WO2017073974A1 - 페로브스카이트 기반 광전변환소자의 재생방법 - Google Patents
페로브스카이트 기반 광전변환소자의 재생방법 Download PDFInfo
- Publication number
- WO2017073974A1 WO2017073974A1 PCT/KR2016/011983 KR2016011983W WO2017073974A1 WO 2017073974 A1 WO2017073974 A1 WO 2017073974A1 KR 2016011983 W KR2016011983 W KR 2016011983W WO 2017073974 A1 WO2017073974 A1 WO 2017073974A1
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- WIPO (PCT)
- Prior art keywords
- photoelectric conversion
- perovskite
- layer
- conversion device
- hole transport
- Prior art date
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- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
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- 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
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Definitions
- the present invention relates to a regeneration method of a photoelectric conversion device including a perovskite light absorption layer.
- photoelectric conversion materials are light absorbers that absorb light energy and convert it into electrical energy.
- Solar cell a representative device using photoelectric conversion material, is a tool for producing electricity by using sunlight, which is an infinite energy source, and is already widely used in our lives.
- Silicon materials used in silicon solar cells are representative photoelectric conversion materials. Recently, studies on organic-inorganic hybrid perovskite devices using light absorbers having perovskite structures have been actively conducted.
- a solar cell using a perovskite light absorber has attracted attention as a next-generation solar cell because not only has excellent photoelectric conversion efficiency but also has a lower process cost compared to other solar cells such as silicon solar cells and organic solar cells.
- perovskite solar cells have to be disposed of at the end of their life due to deterioration in performance, which causes economic losses by discarding substrate components such as electron collectors such as TiO 2 and transparent electrodes such as FTO.
- substrate components such as electron collectors such as TiO 2 and transparent electrodes such as FTO.
- the AMX3 structure contains harmful substances such as Pb, which are mainly used in place of the metal element (M), and thus additional costs are required to deal with them.
- the present invention is to provide a method for recovering and recycling a substrate from a perovskite photoelectric conversion device that has reached the end of its life or has already been used.
- the present invention is to provide a photoelectric conversion device having a high efficiency despite the manufacture of the substrate recovered from the perovskite photoelectric conversion device at the end of life.
- the present invention provides a method for regenerating a perovskite photoelectric conversion device, comprising a step of immersing the waste module of the perovskite photoelectric conversion device in a washing solvent for a time that satisfies the condition of the following equation (1). .
- y immersion time (min)
- x 1 is the dipole moment of the washing solvent
- a1 is a constant of 700 to 850
- b1 is a constant of 4 to 6.
- the dipole moment of the washing solvent may be 1.5 or more.
- the immersion time may satisfy the relationship between pH (x 2 ) of the washing solvent and the following Equation 2.
- y is the immersion time (min)
- x 2 is the pH of the washing solvent
- c is a constant from 40 to 50
- d is a constant from about 0.3 to 0.9.
- the photoelectric conversion device may include a light absorption layer containing an organometallic halide, and the washing solvent may be capable of reacting with the organometallic halide and the SN 2 reaction.
- the perovskite photoelectric conversion device may be a transparent electrode layer, a hole blocking layer, an electron collecting layer, a light absorption layer, a hole transport layer and a metal electrode layer sequentially formed on a transparent substrate.
- the light absorbing layer, the hole transport layer, the metal electrode layer or a combination thereof may be removed by immersing the waste module in the cleaning solution, and the substrate having the transparent electrode layer and the electron collecting layer may be recovered.
- the method may further include forming a light absorption layer, a hole transport layer, a metal electrode layer, or a combination thereof on the recovered substrate.
- the present invention also provides a perovskite photoelectric conversion device regenerated by the above method.
- the present invention improves the existing method of discarding the perovskite photoelectric conversion element at the end of life in the form of a module, to remove the perovskite light absorber, hole transport layer, metal electrode, etc. from the closed module of the photoelectric conversion element By recovering the to be able to re-fabricate at the initial high photoelectric conversion efficiency level can reduce the production cost of the perovskite photoelectric conversion device.
- 1 is a cross-sectional view illustrating a general structure of a solar cell of perovskite.
- 3 and 4 are a cross-sectional view and a plan view showing a structure of a perovskite solar cell according to an embodiment, respectively.
- 5 and 6 are a cross-sectional view and a plan view showing the structure of a solar cell after washing according to the present invention, respectively.
- FIG. 9 and 10 are photographs and result graphs showing an experimental procedure according to Test Example 2.
- FIG. 11 is a photograph of a perovskite solar cell and a solar cell substrate after washing according to Examples 1 to 3 of the present invention.
- FIG. 13 is an EDS (Energy-dispersive X-ray spectroscopy) analysis result for confirming the presence of impurities and components in the solar cell substrate washed according to Example 3 of the present invention.
- the term “combination of these” included in the expression of the makushi form means one or more mixtures or combinations selected from the group consisting of the constituents described in the expression of the makushi form, wherein the constituents It means to include one or more selected from the group consisting of.
- module' refers to a structure having a perovskite light absorption layer between at least the first and second electrodes
- the term 'closed module' refers to a module which is difficult to use any more because its life is almost over. Refers to.
- the substrate refers to a structure in which a conductive layer is formed on at least a rigid or flexible substrate, and further, a hole blocking layer, an electron collecting layer, or both may be formed. It does not contain a metal electrode layer or a light absorption layer.
- the dye-sensitized solar cell 100 may have a sandwich structure in which two electrodes, that is, the first electrode 20 and the second electrode 50 are bonded to each other, but may not be limited thereto.
- the first electrode 20 may be represented as a working electrode or a semiconductor electrode, but may not be limited thereto.
- the first electrode 20 may be formed on the transparent substrate 10.
- a light absorption layer 30 may be formed on the first electrode 20, and the light absorption layer 30 may include an organometallic halide perovskite in which electrons are excited due to absorption of visible light. .
- a hole transport layer 40 may be formed on the light absorption layer 30, and a second electrode 50 may be formed on the hole transport layer 40.
- the hole transport layer 40 may be formed to reduce the oxidized light absorbing layer 30, but may not be limited thereto.
- the hole transport layer 40 may not be limited to being formed in one plane on the light absorption layer 30.
- the perovskite solar cell when sunlight is incident, photons are first absorbed by the perovskite in the light absorption layer 30, and thus the perovskite is excited in the ground state.
- the electron transitions to a state to form an electron-hole pair, and the electrons in the excited state may be injected into the conduction band of the semiconductor fine particle interface.
- the injected electrons are transferred to the first electrode 20 through an interface, and then moved to the second electrode 50, which is a counter electrode facing the first electrode 20 through an external circuit.
- the perovskite oxidized as a result of the electron transfer is reduced by the oxidation-reduction couple ions in the hole transport layer 40, and the oxidized ions of the second electrode 50 are formed to achieve charge neutrality.
- the solar cell can be operated by causing a reduction reaction with electrons reaching the interface.
- the first electrode 20 is also referred to as a transparent electrode, indium tin oxide (ITO), fluorine tin oxide (FTO), ZnO-Ga 2 O 3 , ZnO It may include, but is not limited to, a material selected from the group consisting of -Al 2 O 3 , tin oxide, zinc oxide, and combinations thereof.
- the transparent electrode may be used without particular limitation as long as it has a material having conductivity and transparency.
- the transparent substrate 10 may use a glass substrate or a plastic substrate.
- Plastic substrates include polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polycarbonate (PC), polypropylene (PP), and polyimide. : PI), tri-acetyl cellulose (TAC), and combinations thereof, but may be selected from the group consisting of, but is not limited thereto.
- PVD physical vapor deposition
- the light absorption layer 30 includes an organometallic halide perovskite represented by the following formula (1) as a light absorber.
- A is an alkyl group of C 1-20, an alkyl group of C 1-20 substituted by an amine group, or an alkali metal, an alkaline earth metal metal, and M is a transition metal such as Pb, Sn, Ti, Nb, Zr, Ce, or after transition One selected from the group consisting of metals and combinations thereof, X is a halogen atom.
- the perovskite represented by Formula 1 may have a structure as shown in FIG. 2 and be prepared from MX 2 and AX, but may not be limited thereto.
- the perovskite represented by Chemical Formula 1 is an organic-inorganic composite material having an AMX 3 structure, wherein R is a C 1-20 alkyl group substituted with an C 1-20 alkyl group or an amine group, or Li, Na, K, Rb. , Alkali metals such as Cs, Fs, alkaline earth metals, transition metals such as Pb, Sn, Ti, Nb, Zr, Ce, post-transition metals and combinations thereof, and halogen in X Corresponds to The alkyl group may have 1 to 20 carbon atoms, but may not be limited thereto.
- the carbon number may be about 1 to about 20, about 1 to about 10, about 1 to about 6, about 6 to about 20, about 6 to about 10, or about 10 to about 20, but is not limited thereto.
- the halogen may be F, Br, Cl, or I, but may not be limited thereto.
- the dye represented by Formula 1 may be CH 3 NH 3 PbI 3 , but may not be limited thereto.
- the dye represented by Chemical Formula 1 has an excellent light harvesting effect even in a thin film because the absorption coefficient is higher in an index unit than a general organic dye. Thus, when the dye represented by Chemical Formula 1 is used, the dye is sensitive. Even if the solar cell has a thin light absorption layer, high energy conversion efficiency may be achieved, but may not be limited thereto.
- the hole transport layer 40 may include a hole transport monomolecular material or a hole transport polymer material, but may not be limited thereto.
- a hole transport monomolecular substance inorganic materials such as NiO or CuSCN or spiro-MeOTAD [2,2'7,7'-tetrakis- (N, N-di-p-methoxyphenyl-amine) -9,9 '-spirobifluorene] may be used, and P3HT [poly (3-hexylthiophene)] may be used as the hole transport polymer material, but may not be limited thereto.
- the hole transport layer may further include all selected from the group consisting of Li-based dopants, Co-based dopants, and combinations thereof as a doping material, but may not be limited thereto.
- the hole transport layer may further include an additive such as tBP, but may not be limited thereto.
- tBP a mixture of spiro-MeOTAD, tBP, and Li-TFSI may be used as a material constituting the hole transport layer, but may not be limited thereto.
- hole transport may be efficiently performed even in a thick film, but is not limited thereto. Can be.
- the hole transport material included in the hole transport layer 40 has a short hole transport property, it is difficult to apply when the thickness of the light absorbing layer included in the solar cell is thick, but includes a conventional ruthenium metal complex.
- the light absorbing layer is thinner, there is a problem in that the current density is lowered to increase the energy conversion efficiency, so that the light absorbing layer has difficulty in grafting with the hole transport layer.
- using a perovskite light absorbing layer having a high extinction coefficient instead of the ruthenium metal complex can secure a high current density and a high energy conversion efficiency even if the thickness thereof is thin, to be combined with the hole transport layer. There is an advantage to fit.
- the second electrode 50 is from the group consisting of Pt, Au, Ni, Cu, Ag, In, Ru, Pd, Rh, Ir, Os, C, conductive polymer, and combinations thereof It may include one selected, but may not be limited thereto.
- the second electrode that is, the counter electrode, any conductive metal material may be used without particular limitation. If the conductive material is formed only at a portion facing the first electrode, the conductive electrode may be used, but the present invention is not limited thereto. have.
- the present invention relates to a method for efficiently recovering a substrate from a closed module of a perovskite-based photoelectric conversion device.
- the cleaning capacity of the perovskite photoelectric conversion device waste module is different according to the dipole moment and pH of the cleaning solvent, and as a result, an optimal process time can be derived.
- the present invention includes a method for regenerating a perovskite photoelectric conversion device waste module, comprising the step of immersing the waste module of the perovskite photoelectric conversion device in a washing solvent for a time satisfying the condition of Equation 1 below. to provide.
- y is the dipping time (min)
- x 1 is the dipole moment of the washing solvent
- a is a constant of 700 to 850
- b is a constant of 4 to 6.
- a may be a constant of 750 to 800, b may be a constant of 4.5 to 5.5.
- the immersion time may satisfy the relationship between pH (x 2 ) of the washing solvent and the following Equation 2.
- y is the immersion time (min)
- x 2 is the pH of the washing solvent
- c is a constant from 40 to 50
- d is a constant from about 0.3 to 0.9.
- c may be a constant of 40 to 45
- d may be a constant of 0.4 to 0.8.
- the photoelectric conversion element as described above includes a light-absorbing layer containing an organic metal halide
- the cleaning solvent may be a possible the organic metal halide and S N 2 reaction.
- the dipole moment of the washing solvent may be 1.5 or more.
- a solvent having a large dipole moment may have a partial positive charge ( ⁇ + ) and a partial negative charge ( ⁇ ⁇ ) charge as follows.
- the perovskite cation component is surrounded by the partial negative charge ( ⁇ ⁇ ) of the washing solvent and is not free.
- the halogen component of the perovskite may be free without binding to the partial positive charge ( ⁇ + ) of the washing solvent by the steric hindrance of the washing solvent.
- the S N 2 reaction of the perovskite washing solvent is smooth as shown below, and the halogen atom (X) can be easily removed.
- FIG. 3 schematically shows a cross section of the structure of a perovskite solar cell, which is a representative perovskite photoelectric conversion element.
- FIG. 4 is a plan view of the perovskite solar cell shown in FIG. 3.
- the transparent substrate 10, the transparent electrode 20, the light absorbing layer 30, the hole transport layer 40 and the metal electrode 50 are included, and the electron collecting layer between the transparent electrode 20 and the light absorbing layer 30. 60 and the hole blocking layer 70 are formed.
- the electron collecting layer 60 is for efficiently receiving the electrons excited in the perovskite light absorbing layer to move to the transparent electrode.
- the electron moving distance of the light absorbing layer is short, so that the generated electrons reach the transparent electrode.
- a material having a relatively long electron moving distance is used to transfer electrons to the transparent electrode while reducing recombination.
- the conduction band should be lower than the conduction band of the perovskite photoelectric conversion element, so that electrons can move, and metal oxides such as TiO2 and ZnO (ceramic materials)
- a conductive polymer such as PCBM may be used.
- a high porosity form is advantageous in which electrons can easily increase the electron collection layer / perovskite contact area, and a transparent electron collection layer is advantageous to send sufficient light to the light absorbing layer.
- the hole blocking layer 70 is basically used to prevent the short-circuit from occurring because the valence band, the hole transport layer, or the second electrode of the light absorption layer is in direct contact with the transparent electrode. Prevents recombination with holes.
- the form covering the transparent electrode densely in a thin form is effective so as not to inhibit the generated electrons from moving to the transparent electrode. Generally TiO 2 or ZnO is used.
- the light absorbing layer, the hole transport layer, the metal electrode layer or a combination thereof are removed by immersing the waste module in the cleaning solution under a predetermined condition, and the substrate having the transparent electrode layer and the electron collecting layer can be recovered. have.
- 5 and 6 are schematic cross-sectional and plan views of the module after cleaning. 3 and 4, after washing, the light absorbing layer 30, the hole transport layer 40, and the metal electrode layer 50 are removed, and the transparent electrode layer 20, the hole blocking layer ( 70) and only the electron collecting layer 60 remains.
- the washed substrate may be rinsed with distilled water or ethanol and then subjected to a drying process.
- the rinsing process or the drying process can be applied without limitation as long as it is generally used in the related industry, and thus detailed description thereof is omitted.
- the substrate recovered as described above may be regenerated by a photoelectric conversion device through a process of forming a light absorption layer, a hole transport layer, a metal electrode layer, or a combination thereof in a subsequent process.
- FTO glasses (Pilkington, TEC-8, 8 ⁇ / sq) were washed in acetone, ethanol and distilled water for 20 minutes using ultrasonic waves. The FTO substrate was then subjected to spin coating using a 0.3 M Ti (IV) bis (ethylacetoacetateto) -diisopropoxide (Aldirch) / 1-butanol (Aldrich) solution.
- a transparent conductive substrate including a hole blocking layer was prepared by coating and heat treatment at 500 ° C. for 30 minutes.
- the hole transport material comprises about 0.17 M spiro-MeOTAD, about 0.198 M tBP (4-tert-Butylpyridine), and about 64 mM Li-TFSI (Bis (trifluoromethane) sulfonimide lithium salt)
- Li-TFSI Bis (trifluoromethane) sulfonimide lithium salt
- a hole transport solution was prepared.
- Li-TFSI was first dissolved in acetonitrile at a concentration of 0.1977 g / mL and then added in solution.
- the prepared hole transport solution was spin coated on the light absorbing layer to form a hole transport layer.
- the electrode layer was formed by depositing about 30 nm or more of gold (pressure of 10 ⁇ 6 torr or less) using a thermal evaporator on the hole transport layer.
- the manufactured perovskite solar cell was used until the end of life.
- the solar cell prepared in Preparation Example 1 was immersed in the solvent of Table 1 at room temperature (25 ° C) and then shaken (150 rpm) to measure the time at which the perovskite light absorbing layer, the hole transport layer, and the metal electrode layer were completely dissolved.
- the time point at which the perovskite was completely dissolved was based on when the transmittance of the substrate was maintained at not less than 95%. 7 shows the state at the time point 20 seconds after washing and after the start of washing.
- y immersion time (min)
- x 1 is the dipole moment of the cleaning solvent
- a1 is about 787
- b1 is about 4.9.
- Test Example 2- Check washing characteristics according to pH of washing solution
- y immersion time (min)
- x 2 pH of washing solvent
- c1 is about 43
- d1 is about 0.6.
- the end-of-life perovskite solar cell prepared in Preparation Example was immersed in gamma butyrolactone (GBL), gamma butyrolactone / dimethylsulfoxide mixed solution (GBL / DMSO volume ratio 7/3), and dimethylformamide (DMF).
- GBL gamma butyrolactone
- GL / DMSO volume ratio 7/3 gamma butyrolactone / dimethylsulfoxide mixed solution
- DMF dimethylformamide
- the washing process was immersed in the vibration condition (150rpm) until the perovskite light absorbing layer, the hole transport layer and the metal electrode layer completely dissolved, rinsed with distilled water and heated at 100 °C or more for 30 minutes to remove the solution.
- FIG. 13 shows the results of energy-dispersive X-ray spectroscopy (EDS) analysis to confirm the presence of impurities and components remaining on a substrate washed with a DMF solution.
- the total oxygen, titanium and tin atoms were 95.95% by weight and 93.39% by atom, indicating almost no impurities.
- a light absorbing layer, a hole transport layer, and a metal electrode layer were formed on the substrates recovered in Examples 1 to 3 in the same manner as in Preparation Example to fabricate a perovskite solar cell.
- photocurrent-voltage characteristics were measured.
- the measurement was performed under standard conditions of about 1.5 G AM and 1 solar condition (100 mW / cm 2 ) using a solar simulator.
- the photocurrent density (Jsc), the photovoltage (Voc), the layer density coefficient (FF), and the photoelectric conversion efficiency (PCE) were as shown in Figs. From the above results, it can be seen that various characteristics including photoelectric conversion efficiency before and after washing were improved.
- the present invention improves the existing method of discarding the perovskite photoelectric conversion element at the end of life in the form of a module, to remove the perovskite light absorber, hole transport layer, metal electrode, etc. from the closed module of the photoelectric conversion element By recovering the to be able to re-fabricate at the initial high photoelectric conversion efficiency level can reduce the production cost of the perovskite photoelectric conversion device.
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Abstract
Description
시험예 | 용매 | 쌍극자 모멘트 | 시간(min) |
1-1 | 2-프로판올 | 1.58 | 120.8 |
1-2 | 메탄올 | 1.70 | 58 |
1-3 | 아세톤 | 2.88 | 1.67 |
1-4 | 디메틸포름아마이드 | 3.82 | 1.0 |
1-5 | 감마부티로락톤 | 4.27 | 1.17 |
시험예 | pH | 시간(min) |
2-1 | 1.5 | 115.5 |
2-2 | 3.0 | 265 |
2-3 | 4.5 | 417.7 |
2-4 | 6.0 | 1850 |
2-5 | 8.0 | 4811 |
Claims (9)
- 페로브스카이트 기반의 광전변환소자의 폐모듈을 하기 수학식 1의 조건을 만족하는 시간 동안 세척 용매에 침지하는 단계를 포함하는, 페로브스카이트 광전변환소자 폐모듈의 재생 방법:[수학식 1]y=ax1 -b상기 식에서, y는 침지시간 (min), x1 은 세척용매의 쌍극자 모멘트, a은 700 내지 850의 상수, b은 4 내지 6의 상수임.
- 제1항에 있어서,상기 세척 용매의 쌍극자 모멘트가 1.5 이상인 것인 페로브스카이트 광전변환소자 폐모듈의 재생 방법.
- 제1항에 있어서,상기 침지시간은 세척용매의 pH (x2)와 하기 수학식 2의 관계를 만족하는 것인, 페로브스카이트 광전변환소자 폐모듈의 재생방법:[수학식 2]y=cedx2상기 식에서, y는 침지시간(min), x2 는 세척용매의 pH, c는 40 내지 50 의 상수이고, d는 약 0.3 내지 0.9의 상수임.
- 제1항에 있어서,상기 광전변환소자 폐모듈은 유기금속할라이드를 함유하는 광흡수층을 구비하며, 상기 세척용매는 상기 유기금속할라이드와 SN2 반응이 가능한 것인, 페로브스카이트 광전변환소자 폐모듈의 재생방법.
- 제4항에 있어서,상기 페로브스카이트 광전변환소자는 투명기판 상에 투명전극층, 정공차단층, 전자수집층, 광흡수층, 정공이동층 및 금속전극층이 순차적으로 형성되어 있는 것인 페로브스카이트 광전변환소자 폐모듈의 재생방법.
- 제5항에 있어서,상기 세척 용액에 침지함으로써 광흡수층, 정공이동층, 금속전극층 또는 이들의 조합을 제거하고 투명전극층 및 전자수집층을 구비한 기판을 회수하는 것인 페로브스카이트 광전변환소자 폐모듈의 재생방법.
- 제6항에 있어서,회수된 기판에 광흡수층, 정공이동층, 금속전극층 또는 이들의 조합을 형성하는 단계를 더 포함하는 것인 페로브스카이트 광전변환소자 폐모듈의 재생방법.
- 제7항에 있어서,상기 페로브스카이트 광전변환소자가 페로브스카이트 태양전지인 것인 페로브스카이트 광전변환소자 폐모듈의 재생방법.
- 제1항 내지 제8항 중 어느 한 항의 방법에 의해 재생된 페로브스카이트 광전변환소자.
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CN109638159A (zh) * | 2018-11-06 | 2019-04-16 | 深圳华中科技大学研究院 | 可循环利用的钙钛矿太阳能电池及其制备与循环利用方法 |
CN109786561B (zh) * | 2019-01-22 | 2023-07-11 | 华清创智光电科技(清远)有限公司 | 一种用胺类液化钙钛矿方法回收再利用钙钛矿器件中钙钛矿活性层的工艺 |
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