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。 ）MLF Experimental Report

提出日 Date of Report

2017/08/18

課題番号 Project No. 2014A0267

装置責任者 Name of responsible person

実験課題名 Title of experiment

Stefanus Harjo, Kazuya Aizawa

In-situ investigation on microstructure

装置名 Name of Instrument/（BL No.）

rearrangements and defect kinetics in magnesium

TAKUMI / BL19

and aluminuim alloys

実施日 Date of Experiment

実験責任者名 Name of principal investigator

2014/05/11 9:00-2015/05/13 9:00

Klaus-Dieter Liss

experimental teamKlaus-Dieter Liss, Pingguang Xu,
Stefanus Harjo, Kazuya Aizawa,WuGong,
TakiroKawasaki;(samples: Eitaro Yukutake; BobHarrison)

所属 Affiliation
Australian Nuclear Science and TechnologyOrganisation

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.
Experiment ID and run numbers are listed in Table 1 and the run date in Figure 1.
exID
runNo
sample_name­­­­­­­­­­­­­­­­­­­­­­­­­­
5340
22674
S01­Mg­pure­deformed
5341
22675
S02­Al­1370
5342
22676
S03­Al­1370
5343
22677
S04­Cu­electric­deformed
5344
22678
S05­Cu­electric­Non­deformed
5345
22679
S06­Ti­Grad2­Non­deformed
5346
22680
S07­Ti­Grad2­Non­deformed
5347
22681
S08­Mg­AZ31
5348
22682
S09­Mg­AZ91
5349
22683
S10­Mg­AZX41
5350
22684
S11­Mg­Pure
5351
22685
S12­Mg­Pure
5352
22686
S13­Al­2011­deformed
5353
22687
S14­Al­3.8Cu­deformed
5354
22688
S15­Al­10Sr­deformed
535522689
S16­Zr­2.5Nb­Nondeformed
22249
Vanadium­patternFigure 1: Experiment ID displayed
along experimental time showing
effective usage of the beam time.
Table 1 (left)

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.
Goal of the experiment was to extract microstructural and crystallographic parametersfrom the recorded diffractograms. This can reflect in various parameters, namely peak
position G, shape, e.g. width DH and intensity R. Upon heating and cooling, typical lattice1strain e = -DG/G is dominated by linear thermal expansion, change of phase composition,order parameter and relaxation of residual stresses. The width DH reduces whenintergranular strains relax, e.g. during defect annihilation and upon recrystallization.
Intensity changes are related not only to phase transformations and preferred orientation
evolutions, but also to the amount of defects in a nearly perfect crystallite, as they may
occur at high temperature.
The specimens listed in Table 1 have been measured in-situ in the diffraction dilatometer
upon a heating and cooling cycle. Most of the specimens were cylindric, 12 mm high and
8 mm diameter, unless produced from sheet material. In order to introduce more defects
as starting conditions, some cylinders have been compressed by hammering on an anvil,
to typical 8-9 mm height as feasible. Deformed and un-deformed samples have been run
for comparison. The sample axis has been mounted in diagonal axis such that the
integrated detector arrays 0001 and 0000 probe for scattering vectors in longitudinal andtransverse direction according to L = 南 = SOUTH = 0001 and T = 北 = NORTH = 0000,respectively.
The provided vanadium pattern for each detector bench have been fitted by 16 th-orderpolynomials in order to smoothen the counting statistics, which then were taken tonormalize each measured time-of-flight diffraction pattern channel by channel. The
instrument was calibrated to be momentum transfer Q = 2p / (TOF/15000), where TOF isthe time-of-flight channel number in the data collection. Dilatometer data were stored inadjacent ASCII data files with ending *.CSV.

Figure 2: Representative specimen-run after normalization and calibration.
The run on Zr-2.5Nb shown in Figure 2 displays all the expected features, as thermal
expansion, huge chemical strain in b-phase, peak widening, particularly in b-phase at lowtemperature, phase transformation and reflectivity change in b-phase at high temperature.
The diffractograms have been fitted and the related microstructure evolution model has
been established to quantify these changes with various structural parameters. Similarplots have been established for all examined specimens and further analysis will focus oneach material one by one. KDL is actually taking up an academic university appointment,
and a graduate student will join this research topic for further data analysis and modelingexamination, aiming for the early academic publication.

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