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논문 기본 정보

자료유형
학위논문
저자정보

강찬솔 (충남대학교, 忠南大學校 大學院)

지도교수
白斗鉉
발행연도
2013
저작권
충남대학교 논문은 저작권에 의해 보호받습니다.

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Heterocyclic aromatic polybenzoxazole(PBO) is a well-known frame retardant polymer which exhibits a superior thermo-oxidative stability, chemical resistance and good mechanical properties. However, drawback of PBO is soluble only in strong acids such as sulfuric acids and polyphosphoric acids but not organic solvents. Also, a poor solubility of PBO leads to the corrosion of the equipment and vicious processability. Therefore many researchers have studied to improve solubility of the disadvantage of the PBO.
Recently, Kantor''s group has reported a new way to obtain high performance flame retardant polymers using precursors to heterocyclic aromatic polymers. Polyhydroxyamide(PHA) of these categories have good mechanical properties and can be easily converted to PBO when ignited.
PHA solution in N, N-dimethyl acetamide (DMAc) containing lithium chloride (LiCl) was prepared for wet-spinning PHA fiber. Before wet-spinning, to understand the coagulation behavior, diffusion rate test of PHA dope was performed by Ziabicki theory with various coagulants and coagulation bath temperatures and the morphological features and mechanical properties of wet-spun PHA fibers were also investigated.
The best SEM observation indicated that wet-spun PHA fibers at 20℃ in EtOH had regular cross-section and then tensile strength and initial modulus were showed 130 MPa and 7.34 GPa, respectively.
Thus, structure features-mechanical properties-initial diffusion rate relationship were characterized and identified PHA fiber was well spun Ξ (×10-6cm2/s) ranging from 2.11×10-6cm2/s to 3.11×10-6cm2/s. Among these, it was adjusted that 2.11×10-6cm2/s was ideal conditions.
The structure features and mechanical properties and WAXS analysis of PHA fibers were investigated as a function of SDR ratio during spinning process at 20℃ in EtOH. The molecular orientation of PHA fibers was consistently enhanced with increasing SDR ratio. Also, The tensile strength and initial modulus of the PHA fibers increased with SDR ratio from 84.88 to 139.85 MPa and from 3.42 to 7.77 GPa, respectively. It was resulted that intensity peaks of PHA fibers were enhanced remarkably with increasing SDR ratio with annealing. After wet-spun PHA fiber at 20℃ in EtOH was annealed at over 350℃, the tensile strength of PHA and PBO fibers increased SDR 4.4 ratio from 139.85 MPa to 162.39 MPa and initial modulus of PHA and PBO fibers decreased SDR 4.4 ratio from 7.77 GPa to 6.96 GPa.

목차

1. 서론 1
2. 이론적배경 8
3. 실험 16
3.1 재료 및 시약 16
3.2 PHA 합성 16
3.3 PHA 습식방사 . 18
3.3.1 PHA 방사 dope의 제조 . 18
3.3.2 PHA 방사 dope의 확산속도평가 18
3.3.3 PHA 습식방사 21
3.3.4 방사연신비와 열처리에 따른 PHA 섬유 및 PBO 섬유 . 23
3.4 특성 분석 . 23
3.4.1 1H-NMR 분석 . 23
3.4.2 고유점도 측정. 24
3.4.3 FT-IR 분석 24
3.4.4 열분석 . 24
3.4.4.1. DSC 분석 . 24
3.4.4.2. TGA 분석 . 25
3.4.5 FE-SEM 분석 . 25
3.4.6 인장특성 분석 25
3.4.7 WAXS 분석 25
4. 결과 및 고찰 28
4.1 PHA 합성 28
4.2 FT-IR 분석 30
4.3 PHA 열적 특성분석 32
4.3.1. DSC 분석 32
4.3.2. TGA 분석 . 33
4.4. PHA 습식방사 . 34
4.4.1. PHA 방사 dope의 제조 34
4.4.2. PHA 방사 dope의 확산속도 평가 35
4.5. 형태학적 특성 분석 . 38
4.6. 기계적 물성 분석 . 48
4.7. PHA 섬유 및 PBO 섬유의 방사연신비에 따른 결정구조분석 . 56
4.7.1. PHA 섬유 및 PBO 섬유의 방사연신비에 따른 WAXS 분석 . 56
4.7.2. PHA 섬유 및 PBO 섬유의 방사연신비에 따른 기계적 물성 분석 60
4.7.3. PHA 섬유 및 PBO 섬유의 방사연신비에 따른 형태학적 특성분석 64
5. 결론 66
참고문헌 68
Abstract . 72
감사의 글 . 75

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