scholarly journals ANALISIS KARAKTERISASI XRD SINTESIS GADOLINIUM KARBONAT (Gd2(CO3)3@PEG DENGAN METODE SOLVOTERMAL

2019 ◽  
Vol 5 (1) ◽  
pp. 29-32
Author(s):  
Erika Linda Yani Nasution

Abstrak Telah dilakukan sintesis partikel pegilasi gadolinium karbonat dengan metode solvotermal menggunakan prekursor polietilen glikol (PEG-1000) dan gadolinium asetat hidrat (Gd(CH3CO3)3) pada suhu 180oC dengan waktu pemanasan selama 3 jam, 5 jam, dan 7 Jam. Partikel pegilasi gadolinium karbonat (Gd2(CO3)3@PEG tersebut selanjutnya dianalisis pola difraksi dan bentuk struktur dengan menggunakan X-Ray Diffraction (XRD). Hasil karakterisasi spektrum XRD terhadap partikel Gd2(CO3)3 menunjukkan pila difraksi dengan posisi puncak-puncak difraksi bersesuaian dengan JCPDS No. 37-0559 dengan puncak utama pada 2θ = 11.75o.  Pada waktu  pemanasan 3 jam , sampel memiliki sifat amorf, sedangkan pada sampel waktu pemanasan 5 jam dan 7 jam sampel-sampel memiliki derajat kekristalan yang baik. Pada waktu pemanasan 5 jam lebih tinggi kristalisasinya daripada 7 jam yang mengindikasikan kualitas kristal lebih baik pada lama pemanasan 5 jam.   Kata kunci : Gadolinium karbonat, metode solvotermal, PEG, XRD   Abstract   [Title: Analysis of XRD Characterization of Gadolinium Carbonate (Gd2 (CO3) 3 @ PEG Synthesis by Solvothermal Method] Synthesis of pegylated gadolinium carbonate particles by solvothermal method using polyethylene glycol (PEG-1000) and gadolinium acetate hydrate (Gd (CH3CO3) 3) precursors at 180oC with heating time for 3 hours, 5 hours and 7 hours. The gadolinium carbonate (Gd2 (CO3) 3 @ PEG particle pegylation was further analyzed by diffraction patterns and structural shapes using X-Ray Diffraction (XRD). The results of XRD spectrum characterization of Gd2 (CO3) 3 particles showed diffraction pila with diffraction peaks position. corresponds to JCPDS No. 37-0559 with the main peak at 2θ = 11.75 o At 3 hours of heating, the sample has amorphous properties, while the sample heating time is 5 hours and 7 hours the samples have a good degree of crystallization. 5 hours higher crystallization than 7 hours which indicates better crystal quality at 5 hours heating time.   Keywords: Gadolinium carbonate, solvothermal method, PEG, XRD

2011 ◽  
Vol 409 ◽  
pp. 492-496 ◽  
Author(s):  
Ayumi Hamaguchi ◽  
Masahiro Yoshizawa-Fujita ◽  
Yuko Takeoka ◽  
Masahiro Rikukawa

Layered perovskite (RNH3)2PbI4 (R = organic cation), which contained the fullerene derivatives, [ethyl-3-tert-butoxycarbonylaminopropyl (1,2-methanofullerene C60)]-61,61-di carboxylate iodide (EAF-I) and di [3-tert-butoxycarbonylaminopropyl (1,2-methanofullerene C60)]- 61,61-dicarboxylate diiodide (DAF-I2) in the organic layers were fabricated and compared with previously reported perovkite compound containing N-methyl-2-(4-aminophenyl)-fulleropyrrolidine iodide (AmPF-I). Because the solvent solubilities of EAF-I and DAF-I2 to N,N-dimethylformamide (DMF) were higher than AmPF-I, the film processability of EAF-I and DAF-I2 was improved compared with AmPF-I. The X-ray diffraction patterns proved the construction of the perovskite structure in (EAF)2PbI4 and (AmPF)2PbI4 cast films. EAF was well-organized and closer-packing than AmPF in the perovskite structure. For the diamine-type fullerene, DAF-I2, it is difficult to form layered structure by spin-coated or cast methods. New sharp X-ray diffraction peaks were observed for DAF-I2 films dipped in PbI2 solution. The intercalations and formation of perovskite structure of (DAF)PbI4 were studied.


2006 ◽  
Vol 514-516 ◽  
pp. 269-273
Author(s):  
Décio Dias ◽  
Rui Monteiro ◽  
Patrícia Almeida Carvalho ◽  
Alberto C. Ferro ◽  
Werner Lohwasser

The development of solid electrolytic tantalum capacitors with MnO2 as counter electrode has been carried out in order to decrease the equivalent series resistance (ESR). Capacitor samples produced under different pyrolysis conditions have been characterized in terms of equivalent circuit parameters. The Ta/Ta2O5/MnO2 system has also been characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). X-ray powder diffraction patterns obtained were inconclusive due to the MnO2 complex structure and to the presence of highly intense tantalum peaks that shadow interesting MnO2 diffraction peaks. Electron diffraction TEM results enabled the characterization of the microstructure and furthermore revealed the complex crystalline structure that affects the electrical properties of the semiconductor layer. A relation between the calculated circuit parameters and microstructure of MnO2 is discussed.


2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


Author(s):  
Xianxue Li

Abstract Well-dispersed cerium-doped Y2SiO5 (Ce:YSO) phosphor particles with spherical morphology and good luminescence intensity have been achieved by a solvothermal method with ethanol and water as solvent media. X-ray diffraction, Fourier transform infrared spectroscopy, fluorescence spectrophotometry and transmission electron microscopy were employed to characterize the as-synthesized Ce:YSO precursor and powders. The results showed that pure-phase Ce:YSO powders with a mean particle size of about 162 nm were accurately available at 310°C and above. The fluorescence ability and persistent luminescence decay properties of the Ce:YSO powders were also studied, and the excellent fluorescence properties could be attributed to the homogeneous Ce:YSO particles obtained through the solvothermal method.


Author(s):  
Fikri Alatas ◽  
Fahmi Abdul Azizsidiq ◽  
Titta Hartyana Sutarna ◽  
Hestyari Ratih ◽  
Sundani Nurono Soewandhi

An effort to improve the solubility of albendazole (ABZ), an anthelmintic drug has been successfully carried out through the formation of multicomponent crystal with dl-malic acid (MAL). Construction of phase solubility curve of ABZ in MAL solution and crystal morphological observations after recrystallization in the acetone-ethanol (9:1) mixture were performed for initial prediction of multicomponent crystal formation. ABZ-MAL multicomponent crystal was prepared by wet grinding or also known as solvent-drop grinding (SDG) with acetone-ethanol (9:1) mixture as a solvent followed by characterization of the multicomponent crystal formation by powder X-ray diffraction and Fourier transform infrared (FTIR) methods. The solubility of ABZ-MAL multicomponent crystal was tested in water at ambient temperature and in pH 1.2, 4.5 and 6.8 of buffered solutions at 37°C. The phase solubility curve of the ABZ in the MAL solution showed type Bs. The ABZ-MAL mixture has a different crystalline morphology than pure ABZ and MAL after recrystallization in the acetone-ethanol mixture (9:1). The powder X-ray diffraction pattern and the FTIR spectrum of ABZ-MAL from SDG different from intact ABZ and MAL powder X-ray diffraction patterns and these results can indicate the ABZ-MAL multicomponent crystal formation. The ABZ-MAL multicomponent crystal has better solubility than pure ABZ in all media used. These results can be concluded that ABZ-MAL multicomponent crystal can be prepared by solvent-drop grinding method with acetone-ethanol (9:1) mixture as a solvent and can increase the solubility of albendazole.


2005 ◽  
Vol 03 (2) ◽  
pp. 24-29
Author(s):  
P.M. PIMENTEL ◽  
A.M.G. PEDROSA ◽  
H.K.S. SOUZA ◽  
C.N.S. JÚNIOR ◽  
R.C.A. PINTO ◽  
...  

Spinel oxides with the composition ZnCo2O4 and ZnCo2O4:Eu3+ have been synthesized by the Pechini method and characterized by X-ray diffraction, infrared spectroscopy, thermal analysis and scanning electron microscopy. IR spectroscopy revealed the presence of n1 and n2 bands, typical of spinel structures. The formation of monophase cubic spinel structure was confirmed by X-ray diffraction patterns. Extra lines corresponding to other phase has been observed in the powders calcined at 900 ºC. The results showed the extremely lower synthesis temperature than those presents in conventional methods.


2004 ◽  
Vol 831 ◽  
Author(s):  
Phanikumar Konkapaka ◽  
Huaqiang Wu ◽  
Yuri Makarov ◽  
Michael G. Spencer

ABSTRACTBulk GaN crystals of dimensions 8.5 mm × 8.5 mm were grown at growth rates greater than 200μm/hr using Gallium Vapor Transport technique. GaN powder and Ammonia were used as the precursors for growing bulk GaN. Nitrogen is used as the carrier gas to transport the Ga vapor that was obtained from the decomposition of GaN powder. During the process, the source GaN powder was kept at 1155°C and the seed at 1180°C. Using this process, it was possible to achieve growth rates of above 200 microns/hr. The GaN layers thus obtained were characterized using X-Ray diffraction [XRD], scanning electron microscopy [SEM], and atomic force microscopy [AFM]. X-ray diffraction patterns showed that the grown GaN layers are single crystals oriented along c direction. AFM studies indicated that the dominant growth mode was dislocation mediated spiral growth. Electrical and Optical characterization were also performed on these samples. Hall mobility measurements indicated a mobility of 550 cm2/V.s and a carrier concentration of 6.67 × 1018/cm3


2021 ◽  
Vol 1039 ◽  
pp. 307-312
Author(s):  
Mohammad Malik Abood ◽  
Osama Abdul Azeez Dakhil ◽  
Aref Saleh Baron

Methyl ammonium lead iodide CH3NH3PbI3 Perovskite was synthesized by a new method mixing between one and two steps, in addition, the ethanol solvent was used to dissolve CH3NH3I and compared with isopropanol solvent. The characterizations of synthesized perovskite samples included the structural properties, morphological characteristics and optical properties. The intensity and orientation in X-ray diffraction patterns appear clearly in ethanol solvent while disappearing at a peak at 12o due to the speed reaction of perovskite in this solvent. Additionally, the ethanol solvent increasing the grain size of perovskite which homogeneity of the surface morphology. the ethanol solvent cause a decrease in the wavelength of absorbance edge in addition to an increase in the energy bandgap value. Keywords: Ethanol Solvent, Perovskite, Photovoltaic Technologies, X-ray diffraction.


1996 ◽  
Vol 11 (3) ◽  
pp. 230-234 ◽  
Author(s):  
M. D. Santos ◽  
J. R. Matos ◽  
L. R. F. Carvalho ◽  
L. M. Sant’Agostino ◽  
M. Korn

Characterization of some crystalline species present in atmospheric particulate matter can be investigated by an X-ray diffractometric technique. According to the analytical strategy, filtering media suitable for collecting airborne particles must be selected. In order to recognize the X-ray diffraction patterns and consequently the inherent analytical interference of filtering media, a systematic X-ray diffraction evaluation of several substrates was performed. Although artifact formation during ambient sampling can occur on quartz and glass fiber filters, these filters were also included in the diffractometric characterization. In this work, commercial filters were thermally treated and submitted to X-ray diffraction scanning. Results have shown pronounced variations in the diffractometric profiles of each thermally treated substrate. The selection criteria for choosing the filtering media was established by considering their chemical and physical properties and also the crystalline species to be collected on them.


1994 ◽  
Vol 344 ◽  
Author(s):  
T. Sano ◽  
K. Akanuma ◽  
M. Tsuji ◽  
Y. Tamaura

AbstractOxygen-deficient magnetite (ODM; Fe3O4-δ, δ>0) synthesized by reduction of magnetite with H2 at 300°C decomposed CO2 to carbon with an efficiency of nearly 100% at 300°C. In this reaction, two oxygen ions of the CO2 were incorporated into the spinel structure of ODM and carbon was deposited on the surface of ODM with zero valence to form visible particles. The particles of carbon separated from ODM were studied by Raman, energy-dispersive X-ray and wave-dispersive X-ray spectroscopies. The carbon which had been deposited on the ODM was found to be a mixture of graphite and amorphous carbon in at least two levels of crystallization. X-ray photoelectron spectroscopy and X-ray diffraction patterns of the carbon-bearing magnetite (CBM) showed no indication of carbide (Fe3C) or metallic iron (α-Fe) phase formation. In the C 1s XPS spectra of the CBM, no peaks were observed which could be assigned to CO2 or CO. X-ray diffractometry, chemical analysis and TG-MS measurement showed that the carbon-bearing Ni(II)-ferrite (CBNF) (Ni(II)/Fetotal = 0.15) synthesized by the carbon deposition reaction from CO2 with the H2-reduced Ni(II)-ferrite was represented by (Ni0.28Fe2.72O4.00)1-δ (Ni2+06.9Fe2+2.31O3.00)δCτ (δ= 0.27, τ= 0.17). The carbon of the CBNF gave the CIOlayer-like oxide containing some Ni2+ ions.


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