• Macromolecular Research
• /
• 제14권6호
• /
• 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
• /
• 제6권3호
• /
• 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.

• 한국고분자학회지:고분자과학과기술
• /
• 제8권2호
• /
• pp.201-210
• /
• 1997

• 한국진공학회:학술대회논문집
• /
• 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
• /
• 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
• /
• 제5권3호
• /
• 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.

• 한국진공학회지
• /
• 제6권S1호
• /
• 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.

• 폴리머
• /
• 제36권1호
• /
• pp.9-15
• /
• 2012

용융법을 이용해서 말단에 가교 반응이 가능한 메틸 말레이미드(methyl maleimide)기를 가진 전방향족 에스터 결합의 액정(liquid crystal, LC)을 합성하였고, 합성된 LC를 이용해서 적당한 열처리 과정을 통해 열경화성 액정(liquid crystalline thermoset, LCT) 필름을 제조하였다. 합성된 LC 및 LCT 필름은 FTIR(Fourier transform infrared) 분광기, WAXD(wide angle X-ray diffraction), DSC(differential scanning calorimetry), TGA(thermogravimetric analysis), TMA(thermomechanical analysis), 그리고 가열판이 장착된 편광 현미경으로 특성 분석을 하였다. 유리전이온도($T_g$)와 열팽창 계수는 주사슬 구조의 메소겐에 의해 강한 영향을 받는 것으로 확인되었고, $para$-로 치환된 비페닐구조를 가진 LCT 필름이 가장 좋은 열적 성질을 보여 주었다.

• Carbon letters
• /
• 제12권4호
• /
• 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.

• 유변학
• /
• 제10권2호
• /
• 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.

• 한국염색가공학회지
• /
• 제17권4호
• /
• 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.