Acta Materialia: Dirk Herzog, Vanessa Seyda, Eric Wycisk, Claus Emmelmann
Acta Materialia: Dirk Herzog, Vanessa Seyda, Eric Wycisk, Claus Emmelmann
Acta Materialia: Dirk Herzog, Vanessa Seyda, Eric Wycisk, Claus Emmelmann
Acta Materialia
journal homepage: www.elsevier.com/locate/actamat
a r t i c l e i n f o a b s t r a c t
Article history: Additive Manufacturing (AM), the layer-by layer build-up of parts, has lately become an option for serial
Received 15 February 2016 production. Today, several metallic materials including the important engineering materials steel,
Received in revised form aluminium and titanium may be processed to full dense parts with outstanding properties.
7 July 2016
In this context, the present overview article describes the complex relationship between AM processes,
Accepted 7 July 2016
Available online 20 July 2016
microstructure and resulting properties for metals. It explains the fundamentals of Laser Beam Melting,
Electron Beam Melting and Laser Metal Deposition, and introduces the commercially available materials
for the different processes. Thereafter, typical microstructures for additively manufactured steel,
Keywords:
Additive manufacturing
aluminium and titanium are presented. Special attention is paid to AM specic grain structures, resulting
Metals from the complex thermal cycle and high cooling rates. The properties evolving as a consequence of the
Microstructure microstructure are elaborated under static and dynamic loading. According to these properties, typical
Properties applications are presented for the materials and methods for conclusion.
2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
1. Introduction profound knowledge of the process itself, but also of the micro-
structure resulting from the process parameters and consequently
In contrast to conventional, subtractive manufacturing methods, of the properties of the manufactured parts. From the many tech-
additive manufacturing (AM) is based on an incremental layer-by nologies available, only a handful is able to produce metallic parts
layer manufacturing [1]. As such, most relevant AM technologies that full the requirements of industrial applications. In this over-
commonly use powder or wire as a feedstock which is selectively view, the relationship between process, microstructure and prop-
melted by a focused heat source and consolidated in subsequent erties is studied in detail for three AM technologies with the
cooling to form a part [2,3]. AM has attracted much attention over highest industrial relevance at the moment, Laser Beam Melting
the past ten years due to its immanent advantages, such as unri- (LBM), Electron Beam Melting (EBM), and Laser Metal Deposition
valled design freedom and short lead times [4]. AM techniques have (LMD).
already been known for more than 20 years [5] but were at rst
limited to the rapid manufacturing of porous structures and pro- 2. Additive manufacturing methods
totypes. With the advancement of technology, part density and
quality improved and rst applications in tool inserts with AM methods can essentially be classied by the nature and the
conformal cooling evolved [6], as well as medical applications, e.g. aggregate state of the feedstock as well as by the binding mecha-
in the form of dental prostheses [7]. Today, it has become possible nism between the joined layers of material [10,11]. In AM of metals
to reliably manufacture dense parts with certain AM processes and a powder feedstock or more rarely a wire is fully melted by the
for a number of materials, including steel, aluminium and titanium energy input of a laser or electron beam and transformed layer by
[8]. layer into a solid part of nearly any geometry.
Thus, AM transforms more and more from rapid prototyping to The most popular processes for AM of metals are Laser Beam
rapid manufacturing applications [9], which require not only Melting (LBM), Electron Beam Melting (EBM) and Laser Metal
Deposition (LMD). The process of LBM is also known as Selective
Laser Melting (SLM) [12], Direct Metal Laser Sintering (DMLS) [13],
LaserCUSING [14], Laser Metal Fusion (LMF) [15] or industrial 3D
* Corresponding author. printing. Widely used synonyms for the description of the LMD
E-mail address: dirk.herzog@tuhh.de (D. Herzog). process are amongst others Direct Metal Deposition (DMD) [16],
http://dx.doi.org/10.1016/j.actamat.2016.07.019
1359-6454/ 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
372 D. Herzog et al. / Acta Materialia 117 (2016) 371e392
Fig. 1. Schematics of an LBM machine (left), and of the three process steps iterated during the build (right).
Fig. 5. Section of three layers of LMD-produced austenitic stainless steel (316L) in as-
fabricated condition (from Yadollahi et al. [66]), revealing the footprint of the laser
tracks.
atomization. Especially in the eld of Ti and Ti alloys, low-cost
processes e.g. electrolytic methods, metallothermic processes (e.g.
TIRO process) and the hydride-dehydride process are under
development or already used for cost-effective metal powder
production [43].
The different powder production methods result in different
powder characteristics such as particle morphology, particle size
and chemical composition each of which might be important for
AM. In principle, the AM process requires good ow properties in
order to achieve homogeneous spreading of the powder as well as
good packing characteristics for the formation of a powder layer
with high relative density. These powder characteristics impact the
bulk material properties of the fabricated component such as part
density and porosity.
The most simple and low-cost atomization process is water at-
omization. In this process, liquid metal is atomized by water jets
when free falling through the atomization chamber. Due to the high
cooling rate the particles with a size of a few mm up to 500 mm
adopt an irregular shape during solidication [44]. According to
German [45], an irregular, asymmetric particle shape is at a
disadvantage of high packing density. Thus, these kinds of particles
are not preferred for the use in AM. Compared to gas atomized
powders water atomization yields powder particles with higher
oxygen content [46]. Concerning the application of the produced
metal powder in AM oxygen uptake and the formation of oxide
layers are undesired effects as they not only inuence the powder Fig. 6. TEM bright-eld image revealing dislocations, stacking fault traces and defor-
ow behaviour but also impact the melt pool and consequently mation twin faults (tf) in 17-4PH LBM as-fabricated condition (from Murr et al. [50]).
The selected area electron diffraction pattern reveals a composition of austenite and
martensite.
Fig. 4. Fine-grained microstructure of maraging steel (18Ni-300) in LBM as-fabricated condition (from Kempen et al. [71]), a) top view, b) cross-section, c) magnication of dendritic
structure.
D. Herzog et al. / Acta Materialia 117 (2016) 371e392 375
Fig. 7. Reaustenitization of an LBM-produced specimen of maraging steel during aging at 480 C/5 h (from Ja
gle [72]). Location of atom probe tomography (APT) measurement (a),
and concentration prole along the cylinder shown in (a) for the elements Ni, Co, Mo and Ti (b).
change the bulk material composition and the parts mechanical 3.2. Steels
properties [47]. Obviously, water atomization is not suitable for
reactive materials such as Ti, and the most typical material to be Steel is still the most common engineering material [54].
water atomized is steel [48]. Therefore, steel is obviously also a material of high interest for AM.
To overcome the limitations of water atomization, i.e. the suit- Steel grades available for LBM are mainly common austenitic
ability only for non-reactive materials and the non-spherical par- stainless steels (AISI 316L/EN: 1.4404/X2CrNiMo17-12-2 [55e68]
ticle shape, gas atomization is usually used for producing feedstock and AISI 304L/EN: 1.4306/X2CrNi19-11 [69,70]), maraging steel
for AM. The risk of oxidation is reduced by using an inert gas, such (18Ni-300/1.2709/X3NiCoMoTi18-9-5) [71e74], as well as precipi-
as argon or nitrogen, for atomization of the melt and thus gas at- tation hardenable stainless steels (17-4 PH/EN: 1.4542/X5CrNi-
omization is the preferred method for reactive materials such as Ti, CuNb16-4/AISI: 630 [49,50,58,75,76] and 15e5 PH/EN: 1.4545/
however the method may of course also be used for non-reactive X5CrNiCu15-5 [77]). Besides, a martensitic cutlery grade (AISI 420/
materials such as steel. The particular choice of inert gas in- EN: 1.4034/X46Cr13) has also been investigated for LBM usage
uences the development of the microstructure of the particles and [78,79], while in EBM mainly tool steels (H11/EN: 1.2343/
consequently does also affect the microstructure of the parts X37CrMoV5-1 [80] and H13/EN: 1.2344/X40CrMoV5-1 [81]) as well
manufactured via AM. Experimental work [49,50] revealed that the as austenitic stainless steel (316L) [34] have been used. For LMD,
type of gas used for the atomization inuences the phase compo- the use of austenitic stainless steel (316L) [66,82,83] and tool steel
sition of the powder. Nitrogen and argon have been used to atomize (H13) [84] is also reported. The alloys described above satisfy
steel, yielding different phase compositions in the powder, and typical requirements of general-purpose applications, as well as
consequently also in the AM fabricated steel parts. The micro- increased requirements on strength and hardness, e.g. for mould
structure of the steel parts, however, has also been found to depend and tool applications.
on the choice of the inert gas in the AM process chamber (cf. Sec- On the one hand, the allotropy of iron based alloys in combi-
tion 2.1). nation with the high temperature gradients involved in AM offers
The melt for gas atomization can either be produced by vacuum the potential to generate unique microstructures [49]. On the other
induction melting or may be from a rod which is liqueed by hand, alloys that can produce different phase compositions
electrode induction melting (cp. Electrode induction melting gas depending on cooling rate, e.g. martensite and retained austenite in
atomization, EIGA) [51]. Especially for the production of high-purity precipitation hardening steels [50], will be sensitive to choice of AM
and reactive powder materials, e.g. titanium and its alloys, the parameters, and thus need a careful control of these.
dispension with a ceramic crucible may be benecial. Due to
cooling in an inert gas atmosphere heat conduction between the
3.3. Aluminium alloys
metal and the surrounding gas allows formation of spherical
powder particles. The size of the particles produced by EIGA is
The number of different Al alloys available for AM is still rather
equivalent to particle sizes of water atomized powders, irrespective
limited. One reason is, that Al is e unlike e.g. Ti e comparatively
of the material [44].
easy to machine and the costs of Al parts are comparatively low
Other processes used for production of spherical metal powders
[85]. Processing of aluminium AM parts is therefore often of lower
are plasma melting inert gas atomization (PIGA) as well as induc-
commercial advantage, if any. Another reason is that many Al alloys
tion plasma spheroidization which both are well known for Ti
are known to be hardly weldable. High performance alloys typically
powder production [43]. While in plasma atomization the raw
get their strength from precipitation hardening. Some heavily
material is a wire that is melted and atomized using plasma torches
applied hardenable alloys, e.g. EN AW-7075 of the Al-Zn 7xxx se-
and an inert gas, e.g. argon, the feedstock in the spheroidization
ries, contain highly volatile elements such as Zn, leading to tur-
process is an irregular, non-spherical metal powder that is melted
bulent melt pools, splatter and porosity and are therefore not suited
by inductively coupled plasma [52]. Compared to other atomization
or not easy to use in AM, although current research efforts may
processes the solidied powder particles are ner and feature an
promise AM of such alloys for the future [86]. Under vacuum con-
average particle size of 40 mm [53]. Spherical particles favour the
ditions, alloying elements with a vapour pressure highly different
desired owability and apparent density for AM.
to Al, e.g. Mg and Li, are known to vaporize preferentially. In
376 D. Herzog et al. / Acta Materialia 117 (2016) 371e392
addition, Al has a high reectivity for the laser wavelengths usually Besides, a few recent articles report the usage of invar for ap-
applied in LBM and LMD, which may be seen as another obstacle for plications requiring a low coefcient of thermal expansion in LBM
Al parts fabricated via AM [85]. The low viscosity of molten Al is [111], of Mg [112], refractory materials such as Ta [113], and
another problem and limits AM of aluminium to small melt pool precious metals such as Au [114] in LBM, as well as Cu [37] and g-
sizes, thus favouring LBM over e.g. LMD. On the more favourable TiAl (g/a2 lamellae) [30] in EBM to name only a few for the fabri-
side for AM fabrication of Al parts, the high thermal conductivity of cation of components. A detailed overview of the material science
Al reduces thermally induced stresses, thus also reducing the need of AM of each of these materials would exceed the scope of this
for support structures. In addition, the high thermal conductivity article.
allows for higher processing speeds.
Most common Al alloys for AM available today are the harden-
4. Microstructure and properties
able AlSi10 Mg (EN AC-43000) and the eutectic AlSi12 (EN AC-
44200). For high strength applications, a hardenable Al-Mg-Sc
This section at rst describes the different microstructural fea-
alloy is proposed by Schmidtke et al. (AlMg4.5Sc0.66 [87]). The
tures of AM parts, fabricated from steel, Al- and Ti-alloy powders,
addition of Sc enables precipitation hardening by formation of
and then correlates these to the static and fatigue properties in
Al3Sc precipitates and is also known for grain renement in AlMg
section 5.
alloys. Other commercial Al alloys investigated with regard to their
suitability for AM part fabrication in literature are hardenable Al-
Mg-Si (6061 [88,89]) and Al-Cu (2139 [85]) alloys. It must be 4.1. General remarks on microstructural evolution during AM
stated, however, that LBM and AlSi10 Mg is to date by far the fabrication
dominant combination in AM of Al parts.
During AM, a dened volume element of the material is usually
subjected to a complex thermal cycle [25,35]. This thermal cycle
3.4. Titanium and titanium alloys
involves a rapid heating above melting temperature due to the
absorption of the energy of the laser or electron beam and its
Ti and Ti alloys are of uttermost interest with regard to AM. Ti
transformation into heat, a rapid solidication of the molten ma-
combines broad industrial application in high performance parts
terial after the heat source has moved on, and numerous re-heating
with high machining costs and long lead times in conventional
and re-cooling processes when the following layers are welded and
processing. Thus, many business cases exist for AM of Ti that offer
the volume element is still exposed to heat [35]. Hence, many of the
substantial cost advantages. Besides commercially pure (cp) Ti
AM processes lead to meta-stable microstructures and non-
[90e93], AM parts fabricated from the a-b alloy Ti-6Al-4V have
equilibrium compositions of the resulting phases both of which
been investigated by many research groups and today are widely
even may vary for each layer of deposited material. This renders the
used for commercial fabrication [35,94,95].
modelling of microstructures and composition in AM fabricated
Hitherto, LBM [26,95e100], EBM [35,94,100] and LMD
parts rather difcult and challenging.
[35,101,102] have been successfully applied to fabricate parts from
AM microstructure is therefore a result of the above described
Ti-6Al-4V. The results obtained from the different AM processes
thermal cycle. Irrespective of the material, a ne-grained structure
make it also highly attractive for comparison of the AM processes
has usually been observed for AM in comparison to e.g. casting
and resulting properties. The great variety of alloy composition and
[32,115]. This can be explained by the rapid solidication, which
related microstructure, and the allotropy of Ti in combination with
itself is a result of the very local heat input and the small volumes of
the high temperature gradients and complex thermal cycle usually
molten material. Obviously, the temperature gradients are inu-
involved in AM also make Ti based alloys one of the most inter-
enced by a number of process parameters, e.g. the energy density,
esting materials for research regarding the relationship between
the thickness of the layer and the pre-heating temperature, if
AM process, microstructure and properties.
applied [96]. In addition, the temperature gradients are also
Other Ti alloys of research interest include Ti-24Nb-4Zr-8Sn
affected by the surrounding material, e.g. different heat conduction
[103] and Ti-6Al-7Nb [23] for biomedical applications, and Ti-
of powder and solidied material adjacent to the melt pool in
6.5Al-3.5Mo-1.5Zr-0.3Si for aerospace applications [104].
powder bed-based processes. Thus, microstructures of components
fabricated by AM are also inuenced by the geometry of the part,
3.5. Other metallic materials and may vary within a manufactured part, especially between bulk
material and surface areas [35]. As heat conduction in build di-
Further materials with relevant industrial applications in AM rection (z in Fig. 1) is typically higher than in the other spatial di-
include Ni-based superalloys for high-temperature applications, rections (x, y) as a result of the solidied material from lower,
such as Inconel 625 [105] and Inconel 718 used e.g. in LBM [106] previously built layers, anisotropy in both microstructure and
and EBM [107,108], and CoCr for biomedical applications [109,110]. properties has been observed in selected cases [2,35,107,113]. Under
Table 1
Typical conditions of selected AM methods and resulting grain sizes for Ti-6Al-4V.
AM method Typical process characteristics Typical cooling rate [K/s] a-lath width [mm]
Layer thickness [mm] Energy density [J/mm3] Pre-heating temperature [ C]
LBM 20 150 [18,116] <100 [25,95] 0 200 [25], 500 [26] 103 108 [90] 1 mm (a0 ) [26]
EBM <200 mm [32] 150 900 [34] >700 [35,36,94] 103 104 [36] 1.4 3.2 mm (a) [94]
LMD 40 1000 [18,35] 90 220 [35,102] 0 200 [18] <103 [35] 0.88 1.57 mm (a) [35,117]
It can be concluded, that LBM regularly leads to the highest cooling rates, while LMD features the lowest ones. Consequently, LBM yields the nest grain size, while LMD yields
slightly coarser grains by comparison. Grain size in EBM strongly depends on the pre-heating temperature, thus grain sizes may become considerably large if typical pre-
heating temperatures of 700 C and above are chosen.
D. Herzog et al. / Acta Materialia 117 (2016) 371e392 377
certain conditions and for several materials, an epitaxial grain chromium carbides at grain boundaries due to rapid cooling [69].
growth in build direction has been reported for e.g. LBM of Ti-6Al- 316L shows a very similar microstructure [63] in LBM. An increase
4V [25] and Ta [113], EBM [36] and LMD [2] (both Ti-6Al-4V), in distance from the substrate leads to a coarsening of the micro-
yielding grain sizes in build direction that exceed layer thickness. structure due to usually lower heat conduction through the build
Although the considerations above are valid for all AM pro- structure than close to the build plate, as specically reported for
cesses, the different AM methods still yield different microstruc- LMD in Ref. [82].
tures due to their specic mode of operation. Table 1 exemplies The microstructure of AM fabricated steel grades that are typi-
the basic relationship of process characteristics, cooling rates and cally martensitic in conventional processing, is found to form a
grain sizes (for Ti-6Al-4V, for which a-colony or a-lath width are certain amount of austenite phase in AM, as shown in Fig. 6. This
known to be the most inuential microstructural parameter for the behaviour has been reported for precipitation hardening steel (17-
mechanical properties of lamellar microstructures [115]). 4 PH [50,75,76]) and maraging steel (18-Ni300 [71,72]), but also for
the martensitic stainless steel grade AISI420 (X46Cr13) [78]. Fac-
chini et al. found for LBM of 17-4 PH a microstructure consisting of
4.2. Microstructure of AM fabricated steel parts
large and oriented grains and a ne dendritic substructure [75].
Phase composition was 72% austenite and 28% martensite, with
As a common feature, components fabricated from the steel
highly twinned martensite plates and untwinned regions near the
grades mentioned in Section 3.2, reveal a ne grained microstruc-
martensitic grains with a high density of stacking faults and dis-
ture typical for the high cooling rates of AM [71,72], as shown in
locations. The retained austenite was located in between
Fig. 4. Melt pool boundaries may be visible as a superstructure
martensite plates. LeBrun et al. [76] and Murr et al. [50] also
[63,79], lled with a cellular structure with an intercellular spacing
investigated this phenomenon in the same steel grade. Retained
down to 1 mm [71,72] (also cp. Fig. 4c). Elongated and oriented
austenite is supposed to be mainly a result from residual thermal
grains have also been widely reported, depending on processing
stresses in the material formed during the high cooling rate in LBM,
parameters [69,75,82]. Niendorf et al. [61] showed that larger melt
mechanically stabilizing the metastable austenitic phase [76]. The
pools lead to a coarsening of the microstructure because of slower
behaviour is sensitive to cooling conditions, thus even variation of
cooling rates and also promote texture due to enhanced recrystal-
cover gas in LBM may change phase composition signicantly due
lization while smaller melt pools lead to ne grained, weakly
to different thermal conductivity of the gas [49,50].
textured microstructures.
Krakhmalev et al. showed in Ref. [78] that in LBM of martensitic
LMD, typically having larger melt pools than LBM, consequently
steels, in this case AISI420, an austenitic phase may also be present
showed large grains of 100 mme140 mm and a near-monocrystalline
as a result of austenite reversion. The top layers revealed a mixed
texture [66]. The same report also pointed out that inter-layer time
microstructure of fresh martensite and 21% of retained austenite. In
intervals are crucial regarding cooling rates and thus inuence
contrast, the centre of the specimens appeared to consist of
grain size signicantly. Fig. 5 shows a typical LMD microstructure of
tempered martensite with ~57% austenite. LBM is therefore
a 316L austenitic stainless steel consisting of equiaxed grains within
believed to promote an in-situ partitioning process, where diffu-
the melt pool and columnar grains at the boundary.
sion during permanent re-heating leads to areas with high amounts
Austenitic stainless steels (such as 304L and 316L) typically
of austenite stabilizers such as carbon. As a consequence, austenite
exhibit a completely austenitic microstructure after AM fabrication,
reversion or growth of retained austenite grains appear. This
specically in LBM [58,69]. For LMD however, an amount of ~10.9%
austenite reversion was also reported to occur during aging pre-
retained d-ferrite has been observed in as-fabricated 316L samples,
cipitation hardening Cr-Ni-Cu steels (17-4 PH) manufactured by
transforming to austenite in a subsequent heat treatment at 1150 C
LBM [76], where the diffusion of Ni and Cu in conjunction with the
for 2 h and air cooling [66]. For 304L, Abd-Elghany et al. found a
formation of precipitates leads to a similar effect. However, with
typical LBM microstructure with elongated grains in building di-
heat treatment (>550 C for 4 h), the austenite generated in LBM
rection, with a 100% austenitic phase and no precipitation of
Fig. 8. Analysis of AlSi12 in LBM as-fabricated condition (from Prashanth et al. [119]), a) and b) microstructure showing laser tracks, c) elongated columnar morphology at boundary
between laser tracks, def) EDX composition of cellular structure with a-Al in the cells highlighted in e) and Si in the boundaries highlighted in f).
378 D. Herzog et al. / Acta Materialia 117 (2016) 371e392
Fig. 10. Microstructure of LBM-produced ScalmalloyRP (AlMg,Sc) alloy (from Palm et al. [124]), after ion-etching and examined by SEM in back scattering emission alloy contrast
mode. Overview of microstructure perpendicular to build direction, consisting of ne grained equi-axed regions with a grain size of 100 nm e 1 mm and coarser regions 2e5 mm in
grain size (left); and magnication of the highlighted square area (right). The white dots represent primary and secondary phases containing Fe and Mn; these phases seem to
concentrate in the ne grained regions.
D. Herzog et al. / Acta Materialia 117 (2016) 371e392 379
Fig. 11. Microstructure of AlSi12 LMD in as-fabricated condition (from Dinda et al. [126]). a) Overview revealing laser tracks, b) and c) alternating bands of microcellular structure (b)
and dendritic structure (c), with d) a-Al decorated with brous Si-particles at the boundary of cellular structure and e) eutectic with extremely ne spacing.
Fig. 12. Microstructures of LBM-produced cp-Ti in dependence of process parameters (from Gu et al. [90]). Coarse lath-shaped a phase observed at comparably high volume energy
(a), rened acicular a0 martensite at lower volume energy (b), and further renement of the a0 martensite with even lower volume energy (c, d).
380 D. Herzog et al. / Acta Materialia 117 (2016) 371e392
electron beam free-form fabrication (EBF), a process using an 4.4. AM microstructure of titanium and titanium alloys
electron beam as energy source and wire as the feedstock. A very
ne microstructure with elongated grains was reported. It was 4.4.1. LBM of pure Ti
observed that considerable amounts of magnesium were lost dur- The microstructure of LBM parts fabricated from commercially
ing the process, and this inhibited substantial formation of the U- pure (cp) Ti has been found to depend on the applied scan speed
phase. [90]. While the laser power was held constant at 90 W, the scan
In a study of Dinda et al. [126], the layer-by-layer structure was speed was varied between 100 mm/s and 400 mm/s. At a scan
clearly retrieved in the microstructure of LMD fabricated AlSi12. speed of 100 mm/s (and a resulting high volume energy), a regular
Furthermore, as shown in Fig. 11 the microstructure consisted of phase transition from b-phase to a-phase occurred during cooling
alternating bands of coarse dendritic areas and ne cellular struc- resulting in coarse lath-shaped grains, cf. Fig. 12a.
tures. A very ne eutectic phase was found between the dendrites At higher scan speeds (200 mm/s) and corresponding lower
with a eutectic spacing of 0.22 mm in average. The ne cellular volume energies, a higher degree of undercooling resulted in the
structure was identied as primary Al with brous Si particles at transformation from b into the martensitic a-phase (Fig. 12b). The
the boundaries and possessed a spacing of 0.78 mm. The structure of grain microstructure was found to be a rened acicular shape. With
alternating bands was however lost with increasing build height, a further increase in scan speed, further grain renement to below
which was attributed to slower cooling rates. A texture was also 10 mm and a zigzag-pattern was observed (Fig. 12c,d).
reported, with the dendrites regularly growing in build direction.
Fig. 13. Microstructure of Ti-6Al-4V in LBM as-fabricated condition (from Thijs et al. [25]). a) Fine grained herringbone structure corresponding to scan direction, b) front view, c)
side view showing elongated grains d) schematic of experiment.
D. Herzog et al. / Acta Materialia 117 (2016) 371e392 381
Fig. 14. Ti-6Al-4V LBM microstructure in build direction (a, c) and in plane with layers (b, d), (from Wycisk et al. [95]). a) and b) in stress-relieved condition after heat treatment at
650 C for 3 h in vacuum, c) and d) in HIPed condition.
4.4.2. LBM of Ti-6Al-4V phase. In Refs. [25], the authors postulated that comparative to a
Similar microstructural effects have been observed for LBM of heat treatment the Ti3Al phase precipitates during consecutive re-
the widely used alloy Ti-6Al-4V. Thijs et al. [25] noticed a ne- heating to 500 Ce600 C when further layers are built on top of the
grained acicular martensitic structure in their investigations, and material. Consequently, the precipitates occur with a periodicity of
also identied from XRD the present phase as a. In building di- the layer thickness and are visible in the cross-sections as dark
rection, elongated grains with a size [ 100 mm have been found areas. High temperature gradients and short interaction times lead
that signicantly exceed the layer thickness of 30 mm which was to only a small amount of such precipitates. It has been found,
used in the experiments, Fig. 13. Obviously, an epitaxial growth however, that more precipitates are formed with higher energy
occurred. The width of grains was approximately the same as the density.
width of the scan track. With an increased heat input, a larger To improve the tensile elongation to failure (cf. Section 5) of
width of the scan track resulted, leading to coarser grains. In LBM-manufactured Ti and Ti alloy parts in the as-fabricated con-
addition, the local heat conduction was found to determine the dition, a heat treatment is usually applied. Different heat treat-
orientation of the martensite structure. As the local heat conduc- ments have been investigated by Seyda et al. [127], varying the
tion is inuenced by the scan strategy, the orientation of the temperature range from 700 C (stress-relieved condition) up to
martensite has been found to be inuenced by the scan strategy, 1010 C (solution treated). While the stress-relieved microstructure
too. For a zig-zag scan pattern, a herringbone structure was found showed comparatively little change in grain size, the martensitic
for the x-y-plane (orthogonal to the build direction), while in the x- phases completely dissolved during solution treatment into equi-
z-plane the grains were tilted by around 20 . The grains grow to- librium (a b) structure in combination with a coarsening of the
wards the melt pool, when the scan orientation is unidirectional. grain, as expected. Wycisk et al. [95] proposed a stress-relieve
Thijs et al. also reported the presence of the intermediate Ti3Al treatment at a slightly lower temperature of 650 C, yielding a
Fig. 15. Ti-6Al-4V LBM microstructure (SEM back-scattered), (from Qiu et al. [97]). a) Needle-like martensitic structure in as-fabricated condition, b) and c) after HIP at 920 C/
103 MPa.
382 D. Herzog et al. / Acta Materialia 117 (2016) 371e392
Fig. 16. Ti-6Al-4V LBM microstructure depending on layer thickness (from Xu et al. [96]). a) Fine 15 mm-wide columnar prior-b grains lled with a0 martensite using a layer
thickness of 30 mm, b) ultrane lamellar a b structure using a layer thickness of 60 mm, c) acicular a0 with minor a b lamellae using a layer thickness of 90 mm, d) detail of a0
martensite formed inside the prior-b grains shown in a).
very ne microstructure consisting of a and a0 phases. The thick- top eight layers were found to consist of the a-phase independent
ness of individual a-lamellae was measured to be below 1 mm, as of process parameters, as there are not enough consecutive layers
shown in Fig. 14. for in-situ decomposition. Also, due to different heat conduction
AM manufactured parts may also be treated by hot isostatic conditions in the layers closest to the bottom, coarser grains were
pressing (HIP) in order to relieve stresses and to reduce any observed.
remaining porosity. Qiu et al. [97] found that HIP at 920 C for 4 h
and a pressure of 103 MPa results in a transformation of the as-
fabricated martensitic microstructure into a and b phases while
reducing porosity at the same time, cp. Fig. 15. Wycisk et al. [95]
showed that under similar HIP conditions the a lamellae slightly
coarsen to a thickness of about 4 mm (also cp. Fig. 14).
Recently, Xu et al. studied in much detail the inuence of the
chosen LBM parameters such as the single track and multilayer
deposition, layer thickness, focal offset distance and energy density,
on the resulting microstructure of Ti-6Al-4V parts [96]. They found
that with optimized LBM process parameters, it is possible to
decompose already during LBM fabrication (in-situ) the rather
brittle martensitic a0 phase into a much more ductile (a b)
microstructure, thus potentially avoiding the need of a subsequent
heat treatment. While the powder bed was pre-heated to 200 C,
the layer thickness was varied between 30 mm and 90 mm and the
focal distance was also varied, thus varying the spot size. Columnar
prior-b grains were found for all samples, Fig. 16, and the a0
martensitic phase was present at a layer thickness of 30 mm (cor-
responding to the highest heat gradient and related fastest cooling
rate, Fig. 16a,d). With layer thicknesses of 60 mm and 90 mm, the a0 -
phase was found to decompose, when the focal distance was
selected properly. An ultrane lamellar (a b) structure was the
result. It was proposed that the specic microstructure is a result of
an in-situ heat treatment comparable to solution treatment and
subsequent aging, when the material reaches a temperature range Fig. 17. Schematic Ti-6Al-4V EBM microstructure (from Antonysamy et al. [36]). Large
of around 400 C during build-up of consecutive layers. Hence, the columnar prior-b grains are found in the centre, while towards the outer contour ner
curved grains are present.
D. Herzog et al. / Acta Materialia 117 (2016) 371e392 383
4.4.3. EBM of Ti-6Al-4V Tan et al. [35] determined a volume fraction of 3.6% of the
In EBM of Ti-6Al-4V, the microstructure typically consists of retained bcc b-phase in EBM built Ti-6Al-4V (at a pre-heating
coarse prior b-grains transformed into a ne lamellar a morphology temperature of 730 C and 600e650 C temperature range during
with a small volume fraction of retained b [33]. EBM allows for pre- the process), formed as discrete at rods embedded in the
heating of the powder layer to high temperatures, which will affect continuous hcp a-phase. It has also been reported that a graded
both the cooling rates as well as the resulting microstructure. If the microstructure formed in build direction, as the width and inter-
part is maintained above a temperature of 700 C in the EBM spacing of prior-b-grains increased with build height, which was
manufacturing process, a rather ne annealed ab-structure has attributed to the decreasing cooling rate. The a-b-interface has
been observed. At rst, columnar b-grains nucleate either at the been studied in detail and has been found to consist of the fcc L
base plate or at the surface of the parts during solidication with phase, supposedly a result of the lattice mismatch between the a
grain sizes far larger than the layer thickness and a pronounced and b phases. The fcc L phase had the same composition as the hcp
texture [36]. Afterwards, as the build temperature is in the same a phase. The authors also showed that Ti, Al and O had partitioned
range as the martensite start temperature Ms, the b-phase may to the a phase, while the other trace elements already present in
transform diffusionless to a0 if below Ms and then decompose to a, the Ti-6Al-4V powder, V, Fe and H concentrated in the b phase.
or transform diffusional into a if above Ms [36].
Antonysamy et al. explained schematically in Ref. [36] how 4.4.4. LMD of Ti-6Al-4V
different microstructures evolve for the contour pass compared to Same as for the other two discussed AM technologies (LBM,
the in-ll hatching, as presented in Fig. 17. The bulk material EBM), columnar prior-b-grains have also been observed in LMD of
generated by in-ll hatching showed the highly textured, coarse Ti-6Al-4V [35,128]. Even with the high layer thickness of LMD (cf.
prior-b-grains directed parallel to the build direction, as described Section 2.3), the prior-b-grains grow epitaxial, extend across
above [36]. Wavy grain boundaries have been observed for the in- several layers and reach a length of 1.5 mm to >10 mm. Perpen-
ll hatching, if the melting direction was rotated 90 after each dicular to the build direction, the width of the grains was found to
layer [35]. The skin contour however showed a complex structure be on average 375 mm. The grain boundary a phase was detected on
consisting of an outer layer of ne-curved b-grains which nucleated the boundaries of the prior-b-grains, cp. Fig. 18 [2].
from the surrounding powder bed and then growing inwards Baufeld et al. [128] also reported a graded microstructure but
following the curvature of the melt pool, and an inner layer of lath distinguished three areas. Close to the base plate, where the cooling
shaped grains growing upwards from previously deposited mate- rate is the highest, small a-lamellae were found and the grid-like
rial [36]. structure indicated the presence of a0 martensite. The top-most
layers were dominated by (a b) colonies starting at grain
boundaries. Although the cooling rates are lower, this area features
rather small a-lamellae in the b-matrix as the area is not re-heated,
which in turn is a consequence of no further layers built on top of
these outermost layers. Below these top-most layers, however,
coarser lamellae were observed with a segregation of Al into the a
phase and V into the b phase, as a consequence of periodic heat
treatment during building up the following layers, cp. Fig. 19. Single
lamellae are found to grow at the expense of other lamellae forming
a rectangular grid.
5. Mechanical properties
Fig. 18. Microstructure of Ti-6Al-4V LMD depending on location (from Carroll et al.
[2]). Fine lamellar Widmanstatten structure at the bottom with small amounts of Fig. 19. Microstructure of Ti-6Al-4V LMD (from Baufeld et al. [128]). The arrow shows a
grain-boundary a-phase (a), and slightly coarser structure at the top (b). lamella with increased size, forming a rectangular grid with similar lamellae.
384 D. Herzog et al. / Acta Materialia 117 (2016) 371e392
Table 2
Tensile properties of several stainless steel grades, depending on the microstructure generated by different AM processes and in different material conditions.
AF: as fabricated, AN: annealed, HT: heat treated, AC: air cooled, ArC: cooled in argon atmosphere, SR: stress relieved, ST: solution treated, AG: age hardened, PA: peak aged,
OA: over aged, M: Martensite, A: Austenite, F: Ferrite.
a
In build direction.
b
Orthogonal to build direction.
5.2.2. Tensile properties of AM fabricated aluminium alloys During age hardening of an additive manufactured AlSi10 Mg alloy,
Tensile properties of Al alloys show a similar behaviour as AM the original ne grain structure coarsens and at the same time
fabricated steels with regard to the AM-microstructure/yield precipitates are formed, the rst effect counteracting the intended
property relationship. The ne grain structure resulting from AM strengthening by the latter effect [121] and, thus, maintaining
methods primarily leads to an increase in strength in the as- about the same yield strength as the as-fabricated part (Table 3).
fabricated condition. As no precipitates have been observed e.g. Also, a loss in Mg has been reported for AA 2139 (Al-Cu,Mg) alloy
in as fabricated LBM samples of Al alloys [121,132], tensile strength during AM fabrication, reducing the amount of precipitates and
values for precipitation-hardening alloys such as AlSi10 Mg are thus leading to a reduced yield strength (Table 3) [85]. An LBM-
comparable to solid-solution strengthened alloys such as AlSi12. fabricated scandium based alloy shows the highest performance
Table 3
Tensile properties of several aluminium alloys, depending on the microstructure generated by different AM processes and in different material conditions.
AF: as fabricated, HT: heat treated, FC: furnace cooled, AA: articial aged.
a
In build direction.
b
Orthogonal to build direction.
c
EBF Electron Beam Free-Form Fabrication.
386 D. Herzog et al. / Acta Materialia 117 (2016) 371e392
Table 4
Tensile properties of titanium and Ti-6Al-4V, depending on the microstructure generated by different AM processes and in different material conditions.
AF: as fabricated, HT: Heat treated, SR: Stress relieved, WQ: Water quenched, TE: Tempered, AC: Air cooled, ST: Solution Treated, STA: Solution treated and aged.
a
In build direction.
b
Orthogonal to build direction.
c
Upper part of graded structure.
d
Lower part.
keeping a ne-grained structure while forming fully coherent rates of LBM. Grain renement is increasing the yield strength as
precipitates in articially aged condition [87]. well as ductility [142]. It is also known that the distorted hexagonal
lattice structure of the a0 martensite is stronger than lamellar a,
5.2.3. Tensile properties of AM fabricated titanium and titanium mainly due to its ne lath width, though it does not necessarily
alloys reduce the ductility [143].
Ti and the Ti alloy Ti-6Al-4V are probably the most thoroughly In general, AM processed Ti-6Al-4V also shows increased tensile
investigated group of materials when it comes to AM of metals and strength compared to cast or wrought material. Conventionally
alloys. As Ti is a suitable material for LBM, EBM and LMD, the processed (cast, wrought) a b alloys, such as Ti-6Al-4V, already
complex interrelationship between the different AM processes, exhibit considerably lower elongation values in comparison to cp
their parameters used, resulting microstructures, and tensile titanium due to the blocking of the twinning deformation modes
properties have been studied comprehensively, in particular for Ti- [115]. Formation of microstructural features that further reduce
6Al-4V. Table 4 gives an overview of the available data. elongation at failure are thus a major concern in AM processing of
Referring to Table 4, for cp-Ti, AM processes tend to lead to Ti-6Al-4V. Table 5 gives an overview of some microstructural fea-
signicantly higher yield strengths than sheet metal Ti, whereas tures commonly observed in AM processing of Ti alloys and its
the rather high ductility (~20%) is maintained. The highest strength inuence on properties.
will be achieved, if the process conditions result in a very ne While all AM techniques discussed here are able to meet or even
martensitic (a0 ) microstructure, e.g. by the extremely high cooling exceed yield and ultimate tensile strengths of ASTM specications
D. Herzog et al. / Acta Materialia 117 (2016) 371e392 387
Table 5
Selected microstructural features and effect on properties of titanium alloys [143].
Equiaxed a Strength, ductility, fatigue initiation resistance, LCF resistance Fracture toughness, fatigue crack growth resistance, notched fatigue
resistance
Elongated a Fracture toughness, fatigue crack growth resistance, notched fatigue Ductility, fatigue initiation resistance, LCF resistance
resistance
Widmanst atten a/a- Fracture toughness, fatigue crack growth resistance, notched fatigue Ductility, fatigue initiation resistance, LCF resistance, strength
plates resistance, creep
Colony a Fracture toughness, fatigue crack growth resistance, notched fatigue Strength, ductility, fatigue initiation resistance, LCF resistance
resistance
Grain boundary a Fracture toughness, fatigue crack growth resistance, notched fatigue Ductility, fatigue initiation resistance, LCF resistance
resistance
Elongated grain shape Fracture properties, fatigue crack growth resistance, notched fatigue Fatigue initiation resistance
resistance
Coarse prior b grains Fracture toughness, creep Strength, ductility, fatigue initiation resistance, LCF resistance
Table 6
Fatigue Properties of Ti-6Al-4V, Al alloys and steels depending on material conditions and microstructure generated by different AM processes as compared to conventionally
processed materials (wrought, cast).
Titanium alloy
Ti-6Al-4V Wrought Peters et al. [148]. Polished / Ultrane lamellar, a 1 675
lamellae 0.5 mm
/ Fine lamellar, a lamellae 1 mm 1 600
/ Lamellar, a lamellae 12 mm 1 480
Gerdes [149] Notched / Fine a b lamellae 1 bending 260
Kt 2.4
LBM Leuders et al. [147] / HIP (920 C/100 MPa/2 h) Fine a b lamellae, a 1, tension- 620
needles 4 mm compression
Wirtz [150] Machined ST 930 C ab lamellae 1, bending 375
Ground 400
Brandl [144] AF SR 843 C/2 h Lamellar 0.1 200
Polished 300
Kausch [151] AF STA ab lamellae 0.1 330
Machined 400
Wycisk et al. [145] AF SR (650 C/3 h) Ultrane lamellar a a0 in prior- 0.1 210
Polished b 500
Wycisk et al. [95] Polished SR (650 C/3 h) Ultrane lamellar a a0 in prior- 1, tension- 360
b compression
HIP (920 C/100 MPa/2 h) Fine a b lamellae, a 0.1 680
needles 4 mm 1, tension- 575
compression
EBM Brandl [144] Polished HIP (843 C/100 MPa/4 h) / 0.1 600
LMD Brandl [144] Polished ST (843 C/2 h) / 0.1 ~700
Aluminium alloys
AlSi12 cast Kammer [152] Polished / / 1 bending 55-80a
LBM Siddique et al. Polished 200 C in process SR / 1 tension- 80
[153] (240 C/6 h) compression
AlSi10Mg cast Kammer [152] Polished / / 1 bending 65e100a
LBM Buchbinder [146] AF AF / 0.1 45
Polished AF / 70
T6 / 115
300 C in process T6 / 140
AlMg4.4Sc0.66MnZr LBM Greitemeier et al. Polished AA (325 C/4 h) / 0.1 300
[154]
Steel grades
17-4PH LBM Sehrt [155] Polished / / 1 bending 407
316L Riemer et al. [62] AF None / 1 108
Machined 650 C/2 h / 294
Machined HIP (1150 C/100 MPa/4 h) / 317
a
At 5 107 cycles, AF: as fabricated, SR: Stress relieved, ST: Solution Treated, STA: Solution treated and aged, AA: articial aged.
for cast [139] and wrought [141] materials usually applied in in- in-situ.
dustry, this is not the case regarding elongation at failure. EBM LBM yields very high strength though in combination with little
shows high elongation values in the as fabricated state, as the elongation as compared to standards (ASTM specications) in the
typical pre-heating temperatures are tempering the material as fabricated state. Adequate heat treatments may however
388 D. Herzog et al. / Acta Materialia 117 (2016) 371e392
transform the microstructure and lead to enhanced ductility, if Additionally to the determination of fatigue strength by con-
needed. With careful adjustment of LBM parameters such as layer stant amplitude testing, investigations on fracture mechanical
thickness and volume energy, the temperature cycle during build- behaviour of AM material have been carried out. Due to the high
up may be controlled in a way that the a0 martensite phase de- importance in aircraft applications, Ti-6Al-4V has been in the
composes in-situ, leading to a favourable high strength and high focal point of crack growth and fatigue resistance analysis.
ductility combination, as suggested by Xu et al. [96]. LMD shows Leuders et al. [147] showed that the crack growth behaviour and
lower yield strengths compared to LBM and EBM (Table 4) probably threshold value of Ti-6Al-4V compare to conventional plate ma-
due to the lower cooling rates of LMD, and the elongation at failure terial. In additional investigations, Wycisk et al. [145] used the
shows a high variance depending on the chosen process parame- approach of Kitagawa and Takahashi [156] to predict the fatigue
ters. Oxygen is known to be a major factor in increasing strength life of Ti-6Al-4V depending on process inherent porosity and
and reducing ductility [115]. In addition to the microstructure, even material defects with good agreement to the experimental re-
a small variation in chemical composition may therefore explain sults. Brandl et al. [157] successfully used computer tomography
the observed variance in static properties found in literature. Be- to identify material defects and linear elastic fracture mechanic
sides, the brittle failure mode of as fabricated AM Ti-6Al-4V is software to simulate the inuence of these defects on the fatigue
attributed to the combination of a0 martensite, remnant porosity life of EBM Ti-6Al-4V. In similar investigations, Siddique et al.
and residual stresses [2,35,98]. Intergranular failure along elon- [158] used computer tomography to identify defects and FEM
gated prior-b-grain boundaries has also been observed [96]. simulation to predict stress concentration in LBM of the eutectic
Anisotropic properties of AM Ti-6Al-4V have been reported for AlSi12 alloy. The results show that - similar to static and fatigue
the as fabricated state. A literature survey does not reveal, however, strength - the fracture mechanical properties of AM materials
a unique trend for the tensile strength being always higher in build- compare to their conventional counterparts and that known
direction than orthogonal to the build direction. As shown in concepts from fracture mechanics can be used to evaluate AM
Table 4, sometimes just the opposite is being found. metals and alloys.
6. Applications
5.3. Fatigue strength
The recent extensive gains in knowledge on the inuence of AM
Identical to static mechanical properties the fatigue strength of processing parameters on the microstructure and the related
metallic materials primarily depends on their microstructure. properties of AM metals, as discussed in the previous sections,
However, process-inherent properties such as surface roughness enables AM to become not only a valuable method for rapid pro-
and material defects strongly inuence the fatigue performance of totyping but more and more also for rapid manufacturing. Serial
AM fabricated parts. The layer wise manufacturing process typi- applications reach back some 10 years e.g. in the dental industry,
cally leads to an increased surface roughness, e.g. of Rz z 100 mm where CoCr is used for dental prostheses [7]. Applications of tool
in LBM, causing increased stress concentration and early failure of steel, e.g. H13, in mould inserts and tools have also been reported
AM parts under fatigue loading in as fabricated condition for some time [6]. Shortened lead times and new possibilities in the
[144e146]. Mechanical surface treatments (e.g. polishing) improve position of cooling channels make the technology quite attractive
the fatigue behaviour. However, material defects such as porosity for this market, e.g. as cooling channels close to the surface that are
and insufcient layer bonding result in increased scatter of the not producible by conventional technologies can shorten heat and
experimental data [145], rendering an assessment of the fatigue cooling cycles.
properties rather difcult. Curing these defects and densifying the Ti-6Al-4V has been the material of choice for a variety of
material by hot-isostatic pressing results in improved fatigue biomedical applications, e.g. hip endoprosthesis [159]. The process
properties and values comparable to cast and wrought materials offers the possibility to manufacture osseointegrative structures
[95,144,147]. Table 6 gives an overview on the fatigue strength of such as lattices and thus improves functionality of implants. Ti-6Al-
additive manufactured Ti-6Al-4V as well as several Al alloys and 4V is also in the focus of the aerospace industry, under discussion
steels at 107 cycles achieved for different surface and heat treat- for serial production of brackets (cf. Fig. 20), parts of the fuel system
ment conditions. and many other parts [1].
The aerospace sector is probably the one most radically affected
by AM in the near future due to the enormous lightweight poten-
tial; besides structural elements, this also includes engine parts.
Fuel nozzles for the GE LEAP aero engine (cf. Fig. 21) is a prominent
example with a planned production volume of 25,000 parts [9]. The
manufactured part is said to be 25% lighter and stronger than the
previous conventional design.
through previously built layers, anisotropic microstructures with property of additively manufactured Ti-6Al-4V d Comparison among se-
lective laser melting, electron beam melting, laser metal deposition and
elongated grains are found that consequently lead to anisotropic
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