Crystallographic Properties Research Articles

Enhanced performance of Mg and La co-doped TiO2(98%)−ZrO2(2%) photoanode for dye-sensitized solar cells

Abstract This study explores the effects of magnesium (Mg) and lanthanum (La) doping on the performance of dye-sensitized solar cells (DSSCs) utilizing TiO2(98%)−ZrO2(2%) (TZ, TZM, and TZL) photoanodes. The photoanodes were fabricated using a spin-coating sol–gel method, followed by calcination at 400°C. The structural, morphological, crystallographic, and optical properties of the proposed photoanode composites were characterized by X-ray diffraction, transmission electron microscopy, and ultraviolet–visible spectroscopy. The crystallite sizes of the synthesized thin films varied from 21.16 to 59.04 nm for the TZ, TZM, and TZL compositions. The current–voltage measurements of DSSCs based on TZL8 photoanode, cobalt sulfide-doped graphene counter electrode, and N719 dye revealed the highest efficiency of nearly 5.052%. The assembled DSSCs exhibited an open-circuit voltage of 0.74 V, a short-circuit current density of 9.964 mA/cm2, and a fill factor of 0.685. The enhancement in open-circuit voltage and short-circuit current density could be attributed to the improved electronic and microstructures of the proposed photoanodes.

Impact of the host lattice on crystallographic, Raman, optical, and luminescent properties on the terbium ion

AbstractA comparative study of the Gd2O3:Tb and Y2O3:Tb nanoparticles (NPs) was presented to examine the influence of the host lattices on the crystallographic phase, surface characteristics, optical properties, Raman effect, and photoluminescence properties. Cubic shapes Gd2O3:Tb and Y2O3:Tb NPs with an estimated crystalline size of 17 and 11 nm were recorded from the X‐ray diffraction pattern, respectively. Comparative absorption spectra of both oxides NPs were presented to examine the dispersibility, colloidal stability, and optical behavior of the NPs. Energy bandgap values were estimated to monitor the optical characteristics of the metal oxides in the UV/Vis region. Fourier transform infrared was recorded to confirm the surface‐attached water and organic moieties. The Raman spectra of metal oxides were recorded to examine the symmetrical dis‐order and polarizability of the vibrational bands. The ionic radius of the atoms distorts the bond structure resulting in it greatly influenced the vibrational bands of the materials. The emission spectra certified the effective doping of the luminescent Tb3+‐ion in the metal oxide host lattices. Raman spectra and emission spectra validated the crystal symmetry imperfections; subsequently, the efficiency of the Raman active modes and emission transitions was greatly influenced. In a comparative analysis, Y2O3:Tb NPs exhibited higher luminescence intensity in comparison with the Gd2O3:Tb NPs.

Corrosion and mechanical characterisation of Al/TiO2/Y2O3 hybrid nanocomposites produced by squeeze casting

ABSTRACT In this study, the corrosion and mechanical performance of hybrid aluminium matrix nanocomposites (HAMNCs) reinforced with titanium oxide (TiO2) and yttrium oxide (Y2O3) nanoparticles were investigated. A squeeze-casting process was used to develop five HAMNCs with wt.% of nanoparticles of 2.5, 5, 7.5, and 10. The corrosion resistance of HAMNCs was investigated during a 168-h salt spray test. XRD examined the crystallographic and elemental properties of the HAMNCs. FESEM was used to examine nanoparticle distribution and interaction in the matrix. The microhardness, compression strength and yield strength properties of the fabricated samples were examined. The introduction of nanoparticles at 5 wt.% TiO2 +5 wt.% Y2O3 (HAMNC6) in the Al matrix had the most outstanding properties (corrosion resistance, microhardness, compression strength, yield strength). The properties were shown to be inversely proportional with an increase in the wt.% of the nanoparticles. The SEM analysis of corroded surfaces revealed that TiO2 and Y2O3 nanoparticles were found near the grain boundaries of HAMNC6, causing small pits and minor cracks.

Effect of synthesis temperature on the properties and photocatalytic performance of peroxo-titanate nanotubes prepared by bottom-up synthesis method

The alkaline treatment synthesis of titania/titanate nanotubes (TNTs) requires highly concentrated alkaline solutions (≥ 10 mol/L), which pose environmental and productivity limitations. In contrast, a bottom-up synthesis method for peroxo-titanate nanotubes (PTNTs) has been developed. This method offers two advantages: it can synthesize materials using low-concentration alkaline solutions (1.5 mol/L) and produce photocatalytic materials that are responsive to visible light. In general, the higher the crystallinity of a catalyst, the better its properties. However, PTNTs synthesized at temperatures close to their boiling point (around 100 °C) exhibit low crystallinity. This study hypothesizes a hydrothermal synthesis method at higher temperatures will enhance the crystallinity and photocatalytic performance of PTNTs, synthesizing them at temperatures ranging from 120 to 200 °C using a method capable of exceeding the boiling point. Higher synthesis temperatures resulted in improved morphological and crystallographic properties of the PTNTs. However, the formation of peroxo-bonding, crucial for visible light responsiveness, decreased. Nevertheless, peroxo-bonding formation was still achievable at the highest temperature of 200 °C, and the sample exhibited the best Rhodamine B (Rh B) photodegradation performance under visible light due to its enhanced specific surface area and crystallinity. This study highlights the novelty and environmental significance of hydrothermally synthesized PTNTs as superior photocatalysts by optimizing the synthesis temperature while using lower concentration alkaline solutions.

On the structural and bandgap properties of mist-CVD-grown κ-Ga2O3 post continuous temperature annealing

We investigate the continuous annealing of orthorhombic κ-Ga2O3 films on AlN/c-plane sapphire templates grown by Mist Chemical Vapor Deposition (mist-CVD) using in situ high-temperature x-ray diffraction (HT-XRD). Increasing the annealing temperature from 400 to 1100 °C in both vacuum and ambient air reveals a phase transition onset at 825 °C. High-resolution transmission electron microscopy and XRD demonstrated that annealing within the stability window of 650 to 775 °C effectively improves the crystal quality of the κ-Ga2O3 thin film. Optical transmittance and low-loss electron energy loss spectroscopy (EELS) show the pristine film’s bandgaps to be 4.96 and 4.67 eV, respectively, with reduced bandgaps in annealed films due to increased defect density. EELS-derived optical joint density of states indicates that air-annealing fosters sub-bandgap radiative processes, while vacuum annealing suppresses them, qualitatively correlated with the observed photoluminescence intensity variations. The results of this comprehensive high-temperature annealing study offer crucial insight into the influence of annealing ambient conditions on the crystallographic properties of κ-Ga2O3 films and the associated evolution of extended sub-bandgap states.

The influence of precursor solutions containing an amount of silver bismuth sulfide nanoparticles (AgBiS2 NPs) on the characteristics of CH3NH3PbI3 perovskites solar cells

The utilization of organo-metal halide perovskites as absorbers in thin-film solar cells has garnered considerable interest from the scientific community in recent times. In this study, we present the introduction of silver bismuth sulfide nanoparticles (AgBiS2 NPs) doped into perovskite thin films composed of CH3NH3PbI3 thin film. Our results demonstrate that the perovskites' morphology and structure were significantly improved. The effects of AgBiS2 NPs concentration on the optical, mechanical, and crystallographic properties of CH3NH3PbI3 perovskite thin films were investigated. The findings from the structure investigations revealed that an increase in the concentration of AgBiS2 NPs resulted in a transition from a low-crystalline to a polycrystalline structure of the perovskite thin films. An elevation in the concentration of AgBiS2 NPs from 2 to 8 mg/mL led to the development of perovskite films of superior quality, consisting entirely of PbI3 and CH3NH3. These films exhibited almost impeccable deposition, compactness, and uniformity, and their particle size reached an approximate value of 1.3 μm. Furthermore, an increase in the optical absorption coefficient (∼105 cm−1) in the visible spectrum and subsequent enhancements in photoluminescence (PL) and ultraviolet–visible (UV–Vis) absorption spectroscopy serve as further evidence of the film's enhanced quality. When AgBiS2 NPs are doped into perovskites, the films' quality is significantly improved; they acquire a uniform surface morphology, an exceptional crystal structure, and enhanced light absorption, all of which contribute to accelerated PL quenching and charge transfer. Power conversion efficiency (PCE) was enhanced across all photovoltaic parameters through the use of larger granules in bulk-heterojunction solar cells, as opposed to undoped heterojunction solar cells. The PCE of the perovskite device with CH3NH3PbI3 base is 17.04 % at the optimal concentration of 6 mg/mL AgBiS2 NPs. These findings indicate that the doping of CH3NH3PbI3 perovskite thin films with AgBiS2 NPs is essential for the achievement of high crystallinity, a large particle size, and a high absorption coefficient. These properties are advantageous for the high-power conversion efficiency of solar cell applications.

Enhanced properties of low-density polyethylene composites reinforced with Bridelia ferruginea fibers: effect of low temperature fiber acetylation

In this study, lignocellulosic fibres were extracted from Bridelia ferruginea (BF), a shrub which can be found in sub-Saharan Africa with a view to probing the potential application of the fibres. The chemical properties of the BF were chemically modified by acetylation to evaluate the potential applications of the fibre reinforced polymer composites. The unacetylated and acetylated fibres were characterized using Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD) and Thermogravimetric Analysis (TGA) to compare thermal and crystallographic properties after acetylation over different lengths of time. The acetylated fibres with the most promising properties were used for the fabrication of a polymeric composite. The mechanical properties of the fibre-reinforced polymer composites were studied by hardness and dynamic mechanical measurements. Four types of polymeric samples were prepared for the mechanical measurements: unreinforced polymer (Control) polyester, ATBF/LDPE, ACEBF3/LDPE, ACEBF/LDPE. The SEM micrographs revealed that acetylation led to defibrillation. FTIR peaks at 1250 cm−1 and 1371 cm−1 confirmed that acetylation had occurred. The fibres possessed high crystallinity index of 75% which reduced as time of acetylation increased. Acetylation at mild conditions of 70 °C for 3 h did not result in significant damage to the fibres. For the hardness measurements, the values of the micro-hardness of the composite samples increased from 0.20 GPa to 0.29 GPa. The acetylated fibres tend to further resist deformation due to its dispersion in the polymer matrix providing a stronger cross-linking effect. The properties unearthed show that BF appears to be a promising raw material for the production of polymer composites.

Non-radiative recombination centres in InGaN/GaN nanowires revealed by statistical analysis of cathodoluminescence intensity maps and electron microscopy

The methodology of statistical analysis of cathodoluminescence (CL) intensity mappings on ensembles of several hundreds of InGaN/GaN nanowires (NWs) used to quantify non-radiative recombination centres (NRCs) was validated on InGaN/GaN NWs exhibiting spatially homogeneous cathodoluminescence at the scale of single NWs. Cathodoluminescence intensity variations obeying Poisson's statistics were assigned to the presence of randomly incorporated point defects acting as NRCs. Additionally, another type of NRCs, namely extended defects leading to spatially inhomogeneous cathodoluminescence intensity at the scale of single InGaN/GaN NWs are revealed by high resolution scanning transmission electron microscopy, geometrical phase analysis and two-beam diffraction conditions techniques. Such defects are responsible for deviations from Poisson's statistics, allowing one to achieve a rapid evaluation of the crystallographic and optical properties of several hundreds of NWs in a single cathodoluminescence intensity mapping experiment.

Precision engineering of surface defects of cerium oxide nanostructured fine particles for the multiplexed detection of electrolytes and glucose inside tissue models

The development of biosensors for the detection of glucose and electrolytes has become a crucial field of research nowadays due to the increasing incidence of long-term conditions. Specifically, the use of cerium oxide as a selective material for the detection of glucose is raising interest as an alternative to enzymatic sensors due to their stability and low-cost. This work demonstrates for the first time a significant improvement in the selectivity of glucose sensors based on cerium oxide nanostructured fine particles through doping with nickel ions and using pulse voltammetry for the sensing. By using nickel-doped cerium oxide fine particles, the sensitivity of the devices improved by 10-fold, and the selectivity when testing the devices against lactate increased by 68.5 % as compared to pure cerium oxide fine particles, with a limit of detection in the micromolar level. Crystallographic and compositional properties that led to such increase in sensitivity were determined, as a result of a presence of oxygen defects and amorphous domains at the surface of fine particles. This device could be adapted for the simultaneous measurement of glucose and sodium ions. The pulse voltametric approach enhanced the sensitivity of the sensors towards sodium ions, which reached a super-Nernstian sensitivity of 111 mV Log[Na+]-1, with a response time of 2 mins, and has been used for the testing of the electrodes in a practical environment using a skin-inspired material. This technology will pave the way for the development of miniaturised non-invasive wearable sensors real-time measurement of glucose and electrolytes in patients.

Interfacial Stabilization of Organic Electrochemical Transistors Conferred Using Polythiophene-Based Conjugated Block Copolymers with a Hydrophobic Coil Design.

The recent interest in developing low-cost, biocompatible, and lightweight bioelectronic devices has focused on organic electrochemical transistors (OECTs), which have the potential to fulfill these requirements. In this study, three types of poly(3-hexylthiophene) (P3HT)-based block copolymers (BCPs) incorporating different insulating blocks (poly(nbutyl acrylate) (PBA), polystyrene, and poly(ethylene oxide) (PEO)) were synthesized for application in OECTs. The morphological, crystallographic, and electrochemical properties of these BCPs are systematically investigated. Accordingly, P3HT-b-PBA demonstrates superior performance in the KCl-based aqueous electrolyte, with a higher product of mobility and capacitance (μC*) at 170 F s-1 cm-1 V-1 than that of the P3HT homopolymer at 58 F s-1 cm-1 V-1. P3HT-b-PBA exhibits better stability over 50 ON/OFF switching cycles than do other BCPs and P3HT homopolymers. With regard to the performance in the KPF6-based aqueous electrolyte, P3HT-b-PBA outperforms with a higher μC* of 9.2 F s-1 cm-1 V-1 than that of 8.6 F s-1 cm-1 V-1 observed from P3HT. Notably, both polymers exhibited almost no decay in device performance over 110 ON/OFF switching cycles. The strongly different performance of polymers in these two electrolytes is due to the side chain's hydrophobicity and interdigitated lamellar structures, thereby retarding the doping kinetics of the highly hydrated Cl- ions compared with the slightly hydrated PF6- ions. Concerning the improved performance of P3HT-b-PBA, this is attributed to its soft and hydrophobic backbone. Our morphological and crystallographic analyses reveal that P3HT-b-PBA experiences minimal structural disorder when swelled by the electrolyte, maintaining its original structure better than the P3HT homopolymer and the hydrophilic BCP of P3HT-b-PEO. The hydrophobic nature of P3HT-b-PBA contributes to the stability of its backbone structure, ensuring enhanced capacitance during the operation of the OECT operation. These findings provide reassurance about the stability and performance of P3HT-b-PBA in the field of OECT applications. In summary, this study represents the first exploration of P3HT-based BCPs for OECT applications and investigates their structure-performance relationships in mixed ionic-electronic conductors.

Regulating reaction kinetics used for the preparation of ethylene-vinyl acetate copolymer with high grafting ratio

A feasible and innovative reaction kinetics control method was proposed to reduce the degradation, cross-linking and other side reactions during the melt grafting process. The components in the melt grafting system were firstly blended at a temperature lower than the half-life (170 °C) of the radical initiator. After the system was homogeneous, the temperature was raised to the half-life temperature for high-temperature melting reaction. By regulating the reaction kinetics of silane grafted EVA system, the collision probability between macromolecular free radicals and grafted monomers was effectively increased. The efficiency and grafting rate of EVA grafted by silane were significantly improved, which reached a maximum of 74.45 % and 4.81 wt%, respectively. The thermal behavior, crystallographic, mechanical and electrical properties of the grafts were further characterized, which made the structure-activity relationship of polymers construct and investigate.

A Comparative Study on Structural, Crystallographic and Microstructural Properties of Nano-TiO2 Intermixed and Surface-Coated Portland Cement Mortars

A Comparative Study on Structural, Crystallographic and Microstructural Properties of Nano-TiO2 Intermixed and Surface-Coated Portland Cement Mortars

Sculpting the Electronic Nano-Terrain on a Perovskite Film for Efficient Charge Transport.

Nanopatterned halide perovskites have emerged to improve the performance of optoelectronic devices by controlling the crystallographic and optical properties via morphological modification. However, the correlation between the photophysical property and morphology transformation in nanopatterned perovskite films remains elusive, which hinders the rational design of nanopatterned halide perovskites for optoelectronic devices. In this study, we employed nanoimprinting lithography on a perovskite film to exert a precise control over grain growth and manipulate electronic structures at the level of individual grains. Surface-selective fluorescence lifetime imaging microscopy (FLIM) analyzes the spatiotemporally disentangled geometrical variations in carrier recombination rate and band structure modulation according to different pattern morphologies. Consequently, the stereoscopic mechanism of confined grain growth was unveiled, highlighting the quantitative grain size-based parameters that are crucial for nanoscale material engineering. Notably, the pattern-induced reduction of effective charge mass enabled exclusive control over the subdiffusive carrier transport dynamics on perovskite surfaces, ultimately realizing the surface-selective perovskite photodetectors. The implications of this study are expected to provide valuable guidelines, inspiring innovative design protocols for advancing the next-generation optoelectronic technologies.

Giant chiral amplification of chiral 2D perovskites via dynamic crystal reconstruction.

Chiral hybrid perovskites show promise for advanced spin-resolved optoelectronics due to their excellent polarization-sensitive properties. However, chiral perovskites developed to date rely solely on the interaction between chiral organic ligand cations exhibiting point chirality and an inorganic framework, leading to a poorly ordered short-range chiral system. Here, we report a powerful method to overcome this limitation using dynamic long-range organization of chiral perovskites guided by the incorporation of chiral dopants, which induces strong interactions between chiral dopants and chiral cations. The additional interplay of chiral cations with chiral dopants reorganizes the morphological and crystallographic properties of chiral perovskites, notably enhancing the asymmetric behavior of chiral 2D perovskites by more than 10-fold, along with the highest dissymmetry factor of photocurrent (gPh) of ~1.16 reported to date. Our findings present a pioneering approach to efficiently amplify the chiroptical response in chiral perovskites, opening avenues for exploring their potential in cutting-edge optoelectronic applications.

In Situ Formation of Iodide Precursor for Perovskite Quantum Dots with Application in Efficient Solar Cells.

Perovskite quantum dots (PQDs) become a kind of competitive material for fabricating high-performance solar cells due to their solution processability and outstanding optoelectronic properties. However, the current synthesis method of PQDs is mostly based on the binary-precursor method, which results in a large deviation of the I/Pb input ratio in the reaction system from the stoichiometric ratio of PQDs. Herein, a ternary-precursor method with an iodide source self-filling ability is reported for the synthesis of the CsPbI3 PQDs with high optoelectronic properties. Systematically experimental characterizations and theoretical calculations are conducted to fundamentally understand the effects of the I/Pb input molar ratio on the crystallographic and optoelectronic properties of PQDs. The results reveal that increasing the I/Pb input molar ratio can obtain ideal cubic structure PQDs with iodine-rich surfaces, which can significantly reduce the surface defects of PQDs and realize high orientation of PQD solids, facilitating charge carrier transport in the PQD solids with diminished nonradiative recombination. Consequently, the PQD solar cells exhibit an impressive efficiency of 15.16%, which is largely improved compared with that of 12.83% for the control solar cell. This work provides a feasible strategy for synthesizing high-quality PQDs for high-performance optoelectronic devices.

Finite Size Effects in Antiferromagnetic Highly Strained BiFeO3 Multiferroic Films

AbstractEpitaxially strain‐engineered tetragonal (T)‐like BiFeO3 (BFO) is a multiferroic material with unique crystallographic and physical properties compared to its bulk rhombohedral parent. While the effect of this structural change on ferroelectric properties is understood, the influence on correlated antiferromagnetic (AFM) properties, especially with reduced film thickness, is less clear. Here, the AFM behavior of T‐like BFO films 9–58 nm thick on LaAlO3 (001) substrates fabricated by pulsed laser deposition was studied using conversion electron Mössbauer spectroscopy and X‐ray diffraction. The key findings include: i) Ultrathin T‐like BFO films (<10 nm) show a decoupling of magnetic and structural transitions, with the polar vector tilted 32 degrees from [001] in 9–13 nm films. ii) Films thinner than 13 nm exhibit no structural transition down to 150 K, with a Néel (TN) transition at ≈290 K, ≈35 K lower than thicker films. Interestingly, the TN scaling with thickness suggests realistic scaling exponents considering a critical correlation length for C‐type AFM order, rather than G‐type. The results show that finite size effects can tailor transition temperatures and modulate AFM wave modes in antiferromagnetic oxides, with implications for AFM spintronics for future information technologies.

Analysis of CeO2/SiO2 double-layer thin film stack with antireflection effect for silicon solar cells

This study introduces CeO2/SiO2 double-layer film stacks and its antireflection coating effect. Optical properties were analyzed by spectrophotometer measurements; surface morphology and cross-sections were observed by Scanning Electron Microscopy (SEM); elemental distributions and crystallographic properties were determined by Energy Dispersive Spectroscopy (EDS) and X-ray Diffraction (XRD) measurements. Average reflectance of single-layer 0.3MSiO2, 0.6MSiO2, and 0.3MCeO2 thin films were 30.54%, 20.12%, and 14.23%, respectively. Average reflectance was decreased significantly down to 5.9% by 0.3MCeO2/0.6MSiO2 double-layer thin films comparing to those of the results of single-layer films and bare silicon surface reflection (~40%). Antireflective effect of the films on solar cells was estimated by simulation using the measured reflection data. Simulated solar cells indicate that 0.3MCeO2/0.6MSiO2 double-layer antireflective coatings are capable to increase the efficiency significantly and conversion efficiency of 21.7% could be achieved.

Structure of ZnxFe3−xO4 nanoparticles studied by neutron diffraction and its relation with their response in magnetic hyperthermia experiments

The mixed zinc-ferrite spinel magnetic nanoparticles (MNPs) with the general formula ZnxFe3−xO4 are among the most extensively studied families of Fe oxides due to their interesting and diverse chemical, electronic, and magnetic properties. These systems offer the possibility of surface functionalization and possess high biocompatibility, making them highly attractive for applications in biomedicine, such as magnetic fluid hyperthermia (MFH). The efficiency of the MFH process relies on the magnetic, structural and morphological properties of the MNPs. The substitution with the Zn ion and the cationic distribution, as well as the synthesis process employed, have a direct impact on the final properties of these oxides. Therefore, it is essential to have tools that enable a comprehensive characterization of the system to assess its performance in MFH. In this study, we have synthesized four ZnxFe3−xO4 MNP systems using three different methods: two by thermal decomposition at high temperatures, one by co-precipitation, and another by co-precipitation followed by ball milling. We analyze the effect of these various synthesis processes on the magnetic and crystallographic properties, aiming to correlate them with the response of each system in MFH. Neutron diffraction data are employed to determine the cation site occupation and to investigate the correlation with the synthesis method. MFH measurements were conducted in media of diverse viscosities, revealing different values of specific loss power, thus demonstrating a clear dependence on the synthesis process and Zn content.

Investigations on the crystallographic stacking disordering and properties of novel Ga-containing in-plane chemically ordered (Cr2/3R1/3)2GaC (R=Y, Tb - Lu) i-MAX phases

Eight novel transition metal carbides, nanolaminated (Cr2/3R1/3)2GaC (R=Y, Tb, Dy, Ho, Er, Tm, Yb and Lu) with R in-plane chemical ordered occupation, have been synthesized with mainly Cmcm orthorhombic structure and monotonously decreased lattice parameters due to lanthanide contraction. Stacking disorderings and high-density slidings within c plane have been observed. Two characteristic in-plane sliding, along [100] or [1¯30]o directions have been analyzed with former one leading into the structural evolution between Cmcm and C2/c symmetry. Such an atomic scale co-existence of Cmcm and C2/c structures is explained by more negative charge for Ga and anisotropic bonding with Ga compared with A=Al case. Thus, the Vickers hardness, fracture strength and increased wear depth are reduced in representative (Cr2/3Lu1/3)2GaC i-MAX bulk compared with the (Cr2/3Lu1/3)2AlC counterpart.

The Influence of Annealing on the Compositional and Crystallographic Properties of Sputtered Li–Al–O Thin Films

Li–Al–O materials are interesting for several applications. Herein, a Li–Al–O thin‐film materials library, deposited by inert magnetron sputtering and postdeposition annealing in O2 atmosphere, is used to study the effects of different annealing temperatures (300–850 °C) and durations (1 min to 7 h) on crystallinity and composition of the films. X‐ray photoelectron spectroscopy depth profiling reveals inhomogeneous compositional depth profiles of conventionally annealed films (300–650 °C, 3–7 h) with increased Li contents toward the film surface and increased Al contents toward the film–substrate interface, as confirmed by a combination of Rutherford backscattering spectrometry and deuteron‐induced nuclear reaction analysis. The minimum temperature for the formation of crystalline LiAlO2 in the otherwise amorphous films is 550 °C. The undesired inhomogeneous depth profiles are transformed into homogeneous ones by rapid thermal annealing (750–850 °C, 1–10 min), while simultaneously causing the formation of crystalline LiAlO2. Therefore, rapid thermal annealing is shown to be more suitable than conventional annealing for the thermal processing of Li–Al–O thin films. Moreover, this conclusion is expected to have broader relevance beyond Li–Al–O materials, as it is likely to apply to other Li metal oxides, of which there are many technologically relevant ones.