Intermetallics 95 (2018) 94–101

Contents lists available at ScienceDirect

Intermetallics
journal homepage: www.elsevier.com/locate/intermet

Heat treatment of laser metal deposited TiAl TNM alloy T

a,∗ b c a
Silja-Katharina Rittinghaus , Ulrike Hecht , Valérie Werner , Andreas Weisheit
a
Fraunhofer Institute for Laser Technology ILT, Steinbachstr. 15, 52074 Aachen, Germany
b
Access e.V., Intzestr. 5, 52072 Aachen, Germany
c
Chair for Laser Technology, RWTH Aachen University, Steinbachstr. 15, 52074 Aachen, Germany

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

Keywords: For the manufacturing of low pressure turbine blades, titanium aluminides are used as structural materials,
A. Intermetallics among them the alloy Ti-43.5Al-4Nb-1Mo-0.1B (at.-%) known as TNM™ alloy. In this study, laser metal de-
B. Annealing position (LMD) was investigated as a potential technology to repair defective, damaged or worn blades, and
Phase transformation process conditions were successfully optimized. However, post-process heat treatment is required to optimize the
C. Casting
microstructure. In this work, different annealing treatments and the resulting microstructures were characterized
Heat treatment
for bulk LMD samples as well as for investment cast reference samples. Annealing temperatures were selected
Laser processing and cladding
D. Microstructure from 1245 to 1290 °C. The results show that annealing at 1290 °C for a duration of 60 min with subsequent
G. Aero-engine components furnace cooling can be used so that the LMD and cast micro-hardness nearly match, albeit with significant
differences in microstructure. Nonetheless, yield strength mismatch can be mitigated and LMD can qualify as
prospective additive repair technology, but also as a manufacturing technology for functional TiAl parts.

1. Introduction
Given their low density, high strength and creep resistance com-
bined with good oxidation resistance, intermetallic TiAl-based alloys
have been qualified for aircraft applications, e.g. for low pressure tur-
bine blades [1–6] which operate at temperatures below 800 °C. Con-
ventional manufacturing but also additive manufacturing (AM) have
been considered for blade production [7] and compete with respect to
materials quality, fly-to-buy ratio and production costs. Additive repair
technologies may contribute to increasing cost effectiveness by offering
a means to repair defective parts and thus lower the scrap rate, but they
may also be envisaged for repairing damaged or worn blades within the
Maintenance, Repair and Overhaul business (MRO). Laser metal de-
position (LMD) is an established repair technology for e.g. parts made
from Ni-based and titanium alloys [8]: a corresponding technology for
repair of TiAl turbine blades is currently being investigated [9]. Crack
free samples with low porosity can be built. Among others, a key
challenge is to devise adequate heat treatment steps which would allow
the industry to match the microstructure and properties between the
substrate and the newly and locally deposited alloy.
In this work we selected the β-solidifying TNM™ alloy with nominal
composition Ti-43.5Al-4Nb-1Mo-0.1B (at.-%) [10–17] for investigating
the response of LMD and cast reference material to different annealing
treatments between 1240 and 1290 °C, as according to [18,19] micro-
structures of cast and forged TNM™ do not differ very strongly under
similar heat treatment conditions while creep strength is in the same
range. Annealing is used to coarsen the excessively fine-grained struc-
ture of the LMD material obtained in the as-built condition. A nearly
lamellar microstructure with a small amount of globular γ-phase is
targeted to achieve a good compromise between strength, ductility,
fracture toughness and creep resistance [20]. The amount and size of
globular γ-grains and of lamellar grains, respectively, are strongly de-
pendent on alloy composition, annealing temperature and holding time.
For the TNM™ alloy, the fraction and size distribution of BCC-B2 (or β0-
phase) sensitively also depend on the heat treatment conditions [14].
As a general rule, lower annealing temperatures favor the formation of
globular γ-grains while longer annealing times increase the amount of
α-phase [21,22]. Measured β0-fractions are decreased with both faster
cooling and increased annealing temperature [11]. Finally, the lamellar
spacing is mainly influenced by the cooling rate applied after annealing.
It decreases with increasing cooling rate [17].
With respect to samples processed with LMD, additional aspects
have to be considered: first, the resulting microstructure is expected to
be very fine, which may lead to accelerated phase transformation ki-
netics during annealing treatments. Secondly, oxygen pick-up is likely
to occur, even if processing is conducted under a protective argon at-
mosphere: the increased oxygen content may change phase transfor-
mation temperatures and stabilize the α2 and α-phases [23,24] while γ-
and β0-phase fractions might decrease. Finally, evaporation of alloying
elements during LMD may cause global or local composition changes in

∗
Corresponding author.
E-mail address: siljakatharina.rittinghaus@ilt.fraunhofer.de (S.-K. Rittinghaus).

https://doi.org/10.1016/j.intermet.2018.02.002
Received 21 September 2017; Received in revised form 23 January 2018; Accepted 2 February 2018
0966-9795/ © 2018 Published by Elsevier Ltd.
S.-K. Rittinghaus et al.
addition to meso-scale segregations inherent to the layer-by-layer pro-
cessing. All these issues will have to be accounted for, when the po-
tential of LMD as additive repair technology is developed and assessed
for TiAl-based alloys in comparison with other technologies, including
multipath welding [25], diffusion bonding [26,27] or diffusion brazing
[28].
The present paper is set out to compare microstructure and micro-
hardness evolution in bulk LMD specimens and cast reference speci-
mens as function of the annealing temperature, duration and cooling
conditions for the TNM™ alloy with nominal composition Ti-43.5Al-
4Nb-1Mo-0.1B (at.-%). As a guideline for experimental parameter se-
lection and the interpretation of experiment results, we used the phase
diagram for Ti-xAl-4Nb-1Mo-0.1B proposed by Ref. [29].
2. Experimental
2.1. Material and LMD
Cast reference samples were produced by centrifugal investment
casting with the nominal composition Ti-43.5Al-4Nb-1Mo-0.1B (at.-%).
LMD samples 4 × 10 × 10 mm3 in size were built out of powder with
the same nominal composition. The powder was produced by TLS
Technik GmbH & Co Spezialpulver KG, which used the EIGA atomiza-
tion process with a delivered particle size distribution ranging from 20
to 90 μm. The resulting actual composition was Ti-44.7Al-4.5-Nb-
1.0Mo-0.15B (at-%) and 600–820 ppm oxygen and is further mentioned
in chapter 3.1. The LMD process was performed in an argon purged
inert gas chamber (O2 < 50 ppm) [9] with inductive preheating of the
processing plane to approx. 850 °C, implemented by sequential eleva-
tion of the induction coil with each layer built. The LMD parameters
applied are listed in Table 1. An alternating hatching strategy was used
for adjacent tracks and layers.
The laser-beam source was a 3 kW Nd:YAG laser. Powder was fed
into the processing zone through a continuous coaxial powder nozzle
with an additional protective inert gas stream of 15 l/min.
2.2. Annealing treatment
Post-processing annealing treatment was performed in a THERM-
CONCEPT KLS 05/13 furnace with 300 l/h argon inert gas flow. Table 2
lists the different heat treatment parameters simultaneously applied to
as-cast and as-built LMD samples.
Air cooling (AC) refers to cooling in air immediately after the re-
spective heat treatment cycle ends, while furnace cooling (FC) refers to
passive cooling in the furnace through controlled temperature decrease
down to 300 °C with a maximum rate of 5 K/min followed by shutdown
of the furnace. After the samples reached 300 °C, they were air cooled to
room temperature. For water quenching (WQ) the samples were re-
moved from the furnace immediately after the heat treatment cycle
ended and quenched in a bucket with approx. 5 l of water at 21 °C. The
time span between opening the furnace and the samples hitting the
water surface was less than 10 s. All second heat treatment steps ended
with FC. While the cooling rate during FC ranged from 5 to 1 K/min, AC
leads to cooling rates in the range of 103 K/min. WQ cooling rates were
not determined.
Table 1
LMD parameters used in this study.
Parameter Symbol Unit Value
Laser beam power P W 60
Laser beam diameter D mm 0.6
Velocity V mm/min 500
Layer thickness d mm 0.2
Powder mass flow M g/min 1.5
95
Intermetallics 95 (2018) 94–101
Table 2
Post-processing annealing treatments: list of parameters.
Parameters, step 1 Parameters, step 2
Temperature °C Holding Cooling- Temperature°C Holding Cooling-
time min time min
1245 240 Air cooling 800 360 FC
(AC)
1265 60 Furnace 1085
cooling
(FC)
1290 20 Water
quenching
(WQ)
2.3. Analysis methods
Chemical composition: the oxygen content of as-cast and as-built
material was analyzed by means of hot gas extraction, while metallic
elements were analyzed with Energy Dispersive X-ray Spectroscopy
(EDX). An independent standard was used for TNM™, previously
characterized by Inductively Coupled Plasma Optical Emission
Spectrometry (ICP-OES). Occasionally and for control reasons selected
samples were additionally analyzed by ICP-OES.
Microstructure analysis was performed using an SEM type Gemini
1550 (Zeiss) equipped with an energy dispersive X-ray system (Oxford
INCA). The samples for microstructure analysis were cut parallel to the
build direction “z”. The SEM was operated in the back scatter electron
mode (BSE) to take advantage of the Z-contrast during image analysis.
Two crystal orientation maps were acquired by Electron Backscatter
Diffraction (EBSD) using the Oxford INCA-Crystal software. The aim
was to compare the as-cast and LMD microstructure obtained after an
annealing treatment of 1290 °C/60 min/FC, specifically to verify the
phase fractions obtained by simple image analysis. For simplicity's sake,
a cubic lattice was used for the γ-phase instead of the tetragonal L10-
lattice.
Image analysis: the lamellar colony size and phase fractions were
determined through image analysis of SEM micrographs using the
Stream Motion Software by Olympus. Lamellar (α2+γ) colonies were
measured both along the longest lamella (referred to as length) and
across the respective colony in direction perpendicular to the lamellae
(referred to as width). For each sample, a minimum of three micro-
graphs was used to obtain representative values. Distorting projection
effects caused by lamellae not being cut perpendicular to the respective
growth direction were neglected. For phase fraction measurements,
regions of interests (ROI) in the SEM micrographs were defined. In cases
of unevenly distributed phases, multiple ROIs were used to detect local
differences. The phases were differentiated corresponding to their
measurable shading (grey scale) in the micrographs. Through manual
definition of limit values, the phase fractions were determined as area
segments. The detected areas were accumulated and expressed as phase
fraction relative to the selected ROI area. Since it is manual, this
measurement procedure is, however, subjective. Therefore, the values
presented here can be considered best estimates rather than hard data.
Changes in grey scale settings by two to three units can increase or
decrease the measured phase fraction by up to ± 4.5%. The phases
determined were β0 (bright), α2 (grey) and γ (dark grey).
Micro hardness: the micro-hardness was measured as HV0.3 using a
Leco semi-automatic Vickers tester with a test load of 300 g and a
testing time of 20 s. The test indentation distance was 0.5 mm.
Measurements were performed in the middle section of each sample
and parallel to the build direction.
S.-K. Rittinghaus et al. Intermetallics 95 (2018) 94–101

Fig. 1. SEM micrographs of TNM alloy in the LMD as-built (a) and as-cast (b) condition, magnification 1000x.

3. Results Table 3
Chemical composition of as-built TNM material (integral), quantified by EDX measure-
3.1. Microstructure and chemical composition in the as-built condition ments (average of a minimum of three measurements).

Material Ti, at.% Al, at.% Nb, at.% Mo, at.% B, at.% O, wt-ppmb
3.1.1. Microstructure
LMD leads to fine-grained microstructures caused by high cooling Powder (EDX) 51.2 43.9 4.0 0.9 a
600–820
rates up to 105 K/min. Microstructure inhomogeneities are associated Powder (ICP- 49.4 44.7 4.5 1.0 0.15
OES)
with local differences in composition and cooling rates in the deposited a
LMD-sample 49.0 45.7 4.4 0.9 1500–2000
tracks/layers compared to interlayer boundary regions. The differences Cast reference 51.0 44.1 4.0 1.0 a
400–600
will be presented and discussed in a dedicated paper along with process
a
and microstructure simulation results. Here, we only state that com- Not traceable.
b
position differences at the level of 0.5 at.% Al are found between layers Analysis by carrier hot gas extraction.

and interlayer boundaries, being the origin of minor microstructure

differences. The following results are mainly representative for layers.
The thin interlayer boundary regions have been excluded as far as
possible.
Fig. 1 presents SEM-BSE images from longitudinal sections of the as-
built (a) and as-cast (b) samples. Both microstructures consist of la-
mellar grains (α2+γ colonies) and intergranular γ -grains as well as
BCC-B2 (β0) grains. The phases can be distinguished in Fig. 1 as follows:
α2 (grey), γ (dark grey) and β0 (light grey/white). In the LMD-sample
the lamellar grain size appears to be one order of magnitude smaller
than the as-cast reference microstructure.
Lamellar (α2+γ) colonies and nearly globular γ-phase with β0 at
colony boundaries are characteristic for as-cast samples. The size of the
lamellar (α2+γ) colonies, measured as the mean from their length and
width, ranges from about 15 μm up to 100 μm with an average of ap-
prox. 20 μm ± 7 μm. Lamellar spacings are measured between < 1
and 5 μm with 0.7 ± 0.5 μm in average. The γ- and β0 phase at colony
boundaries appear in coarse clusters [16]. In the as-built sample (LMD),
similar phases are visible: however, all microstructure components are
smaller: the (α2+γ) colony size ranges from few μm up to 10 μm with
an average value of 6–8 μm, being up to one order of magnitude smaller
than in the as-cast condition. The β0-and γ-grains are much smaller,
blocky and rather uniformly distributed. The average size of γ-grains is
3 μm, while lamellar spacings are well below 1 μm with 0.3 ± 0.1 μm
in average. These features primary result from rapid cooling. As such,
the differences between the as-built and as-cast microstructures may be
judged as significant, amounting to about one order of magnitude for all
characteristic length scales. The purpose of post-processing annealing
heat treatments is to mitigate these differences through coarsening at
temperatures selected within two-phase fields, either (α+γ) or (α+β)
which, according to [27], correspond to temperatures in the range
1230 °C–1300 °C depending on the alloy composition, i.e. the aluminum
content.
3.1.2. Chemical composition
In contrast to reported values in literature [30] for e.g. EBM, no loss
but rather gain in Al is measured for LMD samples; see Table 3. When
measurement errors - up to 0.2 at.% calculated standard deviation – are
considered, Al still increases significantly during the LMD process. A
rise from 44.7 at.% Al to 45.7 at.% Al from powder to the solid LMD
samples, respectively, is confirmed by several control measurements,
both EDX and ICP-OES. Any sources for additional aluminum during
storage or LMD processing have been considered and can be excluded.
The powder particles homogenously consist of the listed elements.
Thus, theoretical considerations of flight characteristics of Al-rich par-
ticles differing from the ones of Ti-rich particles are doubtful. The
melting process and, therefore, evaporation of titanium over aluminum
under special circumstances could provide an explanation. Examination
of this possibility requires information about melt pool temperature and
dynamics, which is currently not available. Hence, the reason why Al
increases or Ti decreases remains unexplained for now.
Oxygen pick-up occurs both during powder production and the LMD
process. Control experiments without inert argon atmosphere result
in > 20,000 wt-ppm oxygen in the LMD material, which is prohibitive
for any application. The other alloying elements are detected in the
expected range according to the nominal composition. Because of
complementary effects Al and oxygen might have on microstructure
transformation, experiments with powder material with decreased Al
content are in progress as well as attempts to further decrease oxygen
pick-up during processing. This will allow to examine the effects of Al
and oxygen increase separately.
3.2. Microstructure after heat treatment – the effects of annealing
temperature and cooling rate
Samples with a size of 4 × 4 × 10 mm3 were annealed at 1245 °C,
1265 °C and 1290 °C for 1 h in argon atmosphere and air cooled in order
to determine the phase region reached at the annealing temperature;
see Fig. 2. While in the cast samples, lamellae start to disintegrate at
1245 °C (Fig. 2b) and nearly completely dissolve at 1265 °C (Fig. 2d),
the aluminum-rich LMD samples keep significant amounts of γ-phase
even up to 1290 °C (Fig. 2a, c, e). Moreover, the β0 phase is nearly
absent in the LMD samples, again in agreement with their increased
aluminum content. At T = 1290 °C the LMD sample is thus in the
(α + γ) phase field while the cast sample is in the (α + β) phase field.

96
S.-K. Rittinghaus et al.
Fig. 2. SEM micrographs of LMD (top) and cast (bottom) samples after annealing at 1245 °C (a, b), 1265 °C (c, d) and 1290 °C (e, f), for duration of 1 h, followed by air cooling,
magnification 1000x.
One can observe in Fig. 2e that interboundary layers possibly consist of
pure α-phase.
Fig. 3 shows samples annealed at 1290 °C for 1 h and subsequently
cooled with different cooling methods: The effect of furnace cooling
(Fig. 3a and b) is distinct, leading to coarser γ-lamellae as well as
coarser γ-grains at colony boundaries. Fig. 3a shows the small amount
of β0 grains formed upon cooling at γ-grain boundaries in the LMD
sample. Lenticular γ inside the β0 regions formed during air cooling is
visible in the cast material. Water quenched samples (Fig. 3e and f) are
roughly similar to air cooled samples (Fig. 3c and d) for LMD and cast
material, both of which show supersaturated α2 and ultrafine γ-la-
mellae.
Both cast and LMD furnace cooled microstructures (Fig. 3a and b)
contain typical, fine (α2+γ) secondary lamellar colonies formed out of
former α-grains. However, in the LMD samples higher amounts of
Fig. 3. SEM micrographs of LMD (top) and cast (bottom) samples after annealing at 1290 °C, 1 h, followed by furnace cooling (a, b), air cooling (c, d), and water quenching (e, f),
magnification 1000x.
97
Intermetallics 95 (2018) 94–101
equiaxed γ-grains and also coarse lamellae are visible. The latter are
ripened primary lamellae which have been stabilized by comparatively
higher Al- and/or oxygen contents and therefore not been dissolved
during annealing. Above mentioned microstructure evolution trends
are confirmed by image analysis data, displayed in Fig. 4 for the la-
mellar spacing and the fraction of β0.
The distribution of lamellar spacings for all conditions is broader in
LMD compared to that of cast material (Fig. 4, left). When the types of
lamellae are separated into coarse and fine, the similarity of fine la-
mellae in LMD and cast lamellae becomes apparent, which is not sur-
prising since they stem from the same solid state transformation event
and exhibit similar phase transformation kinetics.
From the diagram in Fig. 4 (right), it follows that the β0-phase is
completely or nearly absent in the LMD samples after fast cooling. The
significantly smaller amount of β0 in LMD compared to that of cast
S.-K. Rittinghaus et al.
Fig. 4. Lamellar spacings and β0-phase fractions as functions of the cooling medium after annealing at 1290 °C, 60 min.
samples can be attributed to the higher Al-content and/or increased
oxygen content.
The colony size of the LMD sample annealed at 1290 °C, 60 min and
furnace cooled increased from < 10 μm in the as-built condition to
approx. 20 μm. In contrast, no increase in colony size is observed for
annealing treatments at 1245 °C and 1260 °C. Here the lamellar colonies
remain at the same size (7–10 μm approximately). This can be ex-
plained by β- and γ-grains hindering the grain growth of α-grains below
Tγ, solv [3,15]. Above or close to Tγ, solv the γ-phase is at least partially
dissolved and less effective in grain boundary pinning. This means that
annealing temperatures close to γ-solvus (e.g. 1290 °C) are required to
initiate major changes in the LMD microstructure.
3.3. Microstructure after heat treatment – the effect of annealing time
Microstructure coarsening was investigated at an annealing tem-
perature of 1290 °C as function of holding time, followed by furnace
cooling. The microstructures obtained are depicted in Fig. 5.
Short-term heat treatment of 30 min above Tγ, solv leads to grain
coarsening as mentioned in Ref. [31]. In the present work this effect is
obtained after 20 min for both LMD and cast samples (Fig. 6, left). The
microstructures after 60 and 240 min of heat treatment duration of each
Fig. 5. SEM micrographs of LMD (top) and cast (bottom) samples after annealing at 1290 °C for holding times 20 min (a, b); 60 min (c, d), and 240 min (e, f), followed by furnace cooling,
magnification 1000x.
98
Intermetallics 95 (2018) 94–101
material type are similar regarding the size of lamellar colonies and
equiaxed γ-grains under consideration of the variance; however, the
coarse LMD γ-lamellae (undissolved γ at 1290 °C) grow visibly after
240 min and reach widths of up to 5 μm with an average of
3.1 ± 1.2 μm compared to 2.3 ± 0.9 μm after 60 min (Fig. 4, coarse
fraction), while the fine lamellae remain similar. In the cast samples no
significant changes were detected when the annealing time was in-
creased from 60 to 240 min. In both materials the phase fractions do not
significantly change with the holding time in the investigated range and
thus correspond to those presented in Fig. 4 (FC samples).
According to Hall-Petch relationships, the colony growth fits well
with the decrease in measured values of micro-hardness for each ma-
terial separately (Fig. 6, left). Despite obvious differences in colony
sizes, the hardness for both cast and LMD samples is similar at the same
level when heat treated. It seems that the smaller colony size is coun-
terbalanced by larger lamellar spacings [32] and, specifically, the
presence of coarse γ-lamellae undissolved γ at 1290 °C. In summary, the
hardness of the LMD sample and the as cast reference sample is nearly
the same after 60 min holding time, suggesting that some mechanical
properties like yield strength may be comparable, while others, like
creep and fatigue, may still be very different. The higher oxygen con-
tent in LMD material might cause embrittlement and therefore
S.-K. Rittinghaus et al. Intermetallics 95 (2018) 94–101

Fig. 6. Colony sizes and hardness as functions of the annealing time for annealing at 1290 °C, FC.

decreased ductility. One may further envisage heat treatments clearly
above Tγ, solv to complete this investigation.
3.4. Microstructure after heat treatment – the effect of a second annealing
step
When the area of application is taken into consideration, a second
heat treatment step has to be applied to ensure a reliable long term high
temperature performance. Thereby, internal stresses are reduced and
the material is transferred into an equilibrium state. Two temperatures,
800 °C and 1080 °C, were tested and the resulting microstructures were
compared with the respective initial state (Fig. 7). No visible or mea-
surable changes occurred in either the LMD or cast material (Fig. 7c and
d) when they were heat treated at 800 °C for 6 h followed by furnace
cooling. However, when the temperature of this second step was in-
creased to 1085 °C, the formation of secondary β0-phase inside the α2-
lamellae can be observed. The effect is more pronounced in the cast
material with lower aluminum and oxygen content and less pronounced
in the LMD material with higher aluminum and oxygen content. Most
likely, the solubility in the α2 phase changes as the temperature rises
with α2 getting gradually richer in Al and poorer in Ti and Mo.
3.5. Comparison of cast and LMD in the selected heat treatment condition
On basis of the observed microstructure evolution, an annealing
treatment at 1290 °C for 60 min followed by furnace cooling and
eventually a second step at 800 °C for 6 h followed by furnace cooling
for stress relaxation are recommended as a heat treatment for the LMD
material and potentially for hybrid material consisting of cast and LMD
parts. Fig. 8 summarizes the main results in term of micro-hardness and
Fig. 9 summarizes the main microstructural features of LMD and cast
materials, respectively.
Micro-hardness measurements (HV0.3) reveal that the hardness of
both the LMD and the cast material decreases due to the annealing
treatment, and the values equalize around 325 to 350 HV0.3. It is no-
teworthy that the scattering of the micro-hardness is also reduced
during annealing for both materials, involving chemical homogeniza-
tion and microstructure re-formation. The remaining scatter in LMD
material can be attributed to systematic differences between layer and
interlayer regions, the latter showing lower γ-fractions. This is shown in
Fig. 8 (right) along with the associated length scales. The influence of
interboundary effects will be discussed elsewhere in detail.
Finally the differences between LMD and the cast reference material
after the annealing treatment 1290/60min/FC are summarized in

Fig. 7. SEM micrographs before the additional second annealing step (a, b) and after the additional second annealing step at 800 °C/6 h/FC (c, d) and 1085 °C/6 h/FC (e, f) for LMD (top)
and cast samples (bottom). The initial structure (a, b) corresponds to the first annealing step at 1290 °C/1 h/FC, magnification 1000x.

99
S.-K. Rittinghaus et al. Intermetallics 95 (2018) 94–101

Fig. 8. Hardness measurements of LMD and cast samples in the as-processed condition and the annealed condition (1290 °C/1 h/FC). The right hand image displays interlayer boundaries
which explain the systematic hardness variations in the LMD material.

Table 4 and Fig. 9 based on EBSD maps. Measured phase fractions are Table 4
listed in Table 4. Most likely, thin α2 –lamellae are not identified at the Phase fractions of heat treated TNM material (1290 °C/60 min/FC), quantified by EBSD
measurements.
magnification and mapping resolution used, such that the fraction of α2
is given as lower bound with an estimated +3% based on analytical Material α2-Ti3Al, area-% γ-TiAl, area-% β0, area- %
experience, while the fraction of γ as upper bound with an estimated
−3%. The most significant difference relates to the fraction of the β0- LMD-sample 20.2 (+3%) < 79.3 (−3%) 0.5
Cast reference 13.7 (+3%) < 73.8 (−3%) 12.5
phase, which is nearly absent in the aluminum and oxygen rich LMD
samples.
rich (approx. 1 at.-%) and titanium-lean, with the aluminum content
4. Summary and conclusions increased relative to the initial powder material. Additionally, higher
amounts of oxygen have been measured. As a consequence, the alloys
Microstructure evolution of LMD and cast reference material from go to distinct phase regions upon annealing at 1290 °C, i.e. LMD to
the TiAl alloy TNM™ with the nominal composition Ti-43.5Al-4Nb- (γ+α) and cast reference to (α+β), respectively. Nonetheless, this
1Mo-0.1B (at.-%) was investigated as function of annealing treatments annealing temperature is close enough to γ solvus to allow the ex-
performed in the temperature range 1245–1290 °C. Unexpectedly, and cessively fine microstructure obtained from LMD to coarsen and
as yet without explanation, the LMD material proved to be aluminum- achieve nearly the same hardness as in the cast reference material:

Fig. 9. EBSD mapping of LMD (left) and cast samples (right) after annealing at 1290 °C/1 h/FC showing the pattern quality maps (top) and the phase maps (bottom), respectively.
(yellow - γ; pink - α2, red - β0). (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.)

100
S.-K. Rittinghaus et al.
around 325 to 350 HV0.3. Microstructure differences, however, persist
after this annealing as follows:
i. Due to differing chemical composition, the LMD material contains
only minor fractions of β0, which lowers the hardness at room
temperature.
ii. The LMD material displays smaller lamellar colonies (average 20 μm
compared to 60 μm in cast reference) and smaller size of equiaxed γ-
grains, with grain size hardening being counter-balanced by larger
lamellar spacings.
iii. Lamellar spacings are partially larger in the LMD microstructure
since annealing is done in the (γ+α) phase field with pronounced
coarsening of the undissolved γ lamellae. This contributes to low-
ering the hardness. Annealing durations at this temperature should,
therefore, not exceed 60 min.
The present results imply that annealing at 1290 °C/60 min/FC al-
lows the LMD material to homogenize and coarsen such that it reaches
hardness values comparable to cast reference material, despite per-
sisting microstructure differences. A second low-temperature annealing
step at 800 °C for 6 h followed by furnace cooling can be applied
without noticeable changes of the microstructure.
Ongoing investigations are focusing on comparing other mechanical
properties, specifically tensile, creep and fatigue properties in order to
verify the suitability of the LMD process and the proposed annealing
treatment for repair applications. Both bulk and hybrid samples are
currently being tested.
Future investigations shall be extended to include short duration
annealing at temperatures in the range from 1300 to 1320 °C, aiming to
investigate the coarsening of LMD material in the (α + β) phase field.
Acknowledgements
This work was supported by the German Federal Ministry for
Economic Affairs and Energy BMWi [grant number 20T1311].
References
[1] K. Kothari, R. Radhakrishnan, N.M. Wereley, T.S. Sudarshan, Microstructure and
mechanical properties of consolidated gamma titanium aluminides, Powder Metall.
(2007) 21–27 50/1.
[2] E.A. Loria, Quo vadis gamma titanium aluminide, Intermetallics 9 (2001)
997–1001.
[3] D. Hu, X. Wu, M.H. Loretto, Advances in optimisation of mechanical properties in
cast TiAl alloys, Intermetallics 13 (2005) 914–919.
[4] M.H. Loretto, D. Hu, Y.G. Li, Microstructural studies on some ordered Ti-based
alloys, Intermetallics 8 (2000) 1243–1249.
[5] F. Appel, M. Oehring, R. Wagner, Novel design concepts for gamma-base titanium
aluminide alloys, Intermetallics 8 (2000) 1283–1312.
[6] K. Kothari, R.U. Radhakrishnan, N.M. Wereley, Advances in gamma titanium alu-
minides and their manufacturing techniques, Prog. Aero. Sci. 55 (2012) 1–16.
[7] M. Varetti, Design and turbine architectures: AM enabling technologies.
Presentation, ICTM, Aachen, 2015.
[8] I. Kelbassa, Qualification of Laser Metal Deposition of BLISKs Out of Nickel and
Titanium Base Alloys, Ph.D. thesis RWTH Aachen University, 2006.
101
Intermetallics 95 (2018) 94–101
[9] Rittinghaus S.-K., Weisheit A., Mathes M., Garcia Vargas W.: Laser metal deposition
of titanium aluminides – a future repair technology for jet engine blades?. In:
Proceedings of the 13th World Conference on Titanium.
[10] B.P. Bewlay, M. Weimer, T. Kelly, A.U. Suzuki, P.R. Subramanian, The science,
technology, and implementation of TiAl alloys in commercial aircraft engines, MRS
Proc. 1516 (2013).
[11] S. Bolz, M. Oehring, J. Lindemann, F. Pyczak, J. Paul, A. Stark, T. Lippmann,
S. Schrüfer, D. Roth-Fagaraseanu, A. Schreyer, S. Weiß, Microstructure and me-
chanical properties of a forged β-solidifying γ TiAl alloy in different heat treatment
conditions, Intermetallics 58 (2015) 71–83.
[12] E. Schwaighofer, H. Clemens, S. Mayer, J. Lindemann, J. Klose, W. Smarsly,
V. Güther, Microstructural design and mechanical properties of a cast and heat-
treated intermetallic multi-phase γ-TiAl based alloy, Intermetallics 44 (2014)
128–140.
[13] P. Erdely, R. Werner, E. Schwaighofer, H. Clemens, S. Mayer, In-situ study of the
time–temperature-transformation behaviour of a multi-phase intermetallic β-sta-
bilised TiAl alloy, Intermetallics 57 (2015) 17–24.
[14] E. Schwaighofer, M. Schloffer, T. Schmoelzer, S. Mayer, J. Lindemann, V. Guether,
et al., Influence of heat treatments on the microstructure of a multi-phase titanium
aluminide alloy, Pract. Metallogr. 49 (2012).
[15] H. Clemens, W. Wallgram, S. Kremmer, V. Güther, A. Otto, A. Bartels, Design of
novel β-solidifying TiAl alloys with adjustable β/B2-phase fraction and excellent
hot-workability, Adv. Eng. Mater. 10 (2008) 707–713.
[16] W. Wessel, Mikrostrukturelle Untersuchungen der Rissinitiierung und -ausbreitung
in inter-metallischen TiAl-Legierungen unter zyklischer und quasistatischer
Belastung, Dissertation (2011) Kassel.
[17] F. Appel, J.D.H. Paul, M. Oehring, Gamma Titanium Aluminide Alloys. Science and
Tech-nology, Wiley, Weinheim, 2012.
[18] M. Kastenhuber, B. Rashkova, H. Clemens, S. Mayer, Enhancement of creep prop-
erties and microstructural stability of intermetallic β-solidifying γ-TiAl based alloys,
Intermetallics 63 (2015) 19–26.
[19] M. Kastenhuber, B. Rashkova, H. Clemens, S. Mayer, Effect of microstructural in-
stability on the creep resistance of an advanced intermetallic γ-TiAl based alloy,
Intermetallics 80 (2017) 1–9.
[20] Y.W. Kim, JOM 46 (1994) 30–39.
[21] H. Clemens, P. Schretter, W. Glatz, Prakt. Metallogr. 33 (1996) 19.
[22] S.A. Jones, M.J. Kaufman, Acta Metall. Mater. 41 (1993) 387–398.
[23] H. Zhong, Y. Yang, J. Li, J. Wang, T. Zhang, S. Li, J. Zhang, Influence of oxygen on
microstructure and phase transformation in high Nb containing TiAl alloys,
Materials Letters, vol. 83, 2012, pp. 198–201.
[24] Zollinger, J.; Lapin, J.; Daloz, D.; Combeau, H.: Influence of Oxygen on
Solidification Behaviour of Cast TiAl-based Alloys.
[25] M.F. Arenas, V.L. Acoff, The effect of postweld heat treatment on gas tungsten arc
welded gamma titanium aluminide, Scripta Mater. 46 (3) (2002) 241–246.
[26] G. Çam, G. İpekoğlu, K.-H. Bohm, M. Koçak, Investigation into the microstructure
and mechanical properties of diffusion bonded TiAl alloys, J. Mater. Sci. 41 (16)
(2006) 5273–5282.
[27] D. Herrmann, F. Appel, Diffusion bonding of γ(TiAl) alloys: influence of composi-
tion, microstructure, and mechanical properties, Metall. Mater. Trans. A 40 (8)
(2009) 1881–1902.
[28] K. Hauschildt, A. Stark, U. Lorenz, N. Schell, T. Fischer, M. Blankenburg, et al.,
Diffusion brazing of γ-TiAl-alloys: investigations of the joint by electron microscopy
and high-energy X-ray diffraction, MRS Proc. 1516 (2013) 319.
[29] H. Clemens, B. Boeck, W. Wallgram, T. Schmoelzer, L.M. Droessler, G.A. Zicker,
H. Leitner, A. Otto, Experimental studies and thermodynamic simulations of phase
transformations in Ti-(41–45)Al-4Nb-1Mo-0.1B alloys, Mater. Res. Soc. Symp. Proc.
vol. 1128, 2009, p. U03.
[30] J. Schwerdtfeger, C. Körner, Selective electron beam melting of Ti-48Al-2Nb-2Cr:
microstructure and aluminium loss, Intermetallics 49 (2014) 29–35.
[31] M. Schloffer, F. Iqbal, H. Gabrisch, E. Schwaighofer, F.-P. Schimansky, S. Mayer,
A. Stark, T. Lippmann, M. Göken, F. Pyczak, H. Clemens, Microstructure develop-
ment and hardness of a powder metallurgical multi-phase γ-TiAl based alloy,
Intermetallics 22 (2012) 231–240.
[32] G. Cao, L. Fu, J. Lin, Y. Zhang, C. Chen, The relationships of microstructure and
properties of a fully lamellar TiAl alloy, Intermetallics 8 (5–6) (2000) 647–653.