CN109904243B - Paper-like base flexible ultraviolet light detector based on interface optimization and preparation method thereof - Google Patents
Paper-like base flexible ultraviolet light detector based on interface optimization and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a paper-like flexible ultraviolet detector based on interface optimization and a preparation method thereof3The nano-film layer is respectively used as a bottom electrode layer, a light sensing layer and an interface optimization layer in CsPbBr3The top of the nano-film layer is attached with single-layer graphene serving as a transparent electrode to construct a nano-film structure with silver nanowires/zinc oxide nanowires/CsPbBr3Provided is a flexible ultraviolet detector with a nano-sheet/graphene structure. The solution method device construction process used by the invention has the advantages of simple process steps, low cost and the potential of large-area industrial mass production, and the prepared paper-like flexible ultraviolet detector has higher ultraviolet response and stable light response performance.
Description
Technical Field
The invention relates to the technical field of ultraviolet detection, in particular to a paper-like base flexible ultraviolet detector based on interface optimization and a preparation method thereof.
Background
In recent years, flexible optical detection equipment is widely applied to the fields of communication, health, safety and the like due to the excellent wearable characteristic, and ultraviolet optical detection equipment is successfully applied to a plurality of fields of optical communication, military detection, biosensing, ozone detection and the like due to the strong anti-interference capability and high detection sensitivity. The flexible wearable ultraviolet detector focuses on fibrous and fabric-shaped optical detectors at present, although a fibrous device can realize 360-degree optical detection, the mechanical strength of an inorganic optical sensing material layer directly grown on a flexible substrate is not high, the dynamic contact between the whole device and the interface of a flexible metal wire substrate in a bending state is weak, the flexible wearable application is difficult to realize, and similar problems exist in the derived fabric-shaped detector.
Chinese patent (CN201810318624.6) discloses a preparation method of an ultraviolet/infrared photoelectric detector based on a graphene-zinc oxide composite nano structure, which comprises the steps of printing graphene oxide on a flexible plastic PET substrate, reducing to form a Reduced Graphene Oxide (RGO) film, preparing a zinc oxide nano array by using a hot solution method to form a zinc oxide seed layer, and completing the preparation of an ultraviolet sensor. Chinese patent (CN201810454313.2) discloses an ultraviolet detector with a Cu/CuI/ZnO structure and a preparation method thereof, wherein a layer of copper nanowire (Cu NWs) conductive network film is deposited on a flexible transparent substrate by spraying, a Cu/CuI structure is obtained after iodination, then a seed crystal of zinc oxide is pre-grown on the substrate by a sol-gel method, an active layer of a zinc oxide nano material is obtained by low-temperature hydrothermal, and then an electrode layer is covered to finish the preparation of an ultraviolet sensor.
According to the method, flexible plastics such as PET (polyethylene terephthalate) are used for replacing a metal wire substrate to construct the device, the overall flexibility of the device is improved, flexible wearable application can be realized, the active layer material is directly grown on the flexible substrate by using a low-temperature hydrothermal method, and the problems that the mechanical strength of a thin film layer is not high, the process flow is relatively complex, and the industrial mass production cannot be compatible exist.
Disclosure of Invention
The invention aims to provide a paper-like base flexible ultraviolet light detector based on interface optimization and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows: a paper-like base flexible ultraviolet light detector based on interface optimization takes a porous filter membrane as a flexible substrate, and a silver nanowire thin film layer, a zinc oxide nanowire thin film layer and CsPbBr are sequentially arranged on the substrate3The nano-film layer is respectively used as a bottom electrode layer, a light sensing layer and an interface optimization layer in CsPbBr3And single-layer graphene is attached to the top of the nanosheet film layer to serve as a transparent electrode.
A preparation method of a paper-like base flexible ultraviolet light detector based on interface optimization is characterized by comprising the following steps:
step 1, taking a silver nanowire isopropanol solution, a zinc oxide nanowire isopropanol solution and CsPbBr3Uniformly dispersing a nanosheet toluene solution by ultrasonic waves for later use;
step 2, taking a polyvinylidene fluoride (PVDF) porous filter membrane as a flexible substrate, infiltrating the PVDF porous filter membrane with isopropanol, and adsorbing the PVDF porous filter membrane on the top of a conical flask of a vacuum filtration system;
and 3, opening a vacuum pump of the vacuum filtration system, respectively carrying out suction filtration on the solution with uniform ultrasonic dispersion, and sequentially constructing a silver nanowire film, a zinc oxide nanowire film and CsPbBr on the surface of the porous filter membrane3Drying the filter membrane substrate;
step 4, in CsPbBr3And (3) attaching a single-layer graphene film on the top of the nanosheet film layer to serve as a transparent electrode, and drying to prepare the paper-like flexible ultraviolet detector.
Compared with the prior art, the invention has the following remarkable advantages: 1) the invention uses CsPbBr3The nano sheet has high light absorption coefficient and high carrier mobility, can collect light to a greater extent for optical detection, is regular and flat in material, is beneficial to forming a compact film, fills holes existing in a zinc oxide nano wire layer, smoothes contact with a graphene electrode, and increases a carrier transmission path in a device; 2) according to the invention, the single-layer graphene film is used as the top transparent electrode, and due to the super-flexible characteristic, the contact between the single-layer graphene film and the functional layer is tighter, the contact defects are fewer, the transmission of current carriers is further promoted, and the flexible detector obtains a faster response speed and a higher on-off ratio; 3) the solution method device construction process used by the invention has the advantages of simple process steps and low cost, and has the potential of large-area industrial mass production.
Drawings
Fig. 1 is a schematic structural diagram of a paper-like base flexible ultraviolet light detector based on interface optimization.
Fig. 2 is a microstructure SEM image of the uv light detector of example 1.
Fig. 3 is a graph showing the current-voltage characteristics of the uv detector of example 1 in the absence of light and under irradiation with 320nm light.
FIG. 4 is a graph showing the optical response of the test device of the UV detector of example 1 under 320nm illumination and an applied bias of-8V.
Fig. 5 is a graph showing the current-voltage characteristics of the uv detector of example 2 in the absence of light and under irradiation with 320nm light.
FIG. 6 is a graph showing the optical response of the test device of the UV detector of example 2 under 320nm illumination and an applied bias of-8V.
Fig. 7 is a graph of the optical response curves of the test device under the irradiation of ultraviolet light with a wavelength band of 320nm under an external bias voltage of-8V at different bending angles (0 °, 30 °, 90 ° and 120 °) in the ultraviolet light detector of example 3.
Fig. 8 is a graph comparing current values of the devices in the presence and absence of light for a plurality of bending cycles with an applied bias voltage of-8V for the uv detector of example 3.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings.
A paper-like base flexible ultraviolet light detector based on interface optimization is characterized in that a porous filter membrane is used as a flexible substrate, and a silver nanowire thin film layer, a zinc oxide nanowire thin film layer and CsPbBr are sequentially prepared on the flexible substrate3The nano-film layer is respectively used as a bottom electrode layer, a light sensing layer and an interface optimization layer in CsPbBr3And single-layer graphene is attached to the top of the nanosheet film layer to serve as a transparent electrode.
As a preferred embodiment, the flexible substrate adopts a polyvinylidene fluoride (PVDF) porous filter membrane with the pore diameter of 1.5-5 μm.
As a preferred embodiment, the diameter of a single silver nanowire of the silver nanowire thin film layer is 20 nm-100 nm.
In a preferred embodiment, the thickness of the zinc oxide nanowire thin film layer is 2 to 5 μm, the length of a single zinc oxide nanowire on the zinc oxide nanowire thin film layer is 10 to 100 μm, and the diameter of the zinc oxide nanowire thin film layer is 50 to 100 nm.
As a preferred embodiment, the CsPbBr is3The thickness of the nano-sheet film layer is 100 nm-300 nm, and CsPbBr is arranged on the nano-sheet film layer3The nano sheet is in a regular rectangle, and the size range is as follows: the length is 0.2-1 μm, and the width is 0.2-1 μm.
A preparation method of a paper-like base flexible ultraviolet light detector based on interface optimization is characterized by comprising the following steps:
step (ii) of1. Taking silver nanowire isopropanol solution, zinc oxide nanowire isopropanol solution and CsPbBr3Uniformly dispersing a nanosheet toluene solution by ultrasonic waves for later use;
step 2, taking a polyvinylidene fluoride (PVDF) porous filter membrane as a flexible substrate, infiltrating the PVDF porous filter membrane with isopropanol, and adsorbing the PVDF porous filter membrane on the top of a conical flask of a vacuum filtration system;
and 3, opening a vacuum pump of the vacuum filtration system, respectively carrying out suction filtration on the solution with uniform ultrasonic dispersion, and sequentially constructing a silver nanowire film, a zinc oxide nanowire film and CsPbBr on the surface of the porous filter membrane3Drying the filter membrane substrate;
step 4, in CsPbBr3And (3) attaching a single-layer graphene film on the top of the nanosheet film layer to serve as a transparent electrode, and drying to prepare the paper-like flexible ultraviolet detector.
In a preferred embodiment, the pore size of the polyvinylidene fluoride (PVDF) porous filter membrane is 1.5-5 μm.
As a preferable embodiment, the concentration of the silver nanowire isopropanol solution is 0.02 mg/mL-1 mg/mL, and the diameter of a single silver nanowire is 20 nm-100 nm.
In a preferable embodiment, the length of each zinc oxide nanowire in the isopropanol solution of the zinc oxide nanowire is 10 to 100 micrometers, the diameter of each zinc oxide nanowire is 50 to 100nm, and the thickness of the prepared zinc oxide nanowire film is 2 to 5 micrometers.
As a preferred embodiment, the CsPbBr is3CsPbBr in nanosheet toluene solution3The nano sheet is in a regular rectangle, and the size range is as follows: 0.2-1 μm long and 0.2-1 μm wide, prepared CsPbBr3The thickness of the layer of the nano-sheet film is 100 nm-300 nm.
As a preferred embodiment, the drying temperature is 40 ℃ to 80 ℃.
The paper-like flexible ultraviolet detector based on interface optimization has high ultraviolet response and stable light response performance. To verify the effectiveness of the inventive protocol, the following experiment was performed.
Example 1
Referring to fig. 1, in the paper-like flexible ultraviolet light detector based on interface optimization, a porous filter membrane is used as a flexible substrate, and a solution suction filtration method is adopted to prepare a silver nanowire thin film layer, a zinc oxide nanowire thin film layer, and CsPbBr on the substrate3The nano-sheet film layer is respectively used as a bottom electrode layer, a light sensing layer and an interface optimization layer, then single-layer graphene is attached to the top of the interface optimization layer to be used as a transparent electrode, and the structure with silver nanowires/zinc oxide nanowires/CsPbBr is constructed3Provided is a flexible ultraviolet detector with a nano-sheet/graphene structure. The preparation method specifically comprises the following steps:
(1) adding 50ml of isopropanol solution into 1ml of zinc oxide nanowire solution, and uniformly dispersing by ultrasonic. The zinc oxide nanowires used had a length of 10 μm and a diameter of 50 nm. And adding 50ml of isopropanol solution into 1ml of silver nanowire solution, and uniformly dispersing by ultrasonic. The diameter of the single silver nanowire is 20 nm. 50ml of toluene solution is taken and CsPbBr is added30.5ml of nanosheet solution, and uniform ultrasonic dispersion. CsPbBr3The size of the nano-sheet is as follows: the length is 0.2 μm, and the width is 0.2 μm-0.5 μm.
(2) And (3) spreading a polyvinylidene fluoride (PVDF) porous filter membrane on the top end of a conical flask of a vacuum filtration system, and infiltrating the PVDF porous filter membrane with isopropanol to enable the filter membrane to be tightly adsorbed on the top of the conical flask. Opening a vacuum pump, sequentially carrying out suction filtration on the solution with uniform ultrasonic dispersion by a solution method to form a membrane, and sequentially constructing a silver nanowire film, a zinc oxide nanowire film and CsPbBr on the surface of the porous filter membrane3A nano-sheet film, and then drying the filter membrane substrate at 40 ℃; the aperture of the polyvinylidene fluoride (PVDF) porous filter membrane is 1.5 mu m, the thickness of the zinc oxide nanowire film is 2 mu m, and CsPbBr3The thickness of the nanosheet film layer is 100 nm. Finally, the filter substrate was dried at 40 ℃.
(3) Placing the graphene film on a sparse pore substrate, carrying out accurate transfer by adhering a Polystyrene (PS) film, and attaching the graphene film to CsPbBr3The top of the nano-sheet film layer is used as a transparent electrode, and then isopropanol is used for infiltrating the whole device, so that the graphene and CsPbBr are mixed3The nanosheet layers are in intimate contact. And (5) drying the device at 50 ℃ to complete the construction of the paper-like base flexible ultraviolet detector.
The base prepared in this exampleThe microstructure of the surface-optimized paper-like base flexible ultraviolet light detector is shown in figure 2. As can be seen from the figure, the structure of the device is respectively a silver nanowire layer, a zinc oxide nanowire layer and CsPbBr from bottom to top3A nanosheet layer. Zinc oxide nanowires and CsPbBr3The nano-sheets form a uniform film layer, and the zinc oxide nano-wires are buried in CsPbBr3In the nanosheet layer. CsPbBr3The nanosheet layer has the function of interface optimization, and the interface (the zinc oxide nanowire layer and CsPbBr) is promoted3Interface between nanosheets, CsPbBr3The interface between the nanosheet and the graphene) is in stable and intimate contact.
The paper-like flexible ultraviolet detector based on interface optimization prepared by the embodiment has high ultraviolet response and stable light response performance. Under the irradiation of ultraviolet light with different light intensities in 320nm wave bands in the absence of light, the characteristic curve of the relation between the current and the voltage of the detector is shown in figure 3, and it can be seen that the prepared device shows a typical rectification characteristic under the absence of light, which is caused by CsPbBr3The maximum photocurrent of the device can reach 8 × 10 under the power of 1.25mW due to a built-in electric field caused by a PN junction formed by the nanosheet layer and the graphene-6A, ratio to dark current of about 103. This illustrates ZnO/CsPbBr3The base photodetector has a high ultraviolet response. Under the irradiation of ultraviolet light with different light intensities in the 320nm wave band, the light response curves of the device in a plurality of light response periods under the external bias of-8V are shown in figure 4, and it can be seen that the prepared device can repeatedly reflect the switching of light and has stable light response performance.
Example 2
The structure of the paper-like flexible ultraviolet detector based on interface optimization in the embodiment is the same as that in embodiment 1, and the preparation method comprises the following steps:
(1) adding 50ml of isopropanol solution into 1ml of zinc oxide nanowire solution, and uniformly dispersing by ultrasonic. The zinc oxide nanowires used had a length of 50 μm and a diameter of 50 nm. And adding 50ml of isopropanol solution into 1ml of silver nanowire solution, and uniformly dispersing by ultrasonic. The diameter of the single silver nanowire is 50 nm. 50ml of toluene solution is taken and CsPbBr is added3Nanosheet solution0.5ml, and ultrasonic dispersion is uniform. CsPbBr3The size of the nano-sheet is as follows: the length is 0.5-1 μm, and the width is 0.5-1 μm.
(2) And (3) spreading a polyvinylidene fluoride (PVDF) porous filter membrane on the top end of a conical flask of a vacuum filtration system, and infiltrating the PVDF porous filter membrane with isopropanol to enable the filter membrane to be tightly adsorbed on the top of the conical flask. Opening a vacuum pump, sequentially carrying out suction filtration on the solution with uniform ultrasonic dispersion by a solution method to form a membrane, and sequentially constructing a silver nanowire film, a zinc oxide nanowire film and CsPbBr on the surface of the porous filter membrane3A nano-sheet film, and then drying the filter membrane substrate at 40 ℃; the aperture of the polyvinylidene fluoride (PVDF) porous filter membrane is 5 mu m, the thickness of the zinc oxide nanowire film is 3.5 mu m, and CsPbBr3The thickness of the nano-sheet film layer is 190 nm. Finally, the filter substrate was dried at 40 ℃.
(3) Placing the graphene film on a sparse pore substrate, carrying out accurate transfer by adhering a Polystyrene (PS) film, and attaching the graphene film to CsPbBr3The top of the nano-sheet film layer is used as a transparent electrode, and then isopropanol is used for infiltrating the whole device, so that the graphene and CsPbBr are mixed3The nanosheet layers are in intimate contact. And (5) drying the device at 50 ℃ to complete the construction of the paper-like base flexible ultraviolet detector.
The paper-like flexible ultraviolet detector based on interface optimization prepared by the embodiment has high ultraviolet response and stable light response performance. Under the irradiation of ultraviolet light with different light intensities in the wavelength band of 320nm and in the absence of light, the characteristic curve of the relationship between the current and the voltage of the detector is shown in fig. 5, and it can be seen that under the states of light and no light, the I-V characteristic curve of the optical detector shows obvious current value difference. The surface low conductive layer is thinned due to the desorption of oxygen ions on the surface of the zinc oxide light sensing layer under the irradiation of ultraviolet light, so that the current value under illumination is far greater than that under the non-illumination state. Therefore, the device prepared by the embodiment has good ultraviolet response performance. Under the irradiation of ultraviolet light with different light intensities in 320nm wave band, the light response curves of the device in a plurality of light response periods under the external bias voltage of-8V are shown in figure 6, it can be seen that the reproducibility of the highest value and the lowest value of the device current under the on state and the off state of the ultraviolet light detector is good, and the on-off ratio of the device under the 320nm illumination under the external bias voltage of-8V is about 103The light response performance is stable.
Example 3
The structure of the paper-like flexible ultraviolet detector based on interface optimization in the embodiment is the same as that in embodiment 1, and the preparation method comprises the following steps:
(1) adding 50ml of isopropanol solution into 1ml of zinc oxide nanowire solution, and uniformly dispersing by ultrasonic. The zinc oxide nanowires used had a length of 100 μm and a diameter of 100 nm. And adding 50ml of isopropanol solution into 1ml of silver nanowire solution, and uniformly dispersing by ultrasonic. The diameter of the single silver nanowire is 100 nm. 50ml of toluene solution is taken and CsPbBr is added30.5ml of nanosheet solution, and uniform ultrasonic dispersion. CsPbBr3The size of the nano-sheet is as follows: the length is 0.5-1 μm, and the width is 0.5-1 μm.
(2) And (3) spreading a polyvinylidene fluoride (PVDF) porous filter membrane on the top end of a conical flask of a vacuum filtration system, and infiltrating the PVDF porous filter membrane with isopropanol to enable the filter membrane to be tightly adsorbed on the top of the conical flask. Opening a vacuum pump, sequentially carrying out suction filtration on the solution with uniform ultrasonic dispersion by a solution method to form a membrane, and sequentially constructing a silver nanowire film, a zinc oxide nanowire film and CsPbBr on the surface of the porous filter membrane3A nano-sheet film, and then drying the filter membrane substrate at 40 ℃; the aperture of the polyvinylidene fluoride (PVDF) porous filter membrane is 5 mu m, the thickness of the zinc oxide nanowire film is 5 mu m, CsPbBr3The thickness of the nano-sheet film layer is 300 nm. Finally, the filter substrate was dried at 40 ℃.
(3) Placing the graphene film on a sparse pore substrate, carrying out accurate transfer by adhering a Polystyrene (PS) film, and attaching the graphene film to CsPbBr3The top of the nano-sheet film layer is used as a transparent electrode, and then isopropanol is used for infiltrating the whole device, so that the graphene and CsPbBr are mixed3The nanosheet layers are in intimate contact. And (5) drying the device at 50 ℃ to complete the construction of the paper-like base flexible ultraviolet detector.
The paper-like flexible ultraviolet light detector based on interface optimization prepared by the embodiment has good flexibility and stable light response performance. The light response curves of the device under different bending angles (0 degrees, 30 degrees, 90 degrees and 120 degrees) under the irradiation of 320nm waveband ultraviolet light under the condition of external bias voltage of-8V are shown in fig. 7, so that the light response performance change of the device under different bending angles (0 degrees, 30 degrees, 90 degrees and 120 degrees) of the light detector under the condition of external bias voltage of-8V is very small, the light response time and the switching ratio of the device are kept stable, and the light detector has high bending resistance and high stable light response performance. The current values of the device in the light and dark states under multiple bending periods when the bias voltage is applied to the device at-8V are shown in FIG. 8, and it can be seen that the dark current is always stable under multiple bending periods, and after 500 bending periods, the photocurrent still maintains 93% of the initial value. This is sufficient to demonstrate the high cycling stability of the device in the bent state.
In addition, in order to prepare the ultraviolet light detector meeting different application scenes, preparation parameters can be adjusted to reach different indexes.
Claims (10)
1. The flexible ultraviolet light detector based on interface optimization is characterized in that a porous filter membrane is used as a flexible substrate, and a silver nanowire thin film layer, a zinc oxide nanowire thin film layer and CsPbBr are sequentially arranged on the flexible substrate3The nano-film layer is respectively used as a bottom electrode layer, a light sensing layer and an interface optimization layer in CsPbBr3And single-layer graphene is attached to the top of the nanosheet film layer to serve as a transparent electrode.
2. The interface optimization-based flexible ultraviolet light detector as claimed in claim 1, wherein the flexible substrate is a polyvinylidene fluoride (PVDF) porous filter membrane with a pore size of 1.5 μm to 5 μm.
3. The interface optimization-based flexible ultraviolet light detector according to claim 1, wherein the diameter of a single silver nanowire of the silver nanowire thin film layer is 20nm to 100 nm.
4. The interface optimization-based flexible ultraviolet light detector of claim 1, wherein the thickness of the zinc oxide nanowire thin film layer is 2 μm to 5 μm, the length of a single zinc oxide nanowire on the zinc oxide nanowire thin film layer is 10 μm to 100 μm, and the diameter of the zinc oxide nanowire thin film layer is 50nm to 100 nm.
5. The interface optimization-based flexible ultraviolet light detector of claim 1, wherein the CsPbBr is configured to be a single chip3The thickness of the nano-sheet film layer is 100 nm-300 nm, and CsPbBr is arranged on the nano-sheet film layer3The nano-sheet is regular rectangle, the length is 0.2-1 μm, and the width is 0.2-1 μm.
6. The preparation method of the flexible ultraviolet light detector based on interface optimization is characterized by comprising the following steps:
step 1, taking a silver nanowire isopropanol solution, a zinc oxide nanowire isopropanol solution and CsPbBr3Uniformly dispersing a nanosheet toluene solution by ultrasonic waves for later use;
step 2, taking a polyvinylidene fluoride (PVDF) porous filter membrane as a flexible substrate, infiltrating the PVDF porous filter membrane with isopropanol, and adsorbing the PVDF porous filter membrane on the top of a conical flask of a vacuum filtration system;
and 3, opening a vacuum pump of the vacuum filtration system, respectively carrying out suction filtration on the solution with uniform ultrasonic dispersion, and sequentially constructing a silver nanowire film, a zinc oxide nanowire film and CsPbBr on the surface of the porous filter membrane3Drying the filter membrane substrate;
step 4, in CsPbBr3And (3) attaching a single-layer graphene film on the top of the nanosheet film layer to serve as a transparent electrode, and drying to prepare the flexible ultraviolet detector.
7. The method according to claim 6, wherein the pore size of the polyvinylidene fluoride (PVDF) porous filter membrane is 1.5-5 μm.
8. The preparation method of claim 6, wherein the concentration of the isopropanol solution of the silver nanowires is 0.02 mg/mL-1 mg/mL, and the diameter of each silver nanowire is 20 nm-100 nm.
9. The preparation method of claim 6, wherein the length of the single zinc oxide nanowire in the isopropanol solution of the zinc oxide nanowire is 10 to 100 μm, the diameter of the single zinc oxide nanowire is 50 to 100nm, and the thickness of the prepared zinc oxide nanowire film is 2 to 5 μm.
10. The method of claim 6, wherein CsPbBr is added3CsPbBr in nanosheet toluene solution3The nano-sheet is in a regular rectangle, the length of the nano-sheet is 0.2-1 mu m, the width of the nano-sheet is 0.2-1 mu m, and the prepared CsPbBr3The thickness of the layer of the nano-sheet film is 100 nm-300 nm.
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