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WO2019036093A2 - Enrobage de grains de pérovskite avec des coquilles de silice pour améliorer la stabilité et l'efficacité de dispositifs électroniques à base de pérovskite - Google Patents

Enrobage de grains de pérovskite avec des coquilles de silice pour améliorer la stabilité et l'efficacité de dispositifs électroniques à base de pérovskite Download PDF

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WO2019036093A2
WO2019036093A2 PCT/US2018/037619 US2018037619W WO2019036093A2 WO 2019036093 A2 WO2019036093 A2 WO 2019036093A2 US 2018037619 W US2018037619 W US 2018037619W WO 2019036093 A2 WO2019036093 A2 WO 2019036093A2
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perovskite
poly
layer
silica
groups
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WO2019036093A3 (fr
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Jinsong Huang
yang BAI
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NuTech Ventures Inc
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NuTech Ventures Inc
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    • 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
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/50—Photovoltaic [PV] devices
    • 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

  • Inorganic-organic halide perovskites represent a major break-through in the development of highly efficient photovoltaic materials. For example, within only several years, polycrystalline thin-film perovskite photovoltaic (“PV”) devices have achieved power conversion efficiency (“PCE”) of 22.1%. The rapid rise in PCE, coupled with the prospect of low-cost precursors and facile synthesis, render perovskite photovoltaic devices highly competitive for commercial applications.
  • PV polycrystalline thin-film perovskite photovoltaic
  • PCE power conversion efficiency
  • the present disclosure provides systems and methods for enhancing the stability and efficiency of perovskite materials, and devices incorporating such perovskite materials. Enhancing the stability of perovskite materials advantageously increases the lifetime of any electronic devices, such as solar cells, incorporating perovskite materials as an active layer.
  • Certain embodiments provide methods for in-situ coating or wrapping perovskite grains with a thin layer silica (S1O2) shell to stabilize the perovskite.
  • S1O2 thin layer silica
  • Most inorganic matrix materials are mechanically robust and airtight.
  • silica is an attractive coating material due to its stability against environmental and chemical factors and excellent optical properties.
  • a method to wrap the perovskite grains (e.g., one or more grains per wrapping) with silica shells to protect the perovskite grains includes mixing silica precursors in perovskite precursor solution. During the formation of perovskite grains, the silica precursor is converted to silica by hydrolysis or other type of reaction.
  • the silica shell layer protects perovskite grain surfaces from defect-generation and provides a passivation function, as evidenced by the dramatically elongated charge recombination lifetime, and thus increases the efficiency of electronic devices incorporating perovskite materials.
  • Preliminary studies indicate the perovskite materials showed much better resistance to moisture-induced degradation of perovskite films after wrapping with a silicon-based coating layer. This method is useful for all perovskite ⁇ - related electronic devices, including photovoltaic devices such as solar cells.
  • a device including a perovskite layer wherein the perovskite layer includes a plurality of perovskite grains, each grain wrapped in a silica shell.
  • a device including a perovskite layer wherein the perovskite layer includes a plurality of groups of one or more perovskite grains, each of said plurality of groups wrapped in a silica shell.
  • a method of forming a perovskite layer wherein the perovskite layer includes a plurality of groups of one or more perovskite grains, each of said plurality of groups wrapped in a silica shell.
  • a method of making or forming a perovskite layer which includes mixing a perovskite solution with a silica shell precursor solution to produce a perovskite-silica precursor solution, and spin casting or drop casting the perovskite-silica precursor solution on a substrate to form a perovskite material or material layer, wherein the perovskite material or material layer includes a plurality of groups of one or more perovskite grains, each of said plurality of groups wrapped in a silica shell.
  • the silica shell precursor solution has a chemical structure of Rn-Si-(OR)4-n, where "R” is an alkyl, aryl, or organofunctional group, and "OR” is a methoxy, ethoxy, or acetoxy group.
  • a semiconductor device includes a cathode layer, an anode layer, and an active layer disposed between the cathode layer and the anode layer, where the active layer includes a perovskite layer, wherein the perovskite layer includes a plurality of groups of one or more perovskite grains, each of said plurality of groups wrapped in a silica shell.
  • the perovskite material or layer includes organometal trihalide perovskite (grains) having the formula ABX 3 , or A2BX4, wherein A is methylammonium (CH 3 H 3 + ), formamidinium (H2NCHNH 2 + ), or an alkali-metal ion, B is a metal cation, and X is a halide anion, thiocyanate (SCN " ) or a mixture thereof.
  • organometal trihalide perovskite having the formula ABX 3 , or A2BX4, wherein A is methylammonium (CH 3 H 3 + ), formamidinium (H2NCHNH 2 + ), or an alkali-metal ion, B is a metal cation, and X is a halide anion, thiocyanate (SCN " ) or a mixture thereof.
  • the perovskite layer includes perovskite (grains) having the formula MAPbI 3 , FAi-xMAxPb(Ii-xBr x ) 3 , CsPb(Ii-xBr x ) 3 , Cs y FAi-x- y MAxPb(Ii-xBr x ) 3 , RbzCs y FAi-x- y -zMA x Pb(Ii- xBr x ) 3 , or RbzCs y FAi-x- y -zMAxPbnSni-n(Ii-xBr x ) 3 where x, y, z, and n may be between 0 and 1.
  • the silica shell precursor solution has a chemical structure of Rn-Si-(OR)4-n, where "R” is an alkyl, aryl, or
  • organofunctional group and "OR” is a methoxy, ethoxy, or acetoxy group.
  • FIG. 1 shows a method of coating perovskite grains with silica shells according to an embodiment.
  • FIG. 2A shows an SEM image of a MAPbL film.
  • FIG. 2B shows an SEM image of a MAPbl3@Si02 film according to an embodiment.
  • FIG. 2C shows FTIR spectra of MAPbL film and MAPbl3@Si0 2 films according to an embodiment.
  • FIG. 2D shows an EDX element line scan profile acquired across the cross-section of a MAPbl3@Si0 2 film according to an embodiment.
  • FIG. 3 A shows the photocurrent density-voltage (J-V) characteristics of a perovskite devices (e.g., solar cells) based on conventional perovskite films and different silica-wrapped perovskite films.
  • J-V photocurrent density-voltage
  • FIG. 3B shows EQE of an optimized silica-wrapped perovskite device.
  • FIG. 3C shows Statistics of the Voc for devices with conventional and silica-wrapped perovskite films.
  • FIG. 3D shows the PCE distribution for devices with conventional and silica-wrapped perovskite films.
  • FIG. 4 A shows normalized time resolved PL decay curves of the MAPbL and MAPbl3@Si0 2 films on glass substrates.
  • FIG. 4B shows transient photovoltage decay curves of perovskite devices based on MAPbL and MAPbl3@Si0 2 films under one sun illumination.
  • FIG. 4C shows total density of states (DOS) of perovskite devices fabricated with MAPbL and MAPbI 3 @Si0 2 films.
  • FIG. 5 A shows XRD of MAPbL and MAPbI 3 @Si0 2 films after storage in air.
  • FIG. 5B shows photovoltaic performance of the typical perovskite solar cells based on conventional perovskite film and silica-wrapped perovskite film exposed to an ambient environment without encapsulation as a function of storage time; air humidity varies from 20 RH% to 70 RH%.
  • FIG. 6A shows photocurrent-voltage (J-V) characteristics of solar cells based on conventional and silica-wrapped FA/MA hybrid perovskite films.
  • FIG. 6B shows EQE of an optimized device with silica-wrapped perovskite.
  • FIG. 6C shows steady-state photocurrent and efficiency at the maximum power point
  • FIG. 7 shows photovoltaic performance of typical perovskite solar cells based on conventional and silica- wrapped FA/MA hybrid perovskite films under continuous AM 1.5 one sun illumination with encapsulation as a function of illumination time.
  • FIG. 1 illustrates a method of coating perovskite grains with silica shells according to an embodiment.
  • FIG 1 illustrates schematically a process of in-situ coating perovskite grains with silica shells and device structure of the silica-coated perovskite planar heteroj unction solar cells.
  • tetraethyl orthosilicate (TEOS) is used as a silica precursor as TEOS can be readily hydrolyzed to form S1O2 over perovskite grains when contacting with the low-content water in toluene.
  • TEOS tetraethyl orthosilicate
  • the silica-coated perovskite films may be used for fabrication of p- i-n solar cells, which have a general structure of transparent conductive oxide (TCO)
  • TEOS is used as a silica precursor included into the perovskite precursor solution according to an embodiment.
  • the low content moisture or OH- group containing organic molecules in the film environment drives the hydrolysis of TEOS, which builds silica shells around perovskite grains.
  • the typical reaction and coating process is illustrated in FIG. 1.
  • a perovskite layer is formed on a substrate.
  • a perovskite solution with a silica shell precursor solution to produce a perovskite-silica precursor solution and in a second step, the perovskite-silica precursor solution is formed, e.g., via spin casting or drop casting or other deposition method, on the substrate to form a perovskite layer, wherein the perovskite layer includes a plurality of groups of one or more perovskite grains, each of said plurality of groups wrapped in a silica shell.
  • the substrate may include, for example, glass or ITO/glass or other rigid or semi rigid material.
  • the substrate may also include other intermediary layers as desired, for example a hole transport material, electrode materials, etc.
  • a hole transport material (HTM) layer e.g., a layer of poly(bis(4-phenyl)(2,4,6-trimethylphenyl)amine) (PTAA) film
  • HTM hole transport material
  • PTAA poly(bis(4-phenyl)(2,4,6-trimethylphenyl)amine)
  • a substrate e.g., ITO/glass substrate or TCO.
  • the HTM may be deposited by spin- coating 0.2 wt% PTAA in toluene at 4000 r.p.m for 35 s.
  • the as-prepared film may then be thermally annealed, e.g., at 100 °C for 10 min.
  • MAPbb films may be fabricated by one-step spin coating with an anti-solvent extraction approach, for example as described in Chen, B , et al ., Efficient Semitransparent Perovskite Solar Cells for 23.0%-Efficiency Perovskite/Silicon Four- Terminal Tandem Cells. Advanced Energy Materials, 2016.
  • the perovskite precursor solution may be prepared by dissolving Phh and MAI in DMF and DM SO (e.g., 461 rng Pbli and 159 mg MAI in 700 ⁇ , DMF and 78 ⁇ , DMSO).
  • a silica shell precursor is blended into or mixed with the perovskite precursor.
  • TEOS was used as the silica shell precursor and was blended into the perovskite precursor solution.
  • different ratios of TEOS were introduced into the perovskite precursor solutions.
  • Tl, T2, and T3 represent the devices fabricated using 3 vol%, 5 vol%, and 10 vol% TEOS modified perovskite precursor solution, respectively.
  • the MAPbls precursor solution (mixed with silica shell precursor) was deposited onto a substrate (e.g., spun onto PTAA at 2000 r.p.m for 2 s and 4000 r.p.m for 20 s).
  • the sample was drop-casted with toluene (e.g., 120 ⁇ toluene at 8 s of the second-step spin- coating). Subsequently, the sample was annealed (e.g., at 65 °C for 10 min and 100 °C for 10 min).
  • the electron-transporter layer e.g., PCBM
  • PCBM electron-transporter layer
  • the electron-transporter layer is deposited on or coated (e.g., by spinning 2 wt% PCBM in dichlorobenzene at 6000 r.p.m for 35 s) on the perovskite layer and then annealed (e.g., at 100 °C for 30 min). Thereafter, the electrode layers are formed. For example, 20 nm C60 and 8 nm bathocuproine (BCP) were sequentially deposited by thermal evaporation, and 80 nm Cu was deposited by thermal evaporation as the device cathode.
  • BCP bathocu
  • Perovskite films on ITO substrates with and without S1O2 wrapping layers were prepared by following the same procedure as that for device fabrication above and the collected powder was subjected to FTIR analysis. As shown in FIG. 2C, the appearance of a new and wide vibration peak between 1, 101 and 1,035 cm "1 confirms the formation of Si-O-Si bonds. To investigate and further confirm the formation of S1O2 wrapping layer, bulk
  • compositional analysis for the S1O2 wrapped perovskite film was performed with energy- dispersive X-ray spectroscopy (EDX).
  • EDX energy- dispersive X-ray spectroscopy
  • FIG. 2D shows the EDX element line scan profile acquired across the cross-section of the film; the majority of S1O2 was distributed at the GBs, indicating the formation of a S1O2 wrapping layer.
  • FIG. 3A shows the photocurrent density-voltage (J-V) characteristics of perovskite devices (e.g., solar cells) based on conventional perovskite films and different silica-wrapped perovskite films.
  • a typical perovskite device had a short-circuit current density (Jsc) of 22.3 mA cm “2 , an open-circuit voltage (Foe) of 1.09 V, and a fill factor (FF) of 76.5% yielding a moderate PCE of 18.6%, which is consistent with previous reported work.
  • Jsc short-circuit current density
  • Moe open-circuit voltage
  • FF fill factor
  • the device employing silica-wrapped perovskite delivered an efficiency of 19.3%.
  • the optimized performance was achieved exhibiting a Jsc of 22.7 mA cm “2 , a Voc of 1.15 V, and a of 80.9%, yielding a PCE ⁇ 2 ⁇ ⁇ %.
  • the integrated Jsc from external quantum efficiency (EQE) spectrum shown in FIG. 3B reached 22.3 mA cm "2 , which is in good agreement with that from J- J 7 measurement. Further increasing the ratio of TEOS to 10 vol% deteriorated the device performance.
  • the photovoltaic parameters of these perovskite devices are summarized in Table 1.
  • the statistics of Voc and PCE distributions shown in FIG. 3C and FIG. 3D demonstrate the reliability and repeatability of the Voc and PCE enhancement obtained by employing SiC -wrapped perovskite.
  • the charge carrier transfer and photo-generated charge recombination lifetime were characterized by time-resolved photoluminescence (TRPL) decay and transient photovoltage (TPV) decay.
  • TRPL time-resolved photoluminescence
  • TPV transient photovoltage
  • FIG. 4A the TRPL decay of the MAPbl3@Si02 film is much slower than that of bare MAPbb film, indicating slower carrier recombination in the silica-wrapped perovskite films.
  • a charge recombination lifetime of 0.8 was deduced from TPV decay curves measured under one sun illumination for the
  • MAPbl3@Si02 based device which was substantially longer than that (0.4 ⁇ ) of the device with pristine, bare MAPbb, as illustrated in FIG. 4C.
  • the longer charge recombination lifetime indicates the suppressed charge recombination at the film surface and/or grain boundaries, which was attributed to the well passivation of the S1O2 layer.
  • the passivation effect of S1O2 was further verified by measuring the trap density of the devices with and without S1O2 wrapping.
  • the variation of charge trap density in the MAPbl3@Si02-based device was analyzed using thermal admittance spectroscopy (TAS) measurements. As shown in FIG.
  • TAS thermal admittance spectroscopy
  • a perovskite material of the form FAi-xMAxPb(Ii-xBr x )3 may be used.
  • An optimized device with FAo.85MAo.i5Pb(Io.85Bro.i5)3@Si0 2 delivered an efficiency of 21.5% shown in FIG.
  • FIG. 6A The integrated Jsc from external quantum efficiency ⁇ /: ⁇ ⁇ '. ) spectrum shown in FIG, 6B reached 22.9 mA cm "2 , which is in good agreement with that from J- V measurement.
  • the steady-state photocurrent and effici ency measured at the maximum power point (1 .00 V) are presented in FIG. 6C, which confirms the devi ce performance parameters (Table 2) extracted from the J-V curve and verifies the absence of photocurrent hysteresis in these devices.
  • MAPbl3@Si0 2 device The devices were kept at a temperature of 80 °C for accelerated degradation study. As shown in the FIG. 7, all devices exhibited a fast degradation over the first 100 hours (h), with the MAPbl3@Si02 cell degrading to below 7% within 400 h. In contrast, the
  • FAo.85MAo.i5Pb(Io.85Bro.i5)3@Si02 cell only degraded by a few percent absolute efficiency over the first 100 h and then proceed to degrade at. a much slower linear rate.
  • the silica shell coated on the perovskite grains should be within about 1-10 nm in thickness so as to not disadvantageously impact the charge transport property of the perovskite.
  • the general chemical structure of the silica precursors is Rn- Si-(OR)4-n, where "R” is an alkyl, aryl, or organofunctional group, and "OR” is a methoxy, ethoxy, or acetoxy group.
  • Example silica shell precursors include tetraethoxysilane (TEOS), tetramethoxysilane (TMOS), Tetrapropyl orthosilicate , organoalkoxysilanes, 3- (trimethoxysilyl)propylmethacrylate (TMSPMA), 3-glycidoxypropyltrimethoxysilane
  • GLYMO methyltrimethoxysilane
  • MTMOS methyltrimethoxysilane
  • MTMOS methyltrimethoxysilane
  • 3-Glycidyloxypropyl)trimethoxysilane 3- Mercaptopropy)trimethoxysilane
  • 3-Glycidyloxypropyl)trimethoxysilane N-[3- (Trimethoxysilyl)propyl]ethylenediamine, 3-Aminopropyl(diethoxy)methylsilane, [3-(2- Aminoethylamino)propyl]trimethoxysilane, 3-(Trimethoxysilyl)propyl methacrylate,
  • Triacetoxy(methyl)silane (3-Aminopropyl)tris(trimethylsiloxy)silane, Triacetoxy(vinyl)silane, Tris(2-methoxyethoxy)(vinyl)silane, Silicon tetraacetate, Mpeg5K-Silane, Triethoxy(4- methoxyphenyl)silane, Cyanom ethyl [3-(trimethoxysilyl)propyl] trithiocarbonate, and
  • a first carrier transport layer (e.g., ETM layer) is disposed between the active layer (e.g., perovskite@silica layer) and the cathode
  • a second carrier transport layer e.g., HTM layer
  • the first carrier transport layer having a higher electron conductivity than the second carrier transport layer
  • the second carrier transport layer having a higher hole conductivity than the first carrier transport layer.
  • the first carrier transport layer comprises at least one of C 6 o, a fullerene, a fullerene-derivative, LiF, CsF, L1C0O2, Cs2cCb, TiOx, T1O2 nanorods (NRs), ZnO, ZnO nanorods (NRs), ZnO nanoparticles (NPs), ZnO, AI2O3, CaO, bathocuproine (BCP), copper phthalocyanine (CuPc), pentacene, pyronin B, pentadecafluorooctyl phenyl-C60-butyrate (F- PCBM), C60, C60/UF, ZnO Rs/PCBM, ZnO/cross-linked fullerene derivative (C-PCBSD), single walled carbon nanotubes (SWCNT), graphene, poly(ethylene glycol) (PEG),
  • PEI Polyethylenimine
  • PDMS-b-PMMA poly(dimethylsiloxaneblock-methyl methacrylate)
  • PF-EP polar polyfluorene
  • PFN polyfluorene bearing lateral amino groups
  • WPF-oxy-F polyfluorene bearing quaternary ammonium groups in the side chains
  • WPF-6-oxy-F polyfluorene bearing quaternary ammonium groups in the side chains
  • fluorene alternating and random copolymer bearing cationic groups in the alkyl side chains PFNBr-DBTI5
  • fluorene alternating and random copolymer bearing cationic groups in the alkyl side chains PFP Br
  • PEO poly(ethylene oxide)
  • the second carrier transport layer comprises at least one poly(3,4-ethylenedioxithiophene) (PEDOT) doped with poly(styrene sulfonicacid) (PSS), 4,4'bis[(ptrichlorosilylpropylphenyl)phenylamino]biphenyl (TPD-Si2), poly(3-hexyl-2,5- thienylene vinylene) (P3HTV) and C60, copper phthalocyanine (CuPc), poly[3,4- (lhydroxymethyl) ethyl enedioxythiophene] (PHEDOT), n-dodecylbenzenesulfonic
  • PEDOT poly(3,4-ethylenedioxithiophene)
  • PSS poly(styrene sulfonicacid)
  • TPD-Si2 4,4'bis[(ptrichlorosilylpropylphenyl)phenylamino]biphenyl
  • a-PANIN acid/hydrochloric acid-doped poly(aniline) nanotubes
  • PS SA-g-PANI poly(styrenesulfonic acid)- graft-poly (aniline)
  • PFT poly[(9,9-dioctylfluorene)-co-N-(4-(l- methylpropyl)phenyl)diphenylamine]
  • PFT poly[(9,9-dioctylfluorene)-co-N-(4-(l- methylpropyl)phenyl)diphenylamine]
  • PFT 4,4'bis[(p-trichlorosilylpropylphenyl)phenylamino] biphenyl
  • TSPP 4,4'bis[(p-trichlorosilylpropylphenyl)phenylamino] biphenyl
  • TSPT 5,5'-bis[(p-trichlorosilylpropyl
  • the anode layer includes at least one of indium tin oxide (ITO), fluorine-doped tin oxide (FTO), aluminum-doped zinc oxide (AZO), antimony -tin mixed oxide (ATO), a conductive polymer, a network of metal nanowire, a network of carbon nanowire, nanotube, nanosheet, nanorod, carbon nanotube, silver nanowire, or graphene.
  • ITO indium tin oxide
  • FTO fluorine-doped tin oxide
  • AZO aluminum-doped zinc oxide
  • ATO antimony -tin mixed oxide
  • a conductive polymer a network of metal nanowire, a network of carbon nanowire, nanotube, nanosheet, nanorod, carbon nanotube, silver nanowire, or graphene.
  • the cathode layer includes at least one of copper, aluminum, calcium, magnesium, lithium, sodium, potassium, strontium, cesium, barium, iron, cobalt, nickel, silver, zinc, tin, samarium, ytterbium, chromium, gold, graphene, an alkali metal fluoride, an alkaline-earth metal fluoride, an alkali metal chloride, an alkaline-earth metal chloride, an alkali metal oxide, an alkaline-earth metal oxide, a metal carbonate, a metal acetate, or a combination of at least two of the above materials.

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Abstract

Cette invention concerne des systèmes et des procédés destinés à améliorer la stabilité et l'efficacité de matériaux à base pérovskite, et des dispositifs incorporant de tels matériaux à base de pérovskite. Un procédé de fabrication d'une couche de pérovskite comprend le mélange d'une solution de pérovskite avec une solution de précurseur de coquille de silice pour produire une solution de précurseur de pérovskite-silice, et le dépôt par centrifugation ou le dépôt par goutte de la solution de précurseur de pérovskite-silice sur un substrat pour former un matériau ou une couche de matériau de pérovskite, le matériau ou la couche de matériau de pérovskite comprenant une pluralité de groupes d'un ou de plusieurs grains de pérovskite, chacun de ladite pluralité de groupes étant enveloppé dans une coquille de silice. La solution de précurseur de coquille de silice peut avoir une structure chimique telle que Rn-Si-(OR)4-n, où "R" est un groupe alkyle, aryle ou organofonctionnel, et "OR" est un groupe méthoxy, éthoxy ou acétoxy.
PCT/US2018/037619 2017-06-14 2018-06-14 Enrobage de grains de pérovskite avec des coquilles de silice pour améliorer la stabilité et l'efficacité de dispositifs électroniques à base de pérovskite Ceased WO2019036093A2 (fr)

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