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WO2016009450A2 - Dispositifs photoniques composés d'un matériau de type pérovskite à base d'halogénures organométalliques et leur procédé de préparation - Google Patents

Dispositifs photoniques composés d'un matériau de type pérovskite à base d'halogénures organométalliques et leur procédé de préparation Download PDF

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WO2016009450A2
WO2016009450A2 PCT/IN2015/000288 IN2015000288W WO2016009450A2 WO 2016009450 A2 WO2016009450 A2 WO 2016009450A2 IN 2015000288 W IN2015000288 W IN 2015000288W WO 2016009450 A2 WO2016009450 A2 WO 2016009450A2
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perovskite
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photonic device
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type region
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WO2016009450A3 (fr
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Dinesh Kabra
Kumar Naresh Kumawat
Amrita Dey
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Indian Institute of Technology Bombay
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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
    • H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/50—Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K39/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic radiation-sensitive element covered by group H10K30/00
    • H10K39/10—Organic photovoltaic [PV] modules; Arrays of single organic PV cells
    • H10K39/15—Organic photovoltaic [PV] modules; Arrays of single organic PV cells comprising both organic PV cells and inorganic PV cells
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/10—Organic polymers or oligomers
    • H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
    • H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/10—Organic polymers or oligomers
    • H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
    • H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene
    • H10K85/1135—Polyethylene dioxythiophene [PEDOT]; Derivatives thereof
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/20—Carbon compounds, e.g. carbon nanotubes or fullerenes
    • H10K85/211—Fullerenes, e.g. C60
    • H10K85/215—Fullerenes, e.g. C60 comprising substituents, e.g. PCBM
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

Definitions

  • the present invention relates to photonic devices in the field of optoelectronics, more specifically photonic devices for electroluminescence application that are based on perovskite semiconductors.
  • the invention also relates to the process of making photonic devices, which are based on perovskite semiconductors.
  • the present invention describes a photonic device or more specifically an electroluminescence device, which comprises an organo-metallic halide based perovskite semiconductor layer and a method of preparation of the same.
  • a photonic or an electroluminescent device with perovskite layer as an active layer is described.
  • the active organo-metallic halide-based perovskite semiconductors with band gaps varying from NIR to visible at room temperature are achieved.
  • the Band gap of a semiconductor is varied by either changing of halide ion or by using mixed halide ion compositions and therefore the halide ion composition has an essential role to play in these photonic devices in lieu of the perovskite semiconductor layer.
  • a method of processing photonic devices with electroluminescence application, with incorporated perovskite material tunable to a range of band gap is also described in the invention.
  • Figure 1 is a schematic diagram of a photonic device representing the various layers including the organo-metallic halide based perovskite semiconductor layer as a light emitting/responsive layer.
  • Figure 2a represents the X-Ray diffraction of an as deposited perovskite (ABI3- xClx) film using spin coating technique on glass substrate and
  • Figure 2b represents X-Ray diffraction of perovskite film on glass substrate after annealing at 90°C for 45 minutes.
  • Figure 3 represents X-ray diffraction of ABbperovskite material on glass substrate after annealing at 100°C for 15 min.
  • Figure 4 represents X-ray diffraction of ABBr3perovskite material on glass substrate after annealing at 100°C for 10 min.
  • Figure 5 represents X-ray diffraction of ABChperovskite material on glass substrate after annealing at 100°C for 1 min.
  • Figure 6 represents x-ray diffraction of AB(Bri- x Cl x )3 perovskite series on glass substrate. Here ABCb mixed with ABB in different concentration XRD was measured.
  • Figure 7 represents x-ray diffraction of AB(Ii -x Br x )3 perovskite series on glass substrate. Here ABBn mixed with ABI3 in different concentration XRD was measured.
  • Figure 8 represents first order peak position vs CI composition of AB(Bn. x Cl )3 .
  • Figure 9 represents first order peak position vs Br composition of AB(Ii -x Br x )3 .
  • the ABBr 3 is mixed with ABCb in different concentration and first order XRD peak shift towards higher angle with Br composition.
  • Figure 10 represents FESEM image of (a) ABI 3 (b) ABBr 3 (c) ABC and (d) ABI3- xClx on glass/PEDOT:PSS substrate after annealing.
  • Figure 11 represents FESEM image of AB(Bn- x Cl x ) series at different concentrations of CI and respective halide composition in the image.
  • Figure 12 represents FESEM image of AB(Il-xBrx) series at different concentrations of Br and respective halide composition in the image.
  • Figure 13 represents Absorbance spectra (absorbance vs energy) of ABI3 ( ⁇ ), ABBr3 (o) and ABCb ( ⁇ ) perovskites on glass substrate after annealing.
  • Figure 14 represents Photoluminescence (PL vs energy) of ABI3 ( ⁇ ), ABBr 3 (o) and ABCb ( ⁇ ) perovskites on glass substrate after annealing.
  • Figure 15 represents Absorbance spectra of AB(Bri -x Clx)3 series using different Br/CI ratio to tune the band gap from 2.2 eV (green) 3.1 eV.
  • Figure 16 represents the Photoluminescence of AB(Bn -x Clx) 3 series using different Br/CI ratio to tune the band gap from 2.2 eV (green) 3.1 eV (UV).
  • Figure 17 represents Band gap vs CI composition of AB(Bn -x Clx)3 series and fitted (Red solid line) using second order polynomial to determine bowing parameter.
  • Inset shows PLQE vs CI composition.
  • Figure 18 represents Lattice parameter vs CI composition of AB(Bri- x Cl x ) series and fitted (red solid line) with straight line.
  • Figure 19 represents Absorbance spectra of AB(Ii -x Brx)3 series using different- Br/1 ratio to tune the band gap from 2.2 eV (green) 1.6 eV (NIR).
  • Figure 20 represents Photoluminescence of AB(Ii -x Br x )3 series using different Br/I ratio to tune the band gap from 2.2 eV (green) 3.1 eV (UV).
  • Figure 21 represents Band gap vs Br composition of AB(Ii -x Br x )3 series and fitted (Red solid line) using second order polynomial to determine bowing parameter.
  • Figure 22 represents Lattice parameter vs Br composition of AB(Bn -x Cl x ) series and fitted (red solid line) with straight line.
  • Figure 23 represents Electroluminescence (EL) spectra of perovskite materials using ITO/HIL/Perovskite/EIL/metal electrode.
  • Figure 24 represents J-V-L characteristics of blue emitting perovskite ITO/PEDOT:PSS/ABBrl .08C11.92/PCBM/Ag and inset image of working blue PeLED inside the figure.
  • Figure 25 represents Cd/A vs Voltage (solid circle) and EQE vs Voltage (open circle) of ITO/PEDOT:PSS/ABBrl .08C11.92/PCBM/Ag PeLED.
  • Figure 26 represents J-V-L characteristics of blue emitting perovskite ITO/PEDOT:PSS/ABBrl .08C11.92/PCBM/Ag and inset image of working blue PeLED inside the figure.
  • Figure 27 represents Cd/A vs Voltage (solid circle) and EQE vs Voltage (open circle) of ITO/PEDOT:PSS/ABBrl .08Cll .92/PCBM/Ag PeLED.
  • Figure 28 represents J-V-L characteristics of blue emitting perovskite ITO PEDOT:PSS/ABBrl .08C11.92/Ag and inset image of working blue PeLED inside the figure.
  • Figure 29 represents J-V-L characteristics of blue emitting perovskite ITO/PEDOT:PSS/ABBr 1.08C11.92/Ag PeLED.
  • Figure 30 represents J-V-L of ITO/PEDOT: PSS/TPD/ABBr 3 /Ag and inset image of working blue PeLED inside the figure.
  • Figure 31 represents Cd/A vs Voltage (empty circle) and EQE vs Voltage (solid circle) of ITO/PEDOT: PSS/TPD/ABBr 3 /Ag PeLED.
  • Figure 32 represents J-V-L of ITO/PEDOT:PSS/ABBrl.87C11.17/Ag PeLED.
  • Figure 33 represents Cd/A vs Voltage (empty circle) and EQE vs Voltage (solid circle) of ITO/PEDOT:PSS/TPD/ABBrl .87C11.17/Ag PeLED.
  • Figure 34 represents J-V-L characteristics of ITO/PEDOT:PSS/ABIi .25Bri. 75 /Ag red PeLED.
  • Figure 35 represents Cd/A vs Voltage (empty circle) and EQE vs Voltage (solid circle) of ITO/PEDOT:PSS/TPD/ABIi 25 Br, 75 /Ag PeLED.
  • Figure 36 represents J-V (solid circle) and Radiance vs voltage for ITO/PEDOT: PSS/ABI3-xClx PCBM/Ag diode.
  • Figure 37a and 37b shows photo luminance spectra of perovskites film with various interfaces of charge transporting layers with respect to wavelength and energy, respectively.
  • Figure 38 represents absorbance, photoluminescence and electroluminescence measurements on energy and wavelength scales. Inset in forth quadrant of figure shows blue shifted EL with respect to higher injection current.
  • Figure 39 represents (a) J-V-L characteristics, (b) luminance (solid) and power efficiency (open) vs applied bias, (c) luminance efficiency versus bias voltage and (d) external quantum efficiency vs. bias voltage for perovskite LED with structure of ITO/Ti0 2 /Al 2 03/CH3NH 3 PbClBr/P3HT/Au, wherein the device area is 4.5 mm 2 . Light emission peak wavelength is 680 nm.
  • Figure 40 wherein the four graphs represents J-V-L characteristics, luminance (solid) and power efficiency (open), luminance efficiency vs. bias voltage and external quantum efficiency vs. bias voltage for perovskite LED with device structure of ITO/ZnO/Ba(OH)2/CH 3 NH3PbClBr/P 3 HT/Au, wherein the Device area is 4.5 mm1 ⁇ 2nd the Light emission peak wavelength is 680 nm.
  • Figure 41 wherein the four graphs represents (a) I-V-L characteristics, (b) luminance (solid) and power efficiency (open)vs bias voltage, (c) luminance efficiency vs. bias voltage and (d) external quantum efficiency vs. bias voltage for perovskite LED(ITO/Ti0 2 / Al 2 0 3 /CH3NH 3 PbClBr/Mo0 3 /Au).
  • Device area is 4.5 mm 2 .
  • Light emission peak wavelength is 680 nm.
  • Figure 42 represents J-V-L characteristics of mixed perovskite of different diodes fabricated on same substrate with device structure of ITO/PEDOT:PSS/CH3NH 3 PbIxCli.x/PCBM/Ag.
  • Light emission peak wavelength is 780 nm.
  • Figure 43 represents external quantum efficiency (EQE) for mixed perovskite LED in ITO/PEODT: PSS/Perovskite (CHsNFhPblxCbxVPCBM/Ag structure for different diodes on same substrate.
  • Light emission peak wavelength is 780 nm.
  • Figure 44 represents external quantum efficiency (EQE) versus current density for mixed perovskite LEDs in ITO/PEODT: PSS/Perovskite (CH3NH 3 PbI x Cl 3x )/PCBM/Ag structure for different diodes on same substrate.
  • Figure 45 represents an overview of the synthesis of halide based perovskite materials.
  • Figure 46 represents an overview of the device fabrication of halide based perovskite materials.
  • the present invention is a photonic device especially for electroluminescence (EL) application.
  • This electroluminescence device which has a light emitting layer comprises a p-type region having a p-type layer for hole injection (hole injection/extraction layer).
  • Figure 1 is a schematic arrangement of the various layers along with the light emitting perovskite film.
  • perovskite it is to be understood that the perovskite crystalline nature in various permutations and combinations is referred.
  • the p-type region and n-type region can be an organic conducting polymer or inorganic or organic material.
  • the perovskite semiconducting material is accountable for the photo generation and charge transportation and thereby enabling the device to be an electroluminescence device.
  • This halide based perovskite can be a p-type or n-type or intrinsic semiconductor layer which is sandwiched in between p-type and n-type hole and electron injection layer respectively or in between one electrode and one p or n-type carrier injection layer and vice versa.
  • the two electrodes mentioned above for electrical contact is such that one is a metallic reflective electrode and the other is a transparent material electrode.
  • the perovskite material when the device is a general photonic/light emitting diode, can been deposited on top of the hole injection/extraction layer followed by a high electron affinity layer for electron injection/extraction and a contact electrode (low work function metal).
  • perovskites can be deposited on top of an electron injection/extraction layer followed up by high work-function conducting layer for holes injection/extraction from top contact electrode (high work-function metal).
  • the perovskite layer is a crystal structure, represented by the formula ABX3, where in “A” and “B” are first and second cations respectively and "X" is an anion.
  • A is represented by R-NH3.
  • R in this case is an alkyl group or aromatic group or a monovalent metal ion and B is a divalent metal cation.
  • B is selected from the group of Cu 2+ , Ni 2+ , Co 2+ , Fe 2+ , Mn 2+ , Pd + , Cd 2+ , Ge 2+ , Sn + , Pb 2+ , Eu 2+ , etc.
  • X is a single halide or a hybrid halide selected from the group of I, CI, Br and F and combinations thereof.
  • the perovskite structure combination used can be CFhNFbPbfli-xBrxK CH 3 NH3Pb(Bri -x Clx)3, CH3NH3PbI 3 -x -y ClxBr y , or similar combinations (Ct NHsPbb-xClx) of perovskites materials where x varies from 0 to 1.
  • the morphology and crystallinity of the perovskite layer depends on the halide ion and substrate wetting conditions, where crystallite size varies from ⁇ 100s nm to few micrometers. Therefore, in lieu of the mentioned parameters that have a huge influence on the optical properties and performance of light emitting diodes (LEDs) using these perovskites as the active layer and photonic devices in general, a new avenue of materials for photonic devices and LEDs specifically is made available in the present invention.
  • LEDs light emitting diodes
  • the invention further describes a method of producing a photonic device with an organo-metallic halide based perovskite semiconductor film layer; the active layer in the photonic device.
  • the low temperature solution processability and the completely tunable optical direct band gap over a wide range makes it a potential candidate for tandem solar cells, wavelength tune able light emitting diodes and electrical injection laser.
  • the band gap of semiconductor is varied by either changing of halide ion or by using mixed halide ion compositions.
  • good wetting of the contact by the perovskite layer is very important for obtaining leakage free devices.
  • the first step involves the synthesis of the precursor followed by the preparation of the perovskite precursor solution.
  • Figure 45 represents an overview of steps in the synthesis of the perovskite materials to make the perovskite solution for the photonic devices and LED application.
  • CH3NH3I was synthesized by reacting 33% by weight of methylamine (CH3NH2) in absolute ethanol (sigma Aldrich) solution with 57 % by weight of hydroiodic acid (HI) in aqueous (sigma Aldrich) solution in an equal (1 : 1) molar ratio. After which methylamine was poured into a round flask, kept at 0°C. Hydroiodic acid was added drop wise and stirred for two hours. The ensuing step is the usage of rotary evaporator to get crystalline methylammonium iodide, i.e., CH3NH3I, (MAI). The resulting precipitate is a white coloured precipitate and thereby serves as a confirmation of the crystallization of MAI. This white coloured precipitate of CH3NH3I was rinsed three times with diethyl ether for 30 minutes and dried using rotary evaporator at temperature and pressure conditions of 55°C and 500 mbar.
  • CH 3 NH3Br was synthesized by reacting 33% by weight of methylamine (CH3NH2) in absolute ethanol (sigma Aldrich) solution with 47 % by weight of hydrobromic acid (HBr) in aqueous solution (Merck) at equal (1 : 1 ) molar ratio. Following which, methylamine was poured in round flask, kept at 0°C. Hydrobromic acid was added drop wise in methylamine solution, and stirred for two hours. After that, rotary evaporator was used to get crystalline (MABr) methylammoniumbromide (CE NFhBr) which is a light orange colored precipitate thereby confirming the crystallization of MABr. The precipitate is then rinsed three times with diethyl ether for 30 minutes and dried using rotary evaporator, at 55°C and 500 mbar.
  • MABr crystalline methylammoniumbromide
  • CH3NH3CI was synthesized using methylamine (CH3NH2) 33 wt% in absolute ethanol (Sigma Aldrich) solution and hydrochloric acid (HC1) 37wt% in aqueous (Merck) solution in equal (1 : 1) molar ratio. Methylamine was kept at 0 °C and Hydrochloric acid was added drop wise to it and stirred for two hours. After that, rotary evaporator was used to get crystalline methylammoniumchloride (CH3NH3CI). White colored precipitate confirmed the crystallization of CH3NH3CI. Further, it was rinsed three times with diethyl ether for 30 min and dried using a rotary evaporator at 50°C followed by vacuum drying for over night.
  • ABh xClx perovskite precursor is prepared by reacting methylammonium iodide (CH3NH3I) precipitate with lead chloride (PbC from Sigma-Aldrich) and later dissolved in (DMF) anhydrous dimethylformamide (C3H7NO from Sigma Aldrich) in 3: 1 molar ratio.
  • CH3NH3I methylammonium iodide
  • PbC lead chloride
  • DMF anhydrous dimethylformamide
  • lead(II)chloride PbCl 2 can be replaced by any divalent metal halide e.g. lead(II)bromide (PbBr ) lead(II)iodide (Pbl 2 ), tin(II)chloride (SnCb), tin(II)bromide (PbBr 2 ), tin(II)iodide (Snl 2 ), lead(II)iodide (Pbl 2 ) and copper halide (here halides are CI, Br and I) for tuning the perovskite band gap from UV to near IR, further varying the concentration of the perovskite.
  • CHsNtbPbb-x-yCl Bry solution can be prepared by reacting methylammonium iodide (CH3NH3I) precipitate with lead(II)chloride (PbCb from Sigma-Aldrich) and lead bromide (PbBr 2 from sigma Aldrich) and the resulting mixture is dissolved in (C3H7NO) dimethylformamide (DMF) (Merck) in 3: 1 : 1 molar ratio.
  • C3H7NO dimethylformamide
  • DMF dimethylformamide
  • 40 % by weight was the perovskite material and 60 % by weight was DMF. This solution was stirred over night at room temperature in nitrogen atmosphere inside the glove box (MBRUAN-MB200B).
  • lead(II)halide (PbCb) and lead(II)bromide (PbBr 2 ) can be replaced by any divalent metal halide (here halide are CI, Br and I) e.g. tin(II)chloride (SnCb), tin(II) bromide (PbBr 2 ) tin(II)iodide (Snl 2 ), lead(II)iodide (Pbl 2 ) and copper halide (here halide are CI, Br and I) for tuning the perovskite band gap.
  • halide are CI, Br and I
  • CF NF PbBn solution is prepared by reacting methylammonium bromide (CFbNFbBr) precipitate with lead bromide (PbBr 2 fromSigma-Aldrich), and dissolved in (DMF) dimethylformamide (C3H7NO from Merck) in 1 : 1 molar ratio.
  • CFbNFbBr methylammonium bromide
  • PbBr 2 lead bromide
  • DMF dimethylformamide
  • C3H7NO dimethylformamide
  • ABBr 3 solution was prepared using, Methylammonium Bromide precipitate and PbBr 2 , are dissolved in DMF in 1 : 1 molar ratio (ABBn 10wt% perovskite in DMF).
  • ABI3 methylammoniumiodide precipitate and Pbl 2 , dissolved in DMSO in 1 : 1 molar ratio (ABI3 10wt% in DMF).
  • AB(Bn -x Cl) 3 solution we mixed ABBr3 and ABI3 in volumetric ratio (1 :9, 1 :4, 3:7,2:3, 1 : 1, 6:5, 7:3, 4:2, 9: 1) in vials.
  • the solution was stirred overnight at room temperature in nitrogen atmosphere.
  • the ensuing step after the synthesis of various perovskite precursor solutions as mentioned above is the cleaning of the substrate in the photonic devices. Again by way of example, the cleaning is done in the following way:
  • the 50 mm x 50 mm x 1.1 mm ITO coated glass substrates have been patterned using an optical mask in a double-sided aligner (DSA).
  • the optimum size in to which the substrates were cut by a diamond cutter is 12.5 mm xl2.5 mm. All the substrates were cleaned with soap water, distilled water (DI), 2-propenol (IPA) and acetone for lOminutes successively in an ultra sonicator. Following which, the cleaned substrates have been put for oxygen plasma ashing at 100 Wt for 10 minutes.
  • the fabrication of the Photonic device using the perovskite material is carried out after cleaning the substrate.
  • the fabrication varies depending on whether it is a standard regular device or inverted device.
  • a standard regular device is one where in the schematic order of the device the metal electrode is followed by an n-type semiconductor and the p-type electrode is coupled with the transparent electrode.
  • An inverted device is where a p-type electrode follows the metal electrode and the n-type is coupled with the transparent electrode.
  • Figure 46 represents a systematic overview of the Photoic device fabrication steps involved in various perovskite light emitting diode, specifically the Blue, Red, Green and the NIR photonic device.
  • the step-by-step process using ClbNHsPbb- Clji tunable to a NIR photonic device or a LED for instance in a standard regular device is as follows:
  • PEDOT:PSS Hole injection/extraction layer for regular (standard) devices
  • PEDOT:PSS Sigma aldrich
  • PEDOT:PSS Sigma aldrich
  • CFbNHsPb -xClx layer was deposited on PEDOT: PSS by spin coating at 2000 rpm for 60 seconds using CHsNHsPbb-xClx precursor.
  • the perovskite layer was annealed at 100°C for 90min to evaporate the solvent and make a dense film of the perovskite.
  • the confirmation test of perovskite film in this case is the film color change from yellow to brown after annealing it.
  • Electron injection layer/extraction layer was deposited on the perovskite film by spin coating at 2000 rpm for 30seconds and annealed at 50°C for 20minutes.
  • the electrode deposition step involves depositing of 200 nm Ag (silver) using evaporation technique in l l O ⁇ mbar vacuum at room temperature.
  • Figure 2a represents the X-Ray diffraction of an as deposited perovskite (ABb-xCL) film using spin coating technique on glass substrate and Figure 2b represents X- Ray diffraction of perovskite film on glass substrate after annealing at 90°C for 45 minutes.
  • Figure 3 represents X-ray diffraction of ABI3 perovskite material on glass substrate after annealing at 100°C for 15 min.
  • Figure 4 represents X-ray diffraction of ABBr3 perovskite material on glass substrate after annealing at 100°C for 10 min.
  • Figure 5 represents X-ray diffraction of ABCb perovskite material on glass substrate after annealing at 100°C for 1 min.
  • Figure 6 represents x-ray diffraction of AB(Bri- x Cl x )3 perovskite series on glass substrate. Here ABCI3 mixed with ABBr3 in different concentration.
  • Figure 7 represents x-ray diffraction of AB(Ii- Br x )3 perovskite series on glass substrate.
  • ABBr3 mixed with ABI3 in different concentration.
  • the other methods which can be employed in the deposition of perovskite material, can be by chemical vapor deposition (CVD), thermal evaporation or dip coating method or PLD (Plus Laser Deposition) or drop casting method or LPE (Liquid Phase epitaxy).
  • CVD chemical vapor deposition
  • PLD Plus Laser Deposition
  • LPE Liquid Phase epitaxy
  • the hole injection/extraction layer can be p-type organic or inorganic semiconducting or conducting materials preferably.
  • the PEDOT:PSS (hole injection/extraction) layer can be replaced by Spiro- MeOTAD(2,2',7,7'-tetrakis(N,Ndipmethoxyphenylamine)9,9spirobifluorene), P3HT(poly(3hexylthiophene-2,5-diyl)),DEH(4-(diethylamino)- benzaldehydediphenylhydrazone), PCPDTBT (Poly[2,6-(4,4-bis-(2-ethylhexyl)- 4H-cyclopenta [2, l -b;3,4-b']dithiophene)-alt-4,7(2, l,3-benzothiadiazole), ,PCDTBT(Poly[N-9'-heptadecanyl-2,7-c
  • the electrode can be replaced by a high electron affinity material e.g. Gold (Au).
  • Au gold
  • the incorporation of a layer in between the n-type and perovskite or p- type and perovskite material would prevent the electroluminescence (EL) and photoluminescence (PL) quenching.
  • An electron injection layer/Extraction layer of Ti0 2 500 ⁇ 1 titanium di- isopropoxidebis (acetylacetonate) solution in 5ml anhydrous ethanol was deposited on the ITO substrate by spray coating (wherein oxygen is used as a carriergas) at 450°C and annealed at 500°C for 30min.
  • the films were annealed at 90°C for 90min to evaporate the solvent and make a dense film of perovskite.
  • the change in film colour from yellow to brown after annealing it was a confirmation of it becoming a perovskite film.
  • P3HT solution (15mg/ml in chlorobenzene) was prepared and deposited by spin coating at 1500rpm for 30sec and annealed at 50°C for 15 min.
  • the deposition of a hole injection layer involves a 5 nm M0O3 layer deposited by thermal evaporation in lxl0 ⁇ 6 mbar vacuum.
  • a 100 nm Au (gold) was deposited using evaporation technique in lxl0 "6 mbar vacuum.
  • electron injection/extraction layer Ti0 2 or ZnO can be replaced by any n-type semiconducting organic or inorganic material e.g.
  • the Ba(OH)2 layer can be replaced by a layer which prevents the EL and PL quenching across the interface e.g. TFB, TPD, PEI or Beta Alanine.
  • the step-by-step fabrication of Photonic device using CH3NibPbBr3 (Green) perovskite material by way of example in an inverted structure is as follows: Hole injection/extraction layer for regular (standard) devices PEDOT:PSS (Sigma aldrich) was spin coated at 4000 rpm for 60 seconds and then annealed at 150°C for 30 min under constant nitrogen flow. After which, the samples were transferred in to a nitrogen filled glove box. Then CH 3 NH 3 PbBr3 layer was deposited on PEDOT: PSS by spin coating, as spin coating gives a good crystalline film. Spin coating is carried out at 2000 rpm for 30 seconds using CH 3 NH 3 PbBr3 precursor.
  • PEDOT:PSS Sigma aldrich
  • the film layer was annealed at 100°C for 15 min to evaporate the solvent and make a dense film of perovskite.
  • the confirmation test of perovskite film in this case is the film color become orange after annealing it.
  • PCMB Electron injection layer/extraction layer
  • the electrode deposition step involves depositing of 200 nm Ag (silver) using evaporation technique in lxl 0 "6 mbar vacuum at room temperature.
  • the other methods which can be employed in the deposition of perovskite material, can be by chemical vapor deposition (CVD), thermal evaporation or dip coating method or PLD (Plus Laser Deposition) or drop casting method or LPE (Liquid Phase epitaxy).
  • CVD chemical vapor deposition
  • PLD Plus Laser Deposition
  • LPE Liquid Phase epitaxy
  • the hole injection/extraction layer can be p-type organic or inorganic semiconducting or conducting materials preferably.
  • the PEDOT.PSS (hole injection/extraction) layer can be replaced by Spiro- MeOTAD(2,2',7,7'-tetrakis(N,N-dipmethoxyphenylamine)9,9spirobifluorene), P3HT(poly(3hexylthiophene-2,5-diyl)),DEH(4-(diethylamino)- benzaldehydediphenylhydrazone), PCPDTBT (Poly[2,6-(4,4-bis-(2-ethylhexyl)- 4H-cyclopenta [2, 1 -b;3,4-b']dithiophene)-alt-4,7(2, 1 ,3-benzothiadiazole), ,PCDTBT(Poly[N-9'-heptadecanyl-2,7-c
  • the electron injection layer can be replaced by any n-type semiconducting or conducting material e.g. Zinc oxide (ZnO), PCBM, PC 6 iBM,
  • the electrode can be replaced by a high electron affinity material e.g. Gold (Au).
  • Au gold
  • the step-by,-step fabrication of LEDs/Photonic device using CHsNibPbili- xBi * x)3 (Red LED) perovskite material by way of example in regular structure is as follows: Hole injection/extraction layer for regular (standard) devices PEDOT:PSS (Sigma aldrich) was spin coated at 4000 rpm for 60 seconds and then annealed at 150°C for 30 min under constant nitrogen flow. After which, the samples were transferred in to a nitrogen filled glove box. Then CthNK PbOi-xBrx);? layer was deposited on PEDOT: PSS by spin coating at 2000 rpm for 30 seconds using CH 3 NH3Pb(Ii-xBr x ) precursor.
  • PEDOT:PSS Sigma aldrich
  • the film layer was annealed at 100°C for 15 min to evaporate the solvent and make a dense film of perovskite.
  • the confirmation test of perovskite film in this case is the film colour becomes light orange after annealing it.
  • PCMB electron injection layer/extraction layer
  • the electrode deposition step involves depositing of 200 nm Ag (silver) using evaporation technique in lxlO ⁇ mbar vacuum at room temperature.
  • the other methods which can be employed in the deposition of perovskite material, can be by chemical vapour deposition (CVD), thermal evaporation or dip coating method or PLD (Plus Laser Deposition) or drop casting method or LPE (Liquid Phase epitaxy).
  • CVD chemical vapour deposition
  • PLD Plus Laser Deposition
  • LPE Liquid Phase epitaxy
  • the hole injection/extraction layer can be p-type organic or inorganic semiconducting or conducting materials preferably.
  • the PEDOT:PSS (hole injection/extraction) layer can be replaced by Spiro- MeOTAD(2,2',7,7'-tetrakis(N,N-dipmethoxyphenylamine)9,9spirobifluorene), P3HT(poly(3hexylthiophene-2,5-diyl)),DEH(4-(diethylamino)- benzaldehydediphenylhydrazone), PCPDTBT (Poly[2,6-(4,4-bis-(2-ethylhexyl)- 4H-cyclopenta [2, 1 -b;3,4-b']dithiophene)-alt-4,7(2, 1 ,3-benzothiadiazole), ,PCDTBT(Poly[N-9'-heptadecanyl-2,7-c
  • the electrode can be replaced by a high electron affinity material e.g. Gold (Au).
  • Au gold
  • the incorporation of a layer in between the n-type and perovskite or p- type and perovskite material would prevent the electroluminescence (EL) and photoluminescence (PL) quenching.
  • PEDOT:PSS Hole injection/extraction layer for regular (standard) devices
  • PEDOT:PSS Sigma aldrich
  • PEDOT:PSS Sigma aldrich
  • CH3NH3Pb(Bri- x Cl x )3 layer was deposited on PEDOT: PSS by spin coating at 2000 rpm for 30 seconds using CH3NH 3 Pb(Bri. x Clx)3 precursor.
  • the film layer was annealed at 100°C for 15 min to evaporate the solvent and make a dense film of perovskite.
  • the confirmation test of perovskite film in this case is the film colour becomes light orange after annealing it.
  • PCMB electron injection layer/extraction layer
  • the hole injection/extraction layer can be p-type organic or inorganic semiconducting or conducting materials preferably.
  • the PEDOT:PSS (hole injection/extraction) layer can be replaced by Spiro- MeOTAD(2,2',7,7'-tetrakis(N,N-dipmethoxyphenylamine)9,9spirobifluorene), P 3 HT(poly(3hexylthiophene-2,5-diyl)),DEH(4-(diethylamino)- benzaldehydediphenylhydrazone), PCPDTBT (Poly[2,6-(4,4-bis-(2-ethylhexyl)- 4H-cyclopenta [2, 1 -b;3,4-b']dithiophene)-alt-4,7(2, 1 ,3-benzothiadiazole), ,PCDTBT(Poly[N-9'-heptadecanyl-2,7-
  • the electron injection layer can be replaced by any n-type semiconducting or conducting material e.g. Zinc oxide (ZnO), PCBM, PCeiBM, PC71BM.
  • the electrode can be replaced by a high electron affinity material e.g. Gold (Au).
  • Au gold
  • the incorporation of a layer in between the n-type and perovskite or p- type and perovskite material would prevent the electroluminescence (EL) and photoluminescence (PL) quenching.
  • EL electroluminescence
  • PL photoluminescence
  • Figure 9 represents first order peak position vs Br composition of AB(Ii- x Br x )3 .
  • ABBr3 mixed with ABCb in different concentration and first order XRD peak shift towards higher angle with Br composition.
  • Figure 10 represents FESEM image of (a) ABI 3 (b) ABBr 3 (c)ABCband (d) ABI 3- xClx on glass/PEDOT:PSS substrate after annealing.
  • Figure 1 1 represents FESEM image of AB(Bri-xCl x ) series at different concentration of CI and respective halide composition in image. FESEM image of (a) ABBr2.49C10.51 (b) ABBrl .86C11.14 (c) ABBrl .5C11.5 (d)
  • ABBrl .08C11.92 (e) ABBr0.87C12.13 (f) ABBr0.21C12.79 perovskite films on ITO/PEDOT:PSSsubstarte after annealing has been illustrated. It is observed that perovskites filmcoverage is good and with chlorine content domain size of AB(Bn. xCl x ) 3 perovskite changed.
  • Figure 12 represents FESEM image of AB(Ii -x Br x ) series at different concentration of Br and respective halide composition in image.
  • Figure 13 represents Absorbance spectra (absorbance vs energy) of ABI3 ( ⁇ ), ABBr 3 (o) and ABC1 3 ( ⁇ ) perovskites on glass substrate after annealing.
  • Figure 14 represents Photoluminescence (PL vs energy) of ABI 3 ( ⁇ ), ABBr 3 (o) and ABCI3 ( ⁇ ) perovskites on glass substrate after annealing.
  • Figure 15 represents UV-Vis Absorbance spectra of AB(Bri -x Clx) 3 series using differentBr/Cl ratio to tune the band gap from 2.2 eV (green) 3.1 eV and where x varies from 0 to 1.
  • Figure 16 represents Photoluminescence of AB(Bri- x Cl x ) 3 series using differentBr/Cl ratio to tune the band gap from 2.2 eV (green) 3.1 eV (UV). This photoluminescence spectra of AB(Bn -x Cl x ) 3 perovskite semiconductor film prepared on quartz substrates with excitation wavelength is indicative of their UV- Vis spectra.
  • Figure 17 represents the quadratic behavior of the bandgap of AB(Br i- x Clx)3perovskite seriesvstheCl composition and fitted (Red solid line) using second order polynomial to determine the bowing parameter.
  • the inset shows PLQE vsCl composition.
  • Figure 18 represents Lattice parameter as a function of CI composition of AB(Bri- xClx) series and fitted (red solid line) with straight line.
  • Figure 19 represents Absorbance spectra of AB(Ii -x Br x )3 series using different-Br/I ratio to tune the band gap from 2.2 eV (green) 1.6 eV (NIR).
  • Figure 20 represents Photoluminescence of AB(li -x Br x )3 series using differentBr/I ratio to tune the band gap from 2.2 eV (green) 3.1 eV (UV).
  • Figure 21 represents Bandgapvs Br composition of AB(Ii-xBr x )3 series and fitted (Red solid line) using second order polynomial to determine bowing parameter.
  • Figure 22 represents Lattice parameter vs Br composition of AB(Bri -x Cl x ) series and fitted (red solid line) with straight line.
  • Figure 23 represents Electroluminescence (EL) spectra of perovskite materials using ITO/HIL/Perovskite/EIL/metal electrode.
  • Figure 24 represents J-V-L characteristics of blue emitting perovskite ITO/PEDOT:PSS/ABBrl .08C11.92/PCBM/Ag and inset image of working blue PeLED.
  • Figure 25 represents Cd/A vs Voltage (solid circle) and EQE vs Voltage (open circle) of ITO/PEDOT:PSS/ABBrl .08C11.92/PCBM/Ag PeLED.
  • Figure 26 represents J-V-Lcharacteristicsof blue emitting perovskite ITO/PEDOT:PSS/ABBrl.08C11.92/PCBM/Ag and inset image of working blue PeLED inside the figure.
  • Figure 27 represents Cd/A vs Voltage (solid circle) and EQE vs Voltage (open circle) of ITO/PEDOT:PSS/ABBr 1.08C11.92/PCBM/Ag PeLED.
  • Figure 28 represents J-V-L characteristics of blue emitting perovskite ITO/PEDOT:PSS/ABBrl .08C11.92/Ag and inset image of working blue PeLED inside the figure.
  • Figure 29 represents J-V-L of blue emitting perovskite ITO/PEDOT:PSS/ABBr 1.08C11.92/Ag PeLED.
  • Figure 30 represents J-V-L characteristics of ITO/PEDOT:PSS/TPD/ABBr 3 /Ag and inset image of a working green PeLED inside the figure.
  • Figure 31 represents Cd/A vs Voltage (empty circle) and EQE vs Voltage (solid circle) of ITO/PEDOT:PSS/TPD/ABBr3/Ag PeLED.
  • Figure 32 represents J-V-L of ITO/PEDOT:PSS/ABBrl.87C11.17/Ag PeLED .
  • Figure 33 represents Cd/A vs Voltage (empty circle) and EQE vs Voltage (solid circle) of ITO/PEDOT:PSS/TPD/ABBrl .87C11.17/Ag PeLED.
  • Figure 34 represents J-V-L of ITO/PEDOT:PSS/ABI1.25Brl .75/Ag and the inset image of a working red PeLED inside the figure.
  • Figure 35 represents Cd/A vs Voltage (empty circle) and EQE vs Voltage (solid circle) of ITO/PEDOT:PSS/TPD/ABIl .25Brl .75/Ag PeLED.
  • Figure 36 represents J-V (solid circle) and Radiance vs voltage for ITO/PEDOT:PSS/ABI3-xClx/PCBM/Ag diode.
  • Figure 37a and 37b shows photoluminance spectra of perovskites film with various interfaces of charge transporting layers with respect to wavelength and energy, respectively.
  • Figure 38 represents absorbance, photoluminescence and electroluminescence measurements on energy and wavelength scales.
  • the inset in forth quadrant of figure shows blue shifted EL with respect to higher injection current.
  • Figure 39 represents (a) J-V-L characteristics, (b) luminance (solid) and power efficiency (open) vs applied bias, (c) luminance efficiency versus bias voltage and (d) external quantum efficiency vs. bias voltage for perovskite LED with structure of ITQ/Ti02/Al203/CH 3 NH3PbClBr/P 3 HT/Au.Device area is 4.5 mm 2 .
  • Light emission peak wavelength is 680 nm.
  • Figure 40 wherein the four graphs represents J-V-L characteristics, luminance (solid) and power efficiency (open), luminance efficiency vs, bias voltage and external quantum efficiency vs. bias voltage for perovskite LED with device structure of ITO/ZnO/Ba(OH) 2 /CH3NH3PbClBr/P 3 HT/Au.
  • the device area in the contention is 4.5 mm 2 .
  • Thelight emission peak wavelength is 680 nm.
  • Figure 41 represents wherein the four graphs represents (a) I-V-L characteristics, (b) luminance (solid) and power efficiency (open) vs bias voltage, (c) luminance efficiency vs. bias voltage and (d) external quantum efficiency vs. bias voltage for perovskite LED (ITO/Ti0 2 / Al 2 0 3 /CH 3 NH3PbClBr/Mo03/Au).
  • Device area is 4.5 mm 2 .
  • Light emission peak wavelength is 680 nm.
  • Figure 42 represents J-V-L characteristics of mixed perovskite of different diodes fabricated on same substrate with device structure of ITO/PEDOT:PSS/CH3NH 3 PbI x Cli-x/PCBM/Ag.
  • Light emission peak wavelength is 780 nm.
  • Figure 43 represents external quantum efficiency (EQE) for mixed perovskite LED in ITO/PEODT: PSS/Perovskite (CH 3 NH 3 PbIxCl3x)/PCBM/Ag structure for different diodes on same substrate.
  • Light emission peak wavelength is 780 nm.
  • Figure 44 represents external quantum efficiency (EQE) versus current density for mixed perovskite LEDs in ITO/PEODT: PSS/Perovskite (CH 3 NH 3 PbI x Cl 3 x)/PCBM/Ag structure ' for different diodes on same substrate.

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Abstract

L'invention porte sur un dispositif photonique pour une application électroluminescente et sur son procédé de préparation, le dispositif comprenant une couche de film semi-conducteur de type pérovskite disposée entre une région de type n et une région de type p, la couche de film semi-conducteur de type pérovskite étant composée d'un halogénure organométallique (ABX3) et étant accordée sur une largeur de bande interdite, la bande interdite variant de l'infrarouge proche à une plage visible à température ambiante et au moins deux couches intermédiaires, les deux, ou plus, couches intermédiaires étant incorporées entre la région de type p et la couche de film semi-conducteur de type pérovskite et la région de type n et la couche de film semi-conducteur de type pérovskite.
PCT/IN2015/000288 2014-07-17 2015-07-16 Dispositifs photoniques composés d'un matériau de type pérovskite à base d'halogénures organométalliques et leur procédé de préparation Ceased WO2016009450A2 (fr)

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WO2018007586A1 (fr) * 2016-07-07 2018-01-11 Technische Universiteit Eindhoven Couche barrière de passivation en contact avec de la pérovskite pour cellules solaires
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