CN115389016A - Artificial eye film and preparation method thereof - Google Patents
Artificial eye film and preparation method thereof Download PDFInfo
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- CN115389016A CN115389016A CN202210981240.9A CN202210981240A CN115389016A CN 115389016 A CN115389016 A CN 115389016A CN 202210981240 A CN202210981240 A CN 202210981240A CN 115389016 A CN115389016 A CN 115389016A
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- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J1/00—Photometry, e.g. photographic exposure meter
- G01J1/42—Photometry, e.g. photographic exposure meter using electric radiation detectors
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- Spectroscopy & Molecular Physics (AREA)
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Abstract
The invention belongs to the technical field of light source detection, and relates to an artificial eye film and a preparation method thereof, which can realize image capture of a three-dimensional curved surface. The invention comprises a transparent flexible substrate, a perovskite-PEGDMA photosensitive array, a metal electrode and a circuit thereof, and a transparent flexible film comprising the flexible substrate, the perovskite-PEGDMA photosensitive array, the metal electrode and a circuit thereof, and a flexible film package. The present invention forms a pixel array by directly irradiating a material having ultraviolet curing characteristics with ultraviolet light, and realizes direct photolithography on the material without performing additional steps of protection, etching, transfer, or lamination by using a photoresist. The prepared sensing unit has small volume and can realize more precise light pattern detection. The artificial eye film provided by the invention is sensitive in response, high in strength, small in volume, light in weight and excellent in image detection capability.
Description
Technical Field
The invention belongs to the technical field of light source detection, and relates to an artificial eye film and a preparation method thereof, which can realize image capture of a three-dimensional curved surface.
Background
The detection of light is one of important research fields, and has wide application prospect for detecting the shape of emitted light. The perovskite material is an advanced photoelectronic device material, has good band gap and corresponding speed, has good photoresponse characteristic, and is widely used in the field of optical detectors. And can exert good effect on a curved surface. The perovskite is adopted as the artificial eye material, so that the perovskite has a wide prospect.
Currently, practical application of perovskite flexible eyes faces two major problems: 1. identify the pixel as low; 2. the device stability is poor. In the process of preparing the artificial eye by using the perovskite, the perovskite is difficult to be compatible with a photoetching technology, and the preparation of the pixel points of the artificial eye can only be carried out by a liquid method, so that the pixel points of the artificial eye prepared by using the perovskite are larger, and the resolution ratio of the same area is lower. Furthermore, since the poor stability of perovskites themselves limits the wider range of applications of perovskites, perovskites are susceptible to phase transitions due to decomposition of their compounds under ambient conditions or to temperature changes.
Polyethylene glycol dimethacrylate (PEGDMA) is a cross-linking agent widely used, widely used in researches such as biomaterials, in-vivo drug delivery and biodegradable networks in the medical field, has certain photocuring characteristic, and can be cured into water-insoluble solid under the irradiation of ultraviolet light. In the existing research, a nontoxic and stable perovskite optical detection device is prepared by using the characteristics of the perovskite optical detection device, but the prepared device has a simple structure and cannot realize the functions of image recognition, bending and the like. But the photocuring capability of the material has application prospect in the field of photoetching.
In the prior art, the term "Ultrathin and compatible Lead Halide Perovskite photo detectors for porous Application in the form of a Retina-Like Vision Sensing" refers to Perovskite-prepared artificial eyes, but is limited by the fact that perovskites cannot be used for high levels of Perovskite productionThe shape of the precision is carved, and only a device with larger pixel points can be prepared by a drop casting method, namely Nanometer-Thick Cs 2 SnI 6 Perovskite-Polyethylene glycol dimethacrylate Composite Films for high level Stable Broad-Band photoresists are used for preparing the optical sensor, and the device can detect the illumination intensity but does not have flexibility and patterning capability, so that the Perovskite material has the photoetching capability by using the PEGDMA material, thereby preparing the optical eye device with higher precision.
Disclosure of Invention
In order to solve the above problems, the present invention provides a structure of an artificial eye which can be manufactured by photolithography and a method for manufacturing the same, and has the advantages of strong shape-distinguishing capability, high flexibility, sensitive response, high strength, small volume, light weight, and stable properties.
The technical purpose of the invention is realized by the following technical scheme:
an artificial eye film comprises a transparent flexible substrate, a perovskite-PEGDMA photosensitive array, metal electrodes and circuits thereof, and a transparent flexible film package; the perovskite-PEGDMA photosensitive array is positioned on the upper surface of the transparent flexible substrate, the metal electrode and the circuit thereof are plated on the perovskite-PEGDMA photosensitive array, and the transparent flexible film is packaged on the upper surface of the perovskite-PEGDMA photosensitive array to package the whole device.
The perovskite-PEGDMA photosensitive array is made of Cs 2 SnI 6 PEGDMA or CsPbI 3 -PEGDMA; wherein the perovskite is Cs 2 SnI 6 Or CsPbI 3 In order to realize the photocuring characteristic in the preparation process, the perovskite is mixed with a bonding agent PEGDMA.
The transparent flexible substrate and the transparent flexible film package are usually made of a transparent flexible organic polymer material with certain strength, such as poly (methyl methacrylate) -poly (n-butyl acrylate) -poly (methyl methacrylate) (PMMA-PnBA-PMMA) and parylene-c films.
The metal electrode and the electrode material in the circuit are Ag, au or pt, and the most preferable material is Au.
The thickness of the artificial eye membrane is 2 to 3 μm, and more preferably, the thickness is 2.4 μm.
The height of the perovskite-PEGDMA photosensitive array is 50-300 nm.
The thickness of the metal electrode and the electrode in the circuit is 30 nm-100 nm.
The thickness of the transparent flexible substrate and the transparent flexible film package is 1-1.5 μm.
The preparation method of the perovskite artificial film comprises the following steps:
step 1: cleaning a substrate: cleaning by standard cleaning process for use.
Step 2: a sacrificial layer, such as dextran, is deposited on the substrate for final removal of the flexible device.
And step 3: and depositing a transparent flexible substrate on the sacrificial layer to serve as a supporting substrate and a package.
And 4, step 4: preparing a photosensitive array on a transparent flexible substrate, wherein the layer preparation comprises the following parts:
(1) And fully mixing the perovskite with the connecting agent, and performing spin coating on the transparent flexible substrate to obtain a layer of perovskite ultraviolet curing polymer.
(2) And irradiating the prepared perovskite ultraviolet light curing polymer through the mask plate by using ultraviolet light to cure each pixel point.
(3) And washing the ultraviolet curing polymer in the uncured area by using an organic solvent, wherein the rest part is the photoetching perovskite layer, and thus the perovskite-PEGDMA photosensitive array is obtained.
And 5: and depositing a layer of metal electrode on the perovskite-PEGDMA photosensitive array, and using a mask plate during deposition to form a corresponding circuit at the same time.
And 6: and depositing a layer of transparent flexible film package above the perovskite-PEGDMA photosensitive array.
And 7: the entire device is removed from the substrate.
In the step (1), the selected substrate can be silicon, silicon dioxide or polyimide film. The ultrasonic cleaning time is 10-20 min, and the ultrasonic frequency is 40-100 Hz. More preferably, the ultrasonic cleaning time is 15min, and the ultrasonic frequency is 70Hz.
In the step (2), the sacrificial layer is prepared by dissolving dextran in deionized water, wherein the concentration of the dissolved dextran is (1/6 g-2/3)/ml, stirring the mixture until the dextran is completely dissolved, uniformly spreading the mixture on the surface of a substrate, and drying the substrate at the temperature of 65-100 ℃.
In the steps (3) and (6), if the transparent flexible substrate and the transparent flexible film packaging material are PMMA-PnBA-PMMA, the PMMA-PnBA-PMMA is dissolved in 2-ethyl-1-hexanol or n-butyl alcohol at the temperature of 70-90 ℃ and the mass fraction is 10-40%, and then the PMMA-PnBA-PMMA is flatly laid on the surface of glucan until the glucan is solidified into gel; more preferably, the mass fraction is selected to be 30%; if the parylene-c film is selected, the parylene-c film is evaporated and deposited at the temperature of 165-175 ℃ by adopting a vacuum deposition technology.
In the step (4), the perovskite is CsPbI respectively 3 Or Cs 2 SnI 6 (ii) a The corresponding prepolymers are CsI and PbI respectively 2 And HI, and CsI and SnI 2 (ii) a The molar ratio of the corresponding pre-polymer is CsI to PbI respectively 2 HI = l (0.5-1.5) and CsI SnI 2 (0.5-1.5), mixing the perovskite solution and PEGDMA according to a proportion to obtain a perovskite solution, and mixing the perovskite solution and the PEGDMA, wherein the mass fraction of the PEGDMA after mixing is 3-9%; then spin-coating the mixed solution of the perovskite solution and PEGDMA, wherein the spin-coating parameter is 2000 rmp-4000 rmp, and the spin-coating time is 30 s-50 s; when ultraviolet light is irradiated and cured, the wavelength of the ultraviolet light is 365nm, and the light intensity is 200-400 mW/cm 2 The energy of irradiation is 8000mJ/cm 2 Above, environmental conditions: the temperature is 20.50 +/-1.10 ℃, and the relative humidity is 26.81 +/-2.56%.
The working principle of the artificial eye of the invention is as follows: perovskites have a smaller bandwidth, so that electrons that cross the forbidden band become less energetic as free electrons, which are then energetic when irradiated with light. Therefore, current is generated in the loop, and the light source detection is realized by collecting the current change of each pixel point loop.
The invention has the beneficial effects that:
1. compared with a product prepared by a mould, the perovskite pixel array prepared by the method has smaller pixel point, denser pixels in unit area and higher resolution.
2. The invention uses Cs 2 SnI 6 The perovskite-polyethylene glycol dimethacrylate (PEGDMA) composite film reduces the toxicity of perovskite, improves the stability of perovskite and enables the perovskite to work for a longer time.
3. The invention utilizes the low bandwidth of perovskite, and the device has faster corresponding speed which can reach several milliseconds.
4. The invention can generate current in a loop when perovskite is irradiated, and whether the perovskite is irradiated or not and the illumination intensity are detected through the current change of different pixel points.
5. According to the invention, the perovskite is arranged into the pixel point array, the loop current change of each pixel point is detected, and the corresponding illumination pattern is reduced according to respective signals.
6. The invention has the advantages of thin total film layer, light weight and flexibility, and can be pasted on a curved surface without influencing the work of the curved surface.
7. The present invention forms a pixel array by directly irradiating a material having uv-curable properties with uv light, enabling direct lithography on the material without the need for additional protection, etching, transfer or lamination steps by using a photoresist.
Drawings
FIG. 1 is a circuit and pixel layout of the artificial eye membrane of the present invention.
FIG. 2 is a schematic view of a single pixel of the artificial eye membrane of the invention.
Fig. 3 is a schematic view showing the structure of the artificial eye membrane of the present invention.
FIG. 4 is a schematic view showing a process for preparing the artificial eye membrane of the present invention.
Figure 5 is a graph of the light sensitivity of the artificial eye membrane of the present invention in various states of flexion.
Figure 6 is a graph of the light sensitivity of the artificial eye membrane of the present invention at different illumination intensities.
Figure 7 is a response time and decay time test of the artificial eye membrane of the present invention.
In the figure: 1 a transparent flexible substrate; 2 perovskite-PEGDMA photosensitive array; 3 metal electrodes and their circuits; 4, packaging by using a transparent flexible film; a, preparing a substrate; b, preparing a photosensitive array; c, preparing an electrode circuit; d, preparing and packaging; and e, taking down the device.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
As shown in fig. 1-3, an artificial eye membrane of the present invention comprises a transparent flexible substrate 1, a perovskite-PEGDMA photosensitive array 2, metal electrodes and their circuitry 3, and a transparent flexible membrane 4; the preparation process is shown in figure 4. The invention is made of flexible materials and has stronger deformability, wherein the transparent flexible substrate 1 and the transparent flexible film 4 have higher strength and better stretchability, and other devices also have certain deformability and extensibility, so that the whole device can still keep normal work under the condition of larger deformation, and has the capability of easily sticking the device on a curved surface, such as the function of imitating eyes by sticking the device on the surface of a sphere. The metal electrode and its circuit 3 are divided into two parts, which are respectively contacted with perovskite-PEGDMA photosensitive array 2, respectively cathode and anode, and respectively lead out contact points for conveniently connecting to corresponding power supply and detecting loop current. When external light irradiates the perovskite-PEGDMA photosensitive array 2, current change can be generated in a short time, current change is generated, whether the pixel point is illuminated or not can be judged according to whether the current changes or not, the illumination intensity and the wavelength can also be judged according to the current change, and higher current corresponds to stronger illumination intensity and shorter wavelength. The loops formed by each pixel point are respectively numbered, the current of each numbered loop of the invention can be acquired in real time through a single chip microcomputer, and the current is transmitted to a corresponding analysis system for analysis so as to judge whether each pixel point is illuminated or not and judge the illumination intensity, and finally, the data can be transmitted to other equipment so as to realize related functions or the acquired illumination position and intensity are marked on a virtual array again through a mapping relation, so that the condition that the device is illuminated can be visually seen.
When the film is used, the film is adhered to the surface of an object to be subjected to illumination detection, the led gold electrodes are respectively connected to the positive electrode and the negative electrode of the voltage-stabilized power supply, the bias voltage is about 1V, at the moment, a device generates a basic current, and the current is taken as a reference, and the loop current of the illuminated pixel points is usually several times of the reference current. The analysis system judges the condition of illumination according to the relation between the loop current and the reference current, and outputs the detection result in a data or image mapping mode for further utilization.
Example 1:
the artificial eye of the embodiment sequentially comprises a flexible transparent substrate, a photosensitive array, an electrode and another flexible packaging layer.
In this embodiment, the substrate is silicon.
In this example, the thickness of PMMA-PnBA-PMMA was selected to be 1 μm for the transparent substrate and the package.
In this embodiment, the photosensitive array material is selected from CsPbI 3 PEGDMA, thickness 300nm.
In this example, au was selected for the electrodes, and the thickness was 30nm.
The method for preparing the artificial eye of the present embodiment includes the following steps:
(1) Preparing a substrate
And (2) carrying out ultrasonic cleaning on the silicon wafer for 10 minutes by sequentially using acetone, absolute ethyl alcohol, deionized water, hydrochloric acid, hydrofluoric acid and deionized water, wherein the ultrasonic frequency is 40Hz to remove organic matters, metal ions and an oxide layer remained on the surface of the silicon wafer, the solution of the next step is used for pre-washing each time when the solution is replaced, the silicon wafer is dried by nitrogen after cleaning is finished, so that deionized water stains on the surface of the silicon wafer are not remained, and the cleaned silicon wafer is placed into an ultraviolet ozone generator for plasma treatment for 5 minutes to improve the hydrophilicity and hydrophobicity of the surface.
(2) Plating of sacrificial layer
50g of dextran was dissolved in 300ml of deionized water, stirred at 1500rpm for 20 minutes, and then dropped on the silicon substrate prepared in step (1), and uniformly spread over the entire substrate with a dropper, after which it was completely dried at a temperature of 65 ℃ on a heat drying table.
(3) Preparation of the substrate
Dissolving PMMA-PnBA-PMMA in a 2-ethyl-1-hexanol solution with the mass fraction of 10%, stirring at the constant temperature of 1800rpm for 10 minutes at the temperature of 70 ℃, spreading the PMMA-PnBA-PMMA on the substrate prepared in the step (2) before cooling, sealing and standing the substrate for 24 hours, and fully cooling to form elastic gel on the sacrificial layer.
(4) Preparation of photosensitive arrays
CsI: pbI 2 HI = l:0.5, followed by adding PEGDMA such that the mass fraction of PEGDMA reaches 3%, followed by spin-coating the substrate prepared in step (3) at a spin-coating parameter of 4000rmp for a spin-coating time of 50s and a thickness of 50nm. Then passing through a mask plate with exposed pixels, and irradiating with light of 365nm and 400mW cm -2 The ultraviolet lamp irradiates for more than 20s, after the ultraviolet curing material is completely cured, acetone is used for slowly washing the uncured material, and then the ultraviolet lamp stands for 2h and is dried.
(5) Evaporation electrode
Evaporating gold electrode on the perovskite photosensitive array prepared in the step (4) by adopting a vacuum evaporation mode, wherein the gold material is powered by direct current, and the vacuum degree is lower than 2 multiplied by 10 -4 And evaporating a 30nm gold electrode in a Pa environment.
(6) Preparing flexible packages
Preparing new PMMA-PnBA-PMMA by the method of the step (3), flatly laying the PMMA-PnBA-PMMA on the electrode layer in the same way, and waiting for the PMMA-PnBA-PMMA to be cooled into gel.
(7) Removing device
And taking the device off the silicon substrate, lifting a non-functional corner of the device, and hanging the device down along the sacrificial layer by using a knife to obtain the prepared artificial eye film.
Example 2:
the artificial eye of the embodiment sequentially comprises a flexible transparent substrate, a photosensitive array, an electrode and another flexible packaging layer.
In this embodiment, the substrate is a polyimide film.
In this example, the transparent substrate and the package were selected to have a parylene-c film thickness of 1.5 μm.
In this embodiment, the photosensitive array material is selected from Cs 2 SnI 6 PEGDMA, thickness 150nm.
In this example, ag was selected as the electrode, and the thickness was 100nm.
The method for preparing the artificial eye of the embodiment comprises the following steps:
(1) Preparing a substrate
And (2) ultrasonically cleaning the silicon wafer for 20 minutes by sequentially using acetone, absolute ethyl alcohol, deionized water, hydrochloric acid, hydrofluoric acid and deionized water, wherein the ultrasonic frequency is 100Hz to remove organic matters, metal ions and oxide layers remained on the surface of the silicon wafer, the solution is pre-washed by using the solution of the next step each time, the silicon wafer is dried by using nitrogen after being cleaned, so that the surface of the silicon wafer is not stained by the deionized water, and the cleaned silicon wafer is placed into an ultraviolet ozone generator for plasma treatment for 10 minutes to improve the hydrophilic and hydrophobic properties of the surface.
(2) Plating of sacrificial layer
200g of dextran was dissolved in 300ml of deionized water, stirred at a rate of 300rpm for 10 minutes, and then dropped on the silicon substrate prepared in step (1), and uniformly spread over the entire substrate with a dropper, after which it was completely dried at a temperature of 100 ℃ on a heat drying table.
(3) Preparation of the substrate
Parylene-c was evaporated to a thickness of 1.5 μm using vacuum deposition technique at a temperature of 160 c to form a substrate of sufficient thickness.
(4) Preparation of photosensitive arrays
With CsI: snI 2 1.5, adding PEGDMA to make the mass fraction of PEGDMA reach 9%, and preparing the perovskite solution in the step (3)Spin coating on the substrate, wherein the spin coating parameter is 2000rmp, the spin coating time is 30s, and the thickness is 300nm. Then, a mask plate with the wavelength of 365nm and the illumination intensity of 200mW cm is used for exposing the pixel points -2 The ultraviolet lamp irradiates for more than 40s, after the ultraviolet curing material is completely cured, acetone is used for slowly washing the uncured material, and then the ultraviolet lamp stands for 2h and is dried.
(5) Evaporation electrode
Evaporating silver electrodes on the perovskite photosensitive array prepared in the step (4) in a vacuum evaporation mode, wherein the silver materials are supplied with direct current, and the vacuum degree is lower than 2 multiplied by 10 -4 And (3) evaporating a 100nm silver electrode in a Pa environment.
(6) Preparing flexible packages
Preparing another layer of poly-p-xylene-c film as the encapsulation of the device by the way of the step (3).
(7) Removing device
And taking the device off the silicon substrate, lifting a non-functional corner of the device, and hanging the device down along the sacrificial layer by using a knife to obtain the prepared artificial eye film.
Example 3:
the artificial eye of the embodiment sequentially comprises a flexible transparent substrate, a photosensitive array, an electrode and another flexible packaging layer.
In this embodiment, the substrate is silicon dioxide.
In this example, the thickness of PMMA-PnBA-PMMA is selected to be 1.2 μm for the transparent substrate and the package.
In this embodiment, the photosensitive array material is selected from CsPbI 3 PEGDMA, thickness 200nm.
In this example, au was selected as the electrode, and the thickness was 50nm.
The method for preparing the artificial eye of the embodiment comprises the following steps:
(1) Preparing a substrate
And (2) ultrasonically cleaning the silicon wafer for 15 minutes by sequentially using acetone, absolute ethyl alcohol, deionized water, hydrochloric acid, hydrofluoric acid and deionized water, wherein the ultrasonic frequency is 50Hz to remove organic matters, metal ions and oxide layers remained on the surface of the silicon wafer, the solution is pre-washed by using the solution of the next step each time, the silicon wafer is dried by using nitrogen after being cleaned, so that the surface of the silicon wafer is not stained by the deionized water, and the cleaned silicon wafer is placed into an ultraviolet ozone generator for plasma treatment for 10 minutes to improve the hydrophilic and hydrophobic properties of the surface.
(2) Plating of sacrificial layer
100g of dextran was dissolved in 300ml of deionized water, stirred at 1200rpm for 15 minutes, and then dropped on the silicon substrate prepared in step (1), and uniformly spread over the entire substrate with a dropper, after which it was completely dried at a temperature of 80 ℃ on a heat drying table.
(3) Preparation of the substrate
Dissolving PMMA-PnBA-PMMA in a 2-ethyl-1-hexanol solution with the mass fraction of 40%, stirring at the constant temperature of 1500rpm for 15 minutes at the temperature of 90 ℃, spreading the PMMA-PnBA-PMMA on the substrate prepared in the step (2) before cooling, sealing and standing the substrate for 24 hours, and fully cooling to form elastic gel on the sacrificial layer.
(4) Preparation of photosensitive arrays
CsI: pbI 2 HI = l:1.5, adding PEGDMA such that the mass fraction of PEGDMA is 5%, and spin-coating the substrate prepared in step (3) at a spin-coating parameter of 3000rmp for a spin-coating time of 40s and a thickness of 150nm. Then passing through a mask plate with exposed pixels, and irradiating with light of 365nm and 300 mW/cm -2 The ultraviolet lamp irradiates for more than 30s, after the ultraviolet curing material is completely cured, acetone is used for slowly washing the uncured material, and then the ultraviolet lamp stands for 2h and is dried.
(5) Evaporation electrode
Evaporating gold electrode on the perovskite photosensitive array prepared in the step (4) by adopting a vacuum evaporation mode, wherein the gold material is powered by direct current, and the vacuum degree is lower than 2 multiplied by 10 -4 And (3) evaporating a 50nm gold electrode in a Pa environment.
(6) Preparing flexible packages
Preparing new PMMA-PnBA-PMMA in the way of the step (3), laying the PMMA-PnBA-PMMA on the electrode layer in the same way, and waiting for the PMMA-PnBA-PMMA to be cooled into gel.
(7) Removing device
And taking the device off the silicon substrate, lifting a non-functional corner of the device, and hanging the device down along the sacrificial layer by using a knife to obtain the prepared artificial eye film.
The artificial eye film obtained in example 3 was subjected to photosensitivity in different bending states (light intensity of 6 mW. Cm) -2 ) And the results of the tests of the light sensitivity, the response time and the decay time under different illumination intensities are shown in fig. 5 to 7. As can be seen from the figure, the artificial eye membrane prepared by the invention has good bending performance, good photosensitive performance and shorter response time.
Claims (10)
1. An artificial eye membrane comprising a transparent flexible substrate, a perovskite-PEGDMA photosensitive array, metal electrodes and their circuitry, and a transparent flexible membrane encapsulation; the perovskite-PEGDMA photosensitive array is positioned on the upper surface of the transparent flexible substrate, the metal electrode and a circuit thereof are plated on the perovskite-PEGDMA photosensitive array, and the transparent flexible film is packaged on the upper surface of the perovskite-PEGDMA photosensitive array to package the whole device.
2. The artificial eye membrane of claim 1, wherein the perovskite-PEGDMA photosensitive array is Cs 2 SnI 6 PEGDMA or CsPbI 3 -PEGDMA。
3. An artificial eye membrane as claimed in claim 1 or 2, wherein the transparent flexible substrate and the transparent flexible membrane are encapsulated by PMMA-PnBA-PMMA or parylene-c membrane.
4. An artificial eye membrane as claimed in claim 1 or 2, wherein the metal electrode and its circuitry are made of Ag, au or pt.
5. An artificial eye membrane as claimed in claim 3, wherein the metal electrode and its circuitry are made of Ag, au or pt.
6. An artificial eye membrane according to claim 1, 2 or 5, wherein the artificial eye membrane has a thickness of 2 to 3 μm and the perovskite-PEGDMA photosensitive array has a height of 50 to 300nm; the thickness of the metal electrode and the electrode in the circuit is 30 nm-100 nm; the thickness of the transparent flexible substrate and the transparent flexible film package is 1-1.5 μm.
7. An artificial eye membrane according to claim 3, wherein the artificial eye membrane has a thickness of 2 to 3 μm, the perovskite-PEGDMA photosensitive array has a height of 50 to 300nm; the thickness of the metal electrode and the electrode in the circuit is 30 nm-100 nm; the thickness of the transparent flexible substrate and the transparent flexible film package is 1-1.5 mu m.
8. An artificial eye membrane according to claim 4, wherein the artificial eye membrane has a thickness of 2 to 3 μm, the perovskite-PEGDMA photosensitive array has a height of 50 to 300nm; the thickness of the metal electrode and the electrode in the circuit is 30 nm-100 nm; the thickness of the transparent flexible substrate and the transparent flexible film package is 1-1.5 mu m.
9. The process for producing the perovskite artificial film as set forth in any one of claims 1 to 8, characterized by comprising the steps of:
step 1: cleaning a substrate;
step 2: depositing a sacrificial layer on a substrate;
and step 3: depositing a layer of transparent flexible substrate on the sacrificial layer to serve as a supporting substrate and a package;
and 4, step 4: preparing a photosensitive array on a transparent flexible substrate, comprising the following steps of:
(4.1) fully mixing the perovskite with the connecting agent, and carrying out spin coating on the transparent flexible substrate to obtain a layer of ultraviolet curing polymer of the perovskite;
(4.2) irradiating the prepared perovskite ultraviolet curing polymer through a mask plate by using ultraviolet light to cure each pixel point;
(4.3) washing off the ultraviolet curing polymer in the uncured area by using an organic solvent, wherein the rest part is the photoetched perovskite layer, and obtaining the perovskite-PEGDMA photosensitive array;
and 5: depositing a layer of metal electrode on the perovskite-PEGDMA photosensitive array, and forming a corresponding circuit by using a mask plate during deposition;
step 6: depositing a layer of transparent flexible film package above the perovskite-PEGDMA photosensitive array;
and 7: the entire device is removed from the substrate.
10. The process for producing a perovskite artificial film according to claim 9,
in the step (1), the substrate is made of silicon, silicon dioxide or polyimide film; the ultrasonic cleaning time is 10-20 min, and the ultrasonic frequency is 40-100 Hz;
in the step (2), the sacrificial layer is dissolved in deionized water by dextran, the concentration of the dissolved dextran is (1/6 g-2/3)/ml, the dextran is stirred until the dextran is completely dissolved, the dextran is uniformly spread on the surface of the substrate, and the substrate is dried at the temperature of 65-100 ℃;
in the steps (3) and (6), if the transparent flexible substrate and the transparent flexible film packaging material are PMMA-PnBA-PMMA, the transparent flexible substrate and the transparent flexible film packaging material are dissolved in 2-ethyl-1-hexanol or n-butyl alcohol at the temperature of 70-90 ℃, the mass fraction is 10-40%, and then the transparent flexible substrate and the transparent flexible film packaging material are flatly laid on the surface of glucan until the glucan is solidified into gel; more preferably, the mass fraction is selected to be 30%; if the parylene-c film is selected, evaporating and depositing at 165-175 ℃ by adopting a vacuum deposition technology;
in the step (4), the perovskite is CsPbI respectively 3 Or Cs 2 SnI 6 (ii) a The corresponding pre-polymers are CsI and P respectivelybI 2 And HI, and CsI and SnI 2 (ii) a The molar ratio of the corresponding prepolymer is CsI to PbI respectively 2 HI = l (0.5-1.5) and CsI SnI 2 (0.5-1.5), mixing the perovskite solution and PEGDMA according to a proportion to obtain a perovskite solution, and mixing the perovskite solution and the PEGDMA, wherein the mass fraction of the PEGDMA after mixing is 3-9%; then spin-coating the mixed solution of the perovskite solution and PEGDMA, wherein the spin-coating parameter is 2000 rmp-4000 rmp, and the spin-coating time is 30 s-50 s; when the ultraviolet light is irradiated and cured, the wavelength of the ultraviolet light is 365nm, and the light intensity is 200-400 mW/cm 2 The energy of irradiation is 8000mJ/cm 2 Above, environmental conditions: the temperature is 20.50 +/-1.10 ℃, and the relative humidity is 26.81 +/-2.56%.
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