Compatibilization of side-chain, thermotropic, liquid-crystalline ionomers to blends of polyamide-1010 and polypropylene

A novel side-chain, liquid-crystalline ionomer (SLCI) with a poly(methyl hydrosiloxane) main chain and side chains containing sulfonic acid groups was used in blends of polyamide-1010 (PA1010) and polypropylene (PP) as a compatibilizer. The morphological structure, thermal behavior, and liquid-crystalline properties of the blends were investigated by Fourier transform infrared, differential scanning calorimetry, thermogravimetric analysis, and scanning electron microscopy. The morphological structure of the interface of the blends containing SLCI was improved with respect to the blend without SLCI. The compatibilization effect of greater than 8 wt % SLCI for the two phases, PA1010 and PP, was better than the effects of other SLCI contents in the blends.

Improved thermal fractionation technique for chain structure analysis of ethylene/alpha-olefin copolymers

In this report, we describe an improved thermal fractionation technique used to characterize the polydispersity of crystalline ethylene sequence length (CESL) of ethylene/alpha -olefin copolymers. After stepwise isothermal crystallization, the crystalline ethylene sequences are sorted into groups by their lengths. The CESLs are estimated using melting points of known hydrocarbons. The content of each group is determined using the calibrated peak area. The statistical terms: the arithmetic mean (L) over bar (n), the weighted mean (L) over bar (w) and the broadness index I = (L) over bar (w)/(L) over bar (n) are used to describe the distribution of CESL. Results show that improved thermal fractionation technique can quantitatively characterize the polydispersity of CESL with a high degree of accuracy.

Crystal structure and variation in unit cell parameters with crystallization temperatures of poly (ether ketone ether ketone ketone)s containing meta-phenyl links (PEKEKmK)

The X-ray diffraction patterns of the crystalline aromatic ketone polymer PEKEKmK (aryl ether ketone ether ketone ketone polymer containing meta-phenyl links) have been investigated (for the chemical structure, see Formula). An orthorhombic unit cell is proposed to contain two chains with a = 0.772 nm, b = 0.604 nm and c = 2.572 nm. According to the orthorhombic system, the 11 reflections of this polymer were indexed. Meanwhile, variation in unit cell parameters with crystallization temperatures of PEKEKmK was also investigated. [GRAPHICS]

Influence of annealing on structure of Nylon 11

Differential scanning calorimeter (DSC), wide-angle X-ray diffraction (WAXD), small-angle X-ray scattering (SAXS), and density techniques have been used to investigate the structural parameters of the solid state of Nylon 11 annealed at different temperatures. The equilibrium heat of fusion Delta H-m(0) and equilibrium melting temperature T-m(0) were estimated to be 189.05 J g(-1) and 202.85 degrees C respectively by using the Hoffman-Weeks approach. The degree of crystallinity (W-c,W-x) ranged approximately 24-42% was calculated by WAXD and compared with those by calorimetry (W-c,W-h) and density (W-c,W-d) measurements. The radius of gyration R-g, crystalline thickness L-c, noncrystalline thickness L-a, long period L, semiaxes of the particles (a, b), electron-density difference between the crystalline and noncrystalline regions eta(c) - eta(a), and the invariant Q increased with increasing annealing temperature. The analysis of the SAXS data was based upon the particle characteristic function and the one-dimensional electron-density correlation function. An interphase region existed between the crystalline and noncrystalline region with a clear dimension of about 2 nm for semicrystalline Nylon 11. Instead of the traditional two-phase model, a three-phase model has been proposed to explain these results by means of SAXS.

Homoepitaxial crystallization in films of a thermotropic liquid crystalline chloro-poly(aryl ether ketone)

The homoepitaxial crystallization in the films of a thermotropic liquid crystalline chloro-ply(aryl ether ketone) is studied by transmission electron microscopy (TEM) and electron diffraction (ED). The homoepitaxy takes place in the temperature range 330-320 degreesC, in which a highly-ordered smectic crystalline phase of the copolymer with a single-crystal-like banded structure is formed during the cooling process from the isotropic melt. The homoepitaxial crystallizations with angles of 32 degrees and 122 degrees between the two b axes are the major populations observed, and possess epitaxial contact planes of (100)(I)-(210)(II) and (010)(I)-(210)(II); respectively.

Phase structure and transitions in a poly(methyloctadecylsilane) oligomer

A poly(methyloctadecylsilane) oligomer was synthesized by a typical Wurtz coupling reaction. Upon cooling, three transitions were observed at temperatures of 39.9, 37.5 and 33.9 degreesC at a rate of 2.5 degreesC/min in differential scanning calorimetry (DSC). The first transition, with enthalpy change of 0.47 kT/mol and supercooling of 0.2 degreesC, was characteristic of the conformational change in the Si-Si backbone into an all-trans conformation, which was detected by temperature-dependent Fourier transform infrared (FT-FR) spectroscopy. The second and the third transitions with large supercooling were identified as the formation of two-dimensional hexagonal crystal packing and three-dimensional two-chain orthorhombic crystal packing, respectively. The crystal structure was determined by the combination of WAXD and transmission electron microscopy (TEM) experiments. (C) 2000 Elsevier Science Ltd. All rights reserved.

Syntheses and crystalline structures of clusters Co-3(CO)(7)(mu(3)-S)(mu, eta(2)-SCNR2)

Through the reaction of Co-2(CO)(8) with four thiuram [R2NC(S)S](2), four new sulfur-capped trinuclear cobalt carbonyl clusters Co-3 (CO)(7) (mu(3)-S) (mu, eta(2)-S* C* NR2) ( I : R = Me; I : R = Et; II : R = i-Pr; IV : NR= -N [GRAPHICS] were prepared and characterized by elementary analysis, IR,H-1 NMR and MS spectroscopy. The crystal structure of the cluster Co-3(CO)(7)(mu(3)-S)[mu, eta(2)-S*C*N (i-Pr)(2)]( III) was determined by X-ray single crystal diffraction method. The crystal of m is monoclinic, belonging to space group P2(1)/n, and the cell parameters are as follows: a = 1, 145 2(2) nm, b = 1. 502 8(3) nm, c = 1, 214 4(2) nmj alpha = 90 degrees, beta = 92, 15(3)degrees, gamma = 90 degrees; V = 2. 088 5(7) nm(3) , Z = 4, F (000) = 1 096, D-c = 1. 747 mg . m(-3), mu = 2. 588 mm(-1), R=0. 040 7, R-w=0. 062 4, The structural analysis shows that cluster II has a pyrimidal Co3S framework and contains a heterocylic bridging bidentate ligand [mu, eta(2)-S* C* N (i-Pr)(2)] linked to the Co2 and Co3 atoms of the cluster by a cobalt-carbon and a cobalt-sulfur bond respectively.

Influence of interface on radiation effects of crystalline polymer - radiation effects on polyamide-1010 containing BMI

Aimed at saving the radiation dose required to crosslinking the polyamid-1010, BMI/PA1010 systems containing different amounts of difunctional crosslinking agent N,N'-bis-maleimide-4,4'-biphenyl methane (BMI) were prepared and the structure changes at the crystallographic and supermolecular levels before and after irradiation were studied by using WAXD, SAXS, and DSC techniques. It was found that by incorporation of BMI the microcrystal size L-100 is lowered due to the formation of hydrogen bond between the carbonyl oxygen of BMI and the amide hydrogen of PA1010 in the hydrogen bonded plane, and the overall crystallinity W-c is also decreased. The presence of BMI causes the crystal lamella thickness d(c) to decrease and greatly thickens the transition zone d(tr) between the crystalline and amorphous regions. As for the irradiated specimen, the maximum increments in the L-100 and W-c against dose curves decrease with BMI content, and the interception point D-i, at which the L-100 and W-c curves intercept their respective horizontal line of L-100/L-100(0) and W-c/W-c(0)=1, shift to lower dose with an increase in BMI concentration. In addition. the mechanism of the radiation chemical reactions in the three different phases under the action of BMI are discussed with special focus on the interface region. (C) 1999 Published by Elsevier Science Ltd. All rights reserved.

Structure and non-linear optical properties of beta-barium borate

The non-linear optical (NLO) properties of crystalline beta-BaB2O4 (beta-barium borate, BBO) have been investigated from the chemical bond viewpoint. The contributions of each type of chemical bond to the total NLO coefficient have been quantitatively determined. The calculations indicate that the true space group of BBO is R3 rather than R3c.

Influence of annealing on structure of poly(aryl ether ether ketone ketone) revealed by SAXS

Structural studies of poly(aryl ether ether ketone ketone) (PEEKK) using small-angle X-ray scattering and one-dimensional electron density correlation function methods revealed that its aggregated state structure was significantly influenced by the annealing temperature. The long period L, the average thickness of the lamellae d, the electron density difference between the crystalline and amorphous regions eta(c) - eta(a), and the invariant Q increased with increasing annealing temperature, but it was opposite to the case of the specific inner surfaces O-s. A transition zone existed between the traditional "two phases" with a dimension about 0.5 nm for semicrystalline PEEKK. (C) 1998 John Wiley & Sons, Inc. J Appl Polym Sci 69: 1829-1835, 1998.

Studies on carbosillane liquid crystalline dendrimer with S-c* phase

A liquid crystalline carbosilane dendrimer with Sc* phase has been synthesized in successive steps, resulting in the formation of defined, unimolecular compound. Twelve biphenyl mesogenic units were attached on its periphery and it has a three dimentional, treelike starburst structure. Its phase behavior was K95S(c)*103Ch118I. Compared.with its biphenyl mesogenic unit , 4-(2'-methylbutyl)-4'-(omega-hydroxyhexyl) azobenzene , which was melted at 128 degrees C and is not a liquid crystal, it is a good liquid crystal material with Sc* phase.

Synthesis and characterization of the side chain liquid crystalline poly(monoester {6-[4-(p-nitrophenyl)azo]phenoxy-1-hexyloxy} of maleic anhydride)

The poly(monoester (6-[4-(p-nitrophenyl) azo]phenoxy-1-hexyloxy) of maleic anhydride) shows a smectic phase with a focal conic fan texture. With the decrease of the monoestering degree the phase transition temperature decreases and the mesomorphic temperature range becomes narrow. The hydrogen bonding between two carboxylic acid groups was found to play a very important role in forming the smectic phase structure. The smectic bilayer structure has been built through self-assembly via. intermolecular hydrogen bonding.

Structure and order of the discotic compound 2,3,6,7,10,11-hexakispentyloxytriphenylene as revealed by diffraction and molecular simulation studies

The aggregate structure of the discotic compound 2,3,6,7,10,11-hexakispentyloxytriphenylene (HPT) was studied both for the crystalline state and the liquid crystalline state by using electron crystallography and a molecular simulation approach. In the crystalline state, HPT was found to adopt an orthorhombic P-2212 space group with cell parameters a = 36.73 Angstrom, b = 27.99 Angstrom and c = 4.91 Angstrom. Molecular packing calculations were conducted to elucidate the molecular conformation and mutual orientational characteristics in the different states. Phase transitions and relationships are discussed from a structural point of view.

The crystal structure and drawing-induced polymorphism in poly(aryl ether ketone)s .1. Poly(oxybiphenyl-4-4'-diyloxy-1,4-phenylenecarbonyl-1,3-phenylenecarbonyl-1,4-phenylene)

Crystal structure and polymorphism induced by uniaxial drawing of a poly(aryl ether ketone) [PEDEKmK] prepared from 1,3-bis(4-fluorobenzoyl)benzene and biphenyl-4,4'-diol have been investigated by means of transmission electron microscopy (TEM), electron diffraction (ED), wide-angle X-ray diffraction (WAXD), and differential scanning calorimetry (DSC) techniques. The melting and recrystallization process in the temperature range of 250-260 degrees C, far below the next melting temperature (306 degrees C), was identified and found to be responsible for the remarkable changes in lamellar morphology. Based on WAXD and ED patterns, it was found that crystal structure of isotropic-crystalline PEDEKmK obtained under different crystallization conditions (melt-crystallization, cold-crystallization, solvent-induced crystallization, melting-recrystallization, and crystallization from solution) keeps the same mode of packing, i.e., a two-chain orthorhombic unit cell with the dimensions a = 0.784 nm, b = 0.600 nm, and c = 4.745 nm (form I). A second crystal modification (form II) can be induced by uniaxial drawing above the glass transition temperature, and always coexists with form I. This form also possesses an orthorhombic unit cell but with different dimensions, i.e., a = 0.470 nm, b = 1.054 nm, c = 5.064 nm. The 0.32 nm longer c-axis of form II as compared with form I is attributed to an overextended chain conformation due to the expansion of ether and ketone bridge bond angles during uniaxial drawing. The temperature dependence of WAXD patterns for the drawn PEDEKmK suggests that form II can be transformed into the more stable form I by relaxation of overextended chains and relief of internal stress at elevated temperature in absence of external tension.

Synthesis and characterization of aromatic liquid crystalline poly(ester-imide)s derived from an imidodicarboxylic acid

A new class of liquid crystalline poly(ester-imide)s was synthesized by melt polycondensation. The basic physical properties of the resulting polymers were investigated by differential scanning calorimetry (d.s.c.), wide-angle X-ray diffraction (WAXD), polarized light microscopy, scanning electron microscopy (SEM), thermogravimetric analysis (t.g.a.), and rheological and mechanical testing. All of these poly(ester-imide)s were amorphous, as reflected by the results obtained from the WAXD and d.s.c. studies. Characterization and comparison of these poly(ester-imide)s with the corresponding polyesters suggested that the introduction of imide groups into the polyester chain is favourable for the formation of liquid crystalline phases. These results, together with the rheological studies, suggested that there existed a form of strong inter- or intramolecular electron donor-acceptor interaction which played a significant role in the liquid crystalline properties of the poly(ester-imide)s. The polymer products thus obtained exhibited good mechanical properties, with flexural strengths and moduli as high as 174 MPa and 6.9 GPa, respectively. The morphology of the fracture surfaces of extruded rod samples showed a sheet-like structure which consisted of ribbons and fibres oriented along the flow direction. The glass transition temperatures and thermal stabilities of the polymers were improved by the incorporation of imide groups. Copyright (C) 1996 Elsevier Science Ltd.