Difference thermal analysis of crystalline solids by the use of energy-dispersive X-ray diffraction

1983 ◽  
Vol 16 (2) ◽  
pp. 259-263 ◽  
Author(s):  
N. Eisenreich ◽  
W. Engel
Keyword(s):  
Zinc Oxide ◽  
Ammonium Nitrate ◽  
Energy Dispersive ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Kinetic Evaluation ◽  
X Ray ◽  
Thermal Gravimetry ◽  
Fully Automatic ◽  
High Or Low Temperature

A method is described to study the structural behavior of solids subjected to various temperature programs. The instrumentation consists of a high- or low-temperature device, a temperature programmer, a system for energy-dispersive X-ray diffraction and a data processing and storing unit and allows the fully automatic acquisition of series of spectra. A strong data reduction is performed by summing up difference diagrams. Plotting the resulting values versus temperature yields curves comparable to those obtained by differential scanning calorimetry (DSC) or thermal gravimetry (TG). A kinetic evaluation as used in the case of DSC or TG curves is possible. The method was applied to study the thermal behavior of a mixture of ammonium nitrate with zinc oxide. The curves indicate the strong anisotropic thermal expansion of the ammonium nitrate phase IV below 323 K, its transition to phase II at 325–329 K and the solid-state reaction with zinc oxide within the temperature interval of 353–383 K.

scholarly journals Bioactivities of Geranium wallichianum Leaf Extracts Conjugated with Zinc Oxide Nanoparticles

Biomolecules ◽  
2019 ◽  
Vol 10 (1) ◽  
pp. 38 ◽  
Author(s):  
Banzeer Ahsan Abbasi ◽  
Javed Iqbal ◽  
Riaz Ahmad ◽  
Layiq Zia ◽  
Sobia Kanwal ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Zinc Oxide ◽  
Zinc Oxide Nanoparticles ◽  
Energy Dispersive ◽  
Oxide Nanoparticles ◽  
X Ray Diffraction ◽  
Leaf Extracts ◽  
Tem Analysis ◽  
X Ray ◽  
Transmission Electron

This study attempts to obtain and test the bioactivities of leaf extracts from a medicinal plant, Geranium wallichianum (GW), when conjugated with zinc oxide nanoparticles (ZnONPs). The integrity of leaf extract-conjugated ZnONPs (GW-ZnONPs) was confirmed using various techniques, including Ultraviolet–visible spectroscopy, X-Ray Diffraction, Fourier Transform Infrared Spectroscopy, energy-dispersive spectra (EDS), scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy. The size of ZnONPs was approximately 18 nm, which was determined by TEM analysis. Additionally, the energy-dispersive spectra (EDS) revealed that NPs have zinc in its pure form. Bioactivities of GW-ZnONPs including antimicrobial potentials, cytotoxicity, antioxidative capacities, inhibition potentials against α-amylase, and protein kinases, as well as biocompatibility were intensively tested and confirmed. Altogether, the results revealed that GW-ZnONPs are non-toxic, biocompatible, and have considerable potential in biological applications.

scholarly journals Synthesis, Characterization, and Thermal Decomposition of Pure and Dysprosium Doped Yttrium Phosphate System

2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
K. K. Bamzai ◽  
Nidhi Kachroo ◽  
Vishal Singh ◽  
Seema Verma
Keyword(s):  
Thermogravimetric Analysis ◽  
Ammonium Hydroxide ◽  
Xrd Analysis ◽  
Lattice Parameter ◽  
Energy Dispersive ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Structural Investigations ◽  
X Ray

Yttrium phosphate and dysprosium doped yttrium phosphate were synthesized from aqueous solutions using rare earth chloride, phosphoric acid, and traces of ammonium hydroxide. The synthesized material was then characterized for their structural investigations using powder X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM) supplemented with energy dispersive X-ray analysis (EDAX). The spectroscopic investigations were carried out using Fourier transform infrared (FTIR) spectroscopy. The thermal stability was studied using differential thermogravimetric analysis (DTA), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC) techniques. X-ray diffraction analysis reveals that both yttrium phosphate and dysprosium doped yttrium phosphate belong to tetragonal system with lattice parameter  Å,  Å and  Å,  Å, respectively. The stoichiometry of the grown composition was established by energy dispersive X-ray analysis. The EDAX analysis suggests the presence of water molecules. The presence of water molecules along with orthophosphate group and metallic ion group was confirmed by FTIR analysis. Thermogravimetric analysis suggests that decomposition in case of yttrium phosphate takes place in three different stages and the final product stabilizes after 706°C, whereas in case of dysprosium doped yttrium phosphate the decomposition occurs in two different stages, and the final product stabilizes after 519°C.

Y3Al5O12 Nanocrystallites Prepared from a Novel Crystalline Precursor

2011 ◽  
Vol 306-307 ◽  
pp. 1142-1147 ◽  
Author(s):  
Rong Jiang Han ◽  
Dan Gao ◽  
Ke Zheng Chen
Keyword(s):  
Precipitation Method ◽  
Test Results ◽  
X Ray Diffraction ◽  
Electronic Microscopy ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Air Atmosphere ◽  
Thermal Gravimetry ◽  
Measured Weight ◽  
Co Precipitation

A novel crystalline precursor for preparing Y3Al5O12 (YAG) nanocrystallite was synthesized via a co-precipitation method using (NH4)2CO3 solution as the precipitator. The precursor was characterized by means of powder X-ray diffraction (XRD), Fourier transform infrared spectra (FTIR), thermal gravimetry (TG), differential thermal gravimetry (DTG) and differential scanning calorimetry (DSC), respectively. The empirical chemical formula of the crystalline precursor can be expressed as 5[(NH4)2Al6(CO3)3(OH)14]×9[Y2(CO3)3×3H2O] according to the test results. The measured weight loss of 46.7% of the precursor without consideration of the absorbed water is in accord with the calculated value of 47.5% according to the above empirical formula. The phase-pure YAG nanocrystallites were obtained by calcining the above precursors at 900°C for 2 hours in air atmosphere. Transmission electronic microscopy (TEM) result showed that the particle size of YAG nanocrystallites is 40-80 nm. The mechanism of themal decomposition of the crystalline precursor was also presented.

Multi-Step Micro-Crystallization Studies on Amorphous Fe90-x Six B10 Alloys

1985 ◽  
Vol 58 ◽  
Author(s):  
W. Minor ◽  
R. Malmhall ◽  
Anna Roig ◽  
A. Inoue ◽  
K. V. Rao
Keyword(s):  
Differential Scanning Calorimetry ◽  
Comparative Study ◽  
Energy Dispersive ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Thermo Gravimetric ◽  
X Ray ◽  
Structure Relaxation

ABSTRACTIn order to elucidate the sensitivity and information that can be obtained from Magneto-Thermo-Gravimetric, MTG, technique, we present a comparative study of our results on structure relaxation as well as crystallization sequences as a function of time and temperature of amorphous Fe90-xSixB10 alloys in the Fe-rich regime, with those obtained from synchrotron Energy-Dispersive- X-ray-Diffraction, EDXD, and Differential Scanning Calorimetry, DSC methods.

scholarly journals Surface Modification of Nanoclay for the Synthesis of Polycaprolactone (PCL) – Clay Nanocomposite

2018 ◽  
Vol 150 ◽  
pp. 02005 ◽  
Author(s):  
Kamal Yusoh ◽  
Shamini Vesaya Kumaran ◽  
Fadwa Sameeha Ismail
Keyword(s):  
Polymer Nanocomposite ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Solution Intercalation ◽  
X Ray ◽  
Degradation Temperature ◽  
Thermal Gravimetry ◽  
Modification Method ◽  
Oligomeric Silsesquioxane

This paper presents a new modification method to modify the surface of nanoclay (Na-MMT) to increase its d-spacing using Aminopropylisooctyl Polyhedral Oligomeric Silsesquioxane (AP-POSS) and the fabrication of Polycaprolactone (PCL) nanocomposite through solution intercalation technique. The structure and morphology of pure nanoclay, modified nanoclay (POSS-MMT) and the PCL nanocomposite were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Field Emission Scanning Electron Microscopy (FESEM). XRD revealed that the d-spacing of the POSS-MMT is increased by 0.64 nm as compared to pure nanoclay. FTIR and FESEM results also showed that AP-POSS were well dispersed and intercalated throughout the interlayer space of Na-MMT. An exfoliated structure was also observed for PCL/POSS-MMT nanocomposite. Thermal properties of the nanocomposite were investigated using Thermal Gravimetry Analysis (TGA) which recorded highest degradation temperature for PCL/POSS-MMT 1% nanocomposite which is 394.1°C at 50% weight loss (T50%) but a decrease in degradation temperature when POSS-MMT content is increased and Differential Scanning Calorimetry (DSC) analysis which showed highest melting and crystallization temperature for PCL/POSS-MMT 5% nanocomposite which is 56.6°C and 32.7°C respectively whereas a decrease in degree of crystallinity for PCL/POSS-MMT nanocomposite as compared to PCL/Na-MMT nanocomposite. This study affords an efficient modification method to obtain organoclay with larger interlayer d-spacing to enhance the properties of polymer nanocomposite.

Studies on the Preparation, Characterization and Solubility of -Cyclodextrin-Roxythromycin Inclusion Complexes

2009 ◽  
Vol 2 (2) ◽  
pp. 523-530
Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  
Keyword(s):  
Dissolution Rate ◽  
Inclusion Complexes ◽  
Phase Solubility ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ir Studies ◽  
Poorly Soluble ◽  
Poorly Soluble Drug

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.

Structural Characterization of Gallbladder Stones Using Energy Dispersive X-ray Spectroscopy and X-ray Diffraction

2018 ◽  
Vol 21 (7) ◽  
pp. 495-500 ◽  
Author(s):  
Hassan A. Almarshad ◽  
Sayed M. Badawy ◽  
Abdalkarem F. Alsharari
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Energy Dispersive ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
Major Health Problem ◽  
X Ray ◽  
Gallbladder Stones ◽  
Pure Cholesterol ◽  
Scanning Electron

Aim and Objective: Formation of the gallbladder stones is a common disease and a major health problem. The present study aimed to identify the structures of the most common types of gallbladder stones using X-ray spectroscopic techniques, which provide information about the process of stone formation. Material and Method: Phase and elemental compositions of pure cholesterol and mixed gallstones removed from gallbladders of patients were studied using energy-dispersive X-ray spectroscopy combined with scanning electron microscopy analysis and X-ray diffraction. Results: The crystal structures of gallstones which coincide with standard patterns were confirmed by X-ray diffraction. Plate-like cholesterol crystals with laminar shaped and thin layered structures were clearly observed for gallstone of pure cholesterol by scanning electron microscopy; it also revealed different morphologies from mixed cholesterol stones. Elemental analysis of pure cholesterol and mixed gallstones using energy-dispersive X-ray spectroscopy confirmed the different formation processes of the different types of gallstones. Conclusion: The method of fast and reliable X-ray spectroscopic techniques has numerous advantages over the traditional chemical analysis and other analytical techniques. The results also revealed that the X-ray spectroscopy technique is a promising technique that can aid in understanding the pathogenesis of gallstone disease.

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