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Structural Characterization of Nanomineral Opal-CT via Synchrotron X-ray Techniques and TEM

Nanomineral opal-CT, a naturally occurring precursor to quartz, is formed through diverse geological processes, including weathering, biological precipitation, hydrothermal alteration, and shock metamorphism. Its formation is integral to the genesis of siliceous rocks and influences abiotic and biogenic interactions within natural systems. Recent discoveries of hydrous opal-CT on the surfaces of Mars and the Moon, identified through microanalysis and remote sensing, have intensified research interest in its structural characteristics. This study investigates the local atomic arrangements in natural opal-CT samples exhibiting varying degrees of crystallinity. We employed a synergistic combination of analytical techniques: synchrotron X-ray diffraction (XRD), total X-ray scattering structure factor S(Q) analysis, transmission electron microscopy (TEM), and pair distribution function (PDF) analysis.Our integrated findings reveal that opal-CT primarily consists of interstratified nanodomains of tridymite and cristobalite, characterized by the presence of twins and stacking faults. The S(Q) analysis aids in deconvoluting the XRD patterns, providing more precise peak profiles and enabling a more accurate determination of the degree of structural ordering. TEM imaging, coupled with selected-area electron diffraction (SAED), directly visualizes the nanodomain architecture and associated planar defects. X-ray PDF analysis proves particularly powerful for unveiling detailed information about local structures, defects, and crystallinity within opal-CT. Notably, an increase in the size of ordered domains, along with the emergence and growth of two distinct peaks at 10.01 Å and 11.16 Å in the G(r) plot, correlates with an increased proportion of cristobalite units and enhanced overall crystallinity. The PDF data further indicate the formation of both four- and eight-membered [SiO₄] tetrahedral rings, resulting from twinning and stacking faults within the intergrown tridymite and cristobalite domain. In conclusion, Synchrotron X-ray Techniques and TEM analysis offers unique quantitative insights into the local structural motifs, effective crystalline domain sizes, and the degree of ordering in opal-CT

  • Open access
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Design and Development of Green Materials through Sustainable Synthesis, Characterization, and Recycling

Green materials are gaining rapid global attention as eco-friendly alternatives to conventional plastics and composites due to their renewable origin and reduced environmental impact. In this study, bio-based resources such as natural polymers and plant-derived additives were used to develop sustainable materials through green chemistry routes and consciously avoiding toxic solvents and high-energy processes. The aim was to design functional materials that balance performance with environmental responsibility.

The synthesized materials were systematically characterized using FTIR, TGA, DSC, and SEM to evaluate their chemical bonding, thermal stability, and surface morphology. The findings confirmed that these materials exhibit desirable mechanical and barrier properties, making them promising for biodegradable packaging and low-impact construction. Recycling was assessed through both mechanical and chemical routes, ensuring resource recovery and waste minimization. Notably, after repeated recycling cycles, a slight deterioration in tensile strength, elasticity, and thermal resistance was observed. While these changes remain acceptable for short-term packaging, they may influence long-term structural applications, highlighting the need for tailored end-use considerations.

Overall, this research demonstrates an integrated approach that combines sustainable synthesis, performance assessment, and recycling strategies. By addressing both functionality and circularity, it offers a practical pathway toward reducing plastic pollution and advancing a greener, circular economy.

  • Open access
  • 1 Read
Synthesis, Characterization, and applications of Silver Nanoparticles (Ag-NPs) as Surface-enhanced Raman Spectroscopy (SERS) substrate

Raman Spectroscopy (RS) has applications in the analysis of various pharmaceutical and food samples. But by using nanoparticles, the plasmonic applications and signal enhancement of RS are enhanced and thus called Surface-enhanced Raman spectroscopy (SERS). Silver nanoparticles (Ag-NPs) are utilized for this purpose because, in contrast to gold nanoparticles (Au-NPs), greater enhancement of signals are seen during utilizing as SERS substrate. The synthesis procedure of Ag-NPs is more cost-effective and requires less labor than Au-NPs when utilizing the chemical reduction method. During the synthesis of Ag-NPs, silver nitrate AgNO3 was reduced by using trisodium citrate Na3C6H5O7 act as both reducing and capping agents. After the characterization of Ag-NPs, the ideal size of Ag-NPs was reported in the range of 25-45 nm. Ideally, the signals were enhanced, and thus, the peaks of spectra were also clarified and obtained with much intensity. Surface-enhanced Raman spectroscopy (SERS) significantly enhances the capabilities of conventional Raman spectroscopy (RS) for analyzing pharmaceutical and food samples through plasmonic signal amplification using nanoparticles. Silver nanoparticles (Ag-NPs) are particularly advantageous as SERS substrates compared to gold nanoparticles (Au-NPs), offering greater signal enhancement. Furthermore, Ag-NP synthesis via the chemical reduction method is more cost-effective and less labor-intensive than Au-NP synthesis. In this study, Ag-NPs were synthesized by reducing silver nitrate (AgNO₃) with trisodium citrate (Na₃C₆H₅O₇), which acts as both a reducing and capping agent. Characterization revealed an optimal Ag-NP size range of 25–45 nm. This optimized substrate yielded significantly enhanced SERS signals, resulting in clearer and more intense spectral peaks.

  • Open access
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Regulation of the rate of biocorrosion and cytotoxicity of magnesium alloys by atomic layer deposition of oxide nanocoatings using

Magnesium and its alloys are materials that show great promise for use in bioresorbable implants, due to their unique mechanical properties and biocompatibility. However, their widespread use is limited due to active biocorrosion, which results in the release of excess magnesium ions and gaseous hydrogen, as well as premature loss of the mechanical properties. The solution to this problem is to control of biodegradation rate using nanocoatings.

The present study investigated the regulation of biocorrosion and biocompatibility of the MA2-1pch magnesium alloy using Al2O3 and TiO2 nanocoatings applied by atomic layer deposition (ALD). Coatings with a thickness ranging from 20 to 100 nanometres were synthesised at temperatures between 100 and 300°C. Trimethylaluminium was used for Al2O3, while titanium tetrachloride (TiCl4) or titanium tetraisopropoxide (TTIP) was used for TiO2.

It was determined through scanning electron microscopy (SEM) that the coatings exhibited high continuity and uniformity. The Al2O3 and TiO2-TTIP coatings are amorphous, while TiO2-TiCl4 consists of crystalline grains with an anatase structure. X-ray photoelectron spectroscopy confirmed the absence of magnesium and zinc on the surface, thereby indicating the conformality of the coatings.

The study of biocorrosion was conducted by measuring the pH, hydrogen evolution, and sample mass loss in Ringer's physiological, phosphate-buffered saline, and simulated body fluid solutions. Amorphous coatings have been demonstrated to reduce biocorrosion with increasing thickness. In contrast, minimal corrosion was observed at thickness of 40 nm for crystalline TiO2.

The evaluation of biocompatibility was conducted through the analysis of the MG-63 osteoblast-like cells, utilising both SEM and fluorescence microscopy. The cytotoxic effect of excess magnesium ions and the effective protection afforded by the Al2O3 coating were confirmed using the MTT test. TiO2-TTIP and Al2O3 samples did not manifest any significant signs of toxicity.

  • Open access
  • 6 Reads
Amino-Functionalized MWCNT/Ecoflex Nanocomposites for Stimuli-Responsive Soft Robotic Actuation and Interfaces

Soft polymer–nanotube composites are of growing interest for robotic and biomedical systems that require flexibility, conductivity, and adaptability. In this work, Ecoflex silicone elastomers were combined with commercially available amino-functionalized multi-walled carbon nanotubes to develop conductive and mechanically resilient nanocomposites. The amino groups are expected to enhance compatibility with the polymer, facilitating better dispersion and the formation of conductive pathways. Electrical conductivity will be modeled and measured across CNT concentrations to map percolation, while the composite’s thermal response will be experimentally characterized via Joule (self-)heating and external heating, recording ΔT–power and resistance–temperature (TCR) curves. Mechanical testing and cyclic actuation studies will assess flexibility and durability. Stimuli responsiveness will be evaluated under three inputs: (i) mechanical/pneumatic loading for strain and contact sensing in bending actuators; (ii) electrical input for on-demand thermal modulation and defogging; and (iii) thermal/photothermal input to characterize the resistance–temperature response and recovery. Preliminary trials indicate that conductivity remains limited at low CNT contents, highlighting the importance of optimizing dispersion and curing strategies. Early actuator prototypes exhibited pneumatic bending and measurable resistance variation under deformation, supporting integrated actuation–sensing. Overall, Ecoflex/amino-MWCNT composites show promise as a scalable, tunable platform for stimuli-responsive soft materials, bridging processing, percolation, and function and enabling applications in soft robotics, rehabilitation devices, and wearable adaptive systems.

  • Open access
  • 3 Reads
Determination the material properties of twill-woven glass fabric polymer composite using experimental modal analysis and numerical technique
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The paper considers a non-destructive method for determining the properties of composite layered materials made of twill-woven glass fabric. A combined numericalexperimental method is used to determine the elastic characteristics of a composite monolayer. The method combines the results of experimental tests and numerical modeling methods using optimization techniques. At the first stage, the method for determining the properties is tested in a virtual experiment to determine the influence of the elastic characteristics of the material that do not affect the frequency response. The adequacy of the approximation equations and the influence of elastic constants on the frequency response are evaluated using Analysis of Variance (ANOVA). Using the results obtained, the properties of the elastic characteristics of composite layered plates made of twill-woven glass fabric using vacuum infusion are determined. To confirm the properties obtained from the dynamic calculation, a series of static tensile measurements of the samples was carried out. The results show that the method allows the elastic properties of the material to be determined with a deviation of about 5% compared to static tests, which is negligible compared to the advantages of the experimental modal analysis method. The technique demonstrates high accuracy and applicability for non-destructive determination of material properties in engineering practice.

  • Open access
  • 2 Reads
Electronic structure and Fermi surfaces of WTe2 Weyl semimetal with strong electron correlations

Quantum material WTe2 is a nearly compensated type-II Weyl semimetal which we investigate using first-principles theoretical calculations taking into account strong electron correlations. The electronic structure is calculated within DFT+U+SOC method, the value of parameter U for W-5d states is resolved from perturbation theory, we calculated it to be 3 eV for the orthorhombic Td-WTe2 structure. In the band structure, we identify two small hole pockets and two larger almost degenerate electron pockets along the Г-X high-symmetry direction. The valence band consists of the W-5d and Te-5p electronic states and the conduction band mostly contains W-5d states. In the band structure we also find two pairs of Weyl nodes and calculate their coordinates in momentum space, both of which lay in kz=0 plane of the Brillouin zone. We also model Fermi surfaces and calculate their maximal cross-section area from DFT+U with the calculated and larger values of U. In the Brillouin zone there are two electron and two closed hole surfaces that correspond to small pockets in the band structure of the compound. There is also an even smaller ellipsoid-like surface around high-symmetry point Г which is very sensitive to the value of U in the calculation. These Fermi surfaces were compared with experimental measurements of Shubnikov-de-Haas oscillations and were found in good agreement with each other. From the quantum oscillations, we also observe non-trivial Berry phase and combined with our theoretical studies we conclude that Weyl points are located inside hole pockets [1]. This research was supported by Russian Science Foundation within project No. 24-72-00168.

  1. B.M. Fominykh, A.N. Perevalova, S.T. Baidak, A.V. Lukoyanov, S.V. Naumov, E.B. Marchenkova, V.V. Marchenkov, J. Alloys Compd. 1039, 182966 (2025).
  • Open access
  • 5 Reads
The influence of the titanium dioxide surface modification on the selected physicochemical and biological characteristics of the biopolymer foams.

This study investigates the impact of titanium dioxide surface modification, applied by atomic layer deposition, on the structure and selected physicochemical and biological properties of biopolymer foams. Porous foams were fabricated using freeze-drying of tailored polymer blends, followed by atomic layer deposition deposition of titanium dioxide layers. The surface modification aimed to enhance the several important characteristics of the material - it's surface properties like stability in biological medium, internal structure and architecture, as well as antibacterial performance, which are critical for applications in regenerative medicine on in general biomedical field. Comprehensive characterization included infrared spectroscopy, electron microscopy and X-ray microtomography. The results demonstrate that the thickness and uniformity of TiO₂ coatings can be precisely tuned by adjusting the number of ALD cycles, yielding homogeneous coverage without compromising the open cellular structure or pore connectivity of the foams. The study confirms that atomic layer deposition can be an effective method for the controlled functionalization of biopolymer foams, offering new possibilities for developing advanced biomaterials with tailored surface properties and enhanced performance in biomedical applications. This study was financed through the Norwegian Financial Mechanism "Norway Grants" via the National Centre for Research and Development in Poland under the Programme SGS 2020, grant agreement no. NOR/SGS/engiSCAF/0293/2020-00.

  • Open access
  • 5 Reads
Tailoring wettability and photocatalytic properties of NiO nanosystems fabricated by plasma-assisted vapor deposition

Thin films and nanomaterials of p-type nickel(II) oxide are attractive candidates for a plethora of technological end-uses, among which heterogeneous (photo)catalysts for various applications and hydrophobic coatings for protection against corrosion, yielding also anti-fouling, self-cleaning, and frost prevention properties [1,2].

In this work, phase-pure NiO supported nanostructures were fabricated via an original plasma assisted-chemical vapor deposition (PA-CVD) on glassy substrates at temperatures of 100°C, the lowest ever reported for similar processes, starting from a second-generation precursor, Ni(tfa)2TMEDA (Htfa = 1,1,1-trifluoro-2,4-pentanedione; TMEDA = N,N,N’,N’-tetramethylethylenediamine) [3]. Variations of the sole process duration from 10 to 90 minutes allowed to modulate the system morphology, and, in particular, grain dimensions and deposit thickness. The control of the latter enabled to tailor the ultimate functional performances in terms of wettability and photocatalytic degradation of aqueous diclofenac {DCF = 2-[2-(2,6-dichloroanilino)phenyl]acetic acid}, a recalcitrant pharmaceutical pollutant. Material behavior is discussed in relation to material structure, composition and morphology, investigated based on a comprehensive characterization performed by complementary analytical tools. The present outcomes open the door to the fabrication of NiO nanostructures with modular features even on thermally sensitive substrates for a variety of functional applications.

[1] D. Barreca, E. Scattolin, C. Maccato, A. Gasparotto, L. Signorin, N. El Habra, A. Šuligoj, U. Lavrenčič Štangar, G.A. Rizzi, Chem. Commun., 2025, 61, 2945.

[2] D. Barreca C. Maccato, A. Gasparotto, G.A. Rizzi, Surf. Sci. Spectra, 2025, 32, 024005.

[3] M. Benedet, D. Barreca, E. Fois, R. Seraglia, G. Tabacchi, M. Roverso, G. Pagot, C. Invernizzi, A. Gasparotto, A.A. Heidecker, A. Pöthig, E. Callone, S. Dirè, S. Bogialli, V. Di Noto, and C. Maccato, Dalton Trans., 2023, 52, 10677.

  • Open access
  • 4 Reads
Synthesis and Characterization of Dual-Responsive Hydrogels for Biomedical Use

This study reports the synthesis and characterization of dual-responsive hydrogels based on polyethylene glycol dimethacrylate (PEGDMA), incorporating N-vinylcaprolactam (NVCL) and Eudragit S100. The formulations (HNE1–HNE5) combine three components: PEGDMA as the hydrogel base ('H'), NVCL ('N') for thermo-responsiveness, and Eudragit S100 ('E') for pH sensitivity. Photopolymerization was initiated using Irgacure 2959. The hydrogels were evaluated for their swelling behaviour, gel fraction, wettability, thermal transitions, and chemical structure. Swelling studies in simulated gastric (pH 1.2) and intestinal (pH 7.4) fluids confirmed the hydrogels’ pH-responsiveness, with maximum swelling occurring at pH 7.4. Among the formulations, HNE1 (550) and HNE3 (750) showed the highest swelling (~90%), highlighting the impact of PEGDMA molecular weight and formulation composition. In contrast, swelling was significantly reduced under acidic conditions (e.g., 27.29% for HNE1 550), consistent with the pH-triggered solubility behaviour of Eudragit S100. Gel fraction values ranged from 70.1% to 99.4%, indicating high crosslinking efficiency across the formulations. Notably, HNE3 (550) and HNE4 (550) exhibited gel fractions above 99% at pH 1.2, demonstrating strong network stability even in acidic conditions. Contact angle measurements revealed moderate hydrophilicity, with values decreasing over time—for example, HNE1 (550) dropped from 74.1° to 50.6° within 10 seconds—indicating dynamic wetting behaviour favourable for drug release. Attenuated Total Reflectance–Fourier Transform Infrared Spectroscopy (ATR-FTIR) confirmed the successful incorporation of monomers, with characteristic peaks such as C=O stretching around 1720 cm⁻¹ and minor residual vinyl peaks, indicating mostly complete photopolymerization. Preliminary Differential Scanning Calorimetry (DSC) analysis revealed glass transition temperatures between –44.5°C and –37.75°C for HNE (750) samples, suggesting polymer chain mobility at physiological temperatures and correlating with the observed swelling behaviour. Further DSC comparisons are currently underway for HNE (550) formulations. These results demonstrate that the formulated hydrogels exhibit tunable pH- and temperature-responsive properties, making them promising candidates for site-specific drug delivery within the gastrointestinal tract.

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