Using Ultrathin-Film, Modulated Composites to Control the Reaction Mechanism of Ternary Compound Formation

1991 ◽  
Vol 238 ◽  
Author(s):  
Loreli Fister ◽  
David C. Johnson
Keyword(s):  
Ternary Compound ◽  
Reaction Pathway ◽  
Experimental Parameter ◽  
Ultrathin Film ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Compound Formation ◽  
One Dimensional ◽  
X Ray ◽  
Made In

ABSTRACTA predictable, controllable approach to the synthesis of ternary compounds through known intermediates is presented. Thin and ultrathin film superlattices were made in the Mo-Se, Cu-Se and Mo-Cu systems. Differential scanning calorimetry, low- and high-angle x-ray diffraction were used to assess the interdiffusion and nucleation reactions between elemental layers in these one-dimensional crystals. The experimental parameter modulation distance was used to influence the interfacial reactions. The results from each binary system were then used to predict the reaction pathway in the synthesis of a ternary compound, Cu2Mo6Se8. Superlattices with two different lengthscales were investigated. In the first, only one intermediate, MoSe2 which typically crystallizes at ∼200'C, is observed prior to the crystallization of Cu2Mo6Se8. In the second, no crystalline intermediates are observed below 6000 C.

scholarly journals Synthesis and Effects of Two Novel Rare-Earth Energetic Complexes on Thermal Decomposition of Cyclotetramethylene Tetranitramine (HMX)

Materials ◽  
2020 ◽  
Vol 13 (12) ◽  
pp. 2811
Author(s):  
Xuefang Cao ◽  
Zhixian Wei ◽  
Jiangfeng Song ◽  
Hedan Zhang ◽  
Yuanyuan Qu ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Rare Earth ◽  
Solid Propellant ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
One Dimensional ◽  
X Ray ◽  
Nitrate Ester ◽  
Energetic Complex ◽  
Cyclotetramethylene Tetranitramine

In order to explore the effect of the energetic complex on the thermal decomposition HMX, two new rare-earth energetic complexes [La(tza)(NO3)2(H2O)4]n (1) and [Ce(tza)(NO3)2(H2O)4]n (2) (Htza = tetrazole-1-acetic acid) were prepared by a solvent evaporation method. The obtained products were structurally characterized by Fourier-transform infrared spectroscopy (FTIR), elemental analysis, powder X-ray diffraction (PXRD), single crystal X-ray diffraction (XRD), and thermogravimetric analysis coupled with differential scanning calorimetry (TG-DSC). In addition, the compatibility of complex 1 with cyclotetramethylene tetranitramine (HMX) was studied by DSC and FTIR, respectively. Structural analysis suggested that complex 1 exhibits an orthorhombic, P 21 21 21 space group, and the La (III) ion was 10-fold coordinated in a distorted double-capped antiprism configuration. Complex 2 featured a one-dimensional, right-handed helical infinite chain. The effect of complexes 1 and 2 on the thermal decomposition of HMX was investigated by DSC, which revealed that complex 1 showed a slightly better effect than 2 on the thermal decomposition of HMX and released more heat. Furthermore, complex 1 had good compatibility with HMX, indicating that it may act as a combustion promoter for nitrate ester plasticized polyether (NEPE) solid propellant.

scholarly journals Synthesis of Two Novel Azilsartan Cocrystals: Preparation, Physicochemical Characterization and Solubility Studies

Crystals ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 739
Author(s):  
Lei Gao ◽  
Xian-Rui Zhang
Keyword(s):  
Water Solubility ◽  
Physicochemical Characterization ◽  
Dimensional Structure ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
One Dimensional ◽  
X Ray ◽  
Solubility Study ◽  
Solution Crystallization

Azilsartan is a novel angiotension II receptor blocker primarily used to treat high blood pressure. This is not a formulation-friendly molecule largely due to the inherent water-solubility pitfalls. In this paper, two novel cocrystals of azilsartan (AZ) were studied (AZ-BIP, AZ-BPE; BIP = 4,4′-bipyridine, BPE = trans-1,2-bis (4-pyridyl) ethylene) by solution crystallization. The structures of these two cocrystals were characterized by powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), including the single-crystal structure determination of AZ-BIP and AZ-BPE. In the cocrystals AZ-BIP (2:1) and AZ-BPE (2:1), two AZ molecules and one coformer formed a sandwich structure through N-H…N interactions. These sandwich structures were extended into a one-dimensional structure through O-H…N hydrogen bonds. The equilibrium solubility study demonstrated that the AZ-BIP and AZ-BPE cocrystals both showed higher solubility than azilsartan in water.

scholarly journals Synthesis, Structure, and Dielectric Properties of (3-Nitroanilinium) (18-Crown) (PF6)

Crystals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1028
Author(s):  
Le Wang ◽  
Liu-lei Qin ◽  
Yang Liu ◽  
Peng Wang ◽  
Hui-ting Xu ◽  
...  
Keyword(s):  
Variable Temperature ◽  
Structural Phase ◽  
Dielectric Measurements ◽  
Slow Evaporation ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
Scanning Calorimetry ◽  
One Dimensional ◽  
X Ray ◽  
Potential Energy Calculations

(3-Nitroanilinium) (18-crown) (PF6) (1), which is an organic-inorganic hybrid containing one-dimensional chains of hydrogen-bonded supramolecular cations, was synthesized under slow evaporation conditions and subjected to differential scanning calorimetry, temperature-dependent dielectric measurements, and variable-temperature single-crystal X-ray diffraction analysis. These analyses revealed the occurrence of a reversible structural phase transition [P21/n P21/c] at 223 K and a dielectric anomaly, which, based on the results of structural analysis and potential energy calculations, was attributed to the synergistic effect between the pendulum-like motion of the nitro group in the supramolecular cation, (3-nitroanilinium)(18-crown), and the order-disorder motion of PF6− anions.

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.

scholarly journals A review of nanotechnology with an emphasis on Nanoplex

2015 ◽  
Vol 51 (2) ◽  
pp. 255-263
Author(s):  
Rupali Nanasaheb Kadam ◽  
Raosaheb Sopanrao Shendge ◽  
Vishal Vijay Pande
Keyword(s):  
Drug Delivery ◽  
Drug Delivery Systems ◽  
Drug Loading ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Conventional Drug ◽  
Anionic Drugs ◽  
Oppositely Charged ◽  
The Brain

<p>The use of nanotechnology based on the development and fabrication of nanostructures is one approach that has been employed to overcome the challenges involved with conventional drug delivery systems. Formulating Nanoplex is the new trend in nanotechnology. A nanoplex is a complex formed by a drug nanoparticle with an oppositely charged polyelectrolyte. Both cationic and anionic drugs form complexes with oppositely charged polyelectrolytes. Compared with other nanostructures, the yield of Nanoplex is greater and the complexation efficiency is better. Nanoplex are also easier to prepare. Nanoplex formulation is characterized through the production yield, complexation efficiency, drug loading, particle size and zeta potential using scanning electron microscopy, differential scanning calorimetry, X-ray diffraction and dialysis studies. Nanoplex have wide-ranging applications in different fields such as cancer therapy, gene drug delivery, drug delivery to the brain and protein and peptide drug delivery.</p>

scholarly journals Diethylstilbestrol Modifies the Structure of Model Membranes and Is Localized Close to the First Carbons of the Fatty Acyl Chains

Biomolecules ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 220
Author(s):  
Alessio Ausili ◽  
Inés Rodríguez-González ◽  
Alejandro Torrecillas ◽  
José A. Teruel ◽  
Juan C. Gómez-Fernández
Keyword(s):  
Membrane Surface ◽  
Water Layer ◽  
Fatty Acyl ◽  
31P Nmr Spectroscopy ◽  
Relaxation Rates ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Acyl Chains ◽  
Dynamics Simulations

The synthetic estrogen diethylstilbestrol (DES) is used to treat metastatic carcinomas and prostate cancer. We studied its interaction with membranes and its localization to understand its mechanism of action and side-effects. We used differential scanning calorimetry (DSC) showing that DES fluidized the membrane and has poor solubility in DMPC (1,2-dimyristoyl-sn-glycero-3-phosphocholine) in the fluid state. Using small-angle X-ray diffraction (SAXD), it was observed that DES increased the thickness of the water layer between phospholipid membranes, indicating effects on the membrane surface. DSC, X-ray diffraction, and 31P-NMR spectroscopy were used to study the effect of DES on the Lα-to-HII phase transition, and it was observed that negative curvature of the membrane is promoted by DES, and this effect may be significant to understand its action on membrane enzymes. Using the 1H-NOESY-NMR-MAS technique, cross-relaxation rates for different protons of DES with POPC (1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine) protons were calculated, suggesting that the most likely location of DES in the membrane is with the main axis parallel to the surface and close to the first carbons of the fatty acyl chains of POPC. Molecular dynamics simulations were in close agreements with the experimental results regarding the location of DES in phospholipids bilayers.

scholarly journals Effects of Sintering Temperature on Densification, Microstructure and Mechanical Properties of Al-Based Alloy by High-Velocity Compaction

Metals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Xianjie Yuan ◽  
Xuanhui Qu ◽  
Haiqing Yin ◽  
Zaiqiang Feng ◽  
Mingqi Tang ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
High Velocity ◽  
Sintered Density ◽  
Sintering Temperature ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Transmission Electron ◽  
High Velocity Compaction ◽  
Sintered Temperature

This present work investigates the effects of sintering temperature on densification, mechanical properties and microstructure of Al-based alloy pressed by high-velocity compaction. The green samples were heated under the flow of high pure (99.99 wt%) N2. The heating rate was 4 °C/min before 315 °C. For reducing the residual stress, the samples were isothermally held for one h. Then, the specimens were respectively heated at the rate of 10 °C/min to the temperature between 540 °C and 700 °C, held for one h, and then furnace-cooled to the room temperature. Results indicate that when the sintered temperature was 640 °C, both the sintered density and mechanical properties was optimum. Differential Scanning Calorimetry, X-ray diffraction of sintered samples, Scanning Electron Microscopy, Energy Dispersive Spectroscopy, and Transmission Electron Microscope were used to analyse the microstructure and phases.

scholarly journals Extraction of Boron from Ludwigite Ore: Mechanism of Soda-Ash Roasting of Lizardite and Szaibelyite

Minerals ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 533 ◽  
Author(s):  
Xin Zhang ◽  
Guanghui Li ◽  
Jinxiang You ◽  
Jian Wang ◽  
Jun Luo ◽  
...  
Keyword(s):  
Sodium Carbonate ◽  
Energy Dispersive Spectrometer ◽  
Low Grade ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Selective Activation ◽  
X Ray ◽  
Shed Light ◽  
Soda Ash ◽  
Scanning Electron

Ludwigite ore is a typical low-grade boron ore accounting for 58.5% boron resource of China, which is mainly composed of magnetite, lizardite and szaibelyite. During soda-ash roasting of ludwigite ore, the presence of lizardite hinders the selective activation of boron. In this work, lizardite and szaibelyite were prepared and their soda-ash roasting behaviors were investigated using thermogravimetric-differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), and scanning electron microscope and energy dispersive spectrometer (SEM-EDS) analyses, in order to shed light on the soda-ash activation of boron within ludwigite ore. Thermodynamics of Na2CO3-MgSiO3-Mg2SiO4-Mg2B2O5 via FactSage show that the formation of Na2MgSiO4 was preferential for the reaction between Na2CO3 and MgSiO3/Mg2SiO4. While, regarding the reaction between Na2CO3 and Mg2B2O5, the formation of NaBO2 was foremost. Raising temperature was beneficial for the soda-ash roasting of lizardite and szaibelyite. At a temperature lower than the melting of sodium carbonate (851 °C), the soda-ash roasting of szaibelyite was faster than that of lizardite. Moreover, the melting of sodium carbonate accelerated the reaction between lizardite with sodium carbonate.

Quantitative Study of Al/W Interaction In Si/SiO2/W-Ti/Al Thin Film System

1988 ◽  
Vol 119 ◽  
Author(s):  
Hung-Yu Liu ◽  
Peng-Heng Chang ◽  
Jim Bohlman ◽  
Hun-Lian Tsai
Keyword(s):  
Thin Film ◽  
Film System ◽  
X Ray Diffraction ◽  
Compound Formation ◽  
X Ray ◽  
Thin Film System ◽  
Glancing Angle ◽  
Integrated Intensity ◽  
Al Thin Film ◽  
Kinetics Of

AbstractThe interaction of Al and W in the Si/SiO2/W-Ti/Al thin film system is studied quantitatively by glancing angle x-ray diffraction. The formation of Al-W compounds due to annealing is monitored by the variation of the integrated intensity from a few x-ray diffraction peaks of the corresponding compounds. The annealing was conducted at 400°C, 450°C and 500°C from 1 hour to 300 hours. The kinetics of compound formation is determined using x-ray diffraction data and verified by TEM observations. We will also show the correlation of the compound formation to the change of the electrical properties of these films.

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