Effect of atmosphere and heating mode on

sintering of 6711 and 7775 alloys

C. Padmavathi1, A. Upadhyaya1 and D. Agrawal*2
The current study examines the effect of sintering atmosphere and heating mode on the
densification, microstructure, phase analysis and properties of Al1Mg0?8Si0?25Cu (6711) and
Al7Zn2?5Mg1Cu (7775) alloys. The compacts were heated in conventional and 2?45 GHz
microwave sintering furnaces under vacuum, N2, Ar and H2 at 630uC. Both alloy compacts
coupled well with microwaves and underwent rapid heating (y22uC min21). The overall
processing time was reduced to about 5558% through microwave sintering. Microwave
sintering resulted in greater densification for 6711 alloy under vacuum followed by N2. In contrast,
7775 alloy resulted in poor densification under all atmospheres as compared with conventional
sintering. For all compositions and atmospheres, microwave sintering resulted in microstructural
inhomogeneity with the absence/presence of a lower amount of intermetallic phases. This has
been correlated with lesser time available for the diffusion of alloying elements into the Al matrix.
The conductivity, hardness and corrosion properties of both compacts improved depending upon
heating mode and atmosphere.
Keywords: 6711 and 7775 alloys, Microwave sintering, Atmosphere effect, Densification, Microstructure, Properties

Introduction attempt has been made to overcome above problems

Sintering of aluminium is considered to be problematic
due to their higher affinity for oxygen1 and the presence
of thermodynamically stable oxide layer.2 Therefore, a
dewpoint of (2140uC at 600uC or PO2 ,10250 atm is
required to reduce the Al2O3,3 which is not physically
attainable and hence atmosphere plays an important
role.4,5 The literature610 reported different views on the
most suitable sintering atmospheres for aluminium alloys.
Several researchers4,6,8 showed N2 atmosphere to be more
effective than vacuum or argon or dissociated ammonia.
However, Martin and Castro8 showed that vacuum is
better than N2 for sintering of AlCuMgSi alloy. Later,
Showaiter and his co-workers1012 reported that vacuum
sintered (degassed) 6061 alloy resulted in higher tensile
properties than N2 under T6 condition. Jha et al.7 claimed
that argon and vacuum have little difference, while N2
was the least effective atmosphere during sintering of
6061Al2O3 composites.
Conventional sintering (radiative heat transfer)13 is a
slow heating process (510uC min21) resulting in longer
cycle times14,15 but providing microstructural homo-
geneity due to prolonged heating. Also owing to its
relatively lower melting temperature and higher homo-
logous temperature, aluminium alloys are prone to
significant microstructural coarsening.16 Therefore, an
1
Department of Materials Science and Engineering, Indian Institute of
Technology, Kanpur, UP, India
2
Materials Research Institute, Pennsylvania State University, University
Park, PA, USA
*Corresponding author, email dxa4@psu.edu
through faster heating rate and protective atmospheres.
Microwave sintering is one such novel technique which
offers tremendous advantages over conventional sinter-
ing including higher heating rate, reduction in cycle time
and energy consumption to fabricate parts at lower
cost and being eco-friendly.1719 In recent years, it has
been shown that metallic particulate compacts (ferrous,
refractory metals, bronze and Mo)1315,2022 couple with
microwaves and very fast heating rate can be achieved.19
Microwave sintering of aluminium based composites
and metallic powders (AlCuFe) has been investigated
by previous researchers.2326 To the best of our knowl-
edge, so far no work has been reported on the
interaction of microwaves with very conductive alloys
like AlMgCuSi and AlZnMgCu. In the current
study, we examine the effect of sintering atmosphere and
heating mode on densification response and properties
in correlation with microstructural and phase evolution
of 6711 and 7775 alloy compacts.
Experimental
As received Al1Mg0?8Si0?25Cu (6711) (d50: 83?6,
shape: irregular) and Al7Zn2?5Mg1Cu (d50: 88?2,
shape: irregular) (7775) alloys were supplied by Ampal
Inc. USA. The powder characteristics have been pro-
vided elsewhere in detail.27 The alloy powders were
compacted at 400 MPa into cylindrical pellets (16 mm in
diameter and 6 mm in height) using a uniaxial semi-
automatic hydraulic press (Ichalkaranji, India). The
thermogravimetric analysis (TGA) was performed up to
700uC at a heating rate of 10uC min21 under N2. The

W. S. Maney & Son Ltd. 2011

Received 4 February 2011; accepted 29 March 2011
DOI 10.1179/143307511X13109310554409 Materials Research Innovations 2011 VOL 15 NO 4 294
 Padmavathi et al. Effect of atmosphere and heating mode on sintering of 6711 and 7775 alloys

2 Thermogravimetry analysis of 6711 alloy sintered in

1 Heating proles for 6711 and 7775 alloys in conven- nitrogen atmosphere
tional and microwave furnaces

Conventionally sintered samples were subjected to three

green compacts were subjected to debinding at 350uC for
6 h in a conventional vacuum furnace before sintering.
The delubricated compacts were sintered at 630uC for
1 h using conventional and microwave furnaces under
vacuum, N2, Ar and H2 (dewpoint:240uC). Microwave
sintering of green compacts were carried out in a 6 kW
furnace (Cober Electronics Inc., USA) in gas atmo-
spheres and a 6 kW, 2?45 GHz vacuum furnace (Cober
Electronics Inc., USA). Further details of the microwave
sintering system set-up have been described elsewhere.27
Conventional sintering was carried out in a SiC heated
tubular furnace (Bysakh & Co., Kolkata, India) in gas
atmospheres and under vacuum in a SiC tubular furnace
(Mahendra Instruments, India). The vacuum level of
1026 torr was maintained in both heating modes.
The sintered density was obtained through dimen-
sional measurements as well as by Archimedes displace-
ment method. Densification parameter was calculated
and procedure is given elsewhere in detail.1 The
microstructural analyses were carried out using an
optical microscope (Zeiss, Germany) and a scanning
electron microscope (SEM) (FEI, The Netherlands). The
phase determination was done using an X-ray powder
diffractometer (Rich Seifert & Co., Germany) with Cu
Ka radiation at a scan rate of 3u min21. Similarly,
surface compositional analyses were performed using X-
ray photoelectron spectroscopy (XPS) (Kratos, Axis
Ultra, UK) on sintered compacts.
Vickers bulk hardness measurements and condu-
ctivity studies were performed on sintered compacts.
point bend test and tensile testing using a universal
testing machine supplied by Instron (UK). The poten-
tiodynamic polarisation and open corrosion potential
testing were conducted in a flat cell containing 3?5
wt-%NaCl solution at a scan rate of 0?2 mV s21 from
21300 to 400 mV. The details of the experimental set-
up used for electrochemical studies have been described
in detail elsewhere.27
Results and discussion
Densification response
Figure 1 shows the typical temperaturetime profile for
6711 and 7775 compacts sintered in conventional and
microwave furnaces at 630uC. Both alloy compacts
coupled well with microwaves and got rapidly heated up
resulting in overall higher heating rate (y22uC min21).
There was about 5558% reduction in processing time
for microwave sintered compacts. Table 1 compares the
densification response of both alloy compacts sintered in
conventional and microwave furnaces under various
atmospheres. The densification response was lower for
all microwave sintered compacts except for vacuum
sintering (6711) as compared with conventional sinter-
ing. Also all microwave sintered compacts underwent
swelling (except for vacuum sintered 6711), while con-
ventionally sintered 6711 compacts exhibited shrinkage
under vacuum and nitrogen. Insufficient diffusion of
transient melt occurred in microwave sintered compacts
leading to poor sinterability and swelling behaviour.

Table 1 Effect of heating mode and sintering atmosphere on densication response of 6711 and 7775 alloys sintered at
630uC*

Sintering atmosphere Sintered density/%Th Densification parameter

Heating mode/alloy composition 6711 7775 6711 7775

Vacuum (CON) 96.8 91.8 0.3 20.3
Vacuum (MW) 97.5 0.5
Nitrogen (CON) 96.1 91.6 0.2 20.4
Nitrogen (MW) 94.2 85.8 20.3 21.3
Argon (CON) 94.7 88.6 20.1 20.8
Argon (MW) 93.4 88 20.4 21.0
Hydrogen (CON) 92.9 86.6 20.5 21.2
Hydrogen (MW) 92.4 77.4 20.6 22.6
*CON: conventional; MW: microwave.

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 Padmavathi et al.
3 Optical photomicrographs of 6711 alloy compacts sintered at 630uC in a conventional and b microwave furnaces under
various atmospheres
Vacuum sintering resulted in better densification due to
effective oxide removal and contaminants leading to
stronger AlAl bonds. The shrinkage behaviour and
enhanced densification for conventionally sintered com-
pacts under N2 can be attributed to AlN formation,
which modifies the wetting characteristics.28,29 Pore
filling is considered as major densification mechanism
occurring during final stages of sintering.4 The forma-
tion of AlN was well supported through TGA analysis
(weight gain) under N2 for 6711 alloy as shown in Fig. 2.
In contrast, during microwave heating, even if AlN
formation occurred, it does not yield better density since
AlN is microwave transparent.17
For both alloy compositions and heating modes,
sintering under argon and hydrogen led to lower
sintered density and swelling behaviour. This may be
attributed to the insolubility of argon in liquid
aluminium,5 which had an inhibiting effect upon
densification. Also hydrogen sintered compacts resulted
in lesser liquid formation which prevented shrinkage.4
H2 has a higher solubility in liquid aluminium1,5 which
degraded wetting behaviour and retarded pore filling.4
The efficacy of sintering atmosphere for 6711 alloy in
terms of sintered density for both heating modes:
H2RArRN2Rvacuum (highest) and for 7775 alloy is
as follows: H2RN2RAr. Unlike for 6711 alloy,
although the vacuum sintering of 7775 alloy in conven-
tional mode exhibited better density, vacuum sintering
should be avoided due to relatively high vapour pressure
Table 2 Effect of heating mode and atmopshere on
weight loss of 7775 alloy at 630uC*
Sintering temperature/uC Heating mode Loss/wt-%
Vacuum CON 2
MW
Nitrogen CON 0.6
MW 0.9
Argon CON 1.2
MW 1.3
Hydrogen CON 1.5
MW 1.2
*CON: conventional; MW: microwave.
Effect of atmosphere and heating mode on sintering of 6711 and 7775 alloys
of Zn.1 This makes these alloy more susceptible to Zn
loss as compared with other atmospheres in both
modes as is evident from Table 2. In contrast, micro-
wave sintering resulted in similar weight loss in all
atmospheres.
Microstructure and phase analysis
Figures 3 and 4 compare the effect of heating mode and
atmosphere on the optical photomicrographs of both
alloys. Irrespective of alloy compositions, microwave
sintering resulted in microstructural coarsening with
pores being restricted to grain boundaries. All con-
ventionally sintered compacts (6711) exhibited less
porosity, developed interparticle bonds and supersolidus
liquid phase formation leading to complete diffusion
into grains and Mg2Si precipitates. For both alloys,
vacuum and nitrogen seem to have relatively lower
porosity levels than other atmospheres in conventional
furnace as seen in Fig. 3.
It was quite interesting to note that all 7775
microwave sintered compacts resulted in a differential
contrast particularly near the grain boundary regions as
shown in Fig. 4. This was mainly due to the incomplete
diffusion of alloying additives into Al matrix. Also 7775
alloy N2 sintered in conventional furnace exhibited
precipitation of some phases from interior of solid
solution grain into grain boundaries leaving pinhole
pores in grains. This interesting phenomenon is called
precipitation induced densification.30 The SEM of
microwave nitrogen sintered 6711 compacts consisted
of relatively inhomogeneous grains with proportionately
larger fraction of eutectic melt phases at grain bound-
aries as shown in Fig. 5a. Similarly, 7775 microwave
sintered compacts exhibited larger accumulation of
liquid phase at grain boundaries with tiny pores near
grain periphery arranged like pearls in a necklace as
shown in Fig. 5b. Similar results on inhomogeneous
microstructure were reported by Upadhyaya and Sethi20
on microwave sintered premixed bronze.
Figures 6 and 7 compare the effect of heating mode and
sintering atmosphere on the phase evolution for 6711 and
7775 compacts using X-ray diffraction (XRD) studies. The
microwave sintered 6711 compacts resulted in presence of
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 Padmavathi et al. Effect of atmosphere and heating mode on sintering of 6711 and 7775 alloys

4 Optical photomicrographs of 7775 alloy compacts sintered at 630uC in a conventional and b microwave furnaces under
various atmospheres

5 Photomicrographs (SEM) of a 6711 and b 7775 alloy compacts sintered in microwave furnace at 630uC under nitrogen
atmosphere

6 X-ray diffraction plots showing effect of sintering atmopshere on phase evolution of 6711 alloy compacts sintered at
630uC in a conventional and b microwave furnaces

only a-Al phase under all sintering atmospheres, i.e.
complete absence of intermetallic phases. This may be
attributed to the lesser time available for diffusion of
alloying species to homogenise.20 Similar observations
have been reported on microwave sintering of premixed
bronze20 and 90WNiCu alloys31 systems. Peelamedu
et al.32 also reported similar results and attributed the
reduction in peak intensities to decrystallisation of ceramic
phases. The conventionally sintered 6711 compacts con-
tained CuMgAl2 and Mg2Si phases besides the a-Al peaks
under all atmospheres. The AlN peak overlapped with
Mg2Si peaks for N2 sintered compacts. The presence
of AlN phase altered surface wetting characteristics,
in turn enhanced rearrangement28 and densification.

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 Padmavathi et al.
7 X-ray diffraction plots showing effect of sintering atmopshere on phase evolution of 7775 alloy compacts sintered at
630uC in a conventional and b microwave furnaces
Conventionally sintered 7775 compacts contained a-Al,
MgZn2 and CuMgAl2 phases under N2 and H2 atmo-
sphere. In contrast, Ar sintered compacts showed a shift in
diffraction angles which may be attributed to the presence
of Mg2Zn11 and Al0?71Zn0?29 phases. Unlike conventional
sintering, there was no noticeable shift in XRD peaks of
microwave sintered compacts. It was inferred that micro-
wave sintered compacts contained lower amount of
intermetallic phases as compared with conventional
sintering.
Figure 8 compares the effect of sintering atmosphere
and heating mode on surface composition of sintered
alloys using XPS analysis. The conventionally sintered
6711 compacts exhibited lower intensities of all elements
in different chemical states as compared with microwave
sintering. The vacuum atmosphere resulted in lower
oxygen contents and indicated predominance presence
of Mg (1 s, KK spectral lines/Auger emissions) in
comparison with both Ar and N2, which might be due
to some reaction products affecting densification at
initial stages.5 The XPS analysis of microwave sintered
compacts showed higher intensity of Mg (1 s, KK) and
8 X-ray photoelectron spectroscopy analysis showing
effect of heating mode and sintering atmopshere on
surface composition of 6711 sintered compacts at
630uC
Effect of atmosphere and heating mode on sintering of 6711 and 7775 alloys
O KK peaks along with N 1 s peaks. In case of
microwave sintering under Ar and H2, it is interesting to
note that O (1 s, KK) peaks are not boarder but they
also occurred at different energy levels. This shift in
binding energy may be due to the formation of complex
oxides leading to poor sinterability.
Similarly, N2 and Ar sintered 7775 compacts in
microwave furnace resulted in higher Zn contents on
surface of broken compacts which confirmed incomplete
diffusion of eutectic melt phases as shown in Fig. 9. The
presence of O and Mg in higher amounts for all
compacts supported the formation of spinel structure
which facilitated densification through breakage of
oxide layers.3 For H2 sintered compacts, the absence
of zinc confirmed either its complete absence or its
dissolution into matrix.
Properties of sintered alloys
Figure 10a and b summarises the effect of heating mode
and sintering atmosphere on electrical conductivity
and microhardness of 6711 and 7775 alloys. Both al-
loy compositions consolidated in microwave furnace
resulted in lower electrical conductivity due to lower
density levels, inhomogeneous microstructure and larger
9 X-ray photoelectron spectroscopy analysis showing
effect of sintering atmosphere on surface composition
of 7775 microwave sintered compacts at 630uC
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 Padmavathi et al. Effect of atmosphere and heating mode on sintering of 6711 and 7775 alloys

10 Effect of heating mode and sintering atmopshere of 6711 and 7775 alloy compacts on a electrical conductivity and b
Vickers hardness

11 Tensile stressstrain curves for a 6711 and b 7775 alloy compacts sintered in conventional furnace under different
atmopsheres

porosity. The least conductivity was noticed in hydrogen
sintered compacts among all atmospheres in both
heating modes. Both alloys sintered in conventional
furnace under N2 resulted in higher conductivity which
can be correlated with again higher sintered density,
supersolidus liquid phase sintering microstructure, lesser
porosity and presence of conductive AlN. Also argon
resulted in marginally higher conductivity in case of
7775 alloy as compared with N2 atmosphere.
From Fig. 10b, it was noticed that all microwave
sintered compacts exhibited higher hardness and stan-
dard deviation values under all atmospheres, except for
vacuum. This enhancement may be correlated with the
presence of intermetallic phases/melt phase at grain
boundaries and microstructural inhomogeneity depend-
ing upon alloy composition. Vacuum sintering of 6711
alloys in conventional furnace exhibited higher hardness
and appreciable uniformity in VHN due to the presence
of equiaxed grains with uniformly distributed Mg2Si
precipitates. Owing to few technical limitations and
distortion occurring during microwave sintering, the
compacts could not be further characterised for com-
pression and tensile properties.
Figure 11a and b compares the tensile stressstrain
curves for 6711 and 7775 compacts sintered at 630uC
in conventional furnace under various atmospheres.

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 Padmavathi et al. Effect of atmosphere and heating mode on sintering of 6711 and 7775 alloys

12 Open corrosion potential and potentiodynamic polarisation curves of 6711 alloy consolidated at 630uC through a con-
ventional and b microwave sintering in various sintering atmospheres

Table 3 summarises the effect of sintering atmosphere
on various mechanical properties. It can be inferred
that vacuum sintering resulted in best combination of
mechanical properties for 6711 alloy (transverse rupture
strength: 276 MPa, ultimate tensile strength: 115 MPa
and yield strength: 100 MPa). This can be correlated
with greater densification response and presence of
Mg2Si precipitates. Nitrogen sintered compacts exhib-
ited ductility levels (23%) for 6711 compacts. Similarly,
N2 sintered 7775 compacts that also resulted in higher
strength (transverse rupture strength: 146 MPa, ultimate
tensile strength: 120 MPa and ductility: 6?4%) can be
again correlated with higher densification response. All
hydrogen sintered compacts exhibited poor mechanical
properties. Previous researchers4,5,8 have shown that H2
is deleterious to densification and mechanical properties.
The effects of heating mode and sintering atmosphere
on the corrosion behaviour of 6711 alloy are shown in

Table 3 Effect of sintering atmospheres on transverse rupture strength and tensile properties of 6711 and 7775
compacts sintered in conventional furnace

Sintering Transverse Ultimate

atmopshere/alloy rupture Yield tensile
composition strength/MPa strength/MPa strength/MPa Ductility/%

6711
Vacuum 276 100 115 19
Nitrogen 237 83 103 23
Argon 228 50 89 13
Hydrogen 157 27 65 8.4
7775
Nitrogen 146 101 120 6.4
Hydrogen 124 32 47 0.3

Table 4 Effect of sintering atmosphere and heating mode on corrosion parameters of 6711 alloy sintered at 630uC in
conventional and microwave furnaces

Sintering Corrosion rate/6

Heating mode atmosphere Ecorr/mV icorr/mA cm22 1023 mmpy

Conventional vacuum 2766 0.478 0.23

N2 2693 0.154 0.18
Ar 2845 2.040 22.32
H2 2935 4.350 45.78
Microwave vacuum 21230 7.540 82.57
N2 2874 0.083 0.91

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 Padmavathi et al.
Fig. 12a and b. Table 4 summarises the corrosion
parameters of sintered compacts. Vacuum sintering in
conventional furnace resulted in stabilisation at highest
corrosion potential (2447 mV) due to the formation of
most protective oxide/passive layer on surface shown in
Fig. 12a. Ar and H2 sintered compacts exhibited a
change of potential from nobler to active end due to the
dissolution of protective oxide layer. Among, microwave
sintered compacts under nitrogen resulted in higher
corrosion potential than vacuum. From potentiody-
namic polarisation curves, microwave sintering under
N2 and vacuum resulted in highest corrosion rates as
compared with conventional sintering. This may be
attributed to the microstructure coarsening, inhomo-
geneity within grains and larger melt phase at grain
boundaries, in spite of improved sintered density.
Among all atmospheres in conventional mode, nitrogen
exhibited the highest corrosion potential (2693 mV),
lowest corrosion current and least corrosion rates as
shown in Table 4. The higher corrosion resistance can
be correlated with higher density, lesser porosity and
grain refinement. The presence of intermetallic phase
(Mg2Si) seemed to have a negligible effect on electrode
potential.33 Argon and hydrogen sintered compacts
resulted in higher corrosion rates due to their lower
sintered density and poorly bonded microstructure.
Conclusions
Both 6711 and 7775 alloy compacts were micro-
wave sintered in significantly less time (5558%) when
compared with conventional sintering. Microwave sin-
tering resulted in poor densification, microstructural
inhomogeniety and absence/presence of small amount of
intermetallics phases for both compositions. The efficacy
of sintering atmosphere in terms of sintered density
for both heating modes increases in the order for
all compacts: H2RArRN2Rvacuum (highest). Overall,
nitrogen atmosphere seems to have most beneficial effect
on densification response and properties due to AlN
formation and as pore filling plays a major densifying
mechanism during both heating modes. All compacts
exhibited enhancement in electrical conductivity, micro-
hardness, tensile properties and corrosion resistance
(6711 only) under N2 during conventional sintering. This
may be attributed to better sintered density, grain
refinement, lesser porosity in supersolidus liquid phase
sintering microstructure and presence of intermetallics
phases. Hydrogen was found to be most detrimental for
densification behaviour and mechanical properties for
all sintered compacts due to their higher solubility in
liquid Al.
Acknowledgements
The authors would like to thank Mr Jessu Joys of
AMPAL Inc., Palmerton, USA for providing the 6711
and 7775 aluminium alloy powders for the present
study. This study was conducted under the Networked
Effect of atmosphere and heating mode on sintering of 6711 and 7775 alloys
Center for Microwave Processing of MetalCeramic
Composites funded by the IndoUS Science and
Technology Forum (IUSSTF), New Delhi, India.
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