????? 1

Size: px

Start display at page:

Download "????? 1"

あいねみやのじょう
5 years ago
Views:

1 Application of Material Characterization to Research & Development of Polypropylenes Sumitomo Chemical Co., Ltd. Petrochemicals Research Laboratory Takashi SAKURAI Shizuto YAMAKOSHI Kenji WATANABE Naoya UMEGAKI Value-added polypropylene is one of the industrial materials desirable for saving energy and reducing stress on environment. As the material performance becomes multi-functional and advanced, material characterization plays an important role because of the complicated material characteristics. The speedy application of suitable characterization methods is very effective for promoting the research and development activities. In this article, we introduce some examples of the application to evaluate polypropylene film and compound. 212

2 1μm 4 (4) Material Die MD drawing (MD: machine direction) TD drawing (TD: transverse direction) 3 2 1 (11) (3) (13) 1. 1.2 1.4 1.6 q / Å 1 Fig.

2 Fig. 1 Electrode (Metallic foil) Dielectric (Polypropylene) Fig. 1 Terminals Dielectric Charge storage Structure of a capacitor and mechanism of charge storage 1) α α α α β β β Fig. 3α β α β βα Fig. 2 1μm 4 (4) Material Die MD drawing (MD: machine direction) TD drawing (TD: transverse direction) (11) (3) (13) q / Å 1 Fig. 2 Casting Schematic illustration of sequentially biaxial drawing process Fig. 3 Optical image and X-ray diffraction pattern of polypropylene with polymorphs: (11), (4) and (13) is the reflection peak of α crystal and (3) reflection is that of β crystal, respectively 212

5 A 2 µm B 8 µm 14β a Optical microscope

MD drawing (a) Necking (b) Draw direction

3 2) α β β3 β β β β 3) TOA Thermo Optical Analysis Fig. 4 POMFig. 5 A 2 µm B 8 µm 14β a Optical microscope Optical microscope Specimen Tensile machine Tensile machine Draw direction Sample holder Light Fig. 4 Experimental system for observing the drawing process by optical microscope (A) MD drawing (a) Necking (b) Draw direction (c) 1μm Necking Necking β form spherulite Formation of anisotropic hollow (B) TD drawing (d) (e) (f) 1μm Draw direction anisotropic hollow Formation of surface roughness Fig. 5 Optical images of film deformation in (A) MD and (B) TD drawing process 212

b c d β f β β α 3) 4) 1) BL6A Fig. 6α β 1 µm12 WAXD WAXD Fig. 7 WAXDFWHM FWHM βwaxd 35sec Fig. 6 FWHM/ Fig. 7 5 4 3 2 1.5.45.4.35.3.25 (11) (3) 1. 1.2 q / Å 1 1.4 1.6 35 sec 3 sec 2 sec 17.5 sec 12.

4 b c d β f β β α 3) 4) 1) BL6A Fig. 6α β 1 µm12 WAXD WAXD Fig. 7 WAXDFWHM FWHM βwaxd 35sec Fig. 6 FWHM/ Fig (11) (3) q / Å sec 3 sec 2 sec 17.5 sec 12.5 sec 7.5 sec sec Time evolution of circular averaged WAXD profiles observed for film with α and β spherulites during MD drawing 5 (11) (3) Time / sec Time evolution of FWHM (Full width at half maximum) observed for film with α and β spherulites during MD drawing: open and filled circles are (11) reflection of α crystal and (3) reflection of β crystal, respectively Fig. 8 SAXS α α β 12.5sec q <.2 Fig. 6 WAXD βα β α β β β 212

8.2.4.6.8 q / nm 1 q / nm 1 Time / sec 35 3 Time / sec Fig.

observed for (A) film with α and β spherulites, and (B)

9 POM Slit Pinhole Helical undulator Sample Before drawing

1 POM Vacuum path X-ray flat-panel detector (WAXD) Tensile

Experimental system for microbeam WAXD-SAXS and POM

During drawing Draw direction 1μm Representative

5 (A) (B) q / nm 1 q / nm 1 Time / sec 35 3 Time / sec Fig. 8 Time evolution of circular averaged SAXS profiles observed for (A) film with α and β spherulites, and (B) film with only α spherulites during MD drawing Fig. 9 POM Slit Pinhole Helical undulator Sample Before drawing 1μm Microbeam X-ray Optical mirror Fig. 1 POM Vacuum path X-ray flat-panel detector (WAXD) Tensile machine Sample Polarized light XRII-CCD (SAXS) Experimental system for microbeam WAXD-SAXS and POM simultaneous measurement POM Beam position WAXD SAXS During drawing Draw direction 1μm Representative POM-WAXD-SAXS data sets during MD drawing 2 β WAXD SAXS SPring-8 BL3XU 21 11), 12) 19 BL3XU Fig. 91 µm Fig. 1 POM Fig. 11α β POMβ WAXDSAXS 3 µm 1β POM SAXS α POMβ 1sec Fig. 12 α SAXS 212

6 POM sec 2sec POM sec 2sec 1μm 4sec 6sec 4sec 6sec 8sec 1sec 8sec 1sec 12sec 14sec Draw direction Beam position SAXS 7 WAXD (11) (3) Draw direction Beam position 14 sec 12 sec 1 sec 8 sec 6 sec 4 sec 2 sec Fig q / nm 1 Time evolution of POM images and circular averaged SAXS profiles in an α spherulite during MD drawing Time / sec Fig. 11 SAXS q /Å 1 sec q / nm 1 Time / sec Time evolution of POM images and circular averaged WAXD and SAXS profiles in a β spherulite during MD drawing αβ βα 212

3 Computed Tomography 13), 14) 3 µm 5 15mm 15) 25.99 31.1 Fig. 13 3 Fig. 13 23 Fig.

7 3 Computed Tomography 13), 14) 3 µm 5 15mm 15) Fig Fig Fig. 14 kv Fig. 14 (A) (B) Snap shots of high-speed impact testing at 3 C for (A) instrument panel made by polypropylene compound and (B) fiber reinforced polypropylene compound X-ray X-ray source Stage Sample Schematic illustration of X-ray CT apparatus Detector 212

fiber reinforced polypropylene compound: (A) 3D image and

16 A B A33 µm B18 µm 25 A B 19.J 16.5J Fig.

cross section Z Y X Flow direction Z Y X Flow direction

16 (A) Representative X-ray CT images of fiber reinforced

tensile testing (B) Representative X-ray CT images of

8 Fig mm 2kV (A) Z Y X Fig. 15 (B) Flow direction Representative X-ray CT images of fiber reinforced polypropylene compound: (A) 3D image and (B) cross section of X-Z plane 16) Fig. 16 A B A33 µm B18 µm 25 A B 19.J 16.5J Fig. 16 AYZ XY (A) 3D image Y-Z cross section (B) 3D image Y-Z cross section Z Y X Flow direction Z Y X Flow direction 3D image X-Y cross section 3D image X-Y cross section Z Y X Flow direction Z Y X Flow direction Fig. 16 (A) Representative X-ray CT images of fiber reinforced polypropylene compound (fiber diameter 33μm) after tensile testing (B) Representative X-ray CT images of fiber reinforced polypropylene compound (fiber diameter 18μm) after tensile testing 212

Fig. 16 BYZ XY 1 Fig. 172mm 2mm (A) (B) Fig.

$Representative SEM images on fracture front (left)$ $fracture front (right) after Izod testing: (A)$ PP/fiber with interfacial reinforcement Breaking

$2mm apart from fracture front of fiber reinforced$

9 Fig. 16 BYZ XY 1 Fig. 172mm 2mm (A) (B) Fig. 18 5μm 5μm Y-Z cross section Y-Z cross section Representative SEM images on fracture front (left) and X-ray CT images of area in 2mm apart from fracture front (right) after Izod testing: (A) PP/fiber without interfacial reinforcement and (B) PP/fiber with interfacial reinforcement Breaking area Y-Z cross section SEM2mm Fig. 18 A B Fig. 18 ASEM Fig. 18 BSEM Test piece Observation area Fig. 17 1μm Representative X-ray CT images of area in 2mm apart from fracture front of fiber reinforced polypropylene compound (fiber diameter 33μm) after tensile testing 17), 18) Izod 3 212

SPring-8 21G54 SPring-8 1),, 1, (27), p. 237. 2),,, (21), p. 121. 3) P Jr,,, (1998), p. 159. 4),,,,, 27-@, 14 (27). 5),,, 2 (7), 419 (28).

9) Y. Nozue, Y. Shinohara, Y. Ogawa, T. Sakurai, H. Hori, T. Kasahara, N. Yamaguchi, N. Yagi and Y. Amemiya, Macromolecules, 4, 236 (27). 1) Y. Shinohara, K.

Ogawa, T. Takano, S. Sasaki, S. Goto, T. Tanaka, T. Seike, S. Takahashi, K. Takeshita, N. Nariyama, H. Ohashi, T. Ohata, Y. Furukawa, T. Matsushita, Y.

Takahashi, K. Yamamoto, M. Hikosaka, S. Sakurai, Y. Shinohara, A. Okada and Y. Sugihara, Polymer J., 43, 471 (211). 13),, Polyfile, 48 (567), 26 (211).

10 SPring-8 21G54 SPring-8 1),, 1, (27), p ),,, (21), p ) P Jr,,, (1998), p ),,,,, 27-@, 14 (27). 5),,, 2 (7), 419 (28). 6),,,, 53 (1), 24 (24). 7) T. Sakurai, Y. Nozue, T. Kasahara, K. Mizunuma, N. Yamaguchi, K. Tashiro and Y. Amemiya, Polymer, 46, 8846 (25). 8),,, 19, 356 (26). 9) Y. Nozue, Y. Shinohara, Y. Ogawa, T. Sakurai, H. Hori, T. Kasahara, N. Yamaguchi, N. Yagi and Y. Amemiya, Macromolecules, 4, 236 (27). 1) Y. Shinohara, K. Yamazoe, T. Sakurai, S. Kimata, T. Maruyama and Y. Amemiya, Macromolecules, 45, 1398 (212). 11),,,,,, Polyfile, 47 (562), 21 (21). 12) H. Masunaga, H. Ogawa, T. Takano, S. Sasaki, S. Goto, T. Tanaka, T. Seike, S. Takahashi, K. Takeshita, N. Nariyama, H. Ohashi, T. Ohata, Y. Furukawa, T. Matsushita, Y. Ishizawa, N. Yagi, M. Takata, H. Kitamura, K. Sakurai, K. Tashiro, A. Takahara, Y. Amamiya, K. Horie, M. Takenaka, T. Kanaya, H. Jinnai, H. Okuda, I. Akiba, I. Takahashi, K. Yamamoto, M. Hikosaka, S. Sakurai, Y. Shinohara, A. Okada and Y. Sugihara, Polymer J., 43, 471 (211). 13),, Polyfile, 48 (567), 26 (211). 14),, 5, 97 (211). 15),, (211). 16),,,,,,,, eye, 55 (8), 32 (29). 17),, (212). 18), (212). PROFILE Takashi SAKURAI Kenji WATANABE Shizuto YAMAKOSHI Naoya UMEGAKI 212

Study on Application of the cos a Method to Neutron Stress Measurement Toshihiko SASAKI*3 and Yukio HIROSE Department of Materials Science and Enginee

Study on Application of the cos a Method to Neutron Stress Measurement Toshihiko SASAKI*3 and Yukio HIROSE Department of Materials Science and Engineering, Kanazawa University, Kakuma-machi, Kanazawa-shi,