scholarly journals Immobilization of (Aqueous) Cations in Low pH M-S-H Cement

2021 ◽  
Vol 11 (7) ◽  
pp. 2968
Author(s):  
Maximilian R. Marsiske ◽  
Christian Debus ◽  
Fulvio Di Lorenzo ◽  
Ellina Bernard ◽  
Sergey V. Churakov ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Metal Cations ◽  
Growth Period ◽  
Magnesium Silicate ◽  
Low Ph ◽  
Secondary Phases ◽  
X Ray ◽  
Early Stages ◽  
Total Metal ◽  
Wide Range

Incorporation of heavy metal ions in cement hydrates is of great interest for the storage and immobilization of toxic, hazardous, and radioactive wastes using cementitious matrix. Magnesium silicate hydrate (M-S-H) is a low pH alternative cementitious binder to commonly used Portland cement. Low pH cements have been considered as promising matrix for municipal and nuclear waste immobilization in the last decades. It is however crucial to assure that the incorporation of secondary ions is not detrimental for the formation of the hydration products. Herein, we investigate the early stages of formation of M-S-H from electrolyte solutions in presence of a wide range of metal cations (LiI, BaII, CsI, CrIII, FeIII, CoII, NiII, CuI, ZnII, PbII, AlIII). The final solid products obtained after 24 h have been characterized via powder X-ray diffraction (PXRD), attenuated total reflectance-Fourier transformed infrared spectroscopy (FTIR-ATR), elemental analysis via energy-dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HR-TEM). In all the experiments, the main precipitated phase after 24 h was confirmed to be M-S-H with a ratio (total metal/Si) close to one. The obtained M-S-H products showed strong immobilization capacity for the secondary metal cations and can incorporate up to 30% of the total metal content at the early stages of M-S-H formation without significantly delaying the nucleation of the M-S-H. It has been observed that presence of Cr, Co, and Fe in the solution is prolonging the growth period of M-S-H. This is related to a higher average secondary metal/total metal ratio in the precipitated material. Secondary phases that co-precipitate in some of the experiments (Fe, Pb, Ni, and Zn) were also effectively trapped within in the M-S-H matrix. Barium was the only element in which the formation of a secondary carbonate phase isolated from the M-S-H precipitates was detected.

scholarly journals A Highly Sensitive Room Temperature CO2 Gas Sensor Based on SnO2-rGO Hybrid Composite

Materials ◽  
2021 ◽  
Vol 14 (3) ◽  
pp. 522
Author(s):  
Zhi Yan Lee ◽  
Huzein Fahmi bin Hawari ◽  
Gunawan Witjaksono bin Djaswadi ◽  
Kamarulzaman Kamarudin
Keyword(s):  
Electron Microscopy ◽  
Carbon Dioxide ◽  
Gas Sensor ◽  
Photoelectron Spectroscopy ◽  
Hybrid Composite ◽  
Room Temperature ◽  
Co2 Gas ◽  
X Ray ◽  
Wide Range ◽  
Co2 Gas Sensor

A tin oxide (SnO2) and reduced graphene oxide (rGO) hybrid composite gas sensor for high-performance carbon dioxide (CO2) gas detection at room temperature was studied. Since it can be used independently from a heater, it emerges as a promising candidate for reducing the complexity of device circuitry, packaging size, and fabrication cost; furthermore, it favors integration into portable devices with a low energy density battery. In this study, SnO2-rGO was prepared via an in-situ chemical reduction route. Dedicated material characterization techniques including field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray (EDX) spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) were conducted. The gas sensor based on the synthesized hybrid composite was successfully tested over a wide range of carbon dioxide concentrations where it exhibited excellent response magnitudes, good linearity, and low detection limit. The synergistic effect can explain the obtained hybrid gas sensor’s prominent sensing properties between SnO2 and rGO that provide excellent charge transport capability and an abundance of sensing sites.

scholarly journals Graphitic Nitrogen in Carbon Catalysts Important for the Reduction of Nitrite Revealed by 15N NMR Spectroscopy at Natural Abundance

2020 ◽  
Author(s):  
Zheng Chen ◽  
Aleksander Jaworski ◽  
Jianhong Chen ◽  
Tetyana Budnyak ◽  
Ireneusz Szewczyk ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Reduction Reaction ◽  
Nitrite Reduction ◽  
15N Nmr ◽  
Carbon Catalyst ◽  
X Ray ◽  
Wide Range ◽  
Alkaline Conditions

Metal-free nitrogen-doped carbon is considered as a green functional material, but the structural determination of the atomic positions of nitrogen remains challenging. We recently demonstrated that directly-excited solid state <sup>15</sup>N NMR (ssNMR) spectroscopy is a powerful tool for the determination of such positions in an N-doped carbon at natural <sup>15</sup>N isotope abundance. Here we present a green chemistry approach to the synthesis of N-doped carbon using cellulose as precursor, and a study of the catalytic properties and atomic structures of the related catalyst. The N-doped carbon (NH<sub>3</sub>) was obtained by oxidation of cellulose with HNO<sub>3</sub> followed by ammonolysis at 800°C. It had a N content of 6.5 wt.% and a surface area of 557 m<sup>2 </sup>g<sup>–1</sup>, and <sup>15</sup>N ssNMR spectroscopy provided evidence for graphitic nitrogen besides of regular pyrrolic and pyridinic nitrogen. This structure determination enabled probing the role of graphitic nitrogen for electrocatalytic reactions, such as the hydrogen evolution reaction (HER), oxygen evolution reaction (OER), and nitrite reduction reaction. The N-doped carbon catalyst (NH<sub>3</sub>) had higher electrocatalytic activities in OER and HER under alkaline conditions and a higher activity for nitrite reduction, as compared with a catalyst prepared by carbonization of the HNO<sub>3</sub>-treated cellulose in N<sub>2</sub>. The electrocatalytic selectivity for nitrite reduction of the N-doped carbon catalyst (NH<sub>3</sub>) was directly related to the graphitic nitrogen functions. Complementary structural analysis by means of <sup>13</sup>C and <sup>1</sup>H ssNMR, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and low-temperature N<sub>2 </sub>adsorption were preformed and provided support to the findings. The results show that directly-excited <sup>15</sup>N ssNMR at natural <sup>15</sup>N abundance is generally capable to provide information on N-doped carbon materials, and it is expected that the approach can be applied to a wide range of solids with an intermediate amount of N atoms.

scholarly journals Facile Fabrication of CeO2/Electrochemically Reduced Graphene Oxide Nanocomposites for Vanillin Detection in Commercial Food Products

Nanomaterials ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 1356 ◽  
Author(s):  
Xue Nie ◽  
Rui Zhang ◽  
Zheng Tang ◽  
Haiyan Wang ◽  
Peihong Deng ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Graphene Oxide ◽  
Reduced Graphene Oxide ◽  
Linear Sweep Voltammetry ◽  
X Ray ◽  
Transmission Electron ◽  
Reduced Graphene ◽  
Electrochemically Reduced Graphene Oxide ◽  
Wide Range ◽  
Facile Fabrication

In this paper, CeO2 nanoparticles were synthesized by the solvothermal method and dispersed uniformly in graphene oxide (GO) aqueous solution by ultrasonication. The homogeneous CeO2-GO dispersion was coated on the surface of a glassy carbon electrode (GCE), and the CeO2/electrochemically reduced graphene oxide modified electrode (CeO2/ERGO/GCE) was obtained by potentiostatic reduction. The results of X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) showed that CeO2 nanocrystals were uniformly coated by gossamer like ERGO nanosheets. The electrochemical behavior of vanillin on the CeO2/ERGO/GCE was studied by cyclic voltammetry (CV). It was found that the CeO2/ERGO/GCE has high electrocatalytic activity and good electrochemical performance for vanillin oxidation. Using the second derivative linear sweep voltammetry (SDLSV), the CeO2/ERGO/GCE provides a wide range of 0.04–20 µM and 20 µM–100 µM for vanillin detection, and the detection limit is estimated to be 0.01 µM after 120 s accumulation. This method has been successfully applied to the vanillin detection in some commercial foods.

Synthesis of Fe2O3/CNTs for the Fast Removal of Tetracycline from Aqueous Solutions

2014 ◽  
Vol 915-916 ◽  
pp. 933-941 ◽  
Author(s):  
Zhong Jie Zhang ◽  
Chang Yu Lu ◽  
Wei Huang ◽  
Wei Sheng Guan ◽  
Yue Xin Peng
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Magnetic Measurements ◽  
Ferrite Nanoparticles ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Wide Range ◽  
Fast Removal ◽  
Scanning Electron

The effective remove to tetracycline still remains a big challenge for scientists. In this work, we used a new method for preparing functional magnetic CNTS with ferrite nanoparticles. A wide range of techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and magnetic measurements were applied to characterize the obtained Fe2O3/CNTs. Moreover, we have also studied the properties of adsorbent to tetracycline. In addition, we have found that the Fe2O3/CNTs are better reusable adsorbent than other traditional adsorbents by magnetic separation recycling method.

scholarly journals Crystallization of Bi–Sr–Ca–Cu–O glasses in oxygen

1992 ◽  
Vol 7 (7) ◽  
pp. 1658-1671 ◽  
Author(s):  
T.G. Holesinger ◽  
D.J. Miller ◽  
L.S. Chumbley
Keyword(s):  
Electron Microscopy ◽  
Crystallization Process ◽  
Secondary Phases ◽  
X Ray Diffraction ◽  
X Ray ◽  
Partial Crystallization ◽  
Full Conversion ◽  
Limited Process ◽  
Step Crystallization ◽  
Scanning Electron

A detailed study of the crystallization process for compositions near Bi2Sr2Ca1Cu2Oy was undertaken using differential thermal analysis (DTA), transmission and scanning electron microscopy (TEM and SEM), and x-ray diffraction (XRD). Glasses prepared by a splat-quench technique were free of secondary phases in most cases. A two-step crystallization process in oxygen was observed in which partial crystallization of the glass occurs initially with the nucleation of “2201” and Cu2O, and is completed with the formation of SrO, CaO, and Bi2Sr3−xCaxOy. No specific thermal event could be associated with the formation of the “2212” phase. Rather, formation occurs via conversion of 2201 into 2212. This was a kinetically limited process at temperatures below 800 °C as other phases were found to evolve in addition to the 2212 phase during extended anneals. In contrast, a nearly full conversion to the 2212 phase occurred after only 1 min of annealing at 800 °C and above. However, changes in resistivity data, secondary phases, and the measured 2212 composition upon extended anneals at 865 °C showed that considerably longer heat treatments were necessary for the sample to reach its equilibrium state.

Hydroxyapatite Scaffolds Produced by Hydrothermal Deposition of Monetite on Polyurethane Sponges Substrates

2011 ◽  
Vol 493-494 ◽  
pp. 820-825 ◽  
Author(s):  
Fernanda Danielle Mishima ◽  
Luis Henrique Leme Louro ◽  
Felipe Nobre Moura ◽  
Luciano Andrade Gobbo ◽  
Marcelo Henrique Prado da Silva
Keyword(s):  
Electron Microscopy ◽  
Aqueous Solution ◽  
Tricalcium Phosphate ◽  
Porous Scaffolds ◽  
New Bone Formation ◽  
Total Conversion ◽  
X Ray ◽  
Heat Treated ◽  
Wide Range ◽  
Scanning Electron

Hydroxyapatite scaffolds have been being produced by a wide range of processes. The optimun material to be used as bone graft has to be partially resorbable, with resorption rates similar to new bone formation ones. The samples must have porosity compatible with tissue ingrowth. Hydroxyapatite and tricalcium phosphate ceramics are good choices for designing such materials. In the present study, polymeric sponges were coated with hydroxyapatite and sintered. The method consists of coating polyurethane sponges substrates in an aqueous solution rich in phosphate (PO4)3-and calcium (Ca)2+ions. The solution is composed by 0.5M Ca(OH)2, 0.3M H3PO4and 1M CH3CHCO2HOH (lactic acid) at pH of 3.7. The sponges were immersed in a beaker with the solution and heated up to 80°C to precipitate monetite on the sponge. Continuous and adherent coatings were formed on the surface of sponges interconections. These coatings were characterised by X-ray diffractometry and the only identified phase was monetite. The substrates were converted to hydroxyapatite in an alkali solution.The total conversion from monetite to hydroxyapatite was confirmed by XRD analyses. The struts were heat treated in order to eliminate the organic sponge and sinter the scaffolds. After sintering, hydroxyapatite and tricalcium phosphate were identified on the struts. Optical microscopy revealed the morphology of the struts, while scanning electron microscopy (SEM) showed the precipitates morphology. The method showed to be efficient in the production of porous scaffolds.

scholarly journals In Situ and In Operando Techniques to Study Li-Ion and Solid-State Batteries: Micro to Atomic Level

Inorganics ◽  
2021 ◽  
Vol 9 (11) ◽  
pp. 85
Author(s):  
Maryam Golozar ◽  
Raynald Gauvin ◽  
Karim Zaghib
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Atomic Level ◽  
X Ray ◽  
In Situ Techniques ◽  
Transmission Electron ◽  
Wide Range ◽  
Li Ion

This work summarizes the most commonly used in situ techniques for the study of Li-ion batteries from the micro to the atomic level. In situ analysis has attracted a great deal of interest owing to its ability to provide a wide range of information about the cycling behavior of batteries from the beginning until the end of cycling. The in situ techniques that are covered are: X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Scanning Transmission Electron Microscopy (STEM). An optimized setup is required to be able to use any of these in situ techniques in battery applications. Depending on the type of data required, the available setup, and the type of battery, more than one of these techniques might be needed. This study organizes these techniques from the micro to the atomic level, and shows the types of data that can be obtained using these techniques, their advantages and their challenges, and possible strategies for overcoming these challenges.

Ultrastructural Localization of Cellulase in Diplodia Maydis and in D. Maydis-Infected Com Stalk Tissue

1977 ◽  
Vol 35 ◽  
pp. 454-455
Author(s):  
Judith A. Murphy ◽  
Mary R. Thompson ◽  
A.J. Pappelis
Keyword(s):  
Culture Medium ◽  
Cupric Oxide ◽  
Cellulase Activity ◽  
Growth Period ◽  
Ultrastructural Localization ◽  
Ultrastructural Level ◽  
Low Ph ◽  
Cellulolytic Enzymes ◽  
Cellulolytic Activity ◽  
X Ray

BeMiller et.al.(l) found that D. maydis did not have the solubilizing enzyme C1. They reported that D- maydis exhibited cellulolytic activity constitutively, and hypothesized that the cellulolytic enzymes were attached to fungal hyphal surfaces because they found cellulase released to the culture medium only after the growth period, when available cellulose had been used up.The purpose of this study was to determine the location of cellulolytic enzymes (EC 3.2.1.4; beta-1,4-glucan glucanohydrolase) in D. maydis and D. maydis-infected corn tissue at the ultrastructural level.Cellulase activity produces glucose as an end product which will reduce cupric oxide and can be visualized with an EM because it is electron dense and the Cu component can be verified with x-ray analysis(Figs.l,2). After thorough washing, samples fixed in aldehydes are incubated in a substrate mixture at a low pH. The enzyme is activated and reducing sugar is released. The sample is then reacted with Benedict's solution at a high temperature, allowing CuO crystals to be deposited at the site of reaction.

Application of in situ Transmission Electron Microscopyfor Tribological Investigations of Magnetron Sputter Assisted Pulsed Laser Deposition of Yttria-stabilized Zirconia-gold Composite Coatings

2005 ◽  
Vol 20 (7) ◽  
pp. 1860-1868 ◽  
Author(s):  
J.J. Hu ◽  
A.A. Voevodin ◽  
J.S. Zabinski
Keyword(s):  
Electron Microscopy ◽  
High Temperature ◽  
Composite Coatings ◽  
Pulsed Laser ◽  
Yttria Stabilized Zirconia ◽  
Stabilized Zirconia ◽  
X Ray ◽  
Transmission Electron ◽  
Wide Range

Yttria-stabilized zirconia (YSZ)-Au composite coatings have great potential as solid film lubricants for aerospace applications over a wide range of environmental conditions. They were grown on steel disks or silicon wafers by pulsed laser ablation of YSZ and simultaneous magnetron sputtering of a Au target. Such a combination of ceramics with soft metals improved the toughness of the composite coating and increased its ability to lubricate at high temperature. Information on the time-dependent response of these microstructures to changes in temperature is essential to tribological investigations of high temperature performance. In situ transmission electron microscopy was used to directly measure the dynamic change of YSZ-Au coating structure at elevated temperatures. High-resolution electron microscopy and electron diffraction showed that amorphous YSZ-5 at.% Au coatings proceeded to crystallize under the irradiation of electron beams. Time varying x-ray energy dispersive spectra measured a loss of oxygen in the sample during about 10 min of irradiation with subsequent slight oxygen recovery. This behavior was related to the activation of oxygen diffusion under electron irradiation. X-ray diffraction patterns from vacuum annealed samples verified crystallization of the coatings at 500 °C. Real-time growth of Au nanograins in the sample was observed as the temperature was increased to 500 °C in a TEM specimen holder that could be heated. The grain growth process was recorded using a charge-coupled device camera installed on the transmission electron microscope. The crystallization and growth of zirconia and Au nanograins resulted in low friction during tribological tests. The nucleation of Au islands on heated ball-on-flat specimens was responsible for lowering friction.

scholarly journals Effect of Excess Silicon on the Formation of Ti3SiC2 Using Free Ti/Si/C Powders Synthesized via Arc Melting

ISRN Ceramics ◽  
2012 ◽  
Vol 2012 ◽  
pp. 1-10 ◽  
Author(s):  
Mohamad Johari Abu ◽  
Julie Juliewatty Mohamed ◽  
Zainal Arifin Ahmad
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Relative Density ◽  
Stoichiometric Ratio ◽  
Secondary Phases ◽  
X Ray ◽  
Excess Silicon ◽  
Arc Melting ◽  
Equiaxed Grains ◽  
Scanning Electron

The aim of this study is to investigate the effect of excess silicon on the formation of Ti3SiC2 from free Ti/Si/C powders synthesized via arc melting. The reactant mixture was prepared according to the off-stoichiometric ratio of 3Ti : (x+1)Si : 2C, where x (excess Si) varied from 0 to 0.5. Samples were analyzed using X-ray diffractometry (XRD), field-emission scanning electron microscopy (FESEM), and energy-dispersive spectroscopy (EDS). The relative density and porosity of products were calculated using the Archimedes method. Through optimization of the arcing schedules (time) and excess Si amounts, 86.9 wt% of Ti3SiC2 with a relative density of 86% was obtained. For all products, Ti3SiC2 was identified as the main phase, while TiC, TiSi2, and Ti5Si3 were identified as secondary phases. Ti3SiC2 grains were in the form of elongated platelets; they were nucleated and grew on the surface of equiaxed TiC grains. The microporosity present in the TiC-equiaxed grains affected the density and porosity of the products.

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