Preparation and Characterization of New Molybdenum Nitride or Oxynitride Phases

1994 ◽  
Vol 368 ◽  
Author(s):  
Roger J. Marchand ◽  
X. Gouin ◽  
F. Tessier ◽  
Y. Laurent

ABSTRACTSeveral methods of synthesizing molybdenum nitride or oxynitride fine powders are presented.We have prepared a γ-Mo2N type oxynitride phase by reacting ammonia with MoO3. The surface area and morphology of the oxynitride powders depend on the synthesis conditions. Characterization of the solids by elemental analysis, X-ray and neutron diffraction, and thermogravimetric analysis shows dramatic modification of the stoichiometry of conventional Mo2N nitride. Aging at room temperature under air results in decreasing the material surface area. The initial surface area can be recovered be fine tuning of experimental conditions. MoCl5 and Ca3N2 are reacted in a molten CaCl2 medium leading to a new Mo2N structure type.The reaction between molybdenum sulfide and NH3 produces two different phases depending on the reaction conditions. They are structurally related to δ-MoN.

2018 ◽  
Vol 69 (3) ◽  
pp. 567-570
Author(s):  
Claudia Cobzaru ◽  
Adriana Marinoiu ◽  
Corina Cernatescu ◽  
Adrian Catalin Puitel ◽  
Amalia Soare

In this study the adsorption of cinnamaldehyde on the dealuminated clinoptilolite has been studied in order to investigate the possibility of using this mineral as carrier for organic compound. The characterization of dealuminated clinoptilolite and adsorption of cinnamaldehyde on the material surface has been investigated by BET, SEM and FTIR methods. These analyses show that by dealumination, significant modifications are produced in chemical composition, pore volume and surface area of the clinoptilolite and the cinnamaldehyde was adsorpted in the structure of dealuminated zeolite. Due to properties of the cinnamaldehyde, the obtained product can be used as an agrichemical.


2006 ◽  
Vol 2006 ◽  
pp. 1-7 ◽  
Author(s):  
Ingeborg Kaus ◽  
Paul Inge Dahl ◽  
Johann Mastin ◽  
Tor Grande ◽  
Mari-Ann Einarsrud

Nanocrystalline yttria-stabilized zirconia (YSZ) powders with 8 mol% Y2O3have been produced using smoldering combustion synthesis with glycine as fuel and nitrate as oxidizer. The YSZ powders prepared by using different glycine to nitrate ratios (0.20–1.0) have been characterized by X-ray diffraction (crystallite size), thermogravimetry, infrared spectroscopy, surface area analysis, transmission electron microscopy, and dilatometry to determine the parameters giving the powder the best properties when it comes to densification properties. The influence of calcination temperature on crystallite size, surface area, and carbonate species remaining from the smoldering combustion reaction has been studied especially for the G/N ratio of 0.23 to reveal the optimal synthesis conditions. A G/N ratio of 0.23 and calcination in the range 650–900ºC in oxygen flow gave high quality powder with a crystallite size less than 10 nm. Densities of sintered bodies exhibit an increase for calcination temperatures above 600ºC, where most of the residual carbonate species has been removed.


2021 ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno

Abstract Analcime is nowadays an important component in dental porcelain sysytems, in heterogeneous catalysis, in the nanoelectronic field, in selective adsorption and in stomatology. Analcime synthesis from a kaolinite rock coming from Romana (Sassari, Italy) is here presented. A synthesis protocol is proposed that aims to make an improvement of synthesis conditions compared to the past. The hydrothermal treatment is in fact here achieved without aging times and without the use of sodium silicate, as reported in the literature. Lower calcination temperature, synthesis temperatures and crystallization times are verified in this work. The kaolin is subjected to calcination at the temperature of 650°C and then mixed with NaOH. The experiment is performed at ambient pressure and 170 ± 0.1°C. The degree of purity of Analcime is calculated in 97,57 % at 10h. Analcime is characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy, inductively coupled plasma optical emission spectrometry and thermal analysis. Density is also calculated. Cell parameters and the amount of amorphous phase in the synthesis powders is estimated with quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. The experimental conditions make the synthesis protocol particularly attractive from an economic point of view. Both chemical and physical characterization of Analcime is satisfactory making the experimental protocol very promising for an industrial transfer.


2016 ◽  
Vol 1133 ◽  
pp. 547-551 ◽  
Author(s):  
Ali E.I. Elkhalifah ◽  
Mohammad Azmi Bustam ◽  
Azmi Mohd Shariff ◽  
Sami Ullah ◽  
Nadia Riaz ◽  
...  

The present work aims at a better understanding of the influences of the intercalated mono-, di- and triethanolamines on the characteristics and CO2 adsorption ability of sodium form of bentonite (Na-bentonite). The results revealed that the molar mass of intercalated amines significantly influenced the structural and surface properties as well as the CO2 adsorption capacity of Na-bentonite. In this respect, a stepwise increase in the d-spacing of Na-bentonite with the molar mass of amine was recorded by XRD technique. However, an inverse effect of the molar mass of amine on the surface area was confirmed by BET method. CO2 adsorption experiments on amine-bentonite hybrid adsorbents showed that the CO2 adsorption capacity inversly related to the molar mass of amine at 25 ͦC and 101 kPa. Accordingly, Na-bentonite modified by monoethanolammonium cations adsorbed as high as 0.475 mmol CO2/g compared to 0.148 and 0.087 mmol CO2/g for that one treated with di- and triethanolammonium cations, respectively.


Water ◽  
2021 ◽  
Vol 13 (13) ◽  
pp. 1757
Author(s):  
Yesica Vicente-Martínez ◽  
Manuel Caravaca ◽  
Antonio Soto-Meca ◽  
Miguel Ángel Martín-Pereira ◽  
María del Carmen García-Onsurbe

This paper presents a novel procedure for the treatment of contaminated water with high concentrations of nitrates, which are considered as one of the main causes of the eutrophication phenomena. For this purpose, magnetic nanoparticles functionalized with silver (Fe3O4@AgNPs) were synthesized and used as an adsorbent of nitrates. Experimental conditions, including the pH, adsorbent and adsorbate dose, temperature and contact time, were analyzed to obtain the highest adsorption efficiency for different concentration of nitrates in water. A maximum removal efficiency of 100% was reached for 2, 5, 10 and 50 mg/L of nitrate at pH = 5, room temperature, and 50, 100, 250 and 500 µL of Fe3O4@AgNPs, respectively. The characterization of the adsorbent, before and after adsorption, was performed by energy dispersive X-ray spectroscopy, scanning electron microscopy, Brunauer-Emmett-Teller analysis and Fourier-transform infrared spectroscopy. Nitrates can be desorbed, and the adsorbent can be reused using 500 µL of NaOH solution 0.01 M, remaining unchanged for the first three cycles, and exhibiting 90% adsorption efficiency after three regenerations. A deep study on equilibrium isotherms reveals a pH-dependent behavior, characterized by Langmuir and Freundlich models at pH = 5 and pH = 1, respectively. Thermodynamic studies were consistent with physicochemical adsorption for all experiments but showed a change from endothermic to exothermic behavior as the temperature increases. Interference studies of other ions commonly present in water were carried out, enabling this procedure as very selective for nitrate ions. In addition, the method was applied to real samples of seawater, showing its ability to eliminate the total nitrate content in eutrophized waters.


Processes ◽  
2021 ◽  
Vol 9 (2) ◽  
pp. 217
Author(s):  
Marin Ugrina ◽  
Martin Gaberšek ◽  
Aleksandra Daković ◽  
Ivona Nuić

Sulfur-impregnated zeolite has been obtained from the natural zeolite clinoptilolite by chemical modification with Na2S at 150 °C. The purpose of zeolite impregnation was to enhance the sorption of Hg(II) from aqueous solutions. Chemical analysis, acid and basic properties determined by Bohem’s method, chemical behavior at different pHo values, zeta potential, cation-exchange capacity (CEC), specific surface area, X-ray powder diffraction (XRPD), scanning electron microscopy with energy-dispersive X-ray analysis (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), as well as thermogravimetry with derivative thermogravimetry (TG-DTG) were used for detailed comparative mineralogical and physico-chemical characterization of natural and sulfur-impregnated zeolites. Results revealed that the surface of the natural zeolite was successfully impregnated with sulfur species in the form of FeS and CaS. Chemical modification caused an increase in basicity and the net negative surface charge due to an increase in oxygen-containing functional groups as well as a decrease in specific surface area and crystallinity due to the formation of sulfur-containing clusters at the zeolite surface. The sorption of Hg(II) species onto the sulfur-impregnated zeolite was affected by the pH, solid/liquid ratio, initial Hg(II) concentration, and contact time. The optimal sorption conditions were determined as pH 2, a solid/liquid ratio of 10 g/L, and a contact time of 800 min. The maximum obtained sorption capacity of the sulfur-impregnated zeolite toward Hg(II) was 1.02 mmol/g. The sorption mechanism of Hg(II) onto the sulfur-impregnated zeolite involves electrostatic attraction, ion exchange, and surface complexation, accompanied by co-precipitation of Hg(II) in the form of HgS. It was found that sulfur-impregnation enhanced the sorption of Hg(II) by 3.6 times compared to the natural zeolite. The leaching test indicated the retention of Hg(II) in the zeolite structure over a wide pH range, making this sulfur-impregnated sorbent a promising material for the remediation of a mercury-polluted environment.


Processes ◽  
2021 ◽  
Vol 9 (2) ◽  
pp. 382
Author(s):  
Camelia-Maria Toma ◽  
Silvia Imre ◽  
Camil-Eugen Vari ◽  
Daniela-Lucia Muntean ◽  
Amelia Tero-Vescan

Plasma protein binding plays a critical role in drug therapy, being a key part in the characterization of any compound. Among other methods, this process is largely studied by ultrafiltration based on its advantages. However, the method also has some limitations that could negatively influence the experimental results. The aim of this study was to underline key aspects regarding the limitations of the ultrafiltration method, and the potential ways to overcome them. The main limitations are given by the non-specific binding of the substances, the effect of the volume ratio obtained, and the need of a rigorous control of the experimental conditions, especially pH and temperature. This review presents a variety of methods that can hypothetically reduce the limitations, and concludes that ultrafiltration remains a reliable method for the study of protein binding. However, the methodology of the study should be carefully chosen.


Photonics ◽  
2021 ◽  
Vol 8 (7) ◽  
pp. 255
Author(s):  
Marie Tahon ◽  
Silvio Montresor ◽  
Pascal Picart

Digital holography is a very efficient technique for 3D imaging and the characterization of changes at the surfaces of objects. However, during the process of holographic interferometry, the reconstructed phase images suffer from speckle noise. In this paper, de-noising is addressed with phase images corrupted with speckle noise. To do so, DnCNN residual networks with different depths were built and trained with various holographic noisy phase data. The possibility of using a network pre-trained on natural images with Gaussian noise is also investigated. All models are evaluated in terms of phase error with HOLODEEP benchmark data and with three unseen images corresponding to different experimental conditions. The best results are obtained using a network with only four convolutional blocks and trained with a wide range of noisy phase patterns.


2019 ◽  
Vol 116 (37) ◽  
pp. 18445-18454 ◽  
Author(s):  
Alan K. Itakura ◽  
Kher Xing Chan ◽  
Nicky Atkinson ◽  
Leif Pallesen ◽  
Lianyong Wang ◽  
...  

A phase-separated, liquid-like organelle called the pyrenoid mediates CO2fixation in the chloroplasts of nearly all eukaryotic algae. While most algae have 1 pyrenoid per chloroplast, here we describe a mutant in the model algaChlamydomonasthat has on average 10 pyrenoids per chloroplast. Characterization of the mutant leads us to propose a model where multiple pyrenoids are favored by an increase in the surface area of the starch sheath that surrounds and binds to the liquid-like pyrenoid matrix. We find that the mutant’s phenotypes are due to disruption of a gene, which we call StArch Granules Abnormal 1 (SAGA1) because starch sheath granules, or plates, in mutants lacking SAGA1 are more elongated and thinner than those of wild type. SAGA1 contains a starch binding motif, suggesting that it may directly regulate starch sheath morphology. SAGA1 localizes to multiple puncta and streaks in the pyrenoid and physically interacts with the small and large subunits of the carbon-fixing enzyme Rubisco (ribulose-1,5-bisphosphate carboxylase/oxygenase), a major component of the liquid-like pyrenoid matrix. Our findings suggest a biophysical mechanism by which starch sheath morphology affects pyrenoid number and CO2-concentrating mechanism function, advancing our understanding of the structure and function of this biogeochemically important organelle. More broadly, we propose that the number of phase-separated organelles can be regulated by imposing constraints on their surface area.


Sign in / Sign up

Export Citation Format

Share Document