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Effect of WC nanoparticles on the thermal stability and mechanical

performance of dispersion-reinforced Cu composites

Article in Scripta Materialia · January 2023

DOI: 10.1016/j.scriptamat.2022.115030

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Contents lists available at ScienceDirect

Scripta Materialia
journal homepage: www.journals.elsevier.com/scripta-materialia

Effect of WC nanoparticles on the thermal stability and mechanical

performance of dispersion-reinforced Cu composites
Lu Han, Zhang Liu, Liming Yu, Zongqing Ma, Yuan Huang, Yongchang Liu, Zumin Wang *
State Key Laboratory of Hydraulic Engineering Simulation and Safety, School of Materials Science & Engineering, Tianjin University, Tianjin 300350, PR China

A R T I C L E I N F O A B S T R A C T

Keywords: WC dispersion-reinforced Cu composites with high thermal stability were fabricated using intermittent elec­
Cu matrix composites trodeposition and the spark plasma sintering (SPS). WC nanoparticles were dispersed uniformly due to the
Thermal stability formation of the Cu cladding WC structures. The pin and impurity drag mechanisms contributed by the dispersed
Activation energy
WC impeded the migration of grain boundaries. Based on the kinetic analysis, the improved grain-growth
Mechanical properties
activation energy was observed for 3.0 wt% WC-reinforced Cu (up to 376.4 ± 3.7 kJ/mol), which is over
three times higher than that for self-diffusion in pure Cu. The yield strength of this composite increased to 282.9
MPa at 300 ◦ C, which is nine times higher than the value in Cu. This work provides an advanced pathway for
designing thermal stable Cu composites for application as heat sinks.

Owing to their excellent thermal and electrical conductivities, Cu boundaries in composites. Such a characteristic microstructure leads to,
alloys are widely used in electronic engineering as electrical contact in particular, much improved thermal stability of the composites. The
materials, in electrodes for resistance welding [1–5], and as heat sink activation energy for grain growth in the composites has been increased
materials [6–8]. However, their poor mechanical performance at by three times as compared to that in pure Cu. Correspondingly, the
elevated temperatures limit their application as structural materials in high-temperature strength of the composites is nine times higher than
other fields [9]. Moreover, their poor high-temperature performances pure Cu at 300 ◦ C. The underlying mechanisms for such much enhanced
are detrimental to their application as heat sink materials [10,11]. high-temperature performance of the developed composites were also
Nanoparticle dispersion-strengthened Cu composites are among the investigated in detail.
most promising advanced Cu matrix composites (CMCs) with high WC@Cu precursor powders were fabricated via pulse-intermittent
strength and electrical conductivity, and with improved thermal sta­ electrodeposition. The average grain size (AGS) of pristine WC pow­
bility [9,10]. CMCs are fabricated by incorporating second-phase ders was approximately 100 nm, and the powders had a purity of 99.99
nanoparticles, such as Al2O3 [12], Y2O3 [10], TiC [13] and WC [14], wt%. After pretreatment in 20% HNO3 for 10 min, the 0.08, 0.16, 0.22,
and refractory metal particles (for example, Ta [15] and W [6]), into the and 0.32 g/L WC powders were added to the plating solution. The
Cu matrix. Furthermore, discontinuous nanoparticle disperse-reinforced composition of the plating solution was CuSO4⋅5H2O (28 g/L),
Cu composites are key candidates for application as heat sink materials (NH4)2SO4 (50 g/L), C6H8O7 (21 g/L), CuCl2 (0.04 g/L), C7H5O3NS
in magnetic confinement fusion devices in the future [16,17]. Therefore, (0.05 g/L), and PEG-6000 (0.1 g/L). Electrodeposition density was 8.3
the thermal stability and mechanical properties of × 102 A/m2 with ton = 200 μs and toff = 800 μs. The deposition lasted for
dispersion-strengthened Cu composites at high temperatures have 4 min, followed by 2 min of ultrasonic stirring, which was cycled ten
attracted much attention. times. For comparison, pure Cu powders were fabricated using the same
In this study, WC-reinforced Cu composites with different contents of method without the addition of WC powders. After electrodeposition for
WC were fabricated by intermittent pulse electrodeposition combined 40 min, the powders were put in a 15 mm-diameter graphite die and
with the spark plasma sintering (SPS). By careful design of a Cu-cladding sintered using a Labox-300 SPS system. The specimens were kept at
WC structure (WC@Cu), the long-existing problem of agglomeration of 650 ◦ C and lasted for 2 min, followed by an applied pressure of 50 MPa,
WC nanoparticles was circumvented. The WC nanoparticles are homo­ and then heated to 850 ◦ C at a heating rate of 100 ◦ C/min. After sin­
genously distributed both within the Cu grains and at the Cu grain tering, the composites and pure Cu were rolled by 50 % at 800 ◦ C (see

* Corresponding author.
E-mail address: [email protected] (Z. Wang).

https://doi.org/10.1016/j.scriptamat.2022.115030
Received 4 July 2022; Received in revised form 24 August 2022; Accepted 1 September 2022
Available online 7 September 2022
1359-6462/© 2022 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
L. Han et al. Scripta Materialia 222 (2023) 115030

Ref. [14] for further details). To evaluate the influence of WC on grain pole figures (IPFs) of the specimens were obtained using a Sigma 300
growth, the sintered specimens were annealed in an OTF-1200X tube SEM microscope equipped with electron backscattered diffraction
furnace (Hefei Kejing) at different temperatures of 900, 950, and 980 ◦ C (EBSD) system (eFlash FS). The step size was 0.2 μm, and the acceler­
for 1, 2, and 3 h, respectively [18]. ating voltage and beam current were 20 kV and 3 nA, respectively. The
The contents of WC in the specimens were confirmed by the induc­ mechanical properties of the specimens at room temperature were
tively coupled plasma–optical emission spectroscopy (ICP–OES) on a characterized by tensile tests, which were performed on a Zwick Z2.5 TH
Thermo iCAP 7400 system. The densities of the specimens were deter­ universal material testing machine. The high-temperature mechanical
mined using Archimedes’ principle. The microstructures of the powders properties of the specimens were analyzed using an Instron 5582 uni­
and sintered composites were characterized by transmission electron versal material-testing machine. The specimens for the tensile tests had a
microscopy (TEM) using a JEOL JEM-2100 microscope equipped with dog-bone shape, and their surfaces were polished to a mirror-like finish.
an energy-dispersive X-ray spectroscopy (EDS) detector. TEM mea­ The gauge, width, and thickness of the specimens were 3, 2, and 1 mm,
surements were performed at a voltage of 300 kV. Orientation inverse respectively, for room-temperature tests, and 5, 1.5, and 0.8 mm for

Fig. 1. (a) TEM image of WC@Cu powders (0.22 g/L WC), (b) the corresponding EDS maps. (c,e) TEM image of the as-sintered 3.0 wt% WC-reinforced Cu composite
and (d) the corresponding EDS maps of (c). (f) HRTEM image of the interface between the Cu matrix and WC marked in red in (e), with an inset of the FFT pattern of
WC and Cu at the interface region.

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L. Han et al. Scripta Materialia 222 (2023) 115030

high-temperature tests, respectively. The strain rate of the tensile tests at nanoparticles are uniformly distributed both within the Cu grains and at
room temperature and elevated temperatures was 0.3 × 10− 3 s− 1. The the Cu grain boundaries. The uniform distribution of the WC indicates
stains were obtained via the equipped laser extension meter. that the core-shell structures fabricated by intermittent pulse electro­
The microstructures of the obtained WC@Cu powders are shown in deposition significantly reduce the agglomeration of second-phase
TEM images in Fig. 1a and b. The corresponding EDS map in Fig. 1b nanoparticles during sintering. Some WC particles are dispersed at the
indicates that the WC particles were completely coated with Cu. The Cu Cu grain boundaries (GBs) and some are embedded within the Cu grains.
coating layer is uniform with a thickness of approximately 20–30 nm. The HRTEM image (Fig. 1f) of the WC particles embedded in the Cu
The WC contents of the four composites are 1.1, 2.1, 3.0, and 5.0 wt% grain (Fig. 1e) shows that no nanoscopic pores or defects formed at the
(corresponding to 0.6, 1.2, 1.7 and 2.9 vol%), respectively. After SPS, interface of the matrix and the second phase. The presence of a Cu
the densities of the as-sintered pure Cu, 1.1, 2.1, 3.0, and 5.0 wt% WC- wetting layer improved the interface bonding strength.
reinforced Cu composites are 8.83, 8.78, 8.79, 8.82, and 8.90 g/cm3, and The EBSD IPF of pure Cu and the composites with different WC
the corresponding relative densities are 99.0, 98.0, 97.7, 97.6, and contents are shown in Fig. 2. The AGS (d0) of as-sintered specimens was
97.6%, respectively. The microstructure of the 3.0 wt% WC-reinforced obtained. The AGS of pure Cu was 4.0 μm, whereas those of the 1.1, 2.1,
Cu composite is shown in the TEM and high-resolution transmission 3.0, and 5.0 wt% WC-reinforced Cu composites were 2.40, 1.52, 1.48,
electron microscopy (HRTEM) images in Fig. 1c–f. The TEM image (see and 0.70 μm, respectively. The AGSs of the composites are smaller than
Fig. 1c) and the corresponding EDS maps (see Fig. 1d) indicate WC pure Cu, and decreased with increasing WC content. Thus, the EBSD

Fig. 2. EBSD IPFs of (a) pure Cu and the composites with different WC contents (b) 1.1 wt.%, (c) 2.1 wt.%, (d) 3.0 wt.%, and (e) 5.0 wt.%.

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L. Han et al. Scripta Materialia 222 (2023) 115030

results confirmed that the grain growth of Cu during the sintering pro­ The AGS of pure Cu significantly increased from 5.51 to 7.60 μm and
cess was impeded by the dispersed WC particles. then 16.52 μm as the annealing time increased from 1 to 2 h and then 3 h
Fig. 3–f display the EBSD IPFs of the pure Cu and 3.0 wt% WC- (see Fig. 3a–c). Conversely, the grain growth in the composite was
reinforced Cu composite after annealing at 900 ◦ C for 1, 2, and 3 h. significantly hindered with increasing annealing time, from 1.79 to 1.84

Fig. 3. (a–i) EBSD IPFs of pure Cu annealed at 900 ◦ C for 1 h (a), 2 h (b), and 3 h (c), and the Cu-3.0 wt.% WC composite annealed at 900, 950, and 980 ◦ C for 1 h (d,
g,j), 2 h (e,h,k) and 3 h (f,i,l), respectively. (m) The evolution of the AGS (d2-d20) of the Cu-3.0 wt% WC composite at different annealing times of 900, 950, and
980 ◦ C. (n) Arrhenius plots of GB mobility as a function of 1000/T.

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L. Han et al. Scripta Materialia 222 (2023) 115030

μm and then 1.93 μm, respectively (Fig. 3d–f). To understand the effect Table 2
of WC on the thermal stability of the composite, the 3.0 wt% WC- The surface energy of Cu at different temperatures.
reinforced Cu composite was further annealed at 950 and 980◦ C for 1, γs<Cu>(hkl) (J/m2) 0 K* 1173.15 K 1223.15 K 1253.15 K
2, and 3 h, respectively (Fig. 3g–l). The annealing temperatures (T),
111 1.952 1.797 1.790 1.786
annealing time (Δt), and corresponding AGS (d) of the composite are
100 2.166 2.011 2.004 2.000
listed in Table 1. The evolution of the AGS (d2-d20) at different annealing 110 2.237 2.082 2.075 2.071
times at 900, 950, and 980 ◦ C is shown in Fig. 3m. The evolution of the *
The surface energy at 0 K was obtained from Ref. [38].
AGS related to the grain boundary (GB) mobility (Mgb) and GB energy
(γ gb) can be expressed as Eq. (1) [19]:
decreases the total interfacial energy, thus improving the stability of
d2 − d02 = 2Mgb γ gb Δt, (1) GB [28,29]. Thus, the activation energy for the motion of loaded grain
boundaries increased considerably.
where 2Mgb γ gb is obtained from the slopes (ks) of the functions of d2-d20 The engineering stress-strain curves of pure Cu and the hot-rolled
and time (Δt) in Fig. 3m. The value of γgb is approximately 1/3 of the composites with different WC contents at room temperature are
surface energy [20]. The surface energy γ s<Cu>hkl (T) of the specimen at shown in Fig. 4a, and their corresponding strengths and elongations are
temperature T can be calculated according to Eq. (2) [20,21]: shown in Fig. 4c. The strength of the composites is higher than that of
s pure Cu. Furthermore, the strength of the composites increases with
S<Cu>
γ s<Cu>hkl (T) = γ s<Cu>hkl (0K) − 2 × T, (2) increasing WC content, whereas the elongation decreases. The slip dis­
f<Cu> ⋅C0 ⋅[V<Cu> ]3 locations are blocked by the nanoparticles and can migrate through the
lattice by bowing between the WC nanoparticles when the external load
where the surface entropy Ss<Cu> of Cu is 7.72 J/mol⋅K, f<Cu> (0.35) is
is increased [1]. The dislocation line continues to bend around the
the fraction of surface area at the film surface contacting with the
particle and the dislocation can move on, leaving a dislocation loop
ambient, the proportionality constant related to the Wigner-Seitz cell C0
around the bypassed particle. The formation of Orowan dislocation
is 4.5 ⅹ 108 mol− 1/3, and the mole volume V<Cu> of Cu is 7.13 × 10− 6
loops leads to an increase in the lattice distortion energy, thereby
m3/mol. The surface energies of the (111), (100), and (110) planes of Cu
increasing the resistance to dislocation movement [1,30]. The Orowan
at different temperatures are listed in Table 2. Based on the EBSD
strengthening mechanism caused by the WC nanoparticles improves the
orientation inverse pole figure results observed in Fig. 3, there was no
strength of the composite (Fig. 1c). Furthermore, the AGS of the Cu
preferred texture in the annealed composite. Thus, the average surface
matrix decreases with increasing WC content (Fig. 2). The grain
energy of the specimen can be estimated according to Eq. (3):
refinement strengthening mechanism caused by WC nanoparticles
γs<Cu>(111) (T) + γs<Cu>(100) (T) + γs<Cu>(110) (T) further improves the strength of the composite [4,14]. After hot rolling,
γ s<Cu> (T) = , (3) the densities of pure Cu and the 1.1, 2.1, 3.0, and 5.0 wt% WC-reinforced
3
Cu composites increase to 8.88, 8.83, 8.86, 8.90, and 8.96 g/cm3,
The activation energy (Q) of the grain growth related to Mgb can be respectively, and the relative densities are 99.5, 98.5, 98. 4, 98.4, and
expressed as Eq. (4) [19]: 98.2%, respectively. The increase in the density increases the interface
( ) bonding strength between the WC and the Cu matrix, therefore the
− Q
load-transfer efficiency. The strength can be further improved when the
(4)
RT
Mgb = M0 ⋅e , applied load is transferred from the matrix to the rigid WC [31].
Simultaneously, the elongation decreases with an increase in the WC
where M0 is a constant and R (8.314 J mol− 1 K− 1) is the gas constant. content owing to the concentration of stress caused by the distribution of
Therefore, Q can be calculated using the slope of the function of ln Mgb WC particles at the grain boundaries [6]. To fabricate composites with
and (T1) (Fig. 3n). The calculated activation energy was 376.4 ± 3.7 kJ/ high strength and high elongation, the optimal WC content range is
mol, which is much higher than that of grain-boundary self-diffusion 2.1–3.0 wt%. Notably, the yield strength (YS) and elongation of the 3.0
(120.0 kJ/mol) and lattice self-diffusion (203.6 kJ/mol) for Cu [22,23]. wt% WC-reinforced Cu composite are 331.9 MPa and 11.0 %,
The dispersed WC particles anchor the grain boundaries and impede respectively.
their migration, thereby increasing the activation energy of grain The mechanical properties of pure Cu and the 3.0 wt% WC-
growth [24]. According to the impurity drag theories proposed by Lücke reinforced Cu composite at high temperatures of 300–500 ◦ C are
and Detert [25] and Cahn [26], the nanoparticle-containing grain shown in Fig. 4b and d. The YS of pure Cu decreases to 30.2 MPa when
boundaries migrate together with the other migrated grain boundaries. the temperature is increased to 300 ◦ C. In contrast, the YS of the WC-
The grain boundaries loaded with WC nanoparticles migrate more reinforced Cu composite is 282.9 MPa at 300 ◦ C, which is over 9.4
slowly than the “pure” grain boundaries of Cu [27]. According to the times the value of Cu at the same temperature. Furthermore, the YS of
EBSD IPFs in Figs. 2 and 3, many twins are observed in the as-prepared the composite is maintained at 51.6 MPa when the temperature is
and annealing specimens. The twin lamellar thickness (l) decreases with increased to 500 ◦ C. YS of the Cu composites with different reinforce­
the increase of WC contents, and l in the 3.0 wt. % WC reinforced Cu ment phases: carbon nanotube (CNT) [32], different contents of W
composite decreases to even nano-scale. The formation of nano-twin particles [33], Al2O3 nanoparticles [34], and different Cu alloys: CuCrZr
[35] and C11000 Cu [36], at room temperature and 300◦ C in previous
studies are shown in Fig. 4e. The 3.0 wt% WC reinforced Cu fabricated in
Table 1
this work has the optimal comprehensive strength performance at room
The parameters of annealing temperatures (T) and holding time (Δt), and
the corresponding average grain size (d) of 3.0 wt% WC reinforced Cu
temperature and the elevated temperature.
composite. Owing to the increase in the activation energy of grain growth, the
average grain size of the composite (3.0 wt% WC) is much smaller even
T (◦ C) Δt (s) d (μm)
at high temperatures. The strength of the composites at elevated tem­
950 3600 2.07 peratures is improved due to the refinement mechanism attributed to the
7200 2.29
presence of dispersed WC nanoparticles. The strength of the composites
10800 2.53
980 3600 2.48 at elevated temperature is not only affected by the grain size but gov­
7200 2.96 erned by GB stability as well [37]. As mentioned previously, the exis­
10800 3.53 tence of nano-twins reduced GB energy and stabilized the GB structures

5
L. Han et al. Scripta Materialia 222 (2023) 115030

Fig. 4. Engineering stress-strain curves of (a) pure Cu and Cu composites with different WC contents obtained by tensile tests at room temperature, and (b) pure Cu
and 3.0 wt% WC-reinforced Cu at elevated temperatures. (c) YS, tensile strength, and elongation of specimens at room temperature obtained from (a). (d) YS, tensile
strength, and elongation of the pure Cu and 3.0 wt% WC-reinforced Cu at elevated temperatures obtained from (b). (e) Comparison of the YS of the Cu composites at
room temperature and 300 ◦ C fabricated in this work (3.0 wt% WC reinforced Cu, corresponding to 1.7 vol%) and values from previous studies.

as the thermodynamic driving force for grain coarsening is lowered. in pure Cu. The YS of this composite at room temperature and 300 ◦ C
Additionally, the pin and impurity drag mechanisms contributed by the were 331.9 and 282.9 MPa, respectively, which were higher than the
dispersed WC nanoparticles at GBs provide kinetic stabilization. The values of pure Cu at the same temperatures. The dispersed WC nano­
stability of GB is improved, and therefore the elevated-temperature particles anchored the grain boundaries, and the WC dispersed at the
strength of the composite is improved. The presence of nano-twins grain boundaries moved together with the migrating grain boundaries to
also blocks the propagation of slip bands, and the strengthening effect prevent the GB migration. In addition, the existence of nano-twins
of twin boundaries act as strong barriers to dislocation motion [29]. lowers the GB energy. Thereby the thermal stability of the composite
In summary, WC-reinforced Cu composites with uniformly dispersed is improved. The prepared composites are suitable heat sink materials,
WC nanoparticles prepared via pulse-intermittent electrodeposition and especially for future application in magnetic confinement fusion devices.
SPS have high thermal stability. Moreover, the activation energy of
grain growth for the 3.0 wt% WC-reinforced Cu composite was 376.4
kJ/mol, which is more than three times higher than that of GB diffusion

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L. Han et al. Scripta Materialia 222 (2023) 115030

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interests or personal relationships that could have appeared to influence fusion reactor materials, J. Nucl. Mater. 189 (3) (1992) 237–276.
the work reported in this paper. [18] J. Wang, L. Han, X. Li, D. Liu, L. Luo, Y. Huang, Y. Liu, Z. Wang, Supermodulus
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Thermodynamics versus kinetics of grain growth control in nanocrystalline
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This work was supported by the National Natural Science Foundation [20] Z.M. Wang, J.Y. Wang, L.P.H. Jeurgens, E.J. Mittemeijer, Thermodynamics and
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