Full text of DOI:10.1002/1521-4052(200101)32:1<20::AID-MAWE20>3.0.CO;2-C

Development of Creep Resistant Mg-Gd-Sc Alloys
with Low Sc Content
Entwicklung kriechbestaÈ ndiger Mg-Gd-Sc-Legierungen mit geringem Sc-Gehalt
I. StulÂõkova , B. Smola, F. von Buch, B. L. Mordike
High thermal stability and good mechanical properties are crucial
HochtemperaturstabilitaÈt und gute mechanische Eigenschaften
for the wider future application of magnesium alloys. One of the sind entscheidend fuÈr die verstaÈrkte Anwendung von Magnesium-
most promising directions is the alloying of Mg with rare earth legierungen. Eine der vielversprechendsten Entwicklungsrichtun-
elements as Gd. The fine dispersion of metastable b0 phase (c- gen ist das Legieren von Mg mit Seltenen Erden wie Gd. Die fein-
base centred orthorhombic, a ˆ 0.641 nm, b ˆ 2.223 nm, disperse metastabile b0-Phase (c-basiszentrierte orthorombisch,
c ˆ 0.521 nm), already known from commercially successful a ˆ 0.641 nm, b ˆ 2.223 nm, c ˆ 0.521 nm), wie sie bereits aus
WE alloys (Mg-Y-Nd-Zr), precipitated in all three possible orienta- kommerziellen WE-Legierungen (Mg-Y-Nd-Zr) bekannt ist, schei-
tion modes during T6 treatment causes very pronounced age hard- det sich im binaÈren Mg-Gd-System bei der T6 WaÈrmebehandlung in
ening in binary Mg-Gd system and inhibits very effectively the allen drei moÈglichen kristallografischen Orientierungen aus. Sie
dislocation motion during the creep. The stable
b phase verursacht dabei eine ausgepraÈgte AushaÈrtung und unterbindet
(Mg5Gd, f.c.c. structure, a ˆ 2.234 nm) ensures the creep resis- auch die Versetzungsbewegung beim Kriechen. Die stabile b-
tance comparable to WE alloys. A high content of Gd (above Phase (Mg5Gd, kfz-Struktur, a ˆ 2.234 nm) verstaÈrkt den Wider-
10 wt.%) is necessary to attain the required microstructure. The stand gegen das Kriechen vergleichbar zu WE-Legierungen. Ein
addition of Sc (below 1 wt.%) and Mn (about 1.5 wt.%) suppresses hoher Gehalt von Gd (uÈber 10 gew.-%) ist noÈtig, um die ge-
the solubility of Gd in Mg considerably. The complex precipitation wuÈnschte Mikrostruktur einzustellen. Die Zugabe von Sc (unter
process involving the precipitation of very stable Mn2Sc, Mn and 1 gew.-%) und Mn (etwa 1.5 gew.-%) begrenzt die LoÈslichkeit
Gd containing phase and metastable b0 phase is responsible for von Gd in Mg betraÈchtlich. Der komplexe Ausscheidungsprozeû
superior creep properties of MgGd5Sc0.3Mn1 alloy at elevated beinhaltet die Bildung sehr stabiler Mn2Sc-Phase, Mn- und Gd-hal-
temperatures. Even at 300 8C the creep resistance is markedly bet- tiger Phase und metastabiler b0-Phase. Diese sind verantwortlich
ter than for WE43 alloy. The increased Gd and Sc contents in fuÈr die verbesserten Kriecheigenschaften von MgGd5Sc0.3Mn1-
MgGd10Sc0.8Mn1 alloy do not further improve the creep resis- Legierungen bei erhoÈhten Temperaturen. Selbst bei 300 8C ist
tance.
die KriechbestaÈndigkeit deutlich besser als bei WE43-Legierung.
Der hoÈhere Gd- und Sc-Gehalt in MgGd10Sc0.8Mn1-Legierungen
verbessert die Kriecheigenschaften nicht weiter.
ganese. The diagrams for complex systems have been calcu-
lated and information on the stability of intermetallic phases
has been obtained to estimate whether homogenisation and
age hardening is possible. Simultaneously the binary system
magnesium gadolinium was investigated. This system ex-
hibits high age hardening in concentrated alloys (15 wt.%
of Gd) due to the precipitation of metastable phases similar
to those in WE 54 [8].
As the precipitation of Mn2Sc, which ensures thermal sta-
bility of mechanical properties in Mg-Sc-Mn and Mg-Sc-Ce-
Mn alloys, is limited by Mn content and the excess of Sc does
not considerably improve the properties of these alloys [9],
[10] a reduction in amount of expensive scandium is possible.
In order to study the combined beneficial influence of scan-
dium, manganese and gadolinium on creep resistance and me-
chanical properties complex Mg-Sc-Gd-Mn alloys with Sc
content lower than 1 wt.% were squeeze cast and the devel-
opment of microstructure was investigated and correlated
with the relevant mechanical properties.
1 Introduction
The increasing demand for reducing weight not only for
space and aeronautical applications but also in automobile
and leisure applications has been the motivation for many
research programmes concerning the magnesium alloys.
The problems are often solved by better design, new produc-
tion methods or coatings but some such as high temperature
mechanical properties are fundamental material properties
which can be improved by sophisticated alloy development
based on a physical metallurgical understanding of the rele-
vant processes of deformation. The starting point can be
the WE series (Mg-Y-Nd-Zr alloy) [1], [2], [3] which is com-
mercially available (MEL, Manchester, U.K.). The alloy
WE43 is suitable for sustained operation at temperatures up
to 250 8C whereas WE54 although superior in strength and
creep resistance exhibits brittleness.
Consequently a programme was started based on the mag-
nesium-scandium system [4], [5], [6]. The problems asso-
ciated with the insufficiency of the phase diagram were
solved with the help of theoretical calculations [7], which re-
sults were experimentally confirmed. The age hardening of
Mg-Sc alloys (up to 19 wt.%) is poor and the alloys were
not capable of providing the desired creep resistance. The al-
loy systems chosen for further investigation were magnesium
scandium manganese and magnesium scandium cerium man-
2 Experimental Details
All alloys studied were melted in the laboratory using the
squeeze casting technique starting from pure materials or a
20
0933-5137/01/0101-0020$17.50 ‡ .50/0
Mat.-wiss. u. Werkstofftech. 32, 20±24 (2001)
Ó WILEY-VCH Verlag GmbH, D-69451 Weinheim, 2001

Table 1. Composition of squeeze cast alloys
Tabelle 1. Zusammensetzung von Druckguûlegierungen
Alloy
Sc [wt.%]
Gd [wt.%]
Mn [wt.%]
MgGd5
MgGd10
MgGd15
MgGd5Sc0.3Mn1
MgGd5Sc0.3Mn1
MgGd10Sc0.8Mn1
±
±
±
0.26
0.34
0.91
4.5
9.3
14.6
4.64
5.08
9.63
±
±
±
1.53
1.49
1.3
master alloy (for Mg-Mn). The measurement of creep rates
and other mechanical properties was supplemented with stan-
dard metallography and transmission electron microscopy
(TEM), electron diffraction (ED) and X-ray microanalysis
(EDX). In order to detect the temperature ranges of the pre-
cipitation the changes of electrical resistivity measured at 77K
were used and correlated to the changes in hardness. The iso-
chronal and isothermal annealing of specimens was under-
taken either in the oil bath (up to 240 8C) or in the furnace
with argon atmosphere. The annealing was followed by im-
mediate cooling into liquid nitrogen or water in order to pre-
serve the microstructure developed during the annealing. The
tensile tests were performed at temperatures from room tem-
perature to 400 8C in the air furnace at a constant strain rate
ꢀ 10 4 s 1. The minimum creep rates were determined by
creep dip tests at 200 8C±400 8C at stresses in the range Fig. 1. Hardness HV3 response of Mg-Gd alloys to isochronal an-
nealing
20±80 MPa. The following alloys, Table 1, were prepared.
Abb. 1. HaÈrte-Auslagerungskurven von Mg-Gd-Legierungen
3 Results and Discussion
3.1 Binary Mg-Gd Alloys
As detected by electrical resistivity measurements the pre-
cipitation processes take place in solution heat treated Mg-Gd
alloys (500 8C/6 hours) in the temperature range of 100 8C±
420 8C. High age hardening was observed in MgGd15 alloy
whereas it is less pronounced in MgGd10 and MgGd5 ±
see Fig. 1, where the response of Vickers hardness HV3 to
isochronal annealing is plotted. The fine dispersion of meta-
stable b0 phase (c-base centred orthorhombic, a ˆ 0.641 nm,
b ˆ 2.223 nm, c ˆ 0.521 nm, particle size 10 to 15 nm) pre-
cipitated in all three possible orientation modes is responsible
for the maximum hardness in MgGd15 at 260 8C. One mode of
the metastable b0 phase persists up to 330 8C only and trans-
forms into the stable b phase (Mg5Gd, f.c.c. structure,
a ˆ 2.234 nm) up to 420 8C. Above 420 8C the redissolution
takes place. The precipitation of all orientation modes of the
b0 phase during the isothermal annealing at 200 8C leads to the
pronounced increase of hardness without any overaging up to
80 hours in MgGd10 and MgGd15. Long annealing at 200 8C
was therefore chosen for T6 heat treatment.
Fig. 2. Minimum creep rates of Mg-Gd alloys compared to com-
mercial WE43 and QE22 alloys at 200 8C and 60 MPa
Abb. 2. Minimale Kriechraten von Mg-Gd-Legierungen im Ver-
gleich zu kommerziellen WE43 und QE22-Legierungen bei
200 8C und 60 MPa
the creep test at 300 8C of T6 treated MgGd10 and
MgGd15 specimens the transformation of b0 metastable
phase into the stable b phase takes place. The similar pre-
cipitation process is well known in WE alloys [11], [12].
Fig. 3 shows the dislocations passing between large Mg5Gd
plates oriented parallel to 1010 prismatic planes in
MgGd15 crept to the fracture at 300 8C and an applied stress
of 60 MPa. In Fig. 4 the creep curves of MgGd10 and
MgGd15 after T6 treatment are compared to that of WE43
T6 (350 8C, 30 MPa). The minimum creep rates of Mg-Gd
alloys are somewhat lower whereas the WE43 is superior
in the creep life.
The b0 precipitates are very effective inhibitors for disloca-
tion movement during the creep. The minimum creep rate
values obtained at 200 8C and 60 MPa for MgGd15 after
11
T6 treatment are in order of magnitude 10
only. As the
b0 phase develops at 200 8C also during the creep test of
cast material, the creep resistance at 60 MPa is still two times
better than that for WE43 T6. Fig. 2 shows the minimum
creep rate for the binary alloys compared to WE43 and
QE22 at 200 8C and an applied stress of 60 MPa. During
Mat.-wiss. u. Werkstofftech. 32, 20±24 (2001)
Kurztitel fuÈr Kol.-titel
21

Fig. 5. Hardness HV3 response to isothermal annealing of Mg-Gd-
Sc-Mn alloys
Abb. 5. HaÈrteverlauf HV3 von Mg-Gd-Sc-Mn-Legierungen in Ab-
haÈngigkeit der GluÈhzeit
heat treatment were chosen as 96 hours for
MgGd5Sc0.3Mn1 and 72 hours for MgGd10Sc0.8Mn1 at
200 8C, where the peak hardness was reached ± see Fig. 5.
Simultaneous precipitation processes are responsible for
the microstructure in T5 treated MgGd5Sc0.3Mn1 alloy
namely: 1) precipitation of very thin plates (diameter
ꢀ 30±100 nm, thickness ꢀ 1.5 nm) of Mn and Gd containing
metastable phase parallel to a-Mg basal plane; 2) precipitation
of fine particles most probably Mn2Sc (size ꢀ 10±15 nm); 3)
precipitation of fine particles of metastable b0 phase, Fig. 6.
Thin Mn and Gd containing basal plates manifest themselves
Fig. 3. Microstructure of MgGd15 T6 treated alloy after fracture in
creep test at 300 8C and an applied stress 60 MPa
Abb. 3. Mikrostruktur von MgGd15 T6 waÈrmebehandelt nach dem
Bruch im Kriechversuch bei 300 8C und angelegte Zugspannung
von 60 MPa
Fig. 4. Creep curves of T6 treated MgGd10 and MgGd15 alloys
compared to T6 treated WE43; creep conditions 350 8C and 30 MPa
Abb. 4. Kriechkurven T6 waÈrmebehandelter MgGd10- und
MgGd15-Legierungen im Vergleich zu T6 waÈrmebehandelter
WE43. Kriechbedingungen 350 8C und 30 MPa
3.2 Complex Mg-Gd-Sc-Mn alloys
The full homogenisation of these complex alloys might be
possible in very narrow region of Mn concentration only ac-
cording to the preliminary calculations of stable phase dia-
gram [13]. The alloys investigated in this work do not fall
into that range. As cast alloys contain a fine dispersion (ap-
prox. 15 nm) of presumably Mn2Sc particles arranged into
ªribbonsº parallel to the basal plane projection. Grain bound-
aries are thickly decorated by coarse particles of stable Mg5Gd
(up to 500 nm). High pressure modification of pure Gd with
f.c.c. structure (a ˆ 0.54 nm) was observed in the form of
square shaped plates (size ꢀ 1 lm). The parameters for T5
Fig. 6. Thin plates of hexagonal metastable phase containing Mn
and Gd parallel to a-Mg basal plane together with fine particles of
Mn2Sc phase in MgGd5Sc0.3Mn1 T5 treated alloy
Abb. 6. DuÈnne Platten aus hexagonaler metastabiler Phase mit Mn
und Gd parallel zur a-Mg Basisebene zusammen mit feinen Parti-
keln der Mn2Sc-Phase in MgGd5Sc0.3Mn1, T5 waÈrmebehandelt
22
I. StulÂõkovaÂ, B. Smola, F. van Buch, B. L. Mordike
Mat.-wiss. u. Werkstofftech. 32, 20±24 (2001)

4 Conclusion
Low content of Sc (under 1 wt.%) and Mn (about 1.5 wt.%)
in magnesium lowers significantly the solid solubility of Gd.
This results in precipitation of the most effective hardening
phase, metastable c-base centred orthorhombic phase, at Gd
concentration of about 10 wt.% lower in Mg-Gd-Sc-Mn alloy
than in the binary Mg-Gd alloy. This phase inhibits also
strongly the dislocation movement during the creep in both
binary Mg-Gd and complex Mg-Gd-Sc-Mn alloys. Fine basal
plane plates of metastable phase containing Mn and Gd may
contribute to good properties of Mg-Gd-Sc-Mn alloy. Pre-
cipitation of thermally stable Mn2Sc phase has a favourable
effect on the thermal stability of the complex precipitation
microstructure as developed by a T5 heat treatment in Mg-
Gd-Sc-Mn alloys. The minimum creep rates of as cast Mg-
Gd-Sc-Mn alloy are of one order of magnitude lower at
300 8C and 40 MPa than that of cast WE54 alloy at the
same conditions. The increased Gd and Sc contents in
MgGd10Sc0.8Mn1 alloy do not further improve the creep
resistance.
Fig. 7. Temperature dependence of yield tensile stress of Mg-Gd-
Sc-Mn alloys after T5 treatment
Abb. 7. TemperaturabhaÈngigkeit der Streckgrenze von Mg-Gd-Sc-
Mn-Legierungen nach einer T5 WaÈrmebehandlung
strongly in ED patterns by streaks of intensity parallel to
(0002)Mg reflection. Diffraction patterns of these plates can
be consistently indexed on the basis of a hexagonal structure
with a ˆ 0.556 nm, c ˆ 0.521 nm equiaxed to a-Mg matrix.
This metastable phase was not observed in the T5 treated
MgGd10Sc0.8Mn1 alloy but the precipitation of b0 phase
is much more pronounced there.
The YTS values of both alloys after T5 treatment deformed
at temperatures up to 400 8C show a good thermal stability up
to 300 8C, Fig. 7. The same conclusion can be drawn for the
UTS. These results are evidence of good thermal stability of
microstructure produced by T5 treatment.
Acknowledgement
The support by the German Research Council (Thrust Re-
search Project SFB 390 ± Magnesium Technology), by the
grant Agency of Czech Republic (Grant # 106/99/0187) and
by Research Goal VZ 190-01/206054 is gratefully acknowl-
edged.
The continuous precipitation takes place during the creep 4 References
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In Table 2 the minimum creep rates at 300 8C and 40 MPa
are compared for Mg-Gd-Sc-Mn alloys, Mg-Gd alloys and
WE54. It is seen that the complex Mg-Gd-Sc-Mn alloys
are markedly better than WE54 under the same conditions.
The minimum creep rates of as cast complex materials
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lower than that for binary Mg-Gd alloy with 15 wt.%Gd. The
same creep resistance can be reached only if previous T6 heat
treatment of MgGd15 is applied. As the minimum creep rates
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and 40 MPa are the same it is not necessary to alloy high con-
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Â
Table 2. Minimum creep rates at 300 8C and an applied stress 40 MPa
Tabelle 2. Minimale Kriechraten bei 300 8C und angelegter Zugspannung von 40 MPa
1
Alloy
Heat treatment
Minimum creep rate [s ]
7
WE54
MgGd15
MgGd15
MgGd5Sc0.3Mn1
MgGd10Sc0.8Mn1
as cast
as cast
T6
as cast
as cast
1.6 Â 10
7
1.0 Â 10
8
1.5 Â 10
8
1.5 Â 10
8
1.3 Â 10
Mat.-wiss. u. Werkstofftech. 32, 20±24 (2001)
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Â
Â
Received: 8/7/01
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I. StulÂõkovaÂ, B. Smola, F. van Buch, B. L. Mordike
Mat.-wiss. u. Werkstofftech. 32, 20±24 (2001)