Materials Science & Engineering A 635 (2015) 118–128

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Laser additive manufacturing of ultrafine TiC particle reinforced

Inconel 625 based composite parts: Tailored microstructures and
enhanced performance
Chen Hong a, Dongdong Gu b,c,n, Donghua Dai b,c, Moritz Alkhayat a, Wolf Urban e,
Pengpeng Yuan b,c, Sainan Cao b,c, Andres Gasser a, Andreas Weisheit a, Ingomar Kelbassa a,
Minlin Zhong d, Reinhart Poprawe a
a
Chair for Laser Technology LLT, RWTH Aachen/Fraunhofer Institute for Laser Technology ILT, Steinbachstraße 15, D-52074 Aachen, Germany
b
College of Materials Science and Technology, Nanjing University of Aeronautics and Astronautics, Yudao Street 29, 210016 Nanjing, PR China
c
Institute of Additive Manufacturing (3D Printing), Nanjing University of Aeronautics and Astronautics, Yudao Street 29, 210016 Nanjing, PR China
d
School of Materials Science and Engineering, Tsinghua University, 100084 Beijing, PR China
e
FH Aachen University of Applied Science, Germany

art ic l e i nf o a b s t r a c t

Article history: Laser metal deposition (LMD) additive manufacturing process was applied to produce ultrafine TiC
Received 25 December 2014 particle reinforced Inconel 625 composite parts. The effects of laser energy input per unit length (LEIPUL)
Received in revised form on microstructure development, densification response, and mechanical performance including wear
11 March 2015
performance and tensile properties were comprehensively studied. A relationship of processing
Accepted 12 March 2015
Available online 20 March 2015
conditions, microstructural characteristics, mechanical performance, and underlying strengthening
mechanisms was proposed for a successful LMD of high-performance Inconel based composite parts.
Keywords: It revealed that using an insufficient LEIPUL of 33 kJ/m lowered the densification behavior of LMD-
Additive manufacturing processed parts, due to the appearance of residual large-sized pores in inter-layer areas of the parts. An
Laser metal deposition
increase in LEIPUL above 100 kJ/m yielded the near fully dense composite parts after LMD. On increasing
Composites
LEIPUL, the TiC reinforcing particles became significantly refined and smoothened via the elevated
Nickel based superalloys
Tensile properties melting of particle surfaces and the dispersion state of ultra-fine reinforcing particles was homogenized
due to the efficient action of Marangoni flow within the molten pool. The dendrites of Ni–Cr γ matrix
underwent a successive change from an insufficiently developed, disordered microstructure to a refined,
ordered microstructure with the increase of LEIPUL. However, the columnar dendrites of the matrix were
coarsened apparently at an excessive LEIPUL of 160 kJ/m because of the elevated thermalization of the
input laser energy. The formation of the refined columnar dendrites of Ni–Cr γ matrix combined with the
homogeneously distributed ultra-fine reinforcing particles contributed to the enhancement of wear
performance of LMD-processed composites with a considerably low coefficient of friction (COF) of 0.30
and reduced wear rate of 1.3
10  4 mm3/N m. The optimally prepared TiC/Inconel 625 composite parts
demonstrated a ductile fracture mode with a sufficiently high tensile strength of 1077.3 MPa, yield
strength of 659.3 MPa, and elongation of 20.7%. The superior tensile properties of LMD-processed parts
were attributed to the significant grain refinement effect of the matrix during laser processing and the
efficient prohibition of ultrafine reinforcing particles on the mobility of dislocations.
& 2015 Elsevier B.V. All rights reserved.

1. Introduction structures has promoted the development of additive manufactur-

ing (AM) (also known as 3D printing, 3DP) technology. Unlike the
In recent years, the demand for production of high- conventional material machining methods, AM/3DP possesses the
performance industrial components with geometrically complex advantages of creating dense parts directly from the feedstock
(typically powder materials) in an entirely opposite philosophy,
i.e., material incremental manufacturing [1–5]. Due to the high
n
Corresponding author at: College of Materials Science and Technology, Nanjing freedom of geometrical design and process manipulation, AM/3DP
University of Aeronautics and Astronautics, Yudao Street 29, 210016 Nanjing,
PR China.
exhibits the outstanding capability of net-shaping user-defined
E-mail addresses: chen.hong@ilt.fraunhofer.de (C. Hong), three-dimensional parts having arbitrary configurations [6–10].
dongdonggu@nuaa.edu.cn (D. Gu). Laser metal deposition (LMD) (also known as laser engineered net

http://dx.doi.org/10.1016/j.msea.2015.03.043
0921-5093/& 2015 Elsevier B.V. All rights reserved.
 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128 119

shaping, LENSs), as a typical AM/3DP process combining laser ceramic particles within the matrix to produce MMCs is expected
cladding and rapid prototyping, has demonstrated its high feasi- to create new technological opportunities for modern industrial
bility in (i) rapid manufacturing and repairing/re-manufacturing applications. MMCs reinforced with discontinuous ceramic rein-
parts with complex geometries; and (ii) preparing coatings to forcements have received extensive research interest within the
modify surface properties of components [11–15]. During the LMD last decades due to their sound high-temperature creep behavior,
process, a high-energy laser beam is focused onto the top surface hot corrosion resistance, wear resistance, etc. Conventionally,
of the work piece to create a molten pool, wherein the powder MMCs parts are produced by powder metallurgy or liquid metal
delivered by the inert gas is steadily injected inside through a processing methods, in which the insufficient densification
coaxial nozzle. The cross-sectional geometry of each layer of the response and inhomogeneous microstructures are most likely to
desired part is built as the work piece moves in the X–Y direction occur. Therefore, the application of novel non-traditional proces-
by a computer-controlled driving system. The component is then sing technology is necessary to produce MMCs with the substan-
created in a layer-by-layer fashion along the Z direction by means tial enhancement of mechanical properties. On the other hand, the
of the unique development method from 2D coating to 3D limited wetting characteristics between ceramic reinforcing
manufacturing. To date, a wide range of refractory alloys, e.g., Ti- phases and metal matrix are regarded as a significant obstacle in
based alloys [16,17], Fe-based stainless steel and tool steel [18,19], achieving the coherent interfacial structures and sufficiently high
and Ni-based superalloys [20,21], have been processed success- mechanical performance. It has been found that the improvement
fully by LMD for manufacturing complex-shaped parts. in the mechanical properties of MMCs is influenced by the size and
Furthermore, recent studies have proved that the LMD process, distribution state of the reinforcement. Refining the reinforcing
due to its unique AM production manner and laser-induced non- particle size can lead to the simultaneous enhancement of
equilibrium rapid melting/solidification mechanism, has a promis- strength and ductility of MMCs [33–35].
ing potential in net-shaping metal matrix composites (MMCs) In our previous work [36,37], the LMD process was applied to
parts with tailored microstructures and high performance. Schoe- produce TiC/Inconel 718 composites using the relatively large micron-
nung et al. [22,23] have produced the dense WC–Co and (Ti,W)C– sized TiC reinforcing particles with the size distribution of 22.5–
Ni MMCs parts from nanostructured WC–Co and (Ti,W)C–Ni 45 μm. In order to improve the interfacial wettability and bonding
powder by using the LENS AM process. Both theoretical and coherence, the in-situ interfacial reaction was tailored between TiC
experiential researches have been carried out to study the thermal reinforcing particles and Ni-based metal matrix. For mechanical
behavior of the LENS process and the mechanisms for the devel- properties, the hardness and wear resistance of LMD-processed TiC/
opment of microstructural and mechanical properties of LENS- Inconel 718 composites were studied. It was found that with an
processed composites. Lavernia et al. [24,25] have deposited optimization of LMD processing conditions, the LMD-processed
IN625-based and Ti6Al4V-based MMCs using LENS with Ni- composites demonstrated a considerably low coefficient of friction
coated TiC reinforcement particles. The integrity of the interface and resultant low wear rate in sliding tests, due to the combined
between matrix and TiC particles and the mechanical properties of strengthening of in-situ interfacial layer and multiple reinforcing
LENS-deposited MMCs are generally improved effectively by using phases. In the present study, the TiC particles with a considerably
Ni-coated TiC particles. Bandyopadhyay et al. [26,27] have applied reduced size distribution were used to reinforce Inconel 625 alloy. The
the LENS process to create Ti–SiC composites on Ti to improve its LMD process was applied to prepare ultrafine TiC particle reinforced
wear resistance. Laser parameters have been found to have a Inconel 625 MMCs parts, which demonstrated the significantly
strong influence on the dissolution of SiC, leading to the in-situ different microstructural and mechanical properties as relative to
formation of Ti5Si3 and TiC with a high amount of SiC on the the Inconel based composites reinforced with large-sized ceramic
surface. In Banerjee et al.'s work [28], MMCs consisting of a particles. The effects of laser energy input per unit length (LEIPUL) on
complex quaternary Ti–35Nb–7Zr–5Ta alloy reinforced by borides the microstructure development, densification response, and mech-
have been deposited from a blend of Ti, Nb, Zr, Ta, and TiB2 anical performance including wear performance and tensile proper-
powders by the LENS process. Wu et al. [29] have fabricated ties are comprehensively studied. In particular, the tensile perfor-
Ti6Al4V/TiB MMCs using the LMD process by injection of pre- mance of LMD-processed Inconel based MMCs has never been
mixed powders of TiB2 and Ti6Al4V. The modulus, yield and studied previously in the existing literature. A relationship between
ultimate strength of Ti6Al4V are increased by the TiB reinforce- processing conditions, microstructural characteristics, and mechanical
ment, but the ductility is decreased. performance was proposed for a successful LMD of Inconel based
Nickel-based superalloys are widely used in applications like MMCs. The underlying strengthening mechanisms were elucidated to
turbine blades and engine components where the combination of obtain high-performance LMD-processed MMCs parts.
superior mechanical property and excellent workability are
required. Inconel 625, a Ni–Cr-based austenite superalloy, is
featured by an improved balance of creep performance, fatigue 2. Experimental procedures
strength, tensile properties, and oxidation resistance, making it an
attractive choice for diverse industrial applications. As a typical 2.1. Powder preparation
material for hot-end components, Inconel 625 has the merits of
maintaining its outstanding mechanical strength and corrosion The gas atomized, spherical Inconel 625 powder with the particle
resistance at both moderate service temperature or up to 650 1C size distribution of 45–95 μm (supplier: Sulzer Metco) (Fig. 1a) and the
[30–32]. The favorable high-temperature performance is con- irregular shaped TiC powder with the refined particle size distribution
trolled mainly by the inherent solid-solution strengthening effect of 5–7 μm (supplier: ABCR GmbH) (Fig. 1b) were used as the starting
of the refractory metal elements such as niobium and molybde- materials. The nominal chemical compositions of Inconel 625 powder
num in Ni–Cr matrix. Nevertheless, with the rapid development of are provided in Table 1. The powder mixture containing Inconel 625
modern industry, Inconel 625 parts with higher performance are powder and 5 wt% TiC powder were mixed in a Fritsch Pulverisette
on increasing demand as the working conditions of components 6 planetary ball mill using a ball-to-powder weight ratio of 5:1, a
become even rigorous in search for a greater efficiency. rotation speed of the main disc of 200 rpm, and a milling time of 8 h.
In order to further enhance the service performance of Inconel The refined TiC particles were dispersed homogeneously around
625 parts, e.g., the elevated strength and wear/tribological resis- Inconel 625 particle surface after ball milling (Fig. 1c). Meanwhile,
tance, the incorporation of hard and temperature-resistant Inconel 625 powder particles did not experience any apparent
120 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128

20μm 1μm

5μm

Fig. 1. Typical morphologies of the starting Inconel 625 powder (a), TiC reinforcing particles (b), and the homogeneously mixed TiC/Inconel 625 composite powder.

Table 1
Chemical compositions of Inconel 625 alloy powder (in weight fraction, wt%).

Ni Cr Mo Nb Fe Co Mn Si Al Ti C P S

58 min 20–23 8–10 3.15–4.15 5 1 0.5 0.5 0.4 0.4 0.1 0.015 0.015

deformation and structural change during the milling process. A sound significant role in determining microstructures and resultant mechan-
flowability of the mixed TiC/Inconel 625 composite powder was ical properties of as-fabricated parts. Through a series of preliminary
accordingly maintained, which was particularly important for a suc- experiments, the laser spot diameter was focused at 1 mm, the laser
cessful LMD process. powers (P) were preset periodically at 500, 800, 500, and 800 W, and
the scan speeds (v) were varied at 900, 900, 300, and 300 mm/min,
2.2. Laser processing respectively. Four different “laser energy input per unit length” (LEIPUL)
of 33, 53, 100, and 160 kJ/m, which was defined by [38]:
The LMD system consisted of a Trumpf Nd:YAG laser system with a LEIPUL ¼ P=v ð1Þ
maximum output power of 3 kW, a powder feeding system, a 5-axis
CNC machine, and a standard optics equipped with a coaxial nozzle. was used to investigate the influence of LMD processing parameters on
The TiC/Inconel 625 composite parts were built by depositing the layer-by-layer deposition process and attendant microstructural and
melted powder onto the prepared C45 carbon steel substrate in a mechanical properties of LMD-processed parts.
powder feeding rate of 2.4 g/min, using argon as the powder carrier gas
as well as the shielding gas to prevent the melt pool from oxidation. 2.3. Microstructure characterization and mechanical properties tests
The multiple tracks were cladded for each layer and multiple layers
were deposited on the substrate to produce the desired 3D parts with a Phase identification of specimens was performed by a Bruker D8
height of 30 mm. For the LMD process, the main parameters including Advance X-ray diffractometer (XRD) with Cu Kα radiation at 40 kV and
laser spot diameter, laser power, and laser scan speed played a 40 mA, using a continuous scan mode. The fabricated composite parts
 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128 121

were cut by a spark-erosion wire cutting machine to obtain cross-

sections. The samples were then inlaid and polished for metallographic
observation in line with the standard procedures. The densification
behaviors were revealed by using optical microscopy (OM). Micro-
structures were characterized using a Hitachi S-4800 scanning electron
microscopy (SEM) with the samples being etched by a solution
containing of HCl (10 ml) and H2O2 (3 ml) for 10 s. EDAX energy
dispersive X-ray spectroscope (EDX) was applied to determine the
chemical compositions, using a super-ultra thin window sapphire
detector. The characteristics of crystal structures of the LMD-
processed samples were further studied by an EDAX high-speed and
high-sensitivity Hikari electron backscatter diffraction (EBSD) camera.
An EDAX OIM data collection and analysis software was applied to
acquire crystallographic data. For specimen preparation for EBSD, the
LMD-processed samples were ground with SiC paper and polished
with diamond suspension down to 1 mm, followed by 1 h polishing
using a Bühler gamma micropolish machine with vibration function. A
FEI Tecnai G2 20 S-TWIN transmission electron microscopy (TEM) was Fig. 2. XRD spectra of LMD-processed TiC/Inconel 625 composite parts, obtained
used to investigate the interior microstructures and strengthening over a wide range of 2θ, using different processing conditions: (a) P¼ 500 W,
v¼ 900 mm/min, LEIPUL ¼33 kJ/m; (b) P¼ 500 W, v ¼300 mm/min, LEIPUL¼
mechanisms of the samples after tensile tests. 100 kJ/m; and (c) P¼ 800 W, v¼ 300 mm/min, LEIPUL ¼160 kJ/m.
The density (ρ) of the LMD-processed TiC/Inconel 625 composite
parts was determined based on the Archimedes' principle. The dry
sliding wear tests on the polished cross-sections of the LMD-
processed parts were conducted in a HT-500 ball-on-disc tribometer
at room temperature 20 1C. A Ø3 mm bearing steel GCr15 ball with a
mean hardness of HRC60 was taken as the counterface material, using
a test load of 6 N. The friction unit was rotated at 560 rpm for 30 min
and the rotation radius was fixed at 2 mm. The coefficient of friction
(COF) was recorded during sliding. The wear volumes (V) of speci-
mens were determined gravimetrically using V¼Mloss/ρ, where Mloss
was the weight loss of specimens after tests and ρ was the density.
The wear rates (ω) were calculated by ω¼ V/(WL), where W was the
contact load and L was the sliding distance. The LMD-processed parts
were cut using a spark-erosion wire cutting machine to prepare
standard specimens for tensile tests, according to the standard ISO
6892-1:2009. The tensile direction was parallel to the laser deposited
layers. The uniaxial tensile tests were performed at room temperature
with a universal testing machine integrated with extensometer
(Zwick Universalprüfmaschine 1488) at a strain rate of 2
10  3/s.
The ultimate tensile strength and elongation were further determined
from the stress–strain curves.

3. Results and discussion

3.1. Constitutional phases

Fig. 3. XRD spectra in the vicinity of the standard diffraction peak of Ni–Cr γ phase
showing the variation of diffraction peaks of LMD-processed TiC/Inconel 625 compo-
The typical XRD patterns of LMD-processed TiC/Inconel 625 com-
site parts using different processing conditions: (a) P¼ 500 W, v¼ 900 mm/min,
posite parts obtained within a wide range of 2θ¼ 30–1101 are depicted LEIPUL¼ 33 kJ/m; (b) P¼ 500 W, v¼300 mm/min, LEIPUL¼ 100 kJ/m; and (c) P¼
in Fig. 2. At all given LEIPUL, the diffraction peaks corresponding to 800 W, v¼300 mm/min, LEIPUL¼160 kJ/m.
Ni–Cr γ matrix phase and TiC reinforcing phase were clearly identified.
In order to exactly investigate the influence of TiC reinforcement on revealed that as the applied LEIPUL increased from 33 to 100 kJ/m, the
diffraction peaks for Ni–Cr γ phase in the composites, XRD character- diffraction peaks for Ni–Cr γ phase became considerably broadened
ization in the vicinity of the 1st (2θ¼ 43.7741) and 2nd (2θ¼50.9921) (Fig. 3) and the intensity showed a significant decrease (Table 2). These
strong peaks for Ni–Cr γ phase was performed, respectively, as depicted phenomena implied that a proper increase in LEIPUL favored the
in Fig. 3. The quantitative determination of 2θ location and intensity of formation of refined crystals and microstructures of Ni–Cr γ phase in
the detected Ni–Cr γ phase are listed in Table 2. The 2θ locations of LMD-processed composites. However, a further enhancement of LEIPUL
diffraction peaks for Ni–Cr γ phase at various LEIPUL generally shifted resulted in the increase of the intensity of Ni–Cr γ diffraction peaks
to lower 2θ angles. According to the Bragg's law [39]: without the apparent broadening of peaks (Fig. 3 and Table 2), which
suggested the coarsening of crystals in this instance with a significantly
2d sin θ ¼ nλ ðn ¼ 1; 2; 3…Þ ð2Þ
elevated laser energy input.
the displacement of 2θ to lower Bragg angles indicated an increase in
the distance between adjacent lattice planes (d), which was believed to 3.2. Densification behavior
be caused by the distortion of lattice due to the incorporation of Ti and
C atoms derived from TiC particles into the Ni–Cr γ lattice. Furthermore, The characteristic microstructures between neighboring layers on
a close comparison of the intensities of Ni–Cr γ phase at different LEIPUL the cross-sections of LMD-processed TiC/Inconel 625 composite parts
122 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128

Table 2
XRD data showing displacement and intensity variations of identified peaks of Ni–Cr γ phase in LMD-processed TiC/Inconel 625 composite parts.

Samples and processing parameters 1st strong peak 2nd strong peak

2θ (deg) Intensity (CPS) 2θ (deg) Intensity (CPS)

Standard 43.774 – 50.992 –

P ¼500 W, v¼ 900 mm/min, LEIPUL¼ 33 kJ/m 43.58 4644.3 50.70 1399.8
P ¼500 W, v¼ 300 mm/min, LEIPUL¼ 100 kJ/m 43.56 2174.7 50.52 374.9
P ¼800 W, v¼ 300 mm/min, LEIPUL¼ 160 kJ/m 43.52 2339.6 50.50 569.9

Micro-pores

500μm 500μm

500μm 500μm

Fig. 4. OM images showing the molten pool configuration and densification behavior of the deposited layers in LMD-processed TiC/Inconel 625 composite parts using
different LMD processing parameters: (a) P¼ 500 W, v ¼900 mm/min, LEIPUL¼ 33 kJ/m; (b) P¼ 800 W, v ¼900 mm/min, LEIPUL¼ 53 kJ/m; (c) P¼ 500 W, v¼300 mm/min,
LEIPUL¼ 100 kJ/m; and (d) P¼ 800 W, v¼ 300 mm/min, LEIPUL ¼160 kJ/m.

under various processing conditions are revealed in Fig. 4. The and the obtained densification rate was as high as 99.0% (Fig. 5a). On
layerwise microstructural features were generally produced, due to further enhancing LEIPUL to 160 kJ/m, the relative density of LMD-
the layer-by-layer incremental manufacturing nature of the LMD processed part slightly increased to 99.5% (Fig. 5a), showing the
process. Fig. 5b depicts the effect of LEIPUL on the average thickness formation of the metallurgically bonded layers free of any micro-
of the deposited layers. On increasing the applied LEIPUL from 33 to pores and micro-cracks (Fig. 4d).
100 kJ/m, the average thickness of the deposited layers increased During the LMD process, a moving molten pool was created by
sharply from 510 to 990 μm; a further enhancement of LEIPUL led to a high-energy laser beam, in which the mixed TiC/Inconel 625 composite
slight increase of the average layer thickness to 1100 μm (Fig. 5b). It powder is injected inside. The sound bonding property obtained in
was accordingly concluded that an increase in laser energy input LMD-processed tracks and layers is guaranteed by the effective diluting
favored the formation of thicker deposited layers during the LMD of the previously solidified materials and the favorable wetting of the
process. The change of the densification rates of the corresponding freshly deposited molten materials with neighboring layers and
parts is depicted in Fig. 5a. At a relatively low LEIPUL of 33 kJ/m, adjacent scanning tracks. Therefore, a sound metallurgical quality of
larger-sized residual pores were observed between the adjacent LMD-processed parts can only be obtained under the coordination of
deposited layers (Fig. 4a). The irregularly shaped molten pools with processing parameters, such as laser power, laser scan speed, powder
the disorderly arranged solidification front were obtained, leaving the feed rate, etc. In the present study, the integrated parameter LEIPUL
insufficient densification response of 96.8% theoretical density (TD) proves to be useful in controlling inter-track/inter-layer metallurgical
(Fig. 5a). On increasing LEIPUL to 53 kJ/m, the configuration of the bonding and resultant densification activity of LMD-processed parts. At
molten pools became clear and regular, showing coherent bonding a relatively low LEIPUL, the operative temperature in the molten pool is
between the neighboring tracks and deposited layers (Fig. 4b). In this low, due to the insufficient thermalization of the absorbed energy from
situation, only a small amount of micro-pores were remained in the laser beam. A limited amount of liquid is generated in the molten pool
deposited layers and the obtained densification level was enhanced to and then solidifies immediately as laser beam moves away, thereby
97.4% TD (Fig. 5a). As LEIPUL increased to 100 kJ/m, the sufficiently restricting the complete spreading of the molten materials on the
strong metallurgical bonding was achieved between the neighboring previously deposited tracks and layers. It accordingly results in the
layers and adjacent scan tracks (Fig. 4c). There were no apparent formation of relatively thin deposited layers with the residual pores in
residual pores formed on the cross-section of LMD-processed part the bonding areas of adjacent tracks and layers (Figs. 4a and 5). As the
 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128 123

sufficiently high LEIPUL was applied for LMD, the significantly elevated
working temperature in the molten pool yields a large amount of liquid
formation by means of the complete melting of matrix metal. Either
chemical concentration gradient or temperature gradient at the solid–
liquid interface may generate surface tension gradient and resultant
Marangoni flow, thereby inducing capillary forces for liquid flow in
conjunction with the reinforcing particles [40,41]. The formation of the
strong stirring behavior in the molten pool induced by Marangoni flow
provides the significant driving forces for the complete spreading of the
molten materials on the previously processed track and layer, thereby
increasing the wetting characteristics of liquid–solid system and
resultant densification response of LMD-processed composite parts
(Figs. 4c, d, and 5a). Therefore, it is reasonable to conclude that the
operating temperature during the LMD process and the attendant
liquid spreading and wetting behavior in the molten pool play a key
role in determining the configuration of molten pool and densification
activity of LMD-processed composite parts.

3.3. Microstructures and compositions

Fig. 6 illustrates the influence of LEIPUL on microstructural evolu-

tions of LMD-processed TiC/Inconel 625 composites observed at a
relatively low magnification. High-magnification characterization was
also carried out on specific positions to reveal microstructures of the
composites, as shown in Fig. 7. At a lower LEIPUL of 33 kJ/m, the
insufficiently developed columnar dendrites were present in LMD-
processed composites, showing a considerably heterogeneous micro-
structure (Fig. 6a). High-magnification observation revealed that the
incorporated reinforcing particles having an original irregular shape
Fig. 5. Quantitative determination of densification rate (a) and average thickness
experienced a severe agglomeration during solidification (Fig. 7a). On
(b) of laser deposited layers in LMD-processed TiC/Inconel 625 composite parts increasing LEIPUL to 53 kJ/m, the disorderly arranged columnar den-
using various LEIPUL. drites in a fragmentized feature were obtained in LMD-processed part

Insufficiently developed Disorderly and

dendrites fragmentized dendrites

Uniformly distributed, refined Relatively coarsened

columnar dendrites columnar dendrites

Fig. 6. FE-SEM images showing typical microstructures on the etched cross-sections of LMD-processed TiC/Inconel 625 composite parts using different processing
parameters: (a) P¼ 500 W, v ¼900 mm/min, LEIPUL ¼33 kJ/m; (b) P¼ 800 W, v¼ 900 mm/min, LEIPUL ¼53 kJ/m; (c) P¼ 500 W, v¼ 300 mm/min, LEIPUL ¼100 kJ/m; and
(d) P¼ 800 W, v¼ 300 mm/min, LEIPUL¼ 160 kJ/m.
124 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128

(Fig. 6b). The reinforcing particles were smoothened on their surfaces surfaces (Fig. 7c). However, care should be taken to control LEIPUL,
and, meanwhile, became dispersed in a microscopic scale (Fig. 7b). As since the columnar dendrites of the matrix have a high tendency
LEIPUL was further elevated to 100 kJ/m, the crystallized columnar to become coarsened as the excessive LEIPUL of 160 kJ/m is
dendrites became uniformly distributed and the primary dendrites applied (Fig. 7d). It has been disclosed that the rearrangement
could be clearly distinguished (Fig. 6c). The surface of TiC reinforcing and attendant distribution of the TiC reinforcing particles are
particles became apparently smoothened and the attendant dispersion highly dependent on the thermal capillary force induced by the
state became much more homogeneous throughout the matrix Marangoni convection within the molten pool. Based on the
(Fig. 7c). Furthermore, it was interesting to note that the average theory established by Arafune and Hirata [42], the dimensionless
diameter of TiC reinforcing particles was significantly refined in the Marangoni number (Ma) can be used to define and evaluate the
scale of several hundred nanometers (Fig. 7c), which indicated the intensity of Marangoni flow:
partial dissolution of the starting micro-sized TiC particles (5–7 μm)
during the LMD process. On further enhancing LEIPUL to 160 kJ/m, the ΔσL
Ma ¼ ð3Þ
severely coarsened columnar dendrites were present in LMD- μd vk
processed structures (Fig. 6d), even though the TiC reinforcing particles
where Δσ is the surface tension difference of Marangoni flow (N/m),
were still refined and homogeneously distributed in the matrix
L the length of free surface, μd the dynamic viscosity (Pa s), and vk is
(Fig. 7d). Table 3 depicts the EDX analysis results of the chemical
the kinematic viscosity (m2/s). Eq. (3) reveals that Ma is inversely
compositions in the inter-dendrite matrix in LMD-processed TiC/
proportional to μd, which is temperature dependant and, normally, a
Inconel 625 composites at various LEIPUL. The contents of matrix
higher working temperature leads to a lower μd [43]. At a relatively
elements (Ni and Cr) and main alloying elements (Mo, Nb, and Fe) of
high LEIPUL, the operative temperature within the molten pool
Inconel 625 did not exhibit any significant change with the variations
elevates apparently, lowering the viscosity μd and accordingly
of LEIPUL. However, as LEIPUL increased from 33 above 100 kJ/m, the
intensifying the Marangoni flow. The liquid capillary forces within
identified content of C element dissolved in the matrix showed at least
double increase. It was noted that a large fraction of incorporated TiC
Table 3
particles became melted on surfaces at a relatively high LEIPUL larger
EDX elemental analysis within areas #1, #2, #3, and #4 in Fig. 7 showing the
than 100 kJ/m (Fig. 7c and d) and the released Ti and C atoms tended to chemical compositions in the inter-dendrite matrix in LMD-processed TiC/Inconel
dissolve in the matrix to form the supersaturated structures. 625 composites.
It is found that the applied LEIPUL plays a crucial role in
Position Element (at%)
determining distribution and morphology of TiC reinforcement
in LMD-processed composites. Using an insufficient LEIPUL ran- Ni Cr Mo Nb Fe Ti C Al
ging from 33 to 53 kJ/m results in the formation of the severe
aggregation of TiC reinforcing particles having a poly-angular Area #1, Fig. 7a 62.50 21.00 4.45 1.14 1.75 1.98 6.06 1.12
morphology (Fig. 7a and b). A reasonable increase in LEIPUL to Area #1, Fig. 7a 55.21 24.21 4.58 1.04 4.48 1.26 8.39 0.83
Area #1, Fig. 7a 50.04 20.02 4.42 1.52 5.54 2.17 16.29 –
100 kJ/m has the capacity to homogenize the distribution state of Area #1, Fig. 7a 57.95 20.89 4.16 1.00 2.97 1.82 11.21 –
reinforcing particles with a significant smoothening of particle

Irregular shaped particles & Partially smoothened

severe agglomeration particle surfaces

3
4

Smoothened, refined particles Further refined particles

& uniform dispersion

Fig. 7. High-magnification FE-SEM images showing composite structures of LMD-processed TiC/Inconel 625 parts using (a) P¼ 500 W, v¼ 900 mm/min, LEIPUL ¼33 kJ/m;
(b) P¼ 800 W, v ¼900 mm/min, LEIPUL ¼53 kJ/m; (c) P¼ 500 W, v¼300 mm/min, LEIPUL ¼100 kJ/m; and (d) P¼ 800 W, v¼ 300 mm/min, LEIPUL ¼ 160 kJ/m.
 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128 125

the pool resulted from the significant Marangoni flow can effectively LEIPUL of 33 kJ/m, the average COF and attendant wear rate of the
accelerate the arrangement rate of reinforcing particles, favoring the LMD-processed part were comparatively high, reaching 0.44 and
homogeneous distribution of the reinforcement throughout the 2.3
10  4 mm3/N m, respectively (Table 4). The worn surface was
inter-dendrite matrix of the finally solidified composites (Fig. 7c considerably rough and consisted of parallel plowing grooves with
and d). Therefore, the distribution state of TiC reinforcement is larger-sized particle-structured fragments (Fig. 8a), implying the
mainly dependant on the interaction between the reinforcing parti- prevailing of severe abrasion wear mechanism in this instance. The
cles and the dynamic Marangoni flow. On the other hand, a larger insufficient densification response of the LMD-processed part due to
volume of melt is obtained within the molten pool as a result of the the formation of residual micro-pores (Figs. 4a and 5a) and the
elevated operative temperature at a higher LEIPUL, thereby improv- presence of the disordered dendritic microstructure (Fig. 6a) with the
ing the rheological properties of the melt in conjunction with the heterogeneous dispersion of poly-angular TiC reinforcing particles
reinforcing particles, due to the elevated wettability of the solid (Fig. 7a) were responsible for the limited wear performance. On
particles by the surrounding melt. Therefore, an increase in LEIPUL increasing the LEIPUL properly to 100 kJ/m, the average COF and wear
favors the significant smoothening and refinement of the initially rate decreased sharply to 0.30 and 1.3
10  4 mm3/N m (Table 4),
irregular TiC reinforcing particles (Fig. 7c and d). In general, the respectively, demonstrating 33% and 43% decrease compared to the
columnar dendrites of the matrix are developed by means of the part processed at 33 kJ/m. The worn surface of LMD-processed part
heterogeneous nucleation of nuclei and subsequent dendrite growth was considerably smooth. The continuously adherent and strain-
during LMD. The internal energy and thermodynamic potentials hardened tribolayer, free of any significant fracturing or local plowing,
caused by heat accumulation are responsible for the microstructure was present in the worn surface (Fig. 8b). In this situation, the
development in LMD-processed composites. A high ratio of G/R is formation of the ordered columnar dendrites of matrix metal (Fig. 6c)
regarded as the driving force for the dendrite nucleation and growth, combined with the homogeneously distributed TiC reinforcing parti-
where G is temperature gradient and R is solidification speed [44]. At cles (Fig. 7c) contributed to the enhancement of wear performance.
a limited LEIPUL caused by a lower laser power or a higher scan At an even high LEIPUL of 160 kJ/m, however, the average COF
speed, the operative temperature produced in the molten pool is increased slightly to 0.36, increasing the resultant wear rate to
relatively low, due to the limited laser energy input or the compara- 1.7
10  4 mm3/N m (Table 4). Although the worn surface was still
tively short laser irradiation time. As a result, a lower G/R ratio is remained dense, the tribolayer on the worn surface was fragmented
obtained, which further inhibits the sufficient development of and the entrapped debris was produced, generating a rough worn
columnar dendrites of matrix metal, producing the heterogeneous surface (Fig. 8c). The decreased wear performance in this instance was
microstructure of LMD-processed composites (Fig. 6a). While at an mainly ascribed to the formation of significantly coarsened columnar
excessive LEIPUL of 160 kJ/m, a large amount of heat is accumulated dendrites of the metal matrix at the excessive laser energy input
around dendrite tips because of the markedly increased thermaliza- (Figs. 6d and 7d).
tion of laser energy. It accordingly provides the sufficient internal
energy and thermodynamic potential for driving the development
and coarsening of the columnar dendrites of the matrix (Fig. 6d). As 3.5. Tensile properties and strengthening mechanisms
the reasonable LEIPUL of 100 kJ/m is set for LMD, the homogeneous
and refined columnar dendrites are well developed (Fig. 6c) and, in The tensile strength and elongation of LMD-processed
this situation, a favorable mode of particle–interface interaction is TiC/Inconel 625 composite parts using the optimal LEIPUL of
realized in the molten pool, i.e., the trapping of the reinforcing 72–100 kJ/m were measured. One batch of tensile experiments
particles by the growing dendrite [45]. The reinforcing particles conducted on each LMD processing condition contained three
having smoothened and refined morphologies are well incorporated specimens and the obtained tensile strength and elongation were
in the growing dendrite trunks and side branches, leading to a the calculated average values. Compared to LMD-processed
homogeneous dispersion of the reinforcing particles in the finally Inconel 625 part without any reinforcing particles (i.e., the tensile
solidified LMD-processed parts (Figs. 6c and 7c). For a comparison, as strength of 840 MPa, the yield strength of 531 MPa, and the
the low LEIPUL of 33 kJ/m is applied, the relatively coarsened, elongation of 16.0% [46]), the LMD-processed TiC/Inconel 625
irregular shaped reinforcing particles are pushed ahead by the composite parts in this study had an apparently improved tensile
growing dendritic interface and have a tendency to travel along with properties of both tensile strength and elongation, with the
the dendrites, resulting in the serious collision of particles and elevated tensile strength of 1077.3 MPa, yield strength of
attendant segregation after solidification. Furthermore, the growth 659.3 MPa, and elongation of 20.7%. The typical morphologies of
direction of the dendrites is significantly disordered or, more the fracture surface of the corresponding LMD-processed TiC/
seriously, the dendrites cannot develop and grow efficiently, caused Inconel 625 composite part is shown in Fig. 9. A low-
by the impediment of the poly-angular and aggregated reinforcing magnification micrograph, which revealed the general overview
particles (Figs. 6a and 7a). of fracture surface, showed a ductile type of fracture of LMD-
processed composite part during tensile tests (Fig. 9a). A high-
3.4. Wear performance – COF, wear rate and worn surface magnification characterization showed that a large amount of
morphology deep and uniform ductile dimples were present on the fracture
surface, having the considerably refined dimple size of 3 μm in
The influence of the applied LEIPUL on wear properties (e.g., COF average (Fig. 9b).
and wear rate) of LMD-processed TiC/Inconel 625 parts is depicted in
Table 4. The characteristic morphologies of the corresponding worn Table 4
surfaces are shown in Fig. 8. For a comparison, the Inconel 625 alloy COFs and wear rates of LMD-processed TiC/Inconel 625 composites using different
LEIPUL.
without any reinforcement was processed using the same LMD
parameters and the COFs measured were typically in the range of LEIPUL (kJ/m) Average COF Wear rate (mm3/N m)
0.50–0.75. The LMD-processed TiC/Inconel 625 composites had an
apparently decreased COF (generally less than 0.45) due to the 33 0.44 2.3
10  4
incorporation of the TiC reinforcement in the matrix. Nevertheless, 53 0.41 2.0
10  4
100 0.30 1.3
10  4
the applied LEIPUL played a key role in affecting the wear perfor- 160 0.36 1.7
10  4
mance of LMD-processed TiC/Inconel 625 parts. At a relatively low
126 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128

Fig. 8. FE-SEM images showing typical morphologies of worn surfaces of LMD-processed TiC/Inconel 625 composite parts using various LEIPUL: (a) LEIPUL ¼33 kJ/m;
(b) LEIPUL¼ 100 kJ/m; and (c) LEIPUL¼ 160 kJ/m.

Fig. 9. FE-SEM characterization of the fracture surface of LMD-processed TiC/Inconel 625 composites at LEIPUL of 100 kJ/m: (a) Low-magnification image showing a ductile
type of fracture. (b) High-magnification micrograph showing the formation of refined ductile dimples.

The ductile fracture mode and attendant increase in tensile of 34.1 mm. For Inconel 625 based composites with the addition of
strength and elongation of the LMD-processed TiC/Inconel 625 5 wt% TiC reinforcement using the same LMD conditions, 5175
composite parts are attributed to the following. grains were counted in this area and the average grain size
The significant grain refinement effect of the matrix, which is decreased markedly to 27.2 mm. Furthermore, the crystallographic
revealed in Fig. 10 from EBSD micrograph: The significant grain features of grain development of Ni–Cr γ matrix became more
refinement effect of LMD-processed composites at a proper regular and uniform in LMD-processed TiC/Inconel 625 compo-
LEIPUL, which was previously disclosed by FE-SEM characteriza- sites (Fig. 10). The elevated degree of grain refinement of compo-
tion (Figs. 6c and 7c), was further approved by EBSD results sites was induced by (i) laser rapid melting/solidification process
(Fig. 10). The quantitative measurement of the average grain sizes and (ii) the pinning effect of the homogeneously dispersed ultra-
was performed within an area of 3 mm2 in LMD-processed fine TiC reinforcing particles upon the crystalline growth of the
structures. For LMD-processed Inconel 625 without reinforcement, metal matrix during LMD (Fig. 7c), which further contribu-
3283 grains were counted in this area, with the average grain size ted to the improvement in strength and ductility properties of
 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128 127

LMD-processed TiC/Inconel 625 composite parts. It reveals that

the presence of the TiC reinforcing particles influences both
crystalline nucleation and crystalline growth of the matrix during
Dislocations
solidification. The reinforcing particles in the molten pool tend to
induce a dragging/pinning effect on the movement of grain and
phase boundaries [47]. Therefore, for the melt in the solidification
system, the impetus for grain growth is weakened and, accord-
ingly, the nucleation rate is enhanced, favoring the formation of
refined crystalline structure.
The above study shows that the fine-grained microstructure of
laser-processed Inconel based parts contributes to the presence of
excellent properties. As Ni-based superalloys are typically applied
at elevated temperatures, the assumed effects of grain refinement
at elevated temperatures are of particular interest. In Wang et al.'s
work on LMD processing of Ni-based superalloy Rene'41 [48,49], a
significantly fine directionally solidified cellular or cellular-
dendrite structure having little features of secondary dendrite 100nm
arms was obtained. The secondary dendrite arm was greatly
suppressed because of the very high temperature gradient and Fig. 11. TEM micrograph showing the interaction of the reinforcing phase with the
dislocations in LMD-processed TiC/Inconel 625 composites.
rapid solidification rate. Extremely fine γ0 precipitates (80–110 nm)
were present in the matrix. High-temperature tensile tests showed
the high-temperature strength and thermo-plasticity of LMD- and Mo metallic elements, had a smooth surface and a consider-
processed Rene'41 at 800 1C exceeded considerably as relative to ably refined size of  200 nm, exhibiting a clean and compatible
the minimum specifications for commercially Rene'41, revealing interface between the reinforcing particles and the matrix. TEM
that the effects of grain refinement of Ni-based superalloys are micrograph also revealed that the ultra-fine reinforcing particles
also effective at elevated working temperatures. could act as the pinning points in the crystals that opposed the
The efficient prohibition of ultrafine reinforcing particles on the motion of dislocations, thereby reducing the dislocation mobility
mobility of dislocations, which is disclosed in Fig. 11 by TEM due to the incorporation of reinforcing particles. Dislocations were
characterization: The interior high-resolution microstructure of further pinned due to stress field interactions with other disloca-
LMD-processed composites was further studied by the TEM tions and reinforcing particles, creating physical barriers from the
method in Fig. 11, in order to have a better understanding of the reinforcing phase along grain/phase boundaries. The strengthen-
effect of ultra-fine reinforcing particles on strengthening effect and ing effect of LMD-processed TiC/Inconel 625 composite parts was
tensile properties enhancement of LMD-processed TiC/Inconel 625 accordingly realized, since the homogeneous incorporation of
composite parts. Typically, the TEM micrograph consisted of the ultrafine reinforcing particles throughout the matrix was an
following microstructural features, i.e., the refined and smooth- efficient method to prevent dislocation motion and propagation,
ened reinforcing particles, the significantly refined crystals of the or make it energetically unfavorable for the dislocation to move
matrix with the crystalline size in a nanometer scale, and the across grain/phase boundaries.
dislocations which were generated across the deformed metal
matrix and were pinned by the reinforcing particles. The chemical
compositions of the reinforcing particle measured by EDX were as 4. Conclusions
follows: C 54.004 at%, Ti 12.165 at%, Cr 1.270 at%, Ni 0.770 at%, Cu
2.670 at%, Nb 23.862 at%, and Mo 5.255 at%. The reinforcing (1) The densification behavior of TiC/Inconel 625 composite parts
particles, identified as titanium carbide dissolved with Cr, Nb, fabricated by LMD was influenced by the applied LEIPUL. Using
an insufficient LEIPUL of 33 kJ/m lowered the relative density
of LMD-processed composite parts, due to the appearance of
residual large-sized pores in inter-layer areas in the finally
solidified parts. An increase in LEIPUL from 100 to 160 kJ/m
yielded the near fully dense composite parts after LMD.
(2) On increasing the applied LEIPUL above 100 kJ/m, the incor-
porated TiC reinforcing particles became significantly refined
and smoothened through the elevated melting of particle
surfaces. An increase in LEIPUL homogenized the dispersion
state of ultra-fine TiC reinforcing particles, due to the efficient
action of Marangoni convection within the molten pool. The
columnar dendrites of Ni–Cr γ matrix underwent a successive
change from an insufficiently developed, disordered micro-
structure to a refined, ordered microstructure with the
increase of LEIPUL. However, the columnar dendrites of Ni–
Cr γ matrix exhibited an apparent coarsening at an excessive
LEIPUL of 160 kJ/m because of the elevated thermalization of
the input laser energy.
(3) A proper increase in the applied LEIPUL to 100 kJ/m led to a
considerably low average COF of 0.30 and reduced wear rate of
Fig. 10. EBSD micrographs showing characteristics of crystal structures of LMD-
1.3
10  4 mm3/N m for LMD-processed composites, due to
processed Inconel 625 without reinforcement and TiC/Inconel 625 composites at the formation of adherent and strain-hardened tribolayer on
LEIPUL of 100 kJ/m. the worn surface during sliding wear tests. The formation of
128 C. Hong et al. / Materials Science & Engineering A 635 (2015) 118–128

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