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1.
Chem Asian J ; : e202400739, 2024 Aug 17.
Artigo em Inglês | MEDLINE | ID: mdl-39152948

RESUMO

In the present study, both short-range and long-range structural features of an ionic bridged silsesquioxane, specifically one containing the 1,4-diazoniabicyclo[2.2.2]octane chloride group (ISSQ), were elucidated. This ionic silsesquioxane was synthesized via direct polycondensation of a bridged organosilane precursor, without any additional functionalization step. Si-O-Si cage structures typical of Polyhedral Oligomeric Silsesquioxanes (POSS) were identified. The average interatomic distances of the POSS cages, including the open T8 cage and the T12 cage for the ISSQ, as well as the T8 cage for a commercially available pendant POSS were determined. It is the first report of the interatomic distance determination of POSS cage; achieved by using total pair distribution function G(r) values obtained through high-resolution synchrotron X-ray diffraction combined with density functional theory (DFT) calculations. The application of DFT was crucial for accurately assigning X-ray peaks and verifying structural details. Furthermore, the analysis of X-ray diffraction peaks and the examination of crystalline domains via transmission electron microscopy enabled the proposal of a hexagonal arrangement of Si-O-Si cages over long ranges within the ionic bridged silsesquioxane. This proposed arrangement highlights a distinctive structural organization that could impact the material's properties and applications.

2.
Sensors (Basel) ; 24(14)2024 Jul 14.
Artigo em Inglês | MEDLINE | ID: mdl-39065959

RESUMO

This research enhances ethanol sensing with Fe-doped tetragonal SnO2 films on glass, improving gas sensor reliability and sensitivity. The primary objective was to improve the sensitivity and operational efficiency of SnO2 sensors through Fe doping. The SnO2 sensors were synthesized using a flexible and adaptable method that allows for precise doping control, with energy-dispersive X-ray spectroscopy (EDX) confirming homogeneous Fe distribution within the SnO2 matrix. A morphological analysis showed a surface structure ideal for gas sensing. The results demonstrated significant improvement in ethanol response (1 to 20 ppm) and lower temperatures compared to undoped SnO2 sensors. The Fe-doped sensors exhibited higher sensitivity, enabling the detection of low ethanol concentrations and showing rapid response and recovery times. These findings suggest that Fe doping enhances the interaction between ethanol molecules and the sensor surface, improving performance. A mathematical model based on diffusion in porous media was employed to further analyze and optimize sensor performance. The model considers the diffusion of ethanol molecules through the porous SnO2 matrix, considering factors such as surface morphology and doping concentration. Additionally, the choice of electrode material plays a crucial role in extending the sensor's lifespan, highlighting the importance of material selection in sensor design.

3.
Materials (Basel) ; 17(13)2024 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-38998310

RESUMO

To meet the current demand for lead-free piezoelectric ceramics, a novel sol-gel synthesis route is presented for the preparation of Ba0.85Ca0.15Ti0.9Zr0.1O3 doped with cerium (Ce = 0, 0.01, and 0.02 mol%) and vanadium (V = 0, 0.3, and 0.4 mol%). X-ray diffraction patterns reveal the formation of a perovskite phase (space group P4mm) for all samples after calcination at 800 °C and sintering at 1250, 1350, and 1450 °C, where it is proposed that both dopants occupy the B site. Sintering studies show that V doping allows the sintering temperature to be reduced to at least 1250 °C. Undoped BCZT samples sintered at the same temperature show reduced functional properties compared to V-doped samples, i.e., d33 values increase by an order of magnitude with doping. The dissipation factor tan δ decreases with increasing sintering temperature for all doping concentrations, while the Curie temperature TC increases for all V-doped samples, reaching 120 °C for high-concentration co-doped samples. All results indicate that vanadium doping can facilitate the processing of BCZT at lower sintering temperatures without compromising performance while promoting thermal property stability.

4.
J Biomater Sci Polym Ed ; 35(10): 1493-1510, 2024 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-38569077

RESUMO

In recent years, there has been a notable surge of interest in hybrid materials within the biomedical field, particularly for applications in bone repair and regeneration. Ceramic-polymeric hybrid scaffolds have shown promising outcomes. This study aimed to synthesize bioactive glass (BG-58S) for integration into a bioresorbable polymeric matrix based on PDLLA, aiming to create a bioactive scaffold featuring stable pH levels. The synthesis involved a thermally induced phase separation process followed by lyophilization to ensure an appropriate porous structure. BG-58S characterization revealed vitreous, bioactive, and mesoporous structural properties. The scaffolds were analyzed for morphology, interconnectivity, chemical groups, porosity and pore size distribution, zeta potential, pH, in vitro degradation, as well as cell viability tests, total protein content and mineralization nodule production. The PDLLA scaffold displayed a homogeneous morphology with interconnected macropores, while the hybrid scaffold exhibited a heterogeneous morphology with smaller diameter pores due to BG-58S filling. The hybrid scaffold also demonstrated a pH buffering effect on the polymer surface. In addition to structural characteristics, degradation tests indicated that by incorporating BG-58S modified the acidic degradation of the polymer, allowing for increased total protein production and the formation of mineralization nodules, indicating a positive influence on cell culture.


Assuntos
Regeneração Óssea , Cerâmica , Vidro , Poliésteres , Alicerces Teciduais , Cerâmica/química , Alicerces Teciduais/química , Regeneração Óssea/efeitos dos fármacos , Vidro/química , Porosidade , Poliésteres/química , Materiais Biocompatíveis/química , Concentração de Íons de Hidrogênio , Humanos , Sobrevivência Celular/efeitos dos fármacos , Teste de Materiais
5.
Polymers (Basel) ; 16(8)2024 Apr 17.
Artigo em Inglês | MEDLINE | ID: mdl-38675044

RESUMO

The addition of nanostructures to polymeric materials allows for a direct interaction between polymeric chains and nanometric structures, resulting in a synergistic process through the physical (electrostatic forces) and chemical properties (bond formation) of constituents for the modification of their properties and potential cutting-edge materials. This study explores a novel in situ synthesis method for PDMS-%SiO2 nanoparticle composites with varying crosslinking degrees (PDMS:TEOS of 15:1, 10:1, and 5:1); particle concentrations (5%, 10%, and 15%); and sol-gel catalysts (acidic and alkaline). This investigation delves into the distinct physical and chemical properties of silicon nanoparticles synthesized under acidic (SiO2-a) and alkaline (SiO2-b) conditions. A characterization through Raman, FT-IR, and XPS analyses confirms particle size and agglomeration differences between both the SiO2-a and SiO2-b particles. Similar chemical environments, with TEOS and ethanol by-products, were detected for both systems. The results on polymer composites elucidate the successful incorporation of SiO2 nanoparticles into the PDMS matrix without altering the PDMS's chemical structure. However, the presence of nanoparticles did affect the relative intensities of specific vibrational modes over composites from -35% to 24% (Raman) and from -14% to 59% (FT-IR). The XPS results validate the presence of Si, O, and C in all composites, with significant variations in atomic proportions (C/Si and O/Si) and Si and C component analyses through deconvolution techniques. This study demonstrates the successful in situ synthesis of PDMS-SiO2 composites with tunable properties by controlling the sol-gel and crosslinking synthesis parameters. The findings provide valuable insights into the in situ synthesis methods of polymeric composite materials and their potential integration with polymer nanocomposite processing techniques.

6.
Pharmaceutics ; 16(3)2024 Feb 23.
Artigo em Inglês | MEDLINE | ID: mdl-38543206

RESUMO

Curcumin (CUR) is a natural compound that can be combined with miconazole (MCZ) to improve vulvovaginal candidiasis (VVC) caused by Candida albicans treatment's efficacy. This study aimed to develop ureasil-polyether (U-PEO) vaginal ovules loaded with CUR and MCZ for the treatment of VVC. Physicochemical characterization was performed by thermogravimetry (TGA), differential thermal analysis (DTA), Fourier transform infrared spectroscopy (FTIR), and in vitro release. Antifungal assays were used to determine minimum inhibitory concentrations (MICs) and synergism between CUR and MCZ, and the activity of U-PEO ovules were performed by microdilution and agar diffusion. TGA results showed high thermal stability of the hybrid ovules. In DTA, the amorphous character of U-PEO and a possible interaction between CUR and MCZ were observed. FTIR showed no chemical incompatibility between the drugs. In vitro release resulted in 80% of CUR and 95% of MCZ released within 144 h. The MICs of CUR and MCZ were 256 and 2.5 µg/mL, respectively. After combining the drugs, the MIC of MCZ decreased four-fold to 0.625 µg/mL, while that of CUR decreased eight-fold to 32 µg/mL. Synergism was confirmed by the fractional inhibitory concentration index (FICI) equal to 0.375. U-PEO alone showed no antifungal activity. U-PEO/MCZ and U-PEO/CUR/MCZ ovules showed the greatest zones of inhibition (≥18 mm). The results highlight the potential of the ovules to be administered at a lower frequency and at reduced doses compared to available formulations.

7.
Molecules ; 29(2)2024 Jan 12.
Artigo em Inglês | MEDLINE | ID: mdl-38257303

RESUMO

We present a study on the green synthesis of undoped and Er-doped ZnO compounds using Mangifera indica gum (MI). A set of tests were conducted to assess the structure of the material. The tests included X-ray diffraction, Raman, and Fourier-transform infrared spectroscopy. Optical properties were studied using diffuse reflectance and photoluminescence. Morphological and textural investigations were done using SEM images and N2 adsorption/desorption. Furthermore, photocatalytic tests were performed with methylene blue (MB), yellow eosin (EY), and the pharmaceutical drug ibuprofen (IBU) under UV irradiation. The study demonstrated that replacing the stabilizing agent with Mangifera indica gum is an effective method for obtaining ZnO nanoparticles. Additionally, the energy gap of the nanoparticles exhibits a slight reduction in value. Photoluminescence studies showed the presence of zinc vacancies and other defects in both samples. In the photocatalytic test, the sample containing Er3+ exhibited a degradation of 99.7% for methylene blue, 81.2% for yellow eosin, and 52.3% for ibuprofen over 120 min. In the presence of methyl alcohol, the degradation of MB and EY dyes is 16.7% and 55.7%, respectively. This suggests that hydroxyl radicals are responsible for the direct degradation of both dyes. In addition, after the second reuse, the degradation rate for MB was 94.08%, and for EY, it was 82.35%. For the third reuse, the degradation rate for MB was 97.15%, and for EY, it was 17%. These results indicate the significant potential of the new semiconductor in environmental remediation applications from an ecological synthesis.


Assuntos
Mangifera , Nanopartículas , Óxido de Zinco , Amarelo de Eosina-(YS) , Azul de Metileno , Fotólise , Ibuprofeno , Corantes
8.
J Biomed Mater Res B Appl Biomater ; 112(1): e35315, 2024 01.
Artigo em Inglês | MEDLINE | ID: mdl-37589245

RESUMO

The development of bioactive membranes with bone repair properties is great interest in the field of tissue engineering. In this study, we aimed to fabricate and characterize a composite membrane composed of sol-gel synthesized bioceramics and electrospun polycaprolactone (PCL) fibers for bone tissue regeneration applications. The bioceramics were prepared using the sol-gel method with nitrate (N) and chloride (CL) as precursors. PCL and bioceramic solutions were electrospun to obtain ultrafine fiber mats. Raman spectroscopy, x-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM) were used to characterize the materials. The results showed that both chlorinated and non-chlorinated bioceramics contained NBOs (non-bridge bonds) and crystallized the α-wollastonite phase, with the chlorinated version doing so at lower temperatures. In vitro tests were performed to evaluate cytotoxicity, cell adhesion, and mineralized matrix formation on the membranes. The composite membranes showed improved cell viability and promoted mineralization nodules formation. This study presents a promising approach for the development of bioactive membranes for bone tissue engineering, with potential applications in bone regeneration therapies.


Assuntos
Poliésteres , Engenharia Tecidual , Poliésteres/química , Engenharia Tecidual/métodos , Espectroscopia de Infravermelho com Transformada de Fourier , Osso e Ossos , Alicerces Teciduais/química , Materiais Biocompatíveis/química
9.
J Biomed Mater Res B Appl Biomater ; 112(1): e35340, 2024 01.
Artigo em Inglês | MEDLINE | ID: mdl-37929804

RESUMO

Effective bone substitute biomaterials remain an important challenge in patients with large bone defects. Glass ceramics produced by different synthesis routes may result in changes in the material physicochemical properties and consequently affect the success or failure of the bone healing response. To investigate the differences in the orchestration of the inflammatory and healing process in bone grafting and repair using different glass-ceramic routes production. Thirty male Wistar rats underwent surgical unilateral parietal defects filled with silicate glass-ceramic produced by distinct routes: BS - particulate glass-ceramic produced via the fusion/solidification route, and BG - particulate glass-ceramic produced via the sol-gel route. After 7, 14, and 21 days from biomaterial grafting, parietal bones were removed to be analyzed under H&E and Massons' Trichome staining, and immunohistochemistry for CD206, iNOS, and TGF-ß. Our findings demonstrated that the density of lymphocytes and plasma cells was significantly higher in the BS group at 45, and 7 days compared to the BG group, respectively. Furthermore, a significant increase of foreign body giant cells (FBGCs) in the BG group at day 7, compared to BS was found, demonstrating early efficient recruitment of FBGCs against sol-gel-derived glass-ceramic particulate (BS group). According to macrophage profiles, CD206+ macrophages enhanced at the final periods of both groups, being significantly higher at 45 days of BS compared to the BG group. On the other hand, the density of transformation growth factor beta (TGF-ß) positive cells on 21 days were the highest in BG, and the lowest in the BS group, demonstrating a differential synergy among groups. Noteworthy, TGF-ß+ cells were significantly higher at 21 days of BG compared to the BS group. Glass-ceramic biomaterials can act differently in the biological process of bone remodeling due to their route production, being the sol-gel route more efficient to activate M2 macrophages and specific FBGCs compared to the traditional route. Altogether, these features lead to a better understanding of the effectiveness of inflammatory response for biomaterial degradation and provide new insights for further preclinical and clinical studies involved in bone healing.


Assuntos
Materiais Biocompatíveis , Substitutos Ósseos , Humanos , Ratos , Animais , Masculino , Teste de Materiais , Ratos Wistar , Materiais Biocompatíveis/química , Regeneração Óssea , Substitutos Ósseos/química , Cerâmica/farmacologia , Cerâmica/química , Macrófagos , Fator de Crescimento Transformador beta , Vidro/química
10.
Gels ; 9(8)2023 Jul 27.
Artigo em Inglês | MEDLINE | ID: mdl-37623063

RESUMO

In the present work, a biocatalytic glucose optical sensor produced by immobilizing glucose oxidase (GOD) as a recognition molecule over a PMMA (polymethylmethacrylate) optical fiber is introduced. An enzymatic encapsulation process was carried out using the sol-gel method, depositing a TEOS-based coating by immersion at the end of an optical fiber; the biosensor was characterized using different glucose levels. Finally, the best way to encapsulate the enzyme and prevent it from degrading is to perform the process at room temperature, and later implement the deposition of the coating on the fiber. The drying process was optimal below 8 °C.

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