5.3 7.

Article

Effect of Nanocarbon on the

Structural and Mechanical
Properties of 6061 Aluminum
Composites by Powder Metallurgy

Wilson Rativa-Parada, Hansika I. Sirikumara, Robinson Karunanithy, Poopalasingam Sivakumar,

Thushari Jayasekera and Sabrina Nilufar

Special Issue
Aluminum Based Nanocomposite and Nanostructured Alloys
Edited by
Dr. Syed Fida Hassan

https://doi.org/10.3390/nano13222917
 nanomaterials

Article
Effect of Nanocarbon on the Structural and Mechanical
Properties of 6061 Aluminum Composites by
Powder Metallurgy
Wilson Rativa-Parada 1 , Hansika I. Sirikumara 2 , Robinson Karunanithy 3 , Poopalasingam Sivakumar 3 ,
Thushari Jayasekera 3 and Sabrina Nilufar 1, *

1 School of Mechanical, Aerospace, and Materials Engineering, Southern Illinois University,

Carbondale, IL 62901, USA
2 E. S. Witchger School of Engineering, Marian University, Indianapolis, IN 46222, USA;
hsirikumara@marian.edu
3 School of Physics and Applied Physics, Southern Illinois University, Carbondale, IL 62901, USA;
robinson.karunanithy@siu.edu (R.K.); thushari@siu.edu (T.J.)
* Correspondence: sabrina.nilufar@siu.edu

Abstract: 6061 aluminum composites with 0.5 and 1 vol. % graphene nanoplatelets as well as 1 and
2 vol. % activated nanocarbon were manufactured by a powder metallurgy method. Scanning
electron microscopy and Raman spectroscopy were used to study the morphology, structure, and
distribution of nanocarbon reinforcements in the composite samples. Density Functional Theory
(DFT) calculations were performed to understand the aluminum-carbon bonding and the effects of
hybridized networks of carbon atoms on nanocarbon aluminum matrix composites. Scanning electron
microscopy showed the good distribution and low agglomeration tendencies of nanoparticles in the
composites. The formation of secondary phases at the materials interface was not detected in the
hot-pressed composites. Raman spectroscopy showed structural changes in the reinforced composites
after the manufacturing process. The results from Density Functional Theory calculations suggest
that it is thermodynamically possible to form carbon rings in the aluminum matrix, which may be
Citation: Rativa-Parada, W.; responsible for the improved mechanical strength. Our results also suggest that these carbon networks
Sirikumara, H.I.; Karunanithy, R.; are graphene-like, which also agrees with the Raman spectroscopy data. Micro-Vickers hardness
Sivakumar, P.; Jayasekera, T.; Nilufar, and compressive tests were used to determine the mechanical properties of the samples. Composites
S. Effect of Nanocarbon on the presented enhanced hardness, yield and ultimate strength compared to the 6061 aluminum alloy with
Structural and Mechanical Properties no nanocarbon reinforcement. Ductility was also affected, as shown by the reduction in elongation
of 6061 Aluminum Composites by
and by the number of dimples in the fractured surfaces of the materials.
Powder Metallurgy. Nanomaterials
2023, 13, 2917. https://doi.org/
Keywords: nanocarbon–aluminum composites; graphene nanoplatelets; activated nanocarbon;
10.3390/nano13222917
micro-Vickers hardness
Academic Editor: Syed Fida Hassan

Received: 11 October 2023

Revised: 1 November 2023
1. Introduction
Accepted: 3 November 2023
Published: 8 November 2023 Aluminum matrix composites (AMCs) have been extensively investigated in the last
few decades owing to the increasing demand for stronger and more lightweight materials
for the automobile, electronic, and aerospace industries [1–6]. AMCs have been produced
using different manufacturing processes such as powder metallurgy, spark plasma sintering,
Copyright: © 2023 by the authors. stir casting, friction stir processing, and severe plastic deformation [7,8]. However, several
Licensee MDPI, Basel, Switzerland. factors, such as the poor dispersion of reinforcement and weak interfacial bonding, can
This article is an open access article deteriorate the properties of these composites [9]. Powder metallurgy is a simple and
distributed under the terms and
low-cost method that has shown effectiveness in homogenously dispersing reinforcements
conditions of the Creative Commons
in the aluminum matrix with enhanced mechanical properties [10,11]. Within the powder
Attribution (CC BY) license (https://
metallurgy process, ball milling has been widely utilized as the procedure to mix and
creativecommons.org/licenses/by/
disperse the reinforcement due to its simplicity and scalability. The properties of AMCs
4.0/).

Nanomaterials 2023, 13, 2917. https://doi.org/10.3390/nano13222917 https://www.mdpi.com/journal/nanomaterials

Nanomaterials 2023, 13, 2917 2 of 14

depend on the duration and speed of milling, as well as the sintering and consolidation
of the composites. The influence of these parameters has been investigated in the last
few years, showing that excessive ball milling can also alter the structures of the milled
materials [12]. Particularly, the consolidation step influences the densification and the
formation of undesirable phases, such as Al4 C3 , which is highly influenced by temperature
and time [13].
Besides this, materials used as reinforcement play a key role in AMCs. Historically,
silicon carbide (SiC) [14], aluminum oxide (Al2 O3 ) [15], and titanium carbide (TiC) [16]
have been the conventional materials used in AMCs. However, persistent issues related
to weak interfacial bonding and poor dispersion limit their use. For this reason, some
alternative reinforcements of AMCs have been investigated with remarkable findings.
Recently, Fuse et al. utilized stir processing to form boron carbide (B4 C)-6061 aluminum
composites that presented the uniform dispersion of B4 C with enhanced hardness and
wear resistance [17]. Desai et al. [18] also obtained fly ash (0 to 25 wt. %)-reinforced AMCs
with enhanced wear behavior, hardness, and tensile strength. Likewise, titanium diboride
(TiB2 ) has been used in 6061 aluminum matrix composites. Pazhouhanfar et al. reinforced
6061 matrix composites with several amounts of TiB2 and tested their mechanical properties.
The results showed that the ultimate strength rose as a function of the volume fraction
of the reinforcement without significant loss of elongation, which was mainly attributed
to load transfer, grain size reduction, and Orowan mechanisms [19]. Moreover, Cham-
roune et al. [20] employed graphite flakes as reinforcement in AMCs by powder metallurgy,
which increased the anisotropic thermal properties due to the preferred orientation of the
graphite flakes and deformations at the interface.
Within the variety of materials studied to reinforce AMCs, carbon allotropes have
drawn the attention of researchers due to their excellent chemical, physical, and mechanical
properties [21–24]. The most common allotropes of carbon include fullerene, nanodia-
mond, carbon nanotubes, graphene, and activated carbon. Graphene, a 2-dimensional
arrangement of sp2 hybridized carbon with outstanding surface, electrical, thermal, and
mechanical properties, has excelled as a reinforcement for AMCs [25–29]. The load transfer
mechanism between aluminum and graphene is superior to that of aluminum with other
sp2 hybridized carbons such as nanotubes and fullerenes, due to a better interface made
of planar graphene and aluminum [30]. Nevertheless, graphene presents some challenges
related to agglomeration and dispersion in the AMCs [31]. Activated carbon is another
carbon allotrope with excellent surface properties [32] and has been employed in metal
matrix composites as a source of carbides [33], graphene [34], and as a reinforcement for
AMCs [35] with remarkable results.
This work focused on determining the influence of the synthesis parameters as well
as the effects of the type of nanocarbon reinforcements, such as activated nanocarbon and
graphene nanoplatelets, on the structure and performance of as-sintered 6061 aluminum
matrix composites. The structural and mechanical properties were determined with Scan-
ning Electron Microscopy (SEM), Raman Spectroscopy, Uniaxial Compression Testing, and
micro-Vickers hardness. DFT calculations were performed to elucidate the atomic scale
phenomena behind the carbon-aluminum interactions. The effects of the volume fraction of
activated nanocarbon and graphene nanoplatelets on the behavior of the as-sintered AMCs
were also discussed.

2. Materials and Methods

2.1. Composite Preparation
Both activated nanocarbon 6061 aluminum and graphene 6061 aluminum composites
were fabricated by a powder metallurgy method. 6061 aluminum powders (Al: 95.8–98.6%.
Chromium: 0.07%. Copper: 0.27%. Iron: 0.17%. Manganese: 0.01%. Magnesium: 0.86%.
Silicon: 0.58%. Zirconium: <0.01%. Titanium: 0.02%. Others: <0.15%) were acquired from
Valimet, Inc. (Stockton, CA, USA). At the same time, both nanocarbon powders, i.e., ac-
tivated nanocarbon (<100 nm; 95%) and graphene nanoplatelets (99.5%), were acquired
Nanomaterials 2023, 13, 2917 3 of 14

from US Research Nanomaterials, Inc. (Houston, TX, USA). A SPEX 8000 mixer from SPEX
SamplePrep (Metuchen, NJ, USA) with a motor speed of 1450 rpm was utilized for milling
the composites. Corresponding amounts of activated nanocarbon/graphene nanoplatelets
and 6061 aluminum powders were mechanically mixed for 4 h within intervals of 30 min
of milling with pauses of 30 min to maintain low-temperature conditions. This was done
in a stainless steel jar using 5 mm steel balls in a 10:1 ratio and 1 wt. % of stearic acid
(CH3 (CH2 )16 COOH) from Sigma Aldrich (95%) as a lubricant agent. Before pressing, the
stearic acid was evaporated for 30 min at 450 ◦ C. Hot isostatic pressing was used to consoli-
date the previously milled powder composites with diverse volume fractions of nanocarbon
reinforcement. The mixture was placed in a graphite die equipped with graphite punches
of 25.4 mm in diameter and pressed for 1 h at 550 ◦ C and 70 MPa under vacuum conditions
in a Front-Loading Hot Press Furnace from Materials Research Furnaces LLC (Allenstown,
NH, USA). The denomination of the final materials is shown in Table 1.

Table 1. Denomination of the samples prepared for this study.

Denomination Description
6061 6061 aluminum without any reinforcement
61Ac1 6061 aluminum reinforced with 1 vol. % of activated nanocarbon
61Ac2 6061 aluminum reinforced with 2 vol. % of activated nanocarbon
61Gn0.5 6061 aluminum reinforced with 0.5 vol. % of graphene nanoplatelets
61Gn1 6061 aluminum reinforced with 1 vol. % of graphene nanoplatelets

2.2. Structural Characterization

The surfaces of the as-sintered composite samples were ground with several abrasive
papers (80, 120, 220, 320, 400, 600, 800, and 1200) and then polished with a soft cloth and a
polishing suspension (sol-gel alumina). Both sintered and fractured morphologies were
observed with a Quanta FEG 450 Scanning Electron Microscope equipped with energy-
dispersive X-ray spectroscopy by Oxford Instruments (Concord, MA, USA). Samples were
sputtered with an alloy of Au-Pt to enhance the definition of the images. The structures of
the reinforcement materials were investigated using a Horiba iHR550 by Horiba Scientific
(Irvine, CA, USA) imaging spectrometer in conjunction with a BX 41 microscope by Olym-
pus (Center Valley, PA, USA) with 10×, 20×, 50×, and 100× magnification objectives and a
near-infrared (NIR) excitation light source of 785 nm iBeam-Smalt-785-S-WS by TOPTICA
Photonics (Pittsford, NY, USA). A grating of 600 gr/mm was used in the spectrometer. For
the powder samples, a 10× object with 10 mW laser power was used to avoid burning the
samples. For the compacted samples, the spectra were collected using the 10× objective at
120 mW laser power with a 15 s acquisition time and with a total of 10 scans over the desired
range. In addition, bulk density was calculated by following the Archimedes principle.

2.3. Computational Calculations

Density Functional Theory calculations were carried out to understand the aluminum-
carbon (Al-C) bonding and the effect of hybridized networks of C atoms in the Al matrix.
Previous studies have investigated interfacial interactions between epitaxial graphene on
the Al surface [36]. In this study, a network of C atoms sandwiched in a matrix of aluminum
was considered. The model consists of a 2 × 2 × 4 Al structure and a C layer with 21 carbon
atoms in the direction (100). The calculation cell has a dimension of 8.1 Å in the x and y
directions and 18.8 Å in the z direction. In its pristine form, the 2 × 2 × 4 supercell of Al
has a periodic length of 16.2 Å in the z-direction. All the atomic coordinates and the cell
dimension in the z direction are elongated to insert the layer of carbon and the z dimension
is fully optimized to minimize the force to 0.02 eV/Å. All energies were calculated using the
ab initio Density Functional Theory implemented in the Quantum Espresso package [37].
Nanomaterials 2023, 13, 2917 4 of 14
𝐸 =𝐸 −𝐸 −𝐸
𝐸
The formation energy of the network of C atoms sandwiched𝐸 in the Al matrix was evaluated
𝐸
by Equation (1):
E f = E AlC − E Al − EC (1)
where E AlC is the total energy of the Al/C system, E Al is the total energy of the Al ma-
trix, and EC is the total energy of the C layer. Additionally, we calculated the phonon
frequency of the Al/C system at the Gamma point, as it is implemented in the quantum
espresso package.

2.4. Mechanical Testing

A micro-Vickers hardness tester HMV-G 31 DT from Shimadzu Scientific Instruments,
Inc. (Pittsburgh, PA, USA) was used to obtain the hardness of the materials by following
the ASTM E384 standard [38]. A load of 1.961 N was employed for all the measurements,
and a total of 5 measurements per sample were taken at distinct locations using a square
pyramidal indenter. Uniaxial compressive tests were performed according to the ASTM
E9 standard [39] at room temperature in an MTS Insight 30 kN Standard Length testing
machine employing rectangular samples with a 2:1 length/width ratio. A total of 3 tests
were carried out for each composition. Yield strength was calculated by using the 0.2%
offset method. Ultimate strength, modulus of toughness, and elongation were determined
from average values obtained from the stress-strain diagrams.

3. Results and Discussion

3.1. Structural Characterization
Figure 1 displays the as-received powders of activated nanocarbon and graphene
nanoplatelets, along with the morphology and size distribution of the 6061 aluminum
alloy powders. The structure and distribution of activated nanocarbon and graphene
nanoplatelets inside the as-sintered 6061 aluminum matrix with no evidence of a large-scale
agglomeration are displayed in Figure 2, along with the EDS elemental mapping with the
distribution for aluminum (Al) and carbon (C).

Figure 1. Morphology of the as-received (a) activated nanocarbon, (b) graphene nanoplatelets and
(c) 6061 aluminum powders, and (d) size distribution of 6061 aluminum powders.
Nanomaterials 2023, 13, 2917 5 of 14

Figure 2. Morphology of the nanocarbon 6061 AMCs with EDS elemental mapping for aluminum
(Al) and carbon (C).

Figure 3 presents the micrographs of the materials at the interface. According to

SEM studies, the formation of intermediate phases such as Al4 C3 at the carbon-aluminum
interface during the synthesis of the composites was not evident. This suggests that the
change in properties cannot be attributed to the inclusion of secondary phases at the
tt
interface but to the strengthening mechanisms between the matrix and reinforcement,
including load transfer [40], thermal expansion mismatch [41], and Orowan Looping [42].
Nanomaterials 2023, 13, 2917 6 of 14

Figure 3. Nanocarbon-6061 aluminum interface of the nanocarbon 6061 aluminum composites

(a) 61Gn0.5, (b) 61Gn1, (c) 61Ac1, and (d) 61Ac2.

Raman characterization of the nanocarbon aluminum 6061 composites after milling

and compression is shown in Figure 4a,b, and Table 2. The spectra for activated nanocarbon
and graphene nanoplatelets display two peaks at 1350 and 1580 cm−1−, corresponding
to the D and G bands, respectively [43]. No peak corresponding to aluminum carbide
(~850 cm− − 1 [44]) can be observed, which supports the SEM-EDS results shown above. The

intensity of these peaks changes for the finalized composites compared to the initial materi-
als, especially for the graphene nanoplatelets due to the structural changes sufferedffafter
the manufacturing process. This is confirmed by determining the intensity ratio between
the D and G bands. The ID /IG ratio for as-received activated nanocarbon and graphene
nanoplatelets are 1.50 and 0.26, respectively. After that, the ID /IG ratio changed to 1.65 and
1.27 for the milled activated nanocarbon and graphene, respectively, due to the increasing
degree of disorder in the sp2 structures of the nanocarbon reinforcements [45]. This follows
previous tendencies in which the increasing milling time accelerated the formation of de-
fects and disorder in the graphene structure of reinforced 6061 aluminum composites [46].
Similarly, the ID /IG ratio continued decreasing after the compression procedure, although
to a smaller degree. The crystallite sizes (Cs) for activated nanocarbon and graphene before
and after the milling process are also determined with Equation (2) [47], showing that
the crystallite sizes for both reinforcements increased with the increasing of defects in the
structure, this value being higher for the activated nanocarbon-reinforced samples:

2.4 × 10−10 × λlaser 4

Cs : (2)
2.4 × 10ID /IG × 𝜆
𝐶𝑠:
𝐼 ⁄𝐼
Table 2. ID /IG ratio and crystallite size of the reinforcements in the nanocarbon 6061 AMCs after
milling and compression procedures.

Graphene Nanoplatelets Activated Nanocarbon 61Ac1 61Gn1

ID /IG ratio 0.26 1.50 1.65 1.67
Milled
Crystallite Size (nm) 345.47 60.43 71.64 54.94
ID /IG ratio - - 1.11 1.33
Compacted
Crystallite Size (nm) - - 81.84 68.46
Nanomaterials 2023, 13, 2917 7 of 14

Figure 4. (a) Raman spectra of the nanocarbon 6061 AMCs after milling, (b) Raman spectra of the
nanocarbon 6061 AMCs after compression, (c) side view, and (d) top view of atomic displacement
pattern (shown in red) for the softest phonon frequency 1360 cm−−1 for the atomistic model used for
tt
this calculation.

In addition to the microstructural analysis of the experimentally sintered compos-

ites, Density Functional Theory (DFT) calculations are shown in Figure 4c,d. There, the
optimized structure, along with the atomic displacements corresponding to the highest
phonon frequencies, is presented. When comparing the density of carbon atoms in pris-
tine graphene, this model has 97% carbon coverage. This particular configuration has
six-member carbon rings in the presence of defects. In a previous article, it was shown
that the C rings in an Al matrix are energetically more favorable than isolated C atoms
in an Al matrix [48]. The formation energy calculations show that the C layer in the Al
matrix has a formation energy of −0.14 eV/atom, which shows that the sp2 hybridized C
layer is thermodynamically − stable. Phonon frequencies were calculated as implemented in
the Quantum Espresso package. Non-negative frequencies for the gamma point phonons
show the dynamical stability of the composite structure. The highest phonon frequency for
C rings in aluminum is shown to be at 1360 cm−1 , which is closer to the graphene peak
−
observed in Raman spectroscopy, whereas isolated C scattered in Al shows 330 cm−1 of the
tt formation of sp2 hybridized
highest phonon frequency. This result suggests the favorable
−
C
rings in the Al matrix. In addition, the atomic displacement pattern presented in the figures
tt The atomic displace-
shows a similarity to that of the D band in pristine carbon structures.
ment pattern also suggests that the C matrix vibrations are decoupled from the Al matrix,
tt
which is in agreement with the findings of previously reported studies on aluminum matrix
composites [49]. Raman spectroscopy data confirm the existence of sp2 hybridized C rings
in our samples. The results from DFT suggest that sp2 -like carbon rings can be formed
inside the aluminum matrix.

3.2. Mechanical Properties Characterization

The mechanical properties of the AMCs were also determined experimentally through
the uniaxial compression test and micro-Vickers hardness test. Experimental mechanical
properties of the composites with and without nanocarbon reinforcements are summarized
in Table 3. Representative compression test curves for each composite and average results
for mechanical properties appear in Figures 5a and 5b–d, respectively. The composites
reached up to 61% and 55% increments of yield strength and up to 49% and 39% increments
of ultimate strength for the activated nanocarbon and graphene reinforcements, respectively.
Nanomaterials 2023, 13, 2917 8 of 14

However, yield and ultimate strength showed a decrease with the increasing graphene
volume fraction due to the increased agglomeration of this carbon allotrope.

Figure 5. (a) Representative stress-strain diagrams for the compression tests of the nanocarbon
6061 AMCs. (b) Average Yield Strength and Ultimate Strength of the nanocarbon 6061 AMCs.
(c) Average Hardness of the nanocarbon 6061 AMCs. (d) Average Modulus of Toughness and
Elongation of the nanocarbon 6061 AMCs.

Conversely, both yield and ultimate strengths increased with the increasing volume
fraction of activated nanocarbon. This behavior is attributed to a stronger dispersion and
interfacial bond between the activated nanocarbon and aluminum matrix. The strength-
ening of the composites can be ascribed to the load transfer from the matrix to the stiffer
reinforcement [50], as well as to the limited dislocation motion of aluminum [51]. Likewise,
elongation and modulus of toughness were affected by the limited motion of dislocations,
propitiated by the presence of the carbonaceous reinforcements, particularly for the samples
with graphene, because of the tendency of graphene for localized agglomeration at the grain
boundaries of the metal matrix [52,53]. However, in the case of the activated nanocarbon-
reinforced samples, after the initial reduction, the values of elongation and modulus of
toughness started to increase with the amount of reinforcement, which could propitiate
a re-establishment of these properties at higher activated nanocarbon volume fractions.
Manufacturing parameters also affect the mechanical properties of the composites, higher
sintering and consolidation temperatures will produce stronger and harder samples. For
example, Gürbüz et al. manufactured graphene/aluminum matrix composites at 550, 600,
and 630 ◦ C. The results show that the composites obtained at 630 ◦ C presented enhanced
apparent density and hardness compared to those fabricated at lower temperatures [54].
However, higher temperatures can also produce negative results, such as the formation of
undesirable amounts of secondary phases (Al4 C3 ), which will reduce the mechanical prop-
erties [55,56]. The introduction of activated nanocarbon and graphene nanoplatelets inside
the metal matrix increased the hardness of the materials, with a maximum increment of
26% for the sample with 2 vol. % of activated nanocarbon, compared to the non-reinforced
6061 alloy. Reinforcement with these specific nanocarbon composites showed a similar
behavior compared with other carbon allotropes such as C60, wherein the reinforcement
with this allotrope increased the hardness of the composites up to 26% [57]. This increase
in hardness has been attributed to good densification and a more limited deformation
produced for activated nanocarbon and graphene in the metal matrix, as well as an effective
refinement of the grains [45,58]. These results confirm previous reports wherein the increase
Nanomaterials 2023, 13, 2917 9 of 14

in volume fraction of graphene nanoplatelets after 1 vol % had an unfavorable effect on the
hardness due to the formation of vacancies and agglomeration [59]. Also, a larger presence
of porosity has been associated with a decrease in the hardness of the composites [60].

Table 3. Mechanical properties of the nanocarbon 6061 AMCs.

Yield Ultimate Modulus of

Hardness % of % of % of Elongation % of % of
Sample Strength Strength Toughness
(HV) Increment Increment Increment (mm mm−1 ) Increment Increment
(MPa) (MPa) (kJ m−3 )
6061 117.6 ± 2 - 178.6 ± 10 - 224 ± 6 - 0.14 ± 0.005 - 273.1 ± 23 -
61Ac1 138.2 ± 1 17.5 255.6 ± 2 43.0 289 ± 2 28.8 0.09 ± 0.01 −33.3 243.1 ± 36 −10.9
61Ac2 148.6 ± 1 26.3 289.3 ± 7 61.9 334 ± 10 49.1 0.10 ± 00.01 −23.8 300.7 ± 47 10.11
61Gn0.5 141.6 ± 1 20.4 278 ± 10 55.5 313 ± 7 39.8 0.09 ± 0.02 −30.9 347.2 ± 84 27.11
61Gn1 133.2 ± 0.8 13.2 235.5 ± 8 31.8 262 ± 10 17.1 0.03 ± 0.008 −73.8 184.1 ± 82 −32.5

Results for the densities of the composites obtained experimentally are displayed
in Figure 6a–d and in Table 4. All the samples presented a lower density, following the
tendency presented by the theoretical values. Theoretical density was calculated using the
rule of mixtures (3):
ρc = Vm ρm + Vr ρr (3)
where ρm and ρr are the density for matrix and reinforcement, respectively. Similarly, Vm
and Vr are the volume fraction of the matrix and reinforcement, respectively.
Porosity was determined using Equation (4). The low level of porosity reflects the
high degree of distribution reached using the powder metallurgy method [61].

ρt − ρe
Porosity (%) = × 100% (4)
ρt

where ρt and ρe are the theoretical and experimental densities, respectively.

Figure 6. (a) Relative Density, (b) Porosity, (c) Specific Strength, and (d) Hardness as a function of
porosity of the nanocarbon 6061 AMCs.

All the compositions presented high relative densities (%), with a maximum of 98%
for the sample with the higher volume fraction of activated nanocarbon due tt to better
packaging and mechanical bonding compared to the other compositions, as also shown
Nanomaterials 2023, 13, 2917 10 of 14

previously for aluminum matrix composites sintered with similar experimental method-
ology [62]. Figure 6d shows how the change in porosity is related to the hardness of the
materials, showing that the materials with the highest levels of porosity present the lowest
hardness, which is associated with gas entrapment during the manufacturing process [63],
and the increasing agglomeration of the reinforcement [64]. Porosity has been linked to
other mechanical properties of the aluminum matrix composites. Samples consolidated at
higher compressive forces have presented lower levels of porosity and higher compressive
strength [65]. Likewise, the increase in activated nanocarbon favored both the increase in
hardness and decrease in porosity, unlike the case of graphene reinforcement, where the
increase in volume fraction generated higher agglomeration, which is in agreement with
the results in the literature [66]. These results of density differ from other conventionally
used reinforcements, such as SiC [67] and TiC [68], whose densities increased with the
reinforcement volume fractions.

Table 4. Theoretical and experimental density-related properties for the nanocarbon 6061 AMCs.

Sample
6061 61Ac1 61Ac2 61Gn0.5 61Gn1
Experimental Density (g cm−3 ) 2.56 2.61 2.62 2.62 2.56
Theoretical Density (g cm−3 ) 2.70 2.67 2.65 2.69 2.69
Relative Density (%) 94.8 97.6 98.9 97.2 95.2
Porosity (%) 5.18 2.34 1.04 2.76 4.73

Figure 7 shows the SEM images of the compression-fractured surfaces of the compos-
ites. They all presented dimples and ridges with regular morphology, as is typical for the
elastic deformation and fracture of ductile materials [69]. These dimples also play a role
as a nucleation site for the formation of voids and the propagation of cracks. However,
the number of dimples and ridges was reduced as the amount of nanocarbon increased,
showing the loss of the ductile nature in the composites, similar to the results shown
elsewhere [70,71]. All the samples fractured at an angle of 45◦ with respect to the direction
of the applied load, indicating that the fracture is a consequence of the shear forces involved
in the load transfer from the matrix to the reinforcement [72].

Figure 7. Cont.
Nanomaterials 2023, 13, 2917 11 of 14

Figure 7. Fractured morphology of the nanocarbon 6061 AMCs, (a) 6061 (b) 61Ac1, (c) 61Ac2,
(d) 61Gn0.5, and (e) 61Gn1.

4. Conclusions
Aluminum matrix composites reinforced with differentff volume fractions of activated
nanocarbon and graphene nanoplatelets were fabricated by the powder metallurgy method.
SEM micrographs presented a good distribution of carbon nanoparticles. After the milling
procedure, a change in the original structure of the activated nanocarbon and graphene was
detected with Raman spectroscopy. There was no evidence of the formation of intermediate
phases, such as Al4 C3, which can affect the interaction between nanocarbon and aluminum.
Mechanical properties were enhanced when compared to the unreinforced 6061 aluminum.
Yield strength increased with both activated nanocarbon and graphene, being superior for
the latter, but yield strength decreased with the increased amount of graphene reinforce-
ment. Hardness presented a maximum increase of 26% for the sample with 2 vol. % of
activated nanocarbon. Strengthening can be attributed to load transfer, dislocation strength-
ening, and grain refinement in hot-pressed composites. Following an initial decrease in
elongation and modulus of toughness, they started to increase with the volume fraction of
activated nanocarbon. The determination of densities also combined to elucidate the influ-
ence of reinforcement on the mechanical properties of the composites. Density Functional
Theory (DFT) calculations for the phonon frequencies involved in the atomic displacements
derived from carbon-aluminum interactions were concordant with the Raman analysis,
which explained the results obtained for the experimental structural characterization.

Author Contributions: Conceptualization, methodology, resources, writing—original draft prepara-

tion, supervision, project administration, funding acquisition, S.N.; methodology, investigation, for-
mal analysis, writing—original draft preparation, W.R.-P.; investigation, R.K.; investigation, writing—
review and editing (supporting), P.S.; investigation, software, formal analysis, writing—original
draft preparation (supporting), H.I.S.; investigation, software, formal analysis, writing—original
draft preparation (supporting) T.J. All authors have read and agreed to the published version of
the manuscript.
Nanomaterials 2023, 13, 2917 12 of 14

Funding: This work is partially supported by the National Science Foundation Engineering Research
Initiation grant number 2138459.
Data Availability Statement: The data presented in this study are available on reasonable request
from the corresponding author.
Acknowledgments: The authors would like to thank supported by the National Science Foundation
Engineering Research Initiation grant number 2138459. S.N. also acknowledges support from the new
faculty startup fund and Materials Technology Center at Southern Illinois University—Carbondale.
The authors would like to thank Southern Illinois University—Carbondale and Marian University
Indianapolis for providing the computer facilities.
Conflicts of Interest: The authors declare no conflict of interest.

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