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Bone quality around dental endosseous implants is a key factor in implant prognosis. Surface coatings represent an important method to increase osseointegration in oral implantology. Newer titanium alloys such as Ti6Al7Nb are under research in order to replace the commonly used Ti6Al4V, for a better osseointegration, with lower risks. Hydroxyapatite (HA) is the most commonly used coating, but others such as SiO2-TiO2 are under development in search for a better biological response. In this study, screw-type Ti6Al7Nb, Ti6Al7Nb-HA, and Ti6Al7Nb-SiO2-TiO2 implants were placed into the femur of six New Zealand White Rabbits. Three months later, the samples were harvested and examined using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDX). The results showed a better osseointegration of surface coated Ti6Al4Nb implants. No differences could be found between hydroxyapatite and SiO2-TiO2 coatings. These Ti6Al7Nb alloy coatings could be considered in the future for implant manufacturing. [ABSTRACT FROM AUTHOR]

The aim of this study was the synthesis and structural characterization of SiO2–Al2O3 microspheres with SiO2 core and (100 − x)Al2O3·xFe2O3 (x = 0, 5, and 10 mol%) shell. Smooth spherical silica particles of uniform size around 1 μm have been synthesized as core material based on the Stöber method. In order to enhance the specific surface area, the silica particles were coated with a thin nanostructurated shell, about 15 nm, of aluminum and iron oxides (100 − x)Al2O3·xFe2O3 (x = 0, 5, and 10 mol%). The embedding of iron oxide in the covering shell was related to potential applications of these composite biomaterials for contrast enhancement in magnetic resonance imaging (MRI) and at the same time for local treatments of cancer by hyperthermia. The XRD results point out the amorphous structure of the obtained core–shell particles. The TEM images evidence continuous shell coating of silica spherical microparticles and the XPS analysis of the surfaces prove the occurrence of iron oxide on the outermost layer of the microspheres. Both FTIR and XPS results evidence the formation of Al–O–Si linkage proving that Al2O3 and SiO2 are chemically bonded in the investigated core–shell microspheres. Highlights: Amorphous SiO2–Al2O3–Fe2O3 core–shell microspheres of mean diameter under 1.5 μm. Silica core was synthetized using Stöber method. Porous Al2O3–Fe2O3 shell of about 15 nm was nucleated by electrostatic attraction. SiO2–Al2O3–Fe2O3 clay type nanocrystalline layer self-assembled as shell on SiO2 core. Iron ions occur on the outermost layer of the core–shell microspheres. [ABSTRACT FROM AUTHOR]

Structural changes induced by temperature rising in binary silico-bismuthate glasses are investigated by differential thermal analysis. Several exothermic peaks are recorded for all samples. Progressive substitution of Bi2O3 by SiO2 contributes to the structural relaxation of vitreous network and leads to diminishing of the melting temperature, even as SiO2 content reaches 40 mol%. Glass stability is enhanced by addition of silicon dioxide. [ABSTRACT FROM AUTHOR]

A new melt derived glass system consisting of Co 2 O 3 added to 40P 2 O 5 ·25B 2 O 3 ·25CaO·10Na 2 O matrix was investigated in order to evaluate the influence of cobalt ions on the network structure. Multiple techniques, i.e. X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) spectroscopy, Raman spectroscopy and X-ray Photoelectron Spectroscopy (XPS) were used to characterize the local structure, the nature of the chemical bonding and the surface composition of these samples. The XRD measurements proved the vitreous character of samples with 0 and 3 mol% Co 2 O 3 . At higher cobalt oxide content (5, 7 and 10 mol%) the occurrence of a crystalline phase characteristic to Co 2 P 4 O 12 has been observed. The complementary spectroscopic studies (FTIR and Raman) revealed that the incorporation of Co 2 O 3 enhances the network connectivity and thereby the short range order in samples. Depending on their amount, the cobalt ions differently influence the borophosphate network via the tetraborate/triborate and metaphosphate/pyrophosphate ratios. For the sample containing 10 mol% Co 2 O 3 the FTIR analysis indicates absorptions assigned to vibrations in CoO 6 tetrahedra and suggests the presence of six-coordinated cobalt ions in Co 3 + valence state. This study has proven that borophosphate based glasses are able to entrap cobalt ions, are sensitive from structural point of view to the amount of Co 2 O 3 and possess interesting structural peculiarities. [ABSTRACT FROM AUTHOR]

Calcium titanate (CTO) photocatalysts were synthesized using a sol-gel method by adopting a cost-efficient, rapid calcination technique. The CTOs were characterized by X-ray diffractometry, X-ray photoelectron spectroscopy, infrared spectroscopy, nitrogen adsorption, porosimetry measurements, scanning/transmission electron microscopy, and diffuse reflectance spectroscopy. Their photocatalytic activity was assessed through the photocatalytic degradation of phenol, oxalic acid, and chlorophenol under UV light exposure, using a commercial CTO as a reference. The stability of the samples was evaluated using compounds with -OH, -COOH, and -Cl functional groups. Characterization results showed that CTO composites containing anatase, rutile, and brookite titania were obtained. Increasing the calcination temperature led to various crystalline compositions, higher crystallinity, larger primary crystallite sizes, and smaller specific surface areas. The photocatalytic activity of all CTO/TiO 2 composites was superior compared to the commercial CTO we used as a reference. The high photocatalytic activity of the best-performing composites was attributed to their higher specific surface areas and the synergistic effect between the crystal phases. A cost comparison was also made between our unique calcination technique and conventional calcination, and it was found that our method is approximately 35% more cost-effective, while retaining the photocatalytic activity., Competing Interests: The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (© 2024 The Authors.)

New cocrystals of praziquantel with suberic, 3-hydroxybenzoic, benzene-1,2,4,5-tetracarboxylic, trimesic, and 5-hydroxyisophthalic acids were obtained through ball milling experiments. The optimal conditions for the milling process were chosen by changing the solvent volume and the mechanical action time. Supramolecular interactions in the new cocrystals are detailed based on single-crystal X-ray diffraction analysis, confirming the expected formation of hydrogen bonds between the praziquantel carbonyl group and the carboxyl (or hydroxyl) moieties of the coformers. Different structural characterization techniques were performed for all samples, but the praziquantel:suberic acid cocrystal includes a wider range of investigations such as thermal analysis, infrared and X-ray photoelectron spectroscopies, and SEM microscopy. The stability for up to five months was established by keeping it under extreme conditions of temperature and humidity. Solubility studies were carried out for all the new forms disclosed herein and compared with the promising cocrystals previously reported with salicylic, 4-aminosalicylic, vanillic, and oxalic acids. HPLC analyses revealed a higher solubility for most of the new cocrystal forms, as compared to pure praziquantel., Competing Interests: The authors declare no competing financial interest., (© 2024 The Authors. Published by American Chemical Society.)

In this study, bismuth- and iron-embedded carbon xerogels (XG) were obtained using a modified resorcinol formaldehyde sol-gel synthesis method followed by additional enrichment with iron content. Pyrolysis treatment was performed at elevated temperatures under Ar or N 2 atmosphere to obtain nanocomposites with different reduction yields (XGAr or XGN). The interest was focused on investigating the extent to which changes in the pyrolysis atmosphere of these nanocomposites impact the structure, morphology, and electrical properties of the material and consequently affect the electroanalytical performance. The structural and morphological particularities derived from X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) measurements revealed the formation of the nanocomposite phases, mostly metal/oxide components. The achieved performances for the two modified electrodes based on XG treated under Ar or N 2 atmosphere clearly differ, as evidenced by the electroanalytical parameters determined from the detection of heavy metal cations (Pb 2+ ) or the use of the square wave voltammetry (SWV) technique, biomarkers (H 2 O 2 ), or amperometry. By correlating the differences obtained from electroanalytical measurements with those derived from morphological, structural, and surface data, a few utmost important aspects were identified. Pyrolysis under Ar atmosphere favors a significant increase in the α-Fe 2 O 3 amount and H 2 O 2 detection performance (sensitivity of 0.9 A/M and limit of detection of 0.17 μM) in comparison with pyrolysis under N 2 (sensitivity of 0.5 A/M and limit of detection of 0.36 μM), while pyrolysis under N 2 atmosphere leads to an increase in the metallic Bi amount and Pb 2+ detection performance (sensitivity of 8.44 × 10 3 A/M and limit of detection of 33.05 pM) in comparison with pyrolysis under Ar (sensitivity of 6.47·10 3 A/M and limit of detection of 46.37 pM).

The majority of present-day white-light emitting devices (WLEDs) are built upon the use of rare-earth elements, which have a short supply, are expensive and can become extremely toxic. Thus, in this work, we synthesized an eco-friendly, efficient and cheap white-light emitting material (WLEM) based on solid-state histidine-stabilized gold nanoclusters (His-AuNCs), obtained through the lyophilization of microwave-synthesized photoluminescent His-AuNCs. Their morphological and structural characterization was followed by thorough evaluation of their intrinsic solid-state photoluminescence properties via steady-state and time-resolved fluorescence spectroscopy and microscopy, at multiple excitation wavelengths. A white-light emission was observed under UV light excitation due to the two-band broad emission, with maxima at 475 and 520 nm, covering a large area of the visible spectrum. In order to evaluate the purity of the white-light emission we calculated the chromaticity coordinates, at different wavelengths, and displayed them on a CIE (Commision Internationale d'Eclairage) diagram. An excellent value of (0.36, 0.33) was found at 420 nm excitation, which falls within the range of pure white-light emission. Moreover, the His-AuNCs show great photo- and thermo-stability, thus proving their ability to perform as a reliable WLEM with potential use in the development of eco-friendly WLEDs., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)

The most important concept behind using bone scaffolds is the biocompatibility of the material to avoid a local inflammatory response and must have the following properties: osteoinduction, osteoconductivity, angiogenesis, and mechanical support for cell growth. Gold nanoparticles/gold and silver nanoparticles -containing bioactive glasses in biopolymer composites have been used to enhance bone regeneration. These composites were tested in vitro on fibroblast and osteoblast cell lines using MTT tests, immunofluorescence, scanning electron microscopy analysis, and in vivo in an experimental bone defect in Sprague-Dawley rats. Both composites promoted adequate biological effects on human fibroblastic BJ (CRL 2522TM) cell lines and human osteoblastic cells isolated from the human patella in terms of cell proliferation, morphology, migration, and attachment. Most importantly, they did not cause cellular apoptosis and necrosis. According to the histological and immunohistochemical results, both composites were osteoinductive and promoted new bone formation at 60 d. Evidence from this study suggests that the small amount of silver content does not influence negatively the in vitro or in vivo results. In addition, we obtained accurate results proving that the existence of apatite layer and proteins on the surface of the recovered composite, supports the validity of in vitro bioactivity research., (© 2023 IOP Publishing Ltd.)

The widespread use of Ag 3 PO 4 is not surprising when considering its higher photostability compared to other silver-based materials. The present work deals with the facile precipitation method of silver phosphate. The effects of four different phosphate sources (H 3 PO 4 , NaH 2 PO 4 , Na 2 HPO 4 , Na 3 PO 4 ·12 H 2 O) and two different initial concentrations (0.1 M and 0.2 M) were investigated. As the basicity of different phosphate sources influences the purity of Ag 3 PO 4 , different products were obtained. Using H 3 PO 4 did not lead to the formation of Ag 3 PO 4 , while applying NaH 2 PO 4 resulted in Ag 3 PO 4 and a low amount of pyrophosphate. The morphological and structural properties of the obtained samples were studied by X-ray diffractometry, diffuse reflectance spectroscopy, scanning electron microscopy, infrared spectroscopy, and X-ray photoelectron spectroscopy. The photocatalytic activity of the materials and the corresponding reaction kinetics were evaluated by the degradation of methyl orange (MO) under visible light. Their stability was investigated by reusability tests, photoluminescence measurements, and the recharacterization after degradation. The effect of as-deposited Ag nanoparticles was also highlighted on the photostability and the reusability of Ag 3 PO 4 . Although the deposited Ag nanoparticles suppressed the formation of holes and reduced the degradation of methyl orange, they did not reduce the performance of the photocatalyst.

Understanding graphene oxide's stability (or lack thereof) in liquid solvents is critical for fine-tuning the material's characteristics and its potential involvement in future applications. In this work, through the use of structural and surface investigations, the alteration of the structural and edge-surface properties of 2D graphene oxide nanosheets was monitored over a period of eight weeks by involving DLS, zeta potential, XRD, XPS, Raman and FT-IR spectroscopy techniques. The samples were synthesized as an aqueous suspension by an original modified Marcano-Tour method centred on the sono-chemical exfoliation of graphite. Based on the acquired experimental results and the available literature, a phenomenological explanation of the two underlying mechanisms responsible for the meta-stability of graphene oxide aqueous dispersions is proposed. It is based on the cleavage of the carbon bonds in the first 3-4 weeks, while the bonding of oxygen functional groups on the carbon lattice occurs, and the transformation of epoxide and hydroxyl groups into adsorbed water molecules in a process driven by the availability of hydrogen in graphene oxide nanosheets.

The co-crystals formation of etravirine with three carboxylic acids was investigated. New co-crystals of etravirine with adipic acid, benzoic acid, and 4-hydroxybenzoic acid have been synthesized by wet milling of ingredients for 120 min. The novelty of these solid forms was first evidenced by powder X-ray diffraction. Their different morphology was evidenced by SEM microscopy. Spectroscopic analyses (FT-IR, MAS-NMR, and XPS) highlighted the hydrogen bonds between etravirine and co-formers, as a result of the solid-state reaction of the ingredients by wet milling. Thermal analyses pointed out that the milling process caused in co-crystals a reduction in the fusion enthalpy and the melting temperature, compared to the values obtained for etravirine. These co-crystals are stable up to four months on storage under extreme conditions, excepting the co-crystal with benzoic acid which begins to transform into a polymorph of etravirine after 30 days. The UV absorption spectra of the samples tested in three simulated physiological media with pH values of 6, 6.3, and 7 have evidenced the conformation change of etravirine due to hydrogen bonds between etravirine and carboxylic acids., (Copyright © 2021 American Pharmacists Association. Published by Elsevier Inc. All rights reserved.)

Using an ideal biomaterial to treat injured bones can accelerate the healing process and simultaneously exhibit antibacterial properties; thus protecting the patient from bacterial infections. Therefore, the aim of this work was to synthesize composites containing silicate-based bioactive glasses and different types of noble metal structures (i.e., AgI pyramids, AgIAu composites, Au nanocages, Au nanocages with added AgI). Bioactive glass was used as an osteoconductive bone substitute and Ag was used for its antibacterial character, while Au was included to accelerate the formation of new bone. To investigate the synergistic effects in these composites, two syntheses were carried out in two ways: AgIAu composites were added in either one step or AgI pyramids and Au nanocages were added separately. All composites showed good in vitro bioactivity. Transformation of AgI in bioactive glasses into Ag nanoparticles and other silver species resulted in good antibacterial behavior. It was observed that the Ag nanoparticles remained in the Au nanocages, which was also beneficial in terms of antibacterial properties. The presence of Au nanoparticles contributed to the composites achieving high cell viability. The most outstanding result was obtained by the consecutive addition of noble metals into the bioactive glasses, resulting in both a high antibacterial effect and good cell viability.

Atomic-scale description of surfaces and interfaces in core-shell aluminosilicate materials is not fully elucidated, partially due to their amorphous character and complex mechanisms that govern their properties. In this paper, new insights into nanostructured core-shell aluminosilicates have been demonstrated, by using different solid-state NMR methods, i.e 29 Si, 29 Si cross-polarization (CP), 27 Al, 27 Al triple-quantum (3Q), and 1 H- 27 Al heteronuclear correlation (HETCOR) MAS NMR. For this purpose, nanostructured silica core-alumina shell microspheres, undoped and doped with gadolinium ions respectively, obtained by a chemical synthesis based on the Stöber method for the silica core and electrostatic attraction for developing the alumina shell were studied. As a result, a new alumino-silicate layer formation was proved at the interface between silica core, where aluminum diffuses, on small scale, in the silica network, and alumina shell, where silicon ions migrate, on a larger scale, in the alumina network, leading to a stable core-shell structure. Moreover, this process is accompanied by significant local structural changes in the transition zone, particularly at the aluminum neighborhood, which is quite well understood now, with the power of solid-state NMR spectroscopy., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Inc. All rights reserved.)

Photoluminescent gold nanoclusters have attracted an extensive research interest in bioimaging and therapeutics due to several distinctive advantages such as high fluorescent photostability, good dispersibility, low toxicity and large Stokes shift. However, a better understanding of the correlation between optical properties in various environments and their uptake by specific cancer cells is still needed. Herein, we developed bovine serum albumin stabilized gold nanoclusters (BSA-AuNCs) with an intrinsic tunable photoluminescence emission in the first biological window. The as-synthetized BSA-AuNCs agents consists in protein polymerized-chains dopped with AuNCs with an average size of 2-3 nm and were found to exhibit relevant properties as high photostability, temperature-dependent and excitation induced tunable red photoluminescence. The photostable BSA-AuNCs were functionalized with folic acid (FA-BSA-AuNCs) in order to achieve for the first time an active targeting of NIH:OVCAR-3 human ovarian adenocarcinoma cells, via AuNCs, towards bioimaging applications. After confirming their biocompatibility up to a concentration of 40 mg/ml, the improved cellular uptake and staining ability of FA-BSA-AuNCs compared to the BSA-AuNCs was validated by conventional wide-field epi-fluorescence microscopy, while the intracellular localization was monitored by confocal fluorescence lifetime imaging microscopy (FLIM). Considering their valuable intrinsic photoluminescent properties, the synthesized FA-BSA-AuNCs hold great promise for direct application in cellular imaging as efficient contrast agents towards early cancer diagnosis and image-guided therapy of cancer., (Copyright © 2020 Elsevier B.V. All rights reserved.)