Jou nal o Non-C ys alline Solids 609 (2023) 122267
A ailable online 14 Ma ch 2023
0022-3093/© 2023 The Au ho (s). Published by Else ie B.V. This is an open access a icle unde he CC BY-NC-ND license (h p://c ea i ecommons.o g/licenses/by-
nc-nd/4.0/).
E ec o he mal ea men s below de i i ica ion empe a u e on he
magne ic and magne ocalo ic p ope ies in mechanically alloyed
Fe
70
Z
30
powde s
A.F. Manch´
on-Go d´
on
a
,
*
, J.S. Bl´
azquez
b
, M. Kowalczyk
c
, J.J. Ipus
b
, T. Kulik
c
, C.F. Conde
b
a
Ins i u o de Ciencia de Ma e iales de Se illa, ICMSE CSIC-Uni e sidad de Se illa, C. Am´
e ico Vespucio 49, Se illa 41092, Spain
b
Dp o. Física de la Ma e ia Condensada, ICMSE-CSIC, Uni e sidad de Se illa, P.O. Box 1065, 41080 Se illa, Spain
c
Facul y o Ma e ials Science and Enginee ing, Wa saw Uni e si y o Technology, 141 Wołoska s ., 02-507 Wa saw, Poland
ARTICLE INFO
Keywo ds:
Amo phous s uc u e
Relaxa ion phenomena
M¨
ossbaue spec oscopy
Magne ic inhomogenei y
Magne ocalo ic p ope ies
ABSTRACT
In his wo k, he elaxa ion o he amo phous s uc u e o mechanically alloyed Fe
70
Z
30
powde s has been
analyzed h ough in e up ed hea ing amps below he de i i ica ion empe a u e. As a esul o such he mal
ea men , Cu ie empe a u e and empe a u e a maximum magne ic en opy change cu es shi o highe
empe a u es as he empe a u e o hea ing ea men inc eases. This e ec can be a ibu ed o bo h he elease
o he s ess accumula ed in he amo phous powde du ing he milling p ocess and o he ini ia ion o nuclea ion
o
α
-Fe c ys alli es, as i has been shown by M¨
ossbaue spec oscopy.
1. In oduc ion
Magne ic p ope ies o Fe- ich amo phous alloys ha e ecei ed sig-
ni ican a en ion in he esea ch communi y om bo h undamen al
and echnological pe spec i es [1,2]. These ma e ials p esen a ypical
magne ic phenomena, such as magne oelas ic beha io [3] o double
ansi ion beha io [4], depending on Fe con en [5] and he local
a omic o de [6]. Mo eo e , hese sys ems can be also conside ed as a
p ecu so o he de elopmen o di e en in e me allics [7]. Fu he -
mo e, hese amo phous so e omagne ic alloys ha e ecei ed
conside able a en ion in he esea ch communi y ocused on magne-
ocalo ic e ec , MCE, and magne ic e ige a ion a empe a u es close
o oom empe a u e [8]. So magne ic amo phous alloys can be clas-
si ied as magne ocalo ic ma e ials wi h a second o de magne ic an-
si ion (SOPT). Al hough he MCE exhibi ed by hese sys ems is no eally
in compe i ion wi h Gd (pa adigma ic ma e ial o magne ic e ige a-
ion a oom empe a u e [9]) o sys ems wi h a i s o de magne ic
ansi ion, such as Ni-based Heusle alloys [10], hey exhibi a eally
educed magne ic hys e esis and an easily unable Cu ie empe a u e
wi h small composi ional changes [11,12]. Fu he mo e, he ield
dependence o MCE o hese sys ems is well es ablished [13].
Al hough amo phous alloys a e ypically p oduced by apid
quenching echniques, he exis ence o wo eu ec ic poin s in he Fe-Z
phase diag am [14,15] es ic s he capabili y o his echnique o
p oduce amo phous alloys o speci ic composi ions, close o Fe
25
Z
75
and Fe
90
Z
10
. Thus, o he echniques ha e been p oposed o p epa e
amo phous Fe-Z compounds in a b oade ange o composi ions, such
as mechanical alloying o spu e ing echniques, which expand he
p oduc ion o amo phous samples o a Fe con en o 30–80 a .% [16]
and 20–90 a .% [17], espec i ely.
The mechanical alloying echnique has been employed o p oduce
many amo phous alloys [18] and, gene ally, leads o s ongly diso de ed
sys ems. Consequen ly, he milled amo phous samples a e in a me a-
s able s a e, which can induce di e en ans o ma ions du ing he mal
ea men s, e en a empe a u es lowe han hose co esponding o he
de i i ica ion p ocess. Al hough some wo ks pay a en ion o he
Fe
70
Z
30
a .% amo phous alloy [5,19-21] and i s de i i ica ion p ocess
[7], including some p e ious wo ks o he au ho s [22–24], he s udy o
he e ec o he elaxa ion phenomena on he magne ic beha io o his
alloy has no ye been pe o med.
The pu pose o his s udy is o analyze he e ec o he elaxa ion
phenomena o amo phous Fe
70
Z
30
powde s p epa ed by mechanical
alloying on hei magne ic beha io . The e o e, o shed some ligh on
he me as able cha ac e o hese samples, he p esen wo k is de o ed o
analyze he he mal dependence o he magne ic p ope ies o he alloy
submi ed o di e en he mal ea men s a empe a u es below he
de i i ica ion empe a u e.
The esul s ob ained in his s udy a e complemen a y o ea lie wo ks
* The co esponding au ho .
E-mail add ess: [email p o ec ed] (A.F. Manch´
on-Go d´
on).
Con en s lis s a ailable a ScienceDi ec
Jou nal o Non-C ys alline Solids
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h ps://doi.o g/10.1016/j.jnonc ysol.2023.122267
Recei ed 23 Janua y 2023; Recei ed in e ised o m 2 Ma ch 2023; Accep ed 6 Ma ch 2023
Jou nal o Non-C ys alline Solids 609 (2023) 122267
2
o he au ho s on he Fe-Z amo phous alloys p epa ed by mechanical
alloying in which se e al aspec s ha e been in es iga ed: i) he e olu-
ion o Fe en i onmen s and he phase composi ion du ing mechanical
amo phiza ion p ocess [25]; ii) he kine ics o he mechanical amo ph-
iza ion [26]; iii) he in luence o milling ime on he magne ic p ope ies
[27]; and i ) he he mal s abili y and he kine ics o c ys alliza ion [7].
2. Expe imen al
Amo phous alloy wi h Fe
70
Z
30
a .% composi ion was syn hesized by
mechanical alloying. De ails on p epa a ion and a de ailed analysis o
he mic os uc u e o he syn hesized powde s can be ound in e . [25].
A e 50 h o milling, mechanical alloying esul s in he alloy wi h
amo phous s uc u e. To explo e he e ec o hea ing on he amo phous
s uc u e, powde samples we e hea ed, a 10 K/min up o di e en
maximum empe a u es in a di e en ial he mal analysis (DTA)
Pe kin-Elme DTA7 uni unde A low. Th ee di e en maximum em-
pe a u es we e eached in he expe imen s pe o med: 473, 573 and
673 K. Subsequen ly, he samples we e cooled down o oom empe a-
u e inside he o en.
Two echniques con i med he amo phous cha ac e o he powde :
X- ay di ac ion using Cu-K
α
adia ion in a Rigaku MiniFlex di ac-
ome e and DTA. T ansmission M¨
ossbaue spec a we e measu ed using
a
57
Co(Rh) sou ce a oom empe a u e and i ed wi h NORMOS p o-
g am [28]. Isome shi has been gi en ela i e o an
α
-Fe oil a oom
empe a u e. Samples o M¨
ossbaue spec oscopy we e p epa ed by
sp eading powde on a Fe- ee adhesi e ape in such a way ha he
hickness o he sample is o he o de o ha o he Fe hin oil s anda d
used o calib a ion. The e o e, hin abso be app oxima ion was used
o he i ing o he spec a.
Tempe a u e and magne ic ield dependen magne iza ion we e ob-
ained using he ib a ing sample magne ome e s anda d op ion o a
Physical P ope ies Measu emen s Sys em (PPMS, Quan um Design)
be ween 100 and 400 K in he applied ield ange o ±1.5 T. Loose
powde was packed in he VSM powde Sample Holde s. E ec o
demagne izing ac o has no been conside ed in his s udy.
3. Resul s and discussion
Fig. 1 depic s he XRD pa e ns aken a oom empe a u e om
powde s hea ing up o he indica ed empe a u es below he de i i i-
ca ion empe a u e, as obse ed in he inse . This inse shows he DTA
scans o he as-milled powde a 10 K/min, whe e an onse empe a u e
∼920 K can be obse ed. The wo peaks de ec ed co espond o he
o ma ion o he Fe
2
Z and Fe
23
Z
6
in e me allics [7]. Despi e o he
hea ing ea men , he amo phous s uc u e is e ained, as can be
in e ed by he exis ence o a b oad halo a 2θ∼43◦in all he s udied
condi ions. In he case o 573 and 673 K annealing empe a u es, a small
di ac ion peak begins o de elop loca ed a a ound 2θ∼45◦, associa ed
wi h he (110) maximum di ac ion peak o he
α
-Fe phase. Al hough
he XRD pa e n o he as-milled and 473 K annealing empe a u e do
no exhibi he p esence o
α
-Fe c ys alli es in he sample, i has been
shown he exis ence o esidual
α
-Fe nanoc ys als by M¨
ossbaue spec-
oscopy a low empe a u es in he as-milled powde s (∼3% phase
con ibu ion) [27]. The e omagne ic cha ac e o he amo phous ma-
ix a empe a u es below oom empe a u e allows o a e omagne ic
coupling be ween he esidual
α
-Fe c ys alli es and he isible
Fig. 1. XRD pa e ns a oom empe a u e o Fe
70
Z
30
as-milled amo phous
alloy and a e hea ing up o he ma ked empe a u es. Inse shows DTA cu es
o he de i i ica ion o he as-milled amo phous alloy unde a cons an hea ing
a e o 10 K/min. Cha ac e is ic empe a u es, onse , Tonse , and peak empe -
a u es, Tpk, ha e been indica ed.
Fig. 2. M¨
ossbaue spec a a oom empe a u e o amo phous samples a e
hea ed up o he ma ked empe a u es.
A.F. Manch´
on-Go d´
on e al.
Jou nal o Non-C ys alline Solids 609 (2023) 122267
3
con ibu ion by M¨
ossbaue spec oscopy. The e o e, he appea ance o
he (110) maximum di ac ion peak in he case o 573 and 673 K
annealing empe a u e co espond o an inc ease o he c ys al size o
hose emaining c ys alli es in he amo phous ma ix.
Fig. 2 p esen s M¨
ossbaue spec a aken a oom empe a u e o he
alloy powde s hea ed up o he ma ked empe a u es. As he annealing
empe a u e inc eased, an inc ease o he peaks a ound ±4 and ±6 mm/
s can be obse ed, indica ing he de elopmen o a magne ically-o de ed
phase a oom empe a u e. Consequen ly, wo componen s ha e been
employed o i he spec a, a quad upola dis ibu ion and a e o-
magne ic sex e . While he i s pa amagne ic con ibu ion can be
asc ibed o he amo phous phase, he e omagne ic si e can be associ-
a ed wi h he o ma ion o he
α
-Fe phase, cha ac e ized by a hype ine
ield o abou 33 T. The quad upole spli ing dis ibu ions, P(QS),a e
displayed in Fig. 3, which exhibi he same beha io o all he samples,
wi h a non-ze o p obabili y o QS=0 mm/s. The ob ained hype ine
pa ame e s om he spec a i ing ha e been collec ed in Table 1. The
mean alue o quad upole spli ing, 〈QS〉,is close o he alues p e i-
ously epo ed o as-milled Fe
70
Z
30
alloy 〈QS〉=0.53±0.07 mm/s [25].
Despi e he de elopmen o he
α
-Fe phase and he co esponding Fe
impo e ishmen o he amo phous alloy, no signi ican e ec s on he
quad upola dis ibu ion ha e been de ec ed.
F om hese i s, an e iden inc ease o he e omagne ic con ibu ion
wi h he inc ease o he empe a u e o ea men can be obse ed,
eaching a alue o 12% o he o al Fe a oms in
α
-Fe si es o he case o
he annealed powde a 673 K (assuming pu e
α
-Fe, his yields 8.5
a omic ac ions o he c ys alline phase). E en hough he
α
-Fe phase
was no de ec ed by XRD, he exis ence o his phase is e iden by he
M¨
ossbaue spec a o he analyzed powde s. The o ma ion o he
α
-Fe
phase a empe a u es lowe o he c ys alliza ion empe a u e o he
amo phous alloy is due o he exis ence o esidual
α
-Fe c ys als a e he
amo phiza ion p ocess. Al hough hese nanoc ys als can no be de ec ed
by XRD echnique a oom empe a u e, hei exis ence is clea ly
con i med when he samples a e analyzed by M¨
ossbaue spec oscopy a
empe a u es below oom empe a u e. In ac , a oom empe a u e, he
pa amagne ic cha ac e o he amo phous ma ix p e en s he coupling
o he dissemina ed
α
-Fe nanoc ys als. Mo eo e , i is well known ha
M¨
ossbaue spec oscopy is a mo e p ecise echnique han XRD o iden-
i y Fe- ich phases [25], pa icula ly in such cases as he one analyzed
he e, whe e he amo phous halo can jeopa dize he p esence o iny bu
b oad c ys alline maximum. On he o he hand, an inc ease o he hy-
pe ine ield o he sex e assigned o he
α
-Fe phase ha e been also
de e mined. This e olu ion can be associa ed wi h he dec ease o Z
a oms in he neighbo hood o he
α
-Fe phase. I has been shown ha he
hype ine ield o Fe is s ongly a ec ed by he p esence o o he a oms
as a nea neighbo s (e.g. ΔB
h
~−3 T o a non-magne ic a om in he wo
i s shells [29]).
Fig. 4a illus a es he magne iza ion dependence on he empe a u e
o he s udied powde s when an ex e nal magne ic ield o 100 Oe is
applied. On cooling, he he momagne ic cu es a e cha ac e ized by a
sudden inc ease o he magne iza ion a ound 240 K, co esponding o
he pa amagne ic o e omagne ic phase ansi ion o he amo phous
phase. I indica es he pa amagne ic beha io o he amo phous powde
a oom empe a u e, in ag eemen wi h he M¨
ossbaue spec oscopy
Fig. 3. P obabili y dis ibu ion o quad upole spli ing o he s udied powde s.
Table 1
Hype ine pa ame e s o he s udied he mally ea ed amo phous samples. A ea
(%) is he ela i e con ibu ion o he componen , and B
h
and δ a e he alues o
he hype ine magne ic ield and he isome shi o he e omagne ic si e,
espec i ely. <Qs>is he mean alue o he quad upola shi .
Annealing
empe a u e
(K)
Componen A ea
(%)
B
h
±0.1
(T)
δ±0.02
(mm/s)
<Qs>±0.05
(mm/s)
473 Quad upola
dis ibu ion
94 – −0.15 0.49
α
-Fe si e 6 31.6 0.06 –
573 Quad upola
dis ibu ion
90 – −0.14 0.47
α
-Fe si e 10 32.5 0.04 –
673 Quad upola
dis ibu ion
88 – −0.14 0.52
α
-Fe si e 12 32.6 0.02 –
Fig. 4. a) Tempe a u e dependence o he speci ic magne iza ion o Fe
70
Z
30
as-
milled amo phous alloys and a e hea ing up o he ma ked empe a u es
unde an applied magne ic ield o 100 Oe. b) Co esponding dM/dT cu es.
Inse shows he e olu ion o he Cu ie empe a u e ob ained as he minima o
dM/dT cu es. The co esponding da a o he as-milled sample has been
included o compa ison.
A.F. Manch´
on-Go d´
on e al.
Jou nal o Non-C ys alline Solids 609 (2023) 122267
4
esul s. I has been shown ha a signi ican change in he magne iza ion
o as-milled powde s occu s only when he powde s a e hea ed up abo e
800 K [7,30]. No mo e ansi ions ha e been obse ed in he ange o
empe a u e and magne ic ields applied o he powde s. Howe e ,
signi ican a ia ions in he magne iza ion can be obse ed wi h he
inc ease in he empe a u e o he he mal ea men s. In his sense,
magne iza ion does no all o ze o in none o he cases analyzed due o
he exis ence o a ce ain
α
-Fe phase con ibu ion, which has a much
highe Cu ie empe a u e han hose o he amo phous one (speci ic
magne iza ion a 400 K inc eases om 4 o 13 kA/m as annealing
empe a u e inc eases om 473 o 573 K in ag eemen wi h he inc ease
obse ed in he e omagne ic a ea om M¨
ossbaue spec oscopy). As
he annealing empe a u e inc eases, he d op o he magne iza ion a
he Cu ie empe a u e dec eases because o he g ow h o he
α
-Fe
ac ion, i.e. he di e ence be ween he magne iza ion be o e and a e
he Cu ie ansi ion o he amo phous phase is educed wi h he he mal
ea men , in ag eemen wi h he e olu ion o he M¨
ossbaue i s.
Acco dingly, he magne iza ion a low empe a u es dec eases due o
he Fe deple ion o he amo phous phase as he annealing empe a u e
inc eases.
The applied ield o 100 Oe ( o measu e he cu es p esen ed in
Fig. 4a) is high enough o exceed he coe ci e ield bu low enough o
allow he obse a ion o a su icien ly poin ed magne ic ansi ion a he
Cu ie empe a u e, TC. This pa ame e has been es ima ed as he
in lexion poin o he magne iza ion as a unc ion o empe a u e,
(minimum in dM/dT cu es, see b). Al hough he ange o empe a u e
a which dM/dT de lec s om ze o is conside able, ypical o sys ems in
which a Cu ie empe a u e dis ibu ion exis s, a clea endency can be
obse ed: TC inc eases wi h he inc ease o he annealing empe a u e.
In ac , i is well known ha TC is s ongly dependen on Fe con en and
he local a omic o de in Fe-Z amo phous compounds [31,32]. In his
sense, i has been epo ed ha in Fe-based amo phous alloys, wi h
non-magne ic a om subs i u ion, TC inc eases as Fe con en dec eases in
he alloy [30]. The inc ease o TC, in his composi ion ange, is due o a
d op o he in e a omic dis ances o o an inc ease o he Fe con en .
Howe e , he he mal ea men o he sample in ol es an inc ease om
6 o 12% o
α
-Fe phase, as de e mined by M¨
ossbaue spec oscopy (see
Table 1). The e o e, he amo phous ma ix o he annealed powde s
exhibi s a sligh impo e ishmen o he Fe con en . I is e i ied by he
enhancemen o he magne iza ion emaining abo e he TC o he
Fig. 5. Magne ic hys e esis loops, aken a di e en empe a u es om 100 K o
300 (100, 150, 200, 220, 240, 250, 260, 280 and 300 K) o he mechanically
alloyed powde s a e hea ing up o he indica ed empe a u es. Inse s show he
low ield egion o he hys e esis loops a 100 and 300 K.
Fig. 6. Pa ame e s ob ained om he app oach o sa u a ion o he magne i-
za ion cu es o Fig. 5 o he powde s hea ed up un il he indica ed empe a-
u es. a) Speci ic sa u a ion magne iza ion and dM
S/dT cu es (inse ), whe e
Tin co esponds o he minimum. b) Pa amagne ic suscep ibili y cu es om
he law o app oach o sa u a ion. Lines a e guide o he eyes.
A.F. Manch´
on-Go d´
on e al.
Jou nal o Non-C ys alline Solids 609 (2023) 122267
5
amo phous s uc u e (see Fig. 4a). Mo eo e , wi h he inc ease o he
annealing empe a u e, he dM/dT cu es become na owe . This ac
could be asc ibed o he elease o he s esses accumula ed in he
amo phous powde du ing he milling p ocess and he educ ion o he
impu i ies due o he nuclea ion o
α
-Fe c ys alli es.
Fig. 5 shows he hys e esis loops o he s udied powde s eco ded a
di e en empe a u es om 100 o 300 K. As expec ed, all he samples
exhibi a simila end, cha ac e ized by a quick inc ease o he
magne iza ion a low ields. This beha io o he hys e esis loops ag ees
wi h he expec ed so -magne ic na u e o he s udied alloys.
The ex ac ed alues o sa u a ion magne iza ion, MS(T), and he
pa amagne ic suscep ibili y,
χ
p(T), o he hys e esis loops a e displayed
in Fig. 6. These pa ame e s ha e been de e mined by i ing he expe -
imen al high- ield magne iza ion cu es (
μ
0H≥1 T) o he linea e sion
o law o app oach o sa u a ion [33]. MS(T)cu es all wi h he e o-
lu ion o he empe a u e due o he e o-pa amagne ic ansi ion o he
amo phous phase. The g ow h o MS as he annealing empe a u e in-
c eases is in ag eemen wi h he g adual ise o he
α
-Fe phase in he
sample, wi h a highe magne iza ion han ha o he amo phous
s uc u e. These esul s a e in ag eemen wi h hose ob ained by
M¨
ossbaue spec oscopy. The inse o he Fig. 6a depic s he dMS /dT
cu es, whose minimum, Tin , is usually app oxima ed o he Cu ie
empe a u e. On he o he hand,
χ
p(T)cu es exhibi a maximum, T
χ
p
peak,
ha sligh ly shi s o highe empe a u es wi h he inc ease o he
annealing empe a u e. The di e gence be ween Tin and T
χ
p
peak ound in
ou esul s indica es he p esence o a dis ibu ion o ansi ion em-
pe a u es [34]. Al hough a me hod o de e mine he pa ame e s o his
dis ibu ion was ecen ly p oposed using Tin and T
χ
p
peak [34], bo h pa-
ame e s need o be e de ined, a oiding a quan i a i e analysis o he
dis ibu ion.
Fig. 7 p esen s he magne ic en opy change, ΔSM, o he s udied
samples as a unc ion o empe a u e o a maximum applied ield
change o 1 T. The M(T,H)da a we e ob ained on cooling cycles as a
unc ion o empe a u e a each magne ic ield, being a empe a u e
in e al o 1 K and he ΔSM was de e mined using a nume ical app ox-
ima ion o he Maxwell ela ion. Demagne izing ield has no been aken
in o accoun and a negligible e ec on ΔSM(T)cu es is assumed [22].
No signi ican di e ences can be obse ed be ween he di e en sam-
ples, eaching a maximum alue o abou 0.45 Jkg
−1
K
−1
a 233 K o he
sample as-milled. This maximum alue sligh ly shi s o highe em-
pe a u es wi h he inc ease o he annealing empe a u e, in ag eemen
wi h he esul s p esen ed abo e. Al hough he ob ained alues o ΔSM
a e simila o hose ound in he li e a u e o samples wi h he same
composi ions ob ained by mechanical milling, he obse ed alues a e
modes when hey a e compa ed wi h amo phous ibbon samples o a
simila composi ion p oduced by apid quenching echniques (see able
2) [35,36]. I is also no ed ha he wid h o ΔSM(T)cu es dec eases o
apidly quenched samples, sugges ing a s onge inhomogenei y in he
samples p epa ed by milling [37]. Recen ly, he C-doping o Fe-Z
amo phous alloys ha e been in es iga ed in o de o imp o e he mag-
ne ocalo ic esponse o hese ma e ials h ough uning he Cu ie em-
pe a u e close o oom empe a u e and achie ing an enhancemen o
ΔSM [38].
4. Conclusions
Relaxa ion o he amo phous s uc u e o Fe
70
Z
30
amo phous alloy
p epa ed by mechanical alloying has been in es iga ed by means o
annealing a empe a u es below he de i i ica ion empe a u e. The
annealing ea men s e ain he amo phous s uc u e o he alloy,
de ec ed by X- ay di ac ion. Howe e , hey induce he ini ia ion o
nuclea ion o
α
-Fe c ys alli es, as es ima ed by M¨
ossbaue spec a, which
need one e omagne ic and one pa amagne ic con ibu ion o be suc-
cess ully i ed. Consequen ly, he amo phous alloy su e s a deple ion in
Fe con en . This ac is e i ied by he augmen a ion o he magne iza-
ion pe sis ing abo e he amo phous alloy’s e omagne ic-
pa amagne ic ansi ion and he Cu ie empe a u e inc ease. Finally,
he na owing o he de i a i e cu es o he magne iza ion wi h he
annealing ea men sugges s ha , despi e he pa i ioning o Fe o he
nuclea ion o he
α
-Fe phase, he amo phous phase o he annealed
samples is mo e chemically and s uc u ally homogeneous han ha o
he o iginal p ecu so .
CRediT au ho ship con ibu ion s a emen
A.F. Manch´
on-Go d´
on: Concep ualiza ion, Da a cu a ion, In es i-
ga ion, Fo mal analysis, Resou ces, W i ing – o iginal d a . J.S.
Bl´
azquez: Concep ualiza ion, Me hodology, Supe ision, W i ing – e-
iew & edi ing, Resou ces. M. Kowalczyk: Da a cu a ion, Supe ision,
Fig. 7. Va ia ion o ΔS
M wi h empe a u e (calcula ed o 1 T ield change) o
he s udied amo phous alloys close o Cu ie empe a u e. Inse shows he
e olu ion o maximum o ΔSM wi h empe a u e.
Table 2
Expe imen al alues o |ΔSM| o FeZ based amo phous alloys p epa ed by di e en echniques.
Composi ion Technique Tann (K) TC (K) ΔH (T) |ΔSM|(Jkg
−1
K
−1
) Re e ence
Fe
70
Z
30
Mechanical alloying as-milled 235 1.0 0.45 [12]
473 238 1.0 0.40 This wo k
573 240 1.0 0.40 This wo k
673 244 1.0 0.38 This wo k
Fe
70
Z
30
Mechanical alloying 244 1.5 ∼0.4 [23]
Fe
91
Z
9
Rapid quenching 233 1.5 1.22 [39]
Fe
90
Z
10
Rapid quenching 245 1 0.87 [33]
Fe
89
Z
11
Rapid quenching 263 1.8 1.3 [34]
Fe
93
Z
7
Spu e ing 160 1.5 ∼0.7 [38]
(Fe
93
Z
7
)
0⋅89
C
0.11
Spu e ing 311 1.5 ∼1
Fe
88
Gd
2
Z
10
Rapid quenching 285 1.5 1.4 [40]
A.F. Manch´
on-Go d´
on e al.
Jou nal o Non-C ys alline Solids 609 (2023) 122267
6
W i ing – e iew & edi ing. J.J. Ipus: Da a cu a ion, Supe ision,
W i ing – e iew & edi ing. T. Kulik: Resou ces, W i ing – e iew &
edi ing. C.F. Conde: Resou ces, Me hodology, Supe ision, W i ing –
e iew & edi ing.
Decla a ion o Compe ing In e es
The au ho s decla e ha hey ha e no known compe ing inancial
in e es s o pe sonal ela ionships ha could ha e appea ed o in luence
he wo k epo ed in his pape .
Da a a ailabili y
No da a was used o he esea ch desc ibed in he a icle.
Acknowledgemen s
This wo k was suppo ed by he PAI o he Regional Go e nmen o
Andalucía and by Jun a de Andalucía-Conseje ía de T ans o maci´
on
Econ´
omica, Indus ia, Conocimien o y Uni e sidades (p oyec P oyEx-
cel_00360). VI and VII-PPUS om Uni e si y o Se ille is also
acknowledged.
Re e ences
[1] M.E. McHen y, M.A. Willa d, D.E. Laughlin, Amo phous and nanoc ys alline
ma e ials o applica ions as so magne s, P og. Ma e Sci. 44 (4) (1999) 291–433.
[2] K. Hono, Nanoscale mic os uc u al analysis o me allic ma e ials by a om p obe
ield ion mic oscopy, P og. Ma e Sci. 47 (6) (2002) 621–729.
[3] K. Balak ishnan, P.D. Babu, V. Ganesan, R. S ini asan, S.N. Kaul, Magne oelas ic
s udy o amo phous Fe90+xZ 10−x alloys, J. Magn. Magn. Ma e . 250 (2002)
110–122.
[4] I. Vincze, D. Kap as, T. Kem´
eny, L. Kiss, J. Balogh, Tempe a u e and ex e nal
magne ic ield dependence o he spin eezing in amo phous Fe93Z 7, J. Magn.
Magn. Ma e . 140 (1995) 297–298.
[5] D. Mish a, A. Pe umal, A. S ini asan, Magne ic p ope ies o mechanically alloyed
Fe100−xZ x (20⩽ x⩽ 35) powde , J Phys D Appl Phys 41 (21) (2008), 215003.
[6] G. Concas, F. Congiu, G. Spano, M. Bionducci, In es iga ion o he e omagne ic
o de in c ys alline and amo phous Fe2Z alloys, J. Magn. Magn. Ma e . 279 (2–3)
(2004) 421–428.
[7] A.F. Manch´
on-Go d´
on, J.J. Ipus, J.S. Bl´
azquez, C.F. Conde, A. Conde, P. S ec,
S udy o he kine ics and p oduc s o he de i i ica ion p ocess o mechanically
amo phized Fe70Z 30 alloy, J. Alloys Compd. 825 (2020), 154021.
[8] V. F anco, J.S. Blazquez, B. Ingale, A. Conde, The Magne ocalo ic E ec and
Magne ic Re ige a ion Nea Room Tempe a u e: ma e ials and Models, Annu. Re .
Ma e . Res. (2012) 305–342.
[9] S.Y. Dan’ko , A.M. Tishin, V.K. Pecha sky, K.A. Gschneidne , Magne ic phase
ansi ions and he magne o he mal p ope ies o gadolinium, Phys. Re . B 57 (6)
(1998) 3478–3490.
[10] A. Planes, L. Manosa, X. Moya, T. K enke, M. Ace , E.F. Wasse mann,
Magne ocalo ic e ec in Heusle shape-memo y alloys, J. Magn. Magn. Ma e . 310
(2) (2007) 2767–2769.
[11] I. Sko anek, J. Ko ac, Magne ocalo ic beha iou in amo phous and
nanoc ys alline FeNbB so magne ic alloys, Czech. J. Phys. 54 (2004) D189–D192.
[12] A.F. Manch´
on-Go d´
on, J.J. Ipus, L.M. Mo eno-Ramí ez, J.S. Bl´
azquez, C.F. Conde,
V. F anco, A. Conde, Co ec ion o he shape e ec on magne ic en opy change in
ball milled Fe70Z 30 alloys, J. Alloys Compd. (2018).
[13] V. F anco, A. Conde, Scaling laws o he magne ocalo ic e ec in second o de
phase ansi ions: om physics o applica ions o he cha ac e iza ion o ma e ials,
In e na ional Jou nal o Re ige a ion-Re ue In e na ionale Du F oid 33 (3) (2010)
465–473.
[14] T. Malakho a, Z. Alekseye a, The Z -Fe phase diag am in he ange 20–40 a .% Fe
and he c ys alline s uc u e o he in e me allic compound Z 3Fe, Jou nal o he
Less Common Me als 81 (2) (1981) 293–300.
[15] M. G ano sky, D. A ias, In e me allic phases in he i on- ich egion o he Z Fe
phase diag am, J. Nucl. Ma e . 229 (1996) 29–35.
[16] L. Schul z, Fo ma ion o amo phous me als by mechanical alloying, Ma e . Sci.
Eng. 97 (1988) 15–23.
[17] K. Un uh, C. Chien, Magne ic p ope ies and hype ine in e ac ions in amo phous
Fe-Z alloys, Phys. Re . B 30 (9) (1984) 4968.
[18] G. He ze , Mode n so magne s: amo phous and nanoc ys alline ma e ials, Ac a
Ma e . 61 (3) (2013) 718–734.
[19] R. Piza o, J. Ga i aonandia, F. Plazaola, J. Ba andia an, J. G eneche, Magne ic
and M¨
ossbaue s udy o mul iphase Fe-Z amo phous powde s ob ained by high
ene gy ball milling, J. Phys. Condens. Ma e 12 (13) (2000) 3101.
[20] A. Gup a, M. Gup a, S. Chak a a y, R. Rü e , H.-.C. Wille, O. Leupold, Fe di usion
in amo phous and nanoc ys alline alloys s udied using nuclea esonance
e lec i i y, Phys. Re . B 72 (1) (2005), 014207.
[21] M. Alouhmy, R. Moubah, G. Alouhmy, M. Abid, H. Lass i, E ec s o hyd ogen
implan a ion on he magne ocalo ic p ope ies o amo phous FeZ ilms, Vacuum
186 (2021), 110063.
[22] A.F. Manch´
on-Go d´
on, J.J. Ipus, L.M. Mo eno-Ramí ez, J.S. Bl´
azquez, C.F. Conde,
V. F anco, A. Conde, Co ec ion o he shape e ec on magne ic en opy change in
ball milled Fe70Z 30 alloys, J. Alloys Compd. 765 (2018) 437–443.
[23] J.S. Blazquez, V. F anco, A. Conde, Enhancemen o he magne ic e ige an
capaci y in pa ially amo phous Fe70Z 30 powde s ob ained by mechanical
alloying, In e me allics 26 (2012) 52–56.
[24] J. Bl´
azquez, J. Ipus, C. Conde, A. Conde, Compa ison o equi alen ball milling
p ocesses on Fe70Z 30 and Fe70Nb30, J. Alloys Compd. 536 (2012) S9–S12.
[25] A.F. Manch´
on-Go d´
on, J.J. Ipus, J.S. Bl´
azquez, C.F. Conde, A. Conde, E olu ion o
Fe en i onmen s and phase composi ion du ing mechanical amo phiza ion o
Fe70Z 30 and Fe70Nb30 alloys, J. Non C ys . Solids 494 (2018) 78–85.
[26] J.S. Bl´
azquez, A.F. Manch´
on-Go d´
on, J.J. Ipus, C.F. Conde, A. Conde, On he use o
JMAK heo y o desc ibe mechanical amo phiza ion: a compa ison be ween
expe imen s, Num. Sol. Simula ions, Me als (2018).
[27] A.F. Manch´
on-Go d´
on, J.J. Ipus, J.S. Bl´
azquez, C.F. Conde, A. Conde, In luence o
milling ime on he homogenei y and magne ism o a Fe70Z 30 pa ially
amo phous alloy: dis ibu ion o cu ie empe a u es, Ma e ials (Basel) 13 (2)
(2020) 490.
[28] R.A. B and, J. Laue , D.M. He lach, The e alua ion o hype ine ield dis ibu ions
in o e lapping and asymme ic mossbaue -spec a: a s udy o he amo phous alloy
PD77.5-XCU6SI16.5FEX, J. Phys. F-Me al Phys. 13 (3) (1983) 675–683.
[29] J.S. Blazquez, J.J. Ipus, V. F anco, C.F. Conde, A. Conde, Ex ac ing he
composi ion o nanoc ys als o mechanically alloyed sys ems using Mossbaue
spec oscopy, J. Alloys Compd. 610 (2014) 92–99.
[30] A.F. Manch´
on-Go d´
on, R. L´
opez-Ma ín, A. Vidal-C espo, I.J. J, J.S. Bl´
azquez, C.
F. Conde, A. Conde, Dis ibu ion o ansi ion empe a u es in magne ic
ans o ma ions sou ces e ec s p ocedu es o ex ac in o ma ion om
expe imen al, Da a, Me als (2020).
[31] R. Piza o, J.S. Ga i aonandia, F. Plazaola, J.M. Ba andia an, J.M. G eneche,
Magne ic and Mossbaue s udy o mul iphase Fe-Z amo phous powde s ob ained
by high ene gy ball milling, J. Phys.: Condens. Ma e 12 (13) (2000) 3101–3112.
[32] R. Moubah, A. Zamani, A. Olsson, S. Shi, A. Hall´
en, S. Ca lson, D. A ani is,
P. No dblad, B. Hj¨
o a sson, P. J¨
onsson, So oom- empe a u e e omagne ism o
ca bon-implan ed amo phous Fe93Z 7 ilms, Appl. Phys. Exp ess 6 (5) (2013),
053001.
[33] J.M. Coey, Magne ism and Magne ic Ma e ials, Camb idge uni e si y p ess, 2010.
[34] A.F. Manch´
on-Go d´
on, L.M. Mo eno-Ramí ez, J.J. Ipus, J.S. Bl´
azquez, C.F. Conde,
V. F anco, A. Conde, A p ocedu e o ob ain he pa ame e s o Cu ie empe a u e
dis ibu ion om he momagne ic and magne ocalo ic da a, J. Non C ys . Solids
520 (2019), 119460.
[35] T. Dang Thanh, Y. Yu, P. Thanh, N. Yen, N. Dan, T.-.L. Phan, A. G ishin, S. Yu,
Magne ic p ope ies and magne ocalo ic e ec in Fe90−x Ni x Z 10 alloy ibbons,
J. Appl. Phys. 113 (21) (2013), 213908.
[36] D. Mish a, M. Gu am, A. Reddy, A. Pe umal, P. Sa a anan, A. S ini asan,
Enhanced so magne ic p ope ies and magne ocalo ic e ec in B subs i u ed
amo phous Fe–Z alloy ibbons, Ma e . Sci. Eng. 175 (3) (2010) 253–260.
[37] L.M. Mo eno-Rami ez, J.J. Ipus, V. F anco, J.S. Blazquez, A. Conde, Analysis o
magne ocalo ic e ec o ball milled amo phous alloys: demagne izing ac o and
Cu ie empe a u e dis ibu ion, J. Alloys Compd. 622 (2015) 606–609.
[38] A. Cha kaoui, R. Moubah, M. Bouhbou, H. Lass i, A. Eloua i, P.E. J¨
onsson, C i ical
beha io and magne ocalo ic e ec in C-implan ed Fe93Z 7 amo phous ilms,
Solid S a e Commun. 316-317 (2020), 113962.
[39] K.S. Kim, Y.S. Kim, J. Zidanic, S.G. Min, S.C. Yu, Magne ocalo ic e ec in as-
quenched and annealed Fe91-xYxZ 9 (x=0.5, 10) alloys, Physica S a us Solidi a-
Appl. Ma e . Sci. 204 (12) (2007) 4096–4099.
[40] T.D. Thanh, N.H. Yen, N.H. Duc, T.L. Phan, N.H. Dan, S.C. Yu, La ge
magne ocalo ic e ec a ound oom empe a u e in amo phous Fe-Gd-Z alloy
ibbon wi h sho - ange in e ac ions, J. Elec on. Ma e . 45 (5) (2016) 2608–2614.
A.F. Manch´
on-Go d´
on e al.