Supported quantum clusters of silver as enhanced catalysts for reduction

Quantum clusters (QCs) of silver such as Ag₇(H₂MSA)₇, Ag₈(H₂MSA)₈ (H₂MSA, mercaptosuccinic acid) were synthesized by the interfacial etching of Ag nanoparticle precursors and were loaded on metal oxide supports to prepare active catalysts. The supported clusters were characterized using high resolution transmission electron microscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, and laser desorption ionization mass spectrometry. We used the conversion of nitro group to amino group as a model reaction to study the catalytic reduction activity of the QCs. Various aromatic nitro compounds, namely, 3-nitrophenol (3-np), 4-nitrophenol (4-np), 3-nitroaniline (3-na), and 4-nitroaniline (4-na) were used as substrates. Products were confirmed using UV-visible spectroscopy and electrospray ionization mass spectrometry. The supported QCs remained active and were reused several times after separation. The rate constant suggested that the reaction followed pseudo-first-order kinetics. The turn-over frequency was 1.87 s^-1 per cluster for the reduction of 4-np at 35°C. Among the substrates investigated, the kinetics followed the order, SiO₂ > TiO₂ > Fe₂O₃ > Al₂O₃.     

Polyaniline grafted chitosan/GO-CNT/Fe3O4 nanocomposite as a superior electrode material for supercapacitor application

Developing appropriate stable electroactive electrode materials for supercapacitor application is the challenging issue, which attracts enormous attention in recent decades. In this regard, Fe₃O₄ nanoparticles are firstly synthesized on chitosan/graphene oxide-multiwall carbon nanotubes (CS/GM/Fe₃O₄). Then, polyaniline (PANI) is grafted on it via in situ chemical polymerization and named as CS/GM/Fe₃O₄/PANI. The as-prepared nanocomposites are characterized by Field emission scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and energy dispersive X-ray spectroscopy. The capacitive properties of the electrodes are investigated in a three electrode configuration in 0.5 M Na₂SO₄ electrolyte by various electrochemical techniques. The specific capacitance of CS/GM/Fe₃O₄/PANI electrode is 1513.4 Fg⁻¹ at 4 Ag⁻¹ which is 1.9 times higher than that of CS/GM/Fe₃O₄ (800 Fg⁻¹). Meanwhile, the electrodes exhibit appropriate cycle life along with 99.8% and 93.95% specific capacitance at 100 Ag⁻¹ for chitosan/GO-CNT/Fe₃O₄ and polyaniline grafted chitosan/GO-CNT/Fe₃O₄, respectively.     

Nanocomposite Fe2O3-Se as a new lithium storage material

The electrochemical properties of nanocomposite Fe₂O₃-Se thin film prepared by pulsed laser deposition (PLD) method have been investigated by cyclic voltammetry and charge/discharge measurements. A large reversible capacity of nanocomposite Fe₂O₃-Se thin film was found to be around 650 mAh g⁻¹. A new couple of reduction and oxidation peaks at 1.4 and 1.8 V were observed from cyclic voltammogram for the first time. Our data demonstrated that nanocomposite Fe₂O₃-Se exhibit larger capacity and better cycle performance than pure Fe₂O₃. The electrochemical reaction mechanisms of Fe₂O₃-Se with lithium were examined by X-ray photoelectron spectroscopy (XPS), high resolution transmission electron microscopy (HRTEM) and selected-area electron diffraction (SAED). The reversible conversions reaction of nanosized metal Fe with Li₂Se and Li₂O formed after initial discharge process into FeSe and Fe₂O₃ respectively were revealed.     

Structural and electrochemical properties of mixed calcium-zinc spinel ferrites nanoparticles

In the current work, we provide the electrochemical (EC) characteristics and considerable size of Ca-doped ZnFe₂O₄ nanoparticles. Mixed transition metal oxides are widely used as excellent electrode materials in superior supercapacitors because of their superior capacitance, low cost, and environmental friendliness. The prepared nanoparticles were characterized by X-ray diffraction (XRD), Field-emission scanning electron microscope (FE-SEM), energy-dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), and EC methods. The results exhibited that the as-synthesized nanoparticles had a cubic spinel crystal structure and efficient EC properties. The EC properties of the prepared electrodes were explored by cyclic voltammetry (CV), galvanostatic charge/discharge (GCD), and electrochemical impedance spectroscopy (EIS) studies. The Ca_0.1Zn_0.9Fe₂O₄ electrode demonstrated a specific capacitance (SC) ～208 Fg^-1 at a 2 mV/s scan rate due to significant morphological behavior. Therefore may be the prepared materials are the finest electrodes for supercapacitor applications.     

Synthesis and Characterization of Novel Heat Resistant,Superparamagnetic Poly(ether-imide) Nanocomposites Containing Xanthene: Representing a Strategy for Improving Thermal Stability of Magnetic Polymer-Based Nanocomposites

Two superparamagnetic and heat resistant xanthene based poly(ether-imide) nanocomposites were successfully synthesized. Field emission scanning electron microscopy, transmission electron microscope, X-ray diffraction, thermal gravimetric analysis, vibrating sample magnetometer, Energy-dispersive X-ray spectroscopy and Fourier-transform infrared (FTIR) techniques were used for studying the morphology, crystalline phase, thermal stability and magnetization properties of the nanocomposites. The neat form of the corresponding poly(ether-imide) was also prepared by thermal imidization method and its structure was confirmed by FTIR, proton nuclear magnetic resonance (¹H NMR), UV–Vis and photoluminescence (PL) spectroscopies. In order to investigate the effects of modifying the surface of Fe₃O₄ nanoparticles on thermal properties of the nanocomposites, the surface of Fe₃O₄ nanoparticles was coated with SiO₂ and polysuccinimide (PSI), sequentially. Then, both the unmodified Fe₃O₄ and surface-modified Fe₃O₄ (Fe₃O₄@SiO₂–PSI) nanoparticles were used as fillers for the polymer matrix. According to the results, the prepared nanocomposites were superparamagnetic and showed higher thermal stability in comparison to the neat poly(ether-imide). Furthermore, poly(ether-imide)/Fe₃O₄@SiO₂–PSI (PIEN 10b) nanocomposite showed higher thermal stability and dispersed better in the polymer matrix [in comparison to poly(ether-imide)/Fe₃O₄ (PIEN 10 a)] due to the presence of imide groups and high hydroxyl content of the functional Fe₃O₄ nanoparticles which caused high interactions between poly(ether-imide) and functional Fe₃O₄. Furthermore, the presence of methyl, ether and bulky xanthene groups in the poly(ether-imide(backbone improved the solubility of the neat polymer in organic solvents. These properties can be very helpful for extending new applications of poly(ether-imide)s.     

A novel biosensor based on electro-co-deposition of sodium alginate-Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>-graphene composite on the carbon ionic liquid electrode for the direct electrochemistry and electrocatalysis of myoglobin

A novel biosensor based on electro-co-deposition of myoglobin (Mb), sodium alginate (SA), Fe₃O₄-graphene (Fe₃O₄-GR) composite on the carbon ionic liquid electrode (CILE) was fabricated using Nafion as the film forming material to improve the stability of protein immobilized on the electrode surface, and the modified electrode was abbreviated as Nafion/Mb-SA-Fe₃O₄-GR/CILE. FT-IR and UV–vis absorption spectra suggested that Mb could retain its native structure after being immobilized in the SA-Fe₃O₄-GR composite film. The electrochemical behavior of the modified electrode was studied by cyclic voltammetry, and a pair of symmetric redox peaks appeared in the cyclic voltammograms, indicating that direct electron transfer of Mb was realized on the modified electrode, which was ascribed to the good electrocatalytic capability of Fe₃O₄-GR composite, the good biocompatibility of SA and the synergistic effects of SA and Fe₃O₄-GR composite. The electrochemical parameters of the electron transfer number (n), the charge transfer coefficient (α) and the electron transfer rate constant (k _s) were calculated as 0.982, 0.357 and 0.234 s^?1, respectively. The modified electrode exhibited good electrocatalytic ability to the reduction of trichloroacetic acid (TCA) with wide linear range from 1.4 to 119.4 mmol/L, low detection limit as 0.174 mmol/L (3σ), good stability and reproducibility.     

聚乙二醇/聚乙烯吡咯烷酮修饰的纳米Fe3O4粒子的制备与表征

为了获得能够在水中稳定分散,具有广泛应用前景的磁性纳米粒子,以不同分子量的聚乙烯吡咯烷酮(PVP)作为修饰剂,在聚乙二醇(PEG)中高温热分解乙酰丙酮铁(Fe(acac)₃)制备了纳米Fe₃O₄粒子。采用X射线粉末衍射仪(XRD)、透射电镜(TEM)、高分辨透射电镜(HRTEM)、超导量子干涉仪(SQUID)、热重分析仪(TGA)、傅里叶变换红外光谱仪(FT-IR)、纳米粒度与zeta电位分析仪对样品进行了表征,并对样品在生理盐水和生理缓冲液中的稳定性进行了研究,结果表明:制备的纳米Fe₃O₄粒子具有高的结晶度以及单分散性,在300 K下,具有超顺磁性和较高的饱和磁化强度;PEG和PVP共同修饰于纳米Fe₃O₄粒子表面,为纳米Fe₃O₄粒子提供了良好的水分散性;制备的纳米Fe₃O₄粒子在生理盐水和多种生理缓冲液中能够高度溶解并稳定地分散。水中的纳米Fe₃O₄粒子表面呈电中性,表面修饰层的空间位阻效应是所制备的纳米粒子在水溶液中高分散的原因。     

Structural,BET and EPR properties of mixed zinc-manganese spinel ferrites nanoparticles for energy storage applications

X-ray diffraction data (XRD) validated the characteristic crystalline spinel cubic structure and a Field-emission scanning electron microscope/energy dispersive spectroscopy (FE-SEM/EDS) validated the proper stoichiometric element ratio of the prepared materials. By using X-ray photoelectron spectroscopy (XPS), the oxidation state of the elements in the prepared materials was verified. An electron paramagnetic resonance (EPR) spectrometer confirmed that Lande factor (g) values decreased as Zn²⁺ concentration in MnFe₂O₄ increased. The electrochemical (EC) characteristics of the materials were verified during production using a three electrode instrument. The EC performances confirm the EC behavior of the electrode materials. We investigated the EC properties of the electrodes using cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD) methods. The Mn_0.85Zn_0.15Fe₂O₄ (code as: MZF1) electrode material has a specific capacitance (Cs) of 62.96 F/g compared to Mn_0.75Zn_0.25Fe₂O₄ (code as: MZF2) and Mn_0.65Zn_0.35Fe₂O₄ (code as: MZF3) electrode at a current density (CD) of 0.5 A/g. According to recent research, electrode materials should be made with the necessary form and size for great act supercapacitor (SC) applications.     

Fabrication of PMMA/PANI/Fe3O4 as a Novel Conducting Hybrid Coating

In this paper, an excellent new hybrid coating including poly(methyl methacrylate) (PMMA), polyaniline (PANI), and magnetite nanoparticles (Fe₃O₄) was obtained. Fe₃O₄ nanoparticles were synthesized using coprecipitation method, and then magnetite nanoparticles have been dispersed into the PANI to increase compatibility with PMMA. Also, PANI/Fe₃O₄ nanocomposites were synthesized through in situ emulsion polymerization, and then PMMA/PANI/Fe₃O₄ hybrid coating was successfully synthesized using batch emulsion polymerization method. Structure, morphology and thermal stability of the samples were characterized using Fourier transform infrared, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and thermal gravimetric analysis (TGA). The synthesized samples were well distributed with an average diameter smaller than 20?nm. Microscopy and X-ray photoelectron spectroscopy results illustrated a great dispersion of magnetite nanoparticles in hybrid matrix. Moreover, the TGA results demonstrated that the PMMA/PANI/Fe₃O₄ hybrid coating nanoparticle is an excellent hybrid coating with high thermal resistance.     

Enhancing electrochemical performance of Fe3O4/graphene hybrid aerogel with hydrophilic polymer

Graphene hybrid aerogels have attracted attention as electrode materials because of their unique porous architectures. However, their electrochemical performance is limited by the intrinsic hydrophobicity and the ease of aggregation of graphene nanosheets. We demonstrate a unique methodology to produce graphene hybrid aerogels through assembly of graphene nanosheets, nanometer‐scale ferroferric oxide (Fe₃O₄), and hydrophilic poly(vinyl alcohol) (PVA) into three‐dimensional hierarchical macrostructures. Electrochemical performance measurements exhibit a significant improvement in the specific capacitance of this ternary hybrid aerogel with remarkable cycling stability. Specifically, the specific capacitance is nearly 6.6 times higher than that of the neat graphene aerogel, and a cycling capacitance retention rate of 99% was achieved after 2000 cycles at a high current density of 0.5 A g^?1. Electrochemical impedance spectroscopy measurements demonstrate a lower resistance in the Fe₃O₄/graphene/PVA aerogel electrode compared with that of both neat graphene and Fe₃O₄/graphene aerogel electrodes. The obtained graphene hybrid aerogels with outstanding cycling performance and high energy density are very promising as electrode materials for supercapacitors. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134 , 45566.     

Functional acrylic acid as stabilizer for synthesis of smart hydrogel particles containing a magnetic Fe3O4 core

This paper reports a novel method to synthesize magnetic, stimuli-sensitive latex nanoparticles made with magnetite/poly(N-isopropylacrylamide-co-acrylic acid) (Fe₃O₄/P(NIPAAm-co-AAc)). To form a stabilized suspended core, iron oxide (Fe₃O₄) was functionalized with AAc such that further polymerization with NIPAAm and AAc monomers could occur. The P(NIPAAm-co-AAc) shell layer exhibited thermosensitive properties. The inclusion of Fe₃O₄ into the latex nanoparticles was confirmed using transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction spectroscopy, thermogravimetric analyzer (TGA), and superconducting quantum interference device magnetometer. The NIP–(AAc2.6–Fe) latex nanoparticles contained 2.25% Fe₃O₄ (by weight), as determined by TGA analysis. The particle diameters measured approximately 160–240 nm with a lower critical solution temperature of 35 °C. These novel magnetic stimuli-responsive latex nanoparticles have potential applications in numerous fields, such as catalyst supports, protein immobilization, cancer therapy, target drug delivery systems, and other biomedical applications.     

A modified composite film electrode of polyoxometalate/carbon nanotubes and its electrocatalytic reduction

Keggin-type polyoxometalate (H₄SiMo₁₂O₄₀) and carbon nanotubes (CNTs) coated by poly(allylamine hydrochloride) (PAH) were alternately deposited on glassy carbon (GC) electrodes by an electrochemical growth method in acidic aqueous solution. The preparation of the film electrode was simple and convenient. Thus-prepared multilayer films and the electrochemical behavior of the composite film modified electrode were characterized by UV–vis spectroscopy and cyclic voltammetry. It was shown that the multilayer films are uniform and stable. The resulting multilayer film modified electrode behaves as an electrochemical sensor because of its low overpotential for the catalytic reduction of S₂O₈ ²⁻ and NO₂ ⁻ in acidic aqueous solution.     

Electroreduction of cation-deficient oxide and dioxygen at a passive iron electrode

The electrochemical characterization of the cation-deficient Fe₂O₃ or passive film with adsorbed oxygen atoms has been given which was produced on iron under the strongly oxidizing conditions of higher potentials. The reduction potential of the cation-deficient Fe₂O₃ lay about 0.5 V anodic to that of the ordinary passive film on iron. The reduction of dioxygen has been studied at a rotating platinum ring-passive iron disk electrode. The passive film was first reduced to porous intermediate [Fe(OH)₂]_ads, and dioxygen was reduced by a four electron process on a film (Fe₃O₄)-covered iron.     

Immobilization of magnetic magnetite nanoparticle film on polyamide fabric

Polyamide (PA) fabric loaded with magnetite (Fe₃O₄) nanoparticle film was prepared by a simple chemical coprecipitation method. The surface morphology, chemical and phase constituents, crystalline structure, magnetic behavior, thermal stability, and mechanical properties of the Fe₃O₄-coated fabric were determined by means of scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, vibrating sample magnetometry, thermogravimetric analysis, differential scanning calorimetry, Fourier transform infrared spectroscopy, and tensile testing. The results show that a thin membrane of Fe₃O₄ nanoparticles was immobilized on the surface of THE PA fabric. The saturation magnetization of the Fe₃O₄-coated fabric was 27.5 emu/g. The onset decomposition temperature increased slightly, but the initial endothermic temperature decreased. The Fe₃O₄ nanoparticles were deposited on the fiber surface by mechanical anchoring action. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Improvement of adherence and anticorrosion properties of an epoxy-polyamide coating on steel by incorporation of an indole-3 butyric acid-modified nanomagnetite

In this study, synthesized magnetite (Fe₃O₄) nanoparticles were treated with a corrosion inhibitor, indole-3 butyric acid (IBA) and incorporated in an epoxy-polyamide coating. The coating was applied on a carbon steel substrate. For comparison, coatings without particles or with nontreated Fe₃O₄ particles were also prepared. The IBA-modified nanomagnetite (IBA–Fe₃O₄) was characterized by infrared spectroscopy and Zeta potential measurements. The inhibitive action of IBA was shown by electrochemical measurements (polarization curves) performed for a bare carbon steel in 0.1 M NaCl solution containing Fe₃O₄ or IBA–Fe₃O₄ nanoparticles. Adherence and anticorrosion properties of the epoxy-based coatings containing Fe₃O₄ or IBA–Fe₃O₄ were compared to those of the pure epoxy-polyamide resin by dry and wet adherence measurements and by salt spray test. The results showed significant improvement of the film adherence and higher corrosion protection of the carbon steel in the presence of IBA–Fe₃O₄. It was concluded that the IBA effect was restricted to the metal/coating interface.     

A novel platform of hemoglobin on core–shell structurally Fe3O4@Au nanoparticles and its direct electrochemistry

A novel platform, which hemoglobin (Hb) was immobilized on core–shell structurally Fe₃O₄/Au nanoparticles (simplified as Fe₃O₄@Au NPs) modified glassy carbon electrode (GCE), has been developed for fabricating the third biosensors. Fe₃O₄@Au NPs, characterized using transmission electron microscope (TEM), scanning electron microscope (SEM) and energy dispersive spectra (EDS), were coated onto GCE mediated by chitosan so as to provide larger surface area for anchoring Hb. The thermodynamics, dynamics and catalysis properties of Hb immobilized on Fe₃O₄@Au NPs were discussed by UV–visible spectrum (UV–vis), electrochemical impedance spectroscopy (EIS), electrochemical quartz crystal microbalance technique (EQCM) and cyclic voltammetry (CV). The electrochemical parameters of Hb on Fe₃O₄@Au NPs modified GCE were further carefully calculated with the results of the effective working area as 3.61 cm², the surface coverage concentration (Γ) as 1.07 × 10⁻¹² mol cm⁻², the electron-transfer rate constant (K_s) as 1.03 s⁻¹, the number of electron transferred (n) as 1.20 and the standard entropy of the immobilized Hb (ΔS⁰′) as calculated to be −104.1 J mol⁻¹ K⁻¹. The electrocatalytic behaviors of the immobilized Hb on Fe₃O₄@Au NPs were applied for the determination of hydrogen peroxide (H₂O₂), oxygen (O₂) and trichloroacetic acid (TCA). The possible functions of Fe₃O₄ core and Au shell as a novel platform for achieving Hb direct electrochemistry were discussed, respectively.     

Rational design of binder-free ZnCo2O4 and Fe2O3 decorated porous 3D Ni as high-performance electrodes for asymmetric supercapacitor

The development of hierarchical, porous film based current collector has created huge interest in the area of energy storage, sensor, and electrocatalysis due to its higher surface area, good electrical conductivity and increased electrode-electrolyte interface. Here, we report a novel method to prepare a hierarchically ramified nanostructured porous thin film as a current collector by dynamic hydrogen bubble template electro-deposition method. At a first time, we report a porous 3D-Ni decorated with ZnCo₂O₄ and Fe₂O₃ by simple, low-cost electrochemical deposition method. The fabricated porous 3D-Ni based electrodes showed an excellent electrochemical property such as high specific capacitance, excellent rate capability, and good cycle stability. The asymmetric solid-state supercapacitor device was fabricated using porous, 3D Ni decorated with ZnCo₂O₄ and Fe₂O₃ as the positive and negative electrodes. The fabricated ZnCo₂O₄//Fe₂O₃ asymmetric device delivered an areal capacitance of 92?mF?cm^?2 at a current density of 0.5?mA?cm^?2 with a maximum areal power density of 3?W?cm^?2 and areal energy density of 28.8?mWh?cm^?2. The higher performances of porous, 3D current collector have a huge potential in the development of high performance supercapacitor.     

Novel electrically conductive and ferromagnetic composites of poly(aniline‐co‐aminonaphthalenesulfonic acid) with iron oxide nanoparticles: Synthesis and characterization

Nanocomposites of iron oxide (Fe₃O₄) with a sulfonated polyaniline, poly(aniline‐co‐aminonaphthalenesulfonic acid) [SPAN(ANSA)], were synthesized through chemical oxidative copolymerization of aniline and 5‐amino‐2‐naphthalenesulfonic acid/1‐amino‐5‐naphthalenesulfonic acid in the presence of Fe₃O₄ nanoparticles. The nanocomposites [Fe₃O₄/SPAN(ANSA)‐NCs] were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X‐ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, elemental analysis, UV–visible spectroscopy, thermogravimetric analysis (TGA), superconductor quantum interference device (SQUID), and electrical conductivity measurements. The TEM images reveal that nanocrystalline Fe₃O₄ particles were homogeneously incorporated within the polymer matrix with the sizes in the range of 10–15 nm. XRD pattern reveals that pure Fe₃O₄ particles are having spinel structure, and nanocomposites are more crystalline in comparison to pristine polymers. Differential thermogravimetric (DTG) curves obtained through TGA informs that polymer chains in the composites have better thermal stability than that of the pristine copolymers. FTIR spectra provide information on the structure of the composites. The conductivity of the nanocomposites (～ 0.5 S cm^?1) is higher than that of pristine PANI (～ 10^?3 S cm^?1). The charge transport behavior of the composites is explained through temperature difference of conductivity. The temperature dependence of conductivity fits with the quasi‐1D variable range hopping (quasi‐1D VRH) model. SQUID analysis reveals that the composites show ferromagnetic behavior at room temperature. The maximum saturation magnetization of the composite is 9.7 emu g^?1. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

Pulsed laser deposited FeOF as negative electrodes for rechargeable Li batteries

FeOF thin film has been successfully fabricated by reactive pulsed laser deposition for the first time, and its electrochemical behavior was examined as a negative electrode active material in lithium-ion batteries. The electrochemical properties of the as-deposited FeOF thin film during the first charging and discharging have been investigated by the galvanostatic cycling and cyclic voltammetry measurements. By using ex situ X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected-area electron diffraction measurements (SAED), it can be found that FeOF was initially decomposed into Fe⁰, LiF, and Fe₂O₃ after discharging to 1.0 V. The newly formed Fe₂O₃ is then subsequently reduced into Li₂O and Fe⁰ after further discharging to 0.01 V. In the subsequent cycle, the reduction peaks at 0.76 V and the oxidation-reduction peaks at 1.6 and 1.9 V could be attributed to the reversible decomposition and formation of Li₂O with the conversion reaction of Fe₂O₃ into Fe.     

Surface layer formation on Li1 + xMn2O4 − δ thin film electrodes during electrochemical cycling

A surface layer formation on positive Li_{1 + x}Mn₂O_{4 − δ} thin film model electrodes as a result of electrochemical cycling procedures has been detected and characterized by scanning electron microscopy and X-ray photoemission spectroscopy. These thin film spinel electrodes, prepared by pulsed laser deposition, were cycled in 1 M LiClO₄ in propylene carbonate between 3.5 and 4.4 V vs. Li/Li⁺ at 40 °C and stopped at defined potentials and cycle numbers. The observed surface layers show, depending on the cycling conditions, a spotty and/or layered appearance and the fraction of this layer covering the cycled electrode depends on the charge potential and the number of electrochemical cycles.