Accepted Manuscript

Diffusionless nature of D03 L12 transition in Fe3Ga alloys

I.S. Golovin, V.V. Palacheva, A.I. Bazlov, J. Cifre, N.Nollmann, S.V. Divinski, G. Wilde
PII:

S0925-8388(15)31297-4

DOI:

10.1016/j.jallcom.2015.10.041

Reference:

JALCOM 35596

To appear in:

Journal of Alloys and Compounds

Received Date: 3 September 2015

Revised Date:

4 October 2015

Accepted Date: 5 October 2015

Please cite this article as: I.S. Golovin, V.V. Palacheva, A.I. Bazlov, J. Cifre, N.Nollmann, S.V.
Divinski, G. Wilde, Diffusionless nature of D03 L12 transition in Fe3Ga alloys, Journal of Alloys and
Compounds (2015), doi: 10.1016/j.jallcom.2015.10.041.
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Diffusionless nature of D03 L12 transition in Fe3Ga alloys

I.S. Golovin*1, V.V. Palacheva1, A.I. Bazlov1,
J. Cifre2, N.Nollmann3, S.V. Divinski3, G. Wilde3
1

National University of Science and Technology MISIS, Leninsky ave. 4, 119049 Moscow, Russia
Universitat de les Illes Balears, Ctra. De Valldemossa, km.7.5, E-07122 Palma de Mallorca, Spain
3
Institute of Materials Science, University of Mnster, Wilhelm-Klemm-Str. 10, 48149 Mnster, Germany

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Abstract

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Temperature dependent internal friction is studied in an Fe3Ga alloy using a dynamical mechanical
analyzer. Apart from several thermally activated relaxation peaks with the Arrhenius parameters
(activation energies of 1.05 and 1.85eV and a pre-factor 0 10-15s) featuring a Snoek-type and Zener
relaxation, respectively, a transient internal friction peak related to a structural transition upon heating
is found and analyzed in detail. This peak substantiates an irreversible transition from a D03 ordered
bcc to an L12 ordered fcc lattice, as further confirmed by in situ X-ray diffraction measurements. The
transient peak is unambiguously shown to feature a diffusionless phase transition.
Keywords: Fe-27Ga alloy; D03 to L12 transition; Anelasticity; Transient diffusionless effect
Introduction

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Fe-Ga alloys (Galfenols) have recently become a focus of active research due to their giant
magnetostriction, , that, in low saturation magnetic fields, approaches 400 ppm along the <100>
direction in a single crystalline state [1]. The tetragonal magnetostriction of polycrystalline Fe-Ga is
maximal for compositions with 19 and 27 at.% Ga [2,3]. Due to the giant magnetostriction, these
rare-earth-free materials are promising for applications in sensors, actuators, energy-harvesting
applications, and spintronic devices. Galfenols reveal a very small hysteresis, high tensile strength
(~ 500MPa) and their magnetomechanical properties are practically not affected by common climatic
temperatures. Nevertheless, this statement is true only if the structure of Fe-Ga alloys, i.e., a Ga
random solid solution in -Fe (the A2 phase), is stable.

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Though the high temperature A2 phase in Fe-Ga alloys can be quenched to room temperature
(RT), it remains highly metastable. Consequently, the disordered A2 phase in Fe3Ga transforms by
ordering of Ga atoms: the type of order and the resulting lattice structure depend on temperature [4].
Ordering decreases the mobility of magnetic domain walls and leads to a low ductility and the
reduction of both, magnetization and damping capacity [5] of Fe-Ga alloys.
The formation of the equilibrium fcc-based L12 ordered phase, according to the equilibrium
Fe-Ga diagram, is rather slow, and in most cases a metastable phase diagram with two body-centered
cubic-based ordered phases, B2 and D03, describes the structure of directly solidified Fe-Ga alloys
most appropriately (for details see [6]). The formation of the equilibrium L12 phase occurs if the
directly solidified samples are heated above 300C in dependence on the heating rate and/or annealing
time.
Systematic studies of the ordering kinetics and types of ordered phases in quenched Fe-Ga
alloys under different annealing conditions have been reported for a few cases [6-9].
*

email: i.golovin@misis.ru

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The D03 to L12 transition cannot occur only by an atomic exchange between the sites; however,
a diffusionless displacive bccfcc reconstruction was proposed [10,11]: the atomic order inherited
from the D03 phase corresponds to a transformed tetragonal (D022 structure) lattice and the
corresponding Bain strain transforms the bcc lattice further into a fct lattice bringing Fe and Ga atoms
to their new positions in an fcc-based lattice without an atomic interchange between these sites. The
Bain orientation relations between the parent bcc-based D03 and fct D022 phases are: [001]D03
[110]D022 , (100)D03 (110)D022, and (010)D03 (110)D022. The orientation relations produce a
tetragonal elastic extension (c) along aD03/2 aD022/22 and an elastic contraction (a) along two
perpendicular axes. Finally, the orientation relations for the diffusionless D03 L12 transition can be
written as [10]:
a D 03
a D 03
(1)
aL12 =
aL12 =
(1 + c )
and
(1 + a ) ,
2
2
with the corresponding values of the elastic deformation being estimated to be c0.265 and a0.105.

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Most recently, a similar scheme of transition was confirmed using a TEM study of a Fe-27Ga
alloy [12]. The D03 nanoclusters were reported to undergo a phase transformation to an intermediate
tetragonal phase (L10-like martensite) via Bain distortion, and finally the L12 structureformed.

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The internal friction, or mechanical spectroscopy, method is exceptionally sensitive to different

anelastic transitions in metals and alloys [13]. Thus, both reversible thermally activated and
irreversible structure-induced anelasticity can be analyzed with respect to the atomic structure of
alloys. In our previous papers, we emphasized reversible thermally activated effects, such as
Snoek-type and Zener relaxations. In this paper, we focus on the kinetics and the features of the
irreversible D03L12 transition during heating.
Materials and methods

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Several Fe-Ga alloys with Ga amounts between 27.2 and 27.6%1 were produced by directional
solidification using pure Fe and Ga by induction melting under the protection of high-purity inert
argon gas using an Indutherm MC20V mini furnace. The studied compositions belong to a
single-phase (L12) structure according to the equilibrium phase diagram. Using energy dispersive
spectroscopy, the chemical compositions of the cast buttons were measured with an accuracy within
0.2%. Most of the samples were annealed at 1000C for 40min, then water quenched (wq) and
annealed at different temperatures (wq+an). In addition, we studied several samples after directional
solidification (ds). The water quenched samples will be designated as wq-XXX, where XXX is the
temperature (in C) from which the samples were quenched.
X-ray scans were performed using copper K radiation (1.54056 ). For room temperature
(RT) measurements, rotated samples were investigated with a Bruker AXS D8 ADVANCE
diffractometer at a step size of 0.04 with an exposure time of 2s for the 2-scans in the range of 20
to 120. The X-ray scans at elevated temperatures (Siemens D5000 diffractometer) were operated
under vacuum (~110-5mbar) conditions without rotation using a step size of 0.02 and an exposure
time of 1 to 3s. Isothermal measurements were done with an exposure time of 1s. The samples were
mounted on a tantalum ribbon for direct heating. During the scan, the temperature was measured in
the middle of the sample with a directly attached thermocouple.

In this paper we use atomic %

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Thermal analysis was done using a Labsys Setaram system with heating rates from 10 to
40 K/min. The magnetic hysteresis loop was measured at RT using a vibrating sample magnetometer
(Foner magnetometer Oxford).

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Simultaneous testing of anelastic (internal friction, Q-1) and elastic (Youngs modulus, E)
properties were carried out using forced bending vibrations on a dynamical mechanical analyzer
(Q800 TA Instruments). The internal friction was measured as tan (=Q-1), where is the phase lag
between the applied cyclic stress, , and the resulting strain, , = 0cos(t) and = 0cos(t+);
= 2f.
Results and discussion

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Temperature dependent internal friction (TDIF). Figures 1a-c represent an overview of

TDIF tests of the Fe-27Ga alloys after different heat treatments. Figures 1d-f show the corresponding
XRD data and substantiate that the structures of the wq-650, wq-750, and wq-1000 samples
correspond to a mixture of D019 (dominating phase a = 2.607 and c = 4.234) and A2/D03, single B2,
and a mixture of A2 (lattice parameter 2.922) and D03 (2.905) phases, respectively.

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There are several thermally activated peaks on the TDIF curves denoted as P1, P2, and P3.
Their characteristic temperatures depend on the measuring frequency of the forced vibrations. The
T-f dependence in an Arrhenius plot (Fig.2a) provides the activation parameters of these peaks. In
contrast, the PTr peak temperature, which is accompanied with an increase of the Youngs modulus,
does not depend on the frequency, while its height is strongly affected by the measurment frequency
and the heating rate. The P1, P2 and PTr peaks were not recorded after water quenching from 650C
that resulted in a microstructure with D019 as the dominating phase (Fig.1a).
Thermally activated relaxation P1, P2, and P3 peaks

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The P1 peak (Fig. 1b,c) represents a broad relaxation effect. Taking into account the activation
parameters of wq-750 and wq-1000 samples, the mean values of the activation energy (H) vary from
1.03 to 1.09 eV, and the inverse frequency factor (0) was found within the range 10-15 to 10-14 s
(Table 1). This peak can be interpreted as a Snoek-type relaxation [14]. The Snoek-type relaxation
occurs due to stress-induced jumps of interstitial atoms (C) in a random A2 bcc solid solution or
bcc-based D03 ordered lattice of Fe-Ga alloys [15-17]. This effect was studied earlier for Fe-Al-based
[18] and Fe-Ge [19] alloys. Similarly, C and Ga atoms do not have a pronounced chemical interaction
in iron, though larger Ga atoms generate compressive strains in the lattice and increase the lattice
parameter of iron. The elastic interaction of Ga with C atoms is stronger, which increases the
activation energy for C-atom jumps with respect to -Fe by approximately 0.2 eV [20], see Table 1.
After quenching from 650C (Fig.1a), i.e., from the hexagonal D019 range of the phase diagram, or
after first heating of a wq-1000 sample to 600C (its structure corresponds to the L12 phase), the P1
peak was not recorded. This fact fully agrees with the main statement of the Snoek theory, which is
applicable for the bcc lattices only and consequently, the Snoek-type relaxation was not found neither
in the samples with the hexagonal D019 (Fig. 1) nor with the fcc-based L12 (Table 1) structures.
The P2 peak (Fig. 1b,c) exhibits the following mean values of the activation parameters: H is
equal to 1.861.89 eV and 010-16 s. The short relaxation time corresponds to point defects, while the
activation energy suggests contributions of substitutional atoms (Ga). The P2 peak disappears after
annealing, which leads to ordering. Such behavior, as well as the activation parameters, may suggest

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a Zener mechanism [21] for the P2 relaxation. The ordering decreases the peak height, which agrees
with the theory and the existing results for the Fe-26Al alloy [22].

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The P3 peak is observed at the high temperature excess (end) of the TDIF curves measured at
low frequencies during both heating and cooling. The peak overlaps with a rapidly growing high
temperature (above 500C) background, which adds difficulties in treating the peak properly.
Calculations of the activation parameters for this peak are hindered by the high-temperature
background. In Table 1 we only note that this peak exists.
Transition induced anelasticity

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The PTr peak appears only in the samples that were water quenched from the A2 (random bcc)
or B2 (ordered bcc) lattices (Fig. 1b,c), but not in the samples water quenched from the D019 phase
(Fig.1a). The PTr peak is accompanied by a Youngs modulus increase. This effect is also recorded in
the ds samples [23]: according to XRD, a high cooling rate leads to retaining the A2 structure at RT.
The peak temperature does not depend on the measuring frequency, while the peak height is roughly
proportional to the inverse frequency of the vibrations and the heating rate (Fig.2b). The peak position
depends on the heating rate: it is 458, 479 and 512C for the heating rates of 0.5, 1, and 2K/min,
respectively. The activation energy of the corresponding structure transformation estimated by the
Kissinger method is 1.14 eV (the same analysis of the DSC data provides an activation energy of
about 1.81eV for the corresponding exothermic effect for heating rates of 10-40 K/min and the
corresponding peak temperatures between 546 and 587C). If heating is interrupted for 30min at a
temperature of 470C, which is the peak maximum, the peak is annealed out during subsequent
heating (Fig. 4b).

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If a cyclic stress is applied, =0cos(t), the internal friction (IF or Q-1) is [24]:
1
Q 1 =
d an
J 02

(2)

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where J is the elastic compliance, 0 is the oscillation amplitude, (=2f) is the angular frequency
and an is the anelastic part of the deformation during one cycle of vibrations. The anelastic
deformation in Eq.(2) for a shear (martensitic) deformation is proportional to the transformed volume
fraction and arises from the lattice deformation:
dan = k (n/t) dt,

(3)

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where n/t is the transformation rate, and n is the amount of the transformed material. In case of
constant heating or cooling with a fixed rate, n/t=n/T T/t. The transient damping due to shear
1
transformations, Q Tr
, is determined by the transformation rate n/t, where n is the amount of

& effect [24].

transformed material [25]. This internal friction peak is also known as T
For an athermal transition, Delorme and Gobin [26] suggested that the transformation
deformation, d=kdn, should linearly depend on the transformed volume fraction and on the applied
stress , leading to
k dn T&
1
Q Tr
=
,
(4)
J dT
where k is an empirical coefficient.
The corresponding plots are given in Fig.2b and substantial deviations from linearity are
obvious. More recent developments of this model have been discussed by San Juan and Prez-Sez

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[24] and practically all the discussed models accept a QTr1

T&

dependence. Fig. 2c presents the

log-log plots of the QTr1 / T& vs. 1/f (since ~ f) dependencies, which give a rough estimate of m0.4.

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A slight tendency towards an increase of m for a higher heating rate is seen. This effect could be
explained by an increasing difficulty of successive shear transformations during the transition that is
naturally more pronounced for slow heating rates.

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A study of the PTr effect using DSC tests (Fig.3a), a RT (Fig.3b) and in situ (Fig.3c,d) X-ray
diffraction, the microstructure examination by scanning electron microscopy and an increase in the
hardness (from 3113HV in the water quenched state to 3555HV after two hours annealing at
475C) suggest a pronounced D03L12 transition (lattice parameter for L12 phase at RT is 3.573)
in the temperature range of the PTr peak. The DSC curves (Fig. 3a) for wq-750 and wq-1000C samples
confirm the D03L12 transformation just above 500C (effect is denoted as I) in contrast with the
sample wq-650 with a dominating D019 phase. The effect II (as denoted on the curves) corresponds to
the L12D019 transition, and effect III is due to the D019B2 transition. The XRD tests at RT after
10min annealing at 350, 450 and 475C indicate the presence of 5%, 12% and 90% of L12 phase in
the sample, respectively (insert in Fig.3b). The in situ XRD tests at different temperatures (Fig.3c)
also illustrate this transition above 425C. Some difference in the transition temperatures is due to
longer times required for the XRD tests as compared to instant heating in DMA and DSC tests and the
fact that the heat flow is proportional to the transformation rate, whereas the XRD signal reveals the
amount of the transformed phase.

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Thus, structural studies vividly prove that the PTr effect is caused by the D03L12
transformation and n in Eq.(3) is the amount of the L12 phase in the sample. Since the parameters of
T&
the PTr effect follow a well-known dependence for a shear transition [24], QTr1 m , we substantiate

that the D03L12 transition in Fe-Ga alloys reveals typical features of a shear transition supporting
Khachaturyans viewpoint [10].

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Applying different methods, we have performed several isothermal tests in the range of the
D03L12 transition. The XRD data in Fig. 4a demonstrate that the fcc L12 phase grows at the
expense of the quenched bcc (A2+D03) phases (lattice parameters for co-existing phases at 390C are
2.92 (A2), 2.91 (D03) and 3,70 for L12). Splitting of the (110) XRD peak at 2 = 44 illustrates
the presence of A2+D03 phases before and during the transformation. Fig. 4b (symbols) shows the
determined kinetics of the transformation as revealed by IF and XRD tests.
The kinetics of the isothermal shear transformation is typically described within Pati and Cohen's
approach [27], which after Thadhani and Meyers [28] could be simplified to 1 n / nmax = exp( Bt ) ,
where n (nmax) is the (maximal) volume fraction of the transformed phase and B is a constant
depending on the nucleation rate and the nucleation energy [28]. However, the present data, both IF at
470C and XRD at 390C, are not perfectly described by this approach - red lines in Fig.3cb. A better
description of the isothermal transformation is provided by an Avrami-like [29] expression,

1 n / nmax = exp Bt k , blue lines in Fig.3c, where the power k is about 1.6 and 2.5 for IF and XRD
tests, respectively. Hereto we assume that IF, Q-1 is a measure of the elastic distortions in the course
of a phase transition (Eq.2), which in turn are proportional to the fraction of the transformed volume n
(d=kdn). At higher temperatures of isothermal IF measurements, both fits have a similar quality,

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while the stretched exponent appears to be more suitable to describe the XRD measurements
performed at a lower temperature where kinetics is more sluggish. The reasons for such behavior
requires a detailed study, which is out of the scope of the current paper. Here we note that the
isothermal kinetics agrees generally with the temperature-dependent IF data, Fig.2, which
substantiate a general power dependence of the mechanical loss in both isochronal and isothermal
tests.

Conclusions

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Using a combination of XRD, SEM, TEM, and DSC studies and internal friction analyses, we
showed that a transient internal friction PTr peak accompanies the D03 to L12 phase transition during
heating. This peak reveals all typical features of a shear deformation, which is crucial for
understanding the character of the D03 to L12 transition. Additionally, some contribution of diffusive
jumps can be substantiated from isothermal data.

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A thermally activated broad internal friction P1 peak recorded in most of the Fe-Ga alloys is
caused by a Snoek-type relaxation. The P2 peak is probably due to a Zener relaxation, i.e.,
reorientation of the Ga-Ga atom pairs under an applied cyclic stress.
Acknowledgements

References

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This study is supported by RFBR project No. 14-03-00165a, Russia. I.S.G. gratefully
acknowledges DAAD grant No.: 91573930. N.N., S.D. and G.W. acknowledge a partial support from
the Deutsche Forschungsgemeinschaft (DFG, Germany) via a research grant. We thank Ms E.
Savchenko for the vibrating sample magnetometry tests.

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[1] A.E. Clark, K.B. Hathaway, M. Wun-Fogle, J.B. Restorff, T.A. Lograsso, V.M. Keppens,
G. Petculescu, R.A. Taylor. J.Appl.Phys.93 (2003) 8621-8623.
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[7] N. Srisukhumbowornchai, S. Guruswamya. J.Appl.Physics. 92 (2002) 5371-5379
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[9] Himalay Basumatary, Mithun Palit, J. Arout Chelvane, S. Pandian. MSE(B) 167 (2010) 210213
[10] A.G. Khachaturyan, D.D. Viehland. MetMatTrans A38 (2007) 2308-2316 and 2317-2328.
[11] J. Boisse, H. Zapolsky, A.G. Khachaturyan. Acta Materialia 59 (2011) 26562668.
[12] Yin-Chih Lina, Chien-Feng Lin. J.Appl.Phys. 117, 17A920 (2015)
[13] M.S. Blanter, I.S. Golovin, H. Neuhauser, H.-R. Sinning, Internal friction in metallic materials.
A Handbook. Berlin, Springer Verlag, 2007.
[14] Snoek JL. Physica VIII 1941;7:711.
[15] I.S. Golovin, A. Rivire. Intermetallics, 19 (2011) 453-459

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[16] I.S. Golovin, J. Cifre. JALCOM, 584 (2014) 322-326

[17] I.S. Golovin, V.V. Palacheva, A.I. Bazlov, J. Cifre, J. Pons. JALCOM, 644 (2015) pp. 959-967
[18] I.S. Golovin. MSE(A), 442/1-2 (2006) 92-98.
[19] I.S. Golovin, H. Neuhuser, H.-R. Sinning, C. Siemers. Intermetallics 18 (2010) 913921
[20] I.S. Golovin, S.B. Golovina. The Physics of Metals and Metallography, 102 (2006) n.6, 593603
[21] C. Zener, Elasticity and Anelasticity of Metals. The Univ. of Chicago Press, 1948.
[22] I.S. Golovin, A. Rivire. Intermetallics, 14 (2006) 570-577.
[23] I.S. Golovin. Materials and Design, 88 (2015) 577-587
[24] J. San Juan and R.P. Perez-Saez. Transitory effects in Schaller R., Fantozzi G., Gremaud G.
(Eds.) Mechanical Spectroscopy Q-1 2001 with Applications to Materials Science. Trans Tech
Publications, Switzerland. 2001, 416-437.
[25] E. Scheil, J. Mller. Arch Eisenhutt (1956) 27:801805
[26] J.F. Delorme, P.F. Gobin. Metaux-Corrosion-Ind (1973) 573:185222
[27] S.R. Pati, M. Cohen, Acta Metall. 17 (1969) 189.
[28] N.N. Thadhani, M.A. Meyers, Acta Metall. 34 (1986) 1625.
[29] J.W. Martin, R.D. Doherty, B. Cantor. Stability of microstructure in metallic systems,
Cambridge University Press, Cambridge, 1997.

Figure captions:

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Fig. 1. Typical TDIF curves with a heating rate of 1 K/min of the Fe-27Ga alloy: a water quenched
after annealing for 5 hrs at 650C, b water quenched after annealing for 5 hrs at 750C, and c water
quenched after annealing for 40min at 1000C. Different colors correspond to different frequencies
from 0.1 to 30 Hz. Symbols P1, P2, P3, and PTr are used to note internal friction peaks. Fig. d-e-f show
the corresponding XRD spectra.
Fig. 2. Fe-27Ga: (a) Arrhenius plots for the P1 and P2 peaks that are presented in Fig. 1b,c; (b) The
height of the PTr peak as a function of the inverse frequency for three different heating rates; (c) The
log-log plots of the height of the PTr peak as function of the inverse frequency.

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Fig. 3. Fe-27Ga alloy: (a) DSC curves for water quenched samples with different heating rates I
formation of L12, II of D019 and III B2 phases; (b) XRD spectra after annealing a water quenched
sample for 10 min at 350, 450 and 475C (inset: per cent of L12 phase vs temperature); (c) in situ
XRD spectra showing the growth of L12, D019 and B2 phases recorded at selected temperatures.
Fig. 4. Isothermal (in situ) measurements: (a) XRD data measured at 390C for 41.5 2 44.5 as
a function of time; (b) analysis of the isothermal transformation kinetics in IF at 470C (squares) and
XRD tests at 390C (circles). Red and blue lines represent the fit of the data after different models, see
text.

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Table 1. Heat treatment, dominating phase, hardness, coercive force, and internal friction peak
parameters for Fe-27Ga alloy after different heat treatments (Fig. 1). The existence of peaks P3 and
PTr is indicated (
), since the activation parameters were not possible to evaluate.

HV

HC
k/m

wq-650

D019

38711

3.2

wq-750

B2

3537

2.8

1.090.007

210-15

wq-1000

A2

3113

2.9

1.030.020

210-14

wq-1000+an-600

L12

3614

H
eV

P2
0
s

PTr

1.860.07

310-16

1.890.11

910-17

P1 and P2 peaks are not recorded

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P3
0
s

P1 and P2 peaks are not recorded

* according to the XRD data at room temperature

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eV

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Sample

P1

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Fe-27Ga
Dominating
phase*

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The A2 to D03 transition in quenched Fe-27Ga is proved by in situ XRD
The L12 phase formation is accompanied by a transient internal friction peak

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This peak reveals all typical features of a shear deformation