Morphological Transitions in Fluorinated and Non-Fluorinated Parylenes

1999 ◽  
Vol 565 ◽  
Author(s):  
Michael Morgen ◽  
Jie-Hua Zhao ◽  
Seung-Hyun Rhee ◽  
E. Todd Ryant ◽  
Huei-Min Ho ◽  
...  
Keyword(s):  
Significant Shift ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Two Phase ◽  
X Ray ◽  
Reversible Phase Transition ◽  
Morphological Transitions ◽  
Crystallinity Changes ◽  
Chain Contraction ◽  
Reversible Phase

AbstractA study of temperature-induced crystallinity changes in fluorinated and nonfluorinated parylene thin films using differential scanning calorimetry, thermal stress and wide angle x-ray diffraction measurements is presented. The nonfluorinated parylene (ppx-N) is shown to undergo two phase transitions between 200°C and 300°C. Both transitions show at least some degree of reversibility. The high temperature (β1 -β2) transition is accompanied by a sudden shift in stress, which is attributed to a contraction of the polymers chains. A single, reversible phase transition, occurring between 360°C and 400°C, is observed for fluorinated parylene (ppx-F). This transition is likewise marked by a significant shift in stress, and is apparently due to a similar chain contraction.

scholarly journals Tris(ethylenediamine) Cobalt(II) and Manganese(II) Nitrates

Crystals ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 472
Author(s):  
Miguel Cortijo ◽  
Ángela Valentín-Pérez ◽  
Mathieu Rouzières ◽  
Rodolphe Clérac ◽  
Patrick Rosa ◽  
...  
Keyword(s):  
Phase Transition ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
Scanning Calorimetry ◽  
Orbital Contribution ◽  
X Ray ◽  
Reversible Phase Transition ◽  
Heat Capacity Measurements ◽  
Reversible Phase

Octahedral tris(ethylenediamine) coordination complexes demonstrate helicoidal chirality, due to the arrangement of the ligands around the metal core. The enantiomers of the nitrate salts [Ni(en)3](NO3)2 and [Zn(en)3](NO3)2 spontaneously resolve to form a mixture of conglomerate crystals, which present a reversible phase transition from space group P6322 to enantiomorphic P6522 or P6122, with the latter depending on the handedness of the enantiomer. We report here the synthesis and characterization of [Mn(en)3](NO3)2 and [Co(en)3](NO3)2, which are isostructural to the Zn(II) and Ni(II) derivatives. The Mn(II) analogue undergoes the same phase transition centered at 150(2) K, as determined by single-crystal X-ray diffraction, Raman spectroscopy, and differential scanning calorimetry. The Co(II) derivative does not demonstrate a phase transition down to 2 K, as evidenced by powder X-ray diffraction and heat capacity measurements. The phase transition does not impact the magnetic properties of the Ni(II) and Mn(II) analogues; these high spin compounds display Curie behavior that is consistent with S = 1 and 5/2, respectively, down to 20 K, while the temperature-dependent magnetic moment for the Co(II) compound reveals a significant orbital contribution.

Thermal, spectroscopic and structural analysis of a thermosalient phase transformation in tapentadol hydrochloride

2019 ◽  
Vol 75 (2) ◽  
pp. 183-191 ◽  
Author(s):  
Pablo Gaztañaga ◽  
Ricardo Baggio ◽  
Emilia Halac ◽  
Daniel R. Vega
Keyword(s):  
Phase Transformation ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Covalent Interaction ◽  
Cell Parameters ◽  
Reversible Phase Transition ◽  
Abrupt Changes ◽  
Structural Differences ◽  
Interaction Scheme ◽  
Reversible Phase

Presented herein are detailed optical, thermal, spectroscopic and structural analyses of the phase transformation occurring in tapentadol hydrochloride (C14H24NO+·Cl−), a phenomenon already reported [Fischer et al. (2006); Patent: WO 2006000441 A2]. The thermal behaviour of the compound was studied using single-crystal X-ray diffraction, differential scanning calorimetry and Raman scattering measurements. The compound undergoes a first-order reversible phase transition at T heat = 318.0 (1) K, T cool = 300.0 (1) K, as assessed by the coexistence of both phases in the vicinity of the transition and the abrupt changes observed in the unit-cell parameters with temperature. The process is accompanied by clear thermosalient behaviour, with a conspicuous movement of the samples. On cooling, the transformation leads from a P212121 symmetry (Z′ = 1) to P21, with an abrupt change in β [90 ↔ 94.78 (1)°] and duplication of the asymmetric unit contents (Z′ = 2). The main structural differences observed across the transition are extremely small, with almost no changes in the stronger, non-covalent interaction scheme involving the `conventional' (N—H...Cl, O—H...Cl) hydrogen bonds.

Phase Transition and Thermochromism of the Hybrid (C12H25NH3)2FeCl4

2006 ◽  
Vol 111 ◽  
pp. 55-58
Author(s):  
L.L. Guo ◽  
Y.D. Dai ◽  
H.X. Liu ◽  
Shi Xi Ouyang
Keyword(s):  
Phase Transition ◽  
Structural Changes ◽  
Energy Transition ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Thermal Gravimetry ◽  
Reversible Phase Transition ◽  
Rotational Motions ◽  
Xrd Patterns ◽  
Reversible Phase

This paper focuses on the structural change and the thermochromism of the phase transition of the hybrid (C12H25NH3)2FeCl4. The temperature and the structures of the phase transition is investigated by a thermal gravimetry (TG) and differential scanning calorimetry (DSC), an infrared spectra (IR) and X-ray diffraction (XRD) patterns. The UV adsorption spectra account for the thermochromism. The results suggest that the reversible phase transition arises from the structural changes of the organic chains. The thermochromism is presumably due to the electrons redistribution on the levels and to the energy transition to translational and rotational motions of the organic chains.

scholarly journals Reversible phase transition in laser-shocked 3Y-TZP ceramics observed via nanosecond time-resolved x-ray diffraction

2012 ◽  
Vol 111 (5) ◽  
pp. 053526 ◽  
Author(s):  
Jianbo Hu ◽  
Kouhei Ichiyanagi ◽  
Hiroshi Takahashi ◽  
Hiroaki Koguchi ◽  
Takeaki Akasaka ◽  
...  
Keyword(s):  
Phase Transition ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Reversible Phase Transition ◽  
Reversible Phase

Phase Diagram Studies on Neopentylglycol and Pentaerythritol-Thermal Energy Storage Materials

1989 ◽  
Vol 33 ◽  
pp. 445-452 ◽  
Author(s):  
Dhanesh Chandra ◽  
Renee A. Lynch ◽  
Wei Ding ◽  
John J. Tomlinson
Keyword(s):  
Phase Diagram ◽  
Phase Transitions ◽  
Molecular Crystals ◽  
Energy Storage Materials ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Two Phase ◽  
X Ray ◽  
Organic Molecular Crystals ◽  
Chain Type

AbstractPentaerythritol (PE) and neopentylglycol (NPG) are organic molecular crystals which have hydrogen-bonded lattices with layered- and chain-type structures, respectively. The PE undergoes solid-state phase transitions at 416K, from tetragonal to a cubic (γ’) structure and NPG also undergoes this transition at 317K from a monoclinic to a cubic (γ) structure. The phase transitions in binary PE-NPG solid solutions show more than one solid-solid transition in which the NPG-rich β transforms to γ at a constant temperature but the transition of the PE-rich a phase to γ’ passes through a two-phase field at a temperature that varies as a function of composition. Structural analyses by high-temperature x-ray diffractometry have revealed some new, interesting transitions. A phase diagram has been constructed for 0-30 mol% NPG in the PE-NPG system, using x-ray diffraction and differential scanning calorimetry results, and work is in progress to complete this diagram. The variation of lattice parameters as a function of temperature in the α, γ and γ’ phases for PE+20 mol% NPG are presented here, together with a discussion of phase transitions for certain compositions.

Die quaternären Systeme ZnAl2S4-ZnGa2S4, ZnAl2S4-CdAl2S4 und ZnAl2S4-ZnAl2Se4. Röntgenographische und schwingungsspektroskopisehe Untersuchungen / Investigation of the Quaternary Systems ZnAl2S4-ZnGa2S4, ZnAl2S4-CdAl2S4 and ZnAl2S4-ZnAl2Se4 by X-Ray Diffraction and Vibrational Spectroscopy

1983 ◽  
Vol 38 (3) ◽  
pp. 311-316 ◽  
Author(s):  
H. Haeuseler ◽  
A. Cansiz
Keyword(s):  
Phase Transition ◽  
Vibrational Spectroscopy ◽  
Solid Solutions ◽  
Homogeneity Range ◽  
Binary Systems ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reversible Phase Transition ◽  
Reversible Phase ◽  
Fir Spectra

The quasi-binary systems Zn1-xCdxAl2S4, ZnAl2(1-x)Ga2xS4 and ZnAl2S4(1-x)Se4x have been investigated by X-ray diffraction and vibrational spectroscopy. In the spinel ZnAI2S4 up to 20% of Zn can be replaced by Cd. In the two other systems, ZnAl2S4 has no detectable homogeneity range. The thiogallate phases have much broader ranges of homogeneity. The compositions of the compounds at the phase boundary of the thiogallate phase are Zn0.4Cd0.6Al2S4, ZnGa0.4Al1.6S4, and ZnAl2S2.8Se1.2. At approximately 950 °C ZnAl2Se4 undergoes a reversible phase transition to a wurtzite-type structure. This phase transition is also observed for the solid solutions ZnAl2S4(1-x)Se4x; with 1.0 > x > 0.3. The FIR spectra are discussed.

Synthesis and Characterization of Thermoplastic Biomaterial Based on Acylated Chitosan Oligosaccharide

2011 ◽  
Vol 117-119 ◽  
pp. 1433-1436 ◽  
Author(s):  
Feng Hong Li ◽  
Yong Sun ◽  
San Xi Li ◽  
Shao Jun Ma
Keyword(s):  
Optical Microscope ◽  
Chitosan Oligosaccharide ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Two Phase ◽  
X Ray ◽  
Chemical Structures ◽  
Chitosan Oligosaccharides ◽  
Diffraction Peaks

A series of acylated chitosan oligosaccharides (LCSOs) were synthesized by reacting chitosan oligosaccharide (CSO) with lauroyl chloride in methane sulfonic acid. The chemical structures of LCSOs were characterized by Fourier transform infrared. Differential scanning calorimetry (DSC) showed that LCSOs had two phase transitions during heating. Thermoplastic chitosan oligosaccharide (LCSO-4) has distinct melting temperature (Tm) at 64 °C and 110°C. X-ray diffraction (XRD) analyses indicated that the crystal structure of CSO was changed through acylation and had created new crystal domains of lauroyl side chains. New strong diffraction peaks were observed around 2θ values of 20.0°, 21.5° and 26.3° for thermoplastic acylated chitosan oligosaccharide (LCSO-4). The melting and crystallization properties of thermoplastic acylated chitosan oligosaccharide were observed by polarized optical microscope (POM).

scholarly journals A Reversible Phase Transition of 2D Coordination Layers by B–H∙∙∙Cu(II) Interactions in a Coordination Polymer

Molecules ◽  
2019 ◽  
Vol 24 (17) ◽  
pp. 3204 ◽  
Author(s):  
Lei Gan ◽  
Pol G. Fonquernie ◽  
Mark E. Light ◽  
Gantulga Norjmaa ◽  
Gregori Ujaque ◽  
...  
Keyword(s):  
Phase Transition ◽  
Coordination Polymer ◽  
Thermal Activation ◽  
Bet Surface Area ◽  
Co2 Uptake ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reversible Phase Transition ◽  
Open Metal Sites ◽  
Reversible Phase

Materials that combine flexibility and open metal sites are crucial for myriad applications. In this article, we report a 2D coordination polymer (CP) assembled from CuII ions and a flexible meta-carborane-based linker [Cu2(L1)2(Solv)2]•xSolv (1-DMA, 1-DMF, and 1-MeOH; L1: 1,7-di(4-carboxyphenyl)-1,7-dicarba-closo-dodecaborane). 1-DMF undergoes an unusual example of reversible phase transition on solvent treatment (i.e., MeOH and CH2Cl2). Solvent exchange, followed by thermal activation provided a new porous phase that exhibits an estimated Brunauer-Emmett-Teller (BET) surface area of 301 m2 g−1 and is capable of a CO2 uptake of 41 cm3 g−1. The transformation is reversible and 1-DMF is reformed on addition of DMF to the porous phase. We provide evidence for the reversible process being the result of the formation/cleavage of weak but attractive B–H∙∙∙Cu interactions by a combination of single-crystal (SCXRD), powder (PXRD) X-ray diffraction, Raman spectroscopy, and DFT calculations.

Synthesis and Phase Behavior of Polysiloxane Nematic Liquid Crystal Elastomers

2012 ◽  
Vol 535-537 ◽  
pp. 1185-1188 ◽  
Author(s):  
Ying Gang Jia ◽  
Kun Ming Song ◽  
Bao Yan Zhang
Keyword(s):  
Differential Scanning Calorimetry ◽  
Phase Behavior ◽  
Liquid Crystalline ◽  
Side Chain ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
One Step ◽  
Liquid Crystal Elastomers ◽  
Reversible Phase

This paper describes the synthesis of new side chain nematic liquid crystalline elastomers (LCEs) by a one-step hydrosilication reaction. The phase behavior and mesomorphism were investigated by differential scanning calorimetry (DSC), polarizing optical microscopy (POM), and x-ray diffraction (XRD). The effect of the content of crosslinking units on the phase behavior and mesomorphism of elastomers P1 – P8 was discussed. The nematic LCEs exhibit elasticity, reversible phase transitions, and nematic thread texture. The experimental results demonstrate that the glass transition temperature and isotropic temperature of nematic LCEs decreased with increasing the content of crosslinking unit.

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