Nano-Co3O4-catalyzed microwave-assisted one-pot synthesis of some seleno [2 , 3-b ] pyridine/quinoline derivatives

For the efficient synthesis of transition-metal cobalt oxide nanoparticles (Co₃O₄ NPs) without using any costly and toxic solvent or complicated equipment, the co-precipitation method was used in this work. Using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), UV–Vis spectrophotometry, Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD), the prepared Co₃O₄ NPs were characterized and identified. The influence of prepared Co₃O₄ NPs on the developmental synthesis of some selenopyridine/quinoline derivatives under different microwave irradiation powers and irradiation times was investigated via click (reaction) chemistry. The reusable Co₃O₄ nanoparticles have high catalytic activity under microwave irradiation for the synthesis of organoselenium compounds with higher yields (>?90%), milder reaction conditions and shorter time without significantly decreasing the reaction rates and yields.

     

Synthesis method-dependent photothermal effects of colloidal solutions of platinum nanoparticles used in photothermal anticancer therapy

One of the most common anticancer therapies is photothermal therapy (PTT). The effectiveness of PTT depends on the photosensitizer being a molecule which is toxic for the cancer cells after electromagnetic wave irradiation. Therefore, a simulation of PTT was performed in this work on two colon cancer cells (SW480 and SW620) using platinum nanoparticles (Pt NPs). Interestingly, in the literature the dependence between the synthesis method and the photothermal properties of Pt NPs was not discussed. Consequently, in this paper, we evaluated the photothermal properties of Pt NPs synthesized by two different methods: polyol (PtI NPs) and green chemistry (PtII NPs). Scanning transmission electron microscopy revealed that the size of both Pt NPs obtained was 2 nm, the NPs were not agglomerated, and that the PtII NPs were distributed on green tea supports. The selected area electron diffraction and X-ray diffraction analysis confirmed the crystallinity of both types of Pt NPs. Fourier-transform infrared (FTIR) spectrum of the PtII NPs showed interactions between the NPs and stretching modes for C=O groups from flavonoids and polyphenols. Therefore, these chemical compounds could be responsible for reducing Pt⁴⁺ ions to Pt⁰. Moreover, the 3-(4,5-dimethylthiazol-2-yl)-5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium (MTS) assay showed that the PtII NPs exhibited 10% and 20% better cytotoxicity effect on SW480 and SW620 cells, than PtI NPs. The viability of cancer cells decreased when Pt NPs were used in PTT. The highest percentage of dead cells (82%) was observed for PtII NPs and 650-nm laser irradiation. FTIR and Raman spectroscopy showed structural changes induced by both Pt NPs and laser irradiation of cells in the range corresponding to levels of DNA, phospholipids, proteins, and lipids. Moreover, the calculated photothermal conversion efficiency showed that the value of this parameter is around 35%, regardless of the synthesis method and used wavelengths.     

Hydrolysis of chitosan under microwave irradiation in ionic liquids promoted by sulfonic acid-functionalized ionic liquids

Hydrolysis of chitosan in ionic liquids was carried out under microwave irradiation (MW) using sulfonic acid-functionalized ionic liquids (SFILs) as catalysts. The effect of microwave power, irradiation time, dosage of SFILs and DMSO was investigated by orthogonal tests. Under the optimal reaction conditions, the yield of total reducing sugars (TRS) reached over 90% within 2 min. The viscosity-average molecular weight of degraded chitosan was determined by viscosity method. The structures of the original and degraded chitosan were characterized by Fourier-transform infrared (FTIR) spectra, X-ray powder diffraction (XRD) analysis and carbon-13 nuclear magnetic resonance spectroscopy (¹³C NMR). The influence of microwave power and irradiation time on the TRS and M_v was further studied. This method can dramatically reduce reaction time.     

Synthesis and characterization of UV-irradiated silver/montmorillonite nanocomposites

We have successfully developed a simple method for preparing silver nanoparticles (Ag NPs) using UV irradiation of AgNO₃ in the interlamellar space of a montmorillonite (MMT) without any reducing agent or heat treatment. The properties of Ag/MMT nanocomposites were studied as a function of the UV irradiation period. UV irradiation disintegrated the Ag NPs into smaller size until a relatively stable size and size distribution were achieved. The results from UV–vis spectroscopy show that particles size of Ag NPs decrease with the increase of irradiation period. The crystalline structure of Ag NPs was determined by powder X-ray diffraction (PXRD).     

Ranolazine-functionalized CuO NPs: efficient homogeneous and heterogeneous catalysts for reduction of 4-nitrophenol

In the present study copper oxide nanoparticles (CuO NPs) were synthesized using a hydrothermal method with ranolazine as a shape-directing agent. Ranolazine-functionalized CuO NPs were characterized by various analytical techniques such as scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). The SEM pattern confirmed the morphology of ranolazine-functionalized CuO NPs with well-defined rice-like structures. FTIR spectroscopy confirmed the interaction between CuO NPs and ranolazine. The XRD analysis indicated that the structure of ranolazine-functionalized CuO NPs was monoclinic crystalline and the size ranged between 9 and 18 nm with an average particle size of 12 nm. The smaller size range of CuO NPs gave a large surface area that enhanced the efficiency of these catalysts employed for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) in the H ₂ O system. In homogeneous catalysis, results showed that 50 μL of CuO NPs was required in the presence of NaBH4 for 99% reduction of 4-NP in 240 s. On the other hand, for heterogeneous catalysis, 0.5 mg of CuO NPs was used in the presence of NaBH4 for 99% catalytic reduction of 4-NP to 4-AP in 320 s. The rate of reaction for homogeneous catalysis and heterogeneous catalysis was determined from the plots of In(Ct /C0) of 4-NP versus time (s), which showed good linearity with values of 1.3 × 10 ^-2 and 8.8 × 10 ^-3 s ^-1 . respectively. The high-quality catalytic efficiency, good reusability, nontoxic nature, and low cost are favorable properties of the synthesized CuO NPs for use as efficient catalysts for reduction of 4-AP to 4-NP in both homogeneous and heterogeneous media.     

Supported silver nanoparticles over alginate-modified magnetic nanoparticles: Synthesis,characterization and treat the human lung carcinoma

This article displays synthesis of Silver nanoparticles (Ag NPs) decorated on sodium alginate covered magnetite (Fe₃O₄/Alg-Ag NPs) nanocomposite. Sodium alginate shell as a natural anionic polysaccharide on Fe₃O₄ microparticles core acted as a stabilizing agent for the reduction of Ag(I) ions into Ag NPs. The structural features of the synthesized nanocomposite were investigated by fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopes (FE-SEM), transmission electron microscopes (TEM), energy-dispersive X-ray spectroscopy (EDX) and vibrating-sample magnetometer (VSM) studies and inductively coupled plasma-optical emission spectroscopy (ICP-OES). 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-2H-tetrazolium bromide (MTT) assay was used on common lung cancer cell lines i.e., NCI-H1975, NCI-H1563, and NCI-H1299 to survey the cytotoxicity and anti-lung cancer effects of the synthesized nanocomposite. The synthesized nanocomposite had very low cell viability and high anti-lung cancer activities dose-dependently against NCI-H1975, NCI-H1563, and NCI-H1299 cell lines without any cytotoxicity on the normal cell line (Human umbilical vein endothelial cells (HUVECs)). To determine the antioxidant properties of the synthesized nanocomposite, the 2,2-diphenyl-1-picrylhydrazyl (DPPH) test was used in the presence of butylated hydroxytoluene as the positive control. The synthesized nanocomposite inhibited half of the DPPH molecules in the concentration of 194 µg/mL. Maybe significant anti-human lung cancer potentials of the synthesized nanocomposite against common human lung cancer cell lines are linked to their antioxidant activities.     

Simple surface functionalization of magnetic nanoparticles with methotrexate-conjugated bovine serum albumin as a biocompatible drug delivery vehicle

Magnetic nanoparticles (MNPs) functionalized with methotrexate (MTX)-conjugated bovine serum albumin (BSA) as a biocompatible drug delivery vehicle were synthesized using a facile method. Characterization of the functionalized MNPs (Fe₃O₄@BSA-MTX NPs) was performed using various techniques including UV–visible spectroscopy, dynamic light scattering, vibrating sample magnetometry and X-ray diffraction. The particle size and zeta potential of Fe₃O₄@BSA-MTX NPs were 105.7 ± 3.81 nm (mean ± SD) and −18.2 mV, respectively. MTX release from Fe₃O₄@BSA-MTX NPs showed an enzyme-dependent release pattern. Hemo-biocompatibility of Fe₃O₄@BSA-MTX NPs was confirmed using hemolysis test. In addition, the cytotoxicity of functionalized MNPs and free MTX against MCF-7 cell line was investigated using MTT assay. The results of experiments revealed that the Fe₃O₄@BSA-MTX NPs as a biocompatible carrier could improve the therapeutic effect of MTX.     

Effect of synthesis parameters on the structural,morphological characteristics,and photocatalytic activity of La2O3 nanoparticles

This study investigates the influence of synthesis processes such as sonication, sol-gel, and microwave on the production of highly crystalline Lanthanum oxide nanoparticles (La₂O₃) employing Lanthanum nitrate and Ammonium hydroxide (NH₄OH) as precursors. X-ray diffraction (XRD), particle size analysis (DLS), Field emission scanning electron microscopy (FESEM), Fourier-transform infrared spectroscopy (FTIR), ultraviolet–visible absorption spectroscopy (UV–Vis), and electrochemical impedance spectroscopy (EIS) were used to examine the most effective processing method and its effects on the nanoparticle characteristics, such as structure, morphology, and optical and electrical behavior. Sonication produces La₂O₃ NPs with a smaller crystalline size, an agglomerated nanorod structure, a higher bandgap, and better electrical responsiveness than sol-gel and microwave techniques. Structural and optical characterization tests discovered this. The photocatalytic degradation activity of cationic Safranin and anionic Congo red dye exhibits degradation efficiency of around 90.13% and 89.66%, respectively.     

Studies on hydrothermal synthesis of photolumniscent rare earth (Eu3+ & Tb3+) doped NG@FeMoO4 for enhanced visible light photodegradation of methylene blue dye

FeMoO₄ nanorods and their rare earth (Eu³⁺ and Tb³⁺) doped composites with nitrogen doped graphene (NG) were synthesized by facile hydrothermal method in aqueous medium. X-ray diffraction (XRD) analysis of the as-synthesized samples was done to study the phase purity and crystalline nature. FTIR and Raman Spectroscopy have been studied for investigating the bonding in nanostructures. The surface morphology of the samples was investigated with field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The photolumniscent nature of the samples was investigated by the using the fluorescence spectrophotometer. The photocatalytic degradation efficiency of the prepared pure FeMoO₄ and its rare earth doped composites with nitrogen doped graphene was evaluated as function of visible light irradiation versus concentration of methylene blue (MB dye). The prepared nanocomposites show enhanced photocatalytic efficiency as compared to the bare FeMoO₄ nanorods.     

纳米钒酸铋的微波快速合成及光催化性能研究

采用微波辅助加热法以NaVO₃溶液和Bi(NO₃)₃·5H₂O的硝酸溶液为反应物,在10～40 min内合成了纳米钒酸铋粉末。利用XRD、FTIR、TEM、UV-Vis等手段研究了反应时间对产物结构及形貌的影响。经测定反应10 min时,得到纯的四方相BiVO₄,随着反应时间的延长,逐渐出现单斜相的衍射峰,当反应40 min时,获得纯的单斜相BiVO₄。同时XRD和IR结果证明了相转变的过程。TEM分析表明不同的反应时间条件下样品呈现不同的形貌。不同反应时间下获得样品的光催化性能的结果表明,微波反应时间对BiVO₄结构的转变及光催化性能的改变起到了重要的作用。     

Facile combustion synthesis of Ag2O nanoparticles using cantaloupe seeds and their multidisciplinary applications

Silver oxide nanoparticles (Ag₂O NPs) were prepared using cantaloupe (Cucumis melo) seeds as a fuel by employing a green synthesis method. The prepared Ag₂O NPs were investigated using powder X-ray diffraction (PXRD), UV–visible spectrum, Fourier transform infrared analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM) with energy-dispersive spectroscopy, and photoluminescence studies. PXRD data reveal the establishment of cubic crystal structure of Ag₂O NPs. According to SEM and TEM results, the morphology of the prepared NPs was agglomerated and spherical. The photodegradation activity of the prepared Ag₂O NPs over methylene blue dye was promising under visible light irradiation. Furthermore, the antimicrobial assay of the synthesized Ag₂O NPs was carried out by the disc diffusion method against Gram-positive and Gram-negative microbial strains.     

Enhanced photo-catalytic activity of TiO2 nanostructured thin films under solar light by Sn and Nb co-doping

In this study, preparation of Sn and Nb co-doped TiO₂ dip-coated thin films on glazed porcelain substrates via sol–gel process have been investigated. The effects of co-doping content on the structural, optical, and photo-catalytic properties of applied thin films have been studied by X-ray diffraction (XRD), field emission SEM (FE-SEM), high resolution transmission electron microscopy (HR-TEM), and UV–Vis absorption spectroscopy. Surface chemical state of thin films was examined by atomic X-ray photoelectron spectroscopy (XPS). XRD results suggest that adding impurities has a great effect on the crystallinity and particle size of TiO₂. Titania Rutile phase formation in thin film was promoted by Sn⁴⁺ addition but was inhibited by Nb⁵⁺ doping. The prepared co-doped TiO₂ photo-catalyst films showed optical absorption edge in the visible light area and exhibited excellent photo-catalytic ability for degradation of methylene blue (MB) solution under solar irradiation. Comparison with undoped and Sn or Nb-doped TiO₂, codoped TiO₂ shows an obviously higher catalytic activity under solar irradiation.     

Enhancement of photodegradation efficiency,photoluminescence quantum yield,and magnetization in highly Yb3+-doped CdO nanoparticles synthesized via sol–gel method

Cd_1?xYb_xO (x?=?0, 1, 5, 10, 15 mol%) nanoparticles (NPs) were successfully synthesized by pulverizing the product obtained from a sol–gel process. The crystalline structure of the synthesized samples was established by X-ray diffraction analysis. Scanning electron microscopy revealed that the prepared samples were nanoscale and the size of the NPs decreased with increasing dopant concentration. Elemental analysis of the products was carried out by energy-dispersive X-ray spectroscopy. Ultraviolet–visible (UV–Vis) and Fourier-transform infrared (FT-IR) spectroscopies were used to characterize the synthesized species. Increasing the Yb³⁺ ion level in the host matter resulted in decreased bandgap energy. Photoluminescence measurements confirmed the enhanced intensity of the characteristic emissions in the Yb³⁺-doped CdO NPs, indicating appropriate substitution of Cd²⁺ with Yb³⁺ ions. Magnetic measurements revealed that, with addition of Yb³⁺ ion, the magnetic behavior of the samples changed. Increasing the dopant ion concentration, thereby decreasing the size of the obtained NPs, changed their behavior from paramagnetic to superparamagnetic, with increased saturation magnetization (M_S) for higher dopant level. Photocatalytic measurements under UV and natural sunlight irradiation revealed that the samples prepared with high dopant concentration (15 mol%) exhibited excellent photocatalytic activity under natural sunlight for decomposition of methylene blue dye.

     

规整、均一纳米水滑石晶体的水热合成与表征

采用一种简便的新方法, 以Mg^2＋/Al^3＋/CO₃^2－摩尔比为6∶2∶1的比例在水热条件下合成了[Mg-Al-CO₃]水滑石. 获得的水滑石样品用XRD, FE-SEM, TEM, HRTEM, TG-DSC进行了物相、晶体形貌结构和热分析. 用动态光散射原理分析了粒度分布, 考察了水热合成的主要条件水热温度和时间对水滑石晶体尺寸及粒度分布的影响. 结果表明, 本法合成的水滑石具有均一、规整的六边形片状晶体形貌, 片状晶体直径在350 nm左右, 片的厚度约20 nm, 纯水滑石相, 粒度分布在80～420 nm. 水热温度和时间主要影响片状晶体的直径, 而对晶体形貌影响不大; 延长反应时间, 升高水热温度可使六边形晶片长大.     

Preparation and characterization of ZnO nanocrystallines in the presence of an ionic liquid using microwave irradiation and photocatalytic activity

Fast, simple and template-free method is proposed for preparation of ZnO nanocrystallines in the presence of 1-ethyl-3- methylimidazolium ethyl sulfate, [EMIM][EtSO₄], a room-temperature ionic liquid (RTIL) under microwave irradiation. The powder X-ray diffraction (XRD) studies display that products are excellently crystallized in the form of wurtzite hexagonal structure. Energy dispersive X-ray spectroscopy (EDX) investigations reveal that the products are extremely pure. The results obtained by scanning electron microscopy (SEM) demonstrate that mean size of ZnO nanocrystallines decreases with microwave irradiation time and the RTIL content of media. Diffuse reflectance spectra (DRS) of the ZnO nanocrystallines shows blue shift relative to the bulk ZnO, which can be attributed to quantum confinement effect of ZnO nanocrystallines. A possible formation mechanism of the ZnO nanocrystallines in aqueous solution of the RTIL is presented. Photocatalytic activity of the ZnO nanocrystallines towards photodegradation of methylene blue (MB) was carried out. The results demonstrate that photocatalytic activity of the ZnO nanocrystallines increases with microwave irradiation time and the RTIL content of media.     

Antibacterial and Photocatalytic Properties of ZnO Nanoparticles Obtained from Chemical versus Saponaria officinalis Extract-Mediated Synthesis

In the present work, the properties of ZnO nanoparticles obtained using an eco-friendly synthesis (biomediated methods in microwave irradiation) were studied. Saponaria officinalis extracts were used as both reducing and capping agents in the green nanochemistry synthesis of ZnO. Inorganic zinc oxide nanopowders were successfully prepared by a modified hydrothermal method and plant extract-mediated method. The influence of microwave irradiation was studied in both cases. The size, composition, crystallinity and morphology of inorganic nanoparticles (NPs) were investigated using dynamic light scattering (DLS), powder X-ray diffraction (XRD), SEM-EDX microscopy. Tunings of the nanochemistry reaction conditions (Zn precursor, structuring agent), ZnO NPs with various shapes were obtained, from quasi-spherical to flower-like. The optical properties and photocatalytic activity (degradation of methylene blue as model compound) were also investigated. ZnO nanopowders’ antibacterial activity was tested against Gram-positive and Gram-negative bacterial strains to evidence the influence of the vegetal extract-mediated synthesis on the biological activity.     

Pure CuCr2O4 nanoparticles: Synthesis,characterization and their morphological and size effects on the catalytic thermal decomposition of ammonium perchlorate

In the present paper a pure phase of the copper chromite spinel nanoparticles (CuCr₂O₄ SNPs) were synthesized via the sol–gel route using citric acid as a complexing agent. Then, the CuCr₂O₄ SNPs has been characterized by field emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). In the next step, with the addition of Cu–Cr–O nanoparticles (NPs), the effects of different parameters such as Cu–Cr–O particle size and the Cu/Cr molar ratios on the thermal behavior of Cu–Cr–O NPs + AP (ammonium perchlorate) mixtures were investigated. As such, the catalytic effect of the Cu–Cr–O NPs for thermal decomposition of AP was evaluated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). TGA/DSC results showed that the samples with different morphologies exhibited different catalytic activity in different stages of thermal decomposition of AP. Also, in the presence of Cu–Cr–O nanocatalysts, all of the exothermic peaks of AP shifted to a lower temperature, indicating the thermal decomposition of AP was enhanced. Moreover, the heat released (ΔH) in the presence of Cu–Cr–O nanocatalysts was increased to 1490 J g⁻¹.     

Radiation synthesis of copper sulphide/poly(vinyl alcohol) nanocomposites films: an efficient and reusable catalyst for p-nitrophenol reduction

ABSTRACT

Copper sulphide nanoparticles (CuS NPs) were in situ synthesised via irradiation process, using Poly (vinyl alcohol) (PVA) as host polymeric matrices. The as-prepared CuS/PVA nanocomposite films were characterised by X-ray diffraction (XRD) spectroscopy, ultraviolet-visible (UV-VIS) spectroscopy, Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). Both UV-VIS spectra and X-ray diffraction patterns confirmed the formation of CuS nanoparticles. The FTIR spectrum indicates the coordination between CuS nanoparticles and the OH groups of the PVA chains. The TEM image showed that the obtained CuS nanoparticles have spherical shape, monodispersed and uniform particle size distribution. The CuS/PVA nanocomposite film was successfully applied in the reduction of p-nitrophenol into p-aminophenol as a catalyst using NaBH₄ as reducing agent. The catalytic test indicates that CuS/PVA nanocomposite film has high activity for the conversion of P-NP into P-AP and effectively recycled and reused for several times.     

Zn3(OH)2V2O7·2H2O纳米片的水热制备

采用硝酸锌、五氧化二钒和氢氧化钠作为反应物,通过一个简单的CTAB辅助的水热方法制备了Zn₃(OH)₂V₂O₇·2H₂O纳米片。运用XRD,ICP-AES,FTIR,HRTEM,EDS,FE-SEM对产物的晶相和形貌进行了表征。结果表明CTAB在控制产物的形貌、尺寸分布和自组装过程中起着关键作用。同时我们研究了产物的晶体生长行为和自组装过程。     

圆形片状纳米复合材料Ag/ZnO-ZrO2微波辅助合成与多模式光催化罗丹明B

采用微波辅助结合沉淀法制备了以Zn O为主体的纳米复合材料Ag/Zn O-Zr O_2。通过X射线粉末衍射(XRD)、紫外-可见漫反射吸收光谱(UV-Vis/DRS)、扫描电子显微镜(SEM)、X射线光电子能谱(XPS)和N2吸附-脱附等表征手段研究了微波辐射对Ag/Zn O-Zr O_2晶型结构、形貌及表面物理化学性质的影响。结果表明,在200 W微波辐射作用下,该样品晶型结构未发生明显变化,但Ag的衍射峰明显增强,同时,其晶粒尺寸、光吸收性质和表面物理化学性质等方面则发生改变,尤其是样品Ag/Zn O-Zr O_2的形貌呈现了圆形片状结构。分别在紫外和微波辅助条件下对纳米复合材料的光催化性能进行了一系列考察,同时为了进一步评价所合成样品在太阳光作用下的实用价值,又考察了Ag/Zn O-Zr O_2在模拟日光条件下的光催化性能。结果显示,紫外光作用下,纳米复合材料Ag/Zn O-Zr O_2的光催化活性高于市售P25以及未经微波处理的样品,且在微波辅助光催化条件下,其活性有较大程度提高。200 W微波功率下所合成样品Ag/Zn O-Zr O_2在模拟日光作用下显现出较高活性。另外,根据紫外光条件下对光催化活性物种的捕获实验提出了Ag/Zn O-Zr O_2可能的光催化机理。