Construction of Highly Pure Nanocrystalline Heteropoly Acid Inside the Channels of Mesoporous Material with the Imprisoned Hydrolyzation Reaction of Heteropoly Acid Etherate

2008 ◽  
Vol 8 (6) ◽  
pp. 3235-3240
Author(s):  
Ying-Ying Gu ◽  
Shu-Yuan Yu ◽  
Ai-Guo Kong ◽  
Chun-Yan Hua ◽  
Han-Ming Ding ◽  
...  
Keyword(s):  
Self Assembly ◽  
Mesoporous Material ◽  
Heteropoly Acid ◽  
Building Blocks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Novel Technique ◽  
Transmission Electron ◽  
Nanocrystalline Particles ◽  
Ft Ir

A novel technique was developed to prepare highly pure heteropoly acid (HPA) nanocrystals inside mesoporous SBA-15 by the imprisoned reaction of HPA etherate and water, which was utilized as a main driving force for the transportation of building-blocks. The transmission electron microscopy, X-ray diffraction, FT-IR spectrum and NMR characterizations unambiguously demonstrate that this method allows the highly pure heteropoly acid nanocrystals with intact Keggin-type structure controlled directionally self-assembly within mesopores of silica SBA-15. Such method may open up a new entry to the highly pure multicomponent nanocrystalline particles inside the cavity of the porous materials.

scholarly journals Hydrothermal Synthesis, Characterization and Exploration of Photocatalytic Activities of Polyoxometalate: Ni-CoWO4 Nanoparticles

Crystals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 456
Author(s):  
Fahad A. Alharthi ◽  
Hamdah S. Alanazi ◽  
Amjad Abdullah Alsyahi ◽  
Naushad Ahmad
Keyword(s):  
Electron Microscopy ◽  
Hydrothermal Synthesis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Structure Morphology ◽  
Photocatalytic Activities ◽  
Ft Ir ◽  
Photocatalytic Reactions ◽  
Cobalt Tungstate

This study demonstrated the hydrothermal synthesis of bimetallic nickel-cobalt tungstate nanostructures, Ni-CoWO4 (NCW-NPs), and their phase structure, morphology, porosity, and optical properties were examined using X-ray Diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), Scanning electron microscopy- energy dispersive X-ray spectroscopy (SEM-EDS), high resolution Transmission electron microscopy (HR-TEM), Brunauer-Emmett-Teller (BET) and Raman instruments. It was found that as-calcined NCW-NPs have a monoclinic phase with crystal size ~50–60 nm and is mesoporous. It possessed smooth, spherical, and cubic shape microstructures with defined fringe distance (~0.342 nm). The photocatalytic degradation of methylene blue (MB) and rose bengal (RB) dye in the presence of NCW-NPs was evaluated, and about 49.85% of MB in 150 min and 92.28% of RB in 90 min degraded under visible light. In addition, based on the scavenger’s study, the mechanism for photocatalytic reactions is proposed.

One Step Synthesis and Characterization of Zirconia-Graphene Composites

2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  
Keyword(s):  
Synthesis And Characterization ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Graphene Composite ◽  
Transmission Electron ◽  
One Step ◽  
Ft Ir ◽  
Xrd Techniques

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.

Effect of Synthesis Temperature on Particles Size and Morphology of Zirconium Oxide Nanoparticle

2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola
Keyword(s):  
Electron Microscopy ◽  
Particle Size ◽  
Zirconium Oxide ◽  
Thermo Gravimetric Analysis ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Crystallite Sizes ◽  
Ft Ir

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.

scholarly journals Dual Light- and pH-Responsive Composite of Polyazo-Derivative Grafted Cellulose Nanocrystals

Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1725 ◽  
Author(s):  
Xiaohong Liu ◽  
Ming Li ◽  
Xuemei Zheng ◽  
Elias Retulainen ◽  
Shiyu Fu
Keyword(s):  
Cellulose Nanocrystals ◽  
Photoelectron Spectroscopy ◽  
Surface Composition ◽  
X Ray Diffraction ◽  
Responsive Materials ◽  
X Ray ◽  
Ph Response ◽  
Transmission Electron ◽  
Ft Ir ◽  
Hexyl Methacrylate

As a type of functional group, azo-derivatives are commonly used to synthesize responsive materials. Cellulose nanocrystals (CNCs), prepared by acid hydrolysis of cotton, were dewatered and reacted with 2-bromoisobuturyl bromide to form a macro-initiator, which grafted 6-[4-(4-methoxyphenyl-azo) phenoxy] hexyl methacrylate (MMAZO) via atom transfer radical polymerization. The successful grafting was supported by Fourier transform infrared spectroscopy (FT-IR) and Solid magnetic resonance carbon spectrum (MAS 13C-NMR). The morphology and surface composition of the poly{6-[4-(4-methoxyphenylazo) phenoxy] hexyl methacrylate} (PMMAZO)-grafted CNCs were confirmed with Transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The grafting rate on the macro-initiator of CNCs was over 870%, and the polydispersities of branched polymers were narrow. The crystal structure of CNCs did not change after grafting, as determined by X-ray diffraction (XRD). The polymer PMMAZO improved the thermal stability of cellulose nanocrystals, as shown by thermogravimetry analysis (TGA). Then the PMMAZO-grafted CNCs were mixed with polyurethane and casted to form a composite film. The film showed a significant light and pH response, which may be suitable for visual acid-alkali measurement and reversible optical storage.

scholarly journals Low-temperature hydrothermal synthesis of hierarchical flower-like CuB2O4 superstructures

2020 ◽  
Vol 14 (2) ◽  
pp. 113-118
Author(s):  
Daniel Ursu ◽  
Anamaria Dabici ◽  
Marinela Miclau ◽  
Nicolae Miclau
Keyword(s):  
Thermal Stability ◽  
Low Temperature ◽  
Self Assembly ◽  
Hydrothermal Solution ◽  
Optical Measurements ◽  
Oriented Attachment ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
One Step

We report for the first time the fabrication of hierarchical ordered superstructure CuB2O4 with flower-like morphology via a one-step, low temperature hydrothermal method. The tetragonal structure of CuB2O4 was determined by X-ray diffraction and high-resolution transmission electron microscopy. Optical measurements attested of the quality of the fabricated CuB2O4 and high temperature X-ray diffraction confirmed its thermal stability up to 600 ?C. The oriented attachment growth and the hierarchical self-assembly of micrometer-sized platelets producing hierarchical superstructures with flower-like morphology are designed by pH of the hydrothermal solution. The excellent band gap, high thermal stability and hierarchical structure of the CuB2O4 are promising for the photovoltaic and photocatalytic applications.

Cobalt(II) chloride adducts with acetonitrile, propan-2-ol and tetrahydrofuran: considerations on nuclearity, reactivity and synthetic applications

2017 ◽  
Vol 73 (2) ◽  
pp. 104-114 ◽  
Author(s):  
Danilo Stinghen ◽  
André Luis Rüdiger ◽  
Siddhartha O. K. Giese ◽  
Giovana G. Nunes ◽  
Jaísa F. Soares ◽  
...  
Keyword(s):  
Single Molecule ◽  
Building Blocks ◽  
Direct Reaction ◽  
X Ray Diffraction ◽  
Single Molecule Magnets ◽  
X Ray ◽  
Ft Ir ◽  
Bond Network ◽  
Solvent Molecules ◽  
Intramolecular Hydrogen

High-spin cobalt(II) complexes are considered useful building blocks for the synthesis of single-molecule magnets (SMM) because of their intrinsic magnetic anisotropy. In this work, three new cobalt(II) chloride adducts with labile ligands have been synthesized from anhydrous CoCl2, to be subsequently employed as starting materials for heterobimetallic compounds. The products were characterized by elemental, spectroscopic (EPR and FT–IR) and single-crystal X-ray diffraction analyses.trans-Tetrakis(acetonitrile-κN)bis(tetrahydrofuran-κO)cobalt(II) bis[(acetonitrile-κN)trichloridocobaltate(II)], [Co(C2H3N)4(C4H8O)2][CoCl3(C2H3N)]2, (1), comprises mononuclear ions and contains both acetonitrile and tetrahydrofuran (thf) ligands, The coordination polymercatena-poly[[tetrakis(propan-2-ol-κO)cobalt(II)]-μ-chlorido-[dichloridocobalt(II)]-μ-chlorido], [Co2Cl4(C3H8O)4], (2′), was prepared by direct reaction between anhydrous CoCl2and propan-2-ol in an attempt to rationalize the formation of the CoCl2–alcohol adduct (2), probably CoCl2(HOiPr)m. The binuclear complex di-μ-chlorido-1:2κ4Cl:Cl-dichlorido-2κ2Cl-tetrakis(tetrahydrofuran-1κO)dicobalt(II), [Co2Cl4(C4H8O)4], (3), was obtained from (2) after recrystallization from tetrahydrofuran. All three products present cobalt(II) centres in both octahedral and tetrahedral environments, the former usually less distorted than the latter, regardless of the nature of the neutral ligand. Product (2′) is stabilized by an intramolecular hydrogen-bond network that appears to favour atransarrangement of the chloride ligands in the octahedral moiety; this differs from thecisdisposition found in (3). The expected easy displacement of the bound solvent molecules from the metal coordination sphere makes the three compounds good candidates for suitable starting materials in a number of synthetic applications.

scholarly journals A novel technique to synthesis of tenorite (CuO) nanoparticles from low concentration CuSO4 solution

2011 ◽  
Vol 47 (1) ◽  
pp. 73-78 ◽  
Author(s):  
E. Darezereshki ◽  
F. Bakhtiari
Keyword(s):  
Electron Microscopy ◽  
Decomposition Method ◽  
Raw Materials ◽  
Spherical Shape ◽  
Cuo Nanoparticles ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermal Decomposition Method ◽  
Novel Technique ◽  
Transmission Electron

In this study CuO nanoparticles were prepared via direct thermal decomposition method using basic copper sulphates as wet chemically synthesized precursor which was calcined in air at 750?C for 2h. Samples were characterized by thermogravimetric (TG-DSC), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), infrared spectrum (IR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The XRD, EDS, and IR results indicated that the synthesized CuO particles were pure. The SEM and TEM results showed that the CuO nanoparticles were of approximate spherical shape, and 170?5 nm in size. Using this method, Cuo nanoparticles could be produced without using organic solvent, expensive raw materials, and complicated equipment.

Synthesis of Indole Derivatives Using Biosynthesized ZnO-CaO Nanoparticles as an Efficient Catalyst

2021 ◽  
Vol 66 ◽  
pp. 61-71
Author(s):  
Tahereh Heidarzadeh ◽  
Navabeh Nami ◽  
Daryoush Zareyee
Keyword(s):  
Electron Microscopy ◽  
Indole Derivatives ◽  
X Ray Diffraction ◽  
Efficient Catalyst ◽  
X Ray ◽  
Transmission Electron ◽  
Solvent Free Conditions ◽  
Ft Ir ◽  
Eggshell Waste ◽  
Aromatic And Aliphatic Amines

The principal aim of this research is using biosynthesized ZnO-CaO nanoparticles (NPs) for preparation of indole derivatives. ZnO-CaO NPs have been prepared using Zn(CH3COO)2 and eggshell waste powder in solvent-free conditions. Morphology and structure of NPs were determined by FT-IR, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy dispersive spectra (EDS). It was used as a highly efficient catalyst for the synthesis of indole derivatives. Some indole derivatives were synthesized by the reaction of indole, formaldehyde, aromatic and aliphatic amines in the presence of ZnO-CaO NPs (5 mol%) in ethanol under reflux conditions. The assigned structure was further established by CHN analyses, NMR, and FT-IR spectra. Because of excellent capacity, the exceedingly simple workup and good yield, eco-friendly catalyst ZnO-CaO NPs were proved to be a good catalyst for this reaction.

scholarly journals Preparation, Characterization, and Performance Analysis of S-Doped Bi2MoO6 Nanosheets

Nanomaterials ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 1341 ◽  
Author(s):  
Ruiqi Wang ◽  
Duanyang Li ◽  
Hailong Wang ◽  
Chenglun Liu ◽  
Longjun Xu
Keyword(s):  
Photoelectron Spectroscopy ◽  
Degradation Rate ◽  
X Ray Diffraction ◽  
Photo Degradation ◽  
X Ray ◽  
Transmission Electron ◽  
Ft Ir ◽  
And Performance ◽  
Adsorption Desorption ◽  
Excellent Stability

S-doped Bi2MoO6 nanosheets were successfully synthesized by a simple hydrothermal method. The as-prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), N2 adsorption–desorption isotherms, Raman spectroscopy, Fourier transform infrared spectroscopy (FT-IR), elemental mapping spectroscopy, photoluminescence spectra (PL), X-ray photoelectron spectroscopy (XPS), and UV-visible diffused reflectance spectra (UV-vis DRS). The photo-electrochemical performance of the samples was investigated via an electrochemical workstation. The S-doped Bi2MoO6 nanosheets exhibited enhanced photocatalytic activity under visible light irradiation. The photo-degradation rate of Rhodamine B (RhB) by S-doped Bi2MoO6 (1 wt%) reached 97% after 60 min, which was higher than that of the pure Bi2MoO6 and other S-doped products. The degradation rate of the recovered S-doped Bi2MoO6 (1 wt%) was still nearly 90% in the third cycle, indicating an excellent stability of the catalyst. The radical-capture experiments confirmed that superoxide radicals (·O2−) and holes (h+) were the main active substances in the photocatalytic degradation of RhB by S-doped Bi2MoO6.

scholarly journals Influence of different synthesis conditions on properties of oleic acid-coated-Fe3O4 nanoparticles

2015 ◽  
Vol 33 (1) ◽  
pp. 100-106 ◽  
Author(s):  
Atieh Aliakbari ◽  
Majid Seifi ◽  
Sharareh Mirzaee ◽  
Hoda Hekmatara
Keyword(s):  
Oleic Acid ◽  
Room Temperature ◽  
Magnetic Measurement ◽  
Precursor Solution ◽  
Vibrating Sample Magnetometer ◽  
X Ray Diffraction ◽  
X Ray ◽  
Synthesis Conditions ◽  
Transmission Electron ◽  
Ft Ir

AbstractIn the present paper, iron oxide nanoparticles coated by oleic acid have been synthesized in different conditions by coprecipitation method. For investigating the effect of time spent on adding the oleic acid to the precursor solution, two different processes have been considered. The as synthesized samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FT-IR). Magnetic measurement was carried out at room temperature using a vibrating sample magnetometer (VSM). The results show that the magnetic nanoparticles decorated with oleic acid decreased the saturation of magnetization. From the data, it can also be concluded that the magnetization of Fe3O4/oleic acid nanoparticles depends on synthesis conditions.

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