scholarly journals Sonochemical-assisted magnesium borate synthesis from different boron sources

2017 ◽  
Vol 19 (1) ◽  
pp. 81-88 ◽  
Author(s):  
Meral Yildirim ◽  
Azmi Seyhun Kipcak ◽  
Emek Moroydor Derun

Abstract In this study, sonochemical-assisted magnesium borate synthesis is studied from different boron sources. Various reaction parameters are successfully applied by a simple and green method. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and Raman spectroscopies are used to characterize the synthesized magnesium borates on the other hand surface morphologies are investigated by using scanning electron microscope (SEM). The XRD analyses showed that the products were admontite [MgO(B2O3)3 · 7(H2O)] with JCPDS (Joint Committee on Powder Diffraction Standards) no. of 01-076-0540 and mcallisterite [Mg2(B6O7(OH)6)2 · 9(H2O)] with JCPDS no. of 01-070-1902. The results that found in the spectroscopic studies were in a good agreement with characteristic magnesium borate bands in both regions of infra-red and visible. According to SEM results, obtained borates were in micro and sub-micro scales. By the use of ultrasonication, reaction yields were found between 84.2 and 97.9%. As a result, it is concluded that the sonochemical approach is a practicable synthesis method to get high efficiency and high crystallinity in the synthesis magnesium borate compounds.

2010 ◽  
Vol 24 (01) ◽  
pp. 51-58 ◽  
Author(s):  
S. C. BAIDOC ◽  
I. ARDELEAN

Structural analysis of x Ag 2 O · (100-x)[ B 2 O 3 · As 2 O 3] glass system, with 0 ≤ x ≤ 10 mol%, was performed by means of FT-IR and Raman spectroscopies. The purpose of this work is to investigate the structural changes that appear in the B 2 O 3 · As 2 O 3 glass matrix with the addition and increase of silver ion content. Boroxol rings, pyro-, ortho-, di-, tri-, tetra- and penta-borate groups, structural units characteristic to As 2 O 3 were found in the structure of the studied glasses. FT-IR spectroscopy measurements show that BO 3 units are the main structural units of the glass system. The presence of structural units characteristic to Ag 2 O were not directly evidenced by FT-IR spectroscopy. The Raman analysis leads to similar conclusions as the FT-IR measurements.


2014 ◽  
Vol 2014 ◽  
pp. 1-9 ◽  
Author(s):  
Azmi Seyhun Kipcak ◽  
Meral Yildirim ◽  
Sureyya Aydin Yuksel ◽  
Emek Moroydor Derun ◽  
Sabriye Piskin

Magnesium borates are significant compounds due to their advanced mechanical and thermal durability properties. This group of minerals can be used in ceramic industry, in detergent industry, and as neutron shielding material, phosphor of thermoluminescence by dint of their extraordinary specialties. In the present study, the synthesis of magnesium borate via hydrothermal method from sodium borates and physical properties of synthesized magnesium borate minerals were investigated. The characterization of the products was carried out by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and Raman spectroscopies, and differential thermal analysis and thermal gravimetry (DTA/TG). The surface morphology was examined by scanning electron microscopy (SEM). B2O3content was determined through titration. The electrical resistivity/conductivity properties of products were measured by Picoammeter Voltage Source. UV-vis spectrometer was used to investigate optical absorption characteristics of synthesized minerals in the range 200–1000 nm at room temperature. XRD results identified the synthesized borate minerals as admontite [MgO(B2O3)3·7(H2O)] with code number “01-076-0540” and mcallisterite [Mg2(B6O7(OH)6)2·9(H2O)] with code number “01-070-1902.” The FT-IR and Raman spectra of the obtained samples were similar with characteristic magnesium borate bands. The investigation of the SEM images remarked that both nano- and microscale minerals were produced. The reaction yields were between 75.1 and 98.7%.


2014 ◽  
Vol 2014 ◽  
pp. 1-10 ◽  
Author(s):  
Emek Moroydor Derun ◽  
Fatma Tugce Senberber

The hydrothermal synthesis of a mcallisterite (Mg2(B6O7(OH)6)2·9(H2O)) mineral at low temperatures was characterized. For this purpose, several reaction temperatures (0–70°C) and reaction times (30–240 min) were studied. Synthesized minerals were subjected to X-ray diffraction (XRD), fourier transform infrared (FT-IR), and Raman spectroscopies and scanning electron microscopy (SEM). Additionally, experimental analyses of boron trioxide (B2O3) content and reaction yields were performed. Furthermore, thermal gravimetry and differential thermal analysis (TG/DTA) were used for the determination of thermal dehydration kinetics. According to the XRD results, mcallisterite, which has a powder diffraction file (pdf) number of “01-070-1902,” was formed under certain reaction parameters. Pure crystalline mcallisterite had diagnostic FT-IR and Raman vibration peaks and according to the SEM analysis, for the minerals which were synthesized at 60°C and 30 min of reaction time, particle size was between 398.30 and 700.06 nm. Its B2O3content and reaction yield were50.80±1.12% and85.80±0.61%, respectively. Finally, average activation energies (conversion values(α)that were selected between 0.1 and 0.6) were calculated as 100.40 kJ/mol and 98.31 kJ/mol according to Ozawa and Kissinger-Akahira-Sunose (KAS) methods, respectively.


2014 ◽  
Vol 70 (a1) ◽  
pp. C995-C995
Author(s):  
Duane Choquesillo-Lazarte ◽  
Cristóbal Verdugo-Escamilla ◽  
Juan Manuel García-Ruiz

The interest in multicomponent solid forms has increased in the last years within the pharmaceutical industry and also the solid-state community due to the possibility of obtaining materials with new properties [1]. Crystallization strategies, supported by solvent- and solid-based techniques, have also received attention in the search and development of methodologies for the screening of multicomponent crystals. In this work, ethenzamide, an anti-inflammatory and analgesic drug, was selected as a model drug to develop cocrystals on the basis of the synthon types using a series of phenolic coformers. Ethenzamide cocrystals and cocrystal solvates have been reported recently [2,3]. Liquid Assisted Grinding (LAG) and solution methods were used as synthetic tools. Attempts to produce cocrystals by LAG and Reaction Crystallization led to the formation of polycrystalline material. The solids obtained were then characterized by powder X-ray diffraction (PXRD), FT-IR and Raman spectroscopy. Recrystallization by slow solvent evaporation was carried out when the above-referred techniques strongly suggest the formation of a new solid form. The structure of five new multicomponent solids has been determined by single crystal X-ray diffraction. Additional stability studies have been performed at controlled relative humidity conditions and followed by PXRD.


2018 ◽  
Vol 15 (1) ◽  
pp. 73-80 ◽  
Author(s):  
Baghdad Science Journal

Polyaniline membranes of aniline were produced using an electrochemical method in a cell consisting of two poles. The effect of the vaccination was observed on the color of membranes of polyaniline, where analysis as of blue to olive green paints. The sanction of PANI was done by FT-IR and Raman techniques. The crystallinity of the models was studied by X-ray diffraction technique. The different electronic transitions of the PANI were determined by UV-VIS spectroscopy. The electrical conductivity of the manufactured samples was measured by using the four-probe technique at room temperature. Morphological studies have been determined by Atomic force microscopy (AFM). The structural studies have been measured by (SEM).


2001 ◽  
Vol 56 (4-5) ◽  
pp. 359-363 ◽  
Author(s):  
N. Stock ◽  
G. D. Stucky ◽  
A. K. Cheetham

Abstract The manganese pyroarsenate hydrate, Mn2As2O7 · 2 H2O, has been obtained as a single phase product using hydrothermal methods and the structure has been determined by single crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/n with a = 6.6576(4), b = 14.555(1), c = 7.8147(5) Å, β = 94.935(1)°, V = 754.46(8) Å3 and Z = 4. The manganese ions are each coordinated to five oxygen atoms and a water molecule in a distorted octahedral arrangement. Edge-sharing MnO6 octahedra form chains which are connected to a three-dimensional framework by As2O74- ions. The pyroarsenate anion, which attains a nearly eclipsed conformation, has a mean As-O distance for the terminal As-O bonds of 1.669(2) Å, while for the bridging oxygen atom a mean value of 1.757(2) Å is observed. Magnetic susceptibility measurements indicate the presence of high-spin Mn2+ ions. Thermogravimetric as well as IR and Raman spectroscopic studies of Mn2As2O7 · 2 H2O are presented.


Materials ◽  
2020 ◽  
Vol 13 (2) ◽  
pp. 274 ◽  
Author(s):  
Andreea Madalina Pandele ◽  
Andreea Constantinescu ◽  
Ionut Cristian Radu ◽  
Florin Miculescu ◽  
Stefan Ioan Voicu ◽  
...  

This article presents a facile synthesis method used to obtain new composite films based on polylactic acid and micro-structured hydroxyapatite particles. The composite films were synthesized starting from a polymeric solution in chloroform (12 wt.%) in which various concentrations of hydroxyapatite (1, 2, and 4 wt.% related to polymer) were homogenously dispersed using ultrasonication followed by solvent evaporation. The synthesized composite films were morphologically (through SEM and atomic force microscopy (AFM)) and structurally (through FT-IR and Raman spectroscopy) characterized. The thermal behavior of the composite films was also determined. The SEM and AFM analyses showed the presence of micro-structured hydroxyapatite particles in the film’s structure, as well as changes in the surface morphology. There was a significant decrease in the crystallinity of the composite films compared to the pure polymer, this being explained by a decrease in the arrangement of the polymer chains and a concurrent increase in the degree of their clutter. The presence of hydroxyapatite crystals did not have a significant influence on the degradation temperature of the composite film.


2017 ◽  
Vol 35 (1) ◽  
pp. 126-134 ◽  
Author(s):  
L. Chandra ◽  
J. Chandrasekaran ◽  
K. Perumal ◽  
B. Babu ◽  
V. Jayaramakrishnan

AbstractNLO active 2-aminopyridinium 4-aminobenzoate (APAB) single crystals were successfully grown by the standard slow evaporation technique. The crystallinity of the grown crystals was analyzed through X-ray diffraction (XRD) measurements. Fourier transform infrared (FT-IR) spectroscopic studies were also performed for the identification of different modes present in the compound. The UV-Vis absorption and transmittance spectra were recorded for the grown crystal and the optical band gap was calculated. Birefringence and etching studies were also carried out. The dielectric study showed that the dielectric constant decreased with an increase in frequency. The photoconductivity study revealed its positive photoconducting nature. Theoretical HOMO LUMO investigations were also made for the crystal. The relative SHG efficiency of the material was investigated by the Kurtz and Perry powder technique. The phase matching property of the crystal was studied through the SHG dependence of average particle sizes.


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