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

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.

1983 ◽  
Vol 16 (2) ◽  
pp. 259-263 ◽  
Author(s):  
N. Eisenreich ◽  
W. Engel

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.


2002 ◽  
Vol 80 (11) ◽  
pp. 1469-1480 ◽  
Author(s):  
Karena Thieme ◽  
Sara C Bourke ◽  
Juan Zheng ◽  
Mark J MacLachlan ◽  
Fojan Zamanian ◽  
...  

The novel zirconatetraferrocenylcyclotrisiloxane Cp2Zr(OSiFc2)2O (6), dizirconatetraferrocenylcyclotetrasiloxane [Cp2Zr(OSiFc2)O]2 (7), boratetraferrocenylcyclotrisiloxane (C6H5)B(OSiFc2)2O (8), and diboratetraferrocenylcyclotetrasiloxane [(C6H5)B(OSiFc2)O]2 (9) with ferrocenyl (Fc = Fe(η-C5H4)(η-C5H5)) substituents at silicon have been prepared from the reactions of Cp2Zr(NMe2)2 and PhBCl2 with diferrocenylsilanediol Fc2Si(OH)2 (3) and tetraferrocenyldisiloxanediol [Fc2SiOH]2O (5). The compounds were characterized by mass spectrometry, elemental analysis, UV–vis, IR, Raman, and multinuclear NMR spectroscopy, as well as single crystal X-ray diffraction. Thermogravimetric analysis and differential scanning calorimetry investigation of 6–9 showed that the cycles decompose before they can undergo any thermal ring-opening polymerization. In addition, no polymerization was detected in the presence of either KOSiMe3 or HOTf. The bulky ferrocenyl substituents on the Si atoms are likely to be at least partially responsible for the inability of these heterocycles to undergo ring-opening polymerization. Key words: heterocyclosiloxanes, ferrocenyl.


2004 ◽  
Vol 19 (12) ◽  
pp. 3586-3591 ◽  
Author(s):  
Jiyang Chen ◽  
Ying Shi ◽  
Jianlin Shi

Nano-sized (Y,Gd)2O3:Eu powders were synthesized by a novel co-precipitation processing in which a mixture of ammonium hydroxide and ammonium hydrogen carbonate was adopted as a complex precipitant. Evolution behaviors of precursors during calcinations were studied by means of thermogravimetry-differential scanning calorimetry-mass spectrum, Fourier transform infrared, x-ray diffraction, scanning electron microscopy, and transmission electron microscopy in detail. Nano-sized (Y,Gd)2O3:Eu powder as prepared possessed a primary grain size of about 30 nm and specific surface area of 38 m2/g after being calcined at 850 °C for 2 h, showing much finer grains and less agglomeration. The as prepared nanopowder shows intense luminescence at 611nm under x-ray or ultraviolet excitation. Transparent (Y,Gd)2O3:Eu ceramics can also be fabricated using this high sinterable nanopowder.


2007 ◽  
Vol 336-338 ◽  
pp. 2340-2343 ◽  
Author(s):  
Song He Meng ◽  
Xing Hong Zhang ◽  
Wei Feng Zhang

The reaction process and kinetics of Al-TiO2-C-Ti-Fe system were investigated by differential scanning calorimetry (DSC) analysis, X-ray diffraction (XRD) analysis and scanning electron microscope (SEM). In order to obtain the information of reaction process for complicated system, the reaction characteristics of Al-TiO2, Al-TiO2-C and Al-TiO2-C-Ti systems are explored firstly. The results show that the reaction process varies with temperature in Al-TiO2-C-Ti-Fe system. At the lower temperature, the dominating reaction in Al-TiO2-C-Ti-Fe system is that between Al and Ti, Al and Fe, and so TiAlx, FeAlx, and Ti2Fe intermetallic compounds form. With the temperature increasing, the intermetallic compounds are decomposed. Then the decomposed Ti and Al react with C and TiO2 respectively and the stable TiC, Al2O3 and Fe three phases form in the final product.


2021 ◽  
Vol 2129 (1) ◽  
pp. 012092
Author(s):  
Suffi Irni Alias ◽  
Banjuraizah Johar ◽  
Syed Nuzul Fadzli Adam ◽  
Mustaffa Ali Azhar Taib ◽  
Fatin Fatini Othman ◽  
...  

Abstract The porcelain formulation containing percentages of treated FGD sludge waste from 5% up to 15% in replacement of feldspar were prepared. The porcelain mixture formulation were mixed by high energy planatery mill at speed 300 rpm for 1 hours. The powder were compacted by using hydraulic press and sintered at temperature 1200 °C for 3 hours. The sintered samples were characterized using X-ray fluorescene (XRF), X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) and Thermogravimetry/Differential scanning calorimetry (TGA/DCS). The primary effect concerning the addition of treated FGD sludge was the change of intensity composition (gypsum and anhydrate) in porcelain formulation. The XRD analysis has shown that the main component in sludge waste were gypsum and anhydrate.


EKSPLORIUM ◽  
2019 ◽  
Vol 40 (2) ◽  
pp. 99
Author(s):  
Sari Hasnah Dewi ◽  
Wisnu Ari Adi ◽  
Suyanti Suyanti

ABSTRAKPotensi logam tanah jarang (LTJ) di Indonesia sangat besar, terutama yang berasal dari mineral monasit. Monasit merupakan gabungan unsur LTJ-U/Th-fosfat yang berkaitan dengan endapan timah dan unsur-unsur radioaktif. Melalui program BATAN incorporated mineral monasit diolah menjadi bahan yang lebih benilai jual secara ekonomi. Lantanum (La) adalah logam yang termasuk dalam kelompok logam tanah jarang yang memiliki sifat-sifat unggul sebagai pigmen dan sebagai penyerap gelombang elektromagnetik. Tujuan penelitian ini adalah memperoleh informasi pengaruh pemanasan tinggi terhadap produk pilot plant pengolahan logam tanah jarang hidroksida (RE(OH)3) dari monasit, khususnya produk La2(C2O4)3 untuk pembuatan Certified Reference Material (CRM) La2O3. Bahan yang telah ditimbang dikalsinasi pada combustion boat dengan menggunakan furnace pada suhu pemanasan 1.000 OC dan 1.300 OC. Dekomposisi termal dianalisis dengan menggunakan Thermogravimetric analysis (TGA). Formasi fasa bahan dianalisis dengan menggunakan teknik X-Ray Diffraction (XRD). Hasil analisis XRD menunjukkan hasil akhir fasa bahan berubah menjadi La2O3 sebesar 28,76% dan La(OH)3 sebesar 71,24%.ABSTRACTRare earth elements (REE) in Indonesia have great potency, mainly from monazite mineral. Monazite is a combination of REE-U/Th-phosphate elements which is associated with tin deposit and radioactive elements. Through BATAN incorporated program, monazite mineral is processed to become more economically valuable materials. Lanthanum (La) is a metal element, part of REE group, which has excellent properties for pigment and electromagnetic absorber. The purpose of this study is to obtain information related to the effect of calcination in high temperature on the product of monazite’s REE hydroxide (RE(OH)3) processing pilot plant, specific on La2(C4O4)3 for Certified Reference Material (CRM) La­2O3 making. The weighed material is calcined on combustion boat by using a furnace at heating temperature of 1,000 OC and 1,300 OC. Thermal decomposition is analyzed by using Thermogravimetric analysis (TGA). Material phase formation is analyzed by using X-Ray Diffraction (XRD) method. XRD analysis shows the material in final phase has been transform to 28.76 % La2O3 and 71.24 % La(OH)3.


2006 ◽  
Vol 45 ◽  
pp. 260-265 ◽  
Author(s):  
Antônio Hortêncio Munhoz Jr. ◽  
Leila Figueiredo de Miranda ◽  
G.N. Uehara

A pseudoboehmite was obtained by sol-gel synthesis using aluminum nitrate as precursor. It was used a 2n full factorial design for studying the effect of the temperature of synthesis, the concentration of ammonium hydroxide, and the radiation dose in the product of sol-gel synthesis. The product of the synthesis was analyzed by scanning electron microscopy, x-ray diffraction of the product (after firing the pseudoboehmite at different temperatures), and it was also analyzed the temperature of endothermic and exothermic transformations using the thermo gravimetric analysis (TG) and differential scanning calorimetry (DSC). The X-ray diffraction data show that α-alumina was obtained at 1100o C.


2006 ◽  
Vol 45 ◽  
pp. 2483-2488
Author(s):  
L. Pablos ◽  
Maria Elena Villafuerte-Castrejón ◽  
A. Ibarra-Palos ◽  
J. Ocotlán-Flores ◽  
R. Sato ◽  
...  

PbBi4Ti4O15 belongs to the bismuth oxide layers family discovered by Aurivillius more than 50 years ago. In the last few years, there has been considerable interest in layered oxides exhibiting ferroelectric, piezoelectric and other related properties due to their wide range of application in technical devices. In the present work the PbBi4Ti4O15 solid solution formed with Eu3+ was synthesized by coprecipitation method and solubility limit was found. All compounds were characterized by scanning electron microscopy, density measurements and X-ray diffraction. The variation of lattice parameter with the Eu3+ concentration was obtained. Raman spectroscopy was carried out in order to determine the Eu3+ site in the lattice. Thermal analysis (thermogravimetry and differencial scanning calorimetry) results are also presented.


Author(s):  
Svetlana Cherepanova ◽  
Dina Markovskaya ◽  
Ekaterina Kozlova

The X-ray diffraction (XRD) pattern of a deleterious phase in the photocatalyst based on Cd1 − xZnxS/Zn(OH)2contains two relatively intense asymmetric peaks withd-spacings of 2.72 and 1.56 Å. Very small diffraction peaks with interplanar distances of (d) ≃ 8.01, 5.40, 4.09, 3.15, 2.49 and 1.35 Å are characteristic of this phase but not always observed. To identify this phase, the XRD patterns for sheet-like hydroxide β-Zn(OH)2and sheet-like hydrozincite Zn5(CO3)2(OH)6as well as for turbostratic hydrozincite were simulated. It is shown that the XRD pattern calculated on the basis of the last model gives the best correspondence with experimental data. Distances between layers in the turbostratically disordered hydrozincite fluctuate aroundd≃ 8.01 Å. This average layer-to-layer distance is significantly higher than the interlayer distance 6.77 Å in the ordered Zn5(CO3)2(OH)6probably due to a deficiency of CO32−anions, excess OH−and the presence of water molecules in the interlayers. It is shown by variable-temperature XRD and thermogravimetric analysis (TGA) that the nanocrystalline turbostratic nonstoichiometric hydrozincite-like phase is quite thermostable. It decomposes into ZnO in air above 473 K.


1992 ◽  
Vol 7 (4) ◽  
pp. 888-893 ◽  
Author(s):  
M. Sherif El-Eskandarany ◽  
K. Sumiyama ◽  
K. Aoki ◽  
K. Suzuki

Nonequilibrium titanium-nitride alloy powders have been fabricated by a high energetic ball mill under nitrogen gas flow at room temperature and characterized by means of x-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Initial hcp titanium is completely transformed to nonequilibrium-fcc Ti–N after 720 ks of the milling time. The fcc Ti–N phase is stable at relatively low temperature and transforms at 855 K to Ti2N and δ phases. At the final stage of milling, the particle- and grain-sizes of alloy powders are 1 mm and 5 nm, respectively, and the lattice parameter is 0.419 nm.


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