CN111180594A - Composite film packaging method of perovskite solar cell - Google Patents
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Abstract
A composite film packaging method of a perovskite solar cell belongs to the technical field of film packaging. Specifically, the mass of two PDMS precursors is diluted by decamethylcyclopentasiloxane (PDMS) 1: 1, spin-coating the diluted viscous mixture on the upper surface and the side surface of the organic metal halide perovskite solar cell, and forming a film through ultraviolet light curing; then, PDMS is processed by remote plasma to form a layer of compact SiOXA film; repeating the operation for many times to obtain PDMS/SiOXAnd (4) a laminated structure, thereby completing the composite film encapsulation of the organic metal halide perovskite solar cell. All packaging processes do not need high temperature conditions, so that damage to the perovskite solar cell caused by high temperature is avoided; the invention applies the remote plasma technology and can grow high water oxygen barrier property at low temperatureAn energy-encapsulating film.
Description
Technical Field
The invention belongs to the technical field of thin film packaging, and particularly relates to a composite thin film packaging method of a perovskite solar cell, namely, Polydimethylsiloxane (PDMS) is processed by utilizing remote oxygen plasma, so that part of PDMS on the surface is converted into compact inorganic silicon oxide (SiO)x) Layer of PDMS/SiOxAn organic-inorganic laminated film.
Background
Perovskite Solar Cells (PSCs) have received much attention due to their advantages of high carrier mobility and long carrier diffusion length. PCE (power conversion efficiency) of rigid PSC has reached around 25.2% today, but its stability is a major bottleneck for the development and commercial application of this technology. Organic materials in PSCs are easily dissolved by reacting with moisture and oxygen in the atmosphere, thus resulting in poor stability of PSCs, and silver ion migration due to moisture also greatly reduces the stability of devices. The thin film encapsulation process is an easy method to block water and oxygen in the external environment, thereby improving the stability of the PSC.
Some studies have been conducted to improve the stability of organic electronic devices by protecting the organic electronic devices from water vapor by encapsulating the organic electronic devices with an organic-inorganic laminate film. Inorganic materials such as silicon nitride (SiN)X),SiO2And Al2O3They exhibit excellent water vapor barrier properties as an encapsulation layer. Inorganic materials are typically deposited by vacuum processes, such as Atomic Layer Deposition (ALD) and Plasma Enhanced Chemical Vapor Deposition (PECVD), to produce high performance barrier films. However, these thin films generally have a process temperature ranging from 80 ℃ to 300 ℃, and such high temperature causes the organic materials in the PSC to be pyrolyzed and denatured, so that the PSC fails, so that it is necessary to develop a new process for preparing a PSC encapsulation layer under a low-temperature weak radiation condition.
Disclosure of Invention
The purpose of the invention isA thin film encapsulation method of a perovskite solar cell is provided. Specifically, a precursor of PDMS is diluted with Decamethylcyclopentasiloxane (D5), the diluted viscous mixture is spin-coated on the PSC surface, and a film is formed by Ultraviolet (UV) light curing; then PDMS is processed through remote plasma for 2-5 minutes to form a layer of compact SiOXA film.
In order to achieve the above purpose, the present invention provides a method for encapsulating a composite thin film of a perovskite solar cell, which comprises the following steps:
1) preparing an organic metal halide perovskite solar cell on a clean rigid substrate (such as a glass substrate) by taking ITO as a lower electrode under an inert atmosphere, wherein the length and the width of the substrate are larger than those of the perovskite solar cell;
2) two precursors of PDMS were mixed in a mass 1: 1 for 3-6 minutes to obtain a viscous mixture; then diluting the viscous mixture to 8-12 times of the original mass by Decamethylcyclopentasiloxane (D5);
3) is full of N2Spin-coating the diluted viscous mixture obtained in the step 2) on the upper surface and the side surface of the organic metal halide perovskite solar cell obtained in the step 1) at the rotating speed of 5000-8000 rpm for 20-40 s in the glove box, then placing the glove box for 5-10 minutes, and evaporating excessive decamethylcyclopentasiloxane at room temperature;
4) curing the device obtained in the step 3) for 50-80 s under ultraviolet light to obtain a solid PDMS layer with the thickness of 80-150 nm, namely an organic barrier layer;
5) processing the solid PDMS layer obtained in the step 4) for 8-15 min under the power of 100-150 w by using remote plasma in a reaction chamber of the ALD device to obtain compact SiO with the thickness of 30-50 nm on the solid PDMS layerXThin films, i.e., inorganic barrier layers;
6) SiO obtained in step 5)XRepeating the operations of the steps 3), 4) and 5) on the film for a plurality of times to obtain PDMS/SiOXA laminated structure;
7) PDMS/SiO obtained in step 6)XAnd (3) repeating the operations of the steps 3) and 4) for 1 time on the laminated structure to obtain a composite barrier layer, thereby completing the composite film packaging of the organic metal halide perovskite solar cell.
The invention relates to a composite film packaging method of a perovskite solar cell, which comprises the following steps:
1) preparing an organic metal halide perovskite solar cell on a clean flexible substrate (such as a PET substrate) in an inert atmosphere by taking Au as a lower electrode, wherein the length and the width of the substrate are larger than those of the perovskite solar cell;
2) two precursors of PDMS were mixed in a mass 1: 1 for 3-6 minutes to obtain a viscous mixture; then diluting the viscous mixture to 8-12 times of the original mass by Decamethylcyclopentasiloxane (D5);
3) is full of N2Spin-coating the diluted viscous mixture obtained in the step 2) on the upper surface and the side surface of the organic metal halide perovskite solar cell obtained in the step 1) at the rotating speed of 5000-8000 rpm for 20-40 s in the glove box, then placing the glove box for 5-10 minutes, and evaporating excessive decamethylcyclopentasiloxane at room temperature;
4) curing the device obtained in the step 3) for 50-80 s under ultraviolet light to obtain a solid PDMS layer with the thickness of 80-150 nm, namely an organic barrier layer;
5) processing the solid PDMS layer obtained in the step 4) for 8-15 min under the power of 100-150 w by using remote plasma in a reaction chamber of the ALD device to obtain compact SiO with the thickness of 30-50 nm on the solid PDMS layerXThin films, i.e., inorganic barrier layers;
6) SiO obtained in step 5)XRepeating the operations of the steps 3), 4) and 5) on the film for a plurality of times to obtain PDMS/SiOXA laminated structure;
7) PDMS/SiO obtained in step 6)XRepeating the operations of the steps 3) and 4) for 1 time on the laminated structure to obtain a composite barrier layer;
8) and repeating the steps 3), 4), 5) and 6) on the lower surface of the flexible substrate to obtain a substrate packaging barrier layer, thereby completing the composite thin film packaging of the organic metal halide perovskite solar cell.
In particular, it is possible to use, for example,
in the step (1), when two PDMS precursors are mixed, the proportion of 1: 1, so as to ensure that compact SiO grows when PDMS is subjected to remote plasma treatmentXA layer;
(2) the spin coating of PDMS and the evaporation of excess D5 was performed at N2Is carried out in the environment of (1).
(3) The power of the remote plasma is strictly set to be 100 w-150 w, a PDMS packaging layer is damaged when the power is too high, and compact SiO cannot grow when the power is too lowXAnd (3) a layer.
The technical scheme of the invention has the advantages that:
1. all packaging processes do not need high temperature conditions, so that damage to the perovskite solar cell caused by high temperature is avoided;
2. the remote plasma technology is applied to the packaging of the perovskite solar cell, and a packaging film with high water oxygen barrier property can grow at low temperature;
3. the PDMS layer plays a role in pre-packaging the perovskite battery, and the damage of an inorganic barrier layer grown by plasma to a device is avoided;
4. through the cooperation of the steps 1, 2 and 3, the growth of the packaging material with high water oxygen barrier performance is realized on the premise of not damaging the perovskite solar cell.
5. The packaging method of the laminated thin film has important research significance on the stability improvement and the commercial feasibility of the perovskite solar cell.
Drawings
FIG. 1 is a schematic cross-sectional structure of a perovskite solar cell fabricated on a rigid substrate according to the present invention after encapsulation; the solar cell comprises a substrate 40, a perovskite solar cell 30, a composite barrier layer 20 (a multilayer laminated structure comprising an organic barrier layer 201 and an inorganic barrier layer 202, wherein the uppermost layer is the organic barrier layer 201);
FIG. 2 is a schematic diagram of an ALD apparatus used in the present invention. Wherein the perovskite solar cell is placed in the reaction chamber of the ALD apparatus far awayProcess plasma device (O)2plasma) is positioned above the reaction chamber, and the power of the remote plasma device is adjusted to process the organic barrier layer. Wherein the mechanical pump is used for vacuumizing the reaction chamber, and the inert gas (N)2) For changing the atmosphere of the reaction chamber.
FIG. 3 is a schematic cross-sectional structure of a perovskite solar cell fabricated on a flexible substrate according to the present invention after encapsulation; the solar cell comprises a substrate 40, a perovskite solar cell 30, a composite barrier layer 20 (a multilayer laminated structure comprising an organic barrier layer 201 and an inorganic barrier layer 202, wherein the uppermost layer is the organic barrier layer 201), and a substrate packaging barrier layer 21 (a multilayer laminated structure comprising the organic barrier layer 201 and the inorganic barrier layer 202, wherein the lowermost layer is the organic barrier layer 201);
fig. 4 is a process schematic diagram of the thin film packaging method of the perovskite solar cell according to the embodiment of the invention.
As shown in fig. 4, the specific steps are as follows:
(1) cleaning, drying and ozone activating the surface of the substrate; fabricating perovskite solar cell devices (PSCs) on clean substrates;
(2) and (2) placing the substrate and the device which are subjected to the step (1) into a glove box, mixing PDMS precursors in a fixed proportion, and diluting the mixture to 8-12 times of the original weight by using D5.
(3) After the PDMS dope preparation is finished, the mixture is filled with N2Spin-coating the viscous mixture on the cell surface at 6000rpm in the glove box.
(4) After the PDMS film is coated in a spinning mode, the device is transferred to a reaction chamber of an ALD device, the reaction chamber is vacuumized to 0-0.03 mTorr, 150w of remote plasma equipment is used for processing the surface of the device for 10min, and a layer of compact SiO is converted from the surface of the PDMSXAnd repeating the operation for multiple times to obtain a composite barrier layer overlapped by the inorganic barrier layer and the organic barrier layer, wherein the repetition times is determined according to the thickness of each layer and the expected packaging effect, and the last layer is the organic barrier layer.
FIG. 5 is a schematic representation of a process using PDMS/SiO2Encapsulation, encapsulation with PDMS and exposure of the unencapsulated rigid substrate cell to 15% RH at 30 deg.CSchematic graph of the change in efficiency at 00 hours.
FIG. 6 is a schematic representation of a process using PDMS/SiO2Schematic representation of the change in efficiency of the encapsulated, encapsulated with PDMS and unencapsulated flexible substrate cells exposed to conditions of 80% RH and 30 ℃ for 1500 hours.
Detailed Description
Example 1
Referring to fig. 1, example 1 of the present invention provides a thin film encapsulation structure of a perovskite solar cell on a rigid substrate, which includes a rigid substrate 40, a perovskite solar cell 30 disposed on the substrate 40, a composite barrier layer disposed on the perovskite solar cell 30 and used for protecting the perovskite solar cell 30 during encapsulation and practical use, and a composite barrier layer 20 (a multi-layer stack structure including an organic barrier layer 201 and an inorganic barrier layer 202, an uppermost layer being the organic barrier layer 201).
Wherein the rigid substrate 40 is a glass substrate, and the perovskite solar cell 30 is a flat-plate perovskite solar cell (structure: glass substrate/ITO/SnO) in organic metal halide perovskite solar cells2/MaPbI3/spiro-MeOTAD/Ag). The composite barrier layer 20 includes 3 PDMS organic barrier layers 201 and 2 inorganic barrier layers 202 disposed between two adjacent organic barrier layers.
The method comprises the following specific steps:
1) preparing 6 ITO glass substrates, respectively wiping the substrates by acetone and ethanol cotton balls repeatedly, and then performing ultrasonic treatment for 15min by using ethanol and acetone respectively. And after the ultrasonic treatment is finished, blowing the surface solvent clean by using a nitrogen gun, then putting the substrate into an oven at 100 ℃ for drying for 30min, sticking one side of the substrate by using an adhesive tape, and then putting the substrate into a UV machine for exposure for 20 min.
2) Sequentially spin-coating an electron transport layer (SnO) on the ITO2100nm), perovskite layer (MaPbI)3300nm), 2',7,7' -tetrabromo-9, 9' -spirodi, tri (4-iodophenyl) amine (spiro-MeOTAD, 200nm), placing in a glove box for 24h, and then placing in an evaporation furnace to grow 100nm Ag electrode, thereby completing the preparation of the perovskite solar cell 30; 4 perovskite solar cells are stored in a nitrogen glove box, and the other 2 perovskite solar cells are placed in an ALD device;
3) Two precursors of PDMS: vinyl-functionalized polydimethylsiloxane and poly (methylhydrosiloxane) were polymerized in the mass ratio of 1: 1 for 5 minutes. The viscous mixture was then diluted with D5 to 9 times the original weight.
4) Is full of N2The diluted viscous mixture was spin-coated at 6000rpm on the upper and side surfaces of the Ag electrode of the perovskite solar cell prepared in step 1) for 30 seconds. Placing the coating in a bath of N2The glove box of (1) was left for 8min, and excess D5 was evaporated.
5) The organic barrier film 201(100nm) was then prepared by UV light curing for 60s on the device surface. Then the reaction chamber is put into the reaction chamber of the ALD device again, the reaction chamber is pumped to 0.03Torr after being pumped, and carrier gas (inert gas N) is introduced2) The gas pressure was stabilized at 0.2 Torr.
6) Processing PDMS layer with remote plasma (100w) for 10min to form a compact SiO layerXA thin film (30nm) to complete the preparation of the inorganic barrier film 202; after multiple cycles, three layers of organic barrier films 201 and two layers of inorganic barrier films 202 grow, wherein the first layer and the last layer are both the organic barrier films 201, and the preparation of the composite barrier film 20(400nm) is realized.
7) Taking out two perovskite solar cells in the ALD device, and placing the perovskite solar cells in the ALD device to be filled with N2Stored in a glove box. And taking out two pieces of the four perovskite solar cells which are placed in the glove box before, and packaging the two pieces of perovskite solar cells only by using a packaging mode of a PDMS laminated film, wherein the preparation method of the cells is the same as the preparation method, the PDMS layer is spin-coated on the surface of the device for 30s at the speed of 6000rpm, and then the polymer film is formed on the surface of the device by using UV light curing for 60 s. Taking out the two perovskite solar cells in the ALD equipment after the completion and placing the two perovskite solar cells in N2And performing PCE test on the four perovskite solar cells stored in the glove box together.
After 1500 hours of exposure at 80% RH and 30 ℃, the encapsulated cells retained 95% of the initial efficiency, whereas the cell efficiency with PDMS encapsulation decreased significantly, with the unencapsulated cell efficiency almost dropping to that of the unencapsulated cell0, experimental spectrum as shown in figure 5. By means of the PDMS/SiO2The laminated film packaging method can effectively reduce the water vapor transmittance of the device and greatly improve the stability of the perovskite solar cell.
Example 2
Referring to fig. 3, the present embodiment provides a thin film encapsulation structure of a perovskite solar cell on a flexible substrate, which includes a flexible substrate 40, a substrate encapsulation barrier layer 21 disposed on a lower surface of the substrate for protecting the perovskite solar cell 30 during an actual application process, and a composite barrier layer 20 disposed on an upper surface of the perovskite solar cell 30 for protecting the perovskite solar cell 30 during an encapsulation process. The composite barrier layer 20 includes 3 organic barrier layers 201 and 2 barrier layers 202 between two adjacent organic barrier layers, and the substrate package barrier layer 21 includes 3 organic barrier layers 201 and 2 barrier layers 202 between two adjacent organic barrier layers. The structure of the solar cell is as follows: flexible substrate/Au/SnO2/MaPbI3/spiro-MeOTAD/Ag。
The method comprises the following specific steps:
1) preparing 6 PET substrates, respectively wiping with acetone and ethanol cotton balls repeatedly, cleaning with nitrogen gun, sticking one side of the substrate with adhesive tape, placing into an evaporation furnace to grow 10nm gold electrode, and exposing in UV machine for 20 min.
2) Sequentially spin-coating electron transport layer (SnO) on gold electrode of PET2100nm), perovskite layer (MaPbI)3300nm), 2',7,7' -tetrabromo-9, 9' -spirodi, tri (4-iodophenyl) amine (spiro-MeOTAD, 200nm), placing in a glove box for 24h, and then placing in an evaporation furnace to grow 100nm Ag electrode, thereby completing the preparation of the perovskite solar cell 30; 4 perovskite solar cells are placed in a nitrogen glove box for storage, and the other 2 perovskite solar cells are placed in ALD equipment;
3) two precursors of PDMS: vinyl-functionalized polydimethylsiloxane and poly (methylhydrosiloxane) were polymerized in the mass ratio of 1: 1 for 5 minutes and then dilute the viscous mixture with D5 to 9 times the original weight.
4) Is full of N2Hand (2)The diluted viscous mixture was spin-coated at 6000rpm in a box for 30s on the upper surface and side surfaces of the Ag electrode of the perovskite solar cell prepared in step 1). Placing the coating in a bath of N2The glove box of (1) was left for 8min, and excess D5 was evaporated.
5) The organic barrier film 201(100nm) was then prepared by UV light curing for 60s on the device surface. Then the reaction chamber is put into the reaction chamber of the ALD device again, the reaction chamber is pumped to 0.03Torr after being pumped, and carrier gas (inert gas N) is introduced2) The gas pressure was stabilized at 0.2 Torr.
6) Processing PDMS layer with remote plasma (100w) for 10min to form a compact SiO layerXA thin film (30nm) to complete the preparation of the inorganic barrier film 202; after multiple cycles, three layers of organic barrier films 201 and two layers of inorganic barrier films 202 grow, wherein the first layer and the last layer are both the organic barrier films 201, and the preparation of the composite barrier film 20(400nm) is realized.
7) And (5) repeatedly carrying out bottom packaging on the perovskite battery by the steps 3), 4), 5) and 6), and growing a substrate packaging barrier layer 21(400 nm).
8) Taking out two perovskite solar cells in the ALD device, and placing the perovskite solar cells in the ALD device to be filled with N2Stored in a glove box. And taking out two pieces of the four perovskite solar cells which are placed in the glove box before, and packaging the two pieces of perovskite solar cells only by using a packaging mode of a PDMS laminated film, wherein the preparation method of the cells is the same as that of the above preparation method, and the PDMS layer is spin-coated on the surface of the device for 30s at the speed of 6000rpm, and then is cured by UV light for 60s to form a polymer film on the surface of the device. Taking out the two perovskite solar cells in the ALD equipment after the completion and placing the two perovskite solar cells in N2And performing PCE test on the four perovskite solar cells stored in the glove box together.
After 1500 hours of exposure at 80% RH and 30 ℃, the packaged flexible cell retained 95% of the initial efficiency, while the cell efficiency with PDMS package was significantly reduced, and the non-packaged cell efficiency was almost reduced to 0, as shown in fig. 6, the experimental spectrum shows that the initial efficiency of the flexible cell is lower and the efficiency is reduced more rapidly than that of the rigid cell.By means of the PDMS/SiO2The laminated film packaging method can effectively reduce the water vapor transmittance of the device and greatly improve the stability of the perovskite solar cell.
Specifically, the material types of the perovskite solar cell 30 and the composite barrier layer 20 on the bottom encapsulation barrier layer 21 are the same as those in example 1. In the embodiment, the power of the organic barrier layer 201 on the perovskite solar cell 30 is processed by using remote plasma is 100w, so that the perovskite solar cell is prevented from being damaged.
The above list of details is only for the concrete description of the feasible embodiments of the present invention, and they are not intended to limit the scope of the present invention, and all equivalent embodiments or modifications without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (4)
1. A composite film packaging method of a perovskite solar cell comprises the following steps:
1) preparing an organic metal halide perovskite solar cell on a clean rigid substrate by taking ITO as a lower electrode in an inert atmosphere, wherein the length and the width of the substrate are greater than those of the perovskite solar cell;
2) two precursors of PDMS were mixed in a mass 1: 1 for 3-6 minutes to obtain a viscous mixture; then diluting the viscous mixture to 8-12 times of the original mass by using decamethylcyclopentasiloxane;
3) is full of N2Spin-coating the diluted viscous mixture obtained in the step 2) on the upper surface and the side surface of the organic metal halide perovskite solar cell obtained in the step 1) at the rotating speed of 5000-8000 rpm for 20-40 s in the glove box, then placing the glove box for 5-10 minutes, and evaporating excessive decamethylcyclopentasiloxane at room temperature;
4) curing the device obtained in the step 3) for 50-80 s under ultraviolet light to obtain a solid PDMS layer with the thickness of 80-150 nm, namely an organic barrier layer;
5) processing the step 4) in a reaction chamber of the ALD device by using remote plasma at the power of 100 w-150 wObtaining a solid PDMS layer for 8-15 min, and obtaining compact SiO with the thickness of 30-50 nm on the solid PDMS layerXThin films, i.e., inorganic barrier layers;
6) SiO obtained in step 5)XRepeating the operations of the steps 3), 4) and 5) on the film for a plurality of times to obtain PDMS/SiOXA laminated structure;
7) PDMS/SiO obtained in step 6)XAnd (3) repeating the operations of the steps 3) and 4) for 1 time on the laminated structure to obtain a composite barrier layer, thereby completing the composite film packaging of the perovskite solar cell.
2. The method for encapsulating a composite thin film of a perovskite solar cell as claimed in claim 1, wherein: the rigid substrate is a glass substrate.
3. A composite film packaging method of a perovskite solar cell comprises the following steps:
1) preparing an organic metal halide perovskite solar cell on a clean flexible substrate in an inert atmosphere by taking Au as a lower electrode, wherein the length and the width of the substrate are greater than those of the perovskite solar cell;
2) two precursors of PDMS were mixed in a mass 1: 1 for 3-6 minutes to obtain a viscous mixture; then diluting the viscous mixture to 8-12 times of the original mass by using decamethylcyclopentasiloxane;
3) is full of N2Spin-coating the diluted viscous mixture obtained in the step 2) on the upper surface and the side surface of the organic metal halide perovskite solar cell obtained in the step 1) at the rotating speed of 5000-8000 rpm for 20-40 s in the glove box, then placing the glove box for 5-10 minutes, and evaporating excessive decamethylcyclopentasiloxane at room temperature;
4) curing the device obtained in the step 3) for 50-80 s under ultraviolet light to obtain a solid PDMS layer with the thickness of 80-150 nm, namely an organic barrier layer;
5) processing the solid PDMS layer obtained in the step 4) for 8-15 min under the power of 100-150 w by using remote plasma in a reaction chamber of the ALD device to obtain a compact solid PDMS layerSiO with a thickness of 30 to 50nmXThin films, i.e., inorganic barrier layers;
6) SiO obtained in step 5)XRepeating the operations of the steps 3), 4) and 5) on the film for a plurality of times to obtain PDMS/SiOXA laminated structure;
7) PDMS/SiO obtained in step 6)XRepeating the operations of the steps 3) and 4) for 1 time on the laminated structure to obtain a composite barrier layer;
8) and repeating the steps 3), 4), 5) and 6) on the lower surface of the flexible substrate to obtain a substrate packaging barrier layer, thereby completing the composite thin film packaging of the perovskite solar cell.
4. The method for encapsulating a composite thin film of a perovskite solar cell as claimed in claim 3, wherein: the flexible substrate is a PET substrate.
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CN111781120A (en) * | 2020-06-24 | 2020-10-16 | 吉林大学 | Testing method for thin film package |
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