実験報告書様式（一般利用課題・成果公開利用）（ ※本報告書は英語で記述してください。ただし、産業利用課題として採択されている方は日本語で記述していただいても結構です。 ）提出日 Date of Report

Experimental Report

2012.9.3

課題番号 Project No.

装置責任者 Name of responsible person

2012A0019

Jun-ichi Suzuki

実験課題名 Title of experiment

装置名 Name of Instrument/（BL No.）

Precise Analysis for shish-kebab structure with various molecular

BL15

weight components

実施日 Date of Experiment

実験責任者名 Name of principal investigator2012.6.22-25

Go Matsuba
所属 Affiliation
Yamagata University
試料、実験方法、利用の結果得られた主なデータ、考察、結論等を、記述して下さい。（適宜、図表添付のこと）
Please report your samples, experimental method and results, discussion and conclusions. Please add figures andtables for better explanation.
1. 試料 Name of sample(s) and chemical formula, or compositions including physical form.
Polyethylene Blend:
2M.

The molecular weight of blended deuterated and protonated polyethylene was 600 k and

The blending ratio was 97:3 by weight.

These polyethylenes was dissolved into dichlorobenzene at

160 °C and participated into methanol. The blended samples were melt pressed, therefore we got the isotropicfilms.

The films were extended in drawing rate, 5 mm/min, and temperature at 125 °C after annealing for 10min.

The drawing ratio (DR) was 1.00 (isotropic sample), 1.07, 1.39, 2.20, 2.87 and 6.00.

Figure 1 shows thedrawing polyethylene filme (DR = 1.39) and aluminum sample cell.

Figure 1: Drawing polyethylene on the sample cell.

2. 実験方法及び結果 （実験がうまくいかなかった場合、その理由を記述してください。）
Experimental method and results.

If you failed to conduct experiment as planned, please describe reasons.

Experimental Method:
These sample films were put on the sample cell as shown in Figure 1.

They were set on the sample changer in

the TAIKAN spectrometer. The exposure time was between 2 hours and 4 hours. These scattering profiles weretransported into 2D scattering profiles by Taikan software.
scattering one and subtracted the background data.

1

Then these profiles were corrected by vanadium2. 実験方法及び結果（つづき） Experimental method and results (continued)
Results:
Figure 2 shows the 2D profiles in various DR conditions.

The drawing is meridional direction of these 2D

profiles. Before drawing (DR = 1.0), the isotropic scattering pattern was observed.

In DR = 1.07, the structuralchange by drawing was quite not so strong that the scattering pattern is almost isotropic.
could observe the scattering parallel to the drawing, then kebab structure.
the lamella orientation could be occurred.

After DR = 1.39, we

The yielding point is DR =1.39, thenAfter the yielding point (DR > 1.39), the streak-like scatteringprofiles normal to the drawing direction were observed in DR = 2.20, 2.87 and 6.00.

The streak-like scatteringprofiles might be caused by the nano-scale shish structure and/or micron-scale fibril-like structure.

Figure 2 2D SANS profiles.

For more detailed analysis, we calculated 1D profiles in various DR conditions.

In Figure 3, the DR evolutionof the sector averaged SANS intensity in the scattering vector, Q. The sector angle is ±120° (0° is the equatorial
direction).

In the low DR conditions, we could find the peak from the lamella (kebab) structure in Q = 0.01 Å-1,

while in the high DR, the peaks from lamella disappeared and the shoulder grew in Q = 0.05 Å-1. This suggeststhat the nano-scale shish structure emerged and grew up.

Now we try to analyse the profiles in high Q(WANS).

Figure 3 DR evolution of SANS profiles.

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