DOI 10.

1007/s11041-017-0177-y
Metal Science and Heat Treatment, Vol. 59, Nos. 7 – 8, November, 2017 (Russian Original Nos. 7 – 8, July – August, 2017)

ALUMINUM ALLOYS
UDC 621.78:669.715

EFFECT OF HOMOGENIZING HEAT TREATMENT OF LIQUID

ALUMINUM–COPPER ALLOYS ON THE STRUCTURE
OF RAPIDLY CRYSTALLIZED SPECIMENS

V. V. Astaf’ev,1 A. R. Kurochkin,2 T. I. Yablonskikh,1 I. G. Brodova,1, 4 and P. S. Popel’3, 5

Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 8, pp. 20 – 25, August, 2017.

Centrifugal casting into a massive slot chill mold was used to prepare two series of specimens of alloys of the
Al – Cu system, containing from 10 to 32.2 at.% Cu. The first series was fabricated without a homogenizing
heat treatment of the melt, while the second series was fabricated with heating of the melt to 1400°C. Both
kinds of specimens were cast at the same temperature in order to provide for the same cooling rate of about
104 K/sec. The structures, phase compositions and microhardnesses of the structural components are com-
pared. It is established that the homogenizing heat treatment changes the kinetics of crystallization and, hence,
the proportion of phases in the alloy structure and the copper content in them.

Key words: alloys of aluminum – copper system, homogenizing of melt, rapid quenching, struc-
ture of alloy.

INTRODUCTION heating to a certain homogenizing temperature (dependent

The notion of metastable microheterogeneity of liquid
metal alloys [1] appeared as a hypothesis for explaining from
common positions the phenomena such as microseparation
in eutectic and monotectic systems, inherited influence of the
structure of charge components on the properties of melt and
resulting crystalline material, and differences of temperature
dependences (hysteresis) in the properties of melts obtained
upon post-melting heating and subsequent cooling. Accord-
ing to this hypothesis, the melting of a heterogeneous initial
ingot or heterogeneous charge is accompanied by the forma-
tion of molten system comprising a dispersion medium of
certain composition in metastable equilibrium with sus-
pended dispersed particles of different composition. Upon
1
Institute of Metal Physics, Ural Branch of the Russian Academy
of Sciences, Ekaterinburg, Russia.
2
Ural Institute of State Fire-Extinguishing Service, Ministry of
Emergency Situations of the Russian Federation, Ekaterinburg,
Russia.
3
Ural State Pedagogical University, Ekaterinburg, Russia.
4 structure of ingots formed upon rapid quenching has not
E-mail: brodova@imp.uran.ru.
5
E-mail: pspopel@mail.ru.
on the composition), the system irreversibly passes to a ther-
modynamically stable state of homogeneous solution that is
retained until crystallization.
The validity of metastable microheterogeneity hypothe-
sis was unambiguously confirmed by experimental data on
the small-angle neutron scattering in Pb – Sn [2] and Al – Si
[3, 4] melts. The hysteresis was clearly manifested in the
temperature dependences of density [5] and kinematic vis-
cosity [6, 7] of Cu – Al melts. The investigation [7] of melts
with compositions close to q-phase (30 and 35 at.% Cu)
showed that their homogenizing temperature was close to
870°C. For most alloys of the Al – Cu system [5, 6], clearly
pronounced branching of the temperature dependences of
density and kinematic viscosity of melts was observed in the
entire concentration interval of their existence. Based on the
results of density measurements by the gamma-ray technique
[5], which is most sensitive to homogenization, the tempera-
ture of melt transition to a homogeneous state for some al-
loys was found to be close to 1300°C. However, the influ-
ence of a homogenizing overheating of Cu – Al melts on the
been studied until now, although these experiments could

491
0026-0673/17/0708-0491 © 2017 Springer Science + Business Media New York
492
à 720
Òåmperature, °Ñ
Rapid
quenching
15 20
Time, min
b
1400
Òåmperature, °Ñ
60
Time, min
help determining a relation between the melt homogeneity
and resulting structure of the crystalline ingot.
In this context, the present work was aimed at experi-
mental investigation of the influence of homogeneity of ini-
tial Al – Cu melts, in which copper aluminides are the main
structural component (up to 32.2% Cu), on the structure of
rapidly quenched crystalline ingots.6
METHODS OF STUDY
Alloy ingots containing 10 – 32.2% Cu were prepared
in a high-temperature box furnace by smelting high-purity
components: A999 grade aluminum and electrolytic copper.
The inherited influence of a homogenizing treatment of the
melt upon the solid phase structure was retained using the
method of rapid quenching.
Rapidly crystallized alloy specimens in the form of disks
with thicknesses within h = 1 – 2.4 mm were obtained using
a centrifugal casting setup in which a preliminarily
heat-treated melt was suppled from ladle into à graphite
spreader rotating at 1000 rpm and rapidly crystallized in a
massive copper slot chill mold. Two series of specimens
were prepared from Al – Cu alloys containing 10, 17.1, 25,
and 32.2% Cu. The first series was cast without homogeniz-
ing heating of the melt, while the second series was cast upon
preliminary heating of the melt to 1400°C. The samples in
both series were cast at 700°C, which ensured equal rates of
metal cooling during crystallization. According to published
data [9], the cooling rate of about 2mm thick samples is close
to 5 ´ 105 K/sec. Figure 1 shows the schemes of heat treat-
6 International Centre for Diffraction Data (ICDD) and Ameri-
Here and below, the copper content in alloy is expressed as per-
centage atomic fraction (at.%).
V. V. Astaf’ev et al.
Cooling in furnace
with partly open door
720
Rapid
quenching Fig. 1. Scheme of alloy smelting regimes
40 15
without (a) and with (b ) homogenizing heat
treatment.
ment of melts without homogenizing heating above liquidus
(regime I ) and with homogenizing heating (regime II ).
Comparative investigations of the structure of alloy in-
gots obtained by centrifugal casting of melts heat treated in
regimes I and II were performed on Neophot-32 optical mi-
croscope. The material structure was revealed by etching in
0.5% aqueous HF acid solution, Keller’s etchant, or 5 – 10%
aqueous NaOH solution. The volume fractions of alloy
phases were calculated according to the standard Glagolev’s
point method. The grain size was determined by the conven-
tional line intercept method. The microhardness was deter-
mined using a PMT-3 hardness meter; the microhardnesses
of structural components were averaged over ten measure-
ments.
The alloy phases were identified using the results of
x-ray diffraction (XRD) analysis. The XRD measurements
were performed on a DRON-3.0 automated diffractometer
using filtered CoKa radiation. XRD patterns for the phase
analysis were measured by stepwise scanning in 2q = 20 –
120° interval of reflection angles at 0.05° step and 5 sec ex-
posure time. This interval of 2q angles contained all the main
reflections from planes of the fcc lattice of aluminum and the
tetragonal lattice of Al 2Cu copper aluminide. The initial
processing of diffractograms and the selection of lines for
qualitative phase analysis were carried out using OUTSET
program package, and the analysis was performed using
PHAN program. PROFILE program was used for approxi-
mation of the profiles of (331)aAl diffraction lines and pre-
cise calculation of the lattice parameters of alloy matrix. Dif-
fraction patterns were interpreted using JCPDS cards of the
can Society for Testing and Materials (ASTM) databases.
Effect of Homogenizing Heat Treatment of Liquid Aluminum–Copper Alloys on the Structure of Specimens
30 mm
30 mm
Fig. 2. Microstructure of Al – 10% Cu alloy ingot obtained from melt heat-treated in regimes I (a, b )
and II (c, d ): a, c) primary a-phase and eutectic (a + Al2Cu); b, d ) eutectic morphology.
RESULTS
Data on the phase composition of Al – Cu alloys accord-
ing to the equilibrium phase diagram [10] are presented in
Table 1. Comparison of the structure (Fig. 2) and hardness of
Al – 10% Cu alloy specimens obtained from melts heat-
treated in regimes I and II revealed some distinctive features.
In particular, the structure of a specimen obtained in regime I
is typical of an alloy with hypo-eutectic composition and is
formed by branched primary dendrites of Al-based a solid
solution with round cross section (Fig. 2a ) and by rodlike
eutectic (a + Al2Cu) occurring in dendritic inter-axial re-
gions and on grain boundaries (Fig. 2b ). The phase composi-
tion of a specimen homogenized in the liquid state (re-
gime II ) remains unchanged. A comparison of the micro-
structures presented in Fig. 2a and c shows that the homoge-
nizing heating results in slight roughening of structural com-
ponents and increasing volume fraction of the primary phase.
Thus, in respect of the phase ratio, the alloy composition
“shifts” toward lower concentrations of aluminum. At the
same time, in addition to regions of hypo-eutectic composi-
TABLE 1. Phase Composition of Al – Cu Alloys Studied
Cu, at.% Phase composition
10.0 Al-based a solid solution + eutectic (a + Al2Cu)
17.1 Eutectic (a + Al2Cu)
25.0 q-Phase (Al2Cu) + eutectic (a + Al2Cu)
32.2 q-Phase (Al2Cu)
493
a 6 mm b
c 11 mm d
tion, there are seldom grains of pure eutectic with cellular
structure (Fig. 2d ).
The microhardness of eutectic did not change with in-
creased overheating of the melt and amounted to 1700 MPa.
The microhardness of a-phase increased from 1200 to
1300 MPa, which might be evidence of increased solid-solu-
tion hardening of the matrix. In order to confirm this fact, we
have measured the profiles of (331)a XRD lines for the spec-
imens of both types (Fig. 3a ). It was found that the XRD line
of specimens cast from melts treated in regime II was shifted
toward greater angles, which corresponded to smaller lattice
periods of the solid solution of copper in aluminum as com-
pared to those for specimens cast from melts treated in re-
gime I (4.0438 ± 0.0001 Å versus 4.0448 ± 0.0002 Å, re-
spectively). Therefore, it can be ascertained that the homoge-
nizing heat treatment of melt leads to increase in the content
of copper in a solid solution.
Thus, specimens of the given composition treated at tem-
peratures studied and cooled at the same rate retain the phase
composition typical of the hypo-eutectic alloy. Increase in
the smelting temperature to 1400°C leads to growth in the
fraction of a-phase and the content of copper in this phase.
According to the equilibrium phase diagram, Al –
17.1% Cu alloy is eutectic, but the increased rate of melt
cooling leads to its crystallization under nonequilibrium con-
ditions and results in deviation of the composition toward a
hyper-eutectic region. For this reason, the structure of a spe-
cimen obtained from the melt treated in regime I represented
predominantly q-phase (Al2Cu), growing in the form of
tetragonal prisms or cross-shaped dendrites (Fig. 4a ), and
494 V. V. Astaf’ev et al.

I, pulses
colony growth shapes may also be indicative of a variable
1200
à degree of melt supercooling prior to crystallization, which is
1000 related to its microheterogeneous structure.
II The overall phase composition of the alloy homogenized
800
in the liquid state remained unchanged, but showed increased
600 number of regions with eutectic structure in comparison to
I
400 that observed for the control specimen. In the regions of
hyper-eutectic composition, the primary q-phase forms
200
needle-like dendrites with developed second-order branches
0 (Fig. 4d ), which are somewhat more rough than in the con-
145 146 147 148 149 150 151 152 153
2q, deg trol. Eutectic (a + Al2Cu) is predominantly globular, with
I, pulses 2 – 5 mm size of intermetallic phase grains (Fig. 4e ).
600 The profiles of (331)aAl XRD lines for both specimens
b of Al – 17.1% Cu alloy almost coincide (Fig. 3b ), which im-
500
plies that the copper content in aluminum-based solid solu-
400 tion is the same to within the measurement error. The lattice
I
300 period of the eutectic a-phase (to within 0.0002 Å error)
II amounts to 4.0510 Å) The microhardness of eutectic formed
200
upon the homogenizing treatment of melt can probably be
100 explained by about two-fold roughening of the eutectic com-
145 146 147 148 149 150 151 152 153
2q, deg
ponents. Thus, based on the results of structure investigation,
I, pulses it may me concluded that the conversion of melt to a homo-
1200 geneous state does not significantly influence the structure
c CuAl2 and phase composition of eutectic alloy.
1000 As the copper content in the alloy increases to 25%, the
800 type of structure formation changes and there appears a
I, II structure (Fig. 5) characteristic of hyper-eutectic composi-
600
tions. The primary component is intermetallic q-phase
CuAl2 CuAl2
400 CuAl2 (Al2Cu) with predominant growth in the form of tetragonal
prisms or plane-face dendrites (Fig. 5a ). The second struc-
200 Al Al Al CuAl2
CuAl CuAl2 CuAl2 Al tural component is oriented eutectic (q + Al2Cu) with an
0
10 20 30 40 50 60 70 80 90 100 110 120 130
interplate spacing on the order of 3 – 5 mm (Fig. 5b ) and a
2q, deg microhardness of 1800 – 1900 MPa.
I, pulses The specimen that was homogenized in the liquid state
3500 (regime II ) exhibited a nonuniform structure comprising
d both the regions corresponding to a hyper-eutectic composi-
3000
2500
tion (Fig. 5c ) and quasi-eutectic regions free of clear evi-
CuAl2

CuAl2 dence for the primary crystallization of intermetallide. In the

CuAl

2000
regions of hyper-eutectic composition, the structure com-
1500
CuAl2
Al, CuAl2 prised the primary q-phase (tetragonal prisms, dendrites with
CuAl
CuAl

1000 CuAl2 CuAl2 CuAl2 developed first-order axis) and eutectics with finer struc-
500 Al Al tures. In particular, the interplate spacing in a eutectic colony
I, II could exhibit a three-fold decrease (Fig. 5d ). The microhard-
0
10 20 30 40 50 60 70 80 90 100 110 120 130 ness of such eutectics was higher and amounted to
2q, deg 2150 MPa. Figure 3c shows the corresponding XRD patterns
Fig. 3. Profiles of (331)aAl XRD lines of Al – 10% Cu (a) and Al – of specimens with this composition measured under identical
17.1% Cu (b ) alloy specimens and XRD patterns of Al – 25% Cu (c) conditions.
and Al – 32% Cu (d ) alloy specimens cast from melts treated in re- Identification of the alloy phases based on the observed
gimes I and II. lines of XRD reflections confirmed the presence of two
structural components, namely, Al-based solid solution and
Al2Cu intermetallide. Thus, comparison of the structures of
eutectic (a + Al2Cu) appearing either as dendritic agglome- Al – 25% Cu alloy specimens formed from different struc-
rates of mutually treading eutectic phases (Fig. 4b ) or as mi- tural states of the melt indicated that a specimen that was ho-
cron-sized globules of copper aluminides on the background mogenized in the liquid state exhibited more pronounced
of aluminum matrix (Fig. 4c ). This difference of eutectic structural inhomogeneity and its eutectic was more finely
Effect of Homogenizing Heat Treatment of Liquid Aluminum–Copper Alloys on the Structure of Specimens 495

30 mm a 6 mm b 6 mm c

Fig. 4. Microstructure of Al – 17.1% Cu

alloy ingot obtained from melt heat-treated
in regimes I (a – c) and II (d, e): a, d ) pri-
30 mm 6 mm mary q-phase and eutectic (a + Al2Cu);
d e
b, c, e) eutectic morphology.

differentiated, which was confirmed by the results of micro-
hardness measurements.
According to its chemical composition, Al – 32.2% Cu
alloy falls in a narrow region of existence of the q-phase
(Al2Cu). However, the kinetics of crystallization under rapid
quenching conditions changes so that additional components
(besides q-phase) appear representing eutectic (q + Al2Cu)
and a copper-rich phase growing in the form of plates
(Fig. 6). According to the equilibrium phase diagram, the lat-
ter phase is Al10Cu10 with a monoclinic lattice of C2/m space
group. The appearance of this phase is evidence of a signifi-
cant liquation of composition in the specimen cross section,
which is caused by both the microinhomogeneity of melt and
the high rate of its crystallization. According to the data of
metallographic analysis, the structure of a specimen obtained
from melt treated in regime I comprises predominantly pris-
matic primary crystals of q-phase and a eutectic screening
these primary crystals (Fig. 6a ). Figure 6b shows separate
crystals of h-phase (Al10Cu10 ) in the form of plates with
lengths on the order of 30 mm and about ten times smaller
widths.

30 mm a 11 mm b

30 mm c 11 mm d

Fig. 5. Microstructure of Al – 25% Cu alloy ingot obtained from melt heat-treated in regimes I
(a, b ) and II (c, d ): a, c) primary q-phase and eutectic (q + Al2Cu); b, d ) eutectic morphology.
496
30 mm
30 mm
Fig. 6. Microstructure of Al – 32.2% Cu alloy ingot obtained from melt heat-treated in regimes I
(a, b ) and II (c, d ): a, c) primary q-phase and eutectic (q + Al2Cu); b ) h-phase laths; d ) sectorial
eutectic morphology.
The structure of a specimen of this alloy homogenized in
the liquid state also exhibits components with various
morphologies and compositions. The predominant form of
growth represents primary crystals of q-phase shaped as
tetragonal prisms (Fig. 6c ), which are screened by finely dif-
ferentiated eutectic (q + Al2Cu). In addition, the structure
contains eutectic colonies of sectorial morphology, which in-
herit the shape of external base q-phase crystals (Fig. 6d ).
This morphology is a predominant growth form of eutectic
colonies, from which separate “quasi-eutectic” zones are
formed. The values of microhardness of the aforementioned
eutectics with different morphologies are rather close (2700
and 2550 MPa, respectively).
Analysis of the XRD patterns showed that, irrespective
of the regime of thermal treatment of the melt, specimens of
Al – 32.2% Cu alloy contain Al2Cu phase (Fig. 3d ). Calcu-
lated reflection angles for all lines and interplanar distances
for each (hkl ) correspond to tabulated data. Note that, be-
cause of a relatively small volume fraction of Al10Cu10 phase
and the coincidence of reflection angles for many planes be-
longing to crystal lattices of the two intermetallic phases, the
obtained XRD patterns do not allow the peaks belonging
exactly to the copper-rich phase to be recognized.
DISCUSSION
The results described above show evidence of a complex
influence of the homogenizing treatment of Al – Cu alloy
melts on the structure formation in rapidly crystallized speci-
V. V. Astaf’ev et al.
a 30 mm b
c 60 mm d
mens. In order to explain the effect of melt overheating and
degree of homogeneity on the structure of solid-state speci-
mens, let us compare the obtained results to peculiarities of
the temperature dependences of alloy density r in the molten
state, which were reported previously [5]. In that work, it
was assumed that the lower part (i.e., that penetrated by
gamma radiation) of a specimen was significantly enriched
by dispersed particles with high copper content and the tem-
perature dependences were constructed for of rm product
(rather than density r), where m is the mass coefficient of
gamma radiation beam attenuation dependent on the chemi-
cal composition of the irradiated zone. According to those
data, the rm(T ) curves of exhibited maximum differences in
the regimes of heating and subsequent cooling for alumi-
num-based melts containing 10 – 32.2% Cu. Then, using
points above which these curves begin to coincide, it is pos-
sible to determine the homogenization temperature (Thom ),
i.e., that of melt transition to a homogeneous state (Table 2).
According to data presented in Table 2, the lowest homoge-
nizing temperature took place in the alloy with 10% Cu. As
the copper content was increased to 17.1%, the homogeniz-
ing temperature exhibited growth to 1330°C, but remained
almost unchanged upon further increase in the copper con-
tent up to 32.2%. Since all specimens obtained with treat-
ment in regime II were heated in the liquid state to 1400°C, it
can be assumed that all of them were homogeneous prior to
crystallization.
According to the results presented and considered above,
the homogenizing heat treatment of molten metal most sig-
nificantly influenced the crystalline structure of rapidly
Effect of Homogenizing Heat Treatment of Liquid Aluminum–Copper Alloys on the Structure of Specimens
TABLE 2. Maximum Differences and Homogenizing Tempera-
tures of rm(T ) Curves Measured during Post-Melting Heat Treat-
ment and Subsequent Cooling of Al – Cu Alloy Melts [5]
Maximum difference Homogenizing
Cu, at.%
of rm(T ) values, % temperature, °C
10.0 1.1 900
17.1 11.0 1330
25.0 15.0 1310
32.2 16.0 1320
quenched ingot with hypo-eutectic composition. This can be
related to some special features of crystallization and to sig-
nificant overheat (by about 500°C) above the homogenizing
temperature. In this case, the homogenizing treatment modi-
fies crystallization kinetics and the ratio of volume fractions
of structural components. In particular, the amount of eutec-
tic decreases and the degree of aluminum-based phase dop-
ing increases, which leads to increasing microhardness of
copper-rich aluminum-based solid solution (solid-solution
hardening).
As the alloy composition approaches the eutectic point,
the role of liquid-state homogenization decreases. Probably,
rather insignificant overheat (by only about 70°C) above the
homogenization temperature, the structures of specimens ob-
tained upon heat treatment of the melt in regimes I and II dif-
fered rather slightly. We can only point out a small increase
in the volume fraction of eutectic with some roughening of
its structural components and reduction in microhardness.
The alloy of hyper-eutectic composition (Al – 25% Cu)
showed increased influence of the homogenizing heat treat-
ment of melt and, despite rather close value of overheat
(about 90°C) above the homogenization temperature, the
eutectic was modified, its microhardness increased, and there
appeared quasi-eutectic zones free of primary phases.
Upon further increase in the content of copper (up to
32.2%), the alloy falls in the region of crystallization of
q-phase, the composition of which according to the equilib-
rium phase diagram can vary within about 1.5% Cu wide ho-
mogeneity interval. Here, crystallization of a specimen from
the melt treated in regime I revealed the presence of an AlCu
phase (untypical of the given composition), the appearance
of which can be related to the microheterogeneous structure
of melt and the liquation phenomena during crystallization.
Upon the heating of melt to 1400°C in regime II (i.e., 80°C
above the homogenization temperature), this phase was not
detected by metallographic and XRD techniques.
In should be noted that specific design features of the
centrifugal casting setup employed in this work did not allow
the melt to be heated above 1400°C in the experiments de-
scribed above. Then, it is not excluded that, in melts of the
last three compositions for which the homogenization tem-
perature is only slightly below 1400°C, a fully homogenized
state was not attained, which could account for rather weakly
497
pronounced effects observed in structures of the correspond-
ing crystallized specimens.
CONCLUSIONS
Despite complexity of the phase diagram of the alumi-
num–copper system and high temperatures of the transition
of melts from a metastable microheterogeneous state to a ho-
mogeneous state, results obtained in this work correspond to
the data obtained previously in investigations of simple
eutectic alloys. These results confirm general laws of the in-
fluence of a homogenizing heat treatment of liquid metal on
the features of ingot structure formation [8], including (i) in-
creased supersaturation of solid solutions, (ii) shift of the
eutectic point toward higher concentrations of second com-
ponent, (iii) formation of a quasi-eutectic structure in speci-
mens of hypo-eutectic compositions, (iv) dispersion of
eutectic phases and primary phase crystallites, and (v) modi-
fication of their morphologies.
Metallographic investigations were performed in the
framework of works according to the State Order of the Fe-
deral Agency of Science and Education of the Russian Fe-
deration, Program “Structure” project No. 01201463331.
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