scholarly journals Phase-Selective Microwave Assisted Synthesis of Iron(III) Aminoterephthalate MOFs

Materials ◽  
2020 ◽  
Vol 13 (6) ◽  
pp. 1469 ◽  
Author(s):  
Ana Arenas-Vivo ◽  
David Avila ◽  
Patricia Horcajada
Keyword(s):  
Reaction Medium ◽  
Microwave Assisted Synthesis ◽  
X Ray Diffraction ◽  
Synthetic Strategy ◽  
Transmission Electron ◽  
Metal Organic ◽  
High Space ◽  
Pure Phases ◽  
The Impact ◽  
Reaction Media

Iron(III) aminoterephthalate Metal-Organic Frameworks (Fe-BDC-NH2 MOFs) have been demonstrated to show potential for relevant industrial and societal applications (i.e., catalysis, drug delivery, gas sorption). Nevertheless, further analysis is required in order to achieve their commercial production. In this work, a systematic synthetic strategy has been followed, carrying out microwave (MW) assisted hydro/solvothermal reactions to rapidly evaluate the influence of different reaction parameters (e.g., time, temperature, concentration, reaction media) on the formation of the benchmarked MIL-101-NH2, MIL-88B-NH2, MIL-53-NH2 and MIL-68-NH2 solids. Characterization of the obtained solids by powder X-ray diffraction, dynamic light scattering and transmission electron microscopy allowed us to identify trends to the contribution of the evaluated parameters, such as the relevance of the concentration of precursors and the impact of the reaction medium on phase crystallization. Furthermore, we presented here for the first time the MW assisted synthesis of MIL-53-NH2 in water. In addition, pure MIL-101-NH2 was also produced in water while MIL-88-NH2 was the predominant phase obtained in ethanol. Pure phases were produced with high space-time yields, unveiling the potential of MW synthesis for MOF industrialization.

scholarly journals The impact of crystal size and temperature on the adsorption-induced flexibility of the Zr-based metal-organic framework DUT-98

2019 ◽  
Author(s):  
Simon Krause ◽  
Volodymyr Bon ◽  
Hongchu Du ◽  
Rafal E Dunin-Borkowski ◽  
Ulrich Stoeck ◽  
...  
Keyword(s):  
Crystal Size ◽  
Metal Organic Framework ◽  
Type I ◽  
Adsorption Behaviour ◽  
X Ray Diffraction ◽  
Transmission Electron ◽  
Adsorption Of Nitrogen ◽  
Metal Organic ◽  
The Impact ◽  
Organic Framework

In this contribution we analyse the influence of adsorption cycling, crystal size, and temperature on the switching behaviour of the flexible Zr-based metal-organic framework DUT-98. We observe a shift in the gate opening pressure upon cycling of adsorption experiments of micro meter-sized crystals and assign this to a fragmentation of the crystals. In a series of modulated syntheses we downsize the average crystal size of DUT-98 crystals from 120 µm to 50 nm and characterize the obtained solids by X-ray diffraction, infrared spectroscopy, as well as scanning and transmission electron microscopy. We analyse the adsorption behaviour by nitrogen and water adsorption at 77 K and 298 K, respectively and show that adsorption-induced flexibility is only observed for micro meter-sized crystals. Nanometer-sized crystals were found to exhibit reversible type I adsorption behaviour upon adsorption of nitrogen and exhibit a crystal-size dependent steep water uptake of up to 20 mmol g-1 at 0.5 p/p 0 with potential for water harvesting and heat pump applications. We furthermore investigate the temperature-induced structural transition by in situ PXRD. At temperatures beyond 110 °C the open pore state of nano meter-sized DUT-98 crystals are found to irreversibly transform in a closed pore state. The connection of crystal fragmentation upon adsorption cycling and the crystal size-dependence of the adsorption-induced flexibility is an important finding for evaluation of these materials in future adsorption-based applications. This work thus extends the limited amount of studies on crystal size effects in flexible MOFs and hopefully motivates further investigations into this field.

scholarly journals Controlled Synthesis of CuS and Cu9S5 and Their Application in the Photocatalytic Mineralization of Tetracycline

Catalysts ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 899
Author(s):  
Murendeni P. Ravele ◽  
Opeyemi A. Oyewo ◽  
Damian C. Onwudiwe
Keyword(s):  
Electron Microscopy ◽  
Visible Light ◽  
Blue Shift ◽  
X Ray Diffraction ◽  
X Ray ◽  
Copper Sulfides ◽  
Transmission Electron ◽  
Single Source Precursor ◽  
Pure Phase ◽  
Pure Phases

Pure-phase Cu2−xS (x = 1, 0.2) nanoparticles have been synthesized by the thermal decomposition of copper(II) dithiocarbamate as a single-source precursor in oleylamine as a capping agent. The compositions of the Cu2−xS nanocrystals varied from CuS (covellite) through the mixture of phases (CuS and Cu7.2S4) to Cu9S5 (digenite) by simply varying the temperature of synthesis. The crystallinity and morphology of the copper sulfides were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), which showed pure phases at low (120 °C) and high (220 °C) temperatures and a mixture of phases at intermediate temperatures (150 and 180 °C). Covellite was of a spherical morphology, while digenite was rod shaped. The optical properties of these nanocrystals were characterized by UV−vis–NIR and photoluminescence spectroscopies. Both samples had very similar absorption spectra but distinguishable fluorescence properties and exhibited a blue shift in their band gap energies compared to bulk Cu2−xS. The pure phases were used as catalysts for the photocatalytic degradation of tetracycline (TC) under visible-light irradiation. The results demonstrated that the photocatalytic activity of the digenite phase exhibited higher catalytic degradation of 98.5% compared to the covellite phase, which showed 88% degradation within the 120 min reaction time using 80 mg of the catalysts. The higher degradation efficiency achieved with the digenite phase was attributed to its higher absorption of the visible light compared to covellite.

scholarly journals The impact of point defects in n-type GaN layers on thermal decomposition of InGaN/GaN QWs

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Mikolaj Grabowski ◽  
Ewa Grzanka ◽  
Szymon Grzanka ◽  
Artur Lachowski ◽  
Julita Smalc-Koziorowska ◽  
...  
Keyword(s):  
Quantum Wells ◽  
High Temperatures ◽  
Point Defects ◽  
X Ray Diffraction ◽  
Helium Ions ◽  
X Ray ◽  
Sapphire Substrates ◽  
Transmission Electron ◽  
The Impact ◽  
Ingan Quantum Wells

AbstractThe aim of this paper is to give an experimental evidence that point defects (most probably gallium vacancies) induce decomposition of InGaN quantum wells (QWs) at high temperatures. In the experiment performed, we implanted GaN:Si/sapphire substrates with helium ions in order to introduce a high density of point defects. Then, we grew InGaN QWs on such substrates at temperature of 730 °C, what caused elimination of most (but not all) of the implantation-induced point defects expanding the crystal lattice. The InGaN QWs were almost identical to those grown on unimplanted GaN substrates. In the next step of the experiment, we annealed samples grown on unimplanted and implanted GaN at temperatures of 900 °C, 920 °C and 940 °C for half an hour. The samples were examined using Photoluminescence, X-ray Diffraction and Transmission Electron Microscopy. We found out that the decomposition of InGaN QWs started at lower temperatures for the samples grown on the implanted GaN substrates what provides a strong experimental support that point defects play important role in InGaN decomposition at high temperatures.

Epitaxial Ferroelectric BaTiO3 Thin Films for Microphotonic Applications

2000 ◽  
Vol 637 ◽  
Author(s):  
F. Niu ◽  
A.R. Teren ◽  
B.H. Hoerman ◽  
B.W. Wessels
Keyword(s):  
Thin Films ◽  
Chemical Vapor ◽  
Silicon Substrates ◽  
X Ray Diffraction ◽  
Insulating Layer ◽  
Ferroelectric State ◽  
Transmission Electron ◽  
Electro Optic ◽  
Metal Organic ◽  
Mgo Layers

AbstractEpitaxial ferroelectric BaTiO3 thin films have been developed as a material for microphotonics. Efforts have been directed toward developing these materials for thin film electro-optic modulators. Films were deposited by metalorganic chemical vapor deposition (MOCVD) on both MgO and silicon substrates. The electro-optic properties of the thin films were measured. For BaTiO3 thin films grown on (100) MgO substrates, the effective electro-optic coefficient, reff depended on the magnitude and direction of the electric field. Coefficients as high as 260 pm/V have been measured. Investigation of BaTiO3 films on silicon has been undertaken. Epitaxial BaTiO3 thin films were deposited by MOCVD on (100) MgO layers grown on silicon (100) substrates by metal-organic molecular beam epitaxy (MOMBE). The MgO serves as the low index optical cladding layer as well as an insulating layer. X-ray diffraction and transmission electron microscopy (TEM) indicated that BaTiO3 was epitaxial with an orientational relation given by BaTiO3 (100)//Si (100) and BaTiO3[011]//Si [011]. Polarization measurements indicated that the BaTiO3 epitaxial films on Si were in the ferroelectric state.

Evaluation of Surfactants on Thermo-Physical Properties of Magnesia-Oil Nanofluid

2018 ◽  
Vol 928 ◽  
pp. 106-112 ◽  
Author(s):  
Abdallah Yousef Mohammed Ali ◽  
Ahmed H. El-Shazly ◽  
M.F. Elkady ◽  
S.E. AbdElhafez
Keyword(s):  
Vinyl Pyrrolidone ◽  
Poly Vinyl Alcohol ◽  
Ammonium Bromide ◽  
X Ray Diffraction ◽  
Mgo Nanoparticles ◽  
Transmission Electron ◽  
Wet Chemical ◽  
Cetyl Trimethyl Ammonium ◽  
Poly Vinyl Pyrrolidone ◽  
The Impact

The prime purpose of the current study was to investigate the consequence of surfactant on the kinematic viscosity, thermal conductivity, and stability of MgO-oil based nanofluid. Magnesia (MgO) nanoparticles were prepared by the wet chemical method. Structural and morphological analysis of synthesized nanoparticles were performed via X-ray diffraction (XRD) and Transmission electron microscope (TEM). Subsequently, nanofluid was prepared at a solid concentration of 0.025% in presence of various surfactants with the aid of ultrasonic technique. The impact of the different surfactants (Cetyl Trimethyl Ammonium Bromide (CTAB), Poly Vinyl Pyrrolidone (PVP), Poly Vinyl Alcohol (PVA), and Oleic Acid) on the nanofluid stability was tested. It was evident that CTAB and PVA surfactants establish the most stable prepared MgO-oil based nanofluid. The experiments revealed that the maximum UV–Vis absorbance of the solution corresponds to the dispersion of CTAB in the base fluid.

Changing the morphology of one-dimensional titanate nanostructures affects its tissue distribution and toxicity

2020 ◽  
Vol 36 (4) ◽  
pp. 272-286
Author(s):  
Nahla Kamal ◽  
AH Zaki ◽  
Ahmed AG El-Shahawy ◽  
Ossama M Sayed ◽  
SI El-Dek
Keyword(s):  
Tissue Distribution ◽  
Surface Area ◽  
Inductively Coupled Plasma ◽  
Histopathological Analysis ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
Inductively Coupled ◽  
Transmission Electron ◽  
Titanate Nanostructures ◽  
The Impact

The present research investigated the impact of the morphology change of titanate (TiO2) nanostructures on its tissue distribution and toxicity. The TiO2 nanotubes, rods, and ribbons were synthesized by the hydrothermal technique, and the morphology was adjusted by alteration of the hydrothermal duration time. The characterization techniques were X-ray diffraction, high-resolution transmission electron microscopy, dynamic light scattering, and the Brunauer–Emmett–Teller method for measuring the surface area. The intravenously administrated dose (5 mg/kg) was injected as a single dose for 1 day and consecutively for 42 days. The quantitative analysis of accumulated TiO2 nanostructures in the liver, spleen, and the heart was performed using an inductively coupled plasma emission spectrometer, and the organs’ toxicity was estimated by histopathological analysis. The prepared nanostructures exhibited differences in morphology, crystallinity, size distribution, surface area, zeta potential, and aspect ratio. The results revealed a tissue distribution difference between the liver, spleen, and heart of these nanostructures, the distribution order was the liver, spleen, and the heart for all TiO2 nanostructures. The toxicity was induced with different degrees. The nanotubes were the most harmful among the three formats. In summary, changes in the morphology of the TiO2 nanostructures change its distribution and toxicity.

scholarly journals Development of a Novel Method for the Fabrication of Nanostructured Zr(x)Ni(y) Catalyst to Enhance the Desorption Properties of MgH2

Catalysts ◽  
2020 ◽  
Vol 10 (8) ◽  
pp. 849
Author(s):  
Gracia Shokano ◽  
Zahir Dehouche ◽  
Basile Galey ◽  
Georgeta Postole
Keyword(s):  
Hydrogen Desorption ◽  
Milling Process ◽  
Hydrogen Release ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Electron Microscope Analysis ◽  
Novel Method ◽  
Temperature Programmed ◽  
The Impact

The present work involves the development of a novel method for the fabrication of zirconium nickel (Zr(x)Ni(y)) alloy used as a nanocatalyst to improve the hydrogen storage properties of the Mg/MgH2 system. The catalyst was fabricated through the high-pressure reactor and activated under hydrogen prior to being mechanically milled with the MgH2 for 5 h under argon. The microstructure characterisation of the samples was determined via SEM-EDX (scanning electron microscope analysis–energy dispersive X-ray spectroscopy), XRD (X-ray diffraction) and FE-HRTEM (field emission high resolution transmission electron microscopy), and the desorption characteristic of the nanocomposite (10 wt.% Zr(x)Ni(y)–MgH2) was determined via TPD (temperature-programmed desorption). The nanostructured MgH2 powder milled with 10 wt.% of the activated Zr(x)Ni(y) based nanocatalyst resulted in a faster hydrogen release—5.9 H2-wt.% at onset temperature 210 °C/peak temperature 232 °C. The observed significant improvement in the hydrogen desorption properties was likely to be the result of the impact of the highly dispersed catalyst on the surface of the Mg/MgH2 system, the reduction in particle size during the ball milling process and/or the formation of Mg0.996Zr0.004 phase during the milling process.

scholarly journals The impact of crystal size and temperature on the adsorption-induced flexibility of the Zr-based metal–organic framework DUT-98

2019 ◽  
Vol 10 ◽  
pp. 1737-1744 ◽  
Author(s):  
Simon Krause ◽  
Volodymyr Bon ◽  
Hongchu Du ◽  
Rafal E Dunin-Borkowski ◽  
Ulrich Stoeck ◽  
...  
Keyword(s):  
Crystal Size ◽  
Metal Organic Framework ◽  
Adsorption Behavior ◽  
Switching Behavior ◽  
Type I ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
The Impact ◽  
Organic Framework

In this contribution we analyze the influence of adsorption cycling, crystal size, and temperature on the switching behavior of the flexible Zr-based metal–organic framework DUT-98. We observe a shift in the gate-opening pressure upon cycling of adsorption experiments for micrometer-sized crystals and assign this to a fragmentation of the crystals. In a series of samples, the average crystal size of DUT-98 crystals was varied from 120 µm to 50 nm and the obtained solids were characterized by X-ray diffraction, infrared spectroscopy, as well as scanning and transmission electron microscopy. We analyzed the adsorption behavior by nitrogen and water adsorption at 77 K and 298 K, respectively, and show that adsorption-induced flexibility is only observed for micrometer-sized crystals. Nanometer-sized crystals were found to exhibit reversible type I adsorption behavior upon adsorption of nitrogen and exhibit a crystal-size-dependent steep water uptake of up to 20 mmol g−1 at 0.5 p/p 0 with potential for water harvesting and heat pump applications. We furthermore investigate the temperature-induced structural transition by in situ powder X-ray diffraction. At temperatures beyond 110 °C, the open-pore state of the nanometer-sized DUT-98 crystals is found to irreversibly transform to a closed-pore state. The connection of crystal fragmentation upon adsorption cycling and the crystal size dependence of the adsorption-induced flexibility is an important finding for evaluation of these materials in future adsorption-based applications. This work thus extends the limited amount of studies on crystal size effects in flexible MOFs and hopefully motivates further investigations in this field.

A Critical Investigation on the Existence of Selective Microwave Absorption in the Synthesis of CdSe Quantum Dots

2014 ◽  
Vol 67 (9) ◽  
pp. 1180 ◽  
Author(s):  
Mojtaba Mirhosseini Moghaddam ◽  
C. Oliver Kappe
Keyword(s):  
Quantum Dots ◽  
Microwave Absorption ◽  
Transmission Electron Microscopy Data ◽  
Microwave Assisted Synthesis ◽  
Cdse Quantum Dots ◽  
X Ray Diffraction ◽  
Heating And Cooling ◽  
Transmission Electron ◽  
Microscopy Data ◽  
Heating Mode

The existence of selective microwave absorption phenomena in the synthesis of CdSe quantum dots has been investigated. These types of microwave effects involving selective microwave absorption by specific reagents have recently been proposed in the microwave-assisted synthesis of various nanoparticles. In the present study, the microwave synthesis of CdSe quantum dots was investigated according to a protocol published by Washington and Strouse to clarify the presence of selective microwave heating. Importantly, control experiments involving conventional conductive heating were executed under otherwise (except for the heating mode) identical conditions, ensuring the same heating and cooling profiles, stirring rates, and reactor geometries. Comparison of powder X-ray diffraction, UV-vis, photoluminescence, and transmission electron microscopy data of the obtained CdSe quantum dots reveals that identical types of nanoparticles are obtained independently of the heating mode. Therefore, no evidence for a selective microwave absorption phenomenon could be obtained.

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