The isothermal section of the Dy-Fe-Sb ternary system at 773 K

Article abstract of DOI:10.1016/j.jallcom.2007.12.073

The isothermal section of the Dy-Fe-Sb ternary system at 773 K has been investigated mainly by X-ray powder diffraction in this work. The existence of eight binary compounds and one ternary compound were conformed in this system. The section consists of t

Full text of DOI:10.1016/j.jallcom.2007.12.073

Journal of Alloys and Compounds 468 (2009) 103–106
The isothermal section of the Dy–Fe–Sb
ternary system at 773 K
a,b,∗
a,b
a,b
a,b
Jingqi Liu
, Bo Zong , Xiaomao Yang , Xuehong Cui ,
a,b
a,b
c,d
Kunpeng Su , Xina Wang , Junqin Li
Institute of Materials Science, Guangxi University, Nanning, Guangxi 530004, PR China
Key Laboratory of Nonferrous Metal Materials and New Processing Technology, Guangxi University,
Ministry of Education, Nanning, Guangxi 530004, PR China
a
b
c
College of Materials Science and Engineering, Shenzhen University 518060, PR China
Shenzhen Key Laboratory of Special Functional Materials, Shenzhen 518060, PR China
d
Received 21 October 2007; received in revised form 20 December 2007; accepted 20 December 2007
Available online 3 January 2008
Abstract
The isothermal section of the Dy–Fe–Sb ternary system at 773 K has been investigated mainly by X-ray powder diffraction in this work. The
existence of eight binary compounds and one ternary compound were conformed in this system. The section consists of twelve single-phase regions,
twenty-two two-phase regions and eleven three-phase regions. The compound Dy
phase extended from about 44 at.% Sb to 46 at.% Sb and the maximum solid solubility of Sb in Fe phase is about 3 at.% Sb at 773 K.
2007 Elsevier B.V. All rights reserved.
4 3
Sb was not stable at 773 K. The homogeneity range of ␧ (FeSb)
©
Keywords: Rare earth alloys and compounds; Phase diagrams; X-ray diffraction
1
. Introduction
Ref. [11] reported the binary diagrams of the Dy–Fe, Dy–Sb
and Fe–Sb systems. At 773 K, there are four intermetallic com-
The rare earth intermetallic compounds have been
pounds Fe2Dy, Fe3Dy, Fe23Dy and Fe17Dy2 in the Dy–Fe
6
studied because of their excellent properties, for exam-
ple, the compounds Tb1−XDyXFe2, Tb0.3Dy0.7(Fe1−XVX)2,
Tb0.3Dy0.7(Fe1−XBeX)2 and Tb Dy (Fe1−YCoY)2 with
binary system, three intermetallic compounds DySb, Dy4Sb3
and Dy Sb3 in the Dy–Sb binary system, two intermetallic com-
5
pounds FeSb and FeSb2 in the Fe–Sb binary system. One ternary
compound FeDy Sb2 was reported in Ref. [12].
6
0
.36
0.64
C15-type phase structure have giant magnetostrictive property
[
1–5]. The phase relationships of the RE–Fe–Sb (RE = La, Pr,
2
. Experimental details
Nd, Ho, Gd, Er and Yb) ternary systems were reported pre-
viously [6–10]. Up to the present, the phase diagram of the
Dy–Fe–Sb ternary system has not been reported. The existence
of compound Dy4Sb3 was disputed in Dy–Fe–Sb ternary sys-
tem. In order to determine the existence of the phases and the
phase relationships in the Dy–Fe–Sb system, to provide use-
ful information for searching new materials, in this paper, we
studied phase relationships in the Dy–Fe–Sb system at 773 K.
The purities of dysprosium, iron and antimony used in this work are 99.9%,
99.9% and 99.99%, respectively. The alloy buttons (each 2 g) were prepared
by arc melting using a non-consumable tungsten electrode and a water-cooled
copper tray under an atmosphere of pure argon. All samples (total 112) were
sealed in evacuated quartz tubes for homogenization heat treatment. The homog-
enization temperatures were chosen on the basis of the binary phase diagrams of
the Dy–Sb, Dy–Fe and Fe–Sb systems. The samples in the Sb-rich region were
annealed at 853 K for 25 days. The other samples were annealed at 993 K for
25 days. Subsequently, the samples were cooled to 773 K at a rate of 9 K/h and
kept at 773 K for 10 days (some samples were re-annealed were kept at 773 K
another 10 days if necessary), then quenched into an ice water mixture.
The samples were powdered for X-ray diffraction (XRD) analysis. The non-
brittle powder, were sealed in evacuated glass tube, annealed at 773 K for 4 days
and then quenched into liquid nitrogen before XRD experiment. The brittle
powder samples were directly used for XRD analysis after grinding. The X-ray
∗
Corresponding author at: Institute of Materials Science, Guangxi University,
No. 100, Daxue Road, Nanning, Guangxi 530004, PR China.
Tel.: +86 771 3236850; fax: +86 771 3233530.
E-mail address: gxuliujq@163.com (J. Liu).
0
925-8388/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.jallcom.2007.12.073

1
04
J. Liu et al. / Journal of Alloys and Compounds 468 (2009) 103–106
Fig. 1. XRDP of sample with composition Fe54Dy31Sb15 under different annealed times: ( ) XRDP of the samples which were only annealed at 773 K for 10 days:
Dy4Sb3 + Dy5Sb3 + DySb + Fe23Dy6; ( ) XRDP of the samples after annealing at 773 K for 10 days again: Dy5Sb3 + DySb + Fe23Dy6.
diffraction analysis was performed using a Rigaku D/Max 2500 V diffractometer
with a copper target, graphite monochromator, a voltage of 40 kV and a current
of 200 mA. The XRD data were analyzed using softwares JADE 5.0 [13] and
Powder Cell Windows (PCW 2.4) [14], Pearson’s Handbook of crystallographic
Data [15] and the Powder Diffraction File (PDF release 2002).
compound Dy4Sb3 is stable in the Dy–Sb system from 473 K to
053 K. HoweverRefs. [16–18]reportedthatcompoundDy4Sb3
2
was not observed at 673 K, 1070 K or 1100 K. The X-ray diffrac-
tion patterns (XRDPs) for the samples near the composition of
Dy4Sb3 showed that the compound Dy4Sb3 is present in some
samples but absent in the others annealed at 773 K for 10 days.
The intensities of XRDP of compound Dy4Sb3 were weaken
markedly or disappeared in the same samples re-annealed at
773 K for another 10 days. The XRDP of the samples with com-
3
. Results and discussion
3
.1. Phase analysis
position of Fe Dy31Sb annealed at 773 K for different time
54
15
In this work, four binary compounds Fe2Dy, Fe3Dy, Fe23Dy6
are shown in Fig. 1. The XRDP for the samples annealed at
773 Kfor10daysconsistsofthepatternsoftheDy4Sb3, Dy5Sb3,
DySb and Fe23Dy6 four phases. The XRDP for the same sample
annealed at 773 K for another 10 days consists of the patterns
of the Dy5Sb3, DySb and Fe23Dy6 three phases. It indicated
that Dy4Sb3 may be decomposed into Dy5Sb3 and DySb for the
annealing time long enough at 773 K. The XRDP of the sam-
ple with composition Fe35Dy41Sb24 annealed at 773 K for 10
days, shown in Fig. 2, consists of Dy5Sb3, DySb and Fe23Dy6
three phases. These results indicated that the compound Dy4Sb3
should not be stable at 773 K. The decomposition of Dy4Sb3 was
and Fe17Dy2 were confirmed at 773 K in the Dy–Fe system. Two
binary compounds FeSb and FeSb2 have been confirmed in the
Fe–Sb system at 773 K. The FeSb intermetallic compound has a
homogeneity range from about 44 at.% Sb to 46 at.% Sb and the
maximum solid solubility of Sb in Fe phase is about 3 at.% Sb at
73 K. The results were estimated by the disappearing method
of the X-ray powder diffraction and were in good agreement
with that reported in Ref. [11].
7
In the Dy–Sb system at 773 K, we confirmed the existence
of compounds DySb and Dy Sb3. Ref. [11] point out that the
5
Fig. 2. XRDP of the sample with composition Fe35Dy41Sb24: Dy5Sb3 + DySb + Fe23Dy6.

J. Liu et al. / Journal of Alloys and Compounds 468 (2009) 103–106
105
Fig. 3. XRDP of sample with composition Fe6Dy74Sb20: Dy5Sb3 + Dy + FeDy6Sb2.
completely at 773 K for long enough time. The result is in good
agreement with that reported in Refs. [16–18].
Table 1
Crystallographic data of the initial components and compounds in the Dy–Fe–Sb
system of 773 K
Ternary compound FeDy Sb2 was confirmed in the
6
Dy–Fe–Sb system at 773 K. The XRDP of the compound
Phase
Space
group
Structure attice parameters
References
type
(nm)
FeDy Sb2 was observed in the XRDPs of samples with compo-
6
a
b
c
sition Fe Dy74Sb20 (Fig. 3, fourth phase in Fig. 3 is Dy2O3) and
6
Fe11Dy Sb24 (Fig. 4). The crystallographic data of the initial
components and compounds in the Dy–Fe–Sb ternary system is
given in Table 1.
¯
65
␣Fe
Im3m
W
0.29315
–
–
–
–
–
–
–
–
–
–
–
[15]
Fe17Dy2
Fe23Dy6
Fe3Dy
Fe2Dy
␣Dy
P63/mmc Ni17Th2 0.8453
0.8287 [15]
[15]
2.4578 [15]
[15]
0.5466 [15]
[15]
¯
Fm3m
Mn23Th6 1.210
Be3Nb
Cu2Mg
–
¯
R3m
Fd3m
P63/mmc Mg
Fm3m
P63/mcm Mn5Si3
R3m
P63/mmc NiAs
Pnn2
0.5125
0.7328
0.3458
0.6154
0.8882
0.43084
0.407
–
3
.2. The isothermal section of the Dy–Fe–Sb ternary system
␣DySb
NaCl
–
at 773 K
Dy5Sb3
Sb
FeSb
FeSb2
0.6270 [15]
1.1274 [15]
0.513
¯
␣-As
By comparing and analyzing the X-ray diffraction patterns
[15]
of all samples, and identifying the existence of phases in each
sample, we constructed the isothermal section of the phase
diagram of the Dy–Fe–Sb ternary system at 773 K. The isother-
mal section, shown in Fig. 5, consists of twelve single-phase
regions, twenty-two two-phase regions and eleven three-phase
regions. Thetwelvesingle-phaseregionsare:A(Dy), B(Fe2Dy),
FeS2
0.58328 0.65376 0.31973 [15]
¯
FeDy6Sb2 P62M
CuSi2Zr 0.81449 0.41641 0.23923 [12]
C (Fe3Dy), D (Fe23Dy ), E (Fe17Dy2), F (Fe), G (FeSb), H
6
Fig. 4. XRDP of sample with composition Fe11Dy65Sb24: Dy5Sb3 + Fe2Dy + FeDy6Sb2.

1
06
J. Liu et al. / Journal of Alloys and Compounds 468 (2009) 103–106
4. Conclusion
We have investigated and constructed the isothermal section
of the Dy–Fe–Sb ternary system at 773 K. Eight binary com-
pounds Fe2Dy, Fe3Dy, Fe23Dy , Fe17Dy2, FeSb, FeSb2 DySb
6
and Dy Sb3 and one ternary compound FeDy Sb2 have been
5
6
confirmed. The compound Dy4Sb3 was not stable at 773 K. The
homogeneity range of FeSb is 44 at.% Sb–46 at.% Sb and the
maximum solid solubility of Sb in Fe phase is about 3 at.% Sb at
773 K. The solid solubilities for the other single-phase regions
were not observed. The isothermal section of the Dy–Fe–Sb
ternary system at 773 K consists of twelve single-phase regions,
twenty-two two-phase regions and eleven three-phase regions.
Acknowledgement
This work was supported by the National Natural Science
Foundation of China (Grant No. 50471108).
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Fig. 5. The isothermal section of Dy–Fe–Sb ternary system at 773 K.
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1
2
3
4
5
6
7
8
9
Dy + FeDy6Sb2 + Fe2Dy
Dy + FeDy6Sb2 + Dy5Sb3
FeDy6Sb2 + Dy5Sb3 + Fe2Dy
Fe2Dy + Dy5Sb3 + Fe3Dy
Fe3Dy + Dy5Sb3 + Fe23Dy6
DySb + Fe23Dy6 + Dy5Sb3
Fe17Dy2 + Fe23Dy6 + DySb
DySb + Fe17Dy2 + Fe
[
[
[
[
[
(
(
(
8
DySb + Fe + FeSb
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DySb + FeSb2 + Sb
1
1
0
1
[
[
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5 6
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