Edge Structure Studies Research Articles

Modifying electronic and physical properties of Fe-NSC catalyst for oxygen reduction reaction via sulfur doping process

The primary challenge in the large-scale production of metal-air batteries or fuel cells is the high cost of Pt, which is used in the oxygen reduction reaction. To address this issue, we synthesized non-precious metal catalysts by doping Fe, N, and S in various sequences. X-ray diffraction and Raman spectroscopy proved that these catalysts had a higher degree of graphitization than carbon black. While the Fe3C phase was found in the catalyst without S, it was absent in all Fe-NSC catalysts. Imaging and X-ray absorption near edge structure (XANES) studies showed atomically dispersed Fe metal in the S-doped non-precious metal catalysts. X-ray photoelectron spectroscopy (XPS) and XANES reveal that the active site concentrations, inactive Fe-S bond, and oxidation number of the Fe species vary according to the N and S doping sequences. Fe-NSC-1 showed fast kinetics and high selectivity, with an onset potential of 0.96 V. Even after 10,000 potential cycles between 0.6 and 1.0 V, the half-wave potential for Fe-NSC-1 decreased by only 3%. Additionally, the Fe-NSC-1 catalyst showed a negligible decrease in current density during the methanol tolerance tests. Overall, this study found that the doping sequence plays a vital role in enhancing the electrochemical performance and stability of these catalysts under suitable operating conditions by influencing their chemical and electronic structures.

Structural and optical properties of Nd doped LaPO4

In this study, effect of Nd doping, as a dopant material on the structural, optical and electronic properties of lanthanum monazite structure has been studied. Pure and Nd:LaPO4 powders with varying Nd concentrations were prepared via conventional high-temperature solid-state reaction method. Compositional information obtained using Energy dispersive X-ray spectroscopy showed that within the detection limit, no impurities were present in the samples. Oxidation states of the elements were confirmed from X-ray photoelectron spectroscopy (La and Nd) and X-ray absorption near edge structure studies (La). X-ray diffraction showed the formation of monoclinic crystal structure without any phase impurity. Fourier transform infra-red spectroscopic measurements confirmed the substitution of Nd in LaPO4 matrix. We also report the first ever local structure analysis using Extended X-ray absorption fine structure which showed that the Nd atoms have successfully substituted La atoms in LaPO4 matrix. The bandgaps were obtained from Diffuse reflectance UV-Visible spectroscopy.

Chromium doped ZnGa2O4 thin films: An X-ray absorption near edge structure (XANES) and X-ray excited optical luminesce (XEOL) study

We report the thermally controlled synthesis of Cr doped ZnGa2O4 thin films and the evolution of their morphology, crystallinity, and optical luminescence tracked with X-ray Absorption Near Edge Structure (XANES) and X-ray Excited Optical Luminescence (XEOL). It is found that the as-prepared ZnGa2O4 thin films doped with/without Cr are amorphous and exhibits no luminescence while annealing induces crystallization which markedly improves crystallinity at higher temperatures. SEM, XRD and O K-edge, Zn and Ga L-edge, and Cr K-edge XANES show disorder to order phase transition upon annealing which is accompanied by the appearance of the N2 line (696 nm) characteristic of the luminescence from Cr-doped ZnGa2O4 where Cr3+ occupies the octahedral Ga3+ site. The N2 line correlates with the crystallinity of the sample in that the higher the annealing temperature, the better the crystallinity and the brighter the N2 line. It is also interesting to note that the optical luminescence from the host ZnGa2O4, which appears in the blue (420 nm), is completely quenched and the energy is transferred to the N2 luminescence in the red (696 nm). These results and their implications are discussed.

Understanding electrochemical and structural properties of copper hexacyanoferrate: Application in hydrogen peroxide analysis

Copper hexacyanoferrate (CuHCF) exhibits great electrocatalytic activity towards H2O2 reduction, making it a suitable electrode material for H2O2 sensors and H2O2-based energy storage devices. In this work, the crystal structures, electronic structures, and electrochemical properties of CuHCF were investigated in detail by both experiments and simulation. Several different samples of CuHCF were synthesized and tested. The effects of Fe oxidation states and the Cu-to-Fe ratios on the electroactivities of CuHCF were evaluated. In-depth voltammetric and X-ray absorption near edge structure (XANES) studies revealed the underlying redox chemistry which contribute to the voltammetric responses of CuHCF. High electroactivity of CuHCF, high cycling stability, and high electrocatalytic activity towards H2O2 reduction were observed for the porous K0.09Cu[Fe(CN)6]0.6 •2.56 H2O particles synthesized at room temperature from chemical co-precipitation of CuSO4 and K3Fe(CN)6 at a 2:1 molar ratio. DFT calculation revealed favorable adsorption of H2O2 on Fe sites. The presence of Cu lowered the local charge on Fe, assisting the adsorption of electron-donating H2O2 molecule on the neighboring Fe atom. The excellent analytical performance of CuHCF towards H2O2 detection was further demonstrated, giving the linear range of 0.0 – 10.0 mM, the sensitivity of 10.6 µA mM‒1, and the limit of detection (3sB/m) of 0.033 mM.

Seed-mediated synthesis and characterization of ZnO@γ-Fe2O3 nanospheres: Building up the core-shell model

This work presents a simple and fast seed-mediated synthesis of ZnO@γ-Fe2O3 nanospheres with structural and optical characterization. A sequential growth of ZnFe2O4 and γ-Fe2O3 components on preformed ZnO seeds was achieved by a sol–gel route. The High-Resolution Transmission Electron Microscopy (HRTEM) disclosed the morphology, particle size and confirmed the core-shell structure of the nanospheres. Qualitative X-ray Photoelectron Spectroscopy (XPS) asserted the presence of O2–, Zn2+ and Fe3+ ions. The complementarity of X-ray Diffraction (XRD) and X-ray Absorption Near Edge Structure (XANES) studies were used for the structural characterization and building up the core-shell model. The UV–Vis and Photoluminescence (PL) spectroscopies were used for optical characterization. The consistency of the bandgap (Eg) values obtained with both techniques assures the obtained results.

Defect persuade paramagnetic properties of nickel doped ZnS nanocrystals and identification of structural, optical, local atomic structure

We have methodically investigated the structural, spectroscopic, local atomic structure and magnetic properties of aquatic \({\text{Zn}}_{{1{\mathbf{ - }}x}} {\text{Ni}}_{x} {\text{S}}\) (0 ≤ x ≤ 0.04) nanocrystals. The structural study of synthesized samples is observed by X-ray diffraction data with Rietveld refinement. Proficient decrease of lattice parameters and inter-planar spacing are determined on \({\text{Zn}}_{{1{\mathbf{ - }}x}} {\text{Ni}}_{x} {\text{S}}\) nanocrystals. The nanocrystalline microstructure is identified by high-resolution transmission electron microscopy. The sphalerite morphology of doped samples are observed by scanning electron microscopy. Shrinkage of energy band gap is observed for doped nanocrystals. Defect formation due to doping of Ni ion is observed by photoluminescence spectroscopy with cyan color emission. X-ray absorption spectroscopy is employed for identification of local structures surrounding of Zn and Ni sites of \({\text{Zn}}_{{1{\mathbf{ - }}x}} {\text{Ni}}_{x} {\text{S}}\) nanocrystals. Extended X-ray absorption fine structure investigation evidenced the existence of nanocluster within the lattice of \({\text{Zn}}_{{1{\mathbf{ - }}x}} {\text{Ni}}_{x} {\text{S}}\) nanocrystals. X-ray absorption near edge structure studies confirmed incorporation of Ni2+ in ZnS lattice of \({\text{Zn}}_{{1{\mathbf{ - }}x}} {\text{Ni}}_{x} {\text{S}}\) nanocrystals. The single pre-edge feature at Ni K-edge is not relying on concentration of Ni dopant in \({\text{Zn}}_{{1{\mathbf{ - }}x}} {\text{Ni}}_{x} {\text{S}}\) nanocrystals. The presence of interstitial Ni is identified by significant fraction of Ni–Ni scattering paths on doped samples. \({\text{Zn}}_{{1{\mathbf{ - }}x}} {\text{Ni}}_{x} {\text{S}}\) nanocrystals exhibit defect persuaded paramagnetism at room temperature.

Chromium doping into NASICON-structured Na3V2(PO4)3 cathode for high-power Na-ion batteries

Na3V2(PO4)3 (NVP) is characterized by a robust 3D structural framework and a high operating potential; these properties have enabled it to be widely studied as a stable and high-energy density cathode material for sodium-ion batteries (SIBs). In the present study, we designed a Na3V1.6Cr0.4(PO4)3/C ([email protected]) cathode by implanting Cr into the crystal structure of NVP and simultaneously coating the surface of NVP with carbon for realizing high power density SIBs. The substitution of Cr to vanadium in the NVP structure significantly enhanced the structural stability of the electrode while the uniform and thin carbon layer improved the electrical conductivity. Interestingly, the [email protected] cathode showed high electrochemical activities with multiple V3+/4+/5+ redox reactions triggered by Cr3+ substitution in a wide voltage range (2.5–4.1 V). Consequently, the [email protected] cathode delivered excellent cycling stability over 500 cycles even at 15C-rate and power capability up to 70 C-rate. Results from the in-situ X-ray diffraction and ex-situ X-ray absorption near edge structure studies were combined to verify the detailed mechanism of the enhanced sodium storage in the [email protected] cathode.

Structural, magnetic, dielectric and $$^{57}\text {Fe}$$ Mössbauer spectroscopic studies on $$\text {Fe}_{1-x}\text {Ce}_x\text {VO}_4$$: a type-II multiferroic material

Here, we report detailed studies on magnetic phase transitions and magneto-electric (ME) coupling in $$\text {Fe}_{1-x}\text {Ce}_x\text {VO}_4$$ . X-ray diffraction (XRD) and Raman spectroscopic measurements confirm triclinic crystal structure (P-1) with small variation in lattice parameters and Ce incorporation into the $$\text {FeVO}_4$$ lattice up to 10% of Ce. The presence of local lattice distortions and electronic inductive effect in $$\text {FeVO}_4$$ between $$\text {Fe}^{3+}$$ and $$\text {V}^{5+}$$ ions were found in X-ray absorption near edge structure (XANES) studies due to the presence of $$\text {Fe}^{3+}$$ –O– $$\text {V}^{5+}$$ linkages. Two antiferromagnetic (AFM) transitions similar to $$\text {FeVO}_4$$ appear at 21.86 K and 16.03 K, and Ce doping has little effect on the magnetic transitions. $$^{57}\text {Fe}$$ Mossbauer spectroscopic results show the invariance of Fe valance. Low temperature high magnetic field Mossbauer data depicts the presence of spiral AFM order in all the samples. A sharp peak at 16.0 K in dielectric permittivity with minimal suppression due to applied magnetic field is observed indicating the presence of ferroelectricity and magneto-dielectric coupling. Magnetic and ME transitions are almost robust against Ce doping.

A Self-Ion Exchange of Na0.53 MnO2+ Cathode for Li+/Na+ Hybrid Ion Battery

P2-structure sodium manganese oxide is synthesized by a simple reduction reaction. The low-cost electrodes of lithium / sodium hybrid ion batteries after the ion exchange process provide new data on the direct use of sodium manganese oxide instead of lithium analogue. As observed by X-ray diffraction analysis, ion exchange occurs in sodium manganese oxide through electrolytes during cell stabilization. Its own ion exchange material has a high discharge capacity of 195 mA h g-1and a stable plateau at 3.0 V for 50 cycles. In-situ X-ray diffraction and ex-situ X-ray absorption close to edge structure studies confirm reversible oxidation reduction reactions and stable structural changes. ex-situ induced coupled plasma atomic emission spectroscopy confirms that residual sodium ions act as pillars during cycling in the structure.

Metallic Tungsten Nanoparticles That Exhibit an Electronic State Like Carbides during the Carbothermal Reduction of WCl6 by Hydrogen.

Carbothermal hydrogen reduction (CHR) is a unique dry chemical process used to fabricate metals and carbides on carbon supports. In this study, a stepwise CHR of WCl6 on a graphite support is demonstrated for the first time. Powder X-ray diffraction studies revealed that, at 773 K, metallic tungsten nanoparticles are produced, whereas, at 1073 K, the metastable W2C phase is generated rather than the thermodynamically stable WC phase. X-ray photoelectron spectroscopy and X-ray absorption near edge structure studies showed that the chemical state of the W nanoparticles simultaneously exhibits metallic W(∼0) and carbide W(δ+) character. The obtained results suggest that, although electronic interactions exist between the metallic W atoms and the graphite support, the body-centered cubic structure of the metallic tungsten is maintained, confirmed by the extended X-ray absorption fine structure. In addition, high-resolution scanning transmission electron microscopy observations revealed that the W nanoparticles exhibit a thin flattened shape on the support. These results support the notion that the mechanism for the formation of the W nanoparticles during the CHR is influenced by the electronic interactions between the W nanoparticles and the graphite support. Our work thus suggests that the combination of early-transition-metal atoms and carbon-based supports would afford modulatable electronic systems though the electronic interactions.

Nanoscale MnO2 cathodes for Li-ion batteries: effect of thermal and mechanical processing

This study investigates the effect of thermal and mechanical processing of MnO2 nanoparticle cathodes on the electrochemical performance, ion intercalation mechanism and structural changes upon cycling. Thermal processing at different temperatures is utilized to tune the sub-nanoparticle polymorph composition, while mechanical processing (high energy ball-milling) is used to change the particle size and create a better contact between active material and conductive graphite additive. The combination of thermal and mechanical processing is also investigated for possible synergistic effects. The structural changes due to processing suggest that thermal treatment of the MnO2 nanoparticles at 400 °C forms a high concentration of pyrolusite domains (1 × 1 channels) leading to improved reversibility of lithium intercalation/de-intercalation and capacity retention. It is also found that ball-milling for a short time (20 min) leads to some amorphization and decrease of the crystallite sizes resulting in improved capacity. The structural changes and ion intercalation mechanism of the pristine and processed electrode materials during cycling are investigated by ex situ synchrotron x-ray diffraction (XRD) and ex situ and in situ x-ray absorption near edge structure (XANES) studies.

Electronic band structure and conduction mechanism of mixed valence Te4+/Te6+ pyrochlore oxides

While many post-transition metals could form mixed valence oxides with high conductivities leading to various interesting applications, oxides of tellurium are usually insulators. The only known mixed valence tellurium oxides that show appreciable electronic conductivities are the $\mathrm{Cs}{(M,\mathrm{Te})}_{2}{\mathrm{O}}_{6}$ series. However, experimental and theoretical investigations of the compounds are scarce. To study the effects of $M$ metal substitution of tellurium on the structural and electronic properties of $\mathrm{Cs}{(M,\mathrm{Te})}_{2}{\mathrm{O}}_{6}$ mixed valence compounds, a series of oxides with the general formula $\mathrm{CsM}{\mathrm{n}}_{x}\mathrm{T}{\mathrm{e}}_{2\text{\ensuremath{-}}x}{\mathrm{O}}_{6}$ have been prepared and characterized. Substituting Te in $\mathrm{CsT}{\mathrm{e}}_{2}{\mathrm{O}}_{6}$ with as small as 2.5% Mn $(x=0.05)$ changes the structure from rhombohedral to cubic symmetry. Based on the x-ray photoelectron spectroscopy and x-ray absorption near edge structure studies, we found that Mn in the samples with $x\ensuremath{\le}0.33$ is in +3 states, while samples with $xg0.33$ contain a mixture of $\mathrm{M}{{\mathrm{n}}^{3}}^{+}$ and $\mathrm{M}{{\mathrm{n}}^{4}}^{+}$. Detailed studies indicate that there are two substitution schemes depending on the $x$ values. The switching between these two schemes occurs at around $x=0.30\ensuremath{-}0.33$, which results in a change in the trend of electronic conductivity. To describe the electronic properties, simple schematic band structure diagrams of the samples are proposed based on experimental results and density functional theory calculations. ${\mathrm{CsMn}}_{\mathrm{x}}{\mathrm{Te}}_{2\text{\ensuremath{-}}x}{\mathrm{O}}_{6}(xl0.33)$ contains $\mathrm{T}{{\mathrm{e}}^{4}}^{+}/\mathrm{T}{{\mathrm{e}}^{6}}^{+}$ mixed valency where both species are in the same crystallographic sites. Yet, the Te $5s$ band is split into two parts with $\mathrm{T}{{\mathrm{e}}^{4}}^{+}$ contributing to the valence band maximum and $\mathrm{T}{{\mathrm{e}}^{6}}^{+}$ contributing to the conduction band minimum. Such a splitting indicates that they are distinguishable because of a local distortion in the lattice. We found that energy levels of $\mathrm{T}{{\mathrm{e}}^{4}}^{+}5s$ states relative to the conduction band exhibit a strong correlation with the unit cell parameters. When the cell parameter is small, $\mathrm{T}{{\mathrm{e}}^{4}}^{+}$ is destabilized in the lattice causing its energy level to increase. While metallic conduction has not been achieved in this series of compounds, the detailed investigation in this work deepens the understanding about their electronic structures and sheds light on the possibility of designing type III mixed valence tellurium oxides.

Molten salt-assisted synthesis of bulk CoOOH as a water oxidation catalyst

Abstract Different sizes of layered CoOOH were synthesized by the molten-salt-assisted method at different temperatures. X-ray diffraction and scanning electron microscope studies reveal that CoOOH grew at (003) with increasing temperature, and its size can reach dozens of microns. X-ray absorption near edge structure and XPS studies demonstrate that the Co valence state of CoOOH-750 is trivalent, and X-ray Absorption Fine Structure shows that it had a higher symmetry and lower disorder degree, indicating that CoOOH-750 has higher crystallinity and Co3+. The results of electrochemical tests show that CoOOH-750 exhibited the best oxygen-evolution-reaction (OER) catalytic activity.

Application of XANES in gamma dosimetry

The thermoluminescence material, CaSO4:Dy, is widely used for the dosimetry of ionizing radiation due to its high sensitivity, low fading and wide dose range from μGy to few tens of gray. However, its application is limited at high doses due to non-linear and saturation effects. In this paper, X-ray Absorption Near Edge Structure (XANES) studies at the Dy L3-edge have been carried out on CaSO4:Dy discs exposed to gamma doses in the range 0–1000 Gy. The results show an increase in white line in XANES spectra with gamma dose. Structural change in CaSO4:Dy also has been studied using X-Ray Diffraction (XRD) and has found no structural change up to 1000 Gy. The study indicates that XANES can be used as an alternative dosimetry technique and is useful in the evaluation of absorbed dose in the case of accidental exposure to high radiation in a radiation facility or during a radiological accident.

Electrochemical Fragmentation of Cu2O Nanoparticles Enhancing Selective C-C Coupling from CO2 Reduction Reaction.

In this study, we demonstrate that the initial morphology of nanoparticles can be transformed into small fragmented nanoparticles, which were densely contacted to each other, during electrochemical CO2 reduction reaction (CO2RR). Cu-based nanoparticles were directly grown on a carbon support by using cysteamine immobilization agent, and the synthesized nanoparticle catalyst showed increasing activity during initial CO2RR, doubling Faradaic efficiency of C2H4 production from 27% to 57.3%. The increased C2H4 production activity was related to the morphological transformation over reaction time. Twenty nm cubic Cu2O crystalline particles gradually experienced in situ electrochemical fragmentation into 2-4 nm small particles under the negative potential, and the fragmentation was found to be initiated from the surface of the nanocrystal. Compared to Cu@CuO nanoparticle/C or bulk Cu foil, the fragmented Cu-based NP/C catalyst achieved enhanced C2+ production selectivity, accounting 87% of the total CO2RR products, and suppressed H2 production. In-situ X-ray absorption near edge structure studies showed metallic Cu0 state was observed under CO2RR, but the fragmented nanoparticles were more readily reoxidized at open circuit potential inside of the electrolyte, allowing labile Cu states. The unique morphology, small nanoparticles stacked upon on another, is proposed to promote C-C coupling reaction selectivity from CO2RR by suppressing HER.

Insights into the new 3d–5f heterometallic quaternary fluorides: Synthesis, crystal structures, spectroscopic properties, and thermodynamic stability

Two new 3d–5f heterometallic quaternary fluorides, Na3CrTh6F30 and Na4NiTh6F30, have been synthesized hydrothermally from the reactions between ThF4, CrF3 or NiF2, NaF, and HF. Single crystal X-ray diffraction studies revealed that Na3CrTh6F30 and Na4NiTh6F30 adopt dense three-dimensional structures with the space group P3¯c1. Surprisingly, these two compounds are isotypic and exhibit a rather unusual case of aliovalent substitution of the 3d metal centers (CrIII ↔ NiII) which is achieved by losing or gaining a Na+ cation in their structures. The valences of CrIII and NiII have been confirmed by corroborating evidences from bond valence sum, UV–vis, and X-ray absorption near edge structure studies. Na3CrTh6F30 and Na4NiTh6F30 exhibit extraordinary thermal stability up to 500 °C and to 800 °C, respectively, and they retain their original structures in strong acids including 14.9 M HNO3 and aqua regia. First-principle calculations based on density functional theory indicat that the formation enthalpy of Na3CrTh6F30 is −118.945 kJ/mol; suggesting that Na3CrTh6F30 is thermodynamically stable under the simulated condition. This finding helps shed light on the potential products generated from corrosion or during the thorium nuclear fuel cycle.

Lead speciation of PM2.5 collected from Greater Cairo, Egypt and Zarqa, Jordan: An energy dispersive X‐ray fluorescence and X‐ray absorption near edge structure study

Fine aerosol particles with an aerodynamic diameter equal or less than 2.5 μm (PM2.5) have been collected from two sites (residential and industrial) in Greater Cairo, Egypt and one site in Zarqa, Jordan. Based on the elemental quantitative analysis of PM2.5 using energy dispersive X‐ray fluorescence with Mo secondary target, Pb concentrations increased remarkably during winter season regardless of the sampling location. Moreover, it reached the maximum concentration at the industrial location of Greater Cairo, Egypt, and it equals 415 ± 485 ng/m3. The remarkable high standard deviation is due to the significant variation of Pb concentration from time to time during that winter season. Depending on the energy dispersive X‐ray fluorescence results, specific PM2.5 samples that have the highest concentration of Pb (two samples/location) have been selected for the X‐ray absorption near edge structure measurements to estimate the oxidation state of Pb species. The X‐ray absorption near edge structure measurements including 13 Pb references have been carried out at Pb‐L3 absorption edge (13.039 keV) using fluorescence mode. It was shown that PM2.5 contains divalent and tetravalent lead in both industrial site in Greater Cairo, Egypt and urban site of Zarqa, Jordan although that of a residential area of Greater Cairo‐Egypt is almost divalent lead.

Mechanism of Sodium Ion Storage in Na7[H2PV14O42] Anode for Sodium‐Ion Batteries

AbstractIn this work, the authors explore the sodium salt of the 14‐vanado(V)phosphate, Na7[H2PV14O42], as a potential anode material for sodium‐ion batteries (NIBs). The multi‐electron redox activity of the polyoxovanadate [H2PV14O42]7‐leads to high capacity. This polyanion is synthesized by a simple aqueous solution procedure and isolate as a sodium salt with different numbers of crystal waters, Na7[H2PV14O42]·nH2O (n = 15–24). Na7[H2PV14O42] as anode in NIBs exhibits a high and reversible capacity of 322 mA h g−1 at 25 mA g−1 with a high cycling stability (with capacity retention of 87% after 120 cycles). Some of the V5+ ions in [H2PV14O42]7‐ can be reduced to V3+ after being discharged to 0.01 V versus Na/Na+, resulting in an average oxidation state of V3.7+, as based on ex situ X‐ray photoelectron spectroscopy and in situ synchrotron X‐ray absorption near edge structure studies. The crystalline material becomes amorphous during the charge/discharge processes, which can be observed by in situ synchrotron X‐ray diffraction, indicating that functionality does not require crystallinity. The authors propose that the charge storage mechanism of Na7[H2PV14O42] anodes mainly involves redox reactions of V accompanied by insertion/extraction of Na ions in‐between polyoxo‐14‐vanadate ions and adsorption/desorption of Na ions on the surface of the vanadate material.

Determination of interstitial oxygen atom position in U2N3+xOy by near edge structure study

The determination of interstitial oxygen atom site in U2N3+xOy film could facilitate the understanding of the oxidation mechanism of α-U2N3 and the effect of U2N3+xOy on anti-oxidation. By comparing the similarities and variances between N K edge and O K edge electron energy loss spectra (EELS) for oxidized α-U2N3 and UO2, the present work looks at the local structure of nitrogen and oxygen atoms in U2N3+xOy film, identifying the most possible position of interstitial O atom.

Atomic Layer Deposition of Lithium Niobium Oxides as Potential Solid-State Electrolytes for Lithium-Ion Batteries.

The development of solid-state electrolytes by atomic layer deposition (ALD) holds unparalleled advantages toward the fabrication of next-generation solid-state batteries. Lithium niobium oxide (LNO) thin films with well-controlled film thickness and composition were successfully deposited by ALD at a deposition temperature of 235 °C using lithium tert-butoxide and niobium ethoxide as Li and Nb sources, respectively. Furthermore, incorporation of higher Li content was achieved by increasing the Li-to-Nb subcycle ratio. In addition, detailed X-ray absorption near edge structure studies of the amorphous LNO thin films on the Nb L-edge revealed the existence of Nb as Nb5+ in a distorted octahedral structure. The octahedrons in niobium oxide thin films experienced severe distortions, which could be gradually alleviated upon the introduction of Li atoms into the thin films. The ionic conductivities of the as-prepared LNO thin films were also measured, with the highest value achieving 6.39 × 10-8 S cm-1 at 303 K with an activation energy of 0.62 eV.