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

13rd February, 2018

課題番号 Project No.

装置責任者 Name of responsible person

2017B0129

Dr. Jun-ichi Suzuki

実験課題名 Title of experiment
Simultaneous investigation of nanoscale precipitates andrecovery in thermally aged Fe-Cu alloy and their comparison withmagnetic hysteresis

装置名 Name of Instrument/（BL No.）

実験責任者名 Name of principal investigator

TAIKAN (BL-15)
実施日 Date of Experiment
18th Dec.-19th Dec., 2017 (36h)Satoru Kobayashi
所属 Affiliation
Iwate University
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.
・ Samples: Iron-Copper alloy (Fe-1wt.%Cu)・ Samples were cold-rolled with rolling reduction (RR) up to 20% (0, 10, and 20%).
・ Samples with dimensions of 15 x 15 x 2 mm were aged at 480 oC. For each RR, 9 samples with different
aging time up to 10000min were prepared as listed in Table1.

Aging time (min.)SampleRollingreduction (%)

Fe-1wt%Cu0102001050

1005001000 2000 5000 10000

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Table 1: Measuring samples (Totally 27 samples)

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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.

Small angle and wide angle neutron scattering measurements were carried out at room temperature. Horizontal
magnetic field of 1 Tesla was applied with an electromagnet. We observed strong magnetic contribution forsmall-angle neutron scattering for all measured samples, which are reflected in butterfly patterns of scattering
intensity in the 2D detector. According to the equation of SANS intensity, I(Q) = I(Q)nuc+I(Q)magsin2θ, themagnetic scattering intensity, I(Q)mag was extracted from the butterfly intensity patterns. Here, θ is the angle
between the applied magnetic field and scattering vector. I(Q)nuc and I(Q)nuc+I(Q)mag were determined fromscattering intensities along and perpendicular to the magnetic field, respectively, and I(Q)mag was obtained fromtheir difference. Figure 1 shows the aging time dependence of I(Q)mag for samples with RR=0 and 20%.
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2. 実験方法及び結果（つづき） Experimental method and results (continued)
Before aging, there is no significant

101100min, magnetic contribution appears at-1

Q~0.1 A and it continuously develops withaging time up to 10000min, associated with

10I(Q)mag (cm-1)

features for both samples. After aging at20% rolling reduction

0% rolling reduction

magnetic scattering related to nanoscale
010-1

10-2

10-3

10000min

10000min

1000min
500min1000min
500min100min0min
0mina shift toward the lower Q. The observed
I(Q)mag was analyzed using a software"Irena"andvolume

weighted

(a)
0.01

size

distribution of non-magnetic Cu precipitates
was determined.

100min(b)
0.1

Q(Å-1)

0.01

0.1

Q(Å-1)

Figure 1: Aging time dependence of magnetic scattering intensity
as a function of Q for (a) RR=0 and (b) RR=20% samples.

Figure 2 shows the volume-weighted size

Volume distribution (Å-1)

0.0007

distribution f(R) for RR=0 and 20%
samples. With aging time, the intensity f(R)develops, associated with a shift of the peaktoward the higher radius. After aging time

RR=0%0.0006100min500min1040min2000min
5000min
10000min

0.00050.00040.00030.00020.00010of 1000 min, f(R) becomes broad and theVolume distribution(Å-1)

0.0007

broadening is significant for RR=20%
sample.
Figure 3 shows the aging time dependenceof volume fraction and mean size of Cu

0.00040.00030.00020.0001
0with that of hardness and the volume
fraction for RR=0% after 100 min is foundto be linearly proportional to coercivity of0.6
0.5

5060

7080

RR=0%
RR=10%
RR=20%

80

0.4
0.3
0.2
0.1

60

40

2000(b)(a)-0.1
10major magnetic hysteresis loop.
significant broadening of nuclear Bragg

40

100
RR=0%
RR=10%
RR=20%0For wide angle scattering data, the300.7

Volume fraction (%)

at 10000 min. This behavior is consistent20Figure 2: The aging time dependence of volume-weighted size
distribution for RR=0 and 20% samples.

samples, the volume fraction appears justincreases after 100 min. and attains ~ 100 A

10Radius(Å)

at 10000 min. For RR=10 and 20 %after ~ 10 min. Mean diameter also steeply

0Mean diameter (Å)

increases after 100 min. and attains ~ 0.6 %100min500min1040min2000min
5000min
10000min

0.0005precipitates for all measuring samples. For
all the samples, the volume fraction steeply

RR=20%

0.0006

102

103

Aging time (hour)104-20010102

103

104

Aging time (hour)

Figure 3: The aging time dependence of volume fraction andmean diameter of Cu precipitates.

peaks was observed before aging for the RR=20 % sample. Just after aging, the peaks become narrower and thewidth becomes almost constant after 100 min. This behavior is very similar to the aging time dependence ofcoercivity for RR=20 %. The results directly demonstrate that the decrease of coercivity just after aging for
RR=20 % is due to recovery such as rearrangement of dislocations.
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