Scientific user facilities generate X-ray scattering data faster than traditional workflows can process them. We address this challenge across two settings, offline dataset exploration and live on-the-fly analysis. We train a domain-specific attention-based Convolutional Variational Autoencoder (C-VAE) on 1.5 million X-ray scattering images to learn low-dimensional representations capturing structural variation across diverse experimental conditions. The learned latent space reveals well-organized clusters and smooth trajectories reflecting experimental progression. It further supports controlled synthetic scattering image generation across diverse structural states. When deployed without retraining, the model organizes time-resolved film formation experiments at two synchrotron facilities into interpretable latent structures. Benchmarking against DINOv3 (ViT-7B), a general-purpose vision foundation model, demonstrates that domain-specific training yields more interpretable latent organization for scattering data. Both workflows are integrated within Latent Space Explorer, a component of the MLExchange platform, supporting interactive structural exploration across archived datasets and live experiments.

Unveiling interfaces at sub-nanometer scales is essential for advancing the understanding of complex chemical transformations. However, characterizing solid-liquid interfaces with high dimensional sensitivity and temporal resolution remains challenging, due to their dynamic nature and inaccessibility by conventional probes. Here we present an approach, Pattern-enhanced Resonant Soft X-ray Scattering, to overcome the challenges. Rooted in a "sample-as-optics" philosophy, this technique utilizes precisely engineered line-grating nanopatterns to modulate near-field X-ray illumination, coherently enhancing scattering signals from the line-gratings. We implement the method using Ni line-grating nanopatterns in electrochemical water oxidation. The periodic nanostructures serve as diffractive optical elements to reveal the Ni oxidation gradients and structural dynamics at the electrode-electrolyte interfaces. Finite-element simulations corroborate the observed trends by modeling variations in compositions and structures during electrocatalysis. Through integrating advanced sample design with coherent wave nature of soft X-rays, our approach opens accessible pathways to operando exploring chemical evolution and sub-nanometer dimensional variations simultaneously in electrochemical systems. This non-destructive method is efficient and element-specific, making it valuable for probing chemical and dimensional dynamics with appropriate modeling.

Vapor-phase infiltration (VPI) of inorganic materials in polymers is increasingly becoming popular for synthesizing various functional hybrid materials. While AlO x infiltration using trimethylaluminum (TMA) has been extensively studied, the mechanism of diethylzinc (DEZ)-based ZnO x infiltration, especially one that is initiated by AlO x priming, has not received much attention because highly reactive hydroxyl groups generated by AlO x -priming are expected to dominate the initial binding of DEZ, thus enabling the overall ZnO x VPI. Here, we interrogate the ZnO x infiltration mechanism in AlO x -primed poly(methyl methacrylate) (PMMA) in comparison to the control AlO x -only infiltration by utilizing a suite of complementary characterizations, including quartz crystal microbalance mass gain measurement, transmission electron microscopy, infrared reflection-absorption spectroscopy (IRRAS), and synchrotron X-ray absorption spectroscopy (XAS). The multivalent TMA precursor and associated hyperbranched AlO x network can quickly saturate the AlO x infiltration by clogging the polymer-free volume near the top. On the contrary, the ZnO x infiltration using divalent DEZ precursor, once activated via AlO x -priming, can lead to accelerated ZnO x infiltration. With the help of IRRAS, XAS, and density functional theory (DFT) simulations, we uncover that the AlO x -priming enhances the reactivity of neighboring carbonyl groups toward DEZ and opens up simultaneous reaction pathways, leading to accelerated high-fidelity infiltration of ZnO x .

Conjugated polymer thin films offer a unique combination of tunable optoelectronic properties and mechanical flexibility, making them as promising materials for intrinsically stretchable optoelectronic devices. However, achieving both mechanical robustness and high device performance remains a key challenge. Addressing this requires a fundamental understanding of how molecular and mesoscale structures evolve under mechanical strain. Here, we employ a comprehensive suite of X-ray spectroscopy and scattering techniques to investigate the multiscale structural evolution of conjugated polymer thin films during uniaxial deformation. We uncover a two-stage morphological response: an initial stage characterized by polymer chain alignment and rapid crystallite disruption, followed by continued chain orientation accompanied by intrachain torsion at higher strains. These correlative structural adaptations govern key material properties, including stress dissipation, optical absorption, and photovoltaic performance. Our findings establish a mechanistic framework for understanding deformation in semiconducting polymers and provide design principles for developing mechanically robust, high-performance stretchable electronics.

Conjugated polymers functionalized with oligoether (OE)-based side chains are a key class of materials for various organic electronic applications, including transparent electrodes, thermoelectrics, electrochromic displays, and electrochemical transistors. Herein, we report a highly soluble OE-functionalized poly(3,4-ethylenedioxythiophene) (PEDOT) homopolymer, prepared by direct (hetero)arylation polymerization, which allows solution processing to yield films with comparable redox properties to oxidatively polymerized PEDOT. This polymer, PEDOT(OE3), when optimally oxidatively doped, reaches among the highest electrical conductivities of any OE-functionalized polymer and is comparable to more synthetically complex OE-functionalized polymers. X-ray scattering and spectroscopy were utilized to rationalize the transport properties resulting from varying the doping level. Comparison of PEDOT(OE3) to a series of OE-functionalized dioxythiophenes with varying amounts of 3,4-ethylenedioxythiophene units allows for a deeper understanding of structure-property relationships through charge-transport models. Ultimately, PEDOT(OE3) is shown to be a material with exceptional charge-transport properties and is promising for various applications.

Conjugated polymers exhibit a rich microstructure with a degree of order between amorphous and crystalline. The performance of semiconductor devices based on conjugated polymers is strongly influenced by this microstructure yet it is difficult to fully characterize. This work investigates the potential of performing resonant diffraction at the selenium K-edge to reveal new microstructural information about conjugated polymer thin films. By studying the variation of diffraction intensity as the X-ray energy is varied across an absorption edge, resonant diffraction, also known as anomalous scattering, can provide new information about molecular packing within the unit cell. With its absorption edge at 12.66 keV, corresponding to a wavelength of ∼ 1 Å, selenium K-edge measurements allow for peaks corresponding to the smallest crystalline spacings (e.g. π--π stacking) to be studied. Two selenium-containing polymers, namely poly(3-hexylselenophene) (P3HS) and poly[(E)-2,7-bis(2-decyltetradecyl)-4-methyl-9-(5-(2-(5-methylselenophen-2-yl)vinyl)selenophen-2-yl)benzo[lmn][3,8] phenanthroline-1,3,6,8(2H,7H)-tetraone] (PNDI-SVS, a naphthalene diimide and selenophene-vinylene-selenophene-based copolymer) are studied. Comparison is made to measurements performed at the sulfur K-edge by studying the thiophene analog of PNDI-SVS. While less pronounced than at the sulfur K-edge, variations in diffraction intensity and anisotropic diffraction at the selenium K-edge are observed, demonstrating the potential for interrogating π--π stacking peaks that may assist with the refining of structural models.

The morphology of block copolymers (BCPs) critically influences material properties and applications. This work introduces a machine learning (ML)-enabled, high-throughput framework for analyzing grazing incidence small-angle X-ray scattering (GISAXS) data and atomic force microscopy (AFM) images to characterize BCP thin film morphology. A convolutional neural network was trained to classify AFM images by surface features, achieving 97% testing accuracy. Classified images were then analyzed to extract 2D grain size measurements from the samples in a high-throughput manner. ML models were trained to predict domain orientation based on processing parameters such as solvent ratio, additive type, and additive ratio. GISAXS-based properties were predicted with strong performances (R-2 > 0.75), while AFM-based property predictions were less accurate (R-2 < 0.60), likely due to the localized nature of AFM measurements compared to the bulk information captured by GISAXS. Beyond model performance, interpretability was addressed using SHapley Additive exPlanations (SHAP). SHAP analysis revealed that the additive ratio had the largest impact on morphological predictions, where additive provides the BCP chains with increased volume to rearrange into thermodynamically favorable morphologies. This interpretability helps validate model predictions and offers insight into parameter importance. Altogether, the presented framework combining high-throughput characterization and interpretable ML offers an approach to exploring and optimizing BCP thin film morphology across a broad processing landscape.

Despite the technological appeal of polymeric organic mixed ionic/electronic conductors (OMIECs) for diverse applications, a deep understanding of the fundamentals of mixed charge transport in these materials, especially regarding the complex interplay between polymer, ion and solvent structure in determining transport, is lacking. Herein, extensive molecular dynamics (MD) simulations of a model OMIEC representing various electrochemically gated states are reported that reveal charge state-dependent counterion condensation. X-ray diffraction simulations based on the MD data predict a measurable change in the scattering intensity at the counterion absorption edge, indicative of counterion repositioning with charging. We leverage an operando resonant X-ray scattering technique to experimentally corroborate the simulated scattering and report excellent agreement between predicted and experimental data, confirming that counterions preferentially reside in the lamellar mid-plane of crystallites at low doping, and near the polymer backbone at higher doping. Driving forces for ion type-dependent spatial repositioning and implications thereof are discussed.

Line-edge roughness (LER) is a critical source of variability in advanced semiconductor manufacturing, yet its accurate quantification remains challenging with conventional imaging-based techniques such as CD-SEM and AFM, which suffer from systematic biases arising from finite resolution and edge-detection artifacts. This paper evaluates critical dimension small-angle X-ray scattering (CD-SAXS) as a complementary route for quantitative LER metrology via the power spectral density (PSD). A dual-track simulation framework injects identical stochastic roughness profiles into both a CD-SAXS scattering simulation and a CD-SEM Monte Carlo imaging pipeline, enabling direct controlled comparison. Both routes recover the three PSD descriptors (sigma, xi, alpha) with R-2 > 0.99 and no significant systematic bias. Experimental validation on etched silicon line-space structures confirms the agreement between the two metrology routes, establishing CD-SAXS as a viable complement to imaging-based LER metrology at advanced technology nodes.

Isoporous membranes can be fabricated by combining self-assembly with nonsolvent induced phase separation (SNIPS) using an amphiphilic block copolymer like polystyrene-b-poly(4-vinylpyridine) (SV). Poly(4-vinylpyridine) (V) is known to complex with metal salts, which are hypothesized to stabilize solution ordering and preserve structure during casting. We explored how the molar ratio of metal additive to the poly(4-vinylpyridine) block affected the final membrane morphology via scanning electron microscopy (SEM). Dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), and in situ grazing-incidence SAXS were used to track changes in solution ordering and chain conformation as a function of the molar ratio of the additive to the V block. Additives induced aggregation, promoted the formation of more compact conformations in solution, and facilitated micelle ordering onto lattices at optimal ratios. These experimental results were supported by random phase approximation calculations, which helped explain how the thermodynamic order-disorder transition shifts with additive binding strength. Stronger additive-polymer interactions reduced the block copolymer volume fraction required for ordering in solution, allowing ordered domains to form at lower polymer concentrations.

Bulk CsPbBr3 is an emerging semiconductor that has shown unprecedented increase in performance over the last decade for optoelectronic applications. However, further development of devices based on CsPbBr3 is hampered by their poor electrical stability under operation. Migration and accumulation of native ions (Cs+, Pb2+, and Br-) under electric fields has been suggested by many groups to be responsible for the observed device instabilities, although direct experimental evidence of ionic motion during operation has been seldom reported. In our study, ion migration has been probed by grazing incidence x-ray fluorescence (GIXRF) in CsPbBr3 polycrystalline layers grown in vapor phase. Our findings indicate that both Cs and Br experience ionic migration under electric field, suggesting that these ions are responsible for the measured current instability in our devices. In the timescale of a few hours, the ionic drifting rates of mobile Cs and Br under the top electrode were found to be similar, as high as ∼ 20 ppm h−1 V−1 mm. This work paves the way for a better understanding of ion motion issues that play a key role in the optoelectronic properties of CsPbBr3 devices.

Liquid crystal elastomers (LCEs) exhibit reversible shape morphing behavior when cycled above their nematic-to-isotropic transition temperature. During extrusion-based 3D printing, LCE inks are subjected to coupled shear and extensional flows that can be harnessed to spatially control the alignment of their nematic director along prescribed print paths. Here, we combine experiment and modeling to elucidate the effects of ink composition, nozzle geometry, and printing parameters on director alignment. From rheological measurements, we quantify the dimensionless Weissenberg number ( Wi ) for the flow field each ink experiences as a function of printing conditions and demonstrate that Wi is a strong predictor of LCE alignment. We find that director alignment in LCE filaments printed through a tapered nozzle varies radially when Wi < 1, while it is uniform when Wi ≫ 1. Based on COMSOL simulations and in operando X-ray measurements, we show that LCE inks printed through nozzles with an internal hyperbolic geometry exhibit a more uniform director alignment for a given Wi compared to those through tapered nozzles. Concomitantly, the stiffness along the print direction and actuation strain of printed LCEs increases substantially under such conditions. By varying Wi during printing through adjusting the flow rate “on the fly”, LCE architectures with uniform composition, yet locally encoded shape morphing transitions can be realized.

Critical Dimension Small-Angle X-ray Scattering (CD-SAXS) has emerged as a powerful metrology for characterizing nanoscale structures in semiconductor devices, offering sub-nanometer precision and non-destructive probing capabilities. However, the complexity of CD-SAXS data analysis demands robust computational tools to accurately translate scattering data into structural information. Current open-source solutions lack the necessary efficiency, modularity, and accessibility to keep pace with evolving metrology needs. This paper presents cdsaxs, a new open-source Python package designed to address these challenges. cdsaxs features a modular architecture that decouples simulation and fitting components, enabling flexible model integration and optimized performance. The package implements key functionalities for CD-SAXS analysis, including CMA-ES-based optimization, MCMC-driven uncertainty quantification, and correlation analysis. We demonstrate the capabilities of cdsaxs through the implementation and fitting of representative nanostructure models, validating its accuracy against both synthetic and experimental datasets. Performance benchmarks showcase significant improvements in computational speed compared to existing solutions, particularly with GPU acceleration. cdsaxs provides a valuable resource for the CD-SAXS community, offering an efficient, extensible, and accessible platform for advancing nanoscale metrology.

Through this work, we aim to give an overview of what is doable with Small Angles X-ray Scattering (SAXS) in the future of overlay metrology and position its role in the production of 7 nm technologies and below. With a metrology budget below 0.35 nm as foreseen by the International Roadmap for Devices and Systems (IRDS)(1) and the reduction of the components dimensions, current optical metrology techniques Image Based Overlay (IBO) and Diffraction Based Overlay (DBO) targets will lack of representativeness. Probing smaller structures that are closer to the real processed technologies with a sub-nanometric resolution and precision becomes necessary. SAXS metrology tools appear to be promising solutions thanks to the high resolution conferred by X-rays sub-nm wavelength. We will review three different methods for overlay measurement with SAXS. The first method consists of a full reconstruction of the in-depth profile of the measured stack. Although efficient, this method requires the acquisition of a large set of data, which translates as hour-scale measurement times on structures others than High Aspect Ratio (HAR) ones. The two other methods, respectively based on Veldman et al. patent and Zhang et al. publication(2, 3) will also be discussed. These methods present the advantage of exploiting the asymmetrical signature of overlay in the SAXS intensity pattern with a limited modeling and reduced data acquisition time. We tested each method on the same set of samples and will discuss their respective strengths and drawbacks, as well as their potential for industrial metrology control.

Solution-based soft matter self-assembly (SA) promises unique material structures and properties from approaches including additive manufacturing/three-dimensional (3D) printing. The 3D printing of periodically ordered porous functional inorganic materials through SA unfolding during printing remains a major challenge, however, due to the often vastly different ordering kinetics of separate processes at different length scales. Here, we report a "one-pot" direct ink writing process to produce hierarchically porous transition metal nitrides and precursor oxides from block copolymer (BCP) SA. Heat treatment protocols identified in various environments enable mesostructure retention in the final crystalline materials with periodic lattices on three distinct length scales. Moreover, embedded printing enables the first BCP directed mesoporous non-self-supporting helical oxides and nitrides. Resulting nitrides are superconducting, with record nanoconfinement-induced upper critical fields correlated with BCP molar mass and record surface areas for compound superconductors. Results suggest scalable porous functional inorganic material formation approaches for applications including catalysis, sensing, and microelectronics.

The relentless scaling of semiconductor features demands ever-greater precision in roughness characterization. Here, we introduce an analytical SAXS simulation for periodic transmission gratings that models line-edge roughness (LER) by laterally shifting cuboid centers and line-width roughness (LWR) via width modulation of each cuboid in a finite stack. By summing the individual sinc form factors, we derive closed-form diffraction intensities and compute the power spectral density (PSD) directly in Fourier space, bypassing image discretization. A vectorized implementation accelerates PSD extraction by over two orders of magnitude compared to binary-FFT methods, while accurately recovering the roughness parameters: root mean square $\sigma$, correlation length $\xi$, and Hurst exponent $\alpha$. This framework offers a rapid, non-destructive route to high-fidelity roughness metrology for next-generation lithographic structures.

The backbone conformation of conjugated polymers (CPs) is essential to their performance in electronic applications. Contrast-variation small-angle neutron scattering (CV-SANS) techniques were used to assess the CP's backbone conformation, which relies on synthesis of deuterated polymers. Such a technique has been proven mature and effective. One drawback is that deuteration labeling might subtly alter polymer's physical properties due to structural modifications. To address these challenges, we introduce a novel approach utilizing tender X-ray scattering near the sulfur K-edge to distinctly evaluate the backbone versus whole chain conformation for a low-bandgap donor-acceptor CP, poly-[(5,6-difluoro- 2,1,3-benzothiadiazol-4,7-diyl)-alt-(3,3‴-dialkyl-2,2';5',2″;5″,2‴-quaterthiophen-5,5‴-diyl)] (PffBT4T). For PffBT4T dissolved in trimethylbenzene (TMB), the sulfur K-edge is identified at approximately 2477 eV using near-edge X-ray absorption fine structure spectroscopy (NEXAFS). Tender X-ray scattering conducted at presulfur K-edge and on-sulfur K-edge at elevated temperatures facilitated the distinction between the backbone and whole chain conformations. The results demonstrate that for highly flexible polymer, the backbone's persistence length could be lower than that of the whole chains, suggesting a more flexible backbone. This rapid, label-free method enhances our ability to characterize CP's backbone conformation efficiently, offering significant implications for the design and optimization of CPs for advanced electronics.

Block copolymer structure direction has been demonstrated as a technique to impart nanostructure and mesoporosity with enhanced properties to a variety of metal oxides for applications including catalysis, energy conversion and storage, as well as superconductivity. Such approaches require polymer-compatible solution synthesis routes toward oxide nanoclusters, which are not generally available for a broad range of functional materials. Here, we report an acetic acid-based sol-gel-derived method for the synthesis of mesoporous ternary strontium titanate with a morphology consistent with alternating gyroid. In-depth structural characterization suggests a periodic gyroidal structure and phase purity of the resultant perovskite. Magnetometry reveals that these normally diamagnetic oxide materials are ferromagnetic at room temperature. This magnetism is significantly enhanced by mild vacuum annealing, suggesting oxygen vacancies as the source of ferromagnetism. Block copolymer self-assembly-directed mesoporous ternary perovskites may provide a rich platform for studying surface and interfacial effects in surface-dominated systems by enhancing normally dilute surface phenomena.

Benzodifuranone (BDF)‐isatin‐based conjugated acceptor copolymers with different stereoelectronic properties are designed, guided by density functional theory calculations. syn ‐ and anti ‐conformations are predicted to depend on both the presence of chlorine substituents as well as on the steric demand of the comonomer. Backbone torsion decreases with the comonomer of the order thiophene (T) > furan (F) > acetylene (A). Six copolymers of BDF‐isatin with T, F, and A are prepared, referred to as H‐BDF‐T, Cl‐BDF‐T, H‐BDF‐F, Cl‐BDF‐F, H‐BDF‐A, and Cl‐BDF‐A. Electrochemically and spectroscopically determined HOMO and LUMO energy levels align qualitatively and confirm a stabilization of the LUMO of the chlorinated copolymers. The thin film microstructures of H‐BDF‐A and Cl‐BDF‐A, having a linear backbone, are characterized by an edge‐on orientation, while the four remaining copolymers with a more curved backbone predominantly orient face‐on. The non‐chlorinated furan copolymer H‐BDF‐F stands out due to its curved yet coplanar backbone, face‐on orientation, high degree of crystallinity, close π−π stacking distance, the highest electrical conductivity of 3 S cm −1 , the best air stability of electrical conductivity among the series, and an appreciably high power factor. These results demonstrate that theory‐guided design allows for optimizing nonhalogenated n‐type copolymers of low synthetic complexity for thermoelectric applications.