Journal of Materials Processing Technology 213 (2013) 21912200

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Journal of Materials Processing Technology

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Additive layer manufacture of Inconel 625 metal matrix composites,

reinforcement material evaluation
D.E. Cooper , N. Blundell, S. Maggs, G.J. Gibbons
WMG, International Manufacturing Centre, University of Warwick, Coventry CV4 7AL, UK

a r t i c l e i n f o a b s t r a c t

Article history: While some high performing nickel based superalloys are difcult to process through additive layer
Received 6 March 2013 manufacturing routes, it is considered that more dilute nickel superalloy (in this case Inconel 625) based
Received in revised form 1 June 2013 metal matrix composite may improve high temperature properties, while retaining good weldability
Accepted 24 June 2013
for use in laser melting deposition technologies. In this paper, the effect of 5 wt% additions of 3 differing
Available online 4 July 2013
ceramic reinforcement particles to an Inconel 625 matrix was observed when processed by high powered
laser melting, and compared to the processing characteristics of the pure matrix alloy. It was found that
Keywords:
while additions of silicon carbide increased material hardness by 130%, levels of porosity and cracking also
Additive layer manufacture
Metal matrix composite
increased. The addition of aluminium oxide had no appreciable effect upon material hardness, while also
Inconel 625 compromising the integrity of the material. However additions of titanium carbide resulted in samples of
Nickel superalloy similar density and consistency as the matrix alloy but with 30% increased hardness. However comparison
Titanium carbide of the width of single laser melted tracks of both Inconel 625 and Inconel 625 with titanium carbide
Silicon carbide composite indicated a need to further characterise the process window for this proposed MMC system.
Alumina 2013 Elsevier B.V. All rights reserved.
Laser melting

1. Introduction precipitates (Reed, 2006). It is generally accepted that increasing

High performance nickel based superalloys are in increasing
demand within the aerospace (Kappmeyer et al., 2012) and power
generation (Henderson et al., 2002) as combustion engines reach
ever higher temperatures in the search for greater efciency. How-
ever their high hardness, low thermal conductivity and high work
hardening rates result in alloys which are classed as difcult to
machine or otherwise process using subtractive methods (Thakur
et al., 2009). The additive layer manufacturing (ALM) process, due
to its tool-less nature, its ability to manufacture net or near-net
shape components, and the increased geometric freedom available
(thus enabling lighter weight component designs (Cooper et al.,
2012)), is an attractive processing route for these otherwise dif-
cult to process superalloys. Metal ALM processes are in essence a
repetitive welding process, with successive additions of layers of
weld to form the 3D object. Also, metal ALM components almost
always require heat treatments to relieve residual stresses, hence
many weldability phenomena also occur in ALM processing.
Many of the alloys desired for high temperature applications are
precipitation hardened by additions of titanium and/or aluminium
which form the gamma prime (  ) phase consisting of Ni3 Ti or Ni3 Al
Corresponding author. Tel.: +44 24 7615 1370.
E-mail address: D.E.Cooper@warwick.ac.uk (D.E. Cooper).
the Ti and Al content of a superalloy increases the quantity of
  phase present, and therefore the materials high temperature
properties. However, this also increases its susceptibility to strain
age cracking (Dupont et al., 2009), whereas dilute alloys are more
readily weldable (Henderson et al., 2002). Rowe (2006) describes
strain age cracking as a loss of ductility during precipitation of the
  phase which induce strains which can exceed the ductility of
the alloy. The limit of weldability beyond which the alloy is usu-
ally deemed unweldable is typically where the combined sum of
titanium, aluminium and niobium is approximately 4 at%. Beyond
this the alloy suffers the phenomena of strain age cracking either
during welding, as a result of repeat pass welding, or during post
weld heat treatment (Dupont et al., 2009). This essentially prevents
their manufacture by ALM.
It is postulated that the addition of ceramic particles to form
a metal matrix composite, utilising a solid solution strengthened
(and thus easily weldable) nickel alloy as the matrix, may provide
a material which improves upon the high temperature mechanical
properties of the matrix alloy, yet retains its benecial weldability
characteristics. MMCs hold the potential for signicant benets in
specic strength and stiffness (Wilson and Shin, 2012), which if
successfully realised could allow such a material to compete with
higher performing but unweldable alloys.
While Inconel 625 products are readily available through ALM
processes, the addition of ceramic particles to provide a metal

0924-0136/$ see front matter 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jmatprotec.2013.06.021
2192 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200

Table 1
Build parameters for Inconel 625 reference samples.

Sample Power (W) Scan (m/min)

1 800 6
2 800 7
3 1000 6
4 1000 7

matrix composite provides the potential to increase not only hard-

ness (wear resistance) (Chawla and Shen, 2001), but also high
temperature mechanical properties (Chou, 1993). As the raw mate-
rial for ALM is typically a ne powder (on the order of 10 m Fig. 1. Macro photography of as-deposited Inconel 625 samples (55 m 100 m
to 100 m), the blending of an MMC feedstock at this stage is a layers).
convenient step in the process chain to achieve an MMC mate-
rial, with particulate reinforced MMCs widely regarded as the most Table 2
economically viable (Chawla and Shen, 2001). ALM also provides a Particle size analysis of ceramic reinforcements, obtained by laser diffraction.
near-net/net shape manufacturing route for an MMC material, so Sample D0.1 (m) D0.5 (m) D0.9 (m)
minimising any concerns related to its machinability, making it an
IN625 23.17 31.28 43.76
ideal manufacturing technology for such a material.
Al2 O3 5.85 8.48 14.41
The use of ALM for Inconel 625TiC composites has been evalu- SiC 3.07 4.60 8.10
ated by Zheng et al. (2010) using a blown powder system, but due TiC 0.22 0.44 1.18
to problems with powder delivery/owability, Ni coated TiC par-
ticles were required to ensure a consistent molten pool. The use
of a powder bed deposition process could remove the need for Ni 2.2. Preparation of MMC samples
coating and remove potential overspray, where the proportion
of TiC content actually delivered to the molten pool is difcult to 2.2.1. Powder preparation
determine. To that end, this paper examines the powder bed laser Three ceramic materials were selected for comparison and were
melting of Inconel 625MMC with three potential reinforcements supplied by Pi Kem Ltd., alumina (99% Al2 O3 ,), silicon carbide (95%
(Al2 O3 , SiC and TiC), and their effect on material hardness as an SiC) and titanium carbide (99% TiC). The particle size distributions
indicator to mechanical properties, as well as their inuence on for all powders were measured by laser diffraction techniques,
process characteristics. using a Mastersizer 2000, with Sirocco 2000 dry dispersion system
(Malvern instruments Ltd., UK); results are given in Table 2.
2. Sample manufacture and testing methodology Prior to deposition, the reinforcement powders were each mixed
at 5 wt% (approx. 10 vol%) with Inconel 625 powder, utilising a hori-
2.1. Laser melting of Inconel 625 matrix alloy powder zontal axis ball mill, with alumina jars and milling media, at a speed
of 150 rpm for a duration of 1 h, until powders appeared visually
The manufacture of samples was undertaken using a well mixed. A qualitative examination of all three powder mixtures
bespoke powder-bed deposition system, with a platform was undertaken using SEM, with 6 samples taken from each batch
resolution of 10 m, utilising mild steel substrates of of powder (an example of each is shown in Fig. 2). The Al2 O3 and
80 mm 60 mm 10 mm, which were restrained against thermal SiC mixtures appeared to show even mixing of the matrix and rein-
stress induced deformation. forcement particles; however the signicantly smaller TiC particles
The material to be consolidated was deposited upon the sub- demonstrated a propensity to agglomerate, although individual
strate by a spring loaded steel blade recoater mechanism; with particles are distributed evenly.
the layer thickness set at 100 m. Samples were dened as a series Ball milling of the powders for all samples presented was under-
of parallel lines measuring a total of 10 mm wide by 30 mm long, taken utilising alumina milling jars and media; however to assess
with a hatch spacing between lines of 0.5 mm and a 0.85 mm diam- the impact of utilising alumina ball milling jars and media, a batch
eter laser focal spot (approximately 27% beam area overlap). The of pure Inconel 625 powder was sampled both before and after 1 h
laser source utilised was a 4 kW Ytterbium bre laser (IPG Photon- milling at 150 rpm. A comparison was also made between the com-
ics, UK), coupled with focusing optics and scanning achieved via a position of powders milled in a steel jar, with steel milling media,
Comau Smartlaser remote laser welding robot (Comau, UK). Four and a batch prepared in a rubber jar with steel media. EDS spec-
samples of Inconel 625 alloy (EOS, UK) were deposited using the tra were collected from samples after milling, the results of which
parameters listed in Table 1, for use as a reference material. are shown in Table 3. It can be seen that some contamination of the
The atmosphere within the build chamber was monitored powder has occurred, with higher quantities of both aluminium and
throughout the process, with deposition of each layer commencing oxygen present in the sample from the alumina jar and media, the
with no more than 300 ppm of O2 present, while during deposi-
tion no more than 2000 ppm of O2 was observed for any layer. To Table 3
prevent excessive material deposition at the start and end of each Composition of alloy powder.
track, a linear ramp in and out of laser power was employed over a
Ni Cr Mo Nb Fe Si O Ti Al
distance of 5 mm, with this portion of the sample being disregarded
Measurement error () 0.4 0.2 0.3 0.3 0.1 0.1 0.2 0.1 0.1
during all further analysis.
Inconel 625 reference 62.7 21.7 6.3 5.2 1.3 0.6 2.1 0.1 0.1
Deposition of the samples was conducted until a total of 55 sample
layers (each 100 m thick) had been deposited, with no apparent Alumina jar and media 60.8 21.3 7.1 3.4 1.3 0.5 3.4 0.1 2.1
alteration of the process dynamics, indicating that a steady state Steel jar and media 63.2 22.0 7.5 3.5 1.5 0.5 1.7 0.1 0.1
processing condition had been reached, the samples produced are Rubber jar and steel 64.3 22.3 7.1 3.2 1.4 0.4 1.2 0.0 0.1
media
shown in Fig. 1.
 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200 2193

Table 4
Build parameters for MMC samples.

Sample Power (W) Scan (m/min)

1 800 6
2 800 6.5
3 800 7
4 1000 6
5 1000 6.5
6 1000 7

is more susceptible to removal from the powder surface and trans-

fer to the milling jar/media. The overall effect of alumina additions
or niobium removal should however be fairly low as it is only the
surface of the powder particles which is modied.

2.2.2. Laser melting of Inconel 625 MMC powders

Each material was loaded into the clean deposition system,
and immediately after ball milling to eliminate standing time.
They were then consolidated according to the parameters listed
in Table 4, with the build layout shown in Fig. 3.
Sample deposition was conducted with the same parameters for
each material, and then repeated a second time for each powder;
the chemical composition of the matrix alloy powder is listed in
Table 3, as measured by EDS.

2.3. Optical microscopy, micro and macro-indentation hardness

testing

Samples were sectioned using an abrasive cutting disc (SiC),

before mounting in phenolic resin. Initial grinding of the sample
surface was conducted with 320 grit SiC wet and dry paper, fol-
lowed by 9 m diamond suspension with a rigid grinding disc. A

Fig. 2. Ball milled powder mixtures (a) Al2 O3 , (b) SiC and (c) TiC.

composition of the samples milled in the steel and rubber jars have
not however altered signicantly. The additional Al and O pres-
ence will undoubtedly have at least a small effect upon the nal
composition of all the powders which were milled in this manner
and presented in this paper. For future reference the use of stainless
steel media within steel or rubber jars is therefore recommended as
being more suitable. For all milled samples, the Niobium content is
notably lower than the reference sample, perhaps indicating that it Fig. 3. Example of IN625SiC built samples.
2194 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200

Fig. 5. Optical microscope montages of sample sections, at 2.5 magnication.

nal polishing stage with 3 m diamond and soft polishing cloth

was completed before optical measurement or hardness testing.
Optical micrographs of a cross section through each sam-
ple were taken using a Leica DM400 M microscope with Buehler
Omnimet v 9.0 software to create a montage and so gain an appre-
ciation of the entire section.
For each sample, a series of 9 micro-indentation hardness mea-
surements was taken at regular intervals across its width, to
evaluate the effect of the reinforcement particles upon the mate-
rials hardness. Indents were performed using a Buehler Micromet
5101 micro-indentation hardness tester with Vickers indenter at a
load of 300 g for 10 s. To ensure the small scale of the reinforcing
particulates did not inuence the result, macro-indentation Vickers
hardness measurements were also made, using a Wilson Hardness
432SVD Vickers Hardness tester at a load of 20 kg for 10 s.

2.4. Scanning electron microscopy with EDS

The sample preparation for SEM followed the same procedure as

for optical microscopy, adding a nal polishing stage with 0.05 m
colloidal silica. The presence of ceramic particles was found to pro-
duce a degree of sample charging which affected image quality at
high magnications, therefore all samples were gold sputtered to
improve imaging.
Scanning electron microscopy was conducted using a Carl Zeiss
Sigma Field Emission Gun Scanning Electron Microscope column,
with Oxford Instruments Energy-dispersive X-ray Spectroscopy
detector and Aztec 2.0 analysis suite.
Fig. 4. Macro photography of as deposited samples (a) IN625, (b) IN625Al2 O3 , (c)
IN625SiC and (d) IN625TiC.
2.5. Single track melting and evaluation by stereo microscopy

To further evaluate the use of TiC as a reinforcement material,

and identify if the processing window may differ signicantly from

Fig. 6. SEM images of IN625Al2 O3 MMC.

 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200
Fig. 7. Liquation crack near substrate, and accompanying EDS maps.
Fig. 8. Distribution of elements in IN625Al2 O3 , obtained by EDS mapping.
that of the matrix alloy, a series of single tracks were consolidated
from a single 100 m layer of powder for both the IN 625TiC com-
posite, and the IN625 matrix alloy for comparison. A wide range
of laser powers and speeds (14 kW at 210 m/min) were selected
for the tracks, in order to observe the effect of laser power and
speed on the formation of individual weld tracks. For each parame-
ter combination, 3 repeats were performed, with all the depositions
occurring in a randomised order. The width of each track was mea-
sured utilising a Nikon Model C-LEDS stereo-microscope in order
to compare the parameters utilised with the width of molten track
produced.
Fig. 9. SEM images of IN625SiC MMC.
2195
3. Results and discussion
3.1. Visual inspection of laser melted samples
Fig. 4 shows a visual inspection of sample quality and density
immediately after deposition, the samples displayed were all pro-
duced at 1000 W and 7 m/min, with little visual difference noted
between samples. The Inconel 625 sample shows consistent stable
melting of the material, with a near at top surface. The Al2 O3 com-
posite shows a rough porous top surface, with signicant excess
material build up at either end of the molten tracks, and appar-
ent poor melting indicated by minimal overlap of tracks. Melt
appears to have been violent and less stable than for the pure matrix
material. Notably the oxygen present in the build chamber during
deposition of the Al2 O3 composite was signicantly higher than for
all other samples, up to 4000 ppm rather than 2000 ppm.
The SiC composite has a smooth top surface, although closer
inspection reveals signicant macro-cracking of the sample both
vertical to the substrate and transversely to the laser scanning
direction.
The TiC composite shows a consistent and stable molten track,
with no signicant edge or end of line build-up of material, no
cracking is evident and the top surface is relatively at compared
to the other composite samples, although not quite as consistent
as the IN625 samples.
Build of both the Al2 O3 and SiC samples was interrupted at
between 15 and 20 layers respectively, as excess sample mate-
rial from the uneven top surface obstructed the re-coating process;
build of the TiC composite was voluntarily ended at 40 layers, with
2196 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200

no evidence to indicate that the build could not continue inde-

nitely.

3.2. Optical microscopy

The optical micrographs presented in Fig. 5 provide an appreci-

ation of a representative cross section of each composite material,
compared to the matrix alloy.
Most notably the SiC composite exhibits signicant macro-
cracks which have propagated both horizontally and vertically,
often interconnected in nature. These seem to have formed inde-
pendently of the large porosity voids which are present, and have
clustered preferentially at either edge of the sample, while the
cracks are dominant in the centre of the sample.
The Al2 O3 composite material shows much lower porosity,
although some large defects are present. Cracks are seen at the
interface with the substrate, aligned vertically, and located cen-
trally in several molten tracks. The top surface of the sample can
be seen to be highly irregular, with build-up at the edges, but
under-deposition in the centre (attributable to insufcient powder
deposition in the lee of the higher edges), this irregular deposition
eventually caused the build to fail, as the higher edges protruded
above the next 100 m layer and jammed the recoating mecha-
nism.
The TiC composite can be seen to vary signicantly from the
Al2 O3 and SiC composites, having a relatively consistent top surface
with only minor deviations in height between molten tracks, the
outer edges have not over-built signicantly and material density
appears to be relatively high.

3.3. SEM and EDS

Observation of the vertical interface cracking in the Al2 O3 sam-

ples (Fig. 6) shows them to have occurred at grain boundaries in
the centre of the molten track, it may be concluded to be an exam-
ple of liquation cracking, whereby lower melting point elements
have accumulated in the hottest zone of the cooling weld pool dur-
ing re-solidication, and having lower tensile strength and melting
point than the surrounding material, have failed during subsequent
passes, as described by both Robinson and Scott (1980) and Dupont
et al. (2009). A more detailed examination shown in Fig. 7 indicates
that the edges of the cracks are rich in Nb and Mo, but poor in Ni
and Cr, which would conrm liquation cracking as the cause, as
described by Robinson and Scott (1980), whereby the substrate is
serving as a restraint in the welding process, hence the cracking
appears only within the rst 23 layers.
The porosity present in the sample appears to have a surround-
ing high concentration of aluminium, as can be seen by the lighter
areas in Fig. 6b, and was conrmed by EDS. Coupled with the high
oxygen content noted in the build chamber, this indicates the likely
thermal destruction of the Al2 O3 , releasing oxygen into the process
chamber, and capturing some bubbles formed during solidication.
Examination using EDS mapping (see Fig. 8), of what appeared
to be large irregular shaped defects when viewed with optical Fig. 10. SEM images of IN625TiC MMC.
microscopy, reveals the presence of small clusters of 26 alumina
particles which have remained intact after the melting process,
presumably offering some mutual protection against complete dis- Cracking of the specimens appears not to be particularly aligned
solution in the molten pool when compared with isolated particles. with grain boundaries, freely cutting through grains, nor does it
Fig. 9 shows the SEM micrographs of the IN625SiC compos- appear localised to the high SiC particle concentrations, although a
ite, while SiC particles are obviously present, their distribution is change of crack direction/orientation seems to occur often when it
far from homogenous, forming bands across the sample, which passes through the SiC rich bands.
appear to have acted as heterogeneous nucleation sites, resulting Inspection by SEM of the TiC composite shown in Fig. 10a at rst
in localised columnar growth. The particles are also signicantly appears to have TiC present only in large agglomerations; however
smaller than the original reinforcement particles added to the higher magnication inspection of the samples shows very ne TiC
powder feedstock, indicating either partial or complete dissolution particles that are evenly distributed throughout the matrix, with
during the melting phases, and subsequent re-precipitation. their size rarely exceeding 1 m across. Some TiC is obvious in the
 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200 2197

Table 5
Comparison of key material properties (Werner Marteinssen, 2005).

Material Density Youngs Hardness (HV) Melting Absorptivity to 1064 nm laser radiation Thermal conductivity
(kg m3 ) modulus (GPa) point ( C) (W m1 K1 )

Inconel 8400 207 200 1355 0.230.25 (Boyden and Zhang, 2006) 11.421.3
Al2 O3 3960 220350 12002000 2072 0.68 (Lawrence, 2004) 1628
SiC 3160 386414 24002500 2730 0.70.9 (Zhang and Modest, 1998) 42.5
TiC 4938 310462 26203200 3167 0.46 (Gaard et al., 2006) 1721

form of agglomerations present in the matrix, a closer inspection
shows signicant rounding of the particles edges compared to their
original angular morphology; while backscatter electron images
show a gradient in composition at their surface (Fig. 10b), indi-
cating a degree of dissolution in the matrix alloy during melting.
The nely dispersed particulates shown in Fig. 10c have a differ-
ent morphology, having a 4-point star form, many of which are
less than 0.5 m across, indicating two different behaviours dur-
ing the melt phase. Presumably the agglomerations of particles
have been mutually protected from complete dissolution during
the laser irradiation phase, whilst dispersed particulates have been
either partially or completely dissolved into the liquid melt and
re-formed during cooling.
All the ceramic materials appear to have been melted to some
degree by exposure to the laser beam, and dissolved into the molten
pool; in the case of SiC and TiC, to re-precipitate back as smaller
particles upon cooling and solidication. The greater absorptivity
of ceramics such as TiC to laser radiation than most metallic mate-
rials has been previously noted by Zheng et al. (2010) and explains
the phenomena of TiC particle melting under laser radiation. While
Zheng et al. cite the higher absorptivity of the TiC to laser radiation,
a brief examination of relative melting points, thermal conduc-
tivity and absorptivity coefcients is presented in Table 5, which
corroborates this observation.
3.4. Micro-indentation hardness testing
The mean hardness values for a set of samples processed with
the same laser power and speed (Sample 6, Table 4, 1000 W at
7 m/min) are shown in Fig. 11. Both micro and macro indentation
methods provide similar results, with indent sizes being at least
one order of magnitude larger than the size of the reinforcement
particulates. Fig. 12 shows the relative scale of reinforcement size
and distribution compared to hardness indentations.
The micro-indentation hardness results show a signicant vari-
ation in hardness between the composite materials. It can be seen
that the addition of Al2 O3 to the Inconel 625 matrix has provided
no signicant increase in material hardness. The greatest increase
is seen in the case of IN625SiC, with mean hardness increased
by 129 4% compared to the pure matrix material. The addition
of TiC shows a measurable and consistent improvement of 32 5%
when compared to the matrix alone. Variability of material hard-
ness is signicant in the SiC reinforced material, with a standard
deviation of 99 HV0.3 , while the TiC composite has a standard devi-
ation of 28 HV0.3 , increased by 47% compared to the deviation of
19 HV0.3 for the matrix alloy. This inconsistency can be attributed
to the un-even distribution of TiC at the powder stage, caused by
agglomeration of the relatively small reinforcement particles, com-
bined with the contamination noted earlier from ball milling in

Fig. 11. Mean hardness of composite samples compared to matrix alloy.

2198 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200

alumina containers. In general though, it can be seen from Fig. 12,

that the hardness indentations cover an area including both matrix
and reinforcement, where an even distribution exists.
While the SiC reinforcement did not exhibit the same poor par-
ticle distribution during powder preparation, the examination by
SEM of the material both pre and post hardness test shows a high
level of segregation of the re-formed SiC particulates, explaining
the high variation in material hardness. As can be seen in Fig. 12c
an indent may be performed in a carbide rich or poor area, with a
pre-existing crack or defect. This SiC particle clustering has been
observed in the work of Zimmerman et al. (2002), who found that
clustering occurred above 2 vol% of SiC; although these ALM sam-
ples exhibit a similar increase in hardness, Zimmerman et al. (2002)
noted no signicant cracking or porosity in their MMC produced by
electrodeposition.
There appears to be some difference in opinion as to the bene-
ts of fully melting TiC particulates within a nickel based matrix.
The work of Li et al. (2009) shows that the formation of TiC par-
ticles from elemental powder mixtures is quite possible within a
pure nickel matrix, while Yin et al. (2003) have undertaken super-
high temperature melt casting to form TiC reinforced superalloy
composites in situ. When working with high energy density lasers
of similar wavelength, the results of Li et al. indicated a hardness
of 365 HV for a 20 vol% TiC reinforcement, roughly comparable to
the mean hardness of 395 HV for a 10 vol% TiC composite within
an Inconel 625 matrix shown in Fig. 11. In contrast, both Zheng
et al. (2010) and Wilson and Shin (2012) suggest that excessive
thermal dissolution of the TiC within the alloy matrix would be
detrimental to the composites properties, with Wilson and Shins
results for only minimal dissolution TiC showing an approximate
35% increase in hardness for a 10 vol% TiC composite. However the
hardness improvement for our own Inconel 625TiC 10 vol% com-
posite which has undergone full dissolution of the carbide and its
subsequent re-precipitation is comparable to that of a low dissolu-
tion composite as reported by Wilson and Shin.

3.5. Effect of TiC additions on molten track geometry

As discussed by Yadroitsev et al. (2010) the formation of each

Fig. 12. SEM micrographs of hardness indentations.
individual laser melted track is important within the process as
width, height, consistency and composition of the consolidated
material affects subsequent tracks within that layer, or subsequent
layers deposited on top. Determining the correct combination of
laser power and scanning speed is therefore crucial to the devel-
opment of any new ALM process when developing new parameter
sets for a new material. In determining the process parameters,
an optimum window exists, whereby the material is fully melted
and combined with the substrate, giving a material of high den-
sity; excessive heating will result in inaccurate components, as the
molten pool exceeds the diameter of the laser beam, while insuf-
cient heating can result in balling of the molten track rather than
complete consolidation (Tolochko et al., 2004).
Fig. 13 shows an example of two tracks formed using the same
laser parameters in identical experiments, the rst utilising only the
Inconel 625 alloy powder, the second the pre-prepared IN625TiC
powder mixture. While the IN625 material shows a segmented
melt behaviour, indicating insufcient power or excessive scan-
ning speed, the composite material exhibits a molten track width
far greater than the diameter of the laser beam (0.85 mm), indicat-
ing a much higher energy absorption or heat retention compared
to the alloy alone.
Fig. 14 shows the width difference of the deposited tracks com-
pared to the beam diameter used for each combination of laser
power and scanning speed. For the Inconel 625 alloy an apparent
trend of increasing track width with increasing energy density is
readily apparent (in agreement with Yadroitsev et al.), that is to
 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200 2199

Fig. 13. Stereoscope images of (a) Inconel 625, (b) Inconel 625TiC 5 wt% both at 2500 W and 4 m/min.

Fig. 14. Molten track over/under sizing for IN625 matrix alloy.

say an increase in power or a decrease in scanning speed increases that track widths are generally greater than the equivalent param-
the width of the weld bead. eters for the matrix alloy alone, indicating a greater heat absorption
The same dataset for the IN625TiC composite material (shown or retention in the welding zone. The trend of increasing track width
in Fig. 15) exhibits no apparent trend whatsoever, except to note with increasing energy density which was apparent for the matrix

Fig. 15. Molten track over/under sizing for IN625 + TiC composite.
2200 D.E. Cooper et al. / Journal of Materials Processing Technology 213 (2013) 21912200
alloy and indeed predicted, is not seen with the composite mate-
rial. While the addition of TiC may account for the wider tracks due
to its greater absorptivity of laser radiation, the absence of a dis-
cernible trend indicates that further work is required to optimise
the laser melting process for such a composite material and to fully
understand the processing windows involved.
4. Conclusions
Upon evaluation of the three composite systems investigated,
the addition of titanium carbide to an Inconel 625 matrix was found
to be preferable to additions of either aluminium oxide or silicon
carbide particulates. The TiC composite demonstrates higher den-
sity, an absence of micro cracking, and an appreciable increase
in the material hardness compared to the alternative reinforce-
ments examined in this paper. Compared to contemporary ALM
systems using 200 W lasers with small spot sizes of the order
of 100 m, the use of a higher power beam (4 kW over 850 m
spot size) appears to more readily melt any ceramic particulates
included in the material, when compared to the level of dissolu-
tion shown by the work of Gaard et al. (2006). In the case of SiC
or TiC these appear to reform during the solidication process, but
at a much smaller size than the original particulates. In the case of
Al2 O3 , the oxygen does not remain dissolved in the molten pool as
carbon is able to, so is not present to permit the ceramic to reform,
resulting in a compromised metallic alloy. While TiC was identied
as the most promising reinforcement particulate, an initial exam-
ination of its effect upon laser melted track formation indicates
that even at 5 wt% the dynamics of the laser melting process are
altered signicantly, and so a new process parameter window must
be dened.
If indeed completely dissolving the ceramic does not impact
the mechanical properties signicantly, this may allow for the
production of composites with signicantly smaller ceramic rein-
forcement (<500 nm), which may be benecial to the material
properties, but without the need to utilise nano materials at the
powder processing stage. The hardness results in Fig. 11 would
seem to indicate that this is the case, although further mechani-
cal testing to obtain tensile strength and stiffness properties will
be required to conrm.
It has been generally considered that the Orowan strengthen-
ing effect is not present in most micro-reinforced MMC materials
(Clyne and Withers, 1993), as the particulate reinforcements are
of too great a size and too widely spaced to prevent the motion
of dislocations (Zhang and Chen, 2006). However if particulate
reinforcements on a sufciently small scale can be achieved, the
presence of the Orowan strengthening effect may be reconsidered.
Zhang and Chen (2008) noted that for particles of 1 m the Orowan
effect is minimal, whereas decreasing particle size down to 10 nm
results in signicant improvements to the strengthening effect,
with Orowan strengthening becoming relatively more signicant
than enhanced dislocation density as the method by which proper-
ties are improved as particle size decreases. ALM using micro sized
particulates as the feedstock, where the processing parameters are
such that the laser completely dissolves the ceramic constituents
and re-precipitates them at a smaller scale may well be a viable
process route to such a nano reinforced composite without the
associated hazards and cost of handling such small particulates.
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