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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 similar heat treatment conditions while creep strength is in the same
range. Annealing is used to coarsen the excessively fine-grained struc-
Given their low density, high strength and creep resistance com- ture of the LMD material obtained in the as-built condition. A nearly
bined with good oxidation resistance, intermetallic TiAl-based alloys lamellar microstructure with a small amount of globular γ-phase is
have been qualified for aircraft applications, e.g. for low pressure tur- targeted to achieve a good compromise between strength, ductility,
bine blades [1–6] which operate at temperatures below 800 °C. Con- fracture toughness and creep resistance [20]. The amount and size of
ventional manufacturing but also additive manufacturing (AM) have globular γ-grains and of lamellar grains, respectively, are strongly de-
been considered for blade production [7] and compete with respect to pendent on alloy composition, annealing temperature and holding time.
materials quality, fly-to-buy ratio and production costs. Additive repair For the TNM™ alloy, the fraction and size distribution of BCC-B2 (or β0-
technologies may contribute to increasing cost effectiveness by offering phase) sensitively also depend on the heat treatment conditions [14].
a means to repair defective parts and thus lower the scrap rate, but they As a general rule, lower annealing temperatures favor the formation of
may also be envisaged for repairing damaged or worn blades within the globular γ-grains while longer annealing times increase the amount of
Maintenance, Repair and Overhaul business (MRO). Laser metal de- α-phase [21,22]. Measured β0-fractions are decreased with both faster
position (LMD) is an established repair technology for e.g. parts made cooling and increased annealing temperature [11]. Finally, the lamellar
from Ni-based and titanium alloys [8]: a corresponding technology for spacing is mainly influenced by the cooling rate applied after annealing.
repair of TiAl turbine blades is currently being investigated [9]. Crack It decreases with increasing cooling rate [17].
free samples with low porosity can be built. Among others, a key With respect to samples processed with LMD, additional aspects
challenge is to devise adequate heat treatment steps which would allow have to be considered: first, the resulting microstructure is expected to
the industry to match the microstructure and properties between the be very fine, which may lead to accelerated phase transformation ki-
substrate and the newly and locally deposited alloy. netics during annealing treatments. Secondly, oxygen pick-up is likely
In this work we selected the β-solidifying TNM™ alloy with nominal to occur, even if processing is conducted under a protective argon at-
composition Ti-43.5Al-4Nb-1Mo-0.1B (at.-%) [10–17] for investigating mosphere: the increased oxygen content may change phase transfor-
the response of LMD and cast reference material to different annealing mation temperatures and stabilize the α2 and α-phases [23,24] while γ-
treatments between 1240 and 1290 °C, as according to [18,19] micro- and β0-phase fractions might decrease. Finally, evaporation of alloying
structures of cast and forged TNM™ do not differ very strongly under 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. Intermetallics 95 (2018) 94–101
2. Experimental
2.3. Analysis methods
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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.
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S.-K. Rittinghaus et al. Intermetallics 95 (2018) 94–101
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 equiaxed γ-grains and also coarse lamellae are visible. The latter are
pure α-phase. ripened primary lamellae which have been stabilized by comparatively
Fig. 3 shows samples annealed at 1290 °C for 1 h and subsequently higher Al- and/or oxygen contents and therefore not been dissolved
cooled with different cooling methods: The effect of furnace cooling during annealing. Above mentioned microstructure evolution trends
(Fig. 3a and b) is distinct, leading to coarser γ-lamellae as well as are confirmed by image analysis data, displayed in Fig. 4 for the la-
coarser γ-grains at colony boundaries. Fig. 3a shows the small amount mellar spacing and the fraction of β0.
of β0 grains formed upon cooling at γ-grain boundaries in the LMD The distribution of lamellar spacings for all conditions is broader in
sample. Lenticular γ inside the β0 regions formed during air cooling is LMD compared to that of cast material (Fig. 4, left). When the types of
visible in the cast material. Water quenched samples (Fig. 3e and f) are lamellae are separated into coarse and fine, the similarity of fine la-
roughly similar to air cooled samples (Fig. 3c and d) for LMD and cast mellae in LMD and cast lamellae becomes apparent, which is not sur-
material, both of which show supersaturated α2 and ultrafine γ-la- prising since they stem from the same solid state transformation event
mellae. and exhibit similar phase transformation kinetics.
Both cast and LMD furnace cooled microstructures (Fig. 3a and b) From the diagram in Fig. 4 (right), it follows that the β0-phase is
contain typical, fine (α2+γ) secondary lamellar colonies formed out of completely or nearly absent in the LMD samples after fast cooling. The
former α-grains. However, in the LMD samples higher amounts of significantly smaller amount of β0 in LMD compared to that of cast
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.
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S.-K. Rittinghaus et al. Intermetallics 95 (2018) 94–101
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 material type are similar regarding the size of lamellar colonies and
oxygen content. equiaxed γ-grains under consideration of the variance; however, the
The colony size of the LMD sample annealed at 1290 °C, 60 min and coarse LMD γ-lamellae (undissolved γ at 1290 °C) grow visibly after
furnace cooled increased from < 10 μm in the as-built condition to 240 min and reach widths of up to 5 μm with an average of
approx. 20 μm. In contrast, no increase in colony size is observed for 3.1 ± 1.2 μm compared to 2.3 ± 0.9 μm after 60 min (Fig. 4, coarse
annealing treatments at 1245 °C and 1260 °C. Here the lamellar colonies fraction), while the fine lamellae remain similar. In the cast samples no
remain at the same size (7–10 μm approximately). This can be ex- significant changes were detected when the annealing time was in-
plained by β- and γ-grains hindering the grain growth of α-grains below creased from 60 to 240 min. In both materials the phase fractions do not
Tγ, solv [3,15]. Above or close to Tγ, solv the γ-phase is at least partially significantly change with the holding time in the investigated range and
dissolved and less effective in grain boundary pinning. This means that thus correspond to those presented in Fig. 4 (FC samples).
annealing temperatures close to γ-solvus (e.g. 1290 °C) are required to According to Hall-Petch relationships, the colony growth fits well
initiate major changes in the LMD microstructure. 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
3.3. Microstructure after heat treatment – the effect of annealing time
level when heat treated. It seems that the smaller colony size is coun-
terbalanced by larger lamellar spacings [32] and, specifically, the
Microstructure coarsening was investigated at an annealing tem-
presence of coarse γ-lamellae undissolved γ at 1290 °C. In summary, the
perature of 1290 °C as function of holding time, followed by furnace
hardness of the LMD sample and the as cast reference sample is nearly
cooling. The microstructures obtained are depicted in Fig. 5.
the same after 60 min holding time, suggesting that some mechanical
Short-term heat treatment of 30 min above Tγ, solv leads to grain
properties like yield strength may be comparable, while others, like
coarsening as mentioned in Ref. [31]. In the present work this effect is
creep and fatigue, may still be very different. The higher oxygen con-
obtained after 20 min for both LMD and cast samples (Fig. 6, left). The
tent in LMD material might cause embrittlement and therefore
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.
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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 3.5. Comparison of cast and LMD in the selected heat treatment condition
above Tγ, solv to complete this investigation.
On basis of the observed microstructure evolution, an annealing
treatment at 1290 °C for 60 min followed by furnace cooling and
3.4. Microstructure after heat treatment – the effect of a second annealing eventually a second step at 800 °C for 6 h followed by furnace cooling
step for stress relaxation are recommended as a heat treatment for the LMD
material and potentially for hybrid material consisting of cast and LMD
When the area of application is taken into consideration, a second parts. Fig. 8 summarizes the main results in term of micro-hardness and
heat treatment step has to be applied to ensure a reliable long term high Fig. 9 summarizes the main microstructural features of LMD and cast
temperature performance. Thereby, internal stresses are reduced and materials, respectively.
the material is transferred into an equilibrium state. Two temperatures, Micro-hardness measurements (HV0.3) reveal that the hardness of
800 °C and 1080 °C, were tested and the resulting microstructures were both the LMD and the cast material decreases due to the annealing
compared with the respective initial state (Fig. 7). No visible or mea- treatment, and the values equalize around 325 to 350 HV0.3. It is no-
surable changes occurred in either the LMD or cast material (Fig. 7c and teworthy that the scattering of the micro-hardness is also reduced
d) when they were heat treated at 800 °C for 6 h followed by furnace during annealing for both materials, involving chemical homogeniza-
cooling. However, when the temperature of this second step was in- tion and microstructure re-formation. The remaining scatter in LMD
creased to 1085 °C, the formation of secondary β0-phase inside the α2- material can be attributed to systematic differences between layer and
lamellae can be observed. The effect is more pronounced in the cast interlayer regions, the latter showing lower γ-fractions. This is shown in
material with lower aluminum and oxygen content and less pronounced Fig. 8 (right) along with the associated length scales. The influence of
in the LMD material with higher aluminum and oxygen content. Most interboundary effects will be discussed elsewhere in detail.
likely, the solubility in the α2 phase changes as the temperature rises Finally the differences between LMD and the cast reference material
with α2 getting gradually richer in Al and poorer in Ti and Mo. 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.
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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.)
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