scholarly journals Structures and thermal stability of the α-LiNH4SO4 polytypes doped with Er3+ and Yb3+

2017 ◽  
Vol 73 (1) ◽  
pp. 122-133 ◽  
Author(s):  
N. P. Sabalisck ◽  
C. Guzmán-Afonso ◽  
C. González-Silgo ◽  
M. E. Torres ◽  
J. Pasán ◽  
...  
Keyword(s):  
Single Crystals ◽  
Slow Evaporation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Β Phase ◽  
Wide Range ◽  
Cyclic Temperature ◽  
Polymorphic Forms ◽  
The Stability ◽  
Thermal Stability Of

In order to clarify the polymorphism in the lithium sulfate family, LiRE x (NH4)1 − x SO4 (0.5 ≤ x ≤ 4.0 mol%, nominal value; RE = Er3+, Yb3+ and Dy3+) crystals were grown from aqueous solution by slow evaporation between 298 and 313 K. The doping of the samples allowed us to obtain two polymorphic forms, α and β, of LiNH4SO4 (LAS). By means of X-ray diffraction (XRD) in single crystals, we determined the crystal structures of two new α-polytypes, which we have named α1- and α2-LAS. They present the same space group P21/c and the following relation among their lattice parameters: a 2 = −c 1, b 2 = −b 1, c 2 = −2a 1 − c 1. In order to evaluate the stability of the new α-polytypes, we performed thermal analysis, X-ray diffraction and dielectric spectroscopy on single crystals and polycrystalline samples over the cyclic temperature range: 190 → 575  → 190 K. The results obtained by all the techniques used in this study demonstrate that α-polytypes are stable across a wide range of temperatures and they show an irreversible phase transition to the paraelectric β-phase above 500 K. In addition, a comparative study of α- and β-polytypes shows that both polymorphic structures have a common axis, with a possible intergrowth that facilitates their coexistence and promotes the reconstructive α → β transition. This intergrowth was related to small anomalies detected between 240 and 260 K, in crystals with an α-habit.

Syntheses, Crystal Structures and Thermal Stability of Co(II) and Zn(II) Complexes with Ethyl Carbazate

2005 ◽  
Vol 60 (5) ◽  
pp. 505-510 ◽  
Author(s):  
Tong-Lai Zhang ◽  
Jiang-Chuang Song ◽  
Jian-Guo Zhang ◽  
Gui-Xia Ma ◽  
Kai-Bei Yu
Keyword(s):  
Thermal Stability ◽  
Aqueous Solutions ◽  
Diffraction Analysis ◽  
Single Crystals ◽  
Slow Evaporation ◽  
X Ray Diffraction ◽  
Element Analysis ◽  
Thermal Stabilities ◽  
X Ray ◽  
Thermal Stability Of

Cobalt(II) and zinc(II) complexes of ethyl carbazate (ECZ), [Co(ECZ)3](NO3)2 and [Zn(ECZ)3] (NO3)2, were synthesized. Single crystals of these two compounds were grown from aqueous solutions using a slow evaporation method. Their structures have been determined by X-ray diffraction analysis. Both of them are monoclinic with space group P21/n. The complexes are further characterized by element analysis and IR measurements. Their thermal stabilities are studied by using TG-DTG, DSC techniques. When heated to 350 °C, only metal oxide was left for both complexes.

Growth, structural, optical, piezoelectric and etching analysis of L-lysine p-nitrophenolate monohydrate single crystals

2017 ◽  
Vol 31 (23) ◽  
pp. 1750174 ◽  
Author(s):  
A. Alexandar ◽  
A. Lakshmanan ◽  
S. Sakthy Priya ◽  
P. Surendran ◽  
P. Rameshkumar
Keyword(s):  
Single Crystals ◽  
Grown Crystal ◽  
Light Emission ◽  
Solution Technique ◽  
Slow Evaporation ◽  
X Ray Diffraction ◽  
Orthorhombic Crystal ◽  
Blue Light Emission ◽  
X Ray ◽  
Thermal Stability Of

Nonlinear optical single crystals of L-lysine p-nitrophenolate monohydrate (LLPNP) were grown in aqueous solution by the slow evaporation solution technique (SEST). The grown crystals were subjected to powder X-ray diffraction analysis, (PXRD) and it was found that the title compound was crystallized in the orthorhombic crystal system with noncentrosymmetric space group of [Formula: see text]212121. The vibrational frequencies of various functional groups present in the crystal were analyzed using the FTIR spectrum with a wavenumber range between 450 cm[Formula: see text] and 4000 cm[Formula: see text]. The microhardness analysis of the sample revealed that the crystal belongs to the soft material category. Piezoelectric analysis was performed to measure the value of the piezoelectric (d[Formula: see text]) coefficient. Blue light emission of the material was confirmed using the photoluminescence spectrum. Thermal stability of the grown crystal was analyzed using a melting point apparatus and it was found that the LLPNP is stable upto 175[Formula: see text]C. Etching analysis was performed at various durations, in order to identify the surface properties of the LLPNP crystal.

scholarly journals The Stability of Icosahedral Cd-Yb

2003 ◽  
Vol 805 ◽  
Author(s):  
Günter Krauss ◽  
Sofia Deloudi ◽  
Andrea Steiner ◽  
Walter Steurer ◽  
Amy R. Ross ◽  
...  
Keyword(s):  
Low Temperature ◽  
Ambient Temperature ◽  
Mechanical Stress ◽  
Single Crystals ◽  
High Temperatures ◽  
Low Temperatures ◽  
Ambient Pressure ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Stability

ABSTRACTThe stability of single-crystalline icosahedral Cd-Yb was investigated using X-ray diffraction methods in the temperature range 20 K ≤ T ≤ 900 K at ambient pressure and from ambient temperature to 873 K at about 9 GPa. Single-crystals remain stable at low temperatures and in the investigated HP-HT-regime. At high temperatures and ambient pressure, the quasicrystal decomposes. The application of mechanical stress at low temperatures yields to the same decomposition, the formation of Cd. A reaction of icosahedral Cd-Yb with traces of oxygen or water causing the decomposition seems reasonable, but a low-temperature instability of this binary quasi-crystal cannot be ruled out totally.

The Flavonoids of Combretum quadrangulare: Crystal structures of the Polymorphic Forms of 5-Hydroxy-2-(4'-hydroxy-3',5'-dimethoxyphenyl)-3,7-dimethoxy-4H-1-benzopyran-4-one

1985 ◽  
Vol 38 (8) ◽  
pp. 1177 ◽  
Author(s):  
IR Castleden ◽  
SR Hall ◽  
S Nimgirawath ◽  
S Thadaniti ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Β Phase ◽  
Α Phase ◽  
Polymorphic Forms

The following substituted 2-phenyl-4H-1-benzopyran-4-ones have been isolated from the dried flowers of Combretum quadrangulare Kurz ( Combretaceae ): 5-hydroxy-3,3′,4′,5′,7-pentamethoxy ( combretol ) (1), 3′,5-dihydroxy-3,4′,7-trimethoxy ( ayanin ) (2) and 4′,5-dihydroxy- 3,3′,5′,7-tetramethoxy (3). The last substance (3) was obtained as a mixture of two polymorphic forms (α and β) each of which was characterized by X-ray diffraction. Diffractometer data at 295 K were refined by full matrix least squares to residuals of 0.043 (1181 'observed' reflections) for the α-phase and 0.044 (1421) for the β phase of (3). Crystals of the α-phase of (3) are triclinic, Pī, a 12.663(6), b 9.592(4), c 7.444(4) Ǻ, α 102.48(3), β 101.39(4), γ 91.72(4)°,Z 2. Crystals of the β-phase of (3) are monoclinic P21/n, a 17.139(8), b 12.728(6), c 7.845(7) Ǻ, β 95.07(6)°, Z 4. An unambiguous synthesis of (3) was also achieved.

Brillouin scattering near the α–β phase transitions of N2 and CO

1988 ◽  
Vol 66 (4) ◽  
pp. 541-548 ◽  
Author(s):  
V. Askarpour ◽  
H. Klefte ◽  
M. J. Clouter
Keyword(s):  
Phase Transition ◽  
Single Crystals ◽  
Elastic Constants ◽  
Brillouin Scattering ◽  
X Ray Diffraction ◽  
X Ray ◽  
Β Phase ◽  
Α Phase ◽  
Mode Softening ◽  
Cubic Structure

The technique of high resolution Brillouin spectroscopy has been used to determine the adiabatic elastic constants of single crystals of β-N2 and β-CO as a function of temperature, in an effort to study the α–β phase transition. For all elastic constants, there is an increase of approximately 1%/K on cooling and there is no evidence of further mode softening, even within 0.5 K of the phase transition. Three large single crystals of α-CO were grown. The orientations were determined, by Laue X-ray diffraction, and correlated to the orientations of the parent β-crystals. The β-phase hexagonal basal planes appear to transform to planes of the form {110} in the α-phase cubic structure.

GROWTH AND CHARACTERIZATION OF NONLINEAR OPTICAL PARA-NITROANILINE (pNA) SINGLE CRYSTALS

2007 ◽  
Vol 21 (29) ◽  
pp. 2025-2032 ◽  
Author(s):  
T. BARANIRAJ ◽  
P. PHILOMINATHAN ◽  
N. VIJAYAN
Keyword(s):  
Single Crystals ◽  
Nonlinear Optical ◽  
Optical Quality ◽  
X Ray Diffraction ◽  
X Ray ◽  
Evaporation Technique ◽  
Optical Behavior ◽  
Good Optical Quality ◽  
Thermal Stability Of

Single crystals of para Nitroaniline ( pNA ), an organic nonlinear optical (NLO) material, have been grown by slow solvent evaporation technique at room temperature. Good optical quality single crystals with dimensions of up to 10 × 11 × 3 mm 3 have been grown by adopting the above technique, and good quality single crystals were obtained. The grown single crystals were subjected to different characterization analyses. The lattice dimensions have been determined from the powder X-ray diffraction analysis. Its functional groups and optical behavior have been identified from the FTIR and UV-Vis. analyses respectively. The thermal stability of the crystal has been analyzed by thermogravimetric (TG) and differential thermal (DT) analyses respectively.

CHARACTERIZATION OF KHCO3 SINGLE CRYSTALS

2004 ◽  
Vol 11 (01) ◽  
pp. 83-86 ◽  
Author(s):  
S. ABOUELHASSAN ◽  
F. SALMAN ◽  
M. ELMANSY ◽  
E. SHEHA
Keyword(s):  
Phase Transition ◽  
Activation Energy ◽  
Aqueous Solution ◽  
Single Crystals ◽  
Slow Evaporation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Slow Evaporation Technique ◽  
Evaporation Technique

Single crystals of KHCO 3 were grown by the slow evaporation technique of an aqueous solution. Characterization of the sample was done using different techniques such as X-ray diffraction, infrared spectra (IR) and the differential scanning calorimeter (DSC) technique. The analysis of the X-ray diffraction pattern indicated that the sample was a single crystal. The results obtained by IR and DSC indicated the presence of phase transition. From the analysis of DSC, the activation energy of transition was carried out by two methods (Kissinger and Ozawa).

scholarly journals The growth of decagonal Al–Co–Ni single crystals as a function of chemical composition

1997 ◽  
Vol 12 (9) ◽  
pp. 2274-2280 ◽  
Author(s):  
B. Zhang ◽  
M. Estermann ◽  
W. Steurer
Keyword(s):  
Single Crystals ◽  
Structural Changes ◽  
Ternary Systems ◽  
X Ray Diffraction ◽  
X Ray ◽  
Decagonal Phase ◽  
Different Types ◽  
Diffraction Patterns ◽  
The Stability ◽  
Diagram Analysis

Decaprismatic single crystals taken from a series of alloys of nominal compositions within Al65–77Co3–22Ni3–22 have been studied by means of x-ray diffraction techniques. The substitution of Co by Ni in increasing amounts changes the (pseudo)decagonal diffraction patterns drastically and indicates structural changes which range from a single-crystalline approximant via orientationally ordered nanodomain structures and quasiperiodic phases with different types of ordering phenomena, to a basic decagonal phase. A quantum phase diagram analysis shows a clear separation of the stability regions of the ternary systems described in this study and other decagonal phases.

scholarly journals Evaluation of Polymorphism Influence in the Finasteride

2014 ◽  
Vol 70 (a1) ◽  
pp. C1567-C1567
Author(s):  
Lucélia da Silva ◽  
Cristina Montanari ◽  
Marilene Ângelo ◽  
Edith Cristina Cazedey ◽  
Rudy Bonfilio ◽  
...  
Keyword(s):  
Physicochemical Properties ◽  
Competitive Inhibitor ◽  
Stability Study ◽  
Dissolution Profile ◽  
X Ray Diffraction ◽  
Intracellular Enzyme ◽  
X Ray ◽  
Solubility Study ◽  
Polymorphic Forms ◽  
The Stability

Finasteride is a specific competitive inhibitor of steroid type-II 5α-reductase, an intracellular enzyme that converts testosterone to dihydrotestosterone (DHT) and is widely used for the treatment of benign prostatic hyperplasia (BPH), prostate cancer , and androgenetic alopecia. Polymorphs are known to give rise to significant differences in the physicochemical properties of the compound as melting point, density, morphology, solubility and colour. Thus, proper monitoring of solid-state forms, both qualitative and quantitative, is crucial in order to ensure high-quality products. The crystal structures of finasteride appear in the Cambridge Crystal Structure Database (CSD) under the codes WOLXOK01 and WOLXOK02 for Form I and WOLXOK03 for Form II. In this context, the aim of this work was study the behavior of the chemical structure and physicochemical properties of polymorphic forms, and to evaluate the possible influence in the dissolution profile and stability of capsules. A stability study was carried out at 500C for 3 months. The Form II of finasteride was obtained by heating Form I to 2350C for 30 minutes. The techniques X-ray diffraction, infrared spectroscopy and thermal analysis were applied to characterize the Forms. The solubility of finasteride polymorphs was determined by equilibrium solubility method. For the dissolution test, water was used as dissolution medium and the basket apparatus at 100 rpm. The samples were analyzed by HPLC at 210 nm. Differences in X-ray diffraction and infrared spectra of the two polymorphs were observed. The DSC curves showed Form I melting peak at 2570C and solid-solid transformation to Form II at about 2300C. In the solubility study was observed higher Form II solubility than Form I in most evaluated pHs. The interaction of the Forms I and II with capsule excipients may have been different since the dissolution profile of the capsules showed higher release to the Form I. In the stability study, the finasteride content was stable for two Forms, however, the dissolution profile of Form II showed greater decline than the Form I. In conclusion, the results show that the dissolution profiles polymorphism may influence the quality of finasteride capsules, being necessary there be a polymorphic quality control for this dosage Form. Acknowledgments: PNPD CAPES and FAPEMIG

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