• Macromolecular Research
• /
• v.14 no.6
• /
• pp.588-595
• /
• 2006

The morphology, structure and melting behaviour of cold-crystallized isotactic polystyrene (iPS) were studied by differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD) and small angle X-ray scattering (SAXS). The polymer was found to crystallize according to the dual-lamellar stack model. The two populations of lamellae, along with a melting-recrystallization phenomenon, determined the appearance of multiple melting peaks in DSC traces. The annealing peak was attributed to the relaxation of a rigid amorphous phase, rather than to the melting of crystalline material.

• Fibers and Polymers
• /
• v.6 no.3
• /
• pp.186-199
• /
• 2005

A selection of commercially available poly(ethy1ene terephtha1ate) fibers with different degrees of molecular alignment and crystallinity have been investigated utilizing a wide range of techniques including optical microscopy, infrared spectroscopy together with thermal and wide-angle X-ray diffraction techniques. Annealing experiments showed increased molecular alignment and crystallinity as shown by the increased values of birefringence and melting enthalpies. Crystallinity values determined from thermal analysis, density, unpolarized infrared spectroscopy and X-ray diffraction are compared and discussed in terms of the inherent capabilities and limitations of each measurement technique. The birefringence and refractive index values obtained from optical microscopy are found to decrease with increasing wavelength of light used in the experiments. The wide-angle X-ray diffraction analysis shows that the samples with relatively low orientation possess oriented non-crystalline array of chains whereas those with high molecular orientation possess well defined and oriented crystalline array of chains along the fiber axis direction. X-ray analysis showed increasing crystallite size trend with increasing molecular orientation. SEM images showed micro-cracks on low oriented fiber surfaces becoming smooth on highly oriented fiber surfaces. Excellent bending characteristics were observed with knotted fibers implying relatively easy fabric formation.

• Polymer Science and Technology
• /
• v.8 no.2
• /
• pp.201-210
• /
• 1997

• Proceedings of the Korean Vacuum Society Conference
• /
• 2013.02a
• /
• pp.181-181
• /
• 2013

Recently, nanostructure and the molecular orientation of organic thin films have been largely paid attention due to its importance in organic electronics such as organic thin film transistors (OTFTs), organic light emitting diodes (OLEDs), and organic photovoltaics (OPVs). Among various methods, the diffraction and scattering techniques based on synchrotron x-rays have shown powerful results in organic thin film systems. In this work, we introduce the in-situ annealing system installed at PLS-II (Pohang Light Source II) for organic thin films by simultaneously conducting various x-ray scattering measurements of x-ray reflectivity, conventional x-ray scattering, grazing incidence wide angle x-ray scattering (GI-WAXS) and so on. Using the in-situ measurement, we could obtain real time variation of nanostructure as well as molecular orientation during thermal annealing in metal-phthalocyanine thin films. The variation of surface and interface also could be simultaneously investigated by the x-ray reflectivity measurement.

• Fibers and Polymers
• /
• v.5 no.3
• /
• pp.245-251
• /
• 2004

Poly(trimethylene terephthalate-co-trimethylene 2,6-naphthalate)s (P(TT-co-TN)s) with various copolymer composition were synthesized, and their chain structure, thermal property and crystalline structure were investigated by using $^1$H-NMR spectroscopy, differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD), respectively. It was found from sequence analysis that all the P(TT-co-TN) copolymers synthesized have a statistical random distribution of TT and TN units. It was also observed from DSC thermograms that the glass transition temperature increases linearly with increasing the TN comonomer content, whereas the melting temperature of copolymer decreases with increasing the corresponding comonomer content in respective PTT- and PTN-based copolymer, showing pseudo-eutectic melting behavior. All the samples melt-crystallized isothermally except for P(TT-co-66 mol % TN) exhibit multiple melting endotherms and clear X-ray diffraction patterns. The multiple melting behavior originates from the dual lamellar population and/or the melting-recrystallization-remelting. The X-ray diffraction patterns are largely divided into two classes depending on the copolymer composition, i.e., PTT and PTN $\beta$-form diffraction patterns, without exhibiting cocrystallization.

• Journal of the Korean Vacuum Society
• /
• v.6 no.S1
• /
• pp.127-132
• /
• 1997

Microstructure of the Fe-Ti system by ion beam mixing of multilayers at 300 K and 77 K has been studied in a wide composition range. The ion bombardment was carried out using $Ar^+$ ions at 80 keV. Using grazing angle x-ray diffraction we find that the lattice parameters of these bcc solid solutions are very close to that of $\alpha$-Fe. Extended x-ray absorption fine-structure spectroscopy have been performed to investgate the short-range order in the ion-beam-mixed state. The structure parameters, such as the interatomic distance and the coordination number are estmated from the Fe K-edge Fourier filtered EXAFS spectra. The interatomic distance is independent of the alloy concentration and it is almost constant. The study of x-ray absorption near-edge structure gives information on the individual $\rho$components of the partial densityof states of the conduction band of the Fe and Ti We also find that a charge transfer from Ti to Fe atoms takes place.

• Polymer(Korea)
• /
• v.36 no.1
• /
• pp.9-15
• /
• 2012

We prepared a series of aromatic liquid crystals (LCs) based on wholly aromatic ester units with the reactive end group methyl maleimide by means of melt condensation method, and the resulting LCs were thermally crosslinked to produce liquid crystalline thermoset (LCT) films. The synthesized LCs and LCTs were characterized with Fourier transform infrared (FTIR) spectroscopy, wide angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), thermomechanical analysis (TMA), and polarizing optical microscopy (POM) with a hot stage. The glass transition temperature ($T_g$) and coefficient of thermal expansion are strongly affected by the mesogen units in their main chain structures. The $p$-substituted biphenyl LC was found to have the highest thermal property value.

• Carbon letters
• /
• v.12 no.4
• /
• pp.229-235
• /
• 2011

Isotactic polyacrylonitrile (PAN) with triad isotacticity of 0.53, which was determined by $^{13}C$ NMR, using dialkylmagnesium as an initiator, was successfully synthesized. Isothermal treatment of iso-PAN was conducted in air at 200, 220, 250 and $280^{\circ}C$. Structural evolutions and chemical changes were studied with Fourier transformation infrared and wide-angle X-ray diffraction during stabilization. A new parameter $CNF={I_{2240cm}}^{-1}/ ({I_{1595cm}}^{-1}+f^*{I_{1595cm}}^{-1})$ was defined to evaluate residual nitrile groups. Crystallinity and crystal size were calculated with X-ray diffraction dates. The results indicated that the nitrile groups had partly converted into a ladder structure as stabilization proceeded. The rate of reaction increased with treatment temperature; crystallinity and crystal size decreased proportionally to pyrolysis temperature. The iso-conversional method coupled with the Kissinger and Flynn-Wall-Ozawa methods were used to determine kinetic parameters via differential scanning calorimetry analysis with different heating rates. The active energy of the reaction was 171.1 and 169.1 kJ/mol, calculated with the two methods respectively and implied the sensitivity of the reaction with temperature.

• The Korean Journal of Rheology
• /
• v.10 no.2
• /
• pp.98-105
• /
• 1998

가공공정중 변형을 수반하게 되는 고분자제품은 대부분 고분자사슬의 배향을 갖게 된다. 이렇나 사슬배향은 제품의 기계적, 광학적, 그리고 전기적 특성에 매우 중요한 영향을 미치는 것으로 알려져있다. 지금까지 고분자사슬의 배향상태를 나타내기 위한 여러방법은 모두 배향의 중심축을이 알려져 있다는 가정하에 전개되었다, 그러나 복잡한 배향모드를 갖 는 고분자가공의 경우에 배향중심측이 실험축과 일치하지 않는 경우가 많다 따라서 본연구 에서는 일반적인 고분자의배향상태를 나타내는 방법에 대해 알아보고 실제 고분자 가공공정 에 적용을 위해 실험적으로 배향의 대칭축을 찾을 수 있는 접근방법을 제시하고자 하였다. 그 결과 결정성 고분자의 배향상태를 광각 x-선 회절 data를 이용한2차배향 tensor를 통해 배향 타원체를 구성할수있었다. 이를PETdustls 필름과 HDPE사출성형물에 적용해 본 결과 이들의 2차 배향 tensor가 타원체를 잘 구성함을 알수 있었다. 또한 주어진 고분자의 결정 면들에 관계없이 고유한 중심축을 지니고 있음을 확인할수 있었다. 이를 통해 복잡한 배향 모드를 갖는 경우에 본연구에서 제안한 x-타원체를 통해 결정의 배향중심축을 효과적으로 찾을수 있음을 알수 있었다.

• Textile Coloration and Finishing
• /
• v.17 no.4 s.83
• /
• pp.41-47
• /
• 2005

Costume heritages of an excavated silk fabrics should be preserved without damage. In order to artificially restore the excavated silk fabrics, alkaline aqueous solution, as a simulated corpse, and two kinds of silk fabrics were used. Two kinds of silk fabrics were treated by aqueous alkaline solution according to strength retention value(100, 80, 60, 40, 20$\%$). The fine structure and physical properties of alkaline treated silk fabrics were investigated with various techniques such as wide-angle X-ray diffraction, tensile test, weight loss, shrinkage, SEM. and yellowness. As the alkaline treatment time increased tensile strength of silk fabrics decreased. However, weight loss and shrinkage slightly increased. The diffraction intensity of $\beta-form$ crystal declined and $\alpha-form$ crystal diffraction intensity disappeared with the treatment.