Sol–Gel Synthesis of Silica-Based Materials with Different Percentages of PEG or PCL and High Chlorogenic Acid Content

Implanted biomedical devices can induce adverse responses in the human body, which can cause failure of the implant—referred to as implant failure. Early implant failure is induced numerous factors, most importantly, infection and inflammation. Natural products are, today, one of the main sources of new drug molecules due to the development of pathogenic bacterial strains that possess resistance to more antibiotics used currently in various diseases. The aim of this work is the sol–gel synthesis of antibacterial biomedical implants. In the silica matrix, different percentages (6, 12, 24, 50 wt %) of polyethylene glycol (PEG) or poly(ε-caprolactone) (PCL) were embedded. Subsequently, the ethanol solutions with high amounts of chlorogenic acid (CGA 20 wt %) were slowly added to SiO2/PEG and SiO2/PCL sol. The interactions among different organic and inorganic phases in the hybrid materials was studied by Fourier transform infrared (FTIR) spectroscopy. Furthermore, the materials were soaked in simulated body fluid (SBF) for 21 days and the formation of a hydroxyapatite layer on their surface was evaluated by FTIR and XRD analysis. Finally, Escherichia coli and Pseudomonas aeruginosa were incubated with several hybrids, and the diameter of zone of inhibition was observed to assessment the potential antibacterial properties of the hybrids.

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Synthesis, Structural, Morphological and Thermal Characterization of Five Different Silica-Polyethylene Glycol-Chlorogenic Acid Hybrid Materials

Polymers ◽

10.3390/polym13101586 ◽

2021 ◽

Vol 13 (10) ◽

pp. 1586

Author(s):

Michelina Catauro ◽

Pavel Šiler ◽

Jiří Másilko ◽

Roberta Risoluti ◽

Stefano Vecchio Ciprioti

Keyword(s):

Polyethylene Glycol ◽

Chlorogenic Acid ◽

Hybrid Materials ◽

Sol Gel ◽

Antibacterial Properties ◽

Silica Matrix ◽

Sem Images ◽

Fixed Amount ◽

Organic Components ◽

Free Material

The present study investigated the structure, morphology, thermal behavior, and bacterial growth analysis of novel three-component hybrid materials synthesized by the sol-gel method. The inorganic silica matrix was weakly bonded to the network of two organic components: a well-known polymer such as polyethylene glycol (PEG, average molar mass of about 4000 g/mol), and an antioxidant constituted by chlorogenic acid (CGA). In particular, a first series was made by a 50 wt% PEG-based (CGA-free) silica hybrid along with two 50 wt% PEG-based hybrids containing 10 and 20 wt% of CGA (denoted as SP50, SP50C10 and SP50C20, respectively). A second series contained a fixed amount of CGA (20 wt%) in silica-based hybrids: one was the PEG-free material (SC20) and the other two contained 12 and 50 wt% of PEG, respectively (SP12C20 and SP50C20, respectively), being the latter already included in the first series. The X-ray diffraction (XRD) patterns and scanning electron microscope (SEM) images of freshly prepared materials confirmed that all the materials were amorphous and homogeneous regardless of the content of PEG or CGA. The thermogravimetric (TG) analysis revealed a higher water content was adsorbed into the two component hybrids (SP50 and SC20) because of the availability of a larger number of H-bonds to be formed with water with respect to those of silica/PEG/CGA (SPC), where silica matrix was involved in these bonds with both organic components. Conversely, the PEG-rich materials (SP50C10 and SP50C20, both with 50 wt% of the polymer) retained a lower content of water. Decomposition of PEG and CGA occurred in almost the same temperature interval regardless of the content of each organic component. The antibacterial properties of the SiO2/PEG/CGA hybrid materials were studied in pellets using either Escherichia coli and Enterococcus faecalis, respectively. Excellent antibacterial activity was found against both bacteria regardless of the amount of polymer in the hybrids.

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Aqueous Sol-Gel Synthesis of Different Iron Ferrites: From 3D to 2D

Materials ◽

10.3390/ma14061554 ◽

2021 ◽

Vol 14 (6) ◽

pp. 1554

Author(s):

Justinas Januskevicius ◽

Zivile Stankeviciute ◽

Dalis Baltrunas ◽

Kęstutis Mažeika ◽

Aldona Beganskiene ◽

...

Keyword(s):

Magnetic Measurements ◽

Substrate Surface ◽

Sol Gel ◽

Synthesis Method ◽

Xrd Analysis ◽

Dip Coating ◽

Yttrium Iron ◽

Iron Garnet ◽

Dip Coating Technique ◽

Sol Gel Synthesis

In this study, an aqueous sol-gel synthesis method and subsequent dip-coating technique were applied for the preparation of yttrium iron garnet (YIG), yttrium iron perovskite (YIP), and terbium iron perovskite (TIP) bulk and thin films. The monophasic highly crystalline different iron ferrite powders have been synthesized using this simple aqueous sol-gel process displaying the suitability of the method. In the next step, the same sol-gel solution was used for the fabrication of coatings on monocrystalline silicon (100) using a dip-coating procedure. This resulted, likely due to substrate surface influence, in all coatings having mixed phases of both garnet and perovskite. Thermogravimetric (TG) analysis of the precursor gels was carried out. All the samples were investigated by X-ray powder diffraction (XRD) analysis. The coatings were also investigated by scanning electron microscopy (SEM), atomic force microscopy (AFM) and Mössbauer spectroscopy. Magnetic measurements were also carried out.

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Sol-Gel Synthesis of SnO2-TiO2 System - Morphologic, Photocatalytic and Antibacterial Properties

Key Engineering Materials ◽

10.4028/www.scientific.net/kem.762.273 ◽

2018 ◽

Vol 762 ◽

pp. 273-277

Author(s):

Anzelms Zukuls ◽

Gundars Mežinskis ◽

Aigars Reinis ◽

Ingus Skadins ◽

Juta Kroica ◽

...

Keyword(s):

Sol Gel ◽

Antibacterial Properties ◽

Soda Lime ◽

Rutile Phase ◽

X Ray Diffraction ◽

Oxide Coatings ◽

Atomic Force ◽

Heat Treated ◽

Soda Lime Silicate Glass ◽

Sol Gel Synthesis

SnO2-TiO2 sol-gel coatings on soda-lime silicate glass heat treated at 500 °C and xerogel specimens also heat treated at 500 °C were investigated in this study. The morphology of 1, 3, 5 and 7 mol% SnO2 doped titanium oxide coatings were evaluated with a scanning electron microscope (SEM), an atomic force microscope (AFM) and an UV-VIS light spectrophotometer, whilst xerogel structure was analysed with X-ray diffraction spectroscopy (XRD). The physicochemical properties of the TiO2-SnO2 systems depended mainly on the Sn-to-Ti ratio. The surface morphology of the layer was compact and homogeneous with no visible cracks. Anatase and rutile phase was found in the tested 1, 3, 5, 7 and 10 mol% SnO2 doped and heat treated xerogel specimens. Rutile phase content in the heat treated xerogel was reduced, if Sn4+ content was increased. Photocatalytic activity and antibacterial properties were evaluated as well.

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Sol–Gel Synthesis and Characterization of Coatings of Mg-Al Layered Double Hydroxides

Materials ◽

10.3390/ma12223738 ◽

2019 ◽

Vol 12 (22) ◽

pp. 3738 ◽

Cited By ~ 3

Author(s):

A. Smalenskaite ◽

M. M. Kaba ◽

I. Grigoraviciute-Puroniene ◽

L. Mikoliunaite ◽

A. Zarkov ◽

...

Keyword(s):

Thin Films ◽

Layered Double Hydroxides ◽

Sol Gel ◽

Xrd Analysis ◽

Dip Coating ◽

Dipping Process ◽

Synthetic Approaches ◽

Sol Gel Synthesis ◽

Double Hydroxides ◽

Steel Substrates

In this study, new synthetic approaches for the preparation of thin films of Mg-Al layered double hydroxides (LDHs) have been developed. The LDHs were fabricated by reconstruction of mixed-metal oxides (MMOs) in deionized water. The MMOs were obtained by calcination of the precursor gels. Thin films of sol–gel-derived Mg-Al LDHs were deposited on silicon and stainless-steel substrates using the dip-coating technique by a single dipping process, and the deposited film was dried before the new layer was added. Each layer in the preparation of the Mg-Al LDH multilayers was separately annealed at 70 °C or 300 °C in air. Fabricated Mg-Al LDH coatings were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), and atomic force microscopy (AFM). It was discovered that the diffraction lines of Mg3Al LDH thin films are sharper and more intensive in the sample obtained on the silicon substrate, confirming a higher crystallinity of synthesized Mg3Al LDH. However, in both cases the single-phase crystalline Mg-Al LDHs have formed. To enhance the sol–gel processing, the viscosity of the precursor gel was increased by adding polyvinyl alcohol (PVA) solution. The LDH coatings could be used to protect different substrates from corrosion, as catalyst supports, and as drug-delivery systems in medicine.

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The sol–gel synthesis of cotton/TiO2 composites and their antibacterial properties

Surface and Coatings Technology ◽

10.1016/j.surfcoat.2014.05.033 ◽

2014 ◽

Vol 253 ◽

pp. 171-179 ◽

Cited By ~ 44

Author(s):

O.L. Galkina ◽

A. Sycheva ◽

А. Blagodatskiy ◽

G. Kaptay ◽

V.L. Katanaev ◽

...

Keyword(s):

Sol Gel ◽

Antibacterial Properties ◽

Sol Gel Synthesis

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Synthesis of SiO2-TiO2:Yb3+ glass-ceramics and characterization of structure and optical properties

Science and Technology Development Journal - Natural Sciences ◽

10.32508/stdjns.v1it1.440 ◽

2017 ◽

Vol 1 (T1) ◽

pp. 114-121

Author(s):

Thanh Tat Huynh ◽

Van Thi Thanh Tran

Keyword(s):

Sol Gel ◽

Glass Ceramics ◽

Xrd Analysis ◽

Silica Matrix ◽

Photoluminescence Intensity ◽

Raman Spectroscopic ◽

Characteristic Emission ◽

Ft Ir ◽

Average Size ◽

20 Nm

In this work, the monoliths of 85 % SiO2-15 % TiO2 doped Yb3+ ions at different contents have been prepared by sol-gel method. The measurement of FT-IR, Raman spectroscopic and XRD analysis show the formation of anatase TiO2 nanocrystals with average size about 15–20 nm in silica matrix. Moreover, the pyrochlore crystals of Yb2Ti2O7 begin to form in the samples when content of Yb3+ reaches to 1 mol %. TiO2 Yb3+ 2F7/2 2F5/2 truyền năng lƣợng kích thích UV EV EC mức khuyết tật 974 nm The energy transferred from TiO2 crystals to Yb3+ ions is proven by the characteristic emission spectrum of Yb3+ at the wavelength of 980 nm when the samples are excited by the wavelength of 300 nm. The photoluminescence intensity is highest at 0.1% mol of Yb3+ and gradually decreases with doping content

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Sol-Gel Synthesis of Functionalized Nanocomposite Sorbtional Material with Polymer-Silica Matrix

Sol-Gel Methods for Materials Processing - NATO Science for Peace and Security Series C: Environmental Security ◽

10.1007/978-1-4020-8514-7_36 ◽

2008 ◽

pp. 413-419 ◽

Cited By ~ 1

Author(s):

Bahodir D. Kabulov ◽

Dilshod H. Shakarova ◽

Kazim A. Akhundjanov ◽

Sayibjan S. Negmatov ◽

Oleg A. Shpigun

Keyword(s):

Sol Gel ◽

Silica Matrix ◽

Sol Gel Synthesis

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Chlorogenic Acid Entrapped in Hybrid Materials with High PEG Content: A Strategy to Obtain Antioxidant Functionalized Biomaterials?

Materials ◽

10.3390/ma12010148 ◽

2019 ◽

Vol 12 (1) ◽

pp. 148 ◽

Cited By ~ 23

Author(s):

Michelina Catauro ◽

Federico Barrino ◽

Giovanni Dal Poggetto ◽

Giuseppina Crescente ◽

Simona Piccolella ◽

...

Keyword(s):

Chlorogenic Acid ◽

Sol Gel ◽

Antioxidant Properties ◽

Radical Scavenging ◽

Antibacterial Properties ◽

Redox Activity ◽

In Vitro Biocompatibility ◽

Dependent Behavior ◽

Nih 3T3

The formation of pro-oxidant species after implantation of biomaterials could be responsible for the failure of the implant itself, because of oxidative stress-induced damage. In this work, the SiO2/polyethylene glycol (PEG)/chlorogenic acid (CGA) hybrids synthesized by the sol–gel method with 50 wt% of the polymer and different amounts of CGA (5, 10, 15 and 20 wt%) were studied. The hybrids soaked in simulated body fluid (SBF) showed the formation of hydroxyapatite layers on their surface, suggesting that the hybrids are bioactive. Their radical scavenging capacity towards DPPH· and ABTS·+ (2,2′-Azino-bis(3-ethylbenzthiazoline-6-sulfonic acid), evaluated at three different doses (0.5, 1 and 2 mg), showed probe- and dose-dependent behavior. In addition, the antioxidant properties of CGA were not affected by the presence of high amounts of the polymer. The in vitro biocompatibility in three cell lines (NIH 3T3, HaCaT and SH-SY5Y) was assessed by using the 3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H-tetrazolium bromide (MTT) assay. Apart from SH-SY5Y, the cell viability—expressed as mitochondrial redox activity percentage of cells directly exposed to powders—and morphology was not affected, suggesting that the hybrids have the ability to interfere and act selectively against tumor cells. The antibacterial properties of the different materials against Escherichia coli and Enterococcus faecalis were affected by different amounts of the natural antioxidant component.

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Synthesis and Characterization of Sol–Gel Prepared Silver Nanoparticles

International Journal of Nanoscience ◽

10.1142/s0219581x14500045 ◽

2014 ◽

Vol 13 (01) ◽

pp. 1450004 ◽

Cited By ~ 20

Author(s):

Dharamvir Singh Ahlawat ◽

Rekha Kumari ◽

Rachna ◽

Indu Yadav

Keyword(s):

Silver Nanoparticles ◽

Absorption Spectra ◽

Annealing Temperature ◽

Sol Gel ◽

Xrd Analysis ◽

Silica Matrix ◽

Silver Clusters ◽

Different Temperatures ◽

Uv Visible ◽

Average Size

Silver nanoparticles (SNPs) have been successfully prepared using sol–gel method by annealing the sample at 550°C for 30 min. The SNPs were not confirmed by X-ray diffraction (XRD) analysis when the annealing temperature was considered at 450°C. They were also not confirmed without calcination of the sample. The physical mechanism of silver clusters formation in the densified silica matrix with respect to thermal treatment has been understood. The presence of silver metal in the silica matrix was confirmed by XRD analysis and TEM image of the samples. The average size of nanoparticles dispersed in silica matrix was determined as 10.2 nm by the XRD technique. The synthesized nanocomposites were also characterized by UV-Visible spectroscopy with a peak in the absorption spectra at around 375 nm. The distribution of particle size has been reported here in the range from 8 nm to 25 nm by TEM observations of the sample prepared at 550°C. The spherically smaller size (≈10 nm) SNPs have reported the surface plasmons resonance (SPR) peak less than or near to 400 nm due to blue-shifting and effect of local refractive index. Without annealing the silica samples the absorption spectra does not show any peak around 375 nm. The FTIR spectroscopy of the three types of samples prepared at different temperatures (room temperature, 450°C and 550°C) has also been reported. This spectra have provided the identification of different chemical groups in the prepared samples. It has been predicted that the size of SNPs by XRD, UV-Visible and TEM results have agreed well with each other. It may be concluded that formation of SNPs is a function of annealing temperature.

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Synthesis of lead-based 1212 and 3212 superconductors by an aqueous sol-gel method

Open Chemistry ◽

10.2478/s11532-009-0025-z ◽

2009 ◽

Vol 7 (3) ◽

pp. 362-368 ◽

Cited By ~ 1

Author(s):

Giedre Nenartaviciene ◽

Ramunas Skaudzius ◽

Rimantas Raudonis ◽

Aivaras Kareiva

Keyword(s):

Sol Gel ◽

Xrd Analysis ◽

Structural Features ◽

Complexing Agents ◽

X Ray Diffraction ◽

X Ray ◽

Resistivity Measurements ◽

Ceramic Samples ◽

Xrd Patterns ◽

Sol Gel Synthesis

AbstractThe aqueous sol-gel synthesis technique for the preparation of (Pb,Sr)Sr2(Y,Ca)Cu2O7±x (Pb-1212) and (Pb2,Cu)Sr2(Y,Ca)Cu2O8±x (Pb-3212) superconductors using two different complexing agents, namely 1,2-ethanediol and tartaric acid was studied. The phase transformations, composition and micro-structural features in the polycrystalline samples were studied by powder X-ray diffraction analysis (XRD), infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). XRD analysis of the ceramic samples obtained by calcination of Pb-Sr-Y-Ca-Cu-O acetate-glycolate precursor gels in air, for 10 hours at 800°C and at 825°C, showed the presence of homogeneous Pb-1212 and Pb-3212 crystallites as major phases. The XRD patterns of the ceramics obtained from Pb-Sr-Y-Ca-Cu-O acetate-tartrate precursor gels, however, showed multiphasic character. The critical temperature of superconductivity (TC (onset)) observed by resistivity measurements were found to be 91 K and 75 K for Pb-1212 and Pb-3212 samples, respectively.

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