X-ray Analysis Research Articles

Accelerated High-Temperature Oxidation Behavior of Ferritic Stainless Steel under Air / H2+H2O Dual Atmosphere

Abstract Improvement in durability is one of the important subjects for utilizing solid oxide electrolyzer cell (SOEC) systems widely. In SOEC stacks, separators are exposed to complexed dual atmosphere (i.e. hydrogen - steam mixed gases and oxygen rich air are on each side). In this study, the degradation phenomena of separator materials (SUS430, ZMG232G10, Crofer22APU) in SOEC dual atmosphere were investigated. The samples were exposed in SOEC dual and simple atmospheres at 700°C for 500 h. Then, their cross sections were analyzed by X-ray diffraction and scanning electron microscopy/energy-dispersive X-ray analysis. The degradation mechanisms of the separator materials in the SOEC stack operating conditions were discussed. ZMG232G10 and Crofer22APU with high Cr content showed thin oxide layer under both the dual or single atmosphere, while SUS430 with low Cr content showed significant oxidation in the H2-steam atmosphere and on the air side under the dual atmosphere condition. The significant oxidation on the air side of the dual atmosphere of SUS430 observed in this study is a unique phenomenon under the dual atmosphere condition and not observed in a single air atmosphere.

X-ray Characterizations of Exfoliated MoS2 Produced by Microwave-Assisted Liquid-Phase Exfoliation

An X-ray analysis of exfoliated MoS2, produced by means of microwave-assisted liquid-phase exfoliation (LPE) from bulk powder in 1-methyl-2-pyrrolidone (NMP) or acetonitrile (ACN) + 1-methyl-2-pyrrolidone (NMP) solvents, has revealed distinct structural differences between the bulk powder and the microwave-exfoliated samples. Specifically, we performed X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) measurements to identify the elements of our exfoliated sample deposited on a Si substrate by drop-casting, as well as their chemical state and its structural crystalline phase. In the exfoliated sample, the peaks pattern only partially resemble the theoretical Miller indices for MoS2. In contrast, the bulk powder’s spectrum shows the characteristic peaks of the 2H polytype of MoS2, but with some broadening. Notable is the retention of partial crystallinity in the post-exfoliation phases, specifically in the normal-to-plane orientation, thus demonstrating the effectiveness of microwave-assisted techniques in producing 2D MoS2 and attaining desirable properties for the material. XPS measurements confirm the success of the exfoliation procedure and that the exfoliated sample retains its original structure. The exfoliation process has been optimized to maintain the structural integrity of MoS2 while enhancing its surface area and electrochemical performance, thereby making it a promising material for advanced electronic and optoelectronic applications ranging from energy storage to sensing devices under ambient conditions.

Leveraging Machine Learning for Advanced Nanoscale X-ray Analysis: Unmixing Multicomponent Signals and Enhancing Chemical Quantification.

Energy dispersive X-ray (EDX) spectroscopy in the transmission electron microscope is a key tool for nanomaterials analysis, providing a direct link between spatial and chemical information. However, using it for precisely determining chemical compositions presents challenges of noisy data from low X-ray yields and mixed signals from phases that overlap along the electron beam trajectory. Here, we introduce a novel method, non-negative matrix factorization based pan-sharpening (PSNMF), to address these limitations. Leveraging the Poisson nature of EDX spectral noise and binning operations, PSNMF retrieves high-quality phase spectral and spatial signatures via consecutive factorizations. After validating PSNMF with synthetic data sets of different noise levels, we illustrate its effectiveness on two distinct experimental cases: a nanomineralogical lamella, and supported catalytic nanoparticles. Not only does PSNMF obtain accurate phase signatures, but data sets reconstructed from the outputs have demonstrably lower noise and better fidelity than from the benchmark denoising method of principle component analysis.

Harnessing the power of Neobacillus niacini AUMC-B524 for silver oxide nanoparticle synthesis: optimization, characterization, and bioactivity exploration

BackgroundBiotechnology provides a cost-effective way to produce nanomaterials such as silver oxide nanoparticles (Ag2ONPs), which have emerged as versatile entities with diverse applications. This study investigated the ability of endophytic bacteria to biosynthesize Ag2ONPs.ResultsA novel endophytic bacterial strain, Neobacillus niacini AUMC-B524, was isolated from Lycium shawii Roem. & Schult leaves and used to synthesize Ag2ONPS extracellularly. Plackett–Burman design and response surface approach was carried out to optimize the biosynthesis of Ag2ONPs (Bio-Ag2ONPs). Comprehensive characterization techniques, including UV–vis spectral analysis, Fourier transform infrared spectroscopy, transmission electron microscopy, X-ray diffraction, dynamic light scattering analysis, Raman microscopy, and energy dispersive X-ray analysis, confirmed the precise composition of the Ag2ONPS. Bio-Ag2ONPs were effective against multidrug-resistant wound pathogens, with minimum inhibitory concentrations (1–25 µg mL−1). Notably, Bio-Ag2ONPs demonstrated no cytotoxic effects on human skin fibroblasts (HSF) in vitro, while effectively suppressing the proliferation of human epidermoid skin carcinoma (A-431) cells, inducing apoptosis and modulating the key apoptotic genes including Bcl-2 associated X protein (Bax), B-cell lymphoma 2 (Bcl-2), Caspase-3 (Cas-3), and guardian of the genome (P53).ConclusionsThese findings highlight the therapeutic potential of Bio-Ag2ONPs synthesized by endophytic N. niacini AUMC-B524, underscoring their antibacterial efficacy, anticancer activity, and biocompatibility, paving the way for novel therapeutic strategies.

Chemical Separation of Copper from the Printed Circuit Board of Dead Electronic Gadget Cell Phone Set (Samsung J-2)

The increasing popularity of electronic devices among the public has increased electronic waste (e-waste). Most electronic devices become obsolescent after their use and generate hazardous chemicals if not disposed properly. The conducting networks in all electronic gadgets are made up of Copper (Cu) that can be retrieved by the chemical segregated method. In this experiment, a hydrometallurgical technique was used as acid leaching, selective recovery of Cu from the leachate using the group separation methods and measured the Cu metal separated from the acid leach. 5.05 g CuO is extracted which is equivalent to 4.03 g of Cu from the Samsung J-2 cell phone having an initial weight of 18.33 g PCBs. Atomic Absorption Spectroscopy (AAS) and Energy Dispersed X-ray analysis (EDX) techniques are used for the characterization of the extract. The recovery of Cu from this technique is about 93 % of the PCB board of Samsung J-2 mobile set.

Synthesis and Biochemical Evaluation of Ethanoanthracenes and Related Compounds: Antiproliferative and Pro-Apoptotic Effects in Chronic Lymphocytic Leukemia (CLL)

Chronic lymphocytic leukemia (CLL) is a malignancy of mature B cells, and it is the most frequent form of leukemia diagnosed in Western countries. It is characterized by the proliferation and accumulation of neoplastic B lymphocytes in the blood, lymph nodes, bone marrow and spleen. We report the synthesis and antiproliferative effects of a series of novel ethanoanthracene compounds in CLL cell lines. Structural modifications were achieved via the Diels–Alder reaction of 9-(2-nitrovinyl)anthracene and 3-(anthracen-9-yl)-1-arylprop-2-en-1-ones (anthracene chalcones) with dienophiles, including maleic anhydride and N-substituted maleimides, to afford a series of 9-(E)-(2-nitrovinyl)-9,10-dihydro-9,10-[3,4]epipyrroloanthracene-12,14-diones, 9-(E)-3-oxo-3-phenylprop-1-en-1-yl)-9,10-dihydro-9,10-[3,4]epipyrroloanthracene-12,14-diones and related compounds. Single-crystal X-ray analysis confirmed the structures of the novel ethanoanthracenes 23f, 23h, 24a, 24g, 25f and 27. The products were evaluated in HG-3 and PGA-1 CLL cell lines (representative of poor and good patient prognosis, respectively). The most potent compounds were identified as 20a, 20f, 23a and 25n with IC50 values in the ranges of 0.17–2.69 µM (HG-3) and 0.35–1.97 µM (PGA-1). The pro-apoptotic effects of the potent compounds 20a, 20f, 23a and 25n were demonstrated in CLL cell lines HG-3 (82–95%) and PGA-1 (87–97%) at 10 µM, with low toxicity (12–16%) observed in healthy-donor peripheral blood mononuclear cells (PBMCs) at concentrations representative of the compounds IC50 values for both the HG-3 and PGA-1 CLL cell lines. The antiproliferative effect of the selected compounds, 20a, 20f, 23a and 25n, was mediated through ROS flux with a marked increase in cell viability upon pretreatment with the antioxidant NAC. 25n also demonstrated sub-micromolar activity in the NCI 60 cancer cell line panel, with a mean GI50 value of 0.245 µM. This ethanoanthracene series of compounds offers potential for the further development of lead structures as novel chemotherapeutics to target CLL.

Exploring green environmental composites as hosts for shielding materials using experimental, theoretical and Geant4 simulation methods

Rice straw is considered an agricultural waste harmful to the environment, which is abundant in most parts of the world. From this point, the present study is devoted to preparing new composites of two types of glue based on rice straw as a plentiful, low-cost matrix. Straw glue samples were prepared by mixing 20% wt. of rice straw with 80% wt. of animal glue (RS-An) and polyvinyl acetate (RS-PVAC) at different thicknesses of 1, 2, and 3 cm. The chemical composition of the prepared samples was identified by energy dispersive X-ray analysis and their morphology was examined using a scanning electron microscope. The mechanical test explored that RS-An and RS-PVAC respectively required a stress of 25.2 and 25.5 MPa before reaching the breaking point. γ-ray shielding performance was analyzed and determined at numerous photon energies from 0.059 to 1.408 MeV emitted from five-point γ-rays sources using NaI (Tl). Linear attenuation coefficient was calculated by obtaining the area under the peak of the energy spectrum observed from Genie 2000 software in the presence and absence of the sample. The experimental results of mass attenuation coefficient were compared with theoretical data of XCOM software with relative deviation ranging from 0.10 to 2.99%. Geant4 Monte Carlo simulation code was also employed to validate the experimental results. The relative deviation of XCOM and Geant4 outcomes was 0.09–1.77%, which indicates a good agreement between them. Other radiation shielding parameters such as half value layer (HVL), tenth value layer, and mean free path were calculated in three ways: experimentally, theoretically from the XCOM database, and by simulation using Geant4 code. Additionally, effective atomic number (Zeff), effective atomic number (Neff), equivalent atomic number (Zeq), and buildup factors were evaluated. It was confirmed that the γ-ray shielding properties were further boosted by mixing rice straw with the animal glue compared to the synthetic one.

Pistia stratiotes L. Biochar for Sorptive Removal of Aqueous Inorganic Nitrogen

Biochar has proven effective in the remediation of excess nitrogen from soil and water. Excess nitrogen from agricultural fields ends up in aquatic systems and leads to reduced water quality and the proliferation of invasive species. This study aimed to assess the efficiency of chemically surface-modified biochar produced from invasive Pistia stratiotes L. for the adsorption of inorganic nitrogen (NH4+ and NO3−). Biochar structure was investigated using scanning electron microscopy, energy-dispersive X-ray analysis, X-ray photoelectron spectroscopy, Fourier-transform infrared spectroscopy, and inductively coupled plasma mass spectrometry. The results from adsorption experiments indicate that NH4+ removal was optimal (0.8–1.3 mg N g−1) at near-neutral pH levels (6.0–7.5), while NO3− removal was optimal (0.4–0.8 mg N g−1) under acidic pH conditions (4.8–6.5) using the modified biochar. These findings highlight the significance of solution pH, biochar morphology, and surface chemistry in influencing the adsorption of NH4+ and NO3−. However, further studies are necessary to assess the potential oxidative transformation of NH4+ to NO3− by biochar, which might have contributed to the reduction in NH4+ in the aqueous phase.

Effect of deposition cycle and annealing on the structural, optical, electrical, and photoluminescence properties of SnS films obtained from rapid S-SILAR technique

AbstractIn this paper, we present an optimized procedure for depositing SnS thin films using the rapid S-SILAR technique. We also analyze the effects of deposition cycles and post-deposition annealing on various film properties. XRD analysis indicates the presence of orthorhombic and cubic phases in the films. Energy dispersive X-ray analysis confirms near-optimal stoichiometry. SEM images depict the growth of closely spaced spherical granules. High optical absorption is observed in the mid-visible to NIR region, with the absorption edge shifting towards the NIR region after annealing. The bandgap values range from 1.6 eV to 1.9 eV, which is ideal for photovoltaic applications. PL spectra show three clusters of peaks corresponding to red and green emissions. Hall measurements confirm that both the as-deposited and annealed SnS films exhibit p-type conductivity, with a hole concentration on the order of 1015 cm−3.

Utilizing Marble Wastewater in Cement Pastes and Mortars for Enhanced Physico-Mechanical and Microstructural Properties

This research explored the potential of marble wastewater (MWW) in cement paste and mortar production, addressing water scarcity, sustainable growth, and resource management. It investigated the physico-mechanical properties and microstructure of cement materials incorporated with varying amounts of MWW. In this study, we utilized tap water and MWW for mortar quality testing, focusing on parameters including setting times, water absorption, and mechanical strength. The viability of MWW in concrete formulations was confirmed by its acceptable total dissolved solids and alkalinity levels. A comprehensive experimental program determined that using marble wastewater in place of tap water reduced the quantity of water required for cement consistency and generated slightly higher compressive strengths (2, 3, 4, and 6%) after 28 days of curing. Analytical techniques, including Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy-dispersive X-ray analysis, and X-ray diffraction (XRD), were employed for molecular and microstructural analyses, which revealed that MWW had a significant influence on portlandite development and CSH formation at higher replacement levels. In short, this research highlights the feasibility of using MWW in cement products, contributing to sustainable water resources, and industrial waste management and utilization.

Resolving high-z galaxy cluster properties through joint X-ray and millimeter analysis: Case study of SPT-CLJ0615-5746

We present a joint millimetric and X-ray analysis of hot gas properties in the distant galaxy cluster SPT-CLJ0615-5746 (z = 0.972). Combining Chandra observations with the South Pole Telescope (SPT) and Planck data, we performed radial measurements of thermodynamical quantities up to a characteristic radius of 1.2 R500. We exploited the high angular resolution of Chandra and SPT to map the innermost region of the cluster and the high sensitivity to the larger angular scales of Planck to constrain the outskirts and improve the estimation of the cosmic microwave background and the galactic thermal dust emissions. In addition to maximizing the accuracy of radial temperature measurements, our joint analysis allows us to test the consistency between X-ray and millimetric derivations of thermodynamic quantities via the introduction of a normalization parameter (ηT) between X-ray and millimetric temperature profiles. This approach reveals a substantial high value of the normalization parameter, ηT = 1.45−0.18+0.17, suggesting that the gas halo is aspherical. Assuming hot gas hydrostatic equilibrium within complementary angular sectors that intercept the major and minor elongation of the X-ray image, we infer a halo mass profile that results from an effective compensation of azimuthal variations of gas densities by variations in the ηT parameter. Consistent with earlier integrated X-ray and millimetric measurements, we infer a cluster mass of M500HE = 10.67−0.50+0.62 1014 M⊙.

Ziziphus Nummularia Leaves Extract Mediated CuO Nanostructures for Photocatalytic degradation of Methylene Blue

In this study, Ziziphus nummularia leaves extract was applied for the synthesis of CuO nanostructures. The material was characterized by various techniques such as Infrared (IR) spectroscopy, X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive X-ray (EDX) and scanning electron microscope (SEM) analysis. The characteristic peaks in powder XRD pattern of nanostructured of CuO at 2θ of 32.33, 35.57, 38.71, 46.11, 48.80, 51.50, 58.22, 61.58, and 68.08◦, correspond to (110), (-111), (111), (-112), (-202), (112), (202), (-113), and (220), respectively, match with diffraction patter of standard monoclinic phase of CuO (JCPDS: 01-080-1916). Tauc plot was plotted and band gap energy was calculated, and found to be 2.4eV. The material was tested as photocatalyst for degradation of MB, and worked well at optimum parameters such as dosage of catalyst 25mg, concentration of MB 20.0mgL-1, pH 7 and time 120min. The proposed method worked very well on synthetic solutions with degradation efficiency (%) ≥83.51 and an RSD (%) of ≤4.0.

Evaluation of adhesive properties and enzymatic activity at the hybrid layer of a simplified adhesive loaded with 0.2% Cu and 5% ZnO nanoparticles: a Randomized Clinical Trial and ex vivo analysis.

ObjectiveThe aim of this study was to evaluate the effect of an adhesive loaded with 0.2% cooper (Cu) and 5% zinc oxide (ZnO) nanoparticles (Nps) on its adhesive properties and enzymatic activity at the hybrid layer ex vivo in a randomized clinical model. MethodsFifteen patients participated in this study, and a total of 30 third molars were used. Occlusal cavities (4 × 4 × 2 mm) were made in each tooth, and randomly divided into 2 groups: (i) Experimental group: commercial adhesive loaded with 0.2wt% CuNps and 5wt% ZnONps; and (ii) Control Group: non-loaded commercial adhesive. Teeth were restored with resin composite. Thirty days later, extractions were performed. Extracted teeth were longitudinally sectioned. Nps in powder were characterized by field emission scanning electron microscope (FE-SEM) and energy dispersive X-ray (EDX) analysis. Microtensile bond strength (μTBS), degree of conversion (DC), and nanoleakeage (NL) tests were executed. In situ zymography (Zym) was performed to evaluate the gelatinolytic activity at the hybrid layer. Student's t-test (α = 0.05) was applied for all tests. ResultsμTBS and DC did not show significant differences (p > 0.05) between both groups. However, NL and gelatinolytic activity at the hybrid layer showed significant values (p < 0.05) for experimental group in comparison with control group. ConclusionThe addition of 0.2% CuNps and 5% ZnONps to a universal adhesive decreases NL and gelatinolytic activity at the hybrid layer, without jeopardizing its adhesive properties. SignificanceThis randomized clinical trial with ex vivo analysis demonstrate that a commercial adhesive modified with 0.2wt% Cu and 5wt% ZnO Nps that does not affect its adhesive properties, reducing gelatinolytic activity and nanoleakage at the hybrid layer, which should contribute to an improvement of long term bonding-dentine clinical performance.

The Deposition by Raffaello Sanzio: New analytical insights on old cross sections for the characterisation of pictorial palette

In 2020, 500th anniversary of Raffaello Sanzio death, his Deposition (1507), -the altarpiece known also as the Pala Baglioni, today located at the Borghese Gallery in Rome-has been subjected to conservative revision and preventive conservation project. This included in-depth diagnostic campaigns through most modern non-invasive techniques, together with the analysis of old cross sections from the same Pala. These latters, prepared between 1966 and 1972, preserved in ICR laboratory of chemistry and testing materials archive, have been used to deepen the knowledge of Raffaello painting techniques. The use of such cross sections was fundamental to verify the original pictorial film and restoration re-paintings before the conservation intervention in the same years.In this paper, the results of analytical insights on Raffaello pictorial palette are presented. The information is obtained by the analysis of the old ICR stratigraphic sections, through the use of Scanning Electron Microscope with Energy Dispersive X-Ray analysis (SEM-EDX) and micro-Raman (632.8 nm), while Surface Enhanced Raman Scattering (SERS) analysis through colloidal paste has been tested for the identification of organic lake-pigments present in low concentration and for the successful recognition of copper resinate, whose SERS spectrum is here reported for the first time, according to our knowledge. This combined diagnostic approach has made it possible to recognize the pigments employed in the different pictorial layers, such species in traces and those from organic materials, responding to open questions arising previous non-invasive analyses and highlighting further aspects of the illustrious master refined painting technique.

Super capacitive electrode performance analysis of facile synthesized α-Fe2O3 aerogel and its nanocomposite with in-situ formed polyaniline (α-Fe2O3/PANI)

This paper presents the synthesis of an α-Fe2O3-assisted polyaniline (α-Fe2O3/PANI) nanocomposite using a straightforward two-step process. Initially, α-Fe2O3 aerogels with cratered nanohexagon structures are synthesized through a solution combustion method assisted by noni (Morinda citrifolia) fruit extract. In the second step, these nanohexagons facilitate the preparation of α-Fe2O3/PANI via in-situ chemical oxidative polymerization of anilinium chloride. The structural, optical, and morphological properties were characterized using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy with energy-dispersive X-ray analysis (SEM-EDAX). Electrical conductivity, wettability, and electrochemical properties of the prepared materials were assessed. The results indicate that the 2D cratered α-Fe2O3 aerogel is effectively embedded within PANI, forming a modified nano α-Fe2O3/PANI composite. The composite exhibited altered DC conductivity and electrolyte wettability. After 200 cycles of cyclic voltammetry (CV), the specific capacitance of the nano α-Fe2O3/PANI was determined to be 153 Fg⁻¹ at a scan rate of 10 mVs⁻¹, retaining approximately 90% of its cycle stability. Electrochemical impedance spectroscopy (EIS) revealed significantly lower charge transfer and equivalent series resistance values for the nano α-Fe2O3/PANI electrode compared to the pure α-Fe2O3-based electrode. Galvanostatic charge-discharge (GCD) tests further demonstrated the superior electrochemical performance of the α-Fe2O3/PANI nanocomposite electrode. Therefore, this α-Fe2O3/PANI is an advanced conducting polymeric electrode for electrochemical applications.

An experimental investigation on mechanical characteristics of steel-fiber-reinforced volcanic concrete

Raw materials of concrete are one of the main pollution resources. Sustainable concrete is one of the significant solutions that can be used to reduce carbon emission. This study aims to use volcanic ash (VA) as a supplementary cementitious material (SCM) for producing sustainable concrete. The effects of VA on the properties of steel fiber reinforced concrete (SFRC) are evaluated. The fresh and hardened concrete's characteristics of steel fiber volcanic ash concrete (SFVC) is presented and assessed. Slump test, compressive strength, splitting tensile tests, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), and Fourier transform infrared (FTIR) spectrophotometry are used to investigate the effect of VA concrete performance. Five groups of SFVC were prepared using sixteen different mixes; 0 %, 2.5 %, 5.0 %, and 7.5 % of VA were used as a partial replacement of cement with 0, 0.5,1.0 %, and 1.5 % of steel fiber (SF). The findings demonstrated that concrete sustainability could be improved by employing VA as a partial replacement for cement, resulting in improved mechanical performance with a slight reduction in workability. The optimum mechanical and microstructure properties of SFVC were achieved with the incorporation of 5 % VA instead of cement with 1 % steel fiber, at age 28 days. The increase in compressive strength and tensile strength up to 25 % and 31 %, respectively. The employing of VA as a SCMs material resulted in better ITZ between aggregate and cement mortar and exhibited a dense surface with less pores compared to control mix.

Synthesis and Characterization of High Dielectric Constant Zirconia Nano-Rods for Advanced Sensors and Energy Storage Applications

Abstract This study reports the synthesis of high dielectric constant zirconia oxide (ZrO2) nanorods (NRs) via a co-precipitation method followed by calcination at 700°C for 2 hours. X-ray diffraction (XRD) confirms a mixed-phase composition of orthorhombic and monoclinic structures, while transmission electron microscopy (TEM) reveals distinct nanorods. Energy dispersive X-ray analysis (EDAX) verifies the elemental composition. Photoluminescence (PL) spectroscopy indicates band gap energy of 1.9 eV, aligning better with orthorhombic zirconia. UV-Vis analysis suggests oxygen vacancy defects potentially influencing the optical properties due to the nanorod morphology. Importantly, dielectric studies show a high dielectric constant of 29 at 1 MHz, which is approximately four times higher than commercially available ZrO2.

Sensing diversity in halogen-bonded multi-stimuli responsive materials: Light, pH, magnetism, and electron-rich species

The present study delves into the synthesis and characterization of multi-stimuli responsive polymers, demonstrating their sensitivity towards magnetic field, pH level, light irradiation, and electron-rich species through halogen bonding (XB). Detailed X-ray analyses of two azobenzene derivatives, each incorporating a tetrafluoroiodobenzene group, provided the compelling evidence of engagement of the building blocks in the formation of halogen bonds. Interestingly, the investigation of an ammonium analog, featuring a tetrahalogenoferrate(III) anion, not only showcased a magnetic response even upheld its ability to undergo isomerization under UV irradiation. These functional properties were subsequently harnessed in the form of multi-responsive compounds through the random quaternization of poly(2-(N,N-dimethylamino) ethyl methacrylate) (PDMAEMA), and by employing varying proportions of XB-donor dye (8, 11, 15, 21, and 43 %) followed by magnetic anion exchange. Leveraging the presence of free ternary amino groups and diazobenzene moieties, the resulting polymers demonstrated pronounced sensitivity towards a variation of pH and UV light stimuli, while a careful modulation of magnetic susceptibility was found to be directly proportional to the degree of quaternization. An NMR titration, conducted using a synthetic intermediate, revealed the formation of I⋯Cl‾ interactions in the solution state, thereby underscoring the materials' sensitivity to electron-rich species. Moreover, the electron microscopic analysis displayed an alteration in morphology upon the application of a magnetic field and UV irradiation. Thus, the presented strategic framework offers an avenue for the development of multi-stimuli responsive materials for remotely controlled smart devices to act in response to a diverse set of four stimuli, and heralding a significant advancement in the realm of responsive material design.

Functionalization of a [2]Catenane with Donor-Acceptor Chromophores Using a Metal Template and Click Reactions.

Synthesizing molecules with significant topological features, such as catenanes, tailored with specific groups to confer desired functionality, is essential for investigating various properties arising from the entanglement due to mechanical bonds. This investigation can pave the way for uncovering novel functional materials employing mechanically interlocked molecules (MIMs). In this direction, we have synthesized ap-donor (D) andp-acceptor (A) functionalized [2]catenane using a non-labile Co(III) metal ion as a template with pyridine-diamide templating center and utilizing click reaction for ring-closing. The donor group is a fluorene derivative, and the acceptor is a benzophenazine derivative, commonly employed in synthesizing conjugated polymers for various optoelectronic devices. Synthetically, the acceptor group was introduced into a macrocycle with a pyridine diamide unit. It was then threaded with a ligand having alkyne terminals to obtain the desired [2]pseudorotaxane utilizing cobalt ion as a template. Ring-closing was then performed with a di-azide functionalized molecule with the donor chromophore. The desired D-A functionalized [2]catenane is obtained after demetalation. All the starting materials, macrocycle, and entangled structures have been characterized by1H-NMR,13C-NMR, and mass spectroscopy. Some of these materials are also characterized by single-crystal X-ray analysis. The photophysical properties are studied by UV-visible and fluorescence spectroscopy.

In Vitro Biocompatibility Assessment of Bioengineered PLA-Hydrogel Core–Shell Scaffolds with Mesenchymal Stromal Cells for Bone Regeneration

Human mesenchymal stromal cells (hMSCs), whether used alone or together with three-dimensional scaffolds, are the best-studied postnatal stem cells in regenerative medicine. In this study, innovative composite scaffolds consisting of a core–shell architecture were seeded with bone-marrow-derived hMSCs (BM-hMSCs) and tested for their biocompatibility and remarkable capacity to promote and support bone regeneration and mineralization. The scaffolds were prepared by grafting three different amounts of gelatin–chitosan (CH) hydrogel into a 3D-printed polylactic acid (PLA) core (PLA-CH), and the mechanical and degradation properties were analyzed. The BM-hMSCs were cultured in the scaffolds with the presence of growth medium (GM) or osteogenic medium (OM) with differentiation stimuli in combination with fetal bovine serum (FBS) or human platelet lysate (hPL). The primary objective was to determine the viability, proliferation, morphology, and spreading capacity of BM-hMSCs within the scaffolds, thereby confirming their biocompatibility. Secondly, the BM-hMSCs were shown to differentiate into osteoblasts and to facilitate scaffold mineralization. This was evinced by a positive Von Kossa result, the modulation of differentiation markers (osteocalcin and osteopontin), an expression of a marker of extracellular matrix remodeling (bone morphogenetic protein-2), and collagen I. The results of the energy-dispersive X-ray analysis (EDS) clearly demonstrate the presence of calcium and phosphorus in the samples that were incubated in OM, in the presence of FBS and hPL, but not in GM. The chemical distribution maps of calcium and phosphorus indicate that these elements are co-localized in the same areas of the sections, demonstrating the formation of hydroxyapatite. In conclusion, our findings show that the combination of BM-hMSCs and PLA-CH, regardless of the amount of hydrogel content, in the presence of differentiation stimuli, can provide a construct with enhanced osteogenicity for clinically relevant bone regeneration.