CN108872077A - A kind of preparation method of the fluorocarbon polymer modification membranaceous multiband light senser element of chemical conversion graphene/zinc oxide films - Google Patents
A kind of preparation method of the fluorocarbon polymer modification membranaceous multiband light senser element of chemical conversion graphene/zinc oxide films Download PDFInfo
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- C25D13/00—Electrophoretic coating characterised by the process
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Abstract
The present invention relates to a kind of preparation methods of fluorocarbon polymer modification membranaceous multiband light senser element of chemical conversion graphene/zinc oxide films, including：Chemical conversion graphene/zinc-oxide film ZnO/rGO is prepared using no reagent electrophoresis assemble method；Fluorocarbon polymer is coated in chemical conversion graphene/zinc oxide films film surface.Operation of the present invention is simple, preparation process fast and easy, at low cost, is with a wide range of applications；Obtained photo-sensing device has good flexibility, is suitable for wearable field and applies light；Obtained photo-sensing device has good sensing capabilities in ultraviolet, visible, infrared band, and photo-signal signal-to-noise ratio is big, and light-intensity test lower limit is low.
Description
Technical field
The invention belongs to the preparation field of flexible optical sensor, in particular to a kind of fluorocarbon polymer modifies chemical conversion stone
The preparation method of the black membranaceous multiband light senser element of alkene/zinc oxide films.
Background technique
Flexible sensor can be divided into physical flexibility sensor (such as photodetection, electronic skin, pressure sensing and temperature sensing
Deng) and chemical flexible sensor (such as gas sensing, ion sensor and biological micromolecule sensing).
It is measurement medium, using photoelectric device as the sensor of conversion element that photoelectric sensor, which is using light, it has non-connect
The excellent properties such as touching, the fast, reliable performance of response.In recent years, continuing to bring out with various Novel Optoelectronic Devices, especially laser
The fast development of technology and image technique, photoelectric sensor have become the key that photoelectric conversion is realized in various photodetector systems
Element plays key player in sensor field.Photoelectric sensor is in national economy and each neck of science and technology at present
Domain is widely used, and plays increasingly important role.Photoelectric sensor technology widely applies to army of various countries
The numerous areas such as thing technology, aerospace, detection technique and Vehicle Engineering.Utilization of the photoelectric sensor in current scientific research field
Range is very wide, and influence power is huge.The novel photoelectric sensor for being based especially on the research and development of photoelectric sensor technology principle and producing
The mainstream as current transducer market is detected.
UV sensor based on ZnO and graphene-based ultraviolet, it is seen that and the detector of infrared light can be applied to more
It is widely applied range, because their spectral response ranges are wide, high sensitivity has flexibly, portable and wearable feature.So
And electric signal noise is big in transducing signal, therefore reduces the work that electric signal noise becomes crucial.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of fluorocarbon polymers to modify chemical conversion graphene/zinc oxide
The preparation method of film-form multiband light senser element, to overcome prior art optical sensor noise big, optical sensor can only be examined
Survey the defect of single wave band.
Under same light intensity, chemical conversion graphene/zinc-oxide film photoelectric current is thinner than chemical graphene in the present invention
Film it is big, by fluorocarbon polymer be coated in chemical conversion graphene/zinc-oxide film after, noise is substantially reduced.In addition, most of
Optical sensor can only detect single wave band, and chemical conversion of the present invention graphene/zinc-oxide film is able to detect multiple wave bands.
A kind of fluorocarbon polymer of the invention modifies the membranaceous multiband light senser element of chemical conversion graphene/zinc oxide films
Preparation method, including：Chemical conversion graphene/zinc-oxide film ZnO/rGO, oxygen are prepared using no reagent electrophoresis assemble method
Change zinc particle to be attached on chemical conversion graphene film by electric field force；Chemical conversion graphene/oxygen is modified with fluorocarbon polymer
Change zinc film.
A kind of fluorocarbon polymer of the invention modifies the membranaceous multiband light senser element of chemical conversion graphene/zinc oxide films
Preparation method, including：
(1) graphene oxide dispersion is dispersed by ultrasonic vibration, obtains graphene oxide dispersion or graphite oxide
The solidifying slurry of alkene, by a series of film-forming methods such as knife coating, suction method, obtains graphene oxide film；
(2) graphene oxide film in step (1) is restored by thermal reduction or chemical reagent, then uses ethyl alcohol or water
Washing, drying at room temperature obtain chemical conversion graphene (rGO) film；
(3) electrophoresis construction from part is used, using Zn foil as anode, using rGO film in step (2) as cathode, direct current electrophoresis is heavy
Product, application electric field strength are 5~25V/cm, electric current 1A, energization 10min or more, are taken out, it is thin to obtain ZnO/rGO for drying at room temperature
Then fluorocarbon polymer is coated on the surface of ZnO/rGO film by film, obtain fluorocarbon polymer modification chemical conversion graphite
The membranaceous multiband light senser element of alkene/zinc oxide films.
The concentration of graphene oxide dispersion is 3~10mg/mL in the step (1)；Solvent is distilled water.
The graphene oxide dispersion is：It adds graphene oxide into distilled water and is made into certain density dispersion liquid.
The time that ultrasonic vibration disperses in the step (1) is 10~12h；Ultrasonic vibration dispersion uses ultrasonic disperse instrument.
The GO property of thin film that the serial of methods such as knife coating, suction method obtain in the step (1) is without significant difference.
The graphene oxide dispersion volume filtered in suction method in the step (1) is 10mL, and filter membrane is 0.45 μ of aperture
The mixed fiber membrane of m, time 3d.
The rGO property of thin film that thermal reduction or chemical reagent reduction obtain in the step (2) is without significant difference.
Thermal reduction temperature is 400~2800 DEG C in the step (2), and the thermal reduction time is 2h.
Chemical reagent reduction is the hydroiodic acid for being 55% with concentration, recovery time 2h in the step (2).
It is with ethyl alcohol or water washing in the step (2)：Ethyl alcohol or water washing with 95% are repeated 2~3 times, are washed every time
The time washed is 2h.
Distance is 1~2cm between cathode and anode in the step (3).
It is medium that electrophoresis group, which is filled with ultrapure water (18.2 Ω cm), in the step (3), other changes such as electrolyte are not used
Learn reagent.
Fluorocarbon polymer includes having-CF in the step (3)3The polymer reactant of functional group.
Fluorocarbon polymer includes perfluoropolyether PFPE or perfluor tetraethylene glycol dimethyl ether PFTG in the step (3).
The invention proposes make zinc oxide be attached to chemical conversion graphene (rGO) film with no reagent electrophoresis construction from part
On, one layer of fluorocarbon polymer then is coated on the surface of film, the fluorocarbon polymer of acquisition modifies chemical conversion graphene/zinc oxide
Film-form multiband light senser element, is able to detect the photoresponse of different illumination intensity.
Beneficial effect
(1) operation of the present invention is simple, preparation process fast and easy, at low cost, is with a wide range of applications；
(2) photo-sensing device that the present invention obtains has good flexibility, is suitable for wearable field and applies light；
(3) photo-sensing device that the present invention obtains has good sensing capabilities, photoelectricity in ultraviolet, visible, infrared band
It is big to flow Signal-to-Noise, and light-intensity test lower limit is low.
Detailed description of the invention
Fig. 1 is that chemical conversion graphene/zinc-oxide film prepares schematic diagram (a) and Photoelectric Detection signal in embodiment 1
Scheme (b)；Wherein, 1, power supply；2, chemical conversion graphene film；3, spelter；4, ultrapure water；5, electrochemical workstation；6, to electricity
Pole；7, reference electrode；8, working electrode；9, computer；10, copper foil；11, light source；12, ZnO particle；13, chemical conversion graphene
Film.
Fig. 2 is chemical conversion graphene/zinc-oxide film XRD diagram in embodiment 1.
Fig. 3 is chemical conversion graphene/zinc-oxide film SEM figure in embodiment 1.
Fig. 4 is the ZnO/rGO film of rGO film in embodiment 1, ZnO/rGO film and PFPE coating in bias 0.4V, light
Strong 7.63mW/cm2Under time current curve；(a) be ZnO/rGO film and rGO film time current correlation curve, (b)
It is the time current correlation curve before and after ZnO/rGO film surface coating PFPE, is (c) ZnO/rGO film surface coating PFPE
The time noise current correlation curve of front and back.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) at room temperature, graphene oxide 300mg is weighed, is placed in the beaker of 200mL, then plus distilled water 100mL matches
Then the dispersion liquid for being 3mg/mL at concentration obtains graphene oxide dispersion 100mL with Ultrasound Instrument processing 10h；It measures every time
10mL graphene oxide dispersion, which is poured into the sand core funnel of diameter 4.5cm, filters 3d to get graphene oxide film is arrived.
(2) graphene oxide film in step (1) is placed in glass culture dish, the hydroiodic acid of 20mL 55% is added, used
Film seals culture dish, is placed in dark place, after 2h, takes out film, and with the infiltration of 95% ethyl alcohol washing 3 times, after drying, obtain rGO
Film.
(3) electrophoresis construction from part is used, using Zn foil as anode in ultrapure water, using rGO film in step (2) as cathode, the two poles of the earth
Between distance be 1cm, apply voltage 25V/cm, electric current 1A, energization 10min, take out, drying at room temperature obtains ZnO/rGO film.
The size of the Zinc oxide particles is 2 μm.0.1mL PFPE is coated into 1cm2ZnO/rGO film, obtain fluorocarbon polymer and repair
Adorn chemical conversion graphene/zinc-oxide film, the film with a thickness of 50 μm.In bias 0.4V, light intensity 7.63mW/cm2Under, it obtains
To rGO film, ZnO/rGO film time current correlation curve (see Fig. 4 a), ZnO/rGO film and there is PFPE coating (to pass through rotation
Coating, revolving speed 400r/min) ZnO/rGO film time current correlation curve (see Fig. 4 b) and corresponding time noise current pair
Than curve (see Fig. 4 c), the results showed that：The photoelectric current ratio rGO's of ZnO/rGO film is big, by the coated ZnO/rGO of PFPE
Film is smaller than the electrochemical noise of the ZnO/rGO film of uncoated PFPE and photoelectric current also faint increase.
Fig. 2 shows：Chemical conversion graphene/zinc oxide has a peak in 2 θ=24.2 °, and in 2 θ=31.45 °, and 2 θ=
34.11 °, 2 θ=35.98 °, 2 θ=47.16 ° and 2 θ=56.26 ° respectively correspond (the 10 of zinc oxide there are five diffraction maximums
0), (0 0 2), (1 0 1), (10 2) and (1 1 0) crystal face correspond to the PDF#36-1451 card of ZnO.
Fig. 3 shows：By no reagent electrophoresis, rGO film surface generates fusiform ZnO particle.
Embodiment 2
(1) at room temperature, graphene oxide 500mg is weighed, is placed in the beaker of 200mL, then plus distilled water 100mL matches
Then the dispersion liquid for being 5mg/mL at concentration obtains graphene oxide dispersion 100mL with Ultrasound Instrument processing 10.5h；Every secondary amounts
It takes 10mL graphene oxide dispersion to pour into the sand core funnel of diameter 4.5cm and filters 3d to get graphene oxide film is arrived.
(2) graphene oxide film in step (1) is placed in glass culture dish, the hydroiodic acid of 20mL 55% is added, used
Film seals culture dish, is placed in dark place, after 2h, takes out film, and with the infiltration of 95% ethyl alcohol washing 3 times, after drying, obtain rGO
Film.
(3) electrophoresis construction from part is used, using Zn foil as anode in ultrapure water, using rGO film in step (2) as cathode, two
Distance is 1.5cm between pole, applies voltage 15V/cm, electric current 1A, is powered 1 hour, is taken out, and it is thin to obtain ZnO/rGO for drying at room temperature
Film.0.1mL PFPE is coated into 1cm2ZnO/rGO film, obtain fluorocarbon polymer modification chemical conversion graphene/zinc oxide
Film.In bias 0.4V, light intensity 7.63mW/cm2Under, it obtains rGO film, ZnO/rGO film and PFPE coating and (passes through spin coating
Method, revolving speed 400r/min) ZnO/rGO film time current correlation curve and time noise current correlation curve, as a result table
It is bright：The photoelectric current ratio rGO's of ZnO/rGO film big, the ZnO/ by PFPE coated ZnO/rGO film than uncoated PFPE
The electrochemical noise of rGO film is small and photoelectric current also faint increase.
Embodiment 3
(1) at room temperature, graphene oxide 600mg is weighed, is placed in the beaker of 200mL, then plus distilled water 100mL matches
Then the dispersion liquid for being 6mg/mL at concentration obtains the solidifying slurry 30mL of graphene oxide with Ultrasound Instrument processing 11h；By solidifying slurry by scraping
Coating obtains graphene oxide film.
(2) graphene oxide film in step (1) is placed in graphitizing furnace, temperature is 400 DEG C, after 2h, takes out film, cold
But to room temperature, rGO film is obtained.
(3) electrophoresis construction from part is used, using Zn foil as anode in ultrapure water, using rGO film as cathode, distance between the two poles of the earth
For 1cm, apply voltage 20V/cm, electric current 1A, be powered 0.5 hour, take out, drying at room temperature obtains ZnO/rGO film.By 0.1mL
PFPE coats 1cm2ZnO/rGO film, obtain fluorocarbon polymer modification chemical conversion graphene/zinc-oxide film.In bias
0.4V, light intensity 11.21mW/cm2Under, rGO film, ZnO/rGO film and PFPE coating are obtained (by spin-coating method, revolving speed 400r/
Min the time current correlation curve and time noise current correlation curve of ZnO/rGO film), the results showed that：ZnO/rGO is thin
Big, the electricity of the ZnO/rGO film by PFPE coated ZnO/rGO film than uncoated PFPE of the photoelectric current ratio rGO of film
Chemical noise is small and photoelectric current also faint increase.
Embodiment 4
(1) at room temperature, graphene oxide 800mg is weighed, is placed in the beaker of 200mL, then plus distilled water 100mL matches
Then the dispersion liquid for being 8mg/mL at concentration obtains the solidifying slurry 30mL of graphene oxide with Ultrasound Instrument processing 11.5h；Solidifying slurry is passed through
Knife coating obtains graphene oxide film.
(2) graphene oxide film in step (1) being placed in graphitizing furnace, temperature is 1600 DEG C, after 2h, film is taken out,
It is cooled to room temperature, obtains rGO film.
(3) electrophoresis construction from part is used, using Zn foil as anode in ultrapure water, using rGO film as cathode, distance between the two poles of the earth
For 1.5cm, apply voltage 20V/cm, electric current 1A, be powered 1 hour, take out, drying at room temperature obtains ZnO/rGO film.By 0.1mL
PFTG coats 1cm2ZnO/rGO film, obtain fluorocarbon polymer modification chemical conversion graphene/zinc-oxide film.In bias
0.4V, light intensity 14.92mW/cm2Under, rGO film, ZnO/rGO film and PFTG coating are obtained (by spin-coating method, revolving speed 400r/
Min the time current correlation curve and time noise current correlation curve of ZnO/rGO film), the results showed that：ZnO/rGO is thin
Big, the electricity of the ZnO/rGO film by PFTG coated ZnO/rGO film than uncoated PFTG of the photoelectric current ratio rGO of film
Chemical noise is small.
Embodiment 5
Then plus distilled water 100mL (1) at room temperature, graphene oxide 1000mg is weighed, is placed in the beaker of 200mL,
It is made into the dispersion liquid that concentration is 10mg/mL, then obtains the solidifying slurry 30mL of graphene oxide with Ultrasound Instrument processing 12h；Solidifying slurry is logical
Knife coating is crossed, graphene oxide film is obtained.
(2) graphene oxide film in step (1) being placed in graphitizing furnace, temperature is 2800 DEG C, after 2h, film is taken out,
It is cooled to room temperature, obtains rGO film.
(3) electrophoresis construction from part is used, using Zn foil as anode in ultrapure water, by rGO film as cathode, the spacing at the two poles of the earth
It is powered 2 hours, takes out from for 2cm, application voltage 5V/cm, electric current 1A, drying at room temperature obtains ZnO/rGO film.ZnO/rGO
Film is respectively in bias 0.4V, wavelength 365,532 and 808nm, light intensity 6mW/cm2Light source irradiation under obtain time current
Curve, the results showed that：Since the optical responsivity of the light source ZnO/rGO film to different wave length is had any different, ZnO/rGO film can be with
Different photoelectric currents is generated under the light source irradiation of different wave length, therefore optical source wavelength can be detected according to photoelectric current.
Claims (6)
1. a kind of preparation side of the fluorocarbon polymer modification membranaceous multiband light senser element of chemical conversion graphene/zinc oxide films
Method, which is characterized in that use prepares chemical conversion graphene/zinc-oxide film ZnO/rGO without reagent electrophoresis assemble method；By fluorine
Carbon polymer is coated in chemical conversion graphene/zinc oxide films film surface.
2. preparation method according to claim 1, which is characterized in that the use is without reagent electrophoresis assemble method：Zinc
As anode, chemical conversion graphene film is as cathode, and direct current electrophoretic deposition, electrophoresis 10min or more, is changed at room temperature
Conversion graphene/zinc-oxide film is learned, wherein the electric field strength of direct current electrophoretic deposition is 5~25V/cm, and electrolyte is ultrapure
Water.
3. preparation method according to claim 2, which is characterized in that the preparation method of the chemical conversion graphene film
Including：Graphene oxide dispersion is prepared into graphene oxide film, graphene oxide film thermal reduction or electronation are washed
It washs, it is dry, obtain chemical conversion graphene film.
4. preparation method according to claim 3, which is characterized in that the graphene oxide film passes through knife coating or pumping
Filter method obtains.
5. preparation method according to claim 1, which is characterized in that the fluorocarbon polymer includes having-CF3Functional group
Polymer reactant.
6. preparation method according to claim 1 or 5, which is characterized in that the fluorocarbon polymer includes perfluoropolyether
PFPE or perfluor tetraethylene glycol dimethyl ether PFTG.
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