materials

Article
Improving Performance of an Open Cell Aluminium
Foam through Electro-Deposition of Nickel
Silvio Genna * , Federica Trovalusci, Nadia Ucciardello and Vincenzo Tagliaferri
Department of Enterprise Engineering, University of Rome Tor Vergata, Via del Politecnico, 1, 00133 Rome, Italy;
federica.trovalusci@uniroma2.it (F.T.); nadia.ucciardello@uniroma2.it (N.U.); taglia@uniroma2.it (V.T.)
* Correspondence: silvio.genna@uniroma2.it




Received: 10 December 2018; Accepted: 26 December 2018; Published: 3 January 2019


Abstract: The aim of this work is to investigate the mechanical performances and corrosion
resistance of open-cell aluminium foams with an electroplated nickel coating. The influence
of two different electrolytic solutions on mechanical properties and corrosion resistance was
studied: The Watts solution (nickel sulphate-based solution) and a nickel sulphamate solution
(widely adopted). Scanning electron microscopy and stereoscopic analysis allowed for the estimation
of the coating uniformity and adhesion to the substrate. In order to assess the improvement of
performances, compression and corrosion tests were performed on coated and uncoated foams.
In addition, annealing was investigated in relation to different operational parameters, related both to
electro-deposition (electrolyte, deposition current and time) and to annealing (treatment temperature).
From the results, the yield stress and the corrosion resistance improved. Moreover, the annealing at
increasing temperature was found to reduce the yield stress, but Ni-coated foams showed higher
values of stress for all the considered treatment temperatures.

Keywords: aluminium foams; electro-deposition; annealing; compression test; corrosion test

1. Introduction
Metal foams are porous materials characterized by a complex 3D structure, which confers to
them interesting properties in terms of light weight, mechanical, thermal and acoustic performances.
In particular, metal foams are widely adopted because of their higher specific strength and stiffness,
as compared to monolithic equivalents. The characteristics of these porous materials make them
suitable for several industrial applications [1,2], from energy-absorbing systems [3] and fuel cells [4],
to cooling systems and heat exchangers [5–7]. In the latter case, open cell structures are used because
of their very high thermal conductivity. From numerical analysis, heat exchangers, based on metal
foams, are superior as compared to conventional finned exchangers at no excess cost [8]. Moreover,
by depositing appropriate coatings on the foam, it is possible to improve some properties, such as heat
exchange and energy absorption capacity. To produce more compact heat exchangers, heat exchange
capacity can be improved by using copper coated foams [9]. At the same time, this seems to be
a promising solution to increase absorption capacity. By comparing Cu-coated and uncoated aluminium
foams with the same overall thickness (i.e., same effective volume), the coated ones had double energy
absorption capacity [10]. Recently, electro deposition of copper on aluminium open cell foams was
studied, with the purpose to improve their thermal properties; moreover, an analytical model was
proposed to estimate the characteristics of the coating [11]. By applying this model, it was possible to
identify the optimal operational parameters to be used in electro-deposition.
The interest in copper deposition is also due to the fact that coppering can be used as the base for
further deposition of other materials, such as nickel [12].

Materials 2019, 12, 133; doi:10.3390/ma12010133 www.mdpi.com/journal/materials

Materials 2019, 12, 133 2 of 12

Recent studies showed that the electro-deposition of nickel determined an improvement in

mechanical properties of open cell aluminium foams [13,14]. Generally, metallic foams are mechanically
characterized by performing a uniaxial compression test [15–17], while in [13] an innovative
non-contact characterization procedure was defined to evaluate the mechanical performance of the
coated foams, with an increased strain measurement resolution.
In the scientific literature, few studies focus on nickel coated foams, the complexity of covering
the inner zone of cellular structures with this material [13] and their final properties [18–20].
However, they showed that the increase in density was related to the increase in mechanical properties.
Other studies [21,22] introduced an analysis that consider the relative properties of the deposited
material, and the beam-bending mechanics of how this influences the overall material behaviour.
Models were also developed to estimate the improvement in mechanical properties due to
the metallic coating [23,24]. They can be adopted to study the influence of the parameters on the
mechanical properties.
The aim of this work is to study the influence of two different electrolytic solutions on the
mechanical properties and corrosion resistance of an aluminium foam electro-deposited with nickel:
The Watts solution (i.e., a nickel sulphate-based solution, as adopted in [13]) and a nickel sulphamate
solution (widely adopted) [25]. For both deposition types, the influence of different electro-deposition
parameters, such as electrolyte, direct current and deposition time were changed and tested. The coating
uniformity and adhesion to the substrate were assessed by scanning electron microscopy and
stereoscopic analysis. In order to assess the improvement of performances, compression and corrosion
tests were performed on coated and uncoated foams. In addition, annealing was investigated in relation
to different operational parameters (electrolyte, deposition current and time), as high temperature
determines a microstructural variation of aluminium, as observed in [26].

2. Materials and Methods

2.1. Coatings Preparation

Parallelepiped samples, 20 × 20 mm2 in size and 30 mm in height, were obtained from the same
commercial panel of open cell foam (Duocel® by ERG Material, Oakland, CA, USA). It was made of
6101 T6 aluminium alloy and the number of pores per inches (PPI) was 10. This foam is fabricated by
the replication of polymeric pattern [1].
Aluminium foam substrates were coated via electro-deposition. An electrolytic cell at 25 ◦ C was
used. Two different electrolytic solutions were studied: the Watts solution (i.e., a nickel sulphate-based
solution) (NiSO4 ·6H2 O: 225 g/L; NiCl2 ·6H2 O: 30 g/L; H3 BO3 : 30 g/L), as adopted in [13], and a nickel
sulphamate solution (Ni(NH2 SO3 )2 ·4H2 O: 300 g/L; NiCl2 ·6H2 O: 30 g/L; H3 BO3 : 30 g/L), generally
adopted for the deposition of functional coatings or for electroforming [25].
The main issue with electro deposition of foams is with the penetration of the Ni ions into the
cellular structure, which is a very complex 3D structure, and; therefore, the obtaining of a very uniform
thickness of Ni on all the brackets of foams. In order to overcome this issue, a magnetic agitator,
working at 3 rpm, was used to keep in agitation the bath during the deposition. The consumable
anode was composed by four Ni plates, 40 × 40 × 3 mm3 in size, forming a hollow parallelepiped,
which surrounded the sample. The cathode was the foam and was connected to the current generator
and immersed in the electrolyte. Different values of operational parameters were considered: direct
current (DC) was set at 1, 1.5 and 2 A; deposition time ranged from 10 to 120 min. Such current values
were chosen on the basis of previous works [11,13] and on the basis of pre-tests, showing that the
further increase of current determined a lack of continuity of the coating.

2.2. Experimental Procedure

A characterization procedure was defined in this work with the aim to identify the effect of the
parameters, adopted during deposition or annealing, on the resulting foams. In particular, the thickness
Materials 2019, 12, 133 3 of 12

Materials 2019, 12, x FOR PEER REVIEW 3 of 12

and the adhesion of the coating were evaluated by scanning electron microscopy (FEG-SEM Leo
Supra 35, Zeiss, Oberkochen, Germany) and stereoscopic microscope (SMZ745T, Nikon, Düsseldorf,
SEM Leo Supra 35, Zeiss, Oberkochen, Germany) and stereoscopic microscope (SMZ745T, Nikon,
Germany). Both the external face and the interior of the foam were analysed.
Düsseldorf, Germany). Both the external face and the interior of the foam were analysed.
In the mechanical characterization tests, the compression of the foams was performed by
In the mechanical characterization tests, the compression of the foams was performed by a
a universal testing machine (Alliance RT 50, MTS, Berlin, Germany); the crosshead speed was
universal testing machine (Alliance RT 50, MTS, Berlin, Germany); the crosshead speed was 10
10 mm/min and the three zones of the stress-strain curves (initial elastic zone, plateau zone and
mm/min and the three zones of the stress-strain curves (initial elastic zone, plateau zone and failure
failure zone) were analysed [23]. Three replications were performed for each condition.
zone) were analysed [23]. Three replications were performed for each condition.
The effect of annealing on mechanical properties was also investigated. Annealing for 30 min at
The effect of annealing on mechanical properties was also investigated. Annealing for 30 min at
various temperatures, from 150 ◦ C up to 450 ◦ C, was performed in a convection oven, both on coated
various temperatures, from 150 °C up to 450 °C, was performed in a convection oven, both on coated
and uncoated foams for comparison.
and uncoated foams for comparison.
The comparison was in terms of yield stress, evaluated by performing compression tests in the
The comparison was in terms of yield stress, evaluated by performing compression tests in the
aforementioned conditions. Microstructural analysis of samples, after annealing tests, was performed
aforementioned conditions. Microstructural analysis of samples, after annealing tests, was performed
to verify the possible occurrence of defects.
to verify the possible occurrence of defects.
In addition, corrosion tests were performed on the samples to evaluate the protection offered
In addition, corrosion tests were performed on the samples to evaluate the protection offered by
by the Ni coating on the aluminium foam. In order to study the corrosion behaviour, the “VoltaLab”
the Ni coating on the aluminium foam. In order to study the corrosion behaviour, the “VoltaLab”
potentiostat (VoltaLab 80, Radiometer Analytical, Villeurbanne, France) was adopted to produce
potentiostat (VoltaLab 80, Radiometer Analytical, Villeurbanne, France) was adopted to produce the
the Tafel curves of the annealed samples. The auxiliary electrode, used for the test, was made in
Tafel curves of the annealed samples. The auxiliary electrode, used for the test, was made in platinum,
platinum, whereas the reference one was a saturated calomel electrode (SCE), according to the
whereas the reference one was a saturated calomel electrode (SCE), according to the schematic of
schematic of Figure 1. The corrosion resistance was evaluated in water solution with 3.5 wt. % of NaCl;
Figure 1. The corrosion resistance was evaluated in water solution with 3.5 wt. % of NaCl; before the
before the tests, the solution was degassed.
tests, the solution was degassed.

Figure 1. Schematic of the corrosion test.

Figure 1. Schematic of the corrosion test.
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3. Results and Discussion
3. Results and Discussion
The amount of deposited nickel (P%), calculated as the variation of the sample mass before and
after The
electro-deposition, was chosen
amount of deposited as thecalculated
nickel (P%), principal as
parameter for evaluating
the variation the mass
of the sample standard of and
before the
deposition process. It is awas
after electro-deposition, mass ratio and
chosen canprincipal
as the be expressed as a function
parameter of the molar
for evaluating mass of nickel
the standard of the
(MM Ni ) and the number of moles of deposited nickel (n Ni ):
deposition process. It is a mass ratio and can be expressed as a function of the molar mass of nickel
(𝑀𝑀 ) and the number of moles of deposited MM nickel ·(𝑛 ):
Ni n Ni
P% = 100 (1)
𝑀𝑀ρ·V∙ 𝑛
𝑃% = 100 (1)
𝜌∙𝑉
The reduction half-reaction that occurs at the cathode:
The reduction half-reaction that occurs at the cathode:
Ni2+ + 2e− → Ni0 (2)
(2)
𝑁𝑖 + 2𝑒 → 𝑁𝑖
suggests that,
suggests that,forforevery
every mole
mole of ion
of Ni Ni that
ion is
that is deposited,
deposited, two of
two moles moles of electrons
electrons are therefore,
are required; required;
therefore,
P% can be P% can be
written as:written as:
MM ·n −
P% = 𝑀𝑀 Ni∙ 𝑛 e ·100 (3)
𝑃% = ρ ·V ·2 ∙ 100 (3)
𝜌∙𝑉∙2
Being e the electric charge of electron, t the time, i the electric current and Na the Avogadro’s
Being
number, it ise possible
the electric charge the
to change of electron,
previous tequation,
the time,ini the electric with
agreement current and Na [11]:
Antenucci the Avogadro’s
number, it is possible to change the previous equation, in agreement with Antenucci [11]:
MM i ·t
P% = 𝑀𝑀 Ni · 𝑖 ∙ 𝑡 ·100 (4)
𝑃% = Na ·2·e ∙ ρ·V ∙ 100 (4)
𝑁 ∙2∙𝑒 𝜌∙𝑉
obtaining aa rearrangement
obtaining rearrangementofofthe theFaraday
Faradaylaw,law,
inin which
which thethe first
first fraction
fraction is aisconstant
a constant
andand assumes
assumes the
−3 A
the value 1.83 × 10 A min/kg.
value 1.83 × 10 −3 min/kg.
Equation (4)
Equation (4) shows
shows thethe relationship
relationship that
that exists
exists between
between P% P% andand the
the operational
operational parameters
parameters of of
the electro-deposition process. In particular, P% is directly proportional to current and time and
the electro-deposition process. In particular, P% is directly proportional to current and time and
inversely proportional
inversely proportional to to sample
sample mass.
mass. Attention
Attention must
must be be paid
paid toto the
the value
value assumed
assumed by by ρ,
ρ, that
that is
is not
not
constant and
constant and has
has to
to bebe calculated
calculated for
for each
each sample.
sample. Thus,
Thus, each
each sample
sample was was weighted
weighted before
before and
and after
after
electro-deposition, the
electro-deposition, the volume
volume waswas estimated
estimated andand then
then the
the density
density waswas calculated.
calculated.
In Figure
In Figure2,2,the
thepercentages
percentagesofofnickel
nickeldeposited
depositedP% P% asas a function
a function of of
thethe variable
variable term
term of Equation
of Equation (4)
(4)reported;
is is reported;thethe slopeofofthe
slope the linear
linear trend
trend (the
(thefirst
firstfraction
fraction of of
Equation
Equation (4))(4))
assumed
assumedthe value 1.8 ×
the value
−3 A min/kg regardless of the electrolyte, which was in good agreement to the calculated value.
10−3×A10min/kg
1.8 regardless of the electrolyte, which was in good agreement to the calculated value.
Thus, Equation
Thus, Equation (4)(4) accurately
accuratelypredicts
predictsthe
theamount
amountof of deposited
depositedNi. Ni. It
It is
is worth
worth noting
noting that
that the
the equation
equation
can be adopted in the case of an open cell foam, for both Ni sulphate and Ni sulphamate solutions.
can be adopted in the case of an open cell foam, for both Ni sulphate and Ni sulphamate solutions.

Figure 2.
Figure 2. Percentages of nickel
Percentages of nickel deposited
deposited P%
P% as
as aa function
function of
of the
the variable
variable term
term of
of Equation
Equation (4).
(4).
Materials 2019, 12, x FOR PEER REVIEW 5 of 12

Table 1 summarizes the values of density and the amount of nickel deposited (calculated by
Materials 2019, 12, 133 5 of 12
Equation (4)) achieved after electro-deposition at 1.5 A (intermediate level), according to the process
time; the initial density (i.e., the uncoated foam density) was 180 ± 20 kg/m3. Significant differences
between
Tablethe two adopted
1 summarizes thesolutions
values of(Ni sulphate/sulphamate)
density and the amount ofwere notdeposited
nickel observed.(calculated
The density by
increase was
Equation about 20 after
(4)) achieved kg/melectro-deposition
3 for the lower deposition time (10 min),level),
at 1.5 A (intermediate and about 230 to
according kg/m for the
the3 process
higherthe
time; time (120density
initial min). (i.e., the uncoated foam density) was 180 ± 20 kg/m3 . Significant differences
The the
between density of the foam
two adopted is strictly
solutions (Ni related to its mechanicalwere
sulphate/sulphamate) properties, the more
not observed. Thethe foam increase
density is dense
the more
was aboutit 20
is resistant
kg/m3 for[27].
the lower deposition time (10 min), and about 230 kg/m3 for the higher
time (120 min).
Table 1. The coated foam density and amount of nickel deposited at 1.5 A.
Table 1. The coated foam density and amount of nickel deposited at 1.5 A.
Nickel Sulphate Nickel Sulphamate
Deposition Time (min)
Final Density (kg/m3)
Nickel Sulphate P% Final Density (kg/m3)
Nickel Sulphamate P%
10
Deposition Time (min) 199 ± 10 10.88 201 ± 8 11.47
Final Density (kg/m3 ) P% Final Density (kg/m3 ) P%
20 205 ± 15 23.43 200 ± 19 23.72
30 10 258
199± ±
1810 30.59
10.88 201256
± 8± 11 11.4730.24
60 20 205± ±
292 1015 57.71
23.43 ± 19
200261 ± 21 23.7254.44
90 30 258 ±
356 ± 12 18 30.59
92.23 256 ± 11
358 ± 14 30.2490.72
60 292 ± 10 57.71 261 ± 21 54.44
120 422 ± 17 116.84 420 ± 28 117.49
90 356 ± 12 92.23 358 ± 14 90.72
120 422 ± 17 116.84 420 ± 28 117.49
The uniformity and the thickness of the electroplated coating were assessed by SEM and
stereoscopic analysis.
The density
Figure of the
3 shows thefoam is strictlyimages
stereoscopic relatedoftosamples
its mechanical
obtainedproperties, the more the
at the intermediate foam is dense
deposition time
the more it is resistant [27].
(60 min) and different DCs (1.0, 1.5, 2.0 A), for both the solutions. From the figure, the uniformity of
The uniformity
the covering layer of and theonthickness
nickel of the
the substrate waselectroplated
verified for coating
both thewerefaces,assessed
external byandSEM and
interior.
stereoscopic
However, this analysis.
observation is particularly useful for choosing the optimum value of direct current to
Figure
be adopted for 3 shows the stereoscopic images
Ni electro-deposition: for allofthe
samples
valuesobtained
of time,atby theincreasing
intermediate the deposition
intensity oftime the
(60 min) and different DCs (1.0, 1.5, 2.0 A), for both the solutions. From the figure,
current from 1 to 1.5 A, both the external face and the interior of the foam were covered in a better the uniformity
of thein
way, covering
fact, lowerlayerDCof did
nickel
noton the substrate
generate forces was
strongverified
enoughfortoboth the faces,
guarantee external
a correct and interior.
deposition, as
However, this observation is particularly useful for choosing the optimum value
found in [11,13]. On the other hand, a further increase (up to 2 A) determined a lack of continuity of direct current to be
of
adopted for Ni electro-deposition: for all the values of time, by increasing the intensity
the coating, as clearly visible in Figure 3, where small points were visible on the last pictures. This of the current
from 1 to 1.5 A,can
phenomenon both
be the external face
contributed andformation
to the the interior
of of the foambubbles
hydrogen were covered
over thein aexternal
better way, in fact,
surface of
lower DC
the foam. did not generate forces strong enough to guarantee a correct deposition, as found in [11,13].
On theTheother
samehand, a further increase
considerations (up toregardless
can be drawn 2 A) determined a lack of continuity
of the electrolyte. of thethe
For this reason, coating,
focus
as clearly visible in Figure 3, where small points were visible on the last pictures.
was mainly on the electro-deposition at 1.5 A, corresponding to the higher final density, with no This phenomenon
can be contributed
defects; the resulting to samples
the formation of hydrogenfor
were considered bubbles over the external
the subsequent mechanical surface
andof the foam.
corrosion tests.

Figure 3.
Figure 3. Images
Images ofof foams
foams after
after Ni
Ni electro-deposition
electro-deposition for
for 60
60 min
min and
and different
different DC
DC (1.0,
(1.0, 1.5
1.5 and
and 22 A):
A):
(a) internal
(a) internal part;
part; (b)
(b) external
external part.
part.

The same considerations can be drawn regardless of the electrolyte. For this reason, the focus was
mainly on the electro-deposition at 1.5 A, corresponding to the higher final density, with no defects;
the resulting samples were considered for the subsequent mechanical and corrosion tests.
 Materials 2019, 12, x FOR PEER REVIEW 6 of 12

Materials 2019, 12, 133 6 of 12

In Figure 4, the stereoscopic images of samples obtained at 1.5 A and different deposition times
(30, 60, 90
Materials min)
2019, are
12, x FORreported, for both the solutions. Similar to the effect of DC variation, a damaged
PEER REVIEW 6 of 12
coating was observable at the highest process time. Moreover, coatings obtained
In Figure 4, the stereoscopic images of samples obtained at 1.5 A and different deposition by using the
In Figure
sulphamate 4, the showed
solution stereoscopic
a images
greater of samples obtained
predisposition to the at 1.5 A and
formation of different
surface deposition
defects, and times
which
times (30, 60, 90 min) are reported, for both the solutions. Similar to the effect of DC variation,
(30, 60,
were 90 min) by
amplified are increasing
reported, fortheboth the solutions.
deposition time. Similar
From the to the effectthe
above, of DC
bestvariation, a damaged
electro-deposition
a damaged coating was observable at the highest process time. Moreover, coatings obtained by using
coating was observable at the highest process time. Moreover,
condition can be obtained at 1.5 A for 60 min, with the sulphate solution. coatings obtained by using the
thesulphamate
sulphamatesolution
solutionshowed
showeda agreater
greaterpredisposition
predisposition toto the
the formation
formation of of surface
surface defects,
defects, andand which
which
were amplified by increasing the deposition time. From the above, the best electro-deposition
were amplified by increasing the deposition time. From the above, the best electro-deposition condition
cancondition
be obtainedcan beat 1.5 A for at
obtained 601.5
min, with
A for 60the
min,sulphate
with thesolution.
sulphate solution.

Figure 4. Images of foams after Ni electro-deposition at 1.5 A and different deposition times: (a)
internal part; (b) external part.

InFigure
Figure order 4.toImages
4. Images assess ofif foams
of foams theafter
solution
after Nicould have an atinfluence
electro-deposition
Ni electro-deposition 1.5atA1.5
andAonandthedifferent
differentadhesion between
deposition
deposition theinternal
times:times:
(a) coating
(a)
andpart;
the substrate,
internal SEM
part; (b)
(b) external analysis
external
part. part.of the foams (electroplated at 1.5 A and 60 min) were performed. In
Figure 5 the images obtained by SEM are reported. From the images, the uniformity and good
In In
adhesion order
order toto
of the assessif ifalong
coatings
assess thesolution
the solution could
the section
could have
arehave anvisible,
clearly
an influence
influence for on
on the
both adhesion
the
the between
solutions.
adhesion between the coating
the coating
andand
the the
In substrate,
addition,
substrate, SEM
the
SEM Energyanalysis
analysis of
of the
thefoams
Dispersive (electroplated
Spectrometer
foams analysis
(electroplated at at
1.5
(EDSA and
1.5 AInca60300,
and min) werewere
60 Oxford
min) performed.
Instruments In
performed.
Figure
InLtd.,
Figure 5 the
Abingdon, images
5 the images obtained
UK) ofobtained by SEM
the foambyafterSEM are
Niare reported. From
electro-deposition
reported. Fromatthe the images,
1.5images, the
A and 60 uniformity
themin and
with the and
uniformity good
nickel
good
adhesion of of
sulphate-based
adhesion thethe coatingsalong
solution
coatings wasalong thesection
section
performed,
the are
asare clearlyinvisible,
reported
clearly visible,
Figure for6. both
for boththethesolutions.
solutions.
In addition, the Energy Dispersive Spectrometer analysis (EDS Inca 300, Oxford Instruments
Ltd., Abingdon, UK) of the foam after Ni electro-deposition at 1.5 A and 60 min with the nickel
sulphate-based solution was performed, as reported in Figure 6.

Figure5.5.SEM
Figure SEMimages
imagesofof foams
foams after
after Ni
Ni electro-deposition
electro-deposition at
at 1.5
1.5 A
Aand
and60 60min;
min;adhesion
adhesionand
andthickness
thickness of
of coating
the the coating
alongalong the section:
the section: (a) nickel
(a) nickel sulphate-based
sulphate-based solution;
solution; (b) nickel
(b) nickel sulphamate-based
sulphamate-based solution.
solution.
In Figure 5. SEM
addition, images
the of foams
Energy after Ni electro-deposition
Dispersive at 1.5 A and
Spectrometer analysis 60 min;
(EDS Incaadhesion and thickness
300, Oxford Instruments
of the coating
Ltd., Abingdon, UK)along the foam
of the section:after
(a) nickel sulphate-based solution;
Ni electro-deposition at 1.5(b)A nickel
and 60sulphamate-based
min with the nickel
solution.
sulphate-based solution was performed, as reported in Figure 6.
Materials 2019, 12, x FOR PEER REVIEW 7 of 12

Materials 2019, 12, 133 7 of 12

Materials 2019, 12, x FOR PEER REVIEW 7 of 12

Figure 6. EDS analysis of the foam after Ni electro-deposition at 1.5 A and 60 min with the nickel
sulphate-based solution.

In order to characterize the mechanical performance of the coated foams, compression tests were
performed.
Figure 6.Figure
Figure 6.
EDS EDS 7analysis
showsofof
analysis the
the typical
thefoam stress-strain
foamafter
after curves for at
Ni electro-deposition
Ni electro-deposition different
at 1.5
1.5AAand deposition
and 60
60min
minwith times
with the at
thenickel1.5 A for
nickel
the nickel sulphatesolution.
sulphate-based
sulphate-based solution.
solution. It is worth noting that the irregularities correspond to the progressive
initiation of plastic buckling of the brackets in the foam [28–30]. According to the scientific literature,
In order
threeIndifferent
order to
to zonescharacterize
characterize
can bethe themechanical
mechanical
identified: performance
first,performance
the elastic zone,of the
of coated
thethen
coated foams,
foams,compression
a plateau, compression
and last, the tests were
tests were
failure of
performed.
performed. Figure
Figure 7 7 showsthe
shows thetypical
typicalstress-strain
stress-strain curves
curves for for different
different deposition
deposition times
times atat1.51.5
AA forfor
the material. After the elastic zone, most of the samples show a drop in resistance; this trend has
thethe nickel
nickel sulphate
sulphate solution.ItItisisworth
solution. worthnoting
noting that that the
the irregularities
irregularities correspond
correspond totothe
theprogressive
progressive
already been verified in other works [18]. In the figure, the mechanical behaviour of the uncoated
initiation
initiation of of plastic
plastic buckling
buckling ofof the
the brackets
brackets in
in the
the foam
foam [28–30].
[28–30]. According
According to the
to thescientific
scientific literature,
literature,
aluminium foam (deposition time of 0 min) is compared to the performances exhibited by the coated
three different
three zones canbebeidentified:
identified:first,
first, the
the elastic
elastic zone,
zone, then aaplateau, and last,
last,the failure of of
ones, different
at increasing zones can
deposition times, using the nickel sulphate then
solution,plateau,
which and
seemed the
to failure
minimize
thethe material.
material. After
After the theelastic
elasticzone,
zone,most
mostof of thethe samples
samples show show aa dropdrop in
inresistance;
resistance; this
this trend
trend hashas
thealready
formation of surface defects. A sliding up of curves proportional
been verified in other works [18]. In the figure, the mechanical behaviour of the uncoated
to the deposition time, and thus
already
to the been verified
density,foamcan be in other
observed.time works [18].
Stiffness In
seemed the figure, the
to be unaffected mechanical behaviour
by the electro-deposition of the uncoated
aluminium (deposition of 0 min) is compared to the performances exhibited by the of nickel.
coated
aluminium
Onones, foam the
the contrary, (deposition
yield timewas
stress of 0clearly
min) isimproved.
compared to the performances exhibited by the coated
at increasing deposition times, using the nickel sulphate solution, which seemed to minimize
ones,Significant
at increasing deposition
differences intimes,
terms using the nickel behaviour
of mechanical sulphate solution,
under which seemed
compression loadto minimize
were
the formation of surface defects. A sliding up of curves proportional to the deposition time, and thusnot
the formation
observed using of surface
different defects. A
electrolytes, sliding
as up
suggestedof curves
by proportional
the comparison toofthe deposition
stress-strain time,
curves and
in thus
Figure
to the density, can be observed. Stiffness seemed to be unaffected by the electro-deposition of nickel.
to the
8. This density,
was can
expected, be observed. Stiffness seemed to be unaffected by the electro-deposition of nickel.
On the contrary, theas the stress
yield good was adhesion
clearlybetween
improved. the coating and the substrate was verified by the
On the contrary,
SEM analysis the
for both
Significant yield stress
the solutions.
differences was clearly improved.
in terms of mechanical behaviour under compression load were not
observed using different electrolytes, as suggested by the comparison of stress-strain curves in Figure
8. This was expected, as the good adhesion between the coating and the substrate was verified by the
SEM analysis for both the solutions.

Figure 7.
Figure 7. Compression
Compression test:
test: Typical
Typical stress-strain
stress-strain curves
curves for
for different
different deposition
deposition times
times at
at 1.5
1.5 A,
A, in
in the
the
nickel sulphate-based solution.
nickel sulphate-based solution.

Figure 7. Compression test: Typical stress-strain curves for different deposition times at 1.5 A, in the
Significant differences in terms of mechanical behaviour under compression load were not
nickel sulphate-based solution.
observed using different electrolytes, as suggested by the comparison of stress-strain curves in Figure 8.
Materials 2019, 12, x FOR PEER REVIEW 8 of 12
Materials 2019, 12, 133 8 of 12

This was expected, as the good adhesion between the coating and the substrate was verified by the
SEM analysis for both the solutions.
Materials 2019, 12, x FOR PEER REVIEW 8 of 12

Figure 8. Compression test: Comparison of stress-strain curves for different electrolytes at 1.5 A: (a)
60 min; (b) 90 min.

From the above, the coatings obtained by using the sulphamate solution showed a greater
predisposition to formation of surface defects, at the same time this electrolyte conferred to the foam
Figure 8.
mechanical
Figure 8.properties
Compression
Compression test:
test:Comparison
similar to the of
Comparison ofstress-strain
ones obtainable
stress-strain curves byforfor
curves different
sulphate electrolytes
different solution.
electrolytesatThus,
1.5 A: further
at 1.5 (a)
A:
60
(a) min;
60 (b)
min; 90
(b) min.
considerations were done referring to the electro-deposition by the sulphate solution.
90 min.
In the following, the compression tests after annealing are reported. In Figure 9, the mechanical
From the
From
behaviour the above,
of above,
aluminium the coatings
the coatings
foam and obtained
obtained by using
by
Ni-coated using the sulphamate
the
aluminium sulphamate
foams is solution
solution
reported showed
showed aa greater
greater
at increasing
predispositionof
predisposition
temperatures to annealing.
to formation of
formation ofThesurface
surface defects,
defects,
initial density at the
at wassame
the the time
same samethis
time forelectrolyte
this electrolyte conferredsamples.
conferred
all the compared to the foam
to the foam
As
mechanical
mechanical properties
properties similar
similar to to
the the
ones ones
obtainable obtainable
by sulphate by sulphate
solution.
expected, the yield stress was reduced after annealing at increasing temperature. Figure 10 allows a Thus,solution.
further Thus, further
considerations
considerations
were
clear done were
referring
comparison, done
it to the referring
suggests to yield
electro-deposition
that the the electro-deposition
by theofsulphate
stress by
the aluminium the sulphate
solution. foam at solution.
room temperature was
In
In the
the following,
following, the
the compression
compression tests
tests after
after annealing
annealing
close to 1.8 MPa, this value decreased with increasing temperatures of annealing up are
are reported.
reported. In
In Figure
Figure 9, the
9, the mechanical
mechanical
to 0.7 MPa (at
behaviour
behaviour of of aluminium
aluminium foam foam
and and
Ni-coatedNi-coated
aluminium aluminium
foams
450 °C). This was due to long treatment time or high treatment temperatures, which determinedis foams
reported isat reported
increasing at increasing
temperatures a
temperatures
of annealing. of
The annealing.
initial densityThe initial
was the density
same for was
all the
the same
compared for
microstructural variation of aluminium, in particular the increase of the grain size, as known in the all the
samples. compared
As expected, samples.
the As
yield
expected,
stress the yield [31].
wasliterature
scientific reduced stress was reduced
after annealing after annealing
at increasing at increasing
temperature. Figure temperature.
10 allows a Figure 10 allows a
clear comparison,
clear
it comparison,
suggests that the it suggests
yield stress that
of the
the yield stress
aluminium of
foamthe aluminium
at room
The results are summarized in Table 2: Ni-coated foams showed higher values of stress foam
temperature at room
was temperature
close to 1.8forwas
MPa,
all
close
this to
value 1.8 MPa,
decreased this value
with decreased
increasing with
temperaturesincreasing
of temperatures
annealing
the considered temperatures of annealing. This fundamental aspect means that Ni-coated foamsup to 0.7of annealing
MPa (at 450 up to 0.7 MPa
◦ C). This was due
(at
450long
to
could°C). This wastime
treatment
also be used due
afterorto longtreatment
high
exposure treatment timetemperature,
or high which
temperatures,
to elevated treatment temperatures,
determined
whereas aluminium whichdo
a microstructural
foams determined
providea
notvariation
microstructural
of aluminium, in variation
particular
adequate mechanical properties. of aluminium,
the increase in
of particular
the grain the
size, asincrease
known of
in the
the grain size,
scientific as known
literature in the
[31].
scientific literature [31].
The results are summarized in Table 2: Ni-coated foams showed higher values of stress for all
the considered temperatures of annealing. This fundamental aspect means that Ni-coated foams
could also be used after exposure to elevated temperature, whereas aluminium foams do not provide
adequate mechanical properties.

Figure 9.
Figure 9. Compression test: Stress-strain
Compression test: Stress-strain curves
curves after
after annealing
annealing at
at different temperature, (a)
different temperature, (a) uncoated
uncoated
foams; (b)
foams; (b) Ni-coated
Ni-coated foams
foams (nickel
(nickel sulphate
sulphate solution).
solution).

Figure 9. Compression test: Stress-strain curves after annealing at different temperature, (a) uncoated
foams; (b) Ni-coated foams (nickel sulphate solution).

Figure10.
Figure 10.Compression
Compressiontest:
test:Stress-strain
Stress-straincurves
curves at
at (a)
(a) 25
25 ◦°C;
C; after
after annealing
annealing at
at (b)
(b)300
300°C;
◦ C;(c)
(c)450
450°C.
◦ C.

The results are summarized in Table 2: Ni-coated foams showed higher values of stress for all the
considered temperatures of annealing. This fundamental aspect means that Ni-coated foams could also

Figure 10. Compression test: Stress-strain curves at (a) 25 °C; after annealing at (b) 300 °C; (c) 450 °C.
Materials 2019, 12, 133 9 of 12

be used after exposure to elevated temperature, whereas aluminium foams do not provide adequate
mechanical properties.
Materials 2019, 12, x FOR PEER REVIEW 9 of 12
Table 2. Compression test: Maximum stress in the range 0–0.1 mm−1 strain and plateau length
Table
after 2. Compression test: Maximum stress in the range 0–0.1 mm−1 strain and plateau length after
annealing.
annealing.
Annealing Temperature Plateau Length (mm) Maximum Stress (MPa)
Annealing(◦Temperature
C) Plateau
Aluminium FoamLength (mm) Foam
Ni-Coated Aluminium Foam Stress
Maximum (MPa) Foam
Ni-Coated
(°C) Aluminium Foam Ni-Coated Foam Aluminium Foam Ni-Coated Foam
25 0.26 0.37 1.72 3.88
25
150 0.26
0.31 0.37
0.39 1.72
1.61 3.88
3.72
150
200 0.31
0.35 0.39
0.41 1.61
1.21 3.72
3.75
200
300 0.35
0.35 0.41
0.38 1.21
1.16 3.75
2.87
300
400 0.35
0.38 0.38
0.39 1.16
0.89 2.87
2.15
400
450 0.38
0.37 0.39
0.40 0.89
0.69 2.15
1.63
450 0.37 0.40 0.69 1.63

In addition, SEM analysis was performed to establish the maximum temperature that did not cause
In addition, SEM analysis was performed to establish the maximum temperature that did not
defects. It was found that the annealing treatment at 300 ◦ C determined porosity inside the aluminium
cause defects. It was found that the annealing treatment at 300 °C determined porosity inside the
(red circle in Figure 11a), which could reduce the mechanical strength of the aluminium foam.
aluminium (red circle in Figure 11a), which could reduce the mechanical strength of the aluminium
This degradation
foam. did not occur
This degradation did not at temperatures
occur at temperatures 300 ◦ C
lower thanlower (Figure
than 300 11b). These 11b).
°C (Figure observations
These
agree with the results of mechanical characterization, which showed significant reduction
observations agree with the results of mechanical characterization, which showed significant of mechanical
performances after annealing
reduction of mechanical performed
performances at annealing
after temperatures higher at
performed than 300 ◦ C. However,
temperatures as visible
higher than 300 °C.in
Figure 10a, the coating was still adherent to the substrate at a high temperature.
However, as visible in Figure 10a, the coating was still adherent to the substrate at a high temperature.

Figure11.
Figure 11.SEM
SEMimages
images of
of Ni-coated
Ni-coated foams
foams after
after annealing
annealing at:
at:(a)
(a)300
300°C;
◦ C;(b)
(b)150
150°C.
◦ C.

Basedonon
Based thethe discussed
discussed results,
results, the improvement
the improvement of properties
of properties achieved
achieved by the electro-
by the electro-deposition
ofdeposition
nickel wasofassessed.
nickel was assessed.
In fact, In fact,
regardless regardless conditions,
of annealing of annealing conditions,
Ni-coated foamsNi-coated
showedfoams
higher
showed higher
performance thanperformance
aluminium than
foamsaluminium foams alsotoafter
also after exposure highexposure to high
temperature, up temperature,
to 450 ◦ C. up to
450 In
°C.addition, corrosion tests were performed on the samples to evaluate the protection offered by
the NiIn addition,
coating on corrosion tests were
the aluminium foam performed on the
at increasing samples temperatures.
annealing to evaluate the The
protection
resultsoffered by
are shown
inthe Ni coating
Table on the12.
3 and Figure aluminium foam at increasing annealing temperatures. The results are shown
in Table 3 and Figure 12.
Table 3. Corrosion test: Tafel current of uncoated and coated samples.
Table 3. Corrosion test: Tafel current of uncoated and coated samples.
Annealing Temperature (◦ C) I (mA/cm2 ) Sample
Annealing Temperature (°C) I (mA/cm2) Sample
- - 0.101 ± 0.04
0.101 ± 0.04uncoated uncoated
25 25 0.278 ± 0.07
0.278 ± 0.07
150 150 0.238 ± 0.09
0.238 ± 0.09
200 200 0.665 ± 0.08 coated
0.665 ± 0.08
300 0.852 ± 0.05 coated
300 0.852 ± 0.05
400 400 0.683 ± 0.07
0.683 ± 0.07
450
450 0.149 ± 0.09
0.149 ± 0.09
Materials 2019, 12, 133 10 of 12
Materials 2019, 12, x FOR PEER REVIEW 10 of 12

Figure 12.
Figure 12. Tafel
Tafel curves
curves of
of uncoated
uncoated and
and coated
coated samples.
samples.

From
Fromthe
theanalysis
analysisofofFigure
Figure12,
12,the
theimprovement
improvementonon corrosion
corrosionresistance, of of
resistance, thethe
coated samples
coated as
samples
compared to the uncoated sample, is clearly visible.
as compared to the uncoated sample, is clearly visible.
From
From the above, the
the above, the NiNi coating
coatingimproved
improvedthe themechanical
mechanicaland and corrosion
corrosion performance
performance of
of an
an aluminium
aluminium open
open cell,
cell, evenatathigh
even hightemperatures,
temperatures,allowing
allowingfor
for their
their adoption,
adoption, whereas
whereas uncoated
uncoated
aluminium foams did not provide an adequate mechanical (and corrosion)
aluminium foams did not provide an adequate mechanical (and corrosion) performance. performance.

4. Conclusions
4. Conclusions
The present work investigated the mechanical performances and corrosion resistance of open-cell
The present work investigated the mechanical performances and corrosion resistance of open-
aluminium foams with an electroplated nickel coating. Two different electrolytic solutions were
cell aluminium foams with an electroplated nickel coating. Two different electrolytic solutions were
indagated to obtain the coatings: The Watts solution (nickel sulphate-based solution) and a nickel
indagated to obtain the coatings: The Watts solution (nickel sulphate-based solution) and a nickel
sulphamate solution (widely adopted). Scanning electron microscopy and stereoscopic analysis was
sulphamate solution (widely adopted). Scanning electron microscopy and stereoscopic analysis was
used to estimate the coating uniformity and adhesion to the substrate. The evaluation of properties of
used to estimate the coating uniformity and adhesion to the substrate. The evaluation of properties
the resulting foams was based on compression and corrosion tests. Based on the experimental results,
of the resulting foams was based on compression and corrosion tests. Based on the experimental
within the checked values, the following conclusions can be drawn:
results, within the checked values, the following conclusions can be drawn:
(1) Both the external face and the interior of the foams were correctly coated by adopting a DC of
(1) Both the external face and the interior of the foams were correctly coated by adopting a DC of
1.5 A, which prevented the formation of hydrogen bubbles over the external surface of the foams;
1.5 A, which prevented the formation of hydrogen bubbles over the external surface of the foams;
(2) The sulphamate solution (i.e., the widely adopted one) showed a higher predisposition to the
(2) The sulphamate solution (i.e., the widely adopted one) showed a higher predisposition to the
formation of hydrogen gas and; therefore, of surface defects on the foam;
formation of hydrogen gas and; therefore, of surface defects on the foam;
(3) The optimal
(3) The optimalduration
durationof deposition
of depositionwas 60wasmin;
60which
min; allowed for a homogenous
which allowed and satisfactory
for a homogenous and
covering of samples to be obtained with the considered shape and dimensions;
satisfactory covering of samples to be obtained with the considered shape and dimensions;
(4) The amounts
(4) The amounts of of nickel
nickel deposited
deposited on on the
the specimens
specimens was was almost
almost the
the same
same for
for the
the two
two solutions;
solutions;
(5) Mechanical properties of coated foams were similar, regardless of the electrolyte;
(5) Mechanical properties of coated foams were similar, regardless of the electrolyte;
(6) The coating
(6) coatingimproved
improved thethe yield,
yield, whereas
whereas the stiffness
the stiffness was tofound
was found to be unaffected
be unaffected by the
by the deposition
deposition of Ni;
of Ni;
(7) The
(7) yield stress
The yield stress was
was reduced
reduced after
after annealing
annealing at at increasing
increasing temperature,
temperature, but
but Ni-coated
Ni-coated foams
foams
showed higher values of stress for all the considered temperatures;
showed higher values of stress for all the considered temperatures;
(8) The
(8) The Ni
Ni coating allowed aa higher
coating allowed higher corrosion
corrosion current,
current, even
even at
at high
high temperatures.
temperatures.

Author Contributions: S.G. and N.U. conceived and designed the experiments; N.U. realized and provided the
Author Contributions: S.G. and N.U. conceived and designed the experiments; N.U. realized and provided the
samples; F.T.
samples; F.T.performed
performedthe
theexperiments;
experiments;V.T.,
V.T.,S.G.
S.G.and
andN.U.
N.U.analysed
analysedthe
thedata;
data;F.T.
F.T. and
and S.G.
S.G. wrote
wrote thethe paper.
paper.
Funding: This research received no external funding.
Materials 2019, 12, 133 11 of 12

Funding: This research received no external funding.

Conflicts of Interest: The authors declare no conflict of interest.

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