capacitance of material, and therefore such composite is in gas
The technical fields such as body sensor, ultracapacitor, solaode receive significant attention.
Conducting polymer belongs to macromolecular material, because its structure diversification, environmental stability are good, easy processing and become and grind
Study carefully focus.But pure conducting polymer is usually insulator, homogenous material has that conductivity is low, not higher than capacitance, price is held high
Your the problems such as.
Content of the invention
It is an object of the invention to provide a kind of graphene-based tri compound thin film gas sensor and preparation method thereof, make not
Form gain complementary mechanisms, the gas sensitization characteristic of reinforced composite body system and stability between composite, meet real
With the demand changed.
The present invention to achieve these goals, employs the following technical solutions:
Graphene-based tri compound thin film gas sensor, it is made up of tri compound thin film and substrate, and tri compound is thin
Film is composited by Graphene, metal or metal oxide nanoparticles, conducting polymer, and described tri compound thin film is divided into point
Tunic and monofilm, described layered membrane by the graphene layer being deposited on substrate and cover on graphene layer by metal or gold
Belong to the composite bed composition that oxide nano particles are formed with conducting polymer, described monofilm is by Graphene, metal or metal oxygen
Compound nano-particle and three kinds of material mixing of conducting polymer are composited.
Further, described substrate is interdigital electrode (idts), SAW oscillator (saw) or QCM
(qcm).
Further, described grapheme material is electronation graphene oxide, intrinsic Graphene and their quantum
Point, the powder of nanometer sheet, nano belt or nanometer line morphology, colloidal sol or dispersion liquid.
Further, described metal nanoparticle includes gold, palladium, platinum, silver, titanium, stannum, nickel, cobalt, manganese or lanthanum nano-particle；
Metal oxide nanoparticles are the nano-particle of the oxide morphology of gold, palladium, platinum, silver, titanium, stannum, nickel, cobalt, manganese or lanthanum.
Further, conducting polymer monomer is aniline monomer and its derivant, pyrrole monomer and its derivant or thiophene
Monomer and its derivant.
The invention also discloses the preparation method of graphene-based tri compound thin film gas sensor, prepare monofilm gas
Sensor comprises the steps:
1. clean substrate, and hydrophilic treated and Electrostatic Treatment are carried out to substrate；
2. utilize magnetic agitation or ultrasonic technique, prepare Graphene, metal or metal oxide nanoparticles composite diffusion
Liquid；
3. add conducting polymer monomer in the composite dispersion liquid 2. obtaining, and adjust polymerization parameter；
4. add reagent and additive in polymerization；
5. step 4. on the basis of, point two ways, the first: when reaction to be polymerized occurs, substrate is inserted polymerization
In solution, carry out in-situ polymerization self assembly；Then take out substrate, clean and be dried, be placed in vacuum drying oven and preserve, obtain three
The compound self-assembled monolayer film gas transducer of unit；Second: composite solution after abundant home position polymerization reaction, by filter,
Washing and grinding obtain product, are configured to composite dispersion liquid；By rotation, spraying or drop coating in deposition on substrate thin film,
Obtain tri compound self-assembled monolayer film gas transducer.
Preparation layering film gas transducer comprises the steps:
1. clean substrate, and hydrophilic treated and Electrostatic Treatment are carried out to substrate；
2. utilize magnetic agitation or ultrasonic technique, prepare graphene dispersing solution；Pass through rotation, spraying or drop coating again in base
One layer graphene thin film is deposited on piece；
3. prepare metal or metal oxide nanoparticles dispersion liquid, toward in dispersion liquid, add conducting polymer monomer, adjust
Section polymerization process condition；
4. add reagent and additive in polymerization；
5. when reaction to be polymerized occurs, the graphene film 2. obtaining substrate is inserted in polymeric solution, carry out poly- in situ
Close self assembly；Then take out substrate, clean and be dried, be placed in vacuum drying oven and preserve, obtain tri compound layered film gas
Body sensor.
In the preparation method of above-mentioned graphene-based tri compound thin film gas sensor, step 1. in, clean base
Piece step is respectively ultrasonic 15 ~ 30min in acetone, ethanol, deionized water, hydrophilizing treatment step be deionized water, ammonia,
Ultrasonic 30min ~ 120min in hydrogen peroxide (volume ratio 5:1:1), Electrostatic Treatment step includes: by the substrate after hydrophilic treated successively
It is placed in 5min ~ 60min in said polycation solution and polyanion solution, wherein said polycation solution includes: polydiene propyl group two
Ammonio methacrylate (pdda) or polyethyleneimine (pei)；Polyanion solution is Sodium Polystyrene Sulfonate (pss) or polyacrylic acid
(paa).
In the preparation method of above-mentioned graphene-based tri compound thin film gas sensor, step 2. in, preparation point
The solvent of dispersion liquid includes water, ethanol, acetone, oxolane, n- methyl pyrrolidone, n, n- dimethyl acetylamide or n, n- diformazan
One or more in base Methanamide, step 3. in, adjust polymerization parameter be telo merization ph be 1 ~ 3, polyreaction temperature
Spend for 0 DEG C ~ 30 DEG C.
In the preparation method of above-mentioned graphene-based tri compound thin film gas sensor, step 4. in, described poly-
Conjunction auxiliary agent is oxidant, and trigger monomer carries out chemical polymerization, adopts when conducting polymer monomer is aniline monomer and its derivant
With Ammonium persulfate., adopt iron chloride when conducting polymer monomer is pyrrole monomer and its derivant, when conducting polymer monomer
For p-methyl benzenesulfonic acid ferrum when thiophene monomer and its derivant.
The present invention compared with prior art has the advantages that
The present invention is formed new using Graphene, conducting polymer and metal or metal oxide nanoparticles three-phase composite
Nano material system, both can fully represent Graphene and the excellent electric property of nano-particle and chemism, and can play and lead
The special response performance of electric polymer；Graphene can play conductive channel between polymer and metal-based nano granule simultaneously
Effect, and strengthen the transfer ability of electronics by effect, reduce the resistivity of system, improve environmental stability.The interface of three
Bonding action and synergistic enhancing effect may also cause composite and embody new chemically or physically characteristic, and realize Graphene and
The fine dispersion of nano-particle and architecture are strengthened so that shown more excellent based on the gas sensor of trielement composite material
Performance.
Method is simple, low cost for present invention offer；Graphene-based tri compound using the method preparation
Thin film gas sensor, because metal or metal oxide nanoparticles are uniformly distributed in Nano grade, in conjunction with Graphene originally
The great specific surface area of body, after being compounded with conducting polymer in the original location, while playing different materials sensitivity characteristic, three
Interface bond effect and cooperative effect enhance motion or the diffusion of carrier, therefore increased matrix conductivity it is achieved that
Graphene and nano-particle fine dispersion and architecture strengthen, and improve electricity and the sensitivity characteristic of polymer.Compare single
Material gas sensor, drastically increases response characteristic and the stability of sensor, is gas sensor under room temperature condition
Develop and open new approach.
Brief description
Fig. 1 is variable concentrations nh3Response characteristic comparison diagram,
Fig. 2 is 20ppmnh3Repeat property comparison diagram,
Fig. 3 is to prepare tri compound self-assembled monolayer schematic flow sheet,
Fig. 4 is to prepare tri compound self assembly layered membrane schematic flow sheet.
Specific embodiment
Embodiment 1 prepares monolayer laminated film gas sensor
With golden interdigital electrode as sensor substrate, its structural representation is as shown in Figure 1.Prepare reduction on interdigital electrode surface
Graphene oxide (rgo)/tin ash (sno2)/polyaniline (pani) tri compound thin film gas sensor, it is embodied as
Step is as follows:
1. golden interdigital electrode is sequentially placed into acetone, ethanol, ultrasonic 15min in deionized water；
2. carry out hydrophilic treated, place the substrate in the mixed solution (1:1:5) of ammonia, hydrogen peroxide and deionized water, and
It is heated to 70 DEG C, keep 1h；
3. carry out Electrostatic Treatment, the interdigital electrode after hydrophilic treated is placed in and is sequentially placed in pdda and pss solution, respectively
Keep 10min；
4., in 50ml, add 15mg Graphene, 15mg tin ash mixed-powder in the hcl solution of 1m and then pass through fully
Sonic oscillation and magnetic agitation, obtain composite dispersion liquid.
5. add 0.1ml aniline monomer in above-mentioned dispersion liquid, and be maintained in ice-water bath and be sufficiently stirred for；
6. add 10ml ammonium persulfate aqueous solution (Solute mass is 0.244g) in aniline monomer composite dispersion liquid, keep
Magnetic agitation at a slow speed；
7. after in-situ polymerization 12h, reaction solution is cleaned with ethanol, deionized water respectively, until filtrate becomes colorless；
8. above-mentioned filtration product dried, grind, in redispersion to ethanol water (volume ratio 3:7), be configured to 1mg/
Ml composite dispersion liquid；
9. utilize lathe turner's skill, forward 500r/min, 10s, after turn 3000r/min, 20s；Above-mentioned composite dispersion liquid is revolved
On interdigital electrode surface, then interdigital electrode is placed in 50 DEG C of vacuum drying ovens and preserves, acquisition Graphene/tin ash/
Polyaniline tri compound thin film gas sensor.
Embodiment 2 prepares monolayer self assembly laminated film gas sensor
With golden interdigital electrode as sensor substrate, its structural representation is as shown in Figure 1.Prepare reduction on interdigital electrode surface
Graphene oxide (rgo)/tin ash (sno2)/polyaniline (pani) ternary monolayer laminated film gas sensor, it is concrete
Implementation steps are as follows:
1. golden interdigital electrode is sequentially placed into acetone, ethanol, ultrasonic 15min in deionized water；
2. carry out hydrophilic treated, place the substrate in the mixed solution (1:1:5) of ammonia, hydrogen peroxide and deionized water, and
It is heated to 70 DEG C, keep 1h；
3. carry out Electrostatic Treatment, the interdigital electrode after hydrophilic treated is placed in and is sequentially placed in pdda and pss solution, respectively
Keep 10min；
4., in 50ml, add 15mg Graphene, 15mg tin ash mixed-powder in the hcl solution of 1m and then pass through fully
Sonic oscillation and magnetic agitation, obtain composite dispersion liquid.
5. add 0.1ml aniline monomer in above-mentioned dispersion liquid, and be maintained in 20 DEG C of room temperature and carried out fully with Glass rod
Stirring；
6. add 10ml ammonium persulfate aqueous solution (Solute mass is 0.244g) in above-mentioned aniline monomer composite dispersion liquid；
7. when polyreaction occurs, by pretreated interdigital electrode insertion polymerization dispersion liquid, when solution temperature no longer
When changing, take out substrate, cleaned with the hcl solution of 1m, nitrogen dries up, be placed in 50 DEG C of vacuum drying ovens and preserve, obtain
Graphene/tin ash/polyaniline ternary monolayer self assembly laminated film gas sensor.Its mechanism schematic diagram is as shown in Figure 3.
Embodiment 3 prepares layered film gas sensor
1. golden interdigital electrode is sequentially placed into acetone, ethanol, ultrasonic 15min in deionized water；
2. carry out hydrophilic treated, place the substrate in the mixed solution (1:1:5) of ammonia, hydrogen peroxide and deionized water, and
It is heated to 70 DEG C, keep 1h；
3. carry out Electrostatic Treatment, the interdigital electrode after hydrophilic treated is placed in and is sequentially placed in pdda and pss solution, respectively
Keep 10min；
4., in 10ml, add 10mg graphene powder to carry out sufficiently ultrasonic and magnetic agitation in the hcl solution of 1m, preparation
Graphene dispersing solution；
5. utilize gas spraying process, spray height 20cm, add the above-mentioned graphene dispersing solution of 1ml in airbrush, at center
Interdigital electrode is put in effective coverage, by uniform for graphene dispersing solution gas blowout in interdigital electrode；
6., in 50ml, add 15mg tin ash mixed-powder in the hcl solution of 1m and then pass through sufficient sonic oscillation
And magnetic agitation, obtain composite dispersion liquid.
7. add 0.1ml aniline monomer in above-mentioned dispersion liquid, and be maintained in ice-water bath and be sufficiently stirred for；
8. add 10ml ammonium persulfate aqueous solution (Solute mass is 0.244g) in aniline monomer composite dispersion liquid, keep
Magnetic agitation at a slow speed；
9. after in-situ polymerization 12h, reaction solution is cleaned with ethanol, deionized water respectively, until filtrate becomes colorless；
10. above-mentioned filtration product dried, grind, in redispersion to ethanol water (volume ratio 3:7), be configured to 1mg/
Ml composite dispersion liquid；
11. utilize lathe turner's skill, forward 500r/min, 10s, after turn 3000r/min, 20s；Above-mentioned composite dispersion liquid is revolved
On interdigital electrode surface, obtain Graphene/tin ash/polyaniline ternary hierarchical composite thin film gas sensor.Its mechanism
Schematic diagram is as shown in Figure 4.
To the Graphene/tin ash/polyaniline tri compound thin film gas sensor obtaining and single polyaniline film
Gas sensor carries out gas-sensitive property test, and its gas-sensitive property curve is as shown in Figures 1 and 2.
Contrast Fig. 1 and Fig. 2, rgo/sno2/ pani tri compound thin film gas sensor is to variable concentrations ammonia response value
Apparently higher than single pani, Repeatability is good.
The method being provided by this patent, between Graphene, metal or metal oxide nanoparticles and conducting polymer
Form collaborative and complementary effect, overcome deficiency in terms of air-sensitive performance for the homogenous material, by in-situ polymerization and self assembly phase
In conjunction with technique increase the adhesive force in substrate surface for the thin film, define composite Nano air-sensitive film controlled in order；Simultaneously
By the compound electrical conductivity that improve thin film, enhance environmental stability.
Claims (7)
1. the preparation method of graphene-based tri compound thin film gas sensor is it is characterised in that graphene-based tri compound is thin
Film gas transducer is made up of tri compound thin film and substrate, and tri compound thin film is received by Graphene, metal or metal-oxide
Rice grain, conducting polymer are composited, and described tri compound thin film is divided into layered membrane and monofilm, and described layered membrane is by depositing
The graphene layer on substrate and cover on graphene layer by metal or metal oxide nanoparticles and conducting polymer
The composite bed being formed is constituted, and described monofilm is by Graphene, metal or metal oxide nanoparticles and three kinds of conducting polymer
Material mixing is composited, wherein:
Prepare monolayer film gas transducer to comprise the steps:
1. clean substrate, and hydrophilic treated and Electrostatic Treatment are carried out to substrate；
2. utilize magnetic agitation or ultrasonic technique, prepare Graphene, metal or metal oxide nanoparticles composite dispersion liquid；
3. add conducting polymer monomer in the composite dispersion liquid 2. obtaining, and adjust polymerization parameter；
4. add reagent and additive in polymerization；
5., when reaction to be polymerized occurs, substrate is inserted in polymeric solution, carries out in-situ polymerization self assembly；Then take out substrate,
Clean and be dried, be placed in vacuum drying oven and preserve, obtain tri compound self-assembled monolayer film gas transducer；
Preparation layering film gas transducer comprises the steps:
(1) clean substrate, and hydrophilic treated and Electrostatic Treatment are carried out to substrate；
(2) utilize magnetic agitation or ultrasonic technique, prepare graphene dispersing solution；Pass through rotation, spraying or drop coating again on substrate
Deposit a layer graphene thin film；
(3) prepare metal or metal oxide nanoparticles dispersion liquid, toward in dispersion liquid, add conducting polymer monomer, adjust poly-
Close process conditions；
(4) add reagent and additive in polymerization；
(5), when reaction to be polymerized occurs, the graphene film substrate that (2) are obtained is inserted in polymeric solution, carries out in-situ polymerization
Self assembly；Then take out substrate, clean and be dried, be placed in vacuum drying oven and preserve, obtain tri compound layered film gas
Sensor.
2. graphene-based tri compound thin film gas sensor according to claim 1 preparation method it is characterised in that
In step 1. and in (1), cleaning substrate step is the ultrasonic 15 ~ 30min of difference, hydrophilic treated in acetone, ethanol, deionized water
Step is ultrasonic 30min ~ 120min in deionized water, ammonia, hydrogen peroxide, and Electrostatic Treatment step includes: after hydrophilic treated
Substrate priority be placed in 5min ~ 60min in said polycation solution and polyanion solution, wherein said polycation solution includes: poly-
Diallyldimethylammonium chloride or polyethyleneimine；Polyanion solution is Sodium Polystyrene Sulfonate or polyacrylic acid.
3. graphene-based tri compound thin film gas sensor according to claim 1 preparation method it is characterised in that
In step 2. and in (2), the solvent preparing dispersion liquid includes water, ethanol, acetone, oxolane, n- methyl pyrrolidone, n, n-
Dimethyl acetylamide or n, one or more in n- dimethylformamide, in step 3. and in (3), adjusting polymerization parameter is to adjust
Polyreaction ph is 1 ~ 3, and polymeric reaction temperature is 0 DEG C ~ 30 DEG C.
4. graphene-based tri compound thin film gas sensor according to claim 1 preparation method it is characterised in that
In step 4. and in (4), described reagent and additive in polymerization is oxidant, and trigger monomer carries out chemical polymerization, when conducting polymer monomer is
Ammonium persulfate. is adopted, when conducting polymer monomer is pyrroles, azole derivatives when aniline, anil or their mixture
Or adopt iron chloride during their mixture, when conducting polymer monomer is thiophene, thiophene derivant or their mixture
Use p-methyl benzenesulfonic acid ferrum.
5. graphene-based tri compound thin film gas sensor according to claim 1 preparation method it is characterised in that
Described substrate is interdigital electrode, SAW oscillator or QCM.
6. graphene-based tri compound thin film gas sensor according to claim 1 preparation method it is characterised in that
Described grapheme material is electronation graphene oxide, intrinsic Graphene and their quantum dot, nanometer sheet, nano belt or
The powder of nanometer line morphology, colloidal sol or dispersion liquid.
7. graphene-based tri compound thin film gas sensor according to claim 1 preparation method it is characterised in that
Described metal nanoparticle includes gold, palladium, platinum, silver, titanium, stannum, nickel, cobalt, manganese or lanthanum nano-particle；Metal oxide nanoparticles
Nano-particle for the oxide morphology of gold, palladium, platinum, silver, titanium, stannum, nickel, cobalt, manganese or lanthanum.
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