Mater. Res. Express 11 (2024) 096518 https://doi.org/10.

1088/2053-1591/ad78b4

PAPER

Microstructure and mechanical properties of TiC reinforced

OPEN ACCESS
NbC-Ni4VC4Mo2C cermets
RECEIVED
30 May 2024
Asad Malik1, Abdul Basit2,5 , Muhammad Farzik Ijaz3, Furqan Anwar1, Malik Adeel Umer1 and
REVISED
30 August 2024
Yang Shao4
1
School of Chemical and Materials Engineering (SCME), National University of Science and Technology, Islamabad, Pakistan
ACCEPTED FOR PUBLICATION
9 September 2024
2
School of Mechanical and Manufacturing Engineering (SMME), National University of Science and Technology, Islamabad, Pakistan
3
Mechanical Engineering Department, College of Engineering, King Saud University, PO Box 800, Riyadh 11421, Saudi Arabia
PUBLISHED 4
18 September 2024
Department of Materials Science and Engineering Dalian Maritime University, 116026 Dalian, People’s Republic of China
5
Co-first authors.

Original content from this

E-mail: [email protected]
work may be used under
the terms of the Creative Keywords: niobium carbide, cermets, microstructure, mechanical properties
Commons Attribution 4.0
licence.
Any further distribution of
this work must maintain Abstract
attribution to the The class of NbC-Ni cermets has emerged as a promising environmentally friendly alternative to WC-
author(s) and the title of
the work, journal citation Co cemented carbide tools, although some inherent properties i.e. room temperature hardness and
and DOI.
flexural strength, of NbC-Ni cermets may require further enhancements. To enhance the properties of
NbC-Ni cermets, diverse methodologies were applied, including grain inhibition and the strengthening
of the cermet through the use of reinforcements. This study systematically examined the impact of TiC
additions, specifically at 10% and 20%, on both the microstructure and mechanical properties of
NbC-12Ni-4VC-4Mo2C cermets. NbC-12Ni cermets were fabricated via vacuum liquid phase sintering
(LPS) at 1400 °C and 1450 °C. Enhancements by incorporating 4% VC and 4% Mo2C, followed by TiC
at 10% and 20% concentrations to the NbC-Ni-4VC4Mo2C cermet were made. XRD and SEM results
confirm the formation of (Nb, X, Y) C solid solution cubic FCC carbides. Significant grain refinement
was evident in the cermet samples, subjected to grain inhibition. The observed grain sizes ranged from a
maximum of 6.84 μm (in NbC12Ni) to a minimum of 2.154 μm (in the sample containing 20% TiC) at
1450 °C. The incorporation of 20TiC at 1450 °C led to a remarkable 26.5% enhancement in average
hardness compared to NbC-Ni cermet, and a 4.2% improvement over the 4VC4Mo2C cermet. At
1450 °C, 20TiC reinforcement led to an average fracture toughness of 9.331 MPa√m, representing a
4.56% improvement over the 4VC4Mo2C cermet. However, there was a marginal reduction in
toughness compared to the NbC-Ni cermet. Moreover, the addition of TiC led to a decrease in the
flexural strength of the cermets, with a maximum flexural strength of 939 N mm−2 recorded for
NbC-Ni-4VC4Mo2C, representing an 11.6% increase compared to the NbC-Ni cermet.

1. Introduction

Tungsten carbide–cobalt (WC-Co) cemented carbides have been well-known for their outstanding mechanical
properties. However, when exposed to high-temperature conditions, tungsten carbide (WC) exhibits higher
solubility in iron-based alloys, which accelerates tool wear during cutting processes due to adhesion with Fe
[1–3]. In 2013, both the European Commission, specifically through the Registration, Evaluation,
Authorization, and Restriction of Chemicals (REACH), and the U.S. National Toxicology Program (NTP)
categorized cobalt as a carcinogenic substance, strongly advising industries to find alternatives to this element
[4]. In response to these concerns, WC-Ni materials were developed as potential alternatives to WC-Co to
reduce toxicity. WC-Ni cermets were found to exhibit comparable mechanical properties, such as hardness and
fracture toughness, while offering improved corrosion resistance and reduced health risks associated with cobalt
exposure. Research demonstrated that WC-Ni composites achieved similar or enhanced performance in various
applications, making them a promising substitute for WC-Co [5, 6]. However, Tungsten (W) and Cobalt (Co)

© 2024 The Author(s). Published by IOP Publishing Ltd

Mater. Res. Express 11 (2024) 096518 A Malik et al

are considered high-risk materials in terms of their availability and have been categorized as critical raw
materials (CRMs) by the European Union (EU) in 2014, 2017, and again in 2019, demanding a focus on their
sustainable utilization [7, 8]. This motivation stems from the need to find materials that deliver on performance
and align with sustainability and safety considerations.
Boasting a high melting point of 3522 °C and a remarkable hardness of 19.6 GPa, along with good wear
resistance, NbC exhibits properties that align well with the demands of cutting tool applications [9, 10]. NbC is
also considered a leading candidate for biocermets due to its wear resistance and durability, making it a
promising material for use in biomedical applications such as bone implants. Literature related to the addition of
NbC to titanium and beta titanium-niobium alloys has already been shown to improve tribocorrosion
resistance, a potential advantage for biomedical applications [11, 12]. Some key features of NbC make it a
promising alternative to WC. Various binding agents, including Co [13–17], Fe [18–22], Ni [23–28], and high
entropy alloy (HEA) [29, 30], have been subject to investigation concerning their application with NbC. Among
these, NbC-Ni cermets have been gaining attraction as prospective substitutes for WC-Co cemented carbides in
specific domains, driven by their favorable mechanical attributes and reduced density. While the mechanical
properties of NbC-Ni cermets exhibit promise, they still fall short when compared to WC-Co cemented
carbides. WC-Co cemented carbides have superior thermal conductivity, fracture toughness, and flexural
strength compared to NbC-Ni cermets [2]. However, NbC-Ni cermets show better wear resistance and chemical
stability against iron or steel [26].
Prior studies have highlighted substantial carbide particle growth in situations where only NbC and Ni were
subjected to sintering [31, 32]. Thus, limited research is being conducted to improve the mechanical
characteristics of NbC-Ni cermets, with a special emphasis on the influence of secondary carbide(s) addition on
the mechanical properties of NbC-Ni cermets.
Previous research employing vacuum pressureless sintering highlighted the potential benefits of incorporating
secondary additives such as VC, Mo2C/Mo, and TiC, which led to substantial reductions in NbC grain size.
Consequently, these additions were found to enhance the hardness and fracture toughness of NbC-Ni cermets.
Notably, the incorporation of Mo2C was observed to elevate hardness concurrently while lowering the toughness
[32–34]. Another study focused on introducing varying concentrations of TiC into NbC-12%Ni underscored its
capability to inhibit grain growth, resulting in noteworthy improvements in both hardness and toughness through
vacuum liquid phase sintering [35]. When added to cermets, TiC, known for its hardness and strong grain growth
inhibition effect, tends to significantly reduce the grain size of the primary carbide phase (e.g., NbC), leading to a
finer microstructure. TiC can form mixed carbides like (Nb, Ti)C when added to NbC-Ni cermets, resulting in a
gradient of Ti within the carbide regions that can enhance hardness and toughness. In addition, TiC has been
reported to improve the wear resistance and high-temperature hardness of cermets [23, 29, 35, 36].
Numerous investigations have aimed to strike a balance between hardness and toughness, with various
studies detailing the collective influence of paired additives like (VC + Mo2C), (Mo2C + TiC), (Mo2C + WC),
(WC + TiC), (WC + TiC0.7N0.3), and (WC + Mo2C + TiC0.7N0.3) within diverse compositions. Notably, the
combination of 4VC+4Mo2C has proven effective in achieving a favorable blend of hardness and fracture
toughness in NbC-Ni cermets [24, 27, 32, 34, 37–40]. The incorporation of TiC into NbC-Ni-4VC-4Mo2C
cermets could potentially elevate their hardness and wear resistance, while also contributing to a more refined
microstructure, enhancing their mechanical properties for demanding applications. It is worth noting that no
research has thus far explored the impact of TiC incorporation in NbC-Ni-4VC4Mo2C (hereby called
4VC4Mo2C) compositions.
This investigation aims to evaluate the effect of adding TiC on 4VC4Mo2C, on grain growth inhibition in
NbC-Ni cermets, and to analyze the resulting impact on the microstructure, and mechanical properties of these
materials. Initially, 4VC4Mo2C was incorporated into the NbC-Ni cermets, followed by the investigation of the
influence of different compositions of TiC (10% and 20%) addition on 4VC4Mo2C. The powders were
processed through vacuum liquid phase sintering at two distinct temperatures. The findings of this study can
have significant implications for the potential applications of NbC-Ni cermets in various industrial settings. The
comprehensive understanding of the synergistic effects of VC, Mo2C, and TiC additives on the properties of
NbC-Ni cermets, including their microstructure, and mechanical properties, can aid in developing improved
materials for use in various industries.

2. Experimental methods

2.1. Materials preparation

NbC (sourced from Huarui Metals, FSSS-1.10 μm), VC (Huarui Metals, FSSS-2.60 μm), Mo2C (Huarui Metals,
FSSS-1.90 μm), and Ni (Merck, FSSS-5 μm) powders were employed in the preparation of NbC-Ni based
cermets alongside additional reinforcements. The morphology of the initial powders is presented in figure 1.

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Figure 1. Morphology of starting powders.

Table 1. Chemical composition of investigated samples.

Sample composition vol%

SampleVol% Abbreviation
NbC Ni VC Mo2C TiC

Density(g/cm3) ρ 7.83 8.90 5.77 9.18 4.93

NbC12Ni NbC12Ni 88 12 — — —
NbC12Ni4VC4Mo2C 4VC4Mo2C 80 12 04 04 —
NbC12Ni4VC4Mo2C10TiC 10TiC 70 12 04 04 10
NbC12Ni4VC4Mo2C20TiC 20TiC 60 12 04 04 20

The chemical composition of the examined specimens is detailed in table 1. The powders were carefully
weighed using an analytical balance to ensure adherence to the specified composition. These powders were
subsequently introduced into a high-density polyethylene (HDPE) vessel possessing a mill volume of 0.25 l, and
the mixing process was initiated at a rotational speed of 200 revolutions per minute (RPM). The mixing media
employed comprised cylindrical WC-6Co balls with 3 mm and 5 mm diameters. The powders were subjected to
a 24 h mixing regimen within an ethanol medium, utilizing a ball-to-powder ratio of 10:1 within a low-energy
ball mill (WIseMixBML-2). Following the mixing phase, the slurry was subjected to vacuum drying at 50 °C for
5 h within a controlled environment. Subsequently, the powders were compacted to form both circular (11 mm
diameter) and rectangular (25 mm × 5 mm × 2 mm) shapes through uniaxial pressing at a pressure of 200 MPa,
followed by cold isostatic pressing at 250 MPa.
The compacts were sintered at a heating rate of 10 °C min−1 till 1200 °C and 5 °C min−1 till 1400 °C and
1450 °C respectively. The samples were subjected to an isothermal dwell time of 1 h within a dynamic vacuum
environment, which was upheld at a pressure of 10−2 Pascal. The samples were then slowly cooled inside the
furnace. The temperatures were measured with a thermocouple till 1000 °C and with a 2-beam laser pyrometer

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Figure 2. XRD of (a) NbC12Ni, 4VC4Mo2C, and (b) 10-20TiC.

till 1400 °C–1450 °C.The sintered cermets were ground using different SiC grit papers and finely polished at 6, 3,
and 1 μm diamond paste.

2.2. Characterization
The characterization of sintered specimens encompassed various techniques. The determination of sintered
body phases employed x-ray diffraction (XRD), with a Bruker D-phaser XRD system utilizing Cu Kα radiation
(30 kV, 10 mA). The XRD procedure followed step-scan data acquisition, employing a 0.02° step size and
spanning the angular range of 20–80°. SEM imaging of polished sintered samples was executed in secondary
electron (SE) mode on a JEOL JSM-6490A SEM with energy-dispersive x-ray spectrometer (EDX) capability.
Hardness measurements (HV30) were conducted using a hardness tester (Model HVRVU-187.5) utilizing a
30Kgf indentation load and a dwell time of 15 s. The Palmqvist indentation toughness (KIC) was computed using
the method outlined by Shetty et al [18] based on radial crack lengths surrounding the Vickers indentation. All
measurements were taken as the average value from a set of five readings. For flexural strength assessment, a
conventional 3-point bend test was performed using a Shimadzu AGX-Plus Universal Testing Machine with a
20kN load cell, employing a span length of 16 mm and crosshead displacement of 0.1 mm min−1.

3. Results and discussion

3.1. X-ray diffraction analysis

The XRD patterns presented in figure 2(a) were subjected to comparison with the ICDD PDF-2 database,
resulting in the identification of key phases within the sintered cermets. The diffraction analysis successfully
recognized the presence of cubic Nickel phase (PDF-00-004-0850) and cubic NbC phase (PDF-00-038-1364) in
the samples. In the case of TiC-reinforced cermets, the cubic TiC phase was identified and matched with the
PDF-00-006-0614 card as depicted in figure 2(b). This comprehensive XRD investigation revealed the
coexistence of FCC cubic nickel and an (Nb-Ti-V/Mo) C solid solution within the TiC-reinforced cermets.
Upon examination, the diffraction peaks corresponding to NbC (111), (200), (220), (311), and (222)
reflections are consistently observed in all the studied compositions and sintering temperatures, indicating the
presence of the NbC phase. Notably, the peak positions and intensities remain relatively consistent, suggesting
that the incorporation of 4VC4Mo2C and subsequent TiC additions do not significantly alter the NbC phase
crystallinity. The incorporation of 4VC4Mo2C had a pronounced influence on the lattice parameter of both
carbide and binder phases as depicted in figure 3. The carbide phase’s lattice parameter experienced a reduction
from 4.47209 Å (in the base cermet NbC-12Ni) to 4.44340 Å in 4VC4Mo2C. This reduction can be attributed to
the formation of a solid solution (Nb-V-Mo) C after sintering [26, 32]. Additionally, the TiC-reinforced cermet
containing 10 vol% TiC exhibited the lowest lattice parameter value of 4.43341 Å, indicative of the development
of (Nb-Ti-V/Mo) C solid solution carbides[25, 35, 41]. Over subsequent strengthening stages, the lattice
parameter of the carbide phase changed due to increased TiC solubility within the NbC crystal lattice.
Of particular interest is the integration of TiC peaks within the carbide NbC phase. This decrease in the
carbide lattice parameter is attributed to the elevated solubility of Mo2C and VC in the carbide phase, along with

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Figure 3. Lattice parameters changes in NbC and Ni for various compositions.

the diminished carbon content in sintered cermets as temperatures rise. The lattice constant of Ni exhibited a
notable increase upon the addition of VC, Mo2C, and TiC, signifying the augmented concentrations of these
elements within the Ni binder.
The matching cubic crystal structures of TiC and VC with NbC facilitated the rapid establishment of a
homogenous solid solution carbide. The enhanced solubility of Mo2C and VC within the binder phase, as
opposed to NbC, allowed them to affect the growth of NbC grains.
An alternative measure to evaluate changes in lattice parameters is the atomic radii of constituent elements,
where Nb(1.429 Å), Ti(1.462 Å), V(1.316 Å), Mo(1.363 Å), and Ni (1.246 Å) contribute to this analysis [42].
The substitution of smaller elements into the NbC structure correspondingly led to a reduction in the unit cell
size, primarily because the smaller atoms occupy the lattice positions originally held by larger atoms. The
complex interplay of lattice constants, solubility, and atomic sizes collectively contributes to the intricate phase
interactions and resultant microstructural characteristics observed in the sintered cermets.

3.2. Microstructural analysis

Microstructural analysis through scanning electron microscopy (SEM) coupled with energy-dispersive x-ray
spectroscopy (EDX) offers insights into the compositional and morphological characteristics of the examined
cermets. In the microstructural analysis of NbC-12Ni cermets, distinct phases are discernible in figure 4(a). The
darker regions correspond to the NbC grains, while the lighter areas represent the Ni binder phase. Notably, the
microstructure exhibits a coarser-grained appearance, especially evident at the sintering temperature of
1400 °C, where numerous micropores become visible.
Despite the absence of distinct Ni binder pools, a uniform distribution of the binder phase is achieved,
emphasizing effective binder integration. However, the presence of binder inclusions, micropores, and free
graphite points toward a slightly compromised wetting behavior. This phenomenon has led to the
amalgamation of neighboring carbide grain clusters, resulting in the coarser grain structure observed [43]. The
phenomenon of NbC grain coarsening during liquid-phase sintering, attributed to the dissolution of smaller
NbC grains in the binder phase and their subsequent re-precipitation onto larger grains, aligns with the well-
established Ostwald-ripening process. This process is driven by the reduction of particle surface energy. The
mean grain size was estimated to be around 4.33 μm for NbC-12Ni cermet.
An elemental distribution map showcasing the distribution of key elements (Nb and Ni) for NbC-12Ni
cermets obtained through EDX analysis confirms the distribution of Ni in binder regions and NbC in the
Carbide region as depicted in figure 5. Notably, the NbC grains remain undissolved within the binder phase
during the sintering process, thereby negating the occurrence of grain refinement in the sintered state.
In figure 4(b), the microstructure of 4VC4Mo2C cermet is depicted. Microstructural examination through
SEM reveals notable grain inhibition, with the darker and lighter contrast regions representing NbC solid
solution and nickel binder, respectively. Micropores and inclusions are present but occur at lower
concentrations than the NbC-12Ni base cermet. Grain morphology exhibits a slight rounding, and a more even

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Figure 4. SEM images of (a) NbC12Ni (b) 4VC4Mo2C (c) 10TiC (d) 20TiC cermets @ 1400 °C.

Figure 5. Elemental mapping and EDX analysis of NbC-12Ni cermet.

binder distribution was observed. The calculated average grain size measures approximately 3.19 μm, signifying
a substantial reduction compared to the base cermet. This reduction in grain size can be attributed to the
inhibitory effects of the added VC and Mo2C, which impede the coarsening of the grains during the sintering
process. As a result, the microstructure of the cermets exhibits a more refined and controlled arrangement of
grains. Additionally, the uniform distribution of the binder phase observed in the micrographs indicates
improved wetting behavior and the effective dispersion of inhibitors, contributing to the enhanced
microstructural characteristics of the cermet materials.
The distribution of elemental constituents as depicted in figure 6, validates the presence of V and Mo in both
NbC grains and the Ni binder. This distribution serves as confirmation for the formation of solid solution
compounds, specifically (Nb, V)C and (Nb, Mo)C, within the structure of the cermet. These findings collectively
emphasize the promising potential of VC and Mo2C as grain growth inhibitors, offering insights into their role
in enhancing the microstructural attributes of NbC-Ni cermets.
Introducing 10TiC reinforcement to the base NbC-Ni cermets, in combination with added inhibitors
(4VC4Mo2C), induces distinct microstructural changes characterized by the presence of rounded smaller grains
alongside faceted larger grains as depicted in figure 4(c). Notably, micropore occurrence is extremely low, and the

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Figure 6. Elemental mapping and EDX analysis of 4VC4Mo2C cermet.

binder exhibits a uniform distribution. The microstructure reveals two distinguishable phases, namely cubic NbC
and Ni distributions, consistent with other cermets. At a sintering temperature of 1400 °C, the solubility of VC,
Mo2C, TiC, and NbC within the Ni binder approximates 36, 14, 11, and 7 wt% respectively [31]. This observation
is attributed to the inverse correlation between higher surface energy and lower solubility in molten binders. EDX
spectral analysis as illustrated in figure 7, unveils a preferential dissolution of Ti in Nb and V, and Mo in the binder.
This results in the formation of mixed carbide solutions, namely (Nb-Ti-V)C and (Nb-Ti-Mo)C. As expected, the
inhibition of grain growth persists, yielding a mean grain size of 2.05 μm, the smallest among all cermets.
However, 20TiC-reinforced cermets exhibit binder agglomeration, suggesting reduced wettability of TiC. A
preference for partial wetting in cermet systems emerges as complete wetting tends to compromise mechanical
properties. At 1400 °C, an increase in binder thickness coupled with reduced spacing between binder pools is
noticeable in figure 4(d). This phenomenon indicates a TiC solubility limit at this temperature. The evident
binder agglomeration leads to diminished mechanical properties, contributing to increased toughness of the
cermet. An extended isothermal dwell time for even binder wetting or elevated sintering temperature is required
to address this challenge. Consequently, the sintering temperature was elevated. This modification enhanced the
wetting behavior of the binder due to higher binder interfacial energy, countering insufficient wetting.
Sintering at 1450 °C, although effective in reducing micropores and free graphite, led to a notable increase in
grain growth which is evident from figure 8(a). The average grain size, calculated at 6.84 μm, underscores this
trend. For 4VC4Mo2C, a significant reduction in porosity and inclusions was observed by increasing the
sintering temperature as depicted in figure 8(b). Despite the higher sintering temperature, the retention of grain
growth inhibition is evident, as indicated by a mean grain size of 2.33 μm, which remains below that of the
1400 °C sintered cermet. Additionally, a substantial reduction in free carbon content is also evident. The
addition of 10%TiC, as illustrated in figure 8(c), further reduces the average grain size to 2.218 μm. In the case of
the 20TiC-reinforced cermet, an even distribution of the binder is observed throughout the cermet at 1450 °C,
with the absence of binder pools. The increased sintering temperature results in an augmented solubility of TiC
within carbide grains, effectively preventing binder agglomeration, as shown in figure 8(d). The addition of
inhibitors consistently leads to a reduction in grain size compared to the base cermet, highlighting their effective
role in grain growth inhibition.
Moreover, at elevated temperature, the base cermet exhibits an increase in grain size, contrasting with other
cermet compositions, where inhibitors and higher sintering temperatures contribute to maintaining smaller
grain sizes. This demonstrates the crucial influence of both inhibitors and sintering conditions on the grain
growth behavior of these cermets.
Table 2 provides an overview of the calculated average grain sizes for various compositions at different
temperatures.

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Figure 7. Elemental mapping and EDX analysis of TiC cermet.

Figure 8. SE-SEM images of (a) NbC12Ni (b) 4VC4Mo2C (c) 10TiC (d) 20TiC cermets @ 1450 °C.

3.3. Mechanical properties

3.3.1. Hardness
The Vickers hardness (HV30) measurements were performed to assess the hardness characteristics of the cermets
under different compositions and sintering temperatures. The Vickers pyramid indenter was employed,
utilizing a load of 30 kg for hardness (HV30) measurements, with a dwell time of 15 s. Figure 9 illustrates the
hardness values obtained for the various cermet compositions at 1400 °C and 1450 °C.
The hardness measurements for the NbC-Ni base cermets revealed values of approximately 1087.1 Kgf mm−2
and 1171.3 Kgf mm−2 for 30 kg load at 1400 °C and 1450 °C, respectively. The increase in hardness value at
1450 °C can be attributed to the reduction in porosity, as illustrated in figure 8(a), compared to the 1400 °C
condition shown in figure 4(a). Porosity, or the presence of voids within the material, can act as stress

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Figure 9. Vickers hardness (HV30) of fabricated samples.

Table 2. Average grain size of samples @1400 °C &1450 °C.

Grain size Grain size

Sample 1400 °C (μm) 1450 °C (μm)

NbC12Ni 4.338 6.840

4VC4Mo2C 3.190 2.339
10TiC 2.054 2.218
20TiC 2.898 2.154

concentration points and weaken the overall structure. The absence of significant porosity enhances material
integrity, allowing it to resist deformation and exhibit higher hardness.
The introduction of 4VC4Mo2C as an inhibitor resulted in a substantial overall increase in hardness values
for both temperatures. This significant increase in hardness corresponds to the notable grain inhibition, as
previously illustrated in figures 4(b) and 8(b), along with the formation of solid solution carbides, as discussed in
the previous section.
The inclusion of TiC also had an overall positive effect in terms of hardness. However, hardness decreased
due to agglomerated binder pools forming at 1400 °C, as observed in the case of 20TiC substitution, as shown in
figure 4(d). Meanwhile, at 1450 °C, as depicted in figure 8(d), binder distribution improved, and no pools were
observed, resulting in improved hardness values.
The formation of mixed carbides (Nb-V-Mo)C and (Nb-Ti-V/Mo)C and the distribution of inhibitors in
both the binder and ceramic phases contributed to the overall improved hardness. Grain size evolution,
influenced by reduced NbC size and differences in carbon content in mixed carbides, may also have played a role
in hardness [2, 35, 41].
Improved densification and binder distribution at 1450 °C led to enhanced hardness with the addition of
inhibitors and reinforcement. The maximum mean hardness of 1482 HV30 was achieved using 20TiC
reinforcement at 1450 °C, representing a remarkable 26.6% and 4.2% improvement over the base cermet (NbC-
Ni) and 4VC4Mo2C respectively.

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Figure 10. Vickers hardness indentation with palmqvist cracks emanating from the edges.

Figure 11. Indentation fracture toughness of fabricated cermets.

3.3.2. Fracture toughness

In the context of indentation fracture toughness assessment, two primary types of cracks, palmqvist cracks, and
median cracks are encountered. Notably, palmqvist crack models find greater applicability in the assessment of
WC-Co hard metals in comparison to median crack approaches. Many equations have been employed to study
palmqvist toughness in hard metals. The Shetty equation has shown the best validity for accurate fracture
toughness measurements for WC-Co cermets for very few indentations [44].
The Shetty equation is explained as follows
P
wk = A H
T
where A is an empirical constant equal to 0.0028, H is the hardness in N/mm2, P is the applied load in Newtons
(294 N), T is the sum of all crack lengths in mm and WK is the Palmqvist fracture toughness represented in
MPa√m. Figure 10 shows the Vickers hardness indentation with palmqvist cracks emanating from the edges.
Using the Shetty equation the indentation fracture toughness of the fabricated cermets was calculated and
presented in figure 11. The relatively modest improvement in fracture toughness observed at 1400 °C, in

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Figure 12. Fracture and toughening mechanisms in NbC12Ni-based cermets.

contrast to the more significant enhancement at 1450 °C, can be attributed to specific factors. One primary
contributing factor is the improved dispersion and densification achieved at higher sintering temperatures.
As the sintering temperature rises, the cermet experiences increased consolidation and reduced porosity,
resulting in a more compact and homogeneous microstructure. This reduction in porosity is particularly
beneficial for fracture toughness because it minimizes the presence of internal voids and potential crack
initiation sites.
The addition of 4VC4Mo2C improves hardness but reduces fracture toughness. Subsequently, the
incorporation of TiC into 4VC4Mo2C enhances fracture toughness, with the greatest improvement observed in
the 20TiC cermet, where fracture toughness increases by 4.56% when compared to the 4VC4Mo2C alone.
Typically observed fracture patterns indicate intergranular fracture mechanisms in NbC-Ni cermets as depicted
in figure 12. This means that cracks tend to propagate along the boundaries between the individual grains of the
cermet. The introduction of secondary carbides, such as TiC, intensifies this behavior by encouraging crack
propagation along the interfaces between the carbide particles and the metallic binder. These secondary particles
act as obstacles for crack propagation, causing the cracks to deflect from their original path to promote fracture
toughness. The dominance of intergranular fracture in the NbC-Ni has already been reported [32].

3.3.3. Flexural strength

The flexural strength using the 3-point bend test was examined at 1400 °C and 1450 °C and is depicted in
figure 13. The flexural strength increased with the rise in temperature across all compositions. The NbC-12Ni
cermet exhibits an average flexural strength of around 830 MPa @1450 °C. The highest 3-point flexural strength,
approximately 926 MPa @1450 °C, was achieved in the NbC-12Ni cermet modified with 4VC4Mo2C,
representing an 11.6% increase compared to the NbC-Ni cermet.
TiC is a ceramic material known for its hardness and strength. When incorporated into the cermet matrix, it
has the potential to significantly augment the material’s overall strength. This enhancement is frequently
ascribed to the reinforcement effect, wherein TiC particles serve as obstacles to hinder crack propagation and
offer resistance against deformation when subjected to a load. Consequently, the addition of TiC can lead to a
notable increase in the flexural strength of the NbC-Ni cermet [45]. However, the impact on flexural strength is
not necessarily directly proportional to the amount of TiC added. Typically, there exists an optimal TiC content
at which flexural strength reaches its peak. Beyond this point, an excessive amount of TiC may result in a decline
in strength [35].
Our experimental findings revealed that incorporating 10% and 20% TiC led to a reduction in flexural
strength. This decrease can be attributed to the potential saturation of the positive effect of TiC on flexural
strength, as explained earlier. To improve the flexural strength of TiC-reinforced cermets, it could be
advantageous to investigate different TiC content levels, increase the binder concentration, or extend the
sintering duration during the fabrication process.

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Figure 13. Flexural strength of fabricated cermets.

Figure 14. Hardness HV30 versus fracture toughness at 1400 °C.

3.4. Comparative analysis

3.4.1. Hardness versus fracture toughness
The graphs depicting Hardness versus Fracture Toughness play a pivotal role in understanding the mechanical
characteristics of cermet materials. These graphs offer a comprehensive perspective on the relationship between
hardness, which signifies resistance to deformation, and fracture toughness, which indicates a material’s ability
to withstand cracking or failure. These graphs aid material scientists and engineers in optimizing cermet
compositions for specific applications, balancing the need for hardness and toughness to ensure superior
performance and durability [13].
Figure 14 illustrates the relationship between hardness and fracture toughness at 1400 °C for the different
cermet compositions. The 10TiC sample exhibits the best combination of hardness and fracture toughness at
1400 °C. It shows an approximately 6.6% increase in hardness compared to the 4VC4Mo2C sample, while

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Mater. Res. Express 11 (2024) 096518 A Malik et al

Figure 15. Hardness (HV30) versus Fracture Toughness at 1450 °C.

maintaining a similar level of toughness as also depicted in figures 9 and 11. In contrast, the 20TiC sample
demonstrates a decrease in hardness by approximately 13.2%, with only a 6.3% increase in toughness. The
presence of a binder pool at 1400 °C in the 20TiC cermet improves fracture toughness but at the expense of
hardness.
Increasing the sintering temperature significantly improved fracture toughness, with an approximate one-
order-of-magnitude increase as depicted in figure 15. All cermets exhibited enhanced resistance to crack
propagation, indicating greater toughness and hardness compared to those sintered at 1400 °C. This
improvement can be attributed to improved binder distribution, enhanced wetting behavior, and higher
densification.
The highest level of hardness, reaching an impressive 1482.6 HV30, was attained in the 20TiC-reinforced
cermet. The addition of TiC significantly enhanced hardness without introducing any detrimental effects on
toughness. This demonstrates that TiC reinforcement not only contributes to increased hardness but also
maintains the material’s toughness at a high level, highlighting its dual benefit in improving the mechanical
properties of the cermet. Figure 15 also presents a compelling comparison between the outcomes of this study
and previous research [31, 32]. It distinctly illustrates that the results obtained in this study exhibit a superior
combination of hardness and toughness, primarily attributed to the addition of TiC. Furthermore, it’s
noteworthy that the incorporation of 4VC4Mo2C in the NbC-Ni cermets also yields an improved combination
of hardness and fracture toughness compared to findings in prior studies. This underscores the significance of
these compositional modifications in enhancing the overall mechanical performance of NbC-Ni cermets.

4. Conclusions

• Dense TiC-modified NbC-Ni-4VC4Mo2C cermet was successfully fabricated by pressure-less liquid phase
sintering (LPS) in a vacuum for 1 h at 1400 °C and 1450 °C. Notably, at 1450 °C, the material exhibited its
superior properties due to reduced porosity.
• XRD analysis revealed a cubic fcc lattice formation for both carbide and binder phases. Additions of secondary
reinforcements did not reveal any phase transformation and the structure remained cubic in all cermets.
• The addition of reinforcements led to the formation of (Nb-V-Mo) C and (Nb-Ti-V/Mo) C solid solutions in
the carbide phase and the dissolution of secondary carbide reinforcements in the binder phase. According to
EDS analysis, TiC was mostly found in NbC, while VC and Mo2C were distributed evenly in the entire cermet.
• By adding VC and Mo2C in the base cermets grain size decreased from 6.840 μm to 2.339 μm. TiC addition
further promoted grain size reduction to 2.154 μm at 1450 °C.

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Mater. Res. Express 11 (2024) 096518 A Malik et al

• The assessments of hardness and fracture toughness demonstrated a consistent rise in both properties as a
result of the successive carbide reinforcements The maximum mean hardness of 1482 HV30 and fracture
toughness of 9.331 MPa√m was achieved using 20TiC reinforcement at 1450 °C. This achievement signifies
notable enhancements, with hardness improving by 4.2% and toughness by 4.56% compared to the
NbC-Ni-4VC4Mo2C cermet.
• Incorporating 10% and 20% TiC led to a reduction in flexural strength. This decrease can be attributed to the
potential saturation of the positive effect of TiC on flexural strength. The maximum flexural strength of
939 N mm−2 was recorded in NbC-Ni-4VC4Mo2C, representing an 11.6% increase compared to the NbC-Ni
cermet.

Acknowledgments

The authors extend their appreciation to the Researchers Supporting Project number (RSPD2024R1072), King
Saud University, Riyadh, Saudi Arabia.

Data availability statement

The data cannot be made publicly available upon publication because no suitable repository exists for hosting
data in this field of study. The data that support the findings of this study are available upon reasonable request
from the authors.

Funding source(s)

This research was funded through Researchers Supporting Project number (RSPD2024R1072), King Saud
University, Riyadh, Saudi Arabia.

ORCID iDs

Abdul Basit https://orcid.org/0000-0001-6189-056X

Malik Adeel Umer https://orcid.org/0000-0003-2623-8474
Yang Shao https://orcid.org/0000-0002-7255-8199

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