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Articles published on Wide-angle X-ray Diffraction

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  • Research Article
  • 10.1021/acsapm.6c00411
2.2]Paracyclophane-Based Polyimides of Intrinsic Microporosity for Gas Separation.
  • Apr 10, 2026
  • ACS applied polymer materials
  • Yuting Li + 10 more

Polyimides (PIs) are a significant class of high-performance polymers due to their exceptional thermal, mechanical, and chemical stability. Their combination with polymers of intrinsic microporosity (PIMs) provides access to materials with structural robustness coupled with permanent microporosity. Progress in this area is frequently constrained by the limited availability of difficult-to-prepare and structurally complex dianhydrides. Building on our recent work on [2.2]-paracyclophane (PCP)-based PIMs for gas sorption, we report a series of PCP-polyimide PIMs synthesized from PCP-derived dianhydrides and amino-PCP monomers. The preparation of these dianhydrides enabled a systematic investigation of the monomer structure and connectivity. Two polymer families were obtained: PCP-PIs incorporating pseudo-para and pseudo-meta-PCP units and an ethanoanthracene analogue and a corresponding series of 4,4'-(hexafluoroisopropylidene)-diphthalic anhydride (6FDA)-based PCP polymers. Gas sorption measurements show very good CO2/N2 separation performance with the highest selectivity observed for the meta-PCP-ethanoanthracene system (PCP-PI4, ∼40). Polymers derived entirely from PCP-based dianhydride and bisaniline units in a pseudo-meta configuration also display a capability for strong separation of gases (CO2/N2 = 32.5), underscoring the role of monomer design in tuning the separation properties. Extensive structural and morphological characterizations were performed using multinuclear solid-state NMR, Fourier-transform infrared spectroscopy (FT-IR), wide-angle X-ray diffraction (WAXD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX), while the thermal stability was determined by thermogravimetric analysis (TGA).

  • Research Article
  • 10.1080/00222348.2026.2647855
Effect of Methylene Segment Length on the Brill Transition in Synthesized Polyamide (4, n), n = 6, 8, 10, 12 Series
  • Mar 25, 2026
  • Journal of Macromolecular Science, Part B
  • Anesh Manjaly Poulose + 2 more

Even–even polyamide (4, n) series are synthesized using the interfacial polymerization technique, and the crystalline transitions during heating and cooling are monitored using High-Temperature Wide-angle X-ray Diffraction (HT-WAXD) and High-Temperature Fourier Transform Infrared spectroscopy (HT-FTIR). On heating, polyamide (4, 6) undergoes two crystalline transitions; a low-temperature transition is from a room-temperature (RT) α-phase to a HT α-phase (130 °C) and from a HT α-phase to a γ-phase (230 °C), and the sample melts in the γ-phase. In polyamide (4, 8), the low-temperature transition shifts to higher temperatures (175 °C), and polyamide (4, 10) and (4, 12) samples melt in the HT α-phase before transforming into a γ-phase. On cooling from the melt, polyamide (4, 6) crystallizes in the γ-phase and transforms into a HT α-phase and then to a RT α-phase. Polyamide (4, 8) crystallizes into a HT α-phase and then transitions into the RT α-phase. In polyamide (4, 10), the HT α-phase forms and transforms into a RT α-phase upon cooling. Polyamide (4, 12) crystallizes into the RT α-phase from the melt and does not undergo any transition. The study shows that the –CH2– segment controls the crystalline transitions in polyamides during heating and cooling from the melt.

  • Research Article
  • 10.1021/acssuschemeng.5c13803
Solution Blow Spinning and Molecular Ordering of Regenerated Silk Fibroin: Linking Degumming, Rheology, and CNC-Induced β-Sheet Formation
  • Mar 4, 2026
  • ACS Sustainable Chemistry & Engineering
  • Karthick Raj Selvam + 1 more

Silk fibroin nanofibers are promising biomaterials for tissue engineering, wound healing, and controlled release, owing to their biocompatibility, biodegradability, and mechanical robustness. This study demonstrates a scalable route for producing regenerated silk fibroin (RSF) nanofibers using solution blow spinning (SBS) and establishes how degumming, doping rheology, and cellulose nanocrystal (CNC) reinforcement collectively govern fiber formation and performance. Three degumming methods, boiling water, autoclave treatment, and sodium carbonate, were systematically compared, revealing significant differences in sericin removal efficiency, viscosity-average molecular weight, and secondary structure. RSF was regenerated through lithium bromide dissolution and ethanol-induced phase separation, eliminating the need for dialysis. A 10 wt % RSF dope provided optimal rheological behavior for SBS, while CNC incorporation (0.5–1.5 wt %) increased viscosity moderately and promoted finer jet stretching. Furthermore, CNC addition enhanced molecular ordering, increased the β-sheet content and crystallinity, reduced the fiber diameter, and significantly improved tensile properties. Uniform, bead-free nanofiber mats were obtained, and characterization by scanning electron microscopy, Fourier transform infrared spectroscopy, wide angle X-ray diffraction (WAXD), thermogravimetric analysis, and mechanical testing confirmed CNC-induced structural refinement and reinforcement. Overall, this work establishes SBS as a practical platform for producing structurally tunable RSF/CNC nanofibers and identifies key processing–structure–property relationships relevant to biomedical applications, including future integration of bioactive agents for sustained release.

  • Research Article
  • 10.1016/j.polymertesting.2026.109136
Effect of molecular weight on the molecular chain orientation and strain-induced crystallization behaviors of HNBR under uniaxial stretching
  • Mar 1, 2026
  • Polymer Testing
  • Jiahui Zhang + 6 more

Effect of molecular weight on the molecular chain orientation and strain-induced crystallization behaviors of HNBR under uniaxial stretching

  • Research Article
  • 10.1038/s41428-026-01154-9
Structure-dielectric property correlations in polysiloxane- and DDSQ-based polyimides measured at high frequencies
  • Feb 27, 2026
  • Polymer Journal
  • Erina Yoshida + 7 more

Abstract The development of polymer dielectrics with extremely low dissipation factors ( D f ) in the GHz range is essential for next-generation high-frequency communication and advanced semiconductor technologies. In this study, silicon-containing polyimides (PIs) were systematically synthesized through the incorporation of polysiloxane and double-decker silsesquioxane (DDSQ) units, aiming to elucidate the correlation between molecular structures, higher-order structures, and dielectric properties. Poly(amic acid) precursors were prepared using various tetracarboxylic dianhydrides and silicon-containing diamines, followed by thermal imidization to obtain PI films. Wide-angle X-ray diffraction analysis revealed the formation of periodic layered structures in polysiloxane-containing PIs and the preservation of the cage-like architecture in DDSQ-containing PIs. Dielectric measurements at 10 and 20 GHz demonstrated that the introduction of silicon-containing units reduced the dielectric constant ( D k ) to less than 3.0 because of increased free volume. Notably, the D f values of DDSQ-containing PIs were markedly lower ( ~ 0.002–0.003) than those of polysiloxane-based PIs because of the effective suppression of dipolar orientational polarization originating from the rigid and highly symmetric DDSQ framework. These findings provide an important molecular design strategy for low-loss polymer dielectrics and highlight the potential of DDSQ-based PIs as promising candidates for interlayer insulating materials in high-frequency electronic devices.

  • Research Article
  • 10.1021/acs.macromol.5c03097
Macro-Micro Deformation Mechanisms of Polycarbonate under High-Strain-Rate Compression: Insights from Multiscale Simulation and Microstructural Characterization
  • Feb 26, 2026
  • Macromolecules
  • Hongyu Lu + 6 more

Polycarbonate (PC) is widely used in impact-resistant transparent components due to its excellent toughness and optical properties. However, its mechanical behavior under high strain rate loading remains insufficiently understood, particularly from a microstructural perspective. In this study, the macro-micro deformation mechanisms of PC under high strain rate compression were systematically investigated through an integrated approach combining multiscale simulations and microstructural characterization. Two PC grades with different molecular weights were subjected to dynamic compression experiments using a split Hopkinson pressure bar at high strain rates (4500, 5500, and 7000 s–1) and temperatures of 233, 296, and 353 K. The results reveal pronounced strain rate and temperature dependence in yield stress, yield strain, strain hardening, and unloading strain. Two-dimensional wide-angle X-ray diffraction and polarized Fourier-transform infrared analyzes demonstrate that molecular chain orientation is significantly enhanced under high strain rate loading, with lower molecular weight PC exhibiting more pronounced strain hardening due to easier chain alignment. Molecular dynamics simulations further elucidate that higher molecular weight PC possesses greater conformational stability and resistance to compression. Additionally, the DSGZ model parameters of different PC was calibrated, and accurately predicting the high strain rate compressive response in finite element simulations. The findings provide deep insights into the microstructural origins of the macroscopic mechanical behavior of PC under high-strain-rate compression, offering valuable guidance for material design and engineering applications.

  • Research Article
  • 10.3390/cosmetics13020049
Effective Skin Hydration Using an Ultra-Micro Liquid Crystal Emulsion Containing Pumpkin Seed Oil and Polysaccharides
  • Feb 24, 2026
  • Cosmetics
  • Setinee Chanpirom + 10 more

Polysaccharides extracted from Japanese pumpkin (Cucurbita maxima Duchesne) possess antioxidant activity and moisturizing effects. To meet the demand for natural skincare, this study aims to develop ultra-micro liquid crystal (ULC) emulsions containing pumpkin seed oil (PO) and Japanese pumpkin polysaccharide (PP). The novelty lies in the synergistic triple-action mechanism of the lipid lamellar structure, emollients and humectants, which together achieve superior moisturization. The formulation is varied by different emulsifiers (Emulgade® PL 68/50 and Olivem® 1000), thickening agents (0.3–0.5% w/w of hydroxyethyl cellulose, xanthan gum, or guar gum), and active concentrations of 2.0–4.0% w/w PO and 0.1% w/w PP. Physicochemical characterization was conducted via polarized light microscopy, particle size analysis, and wide-angle X-ray diffraction (WAXD). Stability was assessed through centrifugation and six heating–cooling cycles, while clinical safety and moisturizing efficacy were evaluated in human volunteers using the Corneometer® and Tewameter®. Polarized light microscopy revealed distinct Maltese cross structures, while WAXD confirmed the presence of α-gel and lamellar (Lα) phases. The ULC emulsion containing PO and PP (F9), comprising 4.5% Emulgade® PL 68/50, 0.3% xanthan gum, 2.0% PO, and 0.1% PP, demonstrated excellent physical stability and a particle size of 4.02 ± 0.02 µm. Clinical results demonstrated that F9 was non-irritating and significantly enhanced skin hydration, while reducing transepidermal water loss compared to the baseline (p < 0.05). Although F9 showed the greatest numerical improvement in barrier function, its efficacy was comparable to placebo cream and ULC emulsion containing PO (F6) (p > 0.05). In conclusion, the successful integration of pumpkin-derived actives into a stable ULC system provides a safe and effective approach for advanced moisturizing skincare applications.

  • Research Article
  • 10.1021/acsomega.5c09497
Effect of Nucleating Agent on Crystallization of Poly[(R)‑3-hydroxybutyrate-co-(R)‑3-hydroxyhexanoate
  • Feb 3, 2026
  • ACS omega
  • Masahiro Fujita + 3 more

The effect of pentaerythritol (PERT) as a nucleating agent on the crystallization behavior of poly-[(R)-3-hydroxybutyrate-co-(R)-3-hydroxy-hexannoate] (P-(3HB-co-3HH)) was examined. Isothermal crystallizations with and without PERT at various temperatures were monitored in real time using simultaneous synchrotron radiation wide-angle X-ray diffraction and small-angle X-ray scattering techniques. Heterogeneous nucleation was observed at significantly higher temperatures, where the crystallization of pure P-(3HB-co-3HH) scarcely occurs. The crystal form and morphological parameters of P-(3HB) remained unchanged in the presence of the nucleating agent. However, the induction period for crystallization with PERT was significantly reduced. Structural analysis confirmed that the nucleating agent enhances overall crystallinity due to a higher density of nucleation sites. In addition, the interaction between the molecular chain and the substrate surface was investigated through molecular dynamics (MD) simulations. The MD simulations indicated that the molecular chain tends to interact attractively with the substrate surface, with the carbonyl groups of P-(3HB) oriented toward the hydroxy groups of PERT. These results suggested that the formation of hydrogen bonds, rather than crystalline lattice matching, plays a crucial role in the heterogeneous nucleation of P-(3HB) on PERT.

  • Research Article
  • 10.3390/molecules31020363
Influence of Filler in the Form of Waste Wood Flour and Microcellulose on the Mechanical, Thermal, and Morphological Characteristics of Hierarchical Epoxy Composites
  • Jan 20, 2026
  • Molecules
  • Anna Sienkiewicz + 1 more

In response to growing interest in green additives derived from natural raw materials or post-production waste of natural origin, epoxy compositions containing the additive in the form of waste wood flour and microcellulose were prepared. The research involved the chemical modification of the additive through a two-stage silanization process using 3-aminopropyltriethoxysilane. Followed by filler’s characterization using Fourier Transformed Infrared Spectroscopy (FT-IR) to analyze the modification in chemical structure, Wide Angle X-Ray Diffraction (WAXD) to detect differences in crystal structure, and Scanning Electron Microscopy (SEM) to observe morphological changes. Next, waste oak flour (WF) and microcrystalline cellulose (MCC) were used in unmodified and silanized form (sil-WF and sil-MCC, respectively) to prepare epoxy composites, followed by testing their influence on the mechanical (hardness, tensile strength, flexural strength, compressive strength, and impact strength), thermal, and morphological characteristics of epoxy composites based on Epidian 6. Comparing the effect of modification on the properties of the analyzed additives, it was found that silanization had a larger impact on increasing the interaction of the waste wood flour with the epoxy matrix than silanization of MCC due to a lesser tendency of the sil-WF than the sil-MCC to agglomerate. An enhanced interaction of sil-WF with the polymer resulted in improved mechanical properties. Composite EP/sil-WF (cured epoxy composite based on low-molecular-weight epoxy resin Epidian 6 filled with 5 wt.% of silanized wood flour) was characterized by improved flexural (61.97 MPa) and compressive properties (69.1 MPa) compared to both EP/WF (cured epoxy composite based on low-molecular-weight epoxy resin Epidian 6 filled with 5 wt.% of unmodified wood flour) (42.39 MPa and 61.0 MPa) and the unfilled reference composition (54.55 MPa and 67.4 MPa, respectively). Moreover, compositions containing a cellulosic additive were characterized by better impact properties than the reference composition.

  • Research Article
  • 10.1103/vtzb-dlwt
Growth evolution in calcium carbonate microparticles involving mixed vaterite-aragonite structures
  • Jan 20, 2026
  • Physical Review Research
  • Daniyal Younas + 10 more

Calcium carbonate ( Ca CO 3 ) is a widely occurring mineral that is crucial to many natural and synthetic processes. Ca CO 3 crystallizes in three anhydrous polymorphs and often serves as a model system to study nucleation and growth phenomena. In this article, we employ coherent diffraction imaging coupled with wide-angle x-ray diffraction (CXDI-WAXD) to investigate the three-dimensional (3D) morphology and crystal structure of Ca CO 3 microparticles crystallized under different reaction temperatures. We report particles containing both vaterite and aragonite, which we interpret as an intermediate growth stage between early vaterite and later aragonite formation. The results are based on the density variations observed in the 3D tomographic CXDI images, x-ray diffraction, and focussed ion beam-transmission electron microscopy study of the mixed vaterite-aragonite microparticles. A computational study based on Monte Carlo and molecular dynamics energy minimization was used to identify the small energetic variations between the different crystalline forms of Ca CO 3 . The results presented in this article provide a better understanding of the morphology-structure correlation for Ca CO 3 polymorphs, depicting a transitional stage where both vaterite and aragonite coexist.

  • Research Article
  • 10.1021/acs.macromol.5c02761
Polymorphic Self-Poisoning in the Isothermal Crystallizationof Thermoplastic Polyurethanes
  • Jan 8, 2026
  • Macromolecules
  • Zakarya Baouch + 8 more

Thermoplastic polyurethanes(TPUs) are multiblock copolymers whoseproperties are strongly influenced by the crystallization of the hardsegments (HS). Crystallized HSs based on 4,4′-methylenediphenyldiisocyanate/1,4-butanediol can develop two distinct polymorphs: thethermodynamically stable triclinic Form II or the kinetically favoredparacrystalline Form I, each associated with different mechanicalresponses. While the effect of cooling rate on polymorphic crystallizationhas been studied, the isothermal crystallization kinetics of TPUswith varying HS content are less explored. Here, we investigate theisothermal crystallization of TPUs containing 29–80 wt % HSusing differential scanning calorimetry (DSC), wide-angle X-ray diffraction(WAXD), polarized light optical microscopy (PLOM), and fast scanningcalorimetry (FSC). TPUs with low HS content (29 and 33 wt %) crystallizeexclusively in Form I, and the overall crystallization rate decreasesmonotonically with increasing temperature at low supercooling. Incontrast, TPUs with ≥50 wt % HS display a nonmonotonic temperaturedependence: the overall crystallization rate first increases withsupercooling, then passes through a relative minimum, and rises againat larger supercooling. Structural analyses confirm that this inversionof the temperature coefficient of the crystallization rate originatesfrom the competition between the formation of the two polymorphs.In agreement with previous literature, the rate minimum is tentativelyattributed to polymorphic self-poisoning, in which Form I temporarilyhinders the crystallization of Form II. These findings establish adirect link between polymorphic competition and crystallization kineticsin TPUs, providing new insights into structure formation and strategiesfor tailoring their properties.

  • Research Article
  • 10.1177/08927057261415822
Processing-driven alignment of carbon nanotubes and crystallization control in thermoplastic nanocomposites: In-situ structural and rheological analysis
  • Jan 5, 2026
  • Journal of Thermoplastic Composite Materials
  • Maziyar Sabet

This study investigates the coupled influence of shear-induced carbon nanotube (CNT) alignment and crystallization control in thermoplastic nanocomposites, providing real-time insight into processing–structure–property relationships. Using in-situ wide-angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC), and rotational rheology, we track the evolution of CNT orientation and crystallization kinetics in a high-density polyethylene (HDPE) matrix under controlled shear. A critical shear threshold of ∼100 s −1 is identified, above which CNTs transition from a random to a highly aligned state, with the orientation factor increasing from 0.12 to 0.87. This alignment markedly accelerates crystallization, elevating the onset temperature by up to 8°C and reducing induction time by more than 50%. Aligned CNTs act as efficient nucleating agents and thermal pathways, generating anisotropic lamellar morphologies and enhanced thermal stability. The synergistic effects of CNT concentration and shear intensity yield a quantitative framework linking processing parameters, structural descriptors, and crystallization response. The methodology and correlations established here provide processing-embedded strategies to engineer thermoplastic nanocomposites with tunable thermal, mechanical, and structural performance, directly relevant to extrusion, fiber spinning, and additive manufacturing.

  • Research Article
  • Cite Count Icon 1
  • 10.1107/s2052252525009686
Anisotropic diffraction of materials with fibre symmetry: application to chitin cuticle.
  • Jan 1, 2026
  • IUCrJ
  • Yanhong Wang + 3 more

Understanding the structure-function relationships in anisotropic fibre-symmetric materials is critical for both biological insight and bioinspired design. We present a generalized analytical model for X-ray diffraction intensity from nanofibrillar materials with fibre symmetry, accommodating arbitrary diffraction rings beyond prior axial and equatorial limits. This model integrates 3D orientation, strain heterogeneity and angular misalignment effects, and is validated using wide-angle X-ray diffraction (WAXD) from the Bouligand-structured cuticle of the mantis shrimp (Odontodactylus scyllarus). Using scanning synchrotron WAXD, we extract depth-averaged and sub-lamellar information on 3D fibre orientation and crystalline parameters from 2D scans. Model simulations and experimental fits show accurate reconstruction of the Bouligand texture and reveal spatial gradients in orientation, strain and angular dispersion. By fitting multiple reflections - axial (002), equatorial (110) and intermediate (013) - we improve the robustness in parameter extraction, especially in regions where the Ewald condition is partially satisfied. Our framework enhances the interpretation of WAXD in heterogeneous fibre-based materials and can be embedded into advanced tomographic or machine-learning workflows. This approach is applicable to a broad class of biological and synthetic composites, facilitating high-throughput structural characterization in scenarios where rotation is impractical or impossible.

  • Research Article
  • 10.1016/j.apradiso.2026.112457
Study of mechanical and electrical properties through positron annihilation spectroscopy for different thickness of NBR/PVC/Gamma 600 blend.
  • Jan 1, 2026
  • Applied radiation and isotopes : including data, instrumentation and methods for use in agriculture, industry and medicine
  • Hamdy F M Mohamed + 4 more

Study of mechanical and electrical properties through positron annihilation spectroscopy for different thickness of NBR/PVC/Gamma 600 blend.

  • Research Article
  • Cite Count Icon 2
  • 10.1016/j.indcrop.2025.122483
Coagulation process-dependent long-chain branching in natural rubber: Relationships with strain-induced crystallization and mechanical properties
  • Jan 1, 2026
  • Industrial Crops and Products
  • Changjin Yang + 7 more

The coagulation process significantly influences the molecular architecture of natural rubber (NR), particularly the formation of long-chain branching (LCB), which plays a crucial role in determining its mechanical properties and strain-induced crystallization (SIC) behavior. This study explores how three distinct coagulation methods — acid-induced, natural, and enzymatic coagulation — shape the LCB structure of NR, and further investigates their cascading effects on the crosslinking network, mechanical performance, and SIC characteristics. Through an integrated approach combining Rubber Processing Analyzer measurements, wide-angle X-ray diffraction (WAXD), crosslink network characterization, and mechanical testing, we found that varying coagulation processes yield NR with distinct LCB features, and LCB exhibits a linear correlation with Mooney viscosity during mastication. A higher LCB index in both raw rubber and compounds was observed to facilitate the initiation of SIC at lower strains, thereby enhancing NR’s self-reinforcement effect. Among the samples, enzyme-coagulated NR exhibits the highest LCB index; its tensile strength (31.54 ± 0.46 MPa) and crystallinity (10.01 %) outperform those of acid-coagulated (24.81 ± 0.31 MPa, 9.38 %) and naturally coagulated (23.47 ± 0.56 MPa, 7.87 %) samples. Furthermore, this work clarifies the regulatory role of coagulation processes in NR network evolution and establishes quantitative relationships between crystallization at a strain of 7, tensile performance, and the LCB index of raw rubber and compounds, offering novel insights into NR molecular design. These findings highlight the pivotal role of coagulation methods in tailoring NR’s LCB structure, paving the way for performance optimization in high-demand applications such as tire manufacturing and industrial elastomer production. • Coagulation methods control long-chain branching (LCB) in NR. • Enzyme-coagulated NR shows highest LCB index and mechanical strength. • LCB enhances strain-induced crystallization in NR. • Quantitative correlation between crystallization, tensile behavior, and LCB was established. • Coagulation process tunes NR performance for industrial applications.

  • Research Article
  • 10.5650/jos.ess25238
Mixed State Diagrams of Rice Starch/glycerol/water Ternary Systems.
  • Jan 1, 2026
  • Journal of oleo science
  • Kaya Torii + 8 more

Amorphous rice starch/glycerol/water ternary systems are used in food, cosmetics, and functional materials. In the present study, we investigated the water adsorption ability of crystalline and amorphous rice starches and the mixed state of rice starch/glycerol/water ternary systems. The effect of amorphization on the mixed state was evaluated with thermogravimetric analysis (TGA) and wide-angle X-ray diffraction measurement (XRD). When amorphous rice starch was mixed with water and glycerol (40-80 wt%), the funicular and capillary states were observed: the funicular state is a dry state where solid and liquid form a continuous phase, and the capillary state is a sticky state where only the liquid is the continuous phase. This was attributed to the greater number of free hydroxyl groups in amorphous rice starch, which enhanced its affinity to hydroxyl groups. Amorphous rice starch systems exhibited a water evaporation temperature 14 °C higher than crystalline rice starch systems. Furthermore, when the mixed system contained amorphous rice starch and glycerol, the funicular region was expanded. A glycerol molecule has three hydroxyl groups, which enhance the adhesive force between starch particles and increase viscosity. These findings are useful for designing formulations for various products utilizing mixtures of rice starch and glycerol.

  • Research Article
  • 10.1002/pen.70348
Fatigue Behavior and Multiscale Structural Evolution of Polyamide 66 Industrial Fiber Under Cyclic Loading
  • Dec 27, 2025
  • Polymer Engineering & Science
  • Bohao Li + 5 more

ABSTRACT This study systematically examines the room‐temperature fatigue behavior and microstructural evolution of high‐tenacity (HT) and super‐high‐tenacity (SHT) polyamide 66 (PA 66) industrial fibers under cyclic loading at various stress levels. By integrating multiple characterization techniques, such as wide‐angle x‐ray diffraction (WAXD), small‐angle x‐ray scattering (SAXS), birefringence measurements, and Fourier transform infrared spectroscopy (FTIR), the underlying fatigue mechanisms were elucidated. The SHT fiber demonstrated significantly lower initial and total fatigue strain than the HT fiber under identical stress conditions. The crystalline structure showed no significant changes, including crystallite size, crystalline orientation, and crystallinity in both fibers before and after fatigue testing. In contrast, the amorphous regions underwent substantial reorganization. The amorphous orientation and amorphous thickness of the SHT fiber increased slightly with increasing fatigue stress, which is attributed to the alignment of coil chains under tensile fatigue stress. The molecular chains in the amorphous regions of the HT fiber were more easily extended and oriented, leading to more significant structural changes in its amorphous regions. The fatigue mechanisms of both fibers involved a transition from gauche to trans conformation, and this conformational change was more evident in the HT fiber. Additionally, the HT fiber sustained a lower maximum cyclic stress, which was associated with its lower degree of amorphous orientation. It is demonstrated that developing industrial fibers with a higher degree of amorphous orientation is crucial for enhancing their fatigue resistance.

  • Research Article
  • 10.1021/acsomega.5c10199
Tuning Ferroelectricityin PVDF-TrFE through ThermalTreatment-Dependent Crystal Orientation
  • Dec 25, 2025
  • ACS Omega
  • Li Li + 6 more

The ferroelectric properties of poly­(vinylidene fluoride-co-trifluoroethylene) (PVDF-TrFE) films are critically dependenton its molecular orientation, due to the dipole-electric field matchproblem. This study systematically investigates the impact of therecrystallization temperature and cooling rate on crystal orientationand resultant ferroelectric performance during melt recrystallizationof PVDF-TrFE thin films on mica substrates. The collective analysisof two-dimensional (2D) grazing incidence wide-angle X-ray diffraction(2D-GIWAXD), atomic force microscope (AFM), Fourier transform infrared-grazingincidence reflection absorption spectroscopy (FTIR-GIRAS), and polarization-electricfield (P-E) hysteresis measurement data reveals that recrystallizationat lower temperatures (25 °C) with a faster cooling rate (100°C/min) facilitates the formation of edge-on lamellar structuresand enhanced ferroelectric performance. During the melt recrystallizationof PVDF-TrFE films, mica substrates can promote the formation of moreedge-on lamellae compared to glass or silicon substrates. These findingsprovide an effective approach to modulate the ferroelectric propertiesof PVDF-TrFE thin films from melt on mica substrates.

  • Research Article
  • 10.1177/0021955x251403130
Preparation of low temperature resistant slow rebound polyurethane foams with reduced flammability based on modified graphene oxide supported nanosilica
  • Dec 16, 2025
  • Journal of Cellular Plastics
  • Jing Cao + 4 more

A slow rebound polyurethane foam (SPUF) with enhanced flammability retardancy by incorporating KH-907 modified graphene oxide-supported nano-silica (SiO 2 @GO-KH-907), in conjunction with silicone-modified polyether (Si-APEG) as a low-temperature resistance agent. The structures of SiO 2 @GO-KH-907 were investigated by Fourier transform infrared spectra (FT-IR), wide-angle X-ray diffraction (WAXD) and scanning electron microscope (SEM). Results showed that KH-907 was chemically bonded with GO, and the SiO 2 particles were uniformly dispersed on GO layers. The influence of SiO 2 @GO-KH-907 on the foam’s structural, mechanical, thermal, and flame-retardant properties was systematically investigated. During the foaming process, SiO 2 @GO-KH-907 acted as an efficient cell nucleating agent, reducing the cell size and narrowing size distribution. When the SiO 2 @GO-KH-907 content reached 2%, the foam demonstrated enhanced tensile strength and toughness, along with improved thermal stability and flame retardancy, while maintaining its low-temperature resistance properties. These findings suggest that the incorporation of SiO 2 @GO-KH-907 represents a promising approach for developing multifunctional polyurethane foams with superior performance characteristics.

  • Research Article
  • Cite Count Icon 3
  • 10.3390/molecules30244800
La-Doped ZnO/SBA-15 for Rapid and Recyclable Photodegradation of Rhodamine B Under Visible Light
  • Dec 16, 2025
  • Molecules
  • Ziyang Zhou + 4 more

La-doped ZnO nanoclusters confined within mesoporous SBA-15 were synthesized using an impregnation–calcination method and evaluated for their visible-light-driven photocatalytic degradation of Rhodamine B (RhB). Small-angle X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the preservation of the 2D hexagonal mesostructure of SBA-15 post-loading. In contrast, wide-angle XRD and Fourier-transform infrared spectroscopy (FT-IR) analyses revealed that the incorporated ZnO existed predominantly as highly dispersed amorphous or ultrafine clusters within the mesopores. N2 adsorption–desorption measurements exhibited Type IV isotherms with H1 hysteresis loops. Compared to pristine SBA-15, the specific surface area and pore volume of the composites decreased from 729.35 m2 g−1 to 521.32 m2 g−1 and from 1.09 cm3 g−1 to 0.85 cm3 g−1, respectively, accompanied by an apparent increase in the average pore diameter from 5.99 nm to 6.55 nm, attributed to non-uniform pore occupation. Under visible-light irradiation, the photocatalytic performance was highly dependent on the La doping level. Notably, the 5% La-ZnO/SBA-15 sample exhibited superior activity, achieving over 99% RhB removal within 40 min and demonstrating the highest apparent rate constant (k = 0.1152 min−1), surpassing both undoped ZnO/SBA-15 (k = 0.0467 min−1) and other doping levels. Reusability tests over four consecutive cycles showed a consistent degradation efficiency exceeding 93%, with only a ~7 percentage-point decline, indicating excellent structural stability and recyclability. Radical scavenging experiments identified h+, ·OH, and ·O2− as the primary reactive species. Furthermore, photoluminescence (PL) quenching observed at the optimal 5% La doping level suggested suppressed radiative recombination and enhanced charge carrier separation. Collectively, these results underscore the synergistic effect of La doping and mesoporous confinement in achieving fast, efficient, and recyclable photocatalytic degradation of organic pollutants.

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