CN108872077B - Preparation method of fluorocarbon polymer modified chemical conversion graphene/zinc oxide film-shaped multiband optical sensing device - Google Patents
Preparation method of fluorocarbon polymer modified chemical conversion graphene/zinc oxide film-shaped multiband optical sensing device Download PDFInfo
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Abstract
The invention relates to a preparation method of a fluorocarbon polymer modified chemical conversion graphene/zinc oxide thin film multi-band optical sensing device, which comprises the following steps: preparing chemical conversion graphene/zinc oxide film ZnO/rGO by using a reagent-free electrophoresis assembly method; and coating the fluorocarbon polymer on the surface of the chemical conversion graphene/zinc oxide film. The method has the advantages of simple operation, convenient and quick preparation process, low cost and wide application prospect; the obtained optical sensing device has good flexibility and is suitable for application light in the wearable field; the obtained optical sensing device has good sensing performance in ultraviolet, visible and infrared bands, the signal-to-noise ratio of photocurrent signals is high, and the lower limit of light intensity detection is low.
Description
Technical Field
The invention belongs to the field of preparation of flexible optical sensors, and particularly relates to a preparation method of a fluorocarbon polymer modified chemical conversion graphene/zinc oxide film-shaped multiband optical sensor.
Background
Flexible sensors can be classified into physical flexible sensors (e.g., photoelectric detection, electronic skin, pressure sensing, temperature sensing, etc.) and chemical flexible sensors (e.g., gas sensing, ion sensing, small-molecule sensing, etc.).
The photoelectric sensor is a sensor which takes light as a measuring medium and a photoelectric device as a conversion element, and has the excellent characteristics of non-contact, quick response, reliable performance and the like. In recent years, with the continuous emergence of various novel photoelectric devices, especially the rapid development of laser technology and image technology, photoelectric sensors have become key elements for realizing photoelectric conversion in various photoelectric detection systems, and play an important role in the field of sensors. At present, photoelectric sensors are widely applied in various fields of national economy and scientific technology and play more and more important roles. The photoelectric sensor technology has been widely applied to various fields such as military technologies, aerospace, detection technologies, vehicle engineering and the like. The photoelectric sensor has wide application range in the current scientific research field and great influence. In particular, new types of photosensors developed and manufactured based on the principle of photosensor technology have been detected as the mainstream of the sensor market today.
ZnO-based UV sensors and graphene-based ultraviolet, visible and infrared light detectors can be used in a wider range of applications because of their wide spectral response range, high sensitivity, flexibility, portability and wearable characteristics. However, the sensing signal has high electrical signal noise, so reducing the electrical signal noise becomes a critical task.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a fluorocarbon polymer modified chemical conversion graphene/zinc oxide film-shaped multiband optical sensor device, so as to overcome the defects that the noise of an optical sensor is high and the optical sensor can only detect a single waveband in the prior art.
Under the same light intensity, the photocurrent of the chemical conversion graphene/zinc oxide film is larger than that of the chemical conversion graphene film, and the noise is obviously reduced after the fluorocarbon polymer is coated on the chemical conversion graphene/zinc oxide film. In addition, most of the optical sensors can only detect a single wave band, and the chemically converted graphene/zinc oxide film can detect a plurality of wave bands.
The invention discloses a preparation method of a fluorocarbon polymer modified chemical conversion graphene/zinc oxide thin film multi-band optical sensing device, which comprises the following steps: preparing chemical conversion graphene/zinc oxide film ZnO/rGO by using a reagent-free electrophoresis assembly method, wherein zinc oxide particles are attached to the chemical conversion graphene film through electric field force; and modifying the chemically converted graphene/zinc oxide film by using a fluorocarbon polymer.
The invention discloses a preparation method of a fluorocarbon polymer modified chemical conversion graphene/zinc oxide thin film multi-band optical sensing device, which comprises the following steps:
(1) dispersing the graphene oxide dispersion liquid through ultrasonic oscillation to obtain a graphene oxide dispersion liquid or graphene oxide coagulation slurry, and obtaining a graphene oxide film through a series of film preparation methods such as a blade coating method and a suction filtration method;
(2) carrying out thermal reduction or chemical reagent reduction on the graphene oxide film obtained in the step (1), washing with ethanol or water, and drying at room temperature to obtain a chemically converted graphene (rGO) film;
(3) and (3) adopting an electrophoresis assembly method, taking a Zn foil as an anode, taking the rGO thin film in the step (2) as a cathode, performing direct current electrophoresis deposition, applying an electric field intensity of 5-25V/cm and a current of 1A, electrifying for more than 10min, taking out, drying at room temperature to obtain a ZnO/rGO thin film, and coating a fluorocarbon polymer on the surface of the ZnO/rGO thin film to obtain the fluorocarbon polymer modified chemically converted graphene/zinc oxide thin film multi-band optical sensing device.
The concentration of the graphene oxide dispersion liquid in the step (1) is 3-10 mg/mL; the solvent is distilled water.
The graphene oxide dispersion liquid is as follows: adding graphene oxide into distilled water to prepare a dispersion liquid with a certain concentration.
The time for ultrasonic oscillation dispersion in the step (1) is 10-12 hours; and an ultrasonic disperser is adopted for ultrasonic vibration dispersion.
The properties of GO thin films obtained by a series of methods such as a blade coating method and a suction filtration method in the step (1) have no obvious difference.
The volume of the graphene oxide dispersion liquid subjected to suction filtration in the step (1) is 10mL, and the filter membrane is a mixed fiber membrane with the aperture of 0.45 mu m and the time is 3 d.
The properties of the rGO thin film obtained by thermal reduction or chemical agent reduction in the step (2) are not obviously different.
The thermal reduction temperature in the step (2) is 400-2800 ℃, and the thermal reduction time is 2 h.
The chemical reagent reduction in the step (2) is carried out by using 55% hydriodic acid, and the reduction time is 2 h.
The step (2) is washed by ethanol or water and comprises the following steps: washing with 95% ethanol or water, repeating for 2-3 times, wherein the washing time is 2 h.
And (4) in the step (3), the distance between the cathode and the anode is 1-2 cm.
In the step (3), the electrophoresis assembly takes ultrapure water (18.2 omega cm) as a medium, and other chemical reagents such as electrolyte and the like are not used.
The fluorocarbon polymer in the step (3) comprises a fluorocarbon polymer with-CF3A functional group-containing polymeric reagent.
The fluorocarbon polymer in the step (3) comprises perfluoropolyether PFPE or perfluorotetraglyme PFTG.
The invention provides a multi-band optical sensing device with a fluorocarbon polymer modified chemical conversion graphene/zinc oxide film shape, which is obtained by attaching zinc oxide on a chemical conversion graphene (rGO) film by a reagent-free electrophoresis assembly method and then coating a layer of fluorocarbon polymer on the surface of the film, and can detect the optical responses with different illumination intensities.
Advantageous effects
(1) The method has the advantages of simple operation, convenient and quick preparation process, low cost and wide application prospect;
(2) the optical sensing device obtained by the invention has good flexibility and is suitable for application light in the wearable field;
(3) the optical sensing device obtained by the invention has good sensing performance in ultraviolet, visible and infrared bands, the signal-to-noise ratio of photocurrent signals is large, and the lower limit of light intensity detection is low.
Drawings
Fig. 1 is a schematic view of preparation (a) and photoelectric detection (b) of the chemically converted graphene/zinc oxide thin film in example 1; wherein, 1, a power supply; 2. chemically converting the graphene film; 3. a zinc block; 4. ultrapure water; 5. an electrochemical workstation; 6. a counter electrode; 7. a reference electrode; 8. a working electrode; 9. a computer; 10. copper foil; 11. a light source; 12. ZnO particles; 13. and chemically converting the graphene film.
Fig. 2 is an XRD pattern of the chemically converted graphene/zinc oxide thin film in example 1.
Fig. 3 is an SEM image of the chemically converted graphene/zinc oxide thin film in example 1.
FIG. 4 shows the rGO film, ZnO/rGO film and PFPE coated ZnO/rGO film of example 1 at 0.4V bias and 7.63mW/cm light intensity2Time current curve of; (a) the time current contrast curve of the ZnO/rGO film and the rGO film, (b) the time current contrast curve before and after the PFPE is coated on the surface of the ZnO/rGO film, and (c) the time noise current contrast curve before and after the PFPE is coated on the surface of the ZnO/rGO film.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Weighing 300mg of graphene oxide at room temperature, placing the graphene oxide in a 200mL beaker, adding 100mL of distilled water to prepare a dispersion liquid with the concentration of 3mg/mL, and treating the dispersion liquid with an ultrasonic instrument for 10 hours to obtain 100mL of graphene oxide dispersion liquid; 10mL of graphene oxide dispersion liquid is measured and poured into a sand core funnel with the diameter of 4.5cm for suction filtration for 3d each time, and the graphene oxide film is obtained.
(2) And (2) placing the graphene oxide film obtained in the step (1) in a glass culture dish, adding 20mL of 55% hydriodic acid, sealing the culture dish by using the film, placing the culture dish in a dark place, taking out the film after 2 hours, soaking and washing the film for 3 times by using 95% ethanol, and drying to obtain the rGO film.
(3) And (3) by an electrophoresis assembly method, using a Zn foil as an anode in ultrapure water, using the rGO film in the step (2) as a cathode, enabling the distance between the two electrodes to be 1cm, applying a voltage of 25V/cm and a current of 1A, electrifying for 10min, taking out, and drying at room temperature to obtain the ZnO/rGO film. The size of the zinc oxide particles is 2 μm. Coating 0.1mL of PFPE by 1cm2The fluorocarbon polymer modified chemical conversion graphene/zinc oxide thin film is obtained, and the thickness of the thin film is 50 micrometers. Under the bias of 0.4V and the light intensity of 7.63mW/cm2Next, a time-current comparison curve (see fig. 4a) of the rGO film and the ZnO/rGO film coated with PFPE (by spin coating at a rotation speed of 400r/min) and a time-noise-current comparison curve (see fig. 4b) corresponding thereto were obtained, and the results showed that: the photocurrent of the ZnO/rGO film is greater than that of rGO, and the electrochemical noise of the ZnO/rGO film coated by the PFPE is lower than that of the ZnO/rGO film not coated by the PFPE, and the photocurrent is also slightly increased.
FIG. 2 shows that: the chemically converted graphene/zinc oxide has a peak at 24.2 ° 2 θ, and has five diffraction peaks at 31.45 °, 34.11 °, 35.98 °, 47.16 ° 2 θ, and 56.26 °, corresponding to the (100), (002), (101), (102), and (110) crystal planes of zinc oxide, respectively, and corresponding to the PDF #36-1451 card of ZnO.
FIG. 3 shows: and (3) generating shuttle-shaped ZnO particles on the surface of the rGO film through reagent-free electrophoresis.
Example 2
(1) Weighing 500mg of graphene oxide at room temperature, placing the graphene oxide in a 200mL beaker, adding 100mL of distilled water to prepare 5mg/mL dispersion liquid, and treating the dispersion liquid for 10.5 hours by using an ultrasonic instrument to obtain 100mL of graphene oxide dispersion liquid; 10mL of graphene oxide dispersion liquid is measured and poured into a sand core funnel with the diameter of 4.5cm for suction filtration for 3d each time, and the graphene oxide film is obtained.
(2) And (2) placing the graphene oxide film obtained in the step (1) in a glass culture dish, adding 20mL of 55% hydriodic acid, sealing the culture dish by using the film, placing the culture dish in a dark place, taking out the film after 2 hours, soaking and washing the film for 3 times by using 95% ethanol, and drying to obtain the rGO film.
(3) And (3) adopting an electrophoresis assembly method, using a Zn foil as an anode in ultrapure water, using the rGO film in the step (2) as a cathode, enabling the distance between the two electrodes to be 1.5cm, applying a voltage of 15V/cm and a current of 1A, electrifying for 1 hour, taking out, and drying at room temperature to obtain the ZnO/rGO film. Coating 0.1mL of PFPE by 1cm2And obtaining the fluorocarbon polymer modified chemically converted graphene/zinc oxide film. Under the bias of 0.4V and the light intensity of 7.63mW/cm2Then, a time current contrast curve and a time noise current contrast curve of the rGO film, the ZnO/rGO film and the ZnO/rGO film coated by PFPE (spin coating at a rotating speed of 400r/min) are obtained, and the results show that: the photocurrent of the ZnO/rGO film is greater than that of rGO, and the electrochemical noise of the ZnO/rGO film coated by the PFPE is lower than that of the ZnO/rGO film not coated by the PFPE, and the photocurrent is also slightly increased.
Example 3
(1) Weighing 600mg of graphene oxide at room temperature, placing the graphene oxide in a 200mL beaker, adding 100mL of distilled water to prepare 6mg/mL dispersion liquid, and treating the dispersion liquid for 11 hours by using an ultrasonic instrument to obtain 30mL of graphene oxide coagulated slurry; and carrying out blade coating on the coagulated slurry to obtain the graphene oxide film.
(2) And (2) putting the graphene oxide film obtained in the step (1) into a graphitization furnace, taking out the film after 2h at the temperature of 400 ℃, and cooling to room temperature to obtain the rGO film.
(3) And (2) adopting an electrophoresis assembly method, using a Zn foil as an anode and a rGO film as a cathode in ultrapure water, enabling the distance between the two electrodes to be 1cm, applying a voltage of 20V/cm and a current of 1A, electrifying for 0.5 hour, taking out, and drying at room temperature to obtain the ZnO/rGO film. Coating 0.1mL of PFPE by 1cm2And obtaining the fluorocarbon polymer modified chemically converted graphene/zinc oxide film. Under the bias of 0.4V and the light intensity of 11.21mW/cm2Then, a time current contrast curve and a time noise current contrast curve of the rGO film, the ZnO/rGO film and the ZnO/rGO film coated by PFPE (spin coating at a rotating speed of 400r/min) are obtained, and the results show that: the photocurrent of the ZnO/rGO film is larger than that of the rGO, and the electrochemical noise of the ZnO/rGO film coated by the PFPE is smaller than that of the ZnO/rGO film not coated by the PFPE, and the photocurrent is weakAnd (4) increasing.
Example 4
(1) Weighing 800mg of graphene oxide at room temperature, placing the graphene oxide in a 200mL beaker, adding 100mL of distilled water to prepare 8mg/mL dispersion liquid, and treating the dispersion liquid for 11.5 hours by using an ultrasonic instrument to obtain 30mL of graphene oxide slurry; and carrying out blade coating on the coagulated slurry to obtain the graphene oxide film.
(2) And (2) putting the graphene oxide film obtained in the step (1) into a graphitization furnace, taking out the film after 2h at 1600 ℃, and cooling to room temperature to obtain the rGO film.
(3) And (2) adopting an electrophoresis assembly method, using a Zn foil as an anode and a rGO film as a cathode in ultrapure water, enabling the distance between the two electrodes to be 1.5cm, applying a voltage of 20V/cm and a current of 1A, electrifying for 1 hour, taking out, and drying at room temperature to obtain the ZnO/rGO film. Coating 0.1mL of PFTG 1cm2And obtaining the fluorocarbon polymer modified chemically converted graphene/zinc oxide film. Under the bias voltage of 0.4V and the light intensity of 14.92mW/cm2Then, a time current comparison curve and a time noise current comparison curve of the rGO film, the ZnO/rGO film and the ZnO/rGO film coated by PFTG (spin coating at a rotating speed of 400r/min) are obtained, and the results show that: the photocurrent of the ZnO/rGO film is greater than that of the rGO, and the electrochemical noise of the PFTG-coated ZnO/rGO film is lower than that of the ZnO/rGO film which is not coated with the PFTG.
Example 5
(1) Weighing 1000mg of graphene oxide at room temperature, placing the graphene oxide in a 200mL beaker, adding 100mL of distilled water to prepare a dispersion liquid with the concentration of 10mg/mL, and treating the dispersion liquid for 12 hours by using an ultrasonic instrument to obtain 30mL of graphene oxide coagulated slurry; and carrying out blade coating on the coagulated slurry to obtain the graphene oxide film.
(2) And (2) putting the graphene oxide film obtained in the step (1) into a graphitization furnace, taking out the film after 2h at the temperature of 2800 ℃, and cooling to room temperature to obtain the rGO film.
(3) And (2) adopting an electrophoresis assembly method, taking a Zn foil as an anode in ultrapure water, taking a rGO film as a cathode, applying a voltage of 5V/cm and a current of 1A for 2 hours, electrifying for 2 hours, taking out, and drying at room temperature to obtain the ZnO/rGO film. ZnO/rGO films are respectively biased at 0.4V and have wavelengths of 365, 532 and 808nm, light intensity of 6mW/cm2The time current curve is obtained under the irradiation of the light source, and the result shows that: because the light responsivity of the ZnO/rGO film with different wavelengths is different, the ZnO/rGO film can generate different photocurrents under the irradiation of light sources with different wavelengths, and the light source wavelength can be detected according to the photocurrents.
Claims (4)
1. A preparation method of a fluorocarbon polymer modified chemical conversion graphene/zinc oxide film-shaped multiband optical sensing device is characterized in that a reagent-free electrophoretic assembly method is used for preparing chemical conversion graphene/zinc oxide film ZnO/rGO; coating a fluorocarbon polymer on the surface of a chemical conversion graphene/zinc oxide film, wherein the fluorocarbon polymer comprises perfluoropolyether PFPE or perfluorotetraglyme PFTG, and shuttle-shaped ZnO particles are generated on the surface of the rGO film through reagent-free electrophoresis.
2. The method of claim 1, wherein the assembly method using reagent-free electrophoresis is: taking zinc as an anode and a chemical conversion graphene film as a cathode, performing direct current electrophoresis deposition, and performing electrophoresis at room temperature for more than 10min to obtain the chemical conversion graphene/zinc oxide film, wherein the electric field intensity of the direct current electrophoresis deposition is 5-25V/cm, and the electrolyte is ultrapure water.
3. The method according to claim 2, wherein the method for preparing the chemically converted graphene thin film comprises: preparing a graphene oxide film from the graphene oxide dispersion liquid, carrying out thermal reduction or chemical reduction on the graphene oxide film, washing, and drying to obtain the chemically converted graphene film.
4. The preparation method according to claim 3, wherein the graphene oxide film is obtained by a doctor blade method or a suction filtration method.
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