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
課題番号 Project No.

2012/10/22
装置責任者 Name of responsible person

2012A0111

実験課題名 Title of experimentJun-ichi Suzuki

Characterization of water-saturated compacted montmorillonites by

装置名 Name of Instrument/（BL No.）

small-angle neutron scattering

TAIKAN (BL No. 15)

実験責任者名 Name of principal investigator

実施日 Date of Experiment

Hiroaki Takahashi

2012/6/3 - 2012/6/4

所属 Affiliation
Japan Atomic Energy Agency
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.
Used as samples is montmorillonite, Kunipia-F (the montmorillonite content is >99 wt.%), which iscommercially available from Kunimine Industries, Japan. The chemical formula of the montmorillonite isNa0.42Ca0.068K0.008(Al1.56Mg0.31Fe(III)0.09Fe(II)0.01)(OH)2(Si3.91Al0.09)O10.

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
The experiments were performed with 20-mm-diameter and 2-mm-thickness samples of deuterated
water-saturated compacted montmorillonites with dry density of 0.08, 0.4, 0.6, 0.8, 1.0, 1.2 and 1.4 Mg m-3. The
saturation of montmorillonite was carried out in a vacuum chamber to accelerate the saturation and to remove air
bubbles for more than 1 month.
Small Angle Neutron Scattering.
The SANS experiments were performed with TAIKAN/BL15 diffractometer. The used beam band was from 0.6
to 7.3 Å, which corresponds to the Q range from 0.02 to 0.6 Å with the then data acquisition. Each sample wasexposed incident neutron beam for two hours.

12. 実験方法及び結果（つづき） Experimental method and results (continued)
Results
As Figure 1 shows, intensity decreases continuously with increasing Q for all deuterated water-saturated
compacted montmorillonites. As a general observation, intensity does not reach a plateau value at low Q andshows Q-2 slope. This experimental evidence may be ascribed to the form factor of the clay thin sheets with thediameters larger than 2π/qmin ≈ 300 Å.
The swelling of montmorillonite has been designated as crystalline swelling for which d(001) is less than 19 Åand osmotic swelling due to the development of diffuse double layers within the interlayer regions leading tod(001) values which may be considerably greater than 19 Å. In the case of dry density of 0.4 Mg m-3, the peakcorresponding to the osmotic interlayer swelling at Q = 0.087 Å-1, which is 72 Å of d(001) value was observed.
Additionally, the d(001) values decreased with increasing dry density of compacted montmorillonite to 40 Å for
1.0 or 1.2 Mg m-3. The peak corresponding to the osmotic interlayer swelling was not observed at dry density of
1.4 Mg m-3. This result and our XRD data indicate that only crystalline interlayer swelling is existed at dry densityof 1.4 Mg m-3. The peak corresponding to the osmotic interlayer swelling was also not observed at dry density of
0.08 Mg m-3. This result indicates that exfoliation into single sheets became prevalent while the swollen
component declined at dry density of 0.08 Mg m-3.

Figure 1. Scattering function of deuterated water-saturated compacted montmorillonite with dry density of 0.08,0.4, 0.6, 0.8, 1.0, 1.2 and 1.4 Mg m-3. Scattering functions have been magnified in intensity by a factor of two,
except in the case of KuniF0.8 by a factor of four to make these patterns clearly visible.
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