scholarly journals MW Synthesis of ZIF-7. The Effect of Solvent on Particle Size and Hydrogen Sorption Properties

Energies ◽  
2020 ◽  
Vol 13 (23) ◽  
pp. 6306
Author(s):  
Vladimir A. Polyakov ◽  
Vera V. Butova ◽  
Elena A. Erofeeva ◽  
Andrei A. Tereshchenko ◽  
Alexander V. Soldatov

We report here fast (15 min) microwave-assisted solvothermal synthesis of zeolitic imidazolate framework material (ZIF-7). We have optimized solvent composition to achieve high porosity and hydrogen capacity and narrow particle size distribution. It was shown that synthesis in N,N-diethylformamide (DEF) results in a layered ZIF-7 III phase, while N,N-dimethylformamide (DMF) as solvent leads to a pure ZIF-7 phase in microwave conditions. A mixture of toluene with DMF allows the production of pure ZIF-7 material only with the triethylamine additive. Obtained materials were comprehensively characterized. We have pointed out that both X-ray diffraction and infrared spectroscopy could be used for the identification of ZIF-7 or ZIF-7 III phases. Although samples obtained in DMF, and in a mixture of DMF, toluene, and triethylamine were assigned to the pure ZIF-7 phase, solvent composition significantly affected the size of particles in the material and nitrogen and hydrogen adsorption process.

2012 ◽  
Vol 510-511 ◽  
pp. 201-205
Author(s):  
G. Asghar ◽  
S. Nasir ◽  
M.S. Awan ◽  
G.H. Tariq ◽  
M. Akram ◽  
...  

Phase purity, particle size and its distribution contributes a lot to the physical properties of M-type hexa-ferrites. These parameters are strongly influenced by the variation in synthesis parameters. In the present work, effect of synthesis parameters such as molar ratio (Fe/Sr) and volume rate of addition of precipitating agent on M-type hexa-ferrite (SrFe12O19) prepared by co-precipitation method have been investigated systematically. The molar ratio (Fe/Sr) in SrFe12O19was varied as 12, 11, 10, 09, and 08. X-ray diffraction analysis revealed that molar ratio does not affect the phase purity. X-ray diffraction analysis of the samples prepared with different volume rate of addition of precipitating agent indicated that phase purity and micro-structural properties of SrFe12O19are greatly influenced by the above synthesis parameter. High volume rate of addition of precipitating agent resulted in high phase purity, smaller particle size, and narrow particle size distribution.


Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 232
Author(s):  
Pedro J. Sánchez-Soto ◽  
Eduardo Garzón ◽  
Luis Pérez-Villarejo ◽  
George N. Angelopoulos ◽  
Dolores Eliche-Quesada

In this work, an examination of mining wastes of an albite deposit in south Spain was carried out using X-ray Fluorescence (XRF), X-ray diffraction (XRD), particle size analysis, thermo-dilatometry and Differential Thermal Analysis (DTA) and Thermogravimetric (TG) analysis, followed by the determination of the main ceramic properties. The albite content in two selected samples was high (65–40 wt. %), accompanied by quartz (25–40 wt. %) and other minor minerals identified by XRD, mainly kaolinite, in agreement with the high content of silica and alumina determined by XRF. The content of Na2O was in the range 5.44–3.09 wt. %, being associated with albite. The iron content was very low (<0.75 wt. %). The kaolinite content in the waste was estimated from ~8 to 32 wt. %. The particle size analysis indicated values of 11–31 wt. % of particles <63 µm. The ceramic properties of fired samples (1000–1350 °C) showed progressive shrinkage by the thermal effect, with water absorption and open porosity almost at zero at 1200–1250 °C. At 1200 °C, the bulk density reached a maximum value of 2.38 g/cm3. An abrupt change in the phase evolution by XRD was found from 1150 to 1200 °C, with the disappearance of albite by melting in accordance with the predictions of the phase diagram SiO2-Al2O3-Na2O and the system albite-quartz. These fired materials contained as main crystalline phases quartz and mullite. Quartz was present in the raw samples and mullite was formed by decomposition of kaolinite. The observation of mullite forming needle-shape crystals was revealed by Scanning Electron Microscopy (SEM). The formation of fully densified and vitrified mullite materials by firing treatments was demonstrated.


2020 ◽  
Vol 18 (1) ◽  
pp. 951-961
Author(s):  
Qiuju Chen ◽  
Tao Hui ◽  
Hongjuan Sun ◽  
Tongjiang Peng ◽  
Wenjin Ding

AbstractVarious morphologies of magnesium carbonate hydrate had been synthesized without using any organic additives by carefully adjusting the reaction temperature and time during the talc carbonation process. At lower temperatures, magnesium carbonate hydrate was prone to display needle-like morphology. With the further increase of the carbonation temperature, the sheet-like crystallites became the preferred morphology, and at higher aging temperatures, these crystallites tended to assemble into layer-like structures with diverse morphologies, such as rose-like particles and nest-like structure. The reaction time had no effect on the crystal morphology, but it affected the particle size and situation of the crystal growth. X-Ray diffraction results showed that these various morphologies were closely related to their crystal structure and compositions. The needle-like magnesium carbonate hydrate had a formula of MgCO3·3H2O, whereas with the morphological transformation from needle-like to sheet-like, rose-like, and nest-like structure, their corresponding compositions also changed from MgCO3·3H2O to 4MgCO3·Mg(OH)2·8H2O, 4MgCO3·Mg(OH)2·5H2O, and 4MgCO3·Mg(OH)2·4H2O.


2014 ◽  
Vol 2014 ◽  
pp. 1-10 ◽  
Author(s):  
K. A. Athmaselvi ◽  
C. Kumar ◽  
M. Balasubramanian ◽  
Ishita Roy

This study evaluates the physical properties of freeze dried tropical (guava, sapota, and papaya) fruit powders. Thermal stability and weight loss were evaluated using TGA-DSC and IR, which showed pectin as the main solid constituent. LCR meter measured electrical conductivity, dielectric constant, and dielectric loss factor. Functional groups assessed by FTIR showed presence of chlorides, and O–H and N–H bonds in guava, chloride and C–H bond in papaya, and chlorides, and C=O and C–H bonds in sapota. Particle size and type of starch were evaluated by X-ray diffraction and microstructure through scanning electronic microscopy. A semicrystalline profile and average particle size of the fruit powders were evidenced by X-ray diffraction and lamellar/spherical morphologies by SEM. Presence of A-type starch was observed in all three fruits. Dependence of electric and dielectric properties on frequency and temperature was observed.


2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola

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.


Author(s):  
Rajni Bhardwaj ◽  
Smita Johar ◽  
Amit Kapila ◽  
Amandeep Sharma

Swarnamakshika is grouped under Updhatu of Swarna and is composed of Copper, Iron and Sulphur. In this study Swarnamakshika was subjected to Shodhana by Bharjana with Nimbuka swarasa and Shudha Swarnamakshika was given Bhavana with Nimbuka swarasa and subjected to Varahaputa. With ten Varahaputa Bhasma Siddhi Lakshanas were attained swarnamakshika Marana was done by using Nimbuka swarasa until bhasma siddi lakshanas found and it took 10 puta till it attained reddish brown color. The X-ray diffraction analysis showed that d-identified peaks after 10th puta Swarnamakshika bhasma composition is of Iron oxide with rhombohedral crystal system as main component. EDX analysis of Swarna makshika bhasma shows that it contains Iron and Oxygen, as major element and Copper, Sulphur, Carbon, Aluminium, Calcium etc. as minor elements. FESEM study revealed that the particle size of Ashudha and Shudha Swarnamakshika was in the range of 500 nm-3nm. Keywords: Swarnamakshika Bhasma, Nimbuka swarasa, puta


PLoS ONE ◽  
2020 ◽  
Vol 15 (12) ◽  
pp. e0244511
Author(s):  
Fernando Gordillo-Delgado ◽  
Jakeline Zuluaga-Acosta ◽  
Gonzalo Restrepo-Guerrero

In this work, the effect of the inoculation of silver-incorporated titanium dioxide nanoparticles (Ag-TiO2 NPs) in spinach seeds was evaluated on certain growth, physiology and phytotoxicity parameters of the plants. This is an important crop for human consumption with high nutritional value due to their low calorie and fat content, providing various vitamins and minerals, especially iron. These NPs were obtained by means of the sol-gel method and heat treatment; the resulting powder material was characterized using X-ray diffraction and scanning electron microscopy and the influence of these NPs on plants was measured by estimating the germination rate, monitoring morphological parameters and evaluating phytotoxicity. The photosynthetic activity of the spinach plants was estimated through the quantification of the Ratio of Oxygen Evolution (ROE) by the photoacoustic technique. Samples of TiO2 powder with particle size between 9 and 43 nm were used to quantify the germination rate, which served to determine a narrower size range between 7 and 26 nm in the experiments with Ag-TiO2 NPs; the presence of Ag in TiO2 powder samples was confirmed by energy-dispersive X-ray spectroscopy. The analysis of variance showed that the dependent variable (plant growth) could be affected by the evaluated factors (concentration and size) with significant differences. The statistical trend indicated that the application of the Ag-TiO2 NPs suspension of lowest concentration and smallest particle size could be a promoting agent of the growth and development of these plants. The inoculation with NPs of 8.3 nm size and lowest concentration was related to the highest average ROE value, 24.6 ± 0.2%, while the control group was 20.2 ± 0.2%. The positive effect of the Ag-TiO2 NPs treatment could be associated to the generation of reactive oxygen species, antimicrobial activity, increased biochemical attributes, enzymatic activity or improvements in water absorption.


2020 ◽  
Vol 56 (1) ◽  
pp. 1
Author(s):  
George Christidis ◽  
Katerina Paipoutlidi ◽  
Ioannis Marantos ◽  
Vasileios Perdikatsis

A great variety of fine grained industrial rocks, which are valued by the industry contain variable amounts of amorphous or poorly crystalline matter, which is not easily detectable by the conventional mineralogical analysis methods based on X-ray diffraction (XRD). The quantification of amorphous matter in industrial rocks is a major task because it provides a thorough characterization of the raw materials and assists to interpret their reactivity. Among the most reliable methods used for quantification of amorphous matter, are those which are based on Rietveld refinement. In this study we prepared 1:1 mixtures of synthetic or natural calcite and quartz with 5-80% glass flour and added corundum (α-Al2O3) internal standard and applied the Autoquan2.80 © software based on the BGMN computer code to quantify the amorphous matter content. The mixtures with synthetic minerals yielded results with minimum absolute error due to the similar particle size of the minerals, the internal standard and the glass. By contrast, the mixtures with natural minerals displayed greater relative error due to the particle size difference between the minerals on the one hand and the internal standard and the glass on the other, due to the microabsorption effect. Moreover, preferred orientation was important in the case of natural calcite, due to perfect  cleavage plane. Mixtures containing up to 25% amorphous matter did not display the characteristic hump at 20-30 °2θ, suggesting that the lack of the hump is not a safe criterion for the recognition of amorphous matter.


Author(s):  
Fredy Kurniawan ◽  
Rahmi Rahmi

SnO2 nanoparticles have been synthesized by high voltage electrolysis. Tin bare was used for anode and cathode. The effect of potentials and electrolyte were studied. The particles obtained after electrolysis was characterized using X-ray Diffraction (XRD). The diffractogram is in agreement with the standard diffraction pattern of SnO2 which is identified as tetragonal structure. The Fourier Transform Infrared (FTIR) spectrum indicates that there is a vibration of Sn–O asymmetric at 580 cm-1. The optimum potential for SnO2 nanoparticles synthesis is 60 V at 0.06 M HCl which shows the highest UV-Vis spectrum. The absorption peak of SnO2 nanoparticles by UV-Vis spectrophotometer appears at about 207 nm. The particle size analysis shows that the SnO2 nanoparticles obtained have the size distribution in a range of 25-150 nm with the highest volume at 83.11 nm. Copyright © 2017 BCREC Group. All rights reservedReceived: 15th November 2016; Revised: 26th February 2017; Accepted: 27th February 2017How to Cite: Rahmi, R., Kurniawan, F. (2017). Synthesis of SnO2 Nanoparticles by High Potential Electrolysis. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (2): 281-286 (doi:10.9767/bcrec.12.2.773.281-286)Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.2.773.281-286 


1989 ◽  
Vol 169 ◽  
Author(s):  
Rollin E. Lakis ◽  
Sidney R. Butler

AbstractY1Ba2Cu3O7 has been prepared by the evaporative decomposition of solutions method. Nitrate and mixed anion solutions were atomized and decomposed at temperatures ranging from 300°C to 950°C. The resulting materials have been characterized using x-ray powder diffraction, Thermal Gravimetric Analysis (TGA), particle size analysis, Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM). The powder consists of 0.3 micron agglomerated hollow spheres with a primary particle size of 0.06 micron. TGA and x-ray diffraction indicate the presence of barium nitrate and barium carbonate due to incomplete decomposition and/or product contamination by the process environment.


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