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

MLF Experimental Report

2017/08/21

課題番号 Project No. 2014A0280

装置責任者 Name of responsible person

実験課題名 Title of experiment

Stefanus Harjo, Kazuya Aizawa

On the crystal perfection and defect kinetics in the

装置名 Name of Instrument/（BL No.）high temperature phases of Zr, Ti and Al alloys: An in-TAKUMI / BL19

situ study of primary extinction

実施日 Date of Experiment

実験責任者名 Name of principal investigator

2014/05/03 9:00-2015/05/08 9:00

Klaus-Dieter Liss

experimental team
Klaus-Dieter Liss, Pingguang Xu,
Stefanus Harjo, Kazuya Aizawa,Wu
Gong,
TakiroKawasaki;(samples: Eitaro Yukutake; BobHarrison)

所属 Affiliation
Australian Nuclear Science and Technology
Organisation

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_name­­­­­­­­­­­­­­­­­­­­­­­­­­5296
22262
Zr_2.5Nb
5297
22263
A2011_Sample65298
22264
Ti_Grade2_T3
5299
22265
Al1370_Sample­B
5300
22266
Ti­grade2­T1­run1
5301
22267
Ti­grade2­T4­run1
5302
22268
Ti­grade2­T2­run1
5303
22269
Ti6Al4V­run1
5304
22270
Zr­2.5Nb­sample4­run1
5305
22271
Zr­2.5Nb­sample4­run1
5306
22272
Zr­2.5Nb­sample6­run1
5307
22273
Ti­grade2­T5_run1
5308
22274
Ti­grade2­T5_run1
5309
22275
Al­1370­PartC_run1
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 obtain the defect kinetics in materials at very hightemperature, where crystallites anneal to become perfect crystals, and upon mechanicaldistortion by plastic deformation. We use the transition between the kinematic and1dynamical theory of diffraction, where primary extinction of radiation plays a role. Upon
heating, dislocations annihilate showing a decrease of intensity. Upon plastic deformation,
the intensity restores due to the introduction of strain fields. Similar distortions are formed
when a second phase precipitates. Furthermore, microstructural and crystallographic
parameters can be extracted from the recorded diffractograms, reflecting in various
parameters, namely peak position G, shape, e.g. width DH and intensity R. Upon heatingand cooling, typical lattice strain e = -DG/G is dominated by linear thermal expansion,change of phase composition, order parameter and relaxation of residual stresses.
Tensile specimens listed in Table 1 have been fabricated and measured in-situ in the loadframe upon a heating, plastic deformation and cooling process. The sample axis has been
mounted in diagonal axis such that the integrated detector arrays 0001 and 0000 probe
for scattering vectors in longitudinal and transverse 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. Load-frame processing data werestored in adjacent 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 shows the a → b phase transformation in Zr-2.5Nb
with a strong b-110 reflection appearing at 2.45 Å-1. Upon holding, it can be recognizedthat its intensity slowly decreases due to increasing crystal perfection by annihilation of
dislocations and microstructure recovery. At around 8 ks, the reflectivity suddenly
increases due to plastic deformation undertaken at this time, which introduces defects,
followed again by subsequent recovery. The remaining a- and other b-reflections do notshow this behavior because their extinction length is larger than the size of the crystallites,
therefore scattering all the time kinematically. Zr alloys demonstrate best this behavior. InTi, recovery has been found to be almost too fast to follow, and Al exposes more intensitychanges by texture, hiding this recovery effect.
KDL is actually taking up an academic university appointment, and will focus on this topic
for further data analysis and microstructure observation and modeling, aiming for the early
academic publication.

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