Chemistry and Materials Science

Abstract: No experimental results are reported in this article. What is reported is a hypothesis, the reasoning that produced it, the specific reasons it may be wrong, an experimental programme capable of falsifying it, and a complete account of how generative artificial intelligence was used to derive it, including the errors those systems made. A programme from the Bhabha Atomic Research Centre, running from 2024, separates neodymium from praseodymium by selectively dissolving Nd₂O₃ out of a thermally conditioned physical mixture of Nd₂O₃ and Pr₆O₁₁, using a fluorinated β-diketone dissolved in an imidazolium bis(trifluoromethylsulfonyl)imide ionic liquid. Across five publications five fluorinated β-diketones have been examined, and secondary discussion indicates the imidazolium cation has also been varied within that family. Every reported dissolution medium located in this search is nonetheless an imidazolium bis(triflimide) ionic liquid; no test has been published in which the bulk phase is replaced by a conventional molecular organic solvent. The hypothesis advanced here is that the bulk ionic liquid may be replaceable by methyl isobutyl ketone, a commodity ketone already used in multistage mixer-settler extraction service and already named as a solvent in rare earth extraction patents, with the ligand and every other condition held constant. In the course of preparing this article I re-read the published supporting information and found a result that reframes the hypothesis. With unsintered oxides, the same ionic liquid and the same 0.1 M 2-thenoyltrifluoroacetone give a separation factor of 1.98 to 2.07 over one to four hours — comparable in magnitude to conventional solvent extraction, although the two quantities are defined differently. After sintering at 900 °C the same medium gives approximately 46. Thermal conditioning is therefore essential to the high selectivity observed under the reported conditions. The data do not show that the liquid plays no part — the selectivity may arise from the interaction between a conditioned surface and the liquid chemistry — but they do show that the liquid alone does not produce it. The sharper form of the hypothesis is therefore whether methyl isobutyl ketone can sustain the selectivity that appears when the liquid meets a thermally conditioned solid. The dielectric argument that originally motivated the choice of solvent is stated here with its correct provenance and is expressly described as a screening heuristic rather than evidence: the relative permittivity of 11 used to represent an imidazolium bis(triflimide) medium appears in a different study, on a different ionic liquid, with a different ligand class, while the selective-dissolution work used periodic density-functional calculations with no continuum dielectric at all. Seven mechanistic reasons the substitution may fail are set out, together with a nine-experiment falsification programme, the stoichiometric ceiling on solids loading, and a decision tree assigning a conclusion to each possible outcome. The final sections are a methodological record rather than a chemical one. They describe how an author with no laboratory and no formal training in chemistry produced this hypothesis through iterative dialogue with large language models, and they log thirteen specific errors those systems made — a fabricated patent application number, a federal solicitation deadline welded onto a programme that had closed three years earlier, a misattributed computational parameter, an experimental design that changed two variables at once in a system where one of them moves the answer fourteenfold, and proposed operating conditions exceeding the ligand stoichiometric ceiling by a factor of eighteen — together with how each was caught. United States Provisional Patent Application No. 64/178,827, covering aspects of the process, was filed by the author before this article was posted; the hypothesis and experimental programme are nonetheless set out here in full so that they can be tested.

Abstract: Tablet coating is affected by tablet-bed dynamics, spray exposure, and liquid application, making robust process control challenging. This study aimed to integrate the discrete element method (DEM) with Quality by Design (QbD) to support process parameter selection and development of a tablet coating control strategy. DEM simulations evaluated the effects of drum rotational speed (15, 25, and 35 rpm) and tablet-bed loading (1250, 2000, and 2750 g) on tablet residence time in a virtual spray zone. Based on the simulations, drum speed and coating suspension mass flow rate were investigated experimentally using a three-level factorial design with nine conditions and one repeated centre point. Disintegration time, tablet mass variability, mechanical strength, and visual coating defects were evaluated. DEM showed a nonlinear effect of drum speed on the variability of tablet residence time in the spray zone, with a stronger effect than bed loading. Experimental models confirmed significant effects of both process parameters on the investigated critical quality attributes (CQAs). Favourable operating regions were identified at approximately 23–30 rpm and 8–14 g/min. Conditions around 25 rpm and 11 g/min provided a favourable overall balance of the investigated quality attributes. The integration of DEM and QbD provided complementary mechanistic and experimental information for tablet coating development. The approach supported identification of a practical operating region and a representative target condition for further development of the process control strategy.

Abstract: Thin-profile broadband microwave absorbers must reconcile impedance matching and strong attenuation, two requirements that usually pull in opposite directions. Here, hollow carbonized kapok fibers (CKF) obtained at 1000 °C were compounded with waterborne polyurethane (WPU) at a mass ratio of 8:2 and consolidated by hot pressing. The film reached a dielectric real part of about 325 and behaved as a frequency-selective layer: it transmitted low-frequency microwaves while reflecting high-frequency ones, governed by the frequency-dependent permittivity, the skin effect, a narrow resonance window, mesopore scattering, and the impedance mismatch with free space. Inserting a 0.62 mm CKF/WPU interlayer between a high-frequency surface layer and a low-frequency bottom layer broadened the effective absorption bandwidth from 4.71 to 9.47 GHz (windows at 3.33–9.30 and 11.6–14.9 GHz), with a minimum reflection loss of −54.8 dB at a total thickness of only 1.53–1.62 mm, covering the whole C band, partial S and X bands. This provides a low-cost route to thin, flexible multiband microwave absorbers through a biomass-derived filtering interlayer.

Abstract: Thermophilic microbial electrolysis cells (MECs) may couple wastewater valorization with hydrogen production, but the microbial dynamics influencing their performance remain poorly understood. This study investigated microbial succession and biofilm development in a single-chamber MEC operated for 132 days at 55 °C with fermented sugarcane vinasse under 0.8, 0.9, and 1.1 V. Hydrogen production and microbial colonization were evaluated by gas analysis, scanning electron microscopy, and 16S rRNA gene amplicon sequencing of suspended and electrode-associated biomass. At 0.8 V, hydrogen accounted for 94.7% of the gas phase with a surface-area-normalized H₂ production rate of 30.4 L H₂ m⁻² d⁻¹. During operation at 1.1 V, these parameters reached 96% and 55.4 L H₂ m⁻² d⁻¹. Microscopy confirmed colonization of the carbon-felt anode at the end of operation. The community underwent marked succession: Akkermansia and Pseudomonas were transiently enriched, Caldanaerobius dominated at 0.8 V, and Moorella predominated at the final stage, representing 41.4% of the suspended and 44.9% of the electrode-associated communities. Thermoanaerobacterium increased from 8.1% in suspended biomass to 18.4% on the electrode. These results demonstrate that long-term thermophilic operation selected a specialized consortium comprising fermentative, acetogenic, and potentially electrode-interacting populations while supporting high-rate hydrogen production from fermented vinasse.

Abstract: Ranges of 5 values for 4 different process parameters in a rankine cycle (heater outlet temperature, turbine outlet pressure, pump outlet pressure, and turbine efficiency) were simulatively experimented with in DWSIM software (an open-source process simulation environment used to model and simulate chemical engineering processes under steady-state and dynamic conditions). These values were changed and three dependent variables were measured for each change: net power output, vapor molar fraction and thermal efficiency. Additionally, sensitivity coefficients to measure deviations for each variable were compared according to a set baseline. It was found that the changes in turbine efficiency directly correlated to most of the dependent variables in a linear relationship, while pump outlet pressure and turbine outlet pressure displayed quadratic relationships with the dependent variables. Heater outlet temperature displayed low sensitivity with thermal efficiency, and all such trends are noted in the article. The results provide insight into key operating parameters in Rankine cycles and how theoretical models display the changes in process efficiency. The results were simulated theoretically using a software, which does not necessarily provide output to realistic situations of Rankine cycles. The explicit values of theoretical calculations may not be present in realistic settings, however the general trends and sensitivity coefficients of each parameter and its dependent variable may help provide insight into changes in Rankine operating parameters.

Abstract: Polyethylene (PE) and polypropylene (PP) waste form a big part of polymer waste, and their separation is complicated by similar densities and frequent combination within a single product, making PE+PP co-pyrolysis a practically relevant recycling approach. The effects of component ratio and co-pyrolysis with metal oxides at the atomistic level are insufficiently studied. Using ReaxFF-MD in AMS, with and without transition metal oxides (Fe₂O₃, NiO) pyrolysis and co-pyrolysis of PE and PP chains (C₁₂₀H₂₄₂) were investigated at PE:PP ratios of 100:0, 80:20, 50:50, 20:80, and 0:100 over 1750–3500 K. Kinetic and thermodynamic activation parameters were determined using first- and second-order kinetics based on the Arrhenius and Eyring equations. The degradation rate depended non-monotonically on the PE:PP ratio, with the 50:50 being the slowest among the mixtures, while the metal oxides lowered the decomposition threshold and reduced the activation energy 1.6–2.6-fold. Metal oxides also altered product selectivity: H₂ replaced C₂H₄ as the dominant product, with its yield rising 5–7-fold; Fe₂O₃ gave the most stable H₂ yield, while NiO gave the highest single value. The mechanisms of H₂, H₂O, and CH₄ formation were examined. These results deepen the understanding of the co-pyrolysis processes of PE and PP involving transition metal oxides.

Abstract: A novel biocomposite denoted Ns-AGS was synthesized from Alaeis guineensis Shells and nanosilica extracted from rice husk through a sol-gel method. The final product was applied in the adsorption of an azo dye namely Azocarmin G in synthetic aqueous solution. The characterization of the biocomposite by X-ray diffraction (XRD), Scanning Electron Microscopy, Fourier transform infrared spectroscopy (FTIR) and FTIR/TGA Analysis revealed an amorphous and porous microstructure with a random distribution of nanosilica particles in the lignocellulosic matrix evidencing several functional groups. The influence of contact time (0-120min), adsorbent dose (0.1-0.3g), initial dye concentration (25-100mg/L) and initial pH (3.5-6.5) were investigated at different temperatures (298°K, 316°K and 327°K). This study showed that adsorption of Azocarmin G onto Ns-AGS is favored by acidic pH values leading to more than 90% removal under optimal conditions of pH = 3.5; 60 min; 327°K for an adsorbent dose of 0.3g/25mL. The experimental kinetics data preferentially fitted the Hô model with a correlation coefficient R2 = 0.9992, indicating that adsorption is the determining step of the process illustrating adsorbate-adsorbent affinity. The equilibrium models demonstrated competitiveness, which may be related to the complex nature of the biocomposite. However, the Redlich-Paterson model, which combines Langmuir and Freundlich models, was more suitable at 327°K. The thermodynamic parameters demonstrated the spontaneity of the adsorption process (ΔG < 0) and the endothermic nature of the reaction (ΔH > 0). The low activation energy value (2.92 kJ/mol < 20 kJ/mol) calculated using the Arrhenius equation reflects a physical adsorption that would involve weak Van der Waals and hydrogen bond interactions which combined to Hô model evolved competitivity between chemical and physical processes.

Abstract: Noble metal-supported catalysts exhibit superior catalytic activity, versatility, and accessibility, making them highly promising for the catalytic oxidation of HCHO under ambient conditions. In the process of defining catalytic performance, metal-support interactions (MSIs), which are characterized by the alteration of active site availability, electronic structure tuning, and increased dispersion of metal nanoparticles, play a vital role. These interactions are among the many influencing aspects that play a role. This review comprehensively analyzes recent advancements in the mechanisms underlying MSIs, particularly focusing on strong metal-support interactions (SMSI) and electronic metal-support interactions (EMSI). It is to establish a comprehensive theoretical framework for atomic-level catalyst design optimization by clarifying how SMSI and EMSI accurately control charge transfer and catalytic active site creation. Furthermore, the review highlights current challenges and future perspectives in utilizing MSIs for efficient formaldehyde (HCHO) oxidation, facilitating the development of advanced catalysts toward practical industrial applications.

Abstract: Thermal insulation materials play a crucial role in improving the energy efficiency and durability of buildings; however, their long-term performance can be significantly affected by moisture exposure. This study investigates the relationship between formulation parameters, water susceptibility, structural stability, environmental performance, and economic efficiency of lightweight thermal insulation composites. Ten experimental formulations were produced by systematically varying the cement content, water-to-cement ratio (W/C), gas-forming powder content, and polymer-modifying additives. Water resistance was evaluated through controlled immersion tests and measurements of mass variation and structural condition, supported by response-surface analysis. The experimentally determined water susceptibility ranged from 2.1% to 6.8%, demonstrating a systematic increase with increasing W/C ratio and gas-forming powder content. The most favorable result was obtained for composition no. 1, characterized by a W/C ratio of 0.55 and a powder content of 0.14 g, which exhibited the lowest water susceptibility of 2.1%. The developed composites achieved densities of up to 550 kg/m³ and thermal conductivity values below 0.12 W/(m·K), confirming their potential for building-envelope applications. Composition No. 1 also showed the lowest estimated material cost, approximately EUR 0.120/kg (EUR 66.04/m³), demonstrating that improved moisture resistance can be achieved without compromising economic efficiency. The results establish a quantitative composition–structure–property relationship and demonstrate that coordinated control of the W/C ratio, pore-forming component, and polymer modifiers is essential for balancing moisture resistance, thermal performance, material cost, and environmental sustainability. The proposed integrated assessment framework supports the development and selection of durable thermal insulation composites for sustainable construction, while further long-term durability, leaching, and life-cycle assessments are required to confirm their environmental performance under realistic service conditions.

Abstract: Sodium naproxen is a widely used nonsteroidal anti-inflammatory drug (NSAID) known for its therapeutic efficacy but also for its poor flowability, which complicates manufacturing processes. This study aimed to improve the flow properties of sodium naproxen through a patented mechanochemical dry coating method using nanostructured silica (Aerosil® R972) as a flow modifier. The process was conducted in a modified V-type tumbler mixer under selected conditions, including a 7:1 ball-to-powder mass ratio, 10-minute mixing time, and 10 rpm rotational speed. Flowability was evaluated using Carr’s indices, while mechanical properties were assessed via shear testing with a Jenike cell. Surface morphology was characterized by SEM. Results showed that the modified sodium naproxen samples demonstrated a substantial improvement in flow indices, a shift to “easy-flowing” classification at higher consolidation stresses, and a marked reduction in cohesion compared to the unmodified material. SEM confirmed uniform silica deposition on particle surfaces. These findings indicate that the applied method effectively improves the handling characteristics of sodium naproxen powders. The process is simple, scalable, and suitable for pharmaceutical applications requiring flow enhancement in cohesive active ingredients.

Abstract: Powder mixing is a critical step in pharmaceutical manufacturing, as the uniform distribution of an active pharmaceutical ingredient (API) affects the quality of the final dosage form. This study investigated the relationship between powder mixing performance and tablet quality attributes using sodium naproxen as a model API with limited flowability. Powder mixtures were prepared in a V-type blender, and the mixing index evolution was evaluated at different rotational speeds. Tablets were subsequently produced either by direct compression or by pan granulation followed by compression, and their critical quality attributes, including tablet mass, thickness, crushing strength, abrasiveness, and API content variability, were evaluated. The mixing index rapidly increased during blending and reached high values for all investigated conditions; however, similar mixing efficiency did not result in equivalent tablet properties. Directly compressed tablets exhibited higher crushing strength, lower abrasiveness, and lower API content variability compared with tablets obtained after pan granulation. The results demonstrated that the powder processing route had a stronger influence on final tablet performance than differences in mixing speed within the investigated range. The combination of mixing index evaluation with tablet quality assessment provides a comprehensive approach for understanding the influence of powder processing conditions on pharmaceutical tablet performance. Two-way ANOVA demonstrated that manufacturing technology exerted a substantially stronger influence on tablet quality attributes than mixing speed.

Abstract: Translating adsorption performance from batch experiments to continuous-flow operation is a key step toward practical water-treatment applications. In this study, a laboratory-scale continuous adsorption system based on a water-insoluble β-cyclodextrin-epichlorohydrin (β-CD-EPI) polymer was validated from hydrodynamic, adsorptive, and operational perspectives. Downflow operation caused progressive bed compaction and excessive pressure development, whereas a 90 mm column operated in upflow expanded/fluidized-bed mode remained stable at superficial linear velocities below approximately 12 m h⁻¹. Under these conditions, removal was strongly contaminant-dependent: cyproconazole exceeded 90%, acetaminophen reached 72–77%, hydrochlorothiazide 40–65%, ciprofloxacin 24–50%, and furosemide remained below 30%. The relative performance of furosemide and hydrochlorothiazide differed from that predicted by previous batch-derived adsorption parameters, demonstrating that batch results cannot be directly extrapolated to dynamic operation. Competitive adsorption in binary and ternary mixtures reduced removal, while cyproconazole removal decreased from >90% in tap water to 48–55% in secondary-treated wastewater. Desorption with 220 mM acetate buffer at pH 4.0 recovered >80% of retained cyproconazole within 10 min, followed by a two-stage rinse restoring operational pH. These results define hydrodynamic, adsorption, matrix, and regeneration criteria for subsequent scale-up of β-CD-EPI adsorption processes.

Abstract: This study presents a comprehensive first-principles investigation of the optoelectronic and thermoelectric properties of AlSb in its cubic and hexagonal phases. Structural optimization was performed using the SCAN meta-GGA functional, while the electronic and optical properties were evaluated within the modified Becke-Johnson potential combined with the Hubbard correction (mBJ+U) framework, which provides an improved description of the electronic structure and band-gap values in closer agreement with available experimental data than conventional GGA and SCAN approaches. Both AlSb phases are found to be quasi-direct band-gap semiconductors, with calculated band gaps of 1.71 eV for the cubic phase and 1.50 eV for the hexagonal phase. Additional mBJ+SOC calculations reveal a noticeable reduction of the band gap due to relativistic effects associated with Sb atoms, while preserving the overall electronic-band topology. The optical response reveals strong absorption in the visible and ultraviolet spectral regions, moderate reflectivity, and high refractive indices, indicating pronounced light-matter interaction characteristic of III-V semiconductors. Owing to its reduced symmetry and narrower band gap, the hexagonal phase exhibits enhanced absorption at lower photon energies and a red-shifted optical response compared with the cubic polymorph. Thermoelectric transport calculations demonstrate large negative Seebeck coefficients, thermally activated carrier generation, and a systematic increase in the power factor with carrier concentration for both phases. The cubic phase exhibits higher power-factor values owing to its more dispersive electronic bands and enhanced electrical transport coefficients, whereas the hexagonal phase benefits from lower thermal conductivity, which is advantageous for thermoelectric applications at elevated temperatures. These results establish AlSb as a multifunctional semiconductor with tunable optoelectronic and thermoelectric properties and provide valuable insight into the relationship between crystal structure, electronic structure, and functional performance in III-V semiconductors.

Abstract: The brine of the Aral Sea is considered a complex source of lithium because it contains large amounts of magnesium, potassium, sulfate, and chloride, which prevent the direct preparation of Li₂CO₃. This work describes a technique based on selective precipitation and crystallization of impurities, followed by the isolation of high-purity Li₂CO₃. Initially, magnesium and potassium were precipitated together with Na₂HPO₄ as MgKPO₄, and sulfate was precipitated as CaSO₄·2H₂O using CaCl₂. Such pretreatment made it possible to remove up to 97.1%, 96.3% and 93.4% of magnesium, potassium and sulfate, respectively. Analysis by XRD and EDAX showed that the obtained precipitates consisted of gypsum and phosphate, which can be used as mineral or fertilizer by-products. Then the purified solution was treated with Na₂CO₃ in a stirred crystallizer at 50 °C. Focused Beam Reflectance Measurement (FBRM) analysis showed that increasing the stirring speed from 400 to 600 rpm resulted in smaller Li₂CO₃ particles. The influence of Na2CO3 feed rate was less, but the aggregation of crystals increased at higher concentrations of Na₂CO₃. The proposed technology made it possible to obtain 99.5% pure Li₂CO₃ (for the production of lithium-ion batteries). It was shown that the separation of impurities allows controlling the formation and growth of Li₂CO₃ from natural brine. The developed method provides the opportunity to prepare lithium carbonate suitable for batteries from Aral Sea brine with separation of useful by-products containing magnesium, potassium, calcium, phosphorus and sulfur.

Abstract: Powder mixing is a critical step in pharmaceutical manufacturing, as the uniform distribution of an active pharmaceutical ingredient (API) affects the quality of the final dosage form. This study investigated the relationship between powder mixing performance and tablet quality attributes using sodium naproxen as a model API with limited flowability. Powder mixtures were prepared in a V-type blender, and the mixing index evolution was evaluated at different rotational speeds. Tablets were subsequently produced either by direct compression or by pan granulation followed by compression, and their critical quality attributes, including tablet mass, thickness, crushing strength, abrasiveness, and API content variability, were evaluated. The mixing index rapidly increased during blending and reached high values for all investigated conditions; however, similar mixing efficiency did not result in equivalent tablet properties. Directly compressed tablets exhibited higher crushing strength, lower abrasiveness, and lower API content variability compared with tablets obtained after pan granulation. The results demonstrated that the powder processing route had a stronger influence on final tablet performance than differences in mixing speed within the investigated range. The combination of mixing index evaluation with tablet quality assessment provides a comprehensive approach for understanding the influence of powder processing conditions on pharmaceutical tablet performance.

Abstract: Diallyl ether possesses unique chemical activities due to its dual functional allyl group and ether bond and is thus a high-value-added fine chemical with diverse applications. In this work, thin-plate ZSM-5 is synthesized and then subjected to alkaline post-treatment to improve its catalytic performance for allyl alcohol etherification to diallyl ether. The study shows that the post-treatment impacts on both the microstructure and acidic properties of ZSM-5. Although the selectivity of diallyl ether obtained over different ZSM-5 catalysts are similarly high, the treatment with tetrapropylammonium hydroxide and/or dilute NaOH solutions enhances the conversion of allyl alcohol. The highest turnover number of the reaction achieves when there is a moderate amount of strong acid sites in ZSM-5. This study contributes to the knowledge base for potential application of ZSM-5 in diallyl ether production from allyl alcohol.

Abstract: In this work, the adsorption of a dye from aqueous solutions onto a waste chicken eggshell biosorbent is under consideration. The aim of this work is to assess the possibility of removing the textile dye, i.e., direct blue BR 200, from water by adsorption on eggshells and to generate the process data such as effective internal and external diffusion coefficients. The results of our experimental studies on adsorption equilibrium and kinetics are presented in this paper. The experiments are conducted for both eggshells and activated carbon in order to compare their adsorption efficiency. As a result of the equilibrium studies, the experimental adsorption isotherms are obtained. Moreover, the parameters of the Henry, Freundlich, Langmuir, Langmuir-Freundlich (Sips) and modified BET isotherms are determined based on the experimental data. In the kinetic studies the aqueous solution of a dye flows through the fixed-bed laboratory column. The adsorbent grains constitute the packing of the column. Based on the results of the kinetic studies, the external and internal diffusion coefficients for different process conditions i.e., different flow rates of the liquid phase in the adsorber, are determined. The internal diffusion coefficient, which describes the transfer from the external surface of an adsorbent grain to its interior, is calculated on the basis of the solution to Fick’s unsteady-state diffusion equation. The results of the experiments and calculations presented in this work can be used to determine the efficiency of eggshells as a biosorbent in water purification systems. It was obtained that the eggshells have very good sorption properties with respect to the dye under investigation. Both equilibrium and kinetic studies revealed that the dye uptakes for eggshells are greater than the uptakes for the activated carbon which is a conventional reference adsorbent. Moreover, the Langmuir-Freundlich (Sips) isotherm provides the best fit for the experimental data for both the eggshells and activated carbon. The external diffusion coefficient of the dye in water is D_AB = 2.21·10−10 m²/s. The kinetic calculations revealed that the effective internal diffusion coefficient D_s for both adsorbents is lower than the external coefficient D_AB and it increases with the liquid flow rate. It was also found that D_s for the eggshells is greater than for activated carbon. The obtained values of the internal diffusion coefficient D_s for the eggshells were 2.55·10−11 m²/s, 4.59·10−11 m²/s, 1.92·10−10 m²/s, for the flow rates 1.72 cm³/s, 2.31 cm³/s and 2.90 cm³/s, respectively. The D_s values refer to the equivalent radius of the eggshells grains R_p = 0.00146 m. The isotherms parameters and diffusion coefficients presented in this work can be used as data for process calculations.

Abstract: The rapid transition toward sustainable energy systems has created an urgent demand for advanced functional materials capable of improving energy conversion, storage, and utilization technologies. Artificial intelligence has emerged as a key enabling technology for accelerating materials discovery through data-driven prediction, inverse design, autonomous experimentation, and intelligent decision-making. This mini-review critically examines recent advances in AI-assisted discovery and optimization of advanced energy materials, covering machine learning, deep learning, graph neural networks, transformer models, generative AI, large language models, and self-driving laboratories. Unlike previous reviews that primarily focus on individual AI methodologies or specific classes of energy materials, this work provides an integrated assessment of recent developments across the entire AI-driven materials discovery workflow, encompassing data infrastructures, predictive modeling, generative design, autonomous experimentation, and intelligent closed-loop optimization. Representative studies demonstrate that AI-assisted optimization has reduced battery fast-charging optimization time from approximately 500 days to 16 days and achieved prediction accuracies of up to R2 = 0.88 in virtual materials screening. Representative studies further demonstrate that recent generative AI models have produced more than twice as many stable novel materials while generating structures over ten times closer to DFT ground-state configurations, whereas AI-assisted image analysis has achieved automated materials characterization with segmentation accuracies exceeding 91%. These advances demonstrate the growing practical value of artificial intelligence across batteries, photovoltaics, electrocatalysis, hydrogen technologies, and other sustainable energy applications. This mini-review further discusses recent progress in open materials databases, autonomous experimentation, foundation models, and AI-enabled research platforms that are reshaping modern materials development. Critical evaluation of the available literature indicates that data quality, model generalization, interpretability, computational cost, and experimental validation remain the principal barriers to broader implementation of AI in materials research. Based on the literature synthesized in this mini-review, future advances are expected to depend on the effective integration of generative AI, foundation models, physics-informed learning, and autonomous experimentation within intelligent closed-loop materials discovery ecosystems.

Abstract: The efficient conversion of solar energy into chemical fuels through artificial photosynthesis represents one of the most promising approaches for mitigating global energy shortages and anthropogenic CO₂ emissions. Nevertheless, simultaneously achieving highly selective CO₂ photoreduction and efficient hydrogen evolution remains challenging because of sluggish reaction kinetics, limited visible-light absorption, rapid charge recombination, and insufficient active sites. Herein, we propose a novel hierarchical photocatalyst comprising atomically dispersed Fe–Co dual single atoms anchored on a covalent organic framework (COF)/g-C₃N₄ heterostructure (Fe–Co-SA/COF/g-C₃N₄). The strong electronic interaction between neighbouring Fe and Co single atoms establishes abundant asymmetric Fe–N₄–Co catalytic motifs, while the crystalline COF provides highly ordered π-conjugated pathways that significantly accelerate charge transport. Simultaneously, intimate interfacial contact between the COF and g-C₃N₄ generates an efficient S-scheme heterojunction, promoting directional migration of photogenerated electrons and holes while preserving their strong redox potentials. Density Functional Theory (DFT) calculations reveal that the Fe–Co dual sites reduce the energy barrier for CO₂ activation by approximately 45% compared with isolated Fe sites, whereas Gibbs free-energy analysis demonstrates favorable adsorption of *COOH and *H intermediates. Artificial intelligence-assisted catalyst optimization further identifies the optimal Fe/Co atomic ratio and coordination environment, enabling ultrabroadband solar harvesting extending from ultraviolet to near-infrared wavelengths (300–1800 nm). Under simulated AM 1.5G solar irradiation, the optimized Fe–Co-SA/COF/g-C₃N₄ photocatalyst achieves remarkable CO evolution rates exceeding 1450 μmol g⁻¹ h⁻¹, CH₄ production of 165 μmol g⁻¹ h⁻¹, and H₂ evolution of 12.4 mmol g⁻¹ h⁻¹, together with an apparent quantum efficiency approaching 18.6% at 420 nm and a solar-to-fuel efficiency of 2.8%. Excellent photocatalytic stability is maintained over ten consecutive reaction cycles with negligible structural degradation. This work demonstrates how dual single-atom engineering integrated with crystalline COF/g-C₃N₄ heterostructures provides a powerful strategy for constructing next-generation artificial photosynthetic systems capable of simultaneously producing solar fuels and green hydrogen with exceptional efficiency.

Abstract: Dry reforming of methane represents a promising approach for the valorization of CO₂ captured from industrial emissions via a high-temperature catalytic process. To this aim, a LaMn1-xNixO3 catalyst with a perovskite structure (x=0.25) for dry reforming was obtained as ultrafine powder by solution combustion synthesis and then softly deposited over -alumina supports as structured catalyst. X-ray diffraction proved that the fresh catalyst exhibits the characteristic framework of corner-sharing BO6 oc-tahedra and Mn substitution in B site. Temperature programmed reduction in H2 showed two main peaks between 200 and 400 °C and between 700 and 900 °C, proving the strong reduction of Mn oxides in different oxidation states and Ni oxide even to the elemental state. Raman spectroscopy on fresh and spent catalyst showed that carbon deposition during reforming was negligible and lattice distortion occurred associated to oxygen vacancies or partial reduction. A 25-hour reforming test with LaMn1-xNixO3 proved conversion of CH4 equal to 75% at 700°C. Dry reforming tests with the struc-tured catalyst confirmed the results obtained with the catalyst powder on a larger scale and different conditions, such as temperature, residence time and CH4/CO2 feed ratio, achieving CH4 conversion of up to 94% at 800 °C.