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  • 1.
    Etman, Ahmed S.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Aqueous Exfoliation of Transition Metal Oxides for Energy Storage and Photocatalysis Applications: Vanadium Oxide and Molybdenum Oxide Nanosheets2019Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Two-dimensional (2D) transition metal oxides (TMOs) are a category of materials which have unique physical and chemical properties compared to their bulk counterparts. However, the synthesis of 2D TMOs commonly includes the use of environmental threats such as organic solvents. In this thesis, we developed environmentally friendly strategies to fabricate TMO nanosheets from the commercially available bulk oxides. In particular, hydrated vanadium pentoxide (V2O5∙nH2O) nanosheets and oxygen deficient molybdenum trioxide (MoO3-x) nanosheets were prepared.  The V2O5∙nH2O nanosheets were drop-cast onto multi-walled carbon nanotube (MWCNT) paper and applied as a free-standing electrode (FSE) for a lithium battery. The accessible capacity of the FSE was dependent on the electrode thickness; the thickest electrode delivered the lowest accessible capacity.  Alternatively, a composite material of V2O5∙nH2O nanosheets with 10% MWCNT (VOx-CNT composite) was prepared and two types of electrodes, FSE and conventionally cast electrode (CCE), were employed as cathode materials for lithium batteries. A detailed comparison between these electrodes was presented. In addition, the VOx-CNT composite was applied as a negative electrode for a sodium-ion battery and showed a reversible capacity of about 140 mAh g-1. On the other hand, the MoO3-x nanosheets were employed as binder-free electrodes for supercapacitor application in an acidified Na2SO4 electrolyte. Furthermore, the MoO3-x nanosheets were used as photocatalysts for organic dye degradation. The simple eco-friendly synthesis methods coupled with the potential application of the TMO nanosheets reflect the significance of this thesis in both the synthesis and the energy-related applications of 2D materials.

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  • 2.
    Etman, Ahmed S.
    et al.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Alexandria University, Egypt.
    Abdelhamid, Hani Nasser
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Yuan, Youyou
    Wang, Ligang
    Zou, Xiaodong
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    Facile Water-Based Strategy for Synthesizing MoO3-x Nanosheets: Efficient Visible Light Photocatalysts for Dye Degradation2018In: ACS Omega, E-ISSN 2470-1343, Vol. 3, no 2, p. 2193-2201Article in journal (Refereed)
    Abstract [en]

    Nanostructured molybdenum oxides are promising materials for energy storage, catalysis, and electronic-based applications. Herein, we report the synthesis of MoO3-x nanosheets (x stands for oxygen vacancy) via an environmentally friendly liquid exfoliation approach. The process involves the reflux of the bulk alpha-MoO3 precursor in water at 80 degrees C for 7 days. Electron microscopy and atomic force microscopy show that the MoO3-x nanosheets are a few nanometer thick. MoO3-x nanosheets exhibit near infrared plasmonic property that can be enhanced by visible light irradiation for a short time (10 min). Photocatalytic activity of MoO3-x nanosheets for organic dye decolorization is examined using two different dyes (rhodamine B and methylene blue). Under visible light irradiation, MoO3-x nanosheets make a rapid decolorization for the dye molecules in less than 10 min. The simple synthesis procedure of MoO3-x nanosheets combined with their remarkable photochemical properties reflect the high potential for using the nanosheets in a variety of applications.

  • 3.
    Etman, Ahmed S.
    et al.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Alexandria University, Egypt.
    Asfaw, Habtom D.
    Yuan, Ning
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Swedish University of Agricultural Sciences, Sweden.
    Li, Jian
    Zhou, Zhengyang
    Peng, Fei
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Persson, Ingmar
    Zou, Xiaodong
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Gustafsson, Torbjörn
    Edström, Kristina
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    A one-step water based strategy for synthesizing hydrated vanadium pentoxide nanosheets from VO2(B) as free-standing electrodes for lithium battery applications2016In: Journal of Materials Chemistry A, ISSN 2050-7488, Vol. 4, no 46, p. 17988-18001Article in journal (Refereed)
    Abstract [en]

    The synthesis of two dimensional (2D) materials from transition metal oxides, chalcogenides, and carbides mostly involve multiple exfoliation steps in which hazardous solvents and reagents are used. In this study, hydrated vanadium pentoxide (V2O5 center dot nH(2)O) nanosheets with a thickness of a few nanometers were prepared via a facile environmentally friendly water based exfoliation technique. The exfoliation process involved refluxing the precursor, vanadium dioxide (VO2(B)), in water for a few days at 60 degrees C. The proposed exfoliation mechanism is based on the intercalation/insertion of water molecules into the VO2(B) crystals and the subsequent cleavage of the covalent bonds holding the layers of VO2(B) together. The thermal and chemical analyses showed that the approximate chemical composition of the nanosheets is H0.4V2O5 center dot 0.55H(2)O, and the percentage of V-V content to that of V-IV in the nanosheets is about 80(3)% to 20(3)%. The exfoliated aqueous suspension of the V2O5 center dot 0.55H(2)O nanosheets was successfully deposited onto multi-walled carbon nanotube (MW-CNT) paper to form free-standing electrodes with a thickness of the V2O5 center dot 0.55H(2)O layer ranging between 45 and 4 mu m. A series of electrochemical tests were conducted on the electrodes to determine the cyclability and rate capability of lithium insertion into V2O5 center dot 0.55H(2)O nanosheets. The electrodes with the thinnest active material coating (similar to 4 mu m) delivered gravimetric capacities of up to 480 and 280 mA h g(-1) when cycled at current densities of 10 and 200 mA g(-1), respectively.

  • 4.
    Etman, Ahmed S.
    et al.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Alexandria University, Egypt.
    Inge, A. Ken
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Xu, Jiaru
    Younesi, Reza
    Edström, Kristina
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    A Water Based Synthesis of Ultrathin Hydrated Vanadium Pentoxide Nanosheets for Lithium Battery Application: Free Standing Electrodes or Conventionally Casted Electrodes?2017In: Electrochimica Acta, ISSN 0013-4686, E-ISSN 1873-3859, Vol. 252, p. 254-260Article in journal (Refereed)
    Abstract [en]

    Ultrathin hydrated vanadium pentoxide (V2O5 center dot nH(2)O) nanosheets are fabricated via a water based exfoliation technique. The exfoliation process involves reflux of the precursor, 1:4 mixture of VO2 and V2O5, in water at 80 degrees C for 24 h. Operando and ex situ X-ray diffraction (XRD) studies are conducted to follow the structural changes during the exfoliation process. The chemical and thermal analyses suggest that the molecular formula of the nanosheet is (H0.2V1.8V0.2O5)-V-V-O-IV center dot 0.5H(2)O. The V2O5 center dot nH(2)O nanosheets are mixed with 10% of multi-walled carbon nanotube (MW-CNT) to form a composite material assigned as (VOx-CNT). Free standing electrodes (FSE) and conventionally casted electrodes (CCE) of VOx-CNT are fabricated and then tested as a positive electrode material for lithium batteries. The FSE shows reversible capacities of 300 and 97 mAhg(-1) at current densities of 10 and 200 mAhg(-1), respectively. This is better than earlier reports for free-standing electrodes. The CCE delivers discharge capacities of 175 and 93 mAhg(-1) at current densities of 10 and 200 mAhg(-1), respectively.

  • 5.
    Etman, Ahmed S.
    et al.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Alexandria University, Egypt.
    Pell, Andrew J.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Svedlindh, Peter
    Hedin, Niklas
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Zou, Xiaodong
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    Bernin, Diana
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Chalmers University of Technology, Sweden.
    Insights into the Exfoliation Process of V2O5 center dot nH(2)O Nanosheet Formation Using Real-Time V-51 NMR2019In: Acs Omega, E-ISSN 2470-1343, Vol. 4, no 6, p. 10899-10905Article in journal (Refereed)
    Abstract [en]

    Nanostructured hydrated vanadium oxides (V2O5 center dot nH(2)O) are actively being researched for applications in energy storage, catalysis, and gas sensors. Recently, a one-step exfoliation technique for fabricating V2O5 center dot nH(2)O nano-sheets in aqueous media was reported; however, the underlying mechanism of exfoliation has been challenging to study. Herein, we followed the synthesis of V2O5 center dot nH(2)O nanosheets from the V2O5 and VO2 precursors in real using solution- and solid-state V-51 NMR. Solution-state V-51 NMR showed that the aqueous solution contained mostly the decavanadate anion [H2V10O28](4-) and the hydrated dioxova-nadate cation [VO2 center dot 4H(2)O](+), and during the exfoliation process, decavanadate was formed, while the amount of [VO2 center dot 4H(2)O](+) remained constant. The conversion of the solid precursor V2O5, which was monitored with solid-state V-51 NMR, was initiated when VO2 was in its monoclinic forms. The dried V2O5 center dot nH(2)O nanosheets were weakly paramagnetic because of a minor content of isolated V4+. Its solid-state V-51 signal was less than 20% of V2O5 and arose from diamagnetic V4+ or V5+.This study demonstrates the use of real-time NMR techniques as a powerful analysis tool for the exfoliation of bulk materials into nanosheets. A deeper understanding of this process will pave the way to tailor these important materials.

  • 6.
    Etman, Ahmed S.
    et al.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Alexandria University, Egypt.
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    Younesi, Reza
    V2O5·nH2O nanosheets and multi-walled carbon nanotube composite as a negative electrode for sodium-ion batteries2019In: Journal of Energy Chemistry, ISSN 2095-4956, Vol. 30, p. 145-151Article in journal (Refereed)
    Abstract [en]

    Two dimensional (2D) transition metal oxides and chalcogenides demonstrate a promising performance in sodium-ion batteries (SIBs) application. In this study, we investigated the use of a composite of freeze dried V2O5·nH2O nanosheets and multi-walled carbon nanotube (MWCNT) as a negative electrode material for SIBs. Cyclic voltammetry (CV) results indicated that a reversible sodium-ion insertion/deinsertion into the composite electrode can be obtained in the potential window of 0.1–2.5 V vs. Na+/Na. The composite electrodes delivered sodium storage capacities of 140 and 45 mAh g−1 under applied current densities of 20 and 100 mA g−1, respectively. The pause test during constant current measurement showed a raise in the open circuit potential (OCP) of about 0.46 V, and a charge capacity loss of ∼10%. These values are comparable with those reported for hard carbon electrodes. For comparison, electrodes of freeze dried V2O5·nH2O nanosheets were prepared and tested for SIBs application. The results showed that the MWCNT plays a significant role in the electrochemical performance of the composite material.

  • 7.
    Etman, Ahmed S.
    et al.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Alexandria University, Egypt.
    Wang, Ligang
    Edström, Kristina
    Nyholm, Leif
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    Molybdenum Oxide Nanosheets with Tunable Plasmonic Resonance: Aqueous Exfoliation Synthesis and Charge Storage Applications2019In: Advanced Functional Materials, ISSN 1616-301X, E-ISSN 1616-3028, Vol. 29, no 4, article id 1806699Article in journal (Refereed)
    Abstract [en]

    Herein, a simple aqueous‐exfoliation strategy is introduced for the fabrication of a series of MoO3−x nanosheets (where x stands for oxygen vacancies) using two commercial molybdenum oxide precursors, MoO2 and MoO3. The nanosheets offer a localized surface plasmon resonance (LSPR) effect which is dependent on the structure and local environment of the nanosheets. The LSPR can be efficiently tuned by changing the weight ratio between the molybdenum oxide precursor(s) and/or by solar light irradiation using a low‐energy UV lamp (36 W). For the pristine MoO3−x nanosheets, the highest LSPR signal is obtained for nanosheets prepared using 80% MoO2. On the contrary, after solar light irradiation, the nanosheets prepared using pure MoO3 offer the highest LSPR response. The nanosheets also show an outstanding rate capability when used as binder‐free supercapacitor electrodes in an acidified Na2SO4 electrolyte. The electrodes exhibit discharge capacities of 110 and 75 C g−1 at a scan rate of 20 and 1000 mV s−1, respectively. The MoO3−x nanosheets can likewise be used as a negative electrode material for lithium‐ion batteries. The efficient eco‐friendly synthesis and the ability to tune the photochemical and electrochemical properties of the nanosheets make this approach interesting to many energy‐related research fields.

  • 8. Huang, Jing
    et al.
    Gatty, Melina Gilbert
    Xu, Bo
    Pati, Palas Baran
    Etman, Ahmed S.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Tian, Lei
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Hammarström, Leif
    Tian, Haining
    Covalently linking CuInS2 quantum dots with a Re catalyst by click reaction for photocatalytic CO2 reduction2018In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 47, no 31, p. 10775-10783Article in journal (Refereed)
    Abstract [en]

    Covalently linking photosensitizers and catalysts in an inorganic-organic hybrid photocatalytic system is beneficial for efficient electron transfer between these components. However, general and straightforward methods to covalently attach molecular catalysts on the surface of inorganic semiconductors are rare. In this work, a classic rhenium bipyridine complex (Re catalyst) has been successfully covalently linked to the low toxicity CuInS2 quantum dots (QDs) by click reaction for photocatalytic CO2 reduction. Covalent bonding between the CuInS2 QDs and the Re catalyst in the QD-Re hybrid system is confirmed by UV-visible absorption spectroscopy, Fourier-transform infrared spectroscopy and energy-dispersive X-ray measurements. Time-correlated single photon counting and ultrafast time-resolved infrared spectroscopy provide evidence for rapid photo-induced electron transfer from the QDs to the Re catalyst. Upon photo-excitation of the QDs, the singly reduced Re catalyst is formed within 300 fs. Notably, the amount of reduced Re in the linked hybrid system is more than that in a sample where the QDs and the Re catalyst are simply mixed, suggesting that the covalent linkage between the CuInS2 QDs and the Re catalyst indeed facilitates electron transfer from the QDs to the Re catalyst. Such an ultrafast electron transfer in the covalently linked CuInS2 QD-Re hybrid system leads to enhanced photocatalytic activity for CO2 reduction, as compared to the conventional mixture of the QDs and the Re catalyst.

  • 9. Huang, Jing
    et al.
    Xu, Bo
    Tian, Lei
    Pati, Palas Baran
    Etman, Ahmed S.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Hammarstrom, Leif
    Tian, Haining
    A heavy metal-free CuInS2 quantum dot sensitized NiO photocathode with a Re molecular catalyst for photoelectrochemical CO2 reduction2019In: Chemical Communications, ISSN 1359-7345, E-ISSN 1364-548X, Vol. 55, no 55, p. 7918-7921Article in journal (Refereed)
    Abstract [en]

    Heavy metal-free CuInS2 quantum dots (QDs) were employed as a photosensitizer on a NiO photocathode to drive an immobilized molecular Re catalyst for photoelectrochemical CO2 reduction for the first time. A photocurrent of 25 mu A cm(-2) at -0.87 V vs. NHE was obtained, providing a faradaic efficiency of 32% for CO production.

  • 10. Lin, Jia
    et al.
    Chen, Hong
    Gao, Yang
    Cai, Yao
    Jin, Jianbo
    Etman, Ahmed S.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Kang, Joohoon
    Lei, Teng
    Lin, Zhenni
    Folgueras, Maria C.
    Quan, Li Na
    Kong, Qiao
    Sherburne, Matthew
    Asta, Mark
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Toney, Michael F.
    Wu, Junqiao
    Yang, Peidong
    Pressure-induced semiconductor-to-metal phase transition of a charge-ordered indium halide perovskite2019In: Proceedings of the National Academy of Sciences of the United States of America, ISSN 0027-8424, E-ISSN 1091-6490, Vol. 116, no 47, p. 23404-23409Article in journal (Refereed)
    Abstract [en]

    Phase transitions in halide perovskites triggered by external stimuli generate significantly different material properties, providing a great opportunity for broad applications. Here, we demonstrate an In-based, charge-ordered (In+/In3+) inorganic halide perovskite with the composition of Cs2In(I)In(III)Cl-6 in which a pressure-driven semiconductor-to-metal phase transition exists. The single crystals, synthesized via a solid-state reaction method, crystallize in a distorted perovskite structure with space group I4/m with a = 17.2604(12) angstrom, c = 11.0113(16) angstrom if both the strong reflections and superstructures are considered. The supercell was further confirmed by rotation electron diffraction measurement. The pressure-induced semiconductor-to-metal phase transition was demonstrated by high-pressure Raman and absorbance spectroscopies and was consistent with theoretical modeling. This type of charge-ordered inorganic halide perovskite with a pressure-induced semiconductor-to-metal phase transition may inspire a range of potential applications.

  • 11.
    Luo, Yi
    et al.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Shanghai Research Institute of Petrochemical Technology, China; East China University of Science and Technology, China.
    Smeets, Stef
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Peng, Fei
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Etman, Ahmed S.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Wang, Zhendong
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    Yang, Weimin
    Synthesis and Structure Determination of Large-Pore Zeolite SCM-142017In: Chemistry - A European Journal, ISSN 0947-6539, E-ISSN 1521-3765, Vol. 23, no 66, p. 16829-16834Article in journal (Refereed)
    Abstract [en]

    SCM-14 (Sinopec Composite Material No. 14), a new stable germanosilicate zeolite with a 12 x 8 x 8-ring channel system, was synthesized using commercially available 4-pyrrolidinopyridine as organic structure-directing agents (OSDAs) in fluoride medium. The framework structure of SCM-14 was determined using rotation electron diffraction (RED), and refined against synchrotron X-ray powder diffraction (SXPD) data for both as-made and calcined materials. The framework structure of SCM-14 is closely related to that of three known zeolites: mordenite (MOR), GUS-1 (GON), and IM-16 (UOS). SCM-14 has the same projection as that of mordenite and GUS-1 when viewed along the 12-ring channels, and possesses two more straight 8-ring channels running perpendicular to the 12-ring channels. The structure of SCM-14 can be constructed by either the same layers as that of GUS-1 or the same columns as that of IM-16. Based on their structural relationship, three topologically reasonable hypothetical zeolites were predicted.

  • 12. Ma, Tianqiong
    et al.
    Li, Jian
    Niu, Jing
    Zhang, Lei
    Etman, Ahmed S.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Lin, Cong
    Shi, Dier
    Chen, Pohua
    Li, Li-Hua
    Du, Xin
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    Wang, Wei
    Observation of Interpenetration Isomerism in Covalent Organic Frameworks2018In: Journal of the American Chemical Society, ISSN 0002-7863, E-ISSN 1520-5126, Vol. 140, no 22, p. 6763-6766Article in journal (Refereed)
    Abstract [en]

    We report herein the first example of interpenetration isomerism in covalent organic frameworks (COFs). As a well-known three-dimensional (3D) COF, COF-300 was synthesized and characterized by the Yaghi group in 2009 as a 5-fold interpenetrated diamond structure (dia-cS topology). We found that adding an aging process prior to the reported synthetic procedure afforded the formation of an interpenetration isomer, dia-c7 COF-300. The 7-fold interpenetrated diamond structure of this new isomer was identified by powder Xray diffraction and rotation electron diffraction analyses. Furthermore, we proposed a universal formula to accurately determine the number of interpenetration degrees of dia-based COFs from only the unit cell parameters and the length of the organic linker. This work not only provides a novel example to the category of interpenetration isomerism but also provides new insights for the further development of 3D COFs.

  • 13. Xu, Bo
    et al.
    Tian, Lei
    Etman, Ahmed S.
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
    Sun, Junliang
    Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, China.
    Tian, Haining
    Solution-processed nanoporous NiO-dye-ZnO photocathodes: Toward efficient and stable solid-state p-type dye-sensitized solar cells and dye-sensitized photoelectrosynthesis cells2019In: Nano Energy, ISSN 2211-2855, E-ISSN 2211-3282, Vol. 55, p. 59-64Article in journal (Refereed)
    Abstract [en]

    A solution-processed NiO-dye-ZnO photocathode was developed for applications in both solid-state p-type dye-sensitized solar cells (p-ssDSCs) and p-type dye-sensitized photoelectrosynthesis cells (p-DSPECs). In p-ssDSCs, the solar cell using ZnO as electron transport material showed a short circuit current, up to 680 mu A cm(-2), which is 60-fold larger than that previously reported device using TiO2 as electron transport material with similar architecture. In the p-DSPECs, a remarkable photocurrent of 100 mu A cm(-2) was achieved in a pH = 5.0 acetate buffer solution under a bias potential at 0.05 V vs RHE with platinum as the proton reduction catalyst. A Faradaic efficiency approaching 100% for the H-2 evolution reaction was obtained after photoelectrolysis for 9 h. Importantly, the solution-processed NiO-dye-ZnO photocathode exhibited excellent long-term stability in both p-ssDSCs and p-DSPECs. To the best of our knowledge, this is the first study where a solution-processable, nanoporous NiO-dye-ZnO photocathode is used for both p-ssDSCs and p-DSPECs having both excellent device performance and stability.

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