CN113013336A - Method for packaging organic photoelectric device based on composite material - Google Patents

Method for packaging organic photoelectric device based on composite material Download PDF

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CN113013336A
CN113013336A CN202110205202.XA CN202110205202A CN113013336A CN 113013336 A CN113013336 A CN 113013336A CN 202110205202 A CN202110205202 A CN 202110205202A CN 113013336 A CN113013336 A CN 113013336A
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layer
preparation
thickness
deposition
organic photoelectric
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吕宜璠
陈飞
卢泓
兰嫒
朱锦涛
张倬涵
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Shenzhen Oufude Photoelectricity Technology Co ltd
Nottingham Ningbo New Materials Institute Co ltd
University of Nottingham Ningbo China
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Shenzhen Oufude Photoelectricity Technology Co ltd
Nottingham Ningbo New Materials Institute Co ltd
University of Nottingham Ningbo China
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/80—Constructional details
    • H10K30/88—Passivation; Containers; Encapsulations
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention provides a method for packaging an organic photoelectric device based on a composite material, which comprises the following preparation steps: 1) preparing an anti-permeation compact layer film on the surface of the prepared organic photoelectric device, wherein the thickness is 2-100 nm; 2) preparing a hydrophobic layer film on the surface of the sample, wherein the thickness of the hydrophobic layer film is 1-20 nm; 3) repeating the steps 1) and 2) to prepare the multi-composite packaging layer, wherein the repetition times are more than or equal to 1. Compared with the prior art, the invention has the following beneficial effects: through the packaging engineering, the compactness of the metal oxide and the water resistance of the hydrophobic layer are combined, the water-oxygen resistance of the device is greatly improved, and the service life of the device stored in the air is prolonged; through the packaging engineering in the invention, due to excellent sealing performance, degradation reaction products are blocked in the device, so that the reaction can not continuously occur, the continuous degradation of the organic photoelectric device in a working environment (illumination and heat) is effectively prevented, and the service life of the device is prolonged.

Description

Method for packaging organic photoelectric device based on composite material
Technical Field
The invention relates to a method for packaging an organic photoelectric device based on a composite material, which comprises the selection of a packaging material and a preparation process of a composite packaging layer.
Background
In recent years, organic photoelectric materials and devices have attracted much attention due to their advantages such as low cost and high efficiency, but the organic materials themselves have a short lifetime and cannot be applied to commercialization due to their stability problems, such as perovskite solar cells. Perovskite solar cells have great potential value in industrial applications due to their high photoelectric conversion efficiency, directly tunable optical band gap, high hole/electron transport capability, low cost solution preparation, high crystallinity and certain flexibility. Through the efforts of researchers in several years, the photoelectric conversion efficiency of perovskite solar cells is improved from the initial 3.8% to 25.2%, and the perovskite solar cells are surpassed. Nevertheless, poor stability, short lifetime, etc. have greatly limited the commercial application of perovskite solar cells.
The working life of the perovskite solar cell is mainly determined by the stability of the perovskite layer and the sealing performance and the water and oxygen resistance of the whole device. In a perovskite solar cell device without protective measures, water and oxygen can easily reach the surface of the perovskite through holes in the transmission layer and decompose the perovskite, and under the working conditions of the device, light irradiation and heat cannot be avoided. These factors can degrade the perovskite layer, which causes the decrease of the photoelectric conversion efficiency of the device and shortens the service life of the device.
At present, methods related to prolonging the service life of perovskite solar cells mainly include: the crystal structure of the perovskite is changed by doping, using additives and the like, or the crystal structure is more stable; the sealing performance of the device is improved to improve the water and oxygen resistance of the device, and the means mainly comprise: using stable and compact transmission layer material and packaging; however, the adoption of these methods can make the preparation process of the perovskite device more complicated and less repeatable, and may damage the photoelectric conversion efficiency of the device, and finally, the improvement of the service life of the device is not enough to support the commercial application.
The deposition of the packaging layer on the surface of the device is also an effective method for delaying the degradation of the organic photoelectric material. Packaging techniques developed in recent years include: ultraviolet light curing and thermosetting epoxy resin, glass coating, oxide deposition, coating of water absorbing materials, hydrophobic organic matters and the like. The ultraviolet light curing and thermosetting epoxy resin is the most common packaging means, has the advantages of simple process and easy operation, can play a certain role in protecting the organic photoelectric material under low humidity, is a packaging means suitable for temporarily storing samples in the air, has obvious defects, and firstly, ultraviolet light and heat are factors capable of causing the decomposition of the organic photoelectric material, and the organic photoelectric material is easily degraded due to improper operation. For example, Ma et al (Advanced Energy Materials,2020,1902472) encapsulate perovskite solar cells with low cost uv curable glue and paraffin such that the devices retain 80% of their initial efficiency after 1000 hours of operation. Due to the fact that the compactness of the packaging layer is poor, water vapor invasion is difficult to completely block, and the packaging effect still has a space for improvement. Glass encapsulation typically uses a laser to locally heat the glass to the melting point ((ii))>380 deg.c) to completely encapsulate the electromechanical device, laser machining has the unique advantage of its accuracy, and the process can be used for the packaging of precision devices. But do notAlso, laser assisted glass encapsulation has its problems, and devices usually require pre-deposition of thermal insulation material to cope with the high temperature of laser processing before glass encapsulation, which undoubtedly increases the complexity of the encapsulation process and increases the manufacturing cost. Depositing dense, stable oxide film (Al)2O3、B2O3ZnO, etc.) are also effective packaging means, and the specific process method comprises the following steps: solution methods, chemical vapor deposition, atomic layer deposition, and the like, which have the lowest requirements for equipment but have a large number of defects, and vacuum deposition techniques such as chemical vapor deposition and atomic layer deposition are used to obtain an oxide thin film with very high quality. Lv et al (Acs Applied Materials)&Interfaces, 2018, 10(28):23928-23937) designs a novel stack structure of atomic layer deposition Al2O3Encapsulation layer (Al)2O3/Al2O3(TMA)/Al2O3). The intermediate of atomic layer deposition is used as a water absorption layer, and the waterproof performance of the oxide film is further improved. After the perovskite solar cell based on the composite packaging layer is stored for 1000 hours in an atmospheric environment, 97% of the initial efficiency can be still maintained. However, the problem of hydrophilicity of the encapsulating layer is not solved, and thus the encapsulating effect is lowered during long-term storage.
Recently, many organic or polymeric materials (PMMA, EVA, PVB, PVDF, etc.) have been used as hydrophobic or water-absorbing layers for the encapsulation of organic opto-electronic devices. Compared with oxide films, organic films have the following outstanding advantages: the preparation process is simple, the hydrophobicity is good, and the like, for example, Chenshufen et al (CN 201310018941) spin-coat the polystyrene xylene solution on the surface of the organic light-emitting device to prepare the hydrophobic packaging layer, so the anti-water oxygen capacity of the device is improved, but the packaging layer is prepared by a solution method, so that the organic packaging layer is easy to have more porous holes, the compactness is not good, and the problem to be solved in the organic film packaging technology is solved. Therefore, multilayer packaging combining compactness of inorganic materials and hydrophobicity of organic materials will be a research hotspot in the packaging direction, for example, an inorganic layer/organic layer overlapping packaging structure developed by xiekeefeng et al (chinese patent application CN2019103518250), which has a prominent packaging effect but a complex structure, a high preparation difficulty, low repeatability, more involved complex and expensive devices, a high preparation period, and is not favorable for commercial application. Moreover, the current packaging technology focuses on preventing the invasion of water and oxygen and neglects the escape of decomposition products in the device, and the multilayer packaging technology still has a space for further improvement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for encapsulating an organic photoelectric device based on a composite material.
The invention improves the packaging performance by combining a compact oxide material and a hydrophobic organic material. The key point and difficulty of the invention is that a high-quality impermeable compact oxide film is deposited on the surface of a hydrophobic material, and the high-quality multilayer composite packaging layer has excellent packaging performance.
The inventors have surprisingly found that the encapsulation technique of the invention also has the following unexpected technical effects:
firstly, the inner degradation product can be prevented from escaping except for the function of blocking external water vapor, and the reaction balance is pulled leftwards, so that the decomposition speed is slowed down;
and secondly, the packaging technology can remarkably and comprehensively improve the stability of the organic photoelectric device, and the performance of the device is hardly reduced in severe environments such as air environment, illumination, heating and even water soaking.
The technical scheme of the invention is as follows:
a method for encapsulating an organic photoelectric device based on a composite material comprises the following preparation steps:
1) preparing an anti-permeation compact layer film on the surface of the prepared organic photoelectric device, wherein the thickness is 2-100 nm;
2) preparing a hydrophobic layer film on the surface of the sample, wherein the thickness of the hydrophobic layer film is 1-20 nm;
3) repeating the steps 1) and 2) to prepare a multi-composite packaging layer, wherein the repetition times are more than or equal to 1;
the anti-seepage compact layer film material comprises one or more of aluminum oxide, titanium oxide, silicon oxide, tin oxide, nickel oxide and molybdenum oxide;
the hydrophobic layer film material comprises: one or more of polypropylene, polystyrene, polytetrafluoroethylene, perfluorohexaalkyl trichlorosilane, perfluorododecyl trichlorosilane, carbon nano tubes and array nano oxides.
In the invention, in the steps 1) and 2), the preparation method is one or more of an atomic layer deposition method, a hydrothermal method, a sol-gel method, a thermal evaporation deposition method, a chemical vapor deposition method, a plasma method and a template method, and the reaction temperature is not more than 100 ℃.
Preferably, the first and second electrodes are formed of a metal,
in the present invention,
in the step 1), the thickness of the anti-seepage compact layer film is 30 nm;
in the step 2), the thickness of the hydrophobic layer film is 2 nm;
in the step 3), the number of repetitions is 1.
More preferably still, the first and second liquid crystal compositions are,
in the preparation method, the organic photoelectric device is a perovskite solar cell, the anti-seepage compact layer film material is aluminum oxide, and the thickness of the film is 30 nm; the hydrophobic layer film material is perfluorododecyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
In the preparation method, the organic photoelectric device is a perovskite solar cell, the anti-seepage compact layer film material is titanium oxide, and the thickness of the film is 30 nm; the hydrophobic layer film material is perfluorododecyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
In the preparation method, the organic photoelectric device is a perovskite solar cell, the anti-seepage compact layer film material is aluminum oxide, and the thickness of the film is 30 nm; the hydrophobic layer film material is perfluorohexaalkyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
In the preparation method, the organic photoelectric device is an organic solar cell, the film material of the anti-seepage compact layer is aluminum oxide, and the thickness of the film is 30 nm; the hydrophobic layer film material is perfluorododecyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
In the preparation method, the organic photoelectric device is an organic fluorescent light emitting diode (OFED), the anti-permeation compact layer film material is aluminum oxide, and the thickness of the film is 30 nm; the hydrophobic layer film material is perfluorododecyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
The packaging method is suitable for comprehensively improving the stability of organic fluorescent light-emitting diodes, organic solar cells and perovskite solar cells, and comprises the water and oxygen resistance, high temperature resistance, radiation resistance and the like. The packaging method is suitable for packaging one or more of perovskite solar cells, perovskite light emitting diodes, perovskite lasers, perovskite photodetectors, organic light emitting diodes, organic field effect transistors, organic lasers, organic photodetectors, dye-sensitized solar cells and other photoelectric semiconductor devices.
Compared with the prior art, the invention has the following beneficial effects:
(1) through the packaging engineering, the compactness of the metal oxide and the water resistance of the hydrophobic layer are combined, the water-oxygen resistance of the device is greatly improved, and the service life of the device stored in the air is prolonged;
(2) through the packaging engineering in the invention, due to excellent sealing performance, degradation reaction products are blocked in the device, so that the reaction can not continuously occur, the continuous degradation of the organic photoelectric device in a working environment (illumination and heat) is effectively prevented, and the working life of the device is prolonged;
(3) the packaging process disclosed by the invention has the following characteristics: the device has good repeatability, does not damage the efficiency of the device, has wide application range and comprehensively improves the stability of the device.
(4) The detection results of the embodiments show that the encapsulation technology of the invention can significantly and comprehensively improve the stability of the organic photoelectric device, and even unexpectedly, the performance of the device is hardly reduced in severe environments such as air environment, illumination, heating and even water immersion.
Drawings
FIG. 1 is a schematic view of a process for encapsulating a perovskite solar cell with a composite encapsulation layer;
FIG. 2 is a structural diagram of a perovskite solar cell device and a packaging structure;
FIG. 3 is a scanning electron micrograph of a surface of atomic layer deposited alumina;
FIG. 4 is a water contact angle test of a perfluorododecyl trichlorosilane film;
FIG. 5 is a statistical plot of efficiency versus time for an unpackaged perovskite solar cell, a single composite layer (30nm alumina +2nm perfluorododecyl trichlorosilane layer), and a double composite layer encapsulated perovskite solar cell at storage conditions of 20 ℃ and 50% humidity;
FIG. 6 is a statistical plot of efficiency versus time for an unpackaged perovskite solar cell, a single composite layer (30nm alumina +2nm perfluorododecyl trichlorosilane layer), and a double composite layer-encapsulated perovskite solar cell at 60 ℃ in nitrogen storage;
FIG. 7 is a statistical graph of efficiency versus time for an unpackaged perovskite solar cell, a single composite layer (30nm alumina +2nm perfluorododecyl trichlorosilane) and a double composite layer encapsulated perovskite solar cell under one standard solar illumination and storage conditions in a nitrogen environment;
FIG. 8 is a statistical plot of efficiency versus time for an unpackaged perovskite solar cell, a single composite layer (30nm alumina +2nm perfluorododecyl trichlorosilane layer), and a double composite layer encapsulated perovskite solar cell at storage conditions of 85 ℃ and 85% humidity;
FIG. 9 is a comparison of voltage-current density curves before and after a perovskite solar cell encapsulated by a double composite layer is soaked in deionized water for 5 hours;
FIG. 10 is a comparison of aged, recovered voltage-current density curves for an unpackaged perovskite solar cell;
FIG. 11 is a comparison of the aging, recovery voltage-current density curves for a dual composite layer encapsulated perovskite solar cell;
FIG. 12 is a statistical plot of efficiency versus time for an unpackaged perovskite solar cell, a single composite layer (30nm titanium oxide +2nm perfluorododecyl trichlorosilane layer), and a double composite layer encapsulated perovskite solar cell at storage conditions of 20 ℃ and 50% humidity;
FIG. 13 is a statistical plot of efficiency versus time for an unpackaged perovskite solar cell, a single composite layer (30nm alumina +2nm perfluorohexaalkyltrichlorosilane layer), and a double composite layer encapsulated perovskite solar cell at storage conditions of 20 ℃ and 50% humidity;
FIG. 14 is a diagram of a structure of an organic solar cell device and a structure of a package;
FIG. 15 is a statistical plot of efficiency versus time for an unpackaged organic solar cell, a single recombination layer (30nm alumina +2nm perfluorododecyl trichlorosilane layer), and a double recombination layer encapsulated organic solar cell at 20 ℃ and 50% humidity storage conditions;
fig. 16 is a view showing a structure of an organic fluorescent light emitting diode device and a structure of a package;
FIG. 17 is a statistical graph of efficiency versus time for an unpackaged OLED, a single composite layer (30nm alumina +2nm perfluorododecyl trichlorosilane) and a double composite layer packaged OLED under blue light excitation.
Detailed Description
In order to illustrate the invention more clearly, the invention is further illustrated by the following specific examples, which are not intended to be limiting.
Example 1
The embodiment provides a method for encapsulating a perovskite solar cell based on a composite encapsulating layer and application of the method for prolonging the service life of a device. As shown in fig. 2, the structure of the battery includes: glass substrate, bottom electrode layer (transparent electrode ITO), bottom charge transport layer (nickel oxide), perovskite layer (MAPbI)3) Top charge transport layer (PCBM), top electrode layer (silver), encapsulation layer (alumina, perfluorododecyl trichlorosilane). The preparation and service life characterization method of the packaging layer comprises the following steps:
1) preparing aluminum oxide by atomic layer deposition: the precursors used to deposit alumina were trimethylaluminum and water. The deposition temperature in the reaction chamber was maintained at 60 ℃. The pressure in the chamber was maintained at 2.5Torr and high purity nitrogen was used as a carrier and purge gas. When the temperature of the pipeline and the reaction cabin reaches the set temperature, the equipment starts to circularly run according to the designed program. The release time of the trimethylaluminum is 10 ms; after the trimethyl aluminum is released, nitrogen purging is carried out in the reaction cabin for 10 seconds; the water release time was 10ms, and after the water release, a nitrogen purge was performed for 20 seconds in the reaction chamber. The two precursors are released at room temperature, the prepared perovskite solar cell is placed in a reaction cabin, and an aluminum oxide layer with the thickness of 30nm is deposited on the surface of the perovskite solar cell at the speed of 0.1nm per cycle, so that the prepared aluminum oxide layer is very compact and uniform in shape (figure 3);
2) thermal evaporation deposition of perfluorododecyl trichlorosilane layer: the prepared sample is stuck on an aluminum foil, 40 mul of perfluorododecyl trichlorosilane is added into a 500ml beaker, the aluminum foil with the sample is sealed on the mouth of the beaker, the sample faces downwards, the beaker is placed on a hot plate at 140 ℃ and is heated for 2 hours, and a perfluorododecyl trichlorosilane layer with the thickness of about 2nm can be deposited, and as shown in figure 4, the sample has excellent hydrophobicity;
3) preparing a double composite packaging layer: the single composite packaging layer is prepared by the process, and the obtained sample is repeatedly operated according to the steps to prepare a double composite packaging layer;
4) and (3) characterization of anti-water-oxygen performance: electrical device encapsulated by unpackaged battery and single composite encapsulation layerThe cell and the cell packaged by the double composite packaging layers are at AM1.5G, 100mW/cm2The cells were tested for current density-voltage (J-V) performance curves under light and then stored in an atmospheric environment (20 ℃ 50% humidity) and the current density-voltage performance curves were continuously monitored over time and normalized to their initial photoelectric conversion efficiency of 1, as shown in fig. 5, with the unencapsulated cells failing completely within 500 hours, while the single composite encapsulated cells and the double composite encapsulated cells maintained initial efficiencies of 84% and 93% after 1500 hours of storage. The existence of the composite packaging layer greatly prolongs the storage life of the device, and the main reason is that the composite packaging layer prevents the invasion of water and oxygen and improves the water and oxygen resistance of the device.
5) And (3) thermal stability characterization: the non-encapsulated cell, the cell encapsulated by the single composite encapsulating layer and the cell encapsulated by the double composite encapsulating layer are at AM1.5G, 100mW/cm2The cells were tested for current density-voltage (J-V) performance curves under light, then stored in a nitrogen environment at 60 ℃, and the current density-voltage performance curves were continuously monitored over time, normalized with their initial photoelectric conversion efficiency of 1, as shown in fig. 6, the unencapsulated cells completely failed within 500 hours, while the single composite encapsulant encapsulated cells and the double composite encapsulant encapsulated cells maintained more than 90% of the initial efficiency after 1000 hours of storage. The composite packaging layer greatly improves the thermal stability of the device, and the main reason is that the composite packaging layer improves the sealing property of the device, prevents the escape of perovskite degradation products and ensures that the degradation reaction can not be continued.
6) And (3) characterizing the illumination stability: the non-encapsulated cell, the cell encapsulated by the single composite encapsulating layer and the cell encapsulated by the double composite encapsulating layer are at AM1.5G, 100mW/cm2Testing the current density-voltage (J-V) performance curve of the cell under illumination, storing in a nitrogen environment, continuously monitoring the current density-voltage performance curve over time under the illumination of standard sunlight, and normalizing with the initial photoelectric conversion efficiency of the curve as 1, as shown in FIG. 7, the efficiency of the unpackaged cell decays rapidly and slowly, and completely fails within 900 hours, while the single composite packaging layer is singleThe encapsulated cells and the cells encapsulated by the double composite encapsulation layer can still maintain the initial efficiency of 85 percent and more than 90 percent after being stored for 1000 hours. The existence of the composite packaging layer greatly improves the illumination stability of the device.
7) And (3) accelerated aging characterization: the non-encapsulated cell, the cell encapsulated by the single composite encapsulating layer and the cell encapsulated by the double composite encapsulating layer are at AM1.5G, 100mW/cm2The current density-voltage (J-V) performance curves of the cells were tested under light and then stored in an environment of 85 ℃ and 85% humidity, the current density-voltage performance curves were continuously monitored over time, normalized with their initial photoelectric conversion efficiency of 1, as shown in fig. 8, the efficiency of the unpackaged cells decayed very rapidly and completely failed within 50 hours, the cells encapsulated with a single composite encapsulation layer failed within 400 hours, while the cells encapsulated with a double composite encapsulation layer could maintain more than 80% of the initial efficiency after 500 hours of storage. The existence of the composite packaging layer greatly improves the stability of the device under accelerated aging.
8) Extreme environmental stability characterization: the non-encapsulated cell, the cell encapsulated by the single composite encapsulating layer and the cell encapsulated by the double composite encapsulating layer are at AM1.5G, 100mW/cm2And testing the current density-voltage (J-V) performance curve of the battery under illumination, soaking the device in deionized water for 5 hours, taking out the device, and testing the J-V curve again. The unpackaged cells were completely decomposed within 1 minute, the cells encapsulated with the single composite encapsulation layer were decomposed to some extent, and the cells encapsulated with the double composite encapsulation layer had no significant change in appearance after being soaked for 5 hours and still maintained the initial efficiency of 98% (fig. 9). The existence of the composite packaging layer greatly improves the stability of the device in the extreme environment.
9) Internal sealing performance characterization: the unpackaged cell was placed at AM1.5G, 100mW/cm2Testing current density-voltage (J-V) performance curve of the battery under illumination, then storing the battery in an environment at 60 ℃ for aging for 200 hours, taking out the battery, immediately testing the J-V curve of the battery, after the J-V curve is taken out, placing the battery in a nitrogen environment for recovering for 48 hours, testing the J-V curve again, comparing three groups of J-V curves (figure 10), the unpackaged battery has obvious degradation after 2 hours of accelerated aging, and the unpackaged battery is degraded in the nitrogen environmentThere was no recovery of efficiency after standing, indicating that the gaseous products generated by degradation inside the device had escaped completely. The same test was performed on the cells encapsulated with the double composite encapsulation layer (fig. 11), the cells encapsulated with the double composite encapsulation layer were degraded to some extent after being heated and aged, but the efficiency was substantially recovered to the initial state after standing in a nitrogen atmosphere, which indicates that the gaseous products generated by the degradation inside the device were completely blocked inside the device, and reversely formed perovskite to recover the efficiency when standing. The existence of the composite packaging layer enhances the internal sealing performance and is beneficial to preventing the continuous degradation.
Example 2
The embodiment provides a method for encapsulating a perovskite solar cell based on a composite encapsulating layer and application of the method for prolonging the service life of a device. As shown in fig. 2, the structure of the battery includes: glass substrate, bottom electrode layer (transparent electrode ITO), bottom charge transport layer (nickel oxide), perovskite layer (MAPbI)3) Top charge transport layer (PCBM), top electrode layer (silver), encapsulation layer (titanium oxide, perfluorododecyl trichlorosilane). The preparation and service life characterization method of the packaging layer comprises the following steps:
1) preparing titanium oxide by atomic layer deposition: the precursors used to deposit the titanium oxide were tetrakis (dimethylamino) titanium and water. The deposition temperature in the reaction chamber was maintained at 60 ℃. The pressure in the chamber was maintained at 2.5Torr and high purity nitrogen was used as a carrier and purge gas. When the temperature of the pipeline and the reaction cabin reaches the set temperature, the equipment starts to circularly run according to the designed program. The release time of tetrakis (dimethylamino) titanium is 50 ms; after the tetra (dimethylamino) titanium is released, nitrogen purging is carried out in the reaction chamber for 10 seconds; the water release time was 10ms, and after the water release, a nitrogen purge was performed for 20 seconds in the reaction chamber. Releasing the two precursors at room temperature, putting the prepared perovskite solar cell into a reaction cabin, and depositing a 30nm titanium oxide layer on the surface of the perovskite solar cell at the speed of 0.1nm per cycle;
3) thermal evaporation deposition of perfluorododecyl trichlorosilane layer: adhering the prepared sample on an aluminum foil, adding 40 mul of perfluorododecyl trichlorosilane into a 500ml beaker, sealing the aluminum foil with the sample on the opening of the beaker with the sample facing downwards, and placing the beaker on a hot plate at 140 ℃ for heating for 2 hours to deposit a perfluorododecyl trichlorosilane layer with the thickness of about 2 nm;
3) preparing a double composite packaging layer: the single composite packaging layer is prepared by the process, and the obtained sample is repeatedly operated according to the steps to prepare a double composite packaging layer;
4) and (3) characterization of anti-water-oxygen performance: the non-encapsulated cell, the cell encapsulated by the single composite encapsulating layer and the cell encapsulated by the double composite encapsulating layer are at AM1.5G, 100mW/cm2The cells were tested for current density-voltage (J-V) performance curves in the light and then stored in an atmospheric environment (20 ℃ 50% humidity) and the current density-voltage performance curves were continuously monitored over time and normalized to their initial photoelectric conversion efficiency of 1, as shown in fig. 12, with the unencapsulated cells failing completely within 500 hours, while the single composite encapsulated cells and the double composite encapsulated cells maintained initial efficiencies of 72% and 87% after 1500 hours of storage. The existence of the composite packaging layer greatly prolongs the storage life of the device, and the main reason is that the composite packaging layer prevents the invasion of water and oxygen and improves the water and oxygen resistance of the device.
Example 3
The embodiment provides a method for encapsulating a perovskite solar cell based on a composite encapsulating layer and application of the method for prolonging the service life of a device. As shown in fig. 2, the structure of the battery includes: glass substrate, bottom electrode layer (transparent electrode ITO), bottom charge transport layer (nickel oxide), perovskite layer (MAPbI)3) Top charge transport layer (PCBM), top electrode layer (silver), encapsulation layer (alumina, perfluorohexaalkyltrichlorosilane). The preparation and service life characterization method of the packaging layer comprises the following steps:
1) preparing aluminum oxide by atomic layer deposition: the precursors used to deposit alumina were trimethylaluminum and water. The deposition temperature in the reaction chamber was maintained at 60 ℃. The pressure in the chamber was maintained at 2.5Torr and high purity nitrogen was used as a carrier and purge gas. When the temperature of the pipeline and the reaction cabin reaches the set temperature, the equipment starts to circularly run according to the designed program. The release time of the trimethylaluminum is 10 ms; after the trimethyl aluminum is released, nitrogen purging is carried out in the reaction cabin for 10 seconds; the water release time was 10ms, and after the water release, a nitrogen purge was performed for 20 seconds in the reaction chamber. Releasing the two precursors at room temperature, putting the prepared perovskite solar cell into a reaction cabin, and depositing an aluminum oxide layer of 30nm on the surface of the perovskite solar cell at the speed of 0.1nm per cycle;
2) thermal evaporation deposition of perfluorohexaalkyltrichlorosilane layer: adhering the prepared sample on an aluminum foil, adding 40 mu l of perfluorohexaalkyl trichlorosilane into a 500ml beaker, sealing the aluminum foil with the sample on the opening of the beaker with the sample facing downwards, and placing the beaker on a hot plate at 140 ℃ for heating for 2 hours to deposit a perfluorohexaalkyl trichlorosilane layer with the thickness of about 2 nm;
3) preparing a double composite packaging layer: the single composite packaging layer is prepared by the process, and the obtained sample is repeatedly operated according to the steps to prepare a double composite packaging layer;
4) and (3) characterization of anti-water-oxygen performance: the non-encapsulated cell, the cell encapsulated by the single composite encapsulating layer and the cell encapsulated by the double composite encapsulating layer are at AM1.5G, 100mW/cm2The cells were tested for current density-voltage (J-V) performance curves under light and then stored in an atmospheric environment (20 ℃ 50% humidity) and the current density-voltage performance curves were continuously monitored over time and normalized to their initial photoelectric conversion efficiency of 1, as shown in fig. 13, with the unencapsulated cells failing completely within 500 hours, while the single composite encapsulated cells and the double composite encapsulated cells maintained initial efficiencies of 80% and 88% after 1500 hours of storage. The existence of the composite packaging layer greatly prolongs the storage life of the device, and the main reason is that the composite packaging layer prevents the invasion of water and oxygen and improves the water and oxygen resistance of the device.
Example 4
The embodiment provides a method for encapsulating an organic solar cell based on a composite encapsulating layer and application thereof to prolonging the service life of a device. As shown in fig. 14, the structure of the battery includes: a glass substrate, a bottom electrode layer (transparent electrode ITO), a bottom charge transport layer (PEDOT: PSS), an active layer (PM6: Y6-BO), a top electrode layer (silver), and an encapsulation layer (aluminum oxide, perfluorododecyl trichlorosilane). The preparation and service life characterization method of the packaging layer comprises the following steps:
1) preparing aluminum oxide by atomic layer deposition: the precursors used to deposit alumina were trimethylaluminum and water. The deposition temperature in the reaction chamber was maintained at 60 ℃. The pressure in the chamber was maintained at 2.5Torr and high purity nitrogen was used as a carrier and purge gas. When the temperature of the pipeline and the reaction cabin reaches the set temperature, the equipment starts to circularly run according to the designed program. The release time of the trimethylaluminum is 10 ms; after the trimethyl aluminum is released, nitrogen purging is carried out in the reaction cabin for 10 seconds; the water release time was 10ms, and after the water release, a nitrogen purge was performed for 20 seconds in the reaction chamber. Releasing the two precursors at room temperature, putting the prepared organic solar cell into a reaction cabin, and depositing an aluminum oxide layer of 30nm on the surface of the organic solar cell at the speed of 0.1nm per cycle;
2) thermal evaporation deposition of perfluorododecyl trichlorosilane layer: adhering the prepared sample on an aluminum foil, adding 40 mul of perfluorododecyl trichlorosilane into a 500ml beaker, sealing the aluminum foil with the sample on the opening of the beaker with the sample facing downwards, and placing the beaker on a hot plate at 140 ℃ for heating for 2 hours to deposit a perfluorododecyl trichlorosilane layer with the thickness of about 2 nm;
3) preparing a double composite packaging layer: the single composite packaging layer is prepared by the process, and the obtained sample is repeatedly operated according to the steps to prepare a double composite packaging layer;
4) and (3) characterization of anti-water-oxygen performance: the non-encapsulated cell, the cell encapsulated by the single composite encapsulating layer and the cell encapsulated by the double composite encapsulating layer are at AM1.5G, 100mW/cm2The current density-voltage (J-V) performance curves of the cells were tested in the light and then stored in an atmospheric environment (20 ℃ at 50% humidity) and continuously monitored over time for normalization with their initial photoelectric conversion efficiency of 1, as shown in fig. 15, the efficiency of the unpackaged cells decreased to 72% after 2000 hours, while the single composite encapsulated cells and the double composite encapsulated cells maintained initial efficiencies of 89% and 94% after 2000 hours of storage. The existence of the composite packaging layer greatly prolongs the storage life of the device, and the main reason is thatThe composite packaging layer prevents the invasion of water and oxygen and improves the water and oxygen resistance of the device.
Example 5
The embodiment provides a method for encapsulating organic fluorescent light emitting diodes (OFEDs) based on a composite encapsulation layer and application thereof to prolonging the service life of devices. As shown in fig. 16, the structure of the OFED includes: the liquid crystal display panel comprises a reflecting plate, a light guide plate, a polarizer 1, a liquid crystal module, an RGB (red, green and blue) filter, a polarizer 2 and an encapsulating layer (aluminum oxide and perfluorododecyl trichlorosilane). The preparation and service life characterization method of the packaging layer comprises the following steps:
1) preparing aluminum oxide by atomic layer deposition: the precursors used to deposit alumina were trimethylaluminum and water. The deposition temperature in the reaction chamber was maintained at 60 ℃. The pressure in the chamber was maintained at 2.5Torr and high purity nitrogen was used as a carrier and purge gas. When the temperature of the pipeline and the reaction cabin reaches the set temperature, the equipment starts to circularly run according to the designed program. The release time of the trimethylaluminum is 10 ms; after the trimethyl aluminum is released, nitrogen purging is carried out in the reaction cabin for 10 seconds; the water release time was 10ms, and after the water release, a nitrogen purge was performed for 20 seconds in the reaction chamber. Releasing the two precursors at room temperature, putting the prepared OFED device into a reaction chamber, and depositing an aluminum oxide layer of 30nm on the surface of the OFED device at the speed of 0.1nm per cycle;
2) thermal evaporation deposition of perfluorododecyl trichlorosilane layer: adhering the prepared sample on an aluminum foil, adding 40 mul of perfluorododecyl trichlorosilane into a 500ml beaker, sealing the aluminum foil with the sample on the opening of the beaker with the sample facing downwards, and placing the beaker on a hot plate at 140 ℃ for heating for 2 hours to deposit a perfluorododecyl trichlorosilane layer with the thickness of about 2 nm;
3) preparing a double composite packaging layer: the single composite packaging layer is prepared by the process, and the obtained sample is repeatedly operated according to the steps to prepare a double composite packaging layer;
4) and (3) characterizing the working life: the unencapsulated OFEDs, single compound encapsulant-encapsulated OFEDs and double compound encapsulant-encapsulated OFEDs were tested for fluorescence intensity under excitation with 465nm blue light, after which irradiation with this blue light and storage in an atmospheric environment (20 ℃ at 50% humidity) was continued and the device fluorescence intensity was monitored continuously over time, normalized to their initial fluorescence intensity of 1, as shown in fig. 17, where the efficiency of the unencapsulated OFEDs decreased to 0% after 140 hours, while the single compound encapsulant-encapsulated OFEDs and double compound encapsulant-encapsulated OFEDs remained at 61% and 75% of their initial efficiencies after 200 hours of storage. The composite packaging layer greatly prolongs the service life of the device, and the main reason is that the composite packaging layer prevents the invasion of water and oxygen and prevents the degradation of the fluorescent material in an excitation state.

Claims (8)

1. A method for encapsulating an organic photoelectric device based on a composite material is characterized by comprising the following preparation steps:
1) preparing an anti-permeation compact layer film on the surface of the prepared organic photoelectric device, wherein the thickness is 2-100 nm;
2) preparing a hydrophobic layer film on the surface of the sample, wherein the thickness of the hydrophobic layer film is 1-20 nm;
3) repeating the steps 1) and 2) to prepare a multi-composite packaging layer, wherein the repetition times are more than or equal to 1;
the anti-seepage compact layer film material comprises one or more of aluminum oxide, titanium oxide, silicon oxide, tin oxide, nickel oxide and molybdenum oxide;
the hydrophobic layer film material comprises: one or more of polypropylene, polystyrene, polytetrafluoroethylene, perfluorohexaalkyl trichlorosilane, perfluorododecyl trichlorosilane, carbon nano tubes and array nano oxides.
2. The method of claim 1, wherein in steps 1) and 2), the method is selected from one or more of atomic layer deposition, hydrothermal method, sol-gel method, thermal evaporation deposition, chemical vapor deposition, plasma method, and template method, and the reaction temperature is not higher than 100 ℃.
3. The production method according to claim 1 or 2,
in the step 1), the thickness of the anti-seepage compact layer film is 30 nm;
in the step 2), the thickness of the hydrophobic layer film is 2 nm;
in the step 3), the number of repetitions is 1.
4. The preparation method according to claim 1 or 2, wherein the organic photoelectric device is a perovskite solar cell, the anti-permeation dense layer thin film material is alumina, and the thin film thickness is 30 nm; the hydrophobic layer film material is perfluorododecyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
5. The preparation method according to claim 1 or 2, wherein the organic photoelectric device is a perovskite solar cell, the material of the anti-permeation dense layer film is titanium oxide, and the thickness of the film is 30 nm; the hydrophobic layer film material is perfluorododecyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
6. The preparation method according to claim 1 or 2, wherein the organic photoelectric device is a perovskite solar cell, the anti-permeation dense layer thin film material is alumina, and the thin film thickness is 30 nm; the hydrophobic layer film material is perfluorohexaalkyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
7. The preparation method according to claim 1 or 2, wherein the organic photoelectric device is an organic solar cell, the thin film material of the anti-permeation dense layer is alumina, and the thickness of the thin film is 30 nm; the hydrophobic layer film material is perfluorododecyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
8. The preparation method according to claim 1 or 2, wherein the organic photoelectric device is an organic fluorescent light emitting diode (OFED), the impermeable dense layer film material is alumina, and the film thickness is 30 nm; the hydrophobic layer film material is perfluorododecyl trichlorosilane, and the film thickness is 2 nm; the preparation method in the step 1) is atomic layer deposition, and the preparation method in the step 2) is thermal evaporation deposition; in the step 3), the number of repetitions is 1.
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