scholarly journals Investigation of Thermal Behavior of Layered Double Hydroxides Intercalated with Carboxymethylcellulose Aiming Bio-Carbon Based Nanocomposites

2019 ◽  
Vol 3 (2) ◽  
pp. 55
Author(s):  
Vagner R. Magri ◽  
Alfredo Duarte ◽  
Gustavo F. Perotti ◽  
Vera R.L. Constantino
Keyword(s):  
Layered Double Hydroxides ◽  
Mixed Oxides ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Experimental Conditions ◽  
X Ray ◽  
Vibrational Spectroscopies ◽  
Xrd Patterns ◽  
Double Hydroxides ◽  
The Degree Of Crystallinity

Carboxymethylcellulose (CMC), a polymer derived from biomass, was intercalated into layered double hydroxides (LDH) composed by M2+/Al3+ (M2Al-CMC, M = Mg or Zn) and evaluated as precursors for the preparation of biocarbon-based nanocomposites by pyrolysis. M2Al-CMC hybrids were obtained by coprecipitation and characterized by X ray diffraction (XRD), vibrational spectroscopies, chemical analysis, and thermal analysis coupled to mass spectrometry. Following, pyrolyzed materials obtained between 500–1000 °C were characterized by XRD, Raman spectroscopy, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Above 600 °C, Raman spectra of all samples showed the presence of graphitic carbon, which plays a role in the degree of crystallinity of produced inorganic phases (for comparison purposes, M2Al-CO3 materials were investigated after calcination in the same experimental conditions). XRD patterns of Mg2Al-CMC pyrolyzed between 600–1000 °C showed poorly crystallized MgO and absence of spinel reflections, whereas for Zn2Al-CMC, it was observed well crystallized nanometric ZnO at 800 °C, and ZnAl2O4 and γ-Al2O3 phases at 1000 °C. Above 800 °C, the carbothermic reaction was noticed, transforming ZnO to zinc vapour. This study opens perspectives for nanocomposites preparation based on carbon and inorganic (mixed) oxides through precursors having organic-inorganic interactions at the nanoscale domain.

Effect of Ethylene Sulphite on the Conductivity and Morphology of PEO-KOH Films

2006 ◽  
Vol 517 ◽  
pp. 89-92
Author(s):  
M.F. Hassan ◽  
N.H. Idris ◽  
S.R. Majid ◽  
Tan Winie ◽  
A.S.A. Khiar ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Electrochemical Impedance ◽  
Degree Of Crystallinity ◽  
Number Density ◽  
X Ray Diffraction ◽  
X Ray ◽  
Xrd Patterns ◽  
Mobile Ions ◽  
The Degree Of Crystallinity ◽  
Scanning Electron

The plasticized PEO-KOH films have been investigated using the electrochemical impedance spectroscopy (EIS), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The conductivity of films increased by about 2 orders of magnitude from 10-5 to 10-3 S cm-1 at r.t. on addition of 0.5 wt.% of ethylene sulphite (ES). The degree of crystallinity was calculated from the XRD patterns. SEM micrographs show that the plasticized films were porous. The highest conductivity of plasticized films at r.t. was (1.3 ± 0.2) x 10-3 S cm-1 for the film with 0.5 wt.% of ES content. The number density of mobile ions was shown to increase indicating that ES has dissociated more salts into ions and thereby increasing the conductivity.

scholarly journals Structural analysis of defects in layered double hydroxides and related mixed oxides

2019 ◽  
Vol 62 (1-2) ◽  
pp. 39-54
Author(s):  
N.N. Leont’eva ◽  
V.A. Drozdov ◽  
O.B. Belskaya ◽  
S.V. Cherepanova
Keyword(s):  
Layered Double Hydroxides ◽  
Mixed Oxides ◽  
Simulation Method ◽  
X Ray Diffraction ◽  
Structural Mechanism ◽  
X Ray ◽  
Physicochemical Methods ◽  
The Difference ◽  
Double Hydroxides

This article provides an overview of the results of studying the defects in the structure of MgAl and NiAl layered double hydroxides and their thermal decomposition products up to 1000 °C, obtained over the last 10 years in the laboratory of analytical and physicochemical methods of research at the Institute of Hydrocarbons Processing of the SB RAS. The presented results were performed using the X-ray diffraction pattern simulation method for onedimensional (1D) disordered crystals. Changes in the type of structure defects are found depending on the calcination temperature, including in situ X-ray diffraction. A structural mechanism for the formation of a dehydrated phase at T=200 °C is proposed. New models of MgAl and NiAl oxide structures are presented. The structures of the phases included in the products of hydration of oxides are established. The difference in the behavior of oxides during hydration is explained.

scholarly journals Photocatalytic Degradation of 2,4,6-Trichlorophenol by MgO–MgFe2O4 Derived from Layered Double Hydroxide Structures

Catalysts ◽  
2019 ◽  
Vol 9 (5) ◽  
pp. 454 ◽  
Author(s):  
Esthela Ramos-Ramírez ◽  
Francisco Tzompantzi-Morales ◽  
Norma Gutiérrez-Ortega ◽  
Héctor G. Mojica-Calvillo ◽  
Julio Castillo-Rodríguez
Keyword(s):  
Photocatalytic Degradation ◽  
Layered Double Hydroxides ◽  
X Ray Diffraction ◽  
Application Study ◽  
Toxic Compounds ◽  
X Ray ◽  
Thermally Activated ◽  
Double Hydroxide ◽  
Double Hydroxides ◽  
Scanning Electron

In recent years, the search for solutions for the treatment of water pollution by toxic compounds such as phenols and chlorophenols has been increasing. Phenols and their derivatives are widely used in the manufacture of pesticides, insecticides, paper, and wood preservers, among other things. Chlorophenols are partially biodegradable but not directly photodegradable by sunlight and are extremely toxic—especially 2,4,6-trichlorophenol, which is considered to be potentially carcinogenic. As a viable proposal to be applied in the treatment of water contaminated with 2,4,6-trichlorophenol, this paper presents an application study of the thermally activated Mg/Fe layered double hydroxides as photocatalysts for the mineralization of this contaminant. Activated Mg/Fe layered double hydroxides were characterized by X-ray diffraction, thermal analysis, N2 physisorption, and scanning electron microscopy with X-ray dispersive energy. The results of the photocatalytic degradation of 2,4,6-trichlorophenol in aqueous solution showed good photocatalytic activity, with an efficiency of degradation of up to 93% and mineralization of 82%; degradation values which are higher than that of TiO2-P25, which only reached 18% degradation. The degradation capacity is attributed to the structure of the MgO–MgFe2O4 oxides derived from double laminate hydroxide Mg/Fe. A path of degradation based on a mechanism of superoxide and hollow radicals is proposed.

Preparation of nanocellulose by hydrolysis with ionic liquids and two-step hydrolysis with ionic liquids and enzymes

2021 ◽  
Vol 116 ◽  
pp. 5-14
Author(s):  
Marta Babicka ◽  
Magdalena Woźniak ◽  
Kinga Szentner ◽  
Sławomir Borysiak ◽  
Krzysztof Dwiecki ◽  
...  
Keyword(s):  
Ionic Liquids ◽  
Degree Of Crystallinity ◽  
Cellulolytic Enzyme ◽  
X Ray Diffraction ◽  
Production Methods ◽  
Step Process ◽  
X Ray ◽  
One Step ◽  
Xrd Patterns ◽  
The One

The aim of this study was to compare parameters of nanocellulose obtained by two different procedures: hydrolysis with ionic liquids (1-allyl-3-methylimidazolium chloride and 1-ethyl-3-methylimidazolium acetate) and hydrolysis with ionic liquids in combination with hydrolysis using a cellulolytic enzyme from Trichoderma reesei. Avicel cellulose was treated with two ionic liquids: 1-allyl-3-methylimidazolium chloride (AmimCl) and 1-ethyl 3-methylimidazolium acetate (EmimOAc). In the two-step hydrolysis cellulose after treatment with ionic liquids was additionally hydrolyzed with a solution of enzymes. In order to characterize the obtained material, the following analyses were used: infrared spectroscopy, X-ray diffraction and dynamic light scattering. The results indicated that cellulose obtained by two-step nanocellulose production methods (first hydrolysis with ionic liquids and then with enzymes) showed similar parameters (particle size, XRD patterns and degree of crystallinity) as the material after the one-step process, i.e. hydrolysis with ionic liquids.

scholarly journals Characterization of Serpentines from Different Regions by Transmission Electron Microscopy, X-ray Diffraction, BET Specific Surface Area and Vibrational and Electronic Spectroscopy

Fibers ◽  
2019 ◽  
Vol 7 (5) ◽  
pp. 47 ◽  
Author(s):  
Miguel A. Rivero Crespo ◽  
Dolores Pereira Gómez ◽  
María V. Villa García ◽  
José M. Gallardo Amores ◽  
Vicente Sánchez Escribano
Keyword(s):  
Electron Microscopy ◽  
Relative Intensity ◽  
Electronic Spectroscopy ◽  
Visible Region ◽  
Band Gap Energy ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Oh Groups ◽  
X Ray ◽  
Xrd Patterns

Serpentinite powdered samples from four different regions were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), SBET and porosity measurements, UV-Vis and Infrared Spectroscopy of the skeletal region and surface OH groups. SEM micrographs of the samples showed a prismatic morphology when the lizardite was the predominant phase, while if antigorite phase prevailed, the particles had a globular morphology. The few fibrous-shaped particles, only observed by SEM and weakly detected by XRD on MO-9C and MO13 samples, were characteristic of the chrysotile phase. All diffraction XRD patterns showed characteristic peaks of antigorite and lizardite serpentine phases, with crystallite sizes in the range 310–250 Å and with different degrees and types of carbonation processes, one derived from the transformation of the serpentine, generating dolomite, and another by direct precipitation of calcite. The SBET reached values between 38–24 m2∙g−1 for the samples less crystalline, in agreement with the XRD patterns, while those with a higher degree of crystallinity gave values close to 8–9 m2∙g−1. In the UV region all electronic spectra were dominated by the absorption edge due to O2− → Si4+ charge transfer transition, with Si4+ in tetrahedral coordination, corresponding to a band gap energy of ca 4.7 eV. In the visible region, 800–350 nm, the spectra of all samples, except Donai, presented at least two weak and broad absorptions centred in the range 650–800 and 550–360 nm, associated with the presence of Fe3+ ions from the oxidation of structural Fe2+ ions in the serpentinites ((MgxFe2+1−x)3Si2O5(OH)4). The relative intensity of the IR bands corresponding to the stretching modes of the OH’s groups indicated the prevalence of one of the two phases, antigorite or lizardite, in the serpentinites. We proposed that the different relative intensity of these bands could be considered as diagnostic to differentiate the predominance of these phases in serpentinites.

scholarly journals Hemp Fibre Reinforced Poly(Lactic Acid) Composites

2007 ◽  
Vol 29-30 ◽  
pp. 337-340 ◽  
Author(s):  
M.A. Sawpan ◽  
K.L. Pickering ◽  
Alan Fernyhough
Keyword(s):  
Lactic Acid ◽  
Degree Of Crystallinity ◽  
Poly Lactic Acid ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Hemp Fibre ◽  
Reinforcing Material ◽  
Fibre Loading ◽  
The Degree Of Crystallinity

The potential of hemp fibre as a reinforcing material for Poly(lactic acid) (PLA) was investigated. Good interaction between hemp fibre and PLA resulted in increases of 100% for Young’s modulus and 30% for tensile strength of composites containing 30 wt% fibre. Different predictive ‘rule of mixtures’ models (e.g. Parallel, Series and Hirsch) were assessed regarding the dependence of tensile properties on fibre loading. Limited agreement with models was observed. Differential scanning calorimetry (DSC) and x-ray diffraction (XRD) studies showed that hemp fibre increased the degree of crystallinity in PLA composites.

scholarly journals High efficient photocatalytic activity of Zn-Al-Ti layered double hydroxides nanocomposite

2018 ◽  
Vol 149 ◽  
pp. 01087 ◽  
Author(s):  
F. Amor ◽  
A. Diouri ◽  
I. Ellouzi ◽  
F. Ouanji ◽  
M. Kacimi
Keyword(s):  
Methylene Blue ◽  
Photocatalytic Activity ◽  
Uv Irradiation ◽  
Layered Double Hydroxides ◽  
Removal Rate ◽  
X Ray Diffraction ◽  
Simple Method ◽  
X Ray ◽  
High Efficient ◽  
Double Hydroxides

This work establishes a simple method for synthesising layered double hydroxides (LDHs) powders with coprecipitation. The characteristics of the samples were investigated y X-ray diffraction (XRD), scanning electron microscopy (SEM) and spectrophotometer UV–Vis (DRS). Non-uniform distribution was shown for LDHs samples by SEM. Photocatalytic efficiencies were tested using methylene blue (MB) dye as a model contaminant under UV irradiation. In particular, Zn–Al-Ti LDH exhibited an excellent performance towards MB degradation compared with commercial TiO2 nanoparticles. Methylene blue removal percentage was reached at almost 100%, whereas commercial TiO2 reached a removal rate of only 66% under the same conditions within 20 min. The aim of the current work is to prepare Zn-Al-Ti layered double hydroxides nanocomposite and to evaluate their photocatalytic activity in the removal of methylene blue under UV irradiation.

scholarly journals Designing Magnetic Layered Double Hydroxides and Two-Dimensional Magnetic Nano-Nets of Cobalt Ferrite through a Novel Approach

2018 ◽  
Vol 8 (11) ◽  
pp. 2099 ◽  
Author(s):  
Osama Saber ◽  
Abdullah Aljaafari ◽  
Sarah Asiri ◽  
Khalid Batoo
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Layered Double Hydroxides ◽  
Cobalt Ferrite ◽  
High Coercivity ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Double Hydroxides

The present study has a dual aim of supporting magnetic nanoparticles over the nanolayers of LDHs and designing two-dimensional magnetic nano-nets of cobalt ferrite. In this trend, nanoparticles of CoFe2O4 were prepared and supported by Co-Fe LDH through urea hydrolysis. The nanolayered structures of Co-Fe LDH were confirmed by X-ray diffraction, energy-dispersive X-ray spectrometry, FT-IR spectra, thermal analyses, and transmission electron microscopy. In addition, they indicated that 13.2% CoFe2O4 were supported over Co-Fe LDH. Transformation of the nanolayered structures of Co-Fe LDH to nano-nets was achieved by the catalytic effect of the supported CoFe2O4 nanoparticles through solvent thermal technique. X-ray diffraction patterns and transmission electron microscopy images confirmed the transformation of the supported Co-Fe LDH to nano-nets of cobalt ferrite. In order to indicate the effect of the LDH for designing the nano-nets, nanoparticles of cobalt ferrite were prepared by the same technique without LDH. The magnetic behavior of the nano-nets and the supported Co-Fe LDH were measured and compared with the nanoparticles through vibrating sample magnetometer technique. The magnetic parameters indicated that the prepared nano-nets have ferromagnetic behavior and high coercivity. However, the prepared nanoparticles revealed a superparamagnetic state and low coercivity. The experimental results concluded that the incorporation of nanoparticles with nanowires into nano-net structures has been found to be an efficient way to improve their magnetic properties and prevent their agglomerations. Finally, layered double hydroxides are an important source for constructing magnetic nanolayered structures and nano-nets.

Study of the structure and thermal characteristics of nanocomposites based on polyvinyl alcohol and intercalated montmorillonite

2019 ◽  
pp. 089270571987919
Author(s):  
Volodymyr Krasinskyi ◽  
Ivan Gajdos ◽  
Oleh Suberlyak ◽  
Viktoria Antoniuk ◽  
Tomasz Jachowicz
Keyword(s):  
Thermal Stability ◽  
Differential Scanning Calorimetry ◽  
Acrylic Acid ◽  
Polyvinyl Alcohol ◽  
Thermal Characteristics ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
The Degree Of Crystallinity

The structure and thermal characteristics of nanocomposites based on polyvinyl alcohol (PVA) and montmorillonite (MMT) intercalated with polyvinylpyrrolidone were investigated by X-ray diffraction analysis and differential scanning calorimetry. The modification of PVA with intercalated MMT reduces the degree of crystallinity of the resulting nanocomposites but significantly increases their thermal stability. Under ultrasound, the intercalated MMT was completely distributed in a PVA solution and formed a monocrystalline structure. Films based on PVA with modified MMT were cross-linked at 110°C in the presence of 5 wt% acrylic acid and 0.5 wt% Ferrous(II) sulfate as an initiator. The formed films have a homogeneous cross-linked structure.

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