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

2012.7.5

課題番号 Project No.

装置責任者 Name of responsible person

2012A0048

Junichi Suzuki

実験課題名 Title of experiment

装置名 Name of Instrument/（BL No.）

Evaluation of Aggregation and Agglomeration of nano-materials
with the small angle neutron scattering technique

BL-15 TAIKAN
実施日時 Date and time of Experiment
2nd June, 2012

実験責任者名 Name of principal investigator
Takeshi Eitoku
所属 Affiliation
Advanced Institute of Science and Technology

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.
Four different forms of Carbon nanotube (CNT) dispersed solution (D2O) with 0.1% polymer Triton X-100
Detail of CNT forms are;(1) Thick and hard rod (30 nm x 1 um) multiwall CNT, made by ark-discharge method as grown.
(2) Same as (1) but purified samples.
(3) Tangled like cotton (10nm x 0.2-0.3 um) multiwall CNT, made by CVD method as grown(4) Same as (3) but purified samples

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.

Method; two different forms of MWNT(multiwall carbon nanotube) dispersion, and blank solution(0.1% Triton-X100, D2O solution) were measured by SANS technique.
Based on our previous TEM measurement, the size and forms were as follows;(1)(2) Hard and straight rod-like; the diameter is around 30-40 nm and the length is about 1 um
This hard, straight shape is consistent with the Raman G/D ratio measurement, which shows
the smaller amount of defect is included in this MWNT. (1) Scince the “as grown” samples
include a little amount of impurities, MWNT tends to connect each other and form a larger
particle. (2) In the case of “purified” sample, in which the impurities graphite is removed, major
component is a mono-dispersed rod, and large particle and bundle is a minor.

12. 実験方法及び結果（つづき） Experimental method and results (continued)(3)(4) Very flexible MWNT, the diameter is around 10nm and the length is about 0.3 um or so. Since
this MWNT is not straight, the evaluation of length is difficult and inaccurate. Also this MWNT
tends to form a large size of tangled particle by interconnecting each other. The existence of
impurities may cause a crucial effect for the formation of large tangled shape, which is notclear.
Detailed measurement conditions are as follows;
Sample (1), 1mg/ml, exposure time; 1h
Sample (2), 1 mg/ml, exposure time; 3h ( see result figure (left))
Sample (2), 0.1 mg/ml, exposure time; 3h
Sample (3), 1mg/ml, exposure time; 1h
Sample (4), 1 mg/ml, exposure time; 3h ( see result figure (right) )Sample (4), 0.1 mg/ml, exposure time; 3hBlank solution sample; 3h
Neutron intensity monitor (no sample) ; 3h
Scattered neutron of λ=0.5-7.8Å was detected with time-resolved device and distinguishedby TOF of neutron, and analyzed by 0.1Å step collection.
Result; Subtle difference could be found between the scattering patterns of MWNT samples andblank solutions as shown in the following figures, in the q-range of 0.02-0.1 Å-1 , which correspond toseveral nanometers in real-space. The structural information of single CNT and high-order CNT-CNT
interaction were very difficult to be extracted from these SANS result. If the detectors at smaller
angles are installed and the q-range of TAIKAN is expanded to the lower q region in the near future,
we will be able to obtain the various information about the form and structure about single CNT and
CNT-CNT interactions, and clarify the nature about the aggregation and agglomeration of CNT
dispersion solution. Thus, the SANS measurement using TAIKAN will have a significant importanceand great potential in the field of material science in the near future.

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SANS profile of Multiwall Carbon nanotube dispersion and blanksolutions. (Left) MWNT made by Arc method (Right) Tangled MWNT by CVD

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