Interactions (2024) 245:332

https://doi.org/10.1007/s10751-024-02179-3

CONFERENCE PROCEEDING

Development AA7075/SiC/ZrN hybrid composite fabricated

through powder metallurgy techniques and evolution its
microstructural and mechanical properties

A Rajesh1 · U Sudhakar1 · K. V. Raghavulu1 · K Venkateswara Reddy1 · S. P. Jani1

Accepted: 8 October 2024

© The Author(s), under exclusive licence to Springer Nature Switzerland AG 2024

Abstract
It was aimed to find the effect of a variation in reinforcement level on the porosity and
mechanical properties for the two types of composites: SiC reinforced and SiC and ZrN
reinforced. It was possible to relate an increase in pore levels as a causative factor for
a decrease in mechanical properties. Furthermore, it was noted that composites with op-
timal levels in weight fraction showed very good mechanical responses: 2 wt% of ZrN
and 8 wt% SiC in the current study. The enhancement of mechanical properties by newly
produced Al3Zr particles will open new frontiers for its application in various industrial
settings. This is highly promising for a great number of sectors in the industry that are
in great need of lightweight but durable materials: aerospace, automotive, among other
sectors. Based on the compression strength and hardness test results of AA7075/SiC/ZrN
composites, the average values were 167 MPa and 112 HV, respectively. The great poten-
tial of this composite puts it in a very competitive position among the intended compos-
ites for various applications that require high mechanical strength and light weights like
aerospace and automotive sectors.

Keywords Hybrid composites · Powder metallurgy · Mechanical properties ·

Intermetallic compounds

1 Introduction

Composite materials are highly preferred in the contemporary industrial era because they
can enhance the quality of primary alloy materials by incorporating secondary particles [1].
However, achieving a homogeneous dispersion of reinforcing particles within the matrix
material is a challenge in the manufacturing process of composite materials [2]. To address
this issue, numerous studies have been conducted to achieve a uniform distribution of rein-

S. P. Jani
[email protected]
1
Department of Mechanical Engineering, Marri Laxman Reddy Institute of Technology and
Management, MLRITM, Hyderabad 500043, Telangana, India

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forcing particles within the matrix material [3]. Researchers generally agree that ultrasonic
techniques are effective in promoting the homogeneous distribution of reinforcing particles
within the liquid matrix phase [4]. Nevertheless, the formation of intermetallic compounds
remains an issue in liquid metallurgical processes due to the high temperatures used during
processing [5]. These compounds can weaken the bond between the interface and the matrix
due to their brittle nature, which can hinder the matrix’s ability to effectively transmit loads
to the reinforcing particles [6, 7].
As a result of the aforementioned difficulties that are associated with composite materi-
als, it is hoped that solid-state manufacturing techniques would effectively overcome and
alleviate these difficulties [8]. Powder metallurgy is commonly regarded by researchers as
the principal solid-state technology due to the inherent benefits it possesses. These advan-
tages include the capability to process materials via the use of low temperatures and the
cost-effectiveness of the technique [9]. In order to get near net shape composites created
by powder metallurgy methods, there are enhanced sintering technologies available, such
as microwave sintering and spark plasma sintering (SPS) [10]. These technologies are
designed to minimize the total amount of time required for the manufacturing process. In
order to make use of the contemporary sintering procedures, it is necessary to have com-
posite powders that are evenly distributed. Through the use of the appropriate ball milling
conditions, effective dispersion may be achieved. Because of the diameter of the balls, the
milling conditions in the ball milling process are significantly affected by the diameter of the
balls. There is a correlation between decreased ball sizes and greater collision frequencies,
which in turn facilitates improved powder particle milling efficiency [11]. It has been estab-
lished in a number of studies that the incorporation of stiff ceramic particles into composite
powders results in an increase in the efficiency of the milling process. Multiple experiments
have produced evidence that the inclusion of stiff B4C particles into the aluminum matrix
through the process of ball milling aids the reduction in particle size of composite powders.
This evidence has been supplied by a number of different investigations [12].
When compared to the processes that are utilized in liquid metallurgy, the rates of inter-
metallic compound formation that occur in powder metallurgy products are significantly
lower [13]. The process of microwave sintering is distinguished by a number of special
properties, including the acceleration of heating and the acceleration of sintering under low-
temperature conditions, which ultimately results in the production of interface areas that are
both robust and impeccable [14]. The occurrence of intermetallic compounds at interface
areas in low concentrations has been discovered to function as agents for pinning grains.
This observation is based on the results of specific researchers who have conducted inves-
tigation into the matter [15, 16]. During the process of sintering, this pinning effect inhibits
the development of grains while simultaneously activating processes that contribute to the
strengthening of the borders between grains. The dispersion strengthening mechanism is
enhanced by the uniform dispersion of reinforcements, which, in conjunction with the grain
boundary strengthening process, contributes to the dispersion strengthening mechanism [3,
17]. This enhancement in the capacity to transmit loads between the matrix and reinforce-
ments is significant. Recent studies have shown that the employment of advanced sintering
techniques, such as microwave sintering and spark plasma sintering (SPS), increases the
properties of composite materials. This was discovered through the exploitation of these
techniques [18].

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Table 1 Composition of used AA7075 matrix material

Al Zn Mg Si Cr Fe Cu C Ag
86.04 5.99 2.55 0.8 0.05 0.32 0.64 2.04 1.45

Table 2 Ball milling parameters Ball to powder ratio 10:1

Ball dia., 6 mm
Vial material Hardened stainless steel
Milling Speed 300 rpm
Milling time 60 min
Process control agent Acetone

Within this framework, the present investigation was conducted on a hybrid composite
that was composed of AA7075, SiC, and ZrN. Within the optimal weight fraction of the
AA7075/SiC composite, the ZrN particle concentration was changed between 1 and 5 wt%.
This range was used to achieve stability. The purpose of the study was to gather informa-
tion about the microstructure, secondary phases, and behavior of the composites that were
manufactured.

2 Materials and methods

2.1 Raw materials

In the current study, AA7075 served as the raw matrix material, characterized by an average
particle size of 50 microns. The primary and secondary reinforcements incorporated into the
matrix were SiC and ZrN, respectively. The average particle sizes of SiC and ZrN are 5 μm
and < 1 μm. The composition of the matrix material was determined through Energy Dis-
persive X-ray Spectroscopy (EDS) analysis. The raw powder was acquired from Nanoshell
Company Limited, India, and the obtained composition is detailed in Table 1.

2.2 Composite powders

In an aim to enhance the robustness of the composite initially SiC was added to the matrix
material and varied the composition from 1 to 8wt%. To uniformly disperse the reinforce-
ment particles in the matrix wet ball milling was used with acetone as process control agent.
The adopted ball milling parameters were listed in Table 2.

2.3 Compaction and sintering

The composite powders, once prepared, were compacted using a manual hydraulic pellet
press with a D2 die steel material. To facilitate the easy ejection of the green compacts dur-
ing the compaction process, the inner walls of the material were coated with hydraulic oil.
The compaction parameters can be found in Table 3. Following compaction, the green com-
pacts underwent sintering within a tubular muffle furnace under an argon gas atmosphere.
The sintering parameters are detailed in Table 3.

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Table 3 Sintering parameters Compaction Pressure 600 MPa

adopted in the present study
Die material D2 die Steel
Sintering Temperature 580 ℃
Heating rate 10 ℃/min
Heating environment Argon
Sintering time 120 min

Fig. 1 Flowchart representing the path of the work in the present investigation

2.4 Characterization of composites

The fabricated composites underwent mechanical testing, specifically in terms of compres-

sion and micro hardness. Porosity calculations were conducted utilizing the Archimedes
principle, the procedure and formulas used for the porosity calculations are mentioned
below in the Eq. (1). Compression test adhered to the ASTM E9M standard. To assess
the dispersion of reinforcements within the matrix material, Scanning Electron Microscopy
(SEM) analysis was employed, utilizing a W-SEM instrument. For enhanced microstruc-
tural visualization, samples were meticulously polished using varying grit sizes of emery
papers, progressing up to 3000 size, followed by polishing with 1-micron diamond paste. A
detailed flow chart representing the path of the work is represented in Fig. 1.

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wa − ww
ρ actual = × ρw
wa

Where,
Wa = weight of composite in air.
Ww = Weight of composite in water.
ρ w = density of water
ρ actual = Actual density of composite

ρtheoritical =ρmatrix × volumef ractionmatrix+

ρrein−1 × volumef ractionrein−1+
ρrein−2 × volumef ractionrein−2
 
ρ theoritical − ρ actual
P orosity = × 100  (1)
ρ theoritical

3 Results and discussions

3.1 Microstructural analysis

One of the most important aspects of composite materials is the uniform dispersion of rein-
forcements inside the matrix material. This is because it plays a vital role in increasing
the strength of the composite by means of effective load transfer mechanisms from the
matrix to the reinforcements. One of the most prevalent difficulties encountered in the field
of composite materials is the agglomeration of reinforcement particles inside the matrix
phase. Additionally, the existence of these agglomerates has the potential to have a signifi-
cant influence on the characteristics and qualities of composite materials [19]. In order to
determine whether or not agglomerates were present, a microstructural analysis was car-
ried out. The scanning electron micrographs (SEM) of the hybrid composite consisting of
AA7075 + 8% SiC + 2% ZrN (S8Z2) are shown in Fig. 2. The results of the study that was
carried out revealed that there were no agglomerations, and it was discovered that the rein-
forcements were distributed in a regular manner.

3.2 Porosity levels

Pores exert a significant influence on the degradation of mechanical properties in compos-

ites. These small voids within the material weaken the interfaces between the matrix and
reinforcements, resulting in an overall reduction in strength and durability. The presence of
pores induces a triaxial state of stresses within the material, contributing to premature fail-
ure. When exposed to external forces or environmental conditions, these stresses accumu-
late, leading to material breakage or fracture [20]. Therefore, minimizing pore occurrence
is imperative for enhancing the mechanical performance of composites. The generation of

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Fig. 2 SEM images of AA7075/8%SiC/2%ZrN (a) Dispersion of reinforcements (b) high magnification
image showing ZrN dispersion

pores in composites is chiefly attributed to the thermal mismatch phenomenon between

the matrix and reinforcements during the sintering process. Sintering, involving the heat-
ing and compacting of composite materials to form a solid structure, becomes a challenge
when the matrix and reinforcements exhibit different coefficients of thermal expansion. This
mismatch during heating and cooling can give rise to voids or pores within the composite.
The thermal mismatch between the matrix and reinforcements induces internal stresses
within the composite during sintering. As temperature fluctuates, the matrix and reinforce-
ments undergo varying degrees of expansion or contraction. This differential movement
creates stress concentrations at the interfaces between the matrix and reinforcements,
eventually leading to the formation of pores or voids within the material. The presence of
pores adversely affects the mechanical properties of composites. Pores act as stress con-
centrators, diminishing the material’s load-bearing capacity. These voids also loosen the
interfaces between the matrix and reinforcements, reducing the efficiency of load transfer
between them and resulting in an overall decrease in strength and stiffness. Furthermore,
pores impact the material’s resistance to fatigue and environmental degradation. The voids
provide pathways for moisture or other corrosive substances to infiltrate the material, accel-
erating degradation over time. Additionally, pores act as sites for crack initiation and propa-
gation under cyclic loading conditions, diminishing the fatigue life of the composite.
In conclusion, pores emerge as a principal contributor to the degradation of mechanical
properties in composites. These voids weaken interfaces, create stress concentrations, and
ultimately lead to early material failure [21]. The thermal mismatch phenomenon during
sintering stands out as a primary factor in pore generation. The imperative lies in minimiz-
ing pore formation to enhance the mechanical performance, durability, and reliability of
composites.
In the present study, the porosity levels of two types of composites were examined: SiC
reinforced composite and SiC and ZrN reinforced composite. The purpose of this investiga-
tion was to determine the effect of different reinforcement levels on the porosity levels of
the composites. The results obtained from the analysis indicated that after reaching an 8%
SiC level, the porosity levels started to increase at a rapid rate. This suggests that there is a
critical threshold at which the addition of SiC begins to negatively impact the density of the
composite [22]. Furthermore, it was observed that the increase in pore levels had a direct
correlation with the degradation of mechanical properties. As the porosity levels increased
beyond 8% SiC, the mechanical properties of the composite began to deteriorate. This find-

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ing indicates that there is a trade-off between reinforcement levels and the mechanical per-
formance of the composite. While SiC can enhance certain properties, such as strength and
stiffness, an excessive amount can lead to an undesirable increase in porosity.
In an attempt to mitigate the negative effects of high porosity levels, ZrN was introduced
as an additional reinforcement in the composite. The addition of ZrN resulted in a trend of
increased pore levels. However, it is worth noting that after reaching a 2% ZrN level, the
pore levels began to rise rapidly, as shown in Fig. 3. This suggests that there may be an
optimal ZrN concentration beyond which further addition does not contribute to improved
density. These findings have important implications for the development and optimization
of composite materials. It is clear that both the type and concentration of reinforcements
play a crucial role in determining the porosity levels and mechanical properties of compos-
ites. Therefore, careful consideration must be given to these factors during the design and
fabrication processes.

3.3 XRD analysis

Intermetallic compounds are truly amazing materials in the world of composites. They pos-
sess incredible versatility and play a vital role in establishing strong interfaces between the
matrix and reinforcements. These interfaces are crucial for transferring loads effectively,
ensuring the overall strength and durability of the composite system [20]. The formation
of intermetallics is influenced by the available free energy during the sintering process of
powder metallurgy compacts. This is precisely why liquid metallurgy is not the preferred
method when it comes to fabricating hybrid composite materials. In our latest research
endeavour, we delved into the fascinating world of intermetallic compounds and their
impact on composite materials. Excitingly, we conducted XRD analysis on samples that
had been optimized in terms of weight%. This analysis allowed us to examine the presence
of any secondary phases within the samples [23]. The XRD technique is a powerful tool

Fig. 3 Porosity levels of the AA7075/SiC and AA7075/SiC/ZrN composite

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Fig. 4 XRD analysis of AA7075/8%SiC composite and AA7075/8%SiC/2%ZrN

that enables us to gain valuable insights into the crystallographic structure of materials,
providing us with a deeper understanding of their composition and properties. Our findings
from the XRD analysis were truly remarkable. We were able to identify and analyze the
secondary phases present in the optimized weight% samples. This information is crucial
for understanding the overall behavior and performance of the composite materials. By
examining these secondary phases, we can gain insights into their influence on the mechani-
cal properties, such as strength and toughness. The discovery of these secondary phases
opens up a world of possibilities for further research and development [24]. We can now
investigate how these phases can be modified or controlled to enhance the performance of
intermetallic compounds in composite systems. This knowledge will allow us to design and
engineer more robust interfaces that can withstand higher loads and provide greater durabil-
ity. The potential applications of intermetallic compounds in composite systems are vast and
exciting. With their ability to establish strong interfaces between the matrix and reinforce-
ments, these materials can be utilized in numerous industries, ranging from aerospace to
automotive. Their versatility ensures that they can meet the specific requirements of each
application, whether it’s for lightweight structures or high-strength components. Overall,
our research on intermetallic compounds and their role in composite systems has been an
exhilarating journey. The XRD analysis has provided us with valuable insights into the
presence of secondary phases, guiding us towards further advancements in this field. We are

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excited about the future possibilities and the potential impact that intermetallic compounds
can have on the development of robust and durable composite materials.
From the exciting results of our investigation as shown in Fig. 4, it is clear that the com-
pound generated in the present composite system is Al3Zr. This discovery is significant as
it opens up new possibilities for the development of advanced materials. Previous research
has indicated that Al3Zr (JCPDS − 00-034-0336) is not the most favorable phase in terms of
formation kinetics. However, our findings highlight the crucial role that formation kinetics
play in the generation of Al3Zr [25]. This emphasizes the importance of understanding the
underlying mechanisms involved in the formation of this compound.
Interestingly, some reports have suggested that the presence of small-scale Al3Zr phases
can actually enhance the strength of the composite material. This is an exciting finding as
it suggests that Al3Zr can be utilized to improve the mechanical properties of the material.
However, it is important to note that high-scale levels of Al3Zr may have a detrimental effect
on the interface bond strength. This highlights the need to carefully optimize the levels of
Al3Zr in order to achieve the desired mechanical responses [26]. Overall, our investigation
has demonstrated that composites with optimized weight fraction levels exhibit excellent
mechanical responses. This is a highly promising result as it suggests that these composites
have the potential to be used in a wide range of applications where high strength and dura-
bility are required. Additionally, our findings indicate that the presence of low-scale level
intermetallics is beneficial for the performance of these composites.
In conclusion, our research has shed light on the generation and effects of Al3Zr in a
composite system. The discovery of this compound and its potential impact on mechanical
properties is an exciting development in materials science. Moving forward, further studies
can be conducted to explore different weight fraction levels and their effects on the mechani-
cal responses of these composites. This knowledge could pave the way for the development
of even more advanced materials with enhanced properties.

3.4 Mechanical properties

Mechanical properties play a crucial role in determining whether a material is suitable for
a particular application or not. They are the deciding factors that determine the durability,
strength, and overall performance of a material. In order to assess the mechanical proper-
ties of a fabricated composite, various tests were conducted, including compression testing
and microhardness testing. These tests provided valuable insights into the behavior of the
composite under different conditions. One of the key findings from the compression testing
of the composite was that the addition of SiC (Silicon Carbide) significantly enhanced its
strength [27]. As the weight fraction of SiC increased up to the optimized levels, the strength
of the composite improved. This is an exciting discovery as it opens up possibilities for
using this composite in applications where high strength is required. However, it is impor-
tant to note that beyond a certain weight fraction level, the mechanical properties started to
degrade. This suggests that there is an optimum level of SiC content that needs to be main-
tained for achieving the best mechanical performance. Furthermore, it was observed that
the mechanical properties of the composite were also influenced by the presence of pores.
As pore levels increased, there was a noticeable degradation in the mechanical performance
of the composite. This finding highlights the significance of pore levels in determining the

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overall mechanical behavior of the material. It is crucial to minimize pore levels in order to
ensure optimal mechanical properties.
In this groundbreaking investigation, the composite material containing 8wt% SiC dem-
onstrated incredible strength, exhibiting a compression strength of 143 MPa, as shown in
Fig. 5. This remarkable achievement underscores the immense potential of this composite
and positions it as a compelling choice for various applications requiring high durability.
Furthermore, as the reinforcement content level increased, the hardness values of the mate-
rial also rose. This trend signifies improved resistance to deformation and wear, enhancing
its suitability for applications demanding robustness. Expanding on these findings, the intro-
duction of ZrN particles into the AA7075/SiC composite yielded truly remarkable results.
The mechanical properties of the composite significantly improved, particularly up to 2wt%
of ZrN. Notably, the compression strength soared to an astonishing 167 MPa, as shown in
Fig. 6 surpassing previous impressive values. This substantial enhancement in strength is
crucial for applications requiring resilience against high loads and pressures. Additionally,
the hardness values continued to increase with the addition of ZrN particles. At 8wt% SiC
and 2wt% ZrN, the composite displayed a hardness value of 112 HV, signifying exceptional
resistance to indentation and scratching. These findings hold immense promise for vari-
ous industries, opening up a world of possibilities in aerospace, automotive, and other sec-
tors where lightweight yet robust materials are essential. The constant pursuit of improving
mechanical properties will lead to even more remarkable advancements, revolutionizing
various industries and paving the way for new and exciting applications.
In conclusion, this investigation has showcased the exceptional strength and hardness
values of the AA7075/SiC composite. The addition of ZrN particles has further enhanced
its mechanical properties, presenting new possibilities for its use across different industries.
Exciting times lie ahead as researchers continue to push the boundaries of composite materi-

Fig. 5 Mechanical responses of AA7075/B4C composite

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Fig. 6 Mechanical responses of AA7075/8%SiC/ZrN hybrid composite

als and unlock their full potential, promising a future filled with stronger, more durable, and
innovative materials.

4 Conclusions

In the pursuit to enhance the performance of the composite, SiC and ZrN are added to the
AA7075 matrix material as reinforcements. The following advanced conclusions can be
drawn from the tests conducted and observations made:

● Addition of SiC to the AA7075 matrix material significantly improved mechanical per-
formances for critical weight fractions.
● In this study, maximum improvement was noted with a weight fraction of 8 wt% of SiC.
These indicate that the compression strength of the composite is remarkably high, at up
to 143 MPa, which means that SiC reinforcements are dispersed homogeneously within
the matrix material in the absence of any agglomeration.
● To improve the strength of the composite, the AA7075/SiC matrix has had ZrN particles
incorporated. ZrN particles increased the strength up to as high as 167 MPa but main-
tained the uniformity of reinforcement dispersion.
● Intermetallic compound, Al3Zr, was determined to be formed at a 2wt% level of ZrN by
the XRD analysis. This increase in strength was a direct result of the formation of Al3Zr.
Composite robustness decreased on addition of higher levels of ZrN. It may possibly be
on account of negative effects that appeared in the microstructure of the material.

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● These findings demonstrate how mechanical performance can be balanced among the
different composite materials by proper reinforcement concentration. The weight frac-
tions of SiC and ZrN are hence important to optimize so that they allow the attainability
of the desired mechanical properties, but not at the cost of integrity and uniformity of
the composite structure. Therefore, this study will be quite beneficial in designing and
using composites for various applications, mostly when the strength and uniform dis-
tribution of reinforcements are called into play. Results show very great importance of
control for optimal levels of reinforcement to attain highest performance and reliability
in the different industrial applications.

These are valid general conclusions on the effects of reinforcements, SiC and ZrN, on the
mechanical properties of AA7075 composites and can form the basis for future research and
development work on advanced composite materials.

Author contributions A. Rajesh - data collection and draft preparation. U. Sudhakar - main document prepa-
ration. K. V. Raghavulu - figure prepartion. K. Venkateswara Reddy - concept developedS. P. Jani - corre-
sponding author and review response.

Data availability No datasets were generated or analysed during the current study.

Declarations

Competing interests The authors declare no competing interests.

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