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。 ）Experimental Report
課題番号 Project No.
2015A0026
実験課題名 Title of experiment
SANS study of the kinetics of nanoparticles in oxide dispersion
strengthened (ODS) steels
実験責任者名 Name of principal investigator
Hiroaki MAMIYA所属 Affiliation

承認日 Date of Approval 2016/12/4
承認者 Approver Jun-ichi SUZUKI
提出日 Date of Report 2016/12/4

装置責任者 Name of Instrument
scientist
Jun-ichi SUZUKI
装置名 Name of Instrument/（BL No.）
TAIKAN/BL-15
実施日 Date of Experiment
22nd Feb. to 23rd Feb.

National Institute for Materials Science
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.
Sample 1: 17.8Cr-13.35Ni-2.2Mo-0.09Mn-0.86Si-0.02C-Fe(Bal.)
Sample 2: 17.8Cr-13.35Ni-2.2Mo-0.09Mn-0.86Si-0.02C-Fe(Bal.)
Sample 3: 13Cr-30Mn-0.5N-0.35Y2O3-Fe(Bal.)
Sample 4: 13Cr-30Mn-0.5N-0.35Y2O3-Fe(Bal.)
Sample 7: 13Cr-30Mn-0.5N-0.35Y2O3-Fe(Bal.)
Sample 8: 13Cr-30Mn-0.5N-0.35Y2O3-Fe(Bal.)
Sample 11: 13Cr-30Mn-0.5N-0.35Y2O3-Fe(Bal.)
Sample 12: 13Cr-30Mn-0.5N-0.35Y2O3-Fe(Bal.)
Sample 3_700, Sample 3_800, Sample 3_900, Sample 3_1000: 13Cr-30Mn-0.5N-0.35Y2O3-Fe(Bal.)
Sample 16: 16Cr-15Co-5Ti-3Mo-2.5Al-1.5W-Ni(Bal.)
Sample 17: 16Cr-15Co-5Ti-3Mo-2.5Al-1.5W-Ni(Bal.)
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
The samples were measured by the small angle neutron scattering (SANS) instrument TAIKAN.
The material was manufactured from elemental powders of Fe, Cr, Mn and Y2O3 by mechanical alloying
under the nitrogen atmosphere. After 40h of milling powder was sintered in four conditions 5 min or 15 min and950ºC or 1000ºC. To investigate thermal stability one sample, sintered in 1000 ºC for 5 min, was annealed infour temperatures, 700, 800 900 and 1000 ºC.
For all of them, the direct beam and scattering from glassy carbon were measured. The measurements weremade for 90000 or 80000 pulses, depending on the sample. The measurements were held in the ambient
temperature with nonpolarized neutron. The q range was 0.005 Å-1 < q < 0.2 Å -1. The measured data wascorrected using the results of the glassy carbon, thickness and analyzed by Irena software.

In the Fig. 1 are presented results of SANS measurementof samples sintered in four various conditions, which show

Shoulders

influence of sintering conditions on the nanoparticles sizedistribution.
For samples sintered in 950ºC, we can observe clear
shoulders, in the q < 0.016 Å-1 region. There is also
observed shoulder for sample sintered in for 5 min in 1000ºC, but it is less visible because of shifting to higher q
value and lower intensity. In case of sample sintered for 15
min in 1000 ºC there is not visible any shoulder. The
analysis of the results by Irena shows that samples sintered in950 ºC are characterized by similar volume size distribution ofFigure 1 SANS, samples sintered in fourconditionsnanoparticles with size around 230 Å. In case of the other sample, the curve shows wider distribution of ofslightly bigger nanoparticles.
The results show the main factor controlling their size is temperature. However holding time is not without
significance. The yellow curve of samples sintered for 15 min in 1000 ºC continuously rises to samll q value,
which suggests, there are bigger nanoparticles, which could not be detected in the q range.
The SANS results were confimed by TEM observation.
Shoulders

However the pictures show existence of nanoparticle withvery various size and shape. We could observe
Intensity (arb)nanoparticle smaller than 100 Å.
None the less SANS as a bulk method indicated themajority. The EDS analysis shows that nanoparticles
with size around 400 Å are manganese oxides. It is
negative phenomena, which causes depletion of matrix andcan lead to brittleness of the matieral.
SANS results of annealed samples show shoulders inq (A-1)

0.006 Å-1 < q < 0.012 Å-1 region. We can observe slight Figure 2 SANS, annealed samples
shoulder shifting to lower q value, with annealing temperature, up to 900 ºC. However it is not significant. In
case of sample sintered in 1000 ºC, we could not observe any shoulder. Possibly nanoparticles are not any more
thermally stable, which caused their growth so much we cannot observe them in the q range (Figure 2). It
express the manganese oxides are stable up to 900ºC.

50 nm

50 nm

50 nm

Figure 3 TEM, nanoparticles of samples sintered in various conditions

50 nm