Accepted Manuscript

Title: Fabrication of iron-rich Fe-Al intermetallics using the

wire-arc additive manufacturing process
Author: Chen Shen Zengxi Pan Yan Ma Dominic Cuiuri
Huijun Li
PII:
DOI:
Reference:

S2214-8604(15)00028-7
http://dx.doi.org/doi:10.1016/j.addma.2015.06.001
ADDMA 39

To appear in:
Received date:
Revised date:
Accepted date:

19-12-2014
25-5-2015
9-6-2015

Please cite this article as: Shen C, Pan Z, Ma Y, Cuiuri D, Li H, Fabrication of iron-rich
Fe-Al intermetallics using the wire-arc additive manufacturing process, Addit Manuf
(2015), http://dx.doi.org/10.1016/j.addma.2015.06.001
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Revised Manuscript v2

Fabrication of iron-rich Fe-Al intermetallics using the wire-arc additive

manufacturing process
Chen Shen, Zengxi Pan, Yan Ma, Dominic Cuiuri, Huijun Li
Corresponding author: Zengxi Pan: E-mail: zengxi@uow.edu.au; Faculty of Engineering &
Information Sciences, University of Wollongong, Northfields Avenue, Wollongong, NSW 2522,
Australia; Tel: +61 2 4221 5498

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Abstract
A wire-arc additive manufacturing (WAAM) system is used to fabricate iron rich Fe-Al
intermetallics with 25at% aluminum content. The alloy is produced in-situ through controlled
addition of the elemental iron and aluminum components into the welding process. The properties
of the fabricated material are assessed using optical microstructure analysis, hardness testing,
tensile testing, X-ray diffraction phase characterization and electron dispersive spectrometry. It is
shown that the WAAM system is capable of producing iron rich Fe-Al intermetallics with higher
yield strength and similar room temperature ductility when compared to equivalent materials
produced using powder metallurgy.
Keywords: iron aluminide; in-situ alloying; additive manufacturing; GTAW

1. Introduction

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Iron rich Fe-Al intermetallic is of interest for its excellent oxidation [1, 2] and corrosion resistance
[3], low density and low material cost. Systematic research on this material has been conducted
since the 1980s when Oak Ridge National Laboratory (ORNL) produced iron rich Fe-Al
compounds by melting and drop casting, and also used micro alloying and heat treatment methods
to assess the effects on the mechanical properties of the material [4, 5]. According to the Fe-Al
binary diagram, iron rich Fe-Al intermetallics mainly contain Fe3Al phase with DO3 structure [6]
and FeAl phase with B2 structure [7]. To date, research has mainly focused on improving the
mechanical properties, especially ambient temperature ductility and yield strength above 600C,
by adding alloying elements to Fe3Al or FeAl based iron aluminides [8, 9, 10]. Improvements in
conventional casting of iron aluminides have stalled. Instead, powder based melting [11] and
mechanical hot pressing [12] have become the preferred methods of producing these alloys.
However, the manufacturing cost of these methods is relatively high therefore the innovative
method of fabricating iron aluminides with lower manufacturing cost has been announced to be
one of the main future research areas [13].

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Considering the low ductility and machinability of Fe-Al intermetallics at room temperature, and
also the current manufacturing trend of free-forming processes, the additive manufacturing (AM)
processes may offer an effective alternative for fabricating full density structural iron aluminides.
AM processes have been increasingly successful since their first introduction into the
manufacturing industry in 1986 [14]. While initially applied to non-metallic materials, AM has
subsequently been adapted to fabricate complex, net-shaped metal components in successive
layers [15]. As a rapid prototyping technique, short lead-times are obtained and design changes
can easily be incorporated [16]. It has proven to be very effective in accelerating product
development by omitting extensive machining and thus reducing time-to-market with respect to

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traditional machining approaches [17]. Currently deposition methods for metal AM processes can
be divided into two categories: powder-based (laid down as a bead or continuously blown into the
melt area by a gas stream) and wire-fed [18]. The present research has chosen the wire-fed
approach as the preferred deposition method. Although powder-based AM process has more
shaping accuracy and higher resolution, for certain materials it does not have the capability to
directly produce functional parts of high structural integrity that can be used in operational
systems [19]. Powder-based AM processes produce parts that are close to full density [20], but
often require expensive processing such as hot isostatic pressing (HIP) to achieve the full-density
that is essential for highly-loaded structural materials. Also, the wire-fed deposition method has
significantly lower material supply cost and there is less potential for oxide contamination when
compared to powder-based methods [21]. The power source chosen for the present AM process is
gas tungsten arc welding (GTAW) arc rather than laser or electron beam, due to a combination of
advantages including low cost, no need for a vacuum chamber (when compare to electron beam),
the ability to economically apply the process to a very large operating volume, and a much higher
deposition rate [22]. Furthermore, compared to GMAW process, the GTAW arc is more stable and
less inclined to generate spatter when applied to a wide range of ferrous, non-ferrous alloys and
their combinations [23], which is more desirable to achieve consistant chemical composition of
the despotion. The GTAW process can be combined with industrial welding robots and
multi-sensor control systems to achieve high arc placement accuracy in industrial applications
where distortion or other small-but-unpredictable component placement errors are likely [24].

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The purpose of this feasibility study is twofold. The first objective is to explore a cost-effective
method for fabricating fully dense iron-rich Fe-Al intermetallics; the second is to prove that AM
processes can be applied to directly fabricate iron rich Fe-Al intermetallics with acceptable
material properties if components made by the AM process had acceptable mechanical properties
for aerospace structural components [25, 26], the method demonstrated in this study should have
the potential to replace conventional powder-based casting or melting manufacturing methods.

2. Experimental setup

2.1 Wire-Arc Additive Manufacturing system

The WAAM system consists of a GTAW system, an auxiliary shielding gas system and a
preheating system and two wire feeders. These elements are coordinated through a program
console. The setup of the two wire feeding nozzles and gas shielding is shown in Figure 1. One is
for aluminum wire and the other is for iron wire. The angle between two wire feeding nozzles is

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approximately 60 and the angle between each nozzle and substrate surface is 30 to ensure the
stability of melting pool during double wire feeding. The arc length is set to 3.5mm to produce a
stable and concentrated arc with sufficient welding voltage and heat input. Besides the shielding
gas from GTAW system itself, additional argon shielding gas system shown in Figure 1a is applied
following after the GTAW torch with a flow rate of 9L/min. The additional shielding gas continues
to flow during the manufacturing process and after the arc is extinguished for approximately 1
minute to avoid oxidation as the recently-deposited layer is cooling. All layers are deposited with
an interpass temperature of 400C to avoid cracking defects that would otherwise result from the
low-temperature brittleness of iron aluminum intermetallics [27].

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Figure 1: Photograph of the wire-arc AM process

2.2 Sample manufacturing

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The feed wires used in the experiment are 0.9mm 1080 aluminum wire and 0.9mm LS422750/4
99.5% black annealed iron wire. The feeding speeds are set so that the resulting aluminum content
is controlled at 25at% to produce a Fe3Al based intermetallic according to the Fe-Al binary phase
diagram (Figure 2). A total of 25 layers are built up in a wall-shaped sample using 140A welding
current and the specific deposition energy is maintained at approximately 20kJ/g in order to
provide sufficient energy to achieve homogeneous alloying, avoid shielding gas entrapment, and
therefore obtain full-density deposited material. The substrate material used in the experiment is
DH36 low carbon steel. Therefore the dilution influence from the substrate can be identified and
measured by noting the acicular carbon precipitation phase. The interpass temperature is
controlled at 400C using 2 pairs of thermal couples, one for the heating equipment and one for
the computer, attached 20mm from the additive manufacturing position. The process is paused
between each layer until the temperature of the previous layer fall to 400C. Specific welding
parameters for the produced sample are shown in Table 1. The resultant deposition parameters are
listed in Table 2.

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Figure 2: Fe-Al binary diagram [28]

Parameter

Unit

Current
Voltage
Travel speed

A
V
mm/min

140
12.7
100

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Aluminum wire feed rate

Iron wire feed rate

mm/min
mm/min

695
1000

Table 1: Details of welding parameters

Aluminum content
Specific deposition energy
Deposition rate
Wall build height
Wall width
Number of layers

at%
kJ/mm
g/min
mm
mm
--

25
20.6
6
24
12
25

Table 2: Resultant deposition parameters

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2.3 Microscope sample preparation

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The sample cross sections are cut from the additively manufactured wall by wire electrical
discharge machining (EDM) since the low temperature brittleness of the Fe-Al intermetallic
precludes cutting by conventional machining processes. Sample polishing is performed using a
Struers TegraPol-21 automatic polishing machine. The polishing procedure after grinding the
sample surfaces to P1200 is 9m Largo, 3m Dac and finally OPS. The etchant is 50% aqua regia
with a 5 seconds etching time. Optical microstructures are inspected with a Leica MMRM
research microscope.

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2.4 Mechanical property tests (Hardness, tensile test)

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Vickers microhardness is measured with a Leco M-400-H1 hardness testing machine along the
vertical centerline of the wall-shaped sample using a 1kg load and 0.5mm step size, indentation
time for each testing point is 7s. Three tensile specimens with a gage section of
10mm2mm1.5mm are cut from the middle section of the deposited wall along the longitudinal
direction using wire EDM. The extract location and the sequence for producing the specimens
making procedure is shown in Figure 3. The specimens are tested at room temperature with a
MTS370 load unit at strain rate of 510-2s-1.

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Figure 3: Tensile specimen manufacturing procedure

2.5 Phase characterization and chemical composition measurement

In order to further investigate the hardness variations, chemical composition measurement is

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performed with a JEOL JSM-6490LA scanning electron microscopy (SEM) equipped with an
energy dispersive X-ray spectrometer (EDS) at 20kV. The composition testing points are located
approximately 50m laterally from the hardness testing points. The accuracy of chemical
composition measurement is 0.5at%. Phase characterization is identified using a GBC MMA

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X-ray diffractometer (XRD) with CuKa radiation (= 1.5418); scanning angle (2) is set from
20 to 100. XRD sample is taken from top layers of the sample so the influence from dilution
occurring in the near-substrate zone can be excluded.

3. Results and discussion

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3.1 Morphology

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An integral cross-section of the built up wall (composed of a collage of smaller detailed

metallographic images) is shown in Figure 4. Large columnar grains exhibit growth in the vertical
build up direction with width from 300m to 500m measured according to ASTM E112-10
standard. Some comparatively smaller equiaxed grains can be observed in the upper layers, but
also in the near-substrate zone. Generally the buildup wall shows a typical macrostructure for
welded Fe3Al based intermetallics [29].

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Figure 4: Integral cross-section of the additive manufactured wall

Higher magnification metallographic images (Figure 5) are taken from the top, middle and bottom
regions. In the bottom dilution region the acicular carbide precipitates (Figure 5a) induced by
carbon from the substrate steel plate, distribute in grains and along grain boundaries [30]. Also
some bainite (Figure 5b) separates out in the columnar grains near the substrate, since the time
length during which the material is molten experienced by the first few layers is relatively short so

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that the deposited material and melted base metal cannot homogeneously fuse with each other.

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The middle section of the wall (Figure 5c) contains mainly large columnar Fe3Al grains with some
small grains among them. There are finer white lines with precipitates (Figure 5d) like grain
boundaries in the large columnar grains which are not evident in bottom layers and top region of
the wall. These are probably the vestiges of the grain boundaries left after the grain growth of the
large columnar grains. Although the small grains are engulfed during grain growth, the
precipitates in the grain boundaries are left. Therefore after the etching the precipitate regions
form the lines.

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Grains in top region of the wall are relatively smaller than the columnar grains in middle region,
especially the equiaxed grains near the top surface (Figure 5e) since the last layer of the wall is
deposited without further thermal cycling. Therefore the columnar grain growth of the middle
region is arrested, leaving the as-deposited grain structure intact in top region, and particularly
in the top layer.

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Figure 5: Microstructures in different regions (small dots are etching pits): (a) acicular carbide
precipitates in bottom region (500); (b) bainite in bottom region near substrate (500); (c) white
lines in middle region (500); (d)precipitates distribution along the white lines (1000); (e) small
grain in top region (500)

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3.2 Phase characterization

The XRD patterns of produced from the deposited material (Figure 6) are uncluttered and all three
peaks are characterized as Fe3Al phase. Therefore all grains in the built up wall are Fe3Al grains.
The reference code of this Fe3Al phase is 03-065-4419.

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3.3 Hardness and chemical composition measurement

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Figure 6: XRD pattern of the manufactured wall

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The variation of hardness and aluminum content as a function of the vertical distance from the top
of the deposited wall are shown in Figure 7. The dilution affected height from the substrate, as
determined by the effect on aluminum content, is 7mm. This corresponds with the presence of
acicular carbide precipitates in the microstructure [10], as exemplified in Figure 5a. The mean
hardness of designed composition (25at% Al) layers is approximately 290Hv. In the dilution
affected zone, there is a strengthening (high hardness) area which is approximately 21mm from
top surface of the wall with about 15at% Al content. As observed from the microstructure, the
carbide precipitates are relatively small and short in the upper section of the dilution part while the
carbide precipitates appear to be large and long in the strengthening area. Since the acicular
carbide precipitates are not present in the bottom region that is immediately adjacent to the
substrate material, the sudden hardness increase can be attributed to the precipitation
strengthening of carbide precipitates.

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Figure 7: (a) Centerline hardness vs vertical location; (b) Al content vs vertical location (adjacent
to hardness testing points)
The consistent aluminum content measurements in the top and middle regions acquired by EDS,
together with and the clear XRD peaks indicate a single phase Fe3Al deposit with uniform
chemical composition has been fabricated. During the in-situ alloying WAAM process, alloy that
has been produced in previously-deposited layers is remelted once in the upper section of the

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buildup wall or twice in the first several layers. Therefore, the deposited alloy in the built up wall
is allowed the opportunity to be thoroughly mixed (the number of times being dependent on the
layer thickness and the weld pool penetration depth) in order to produce a final deposit with
uniform chemical composition and the expected phase. Although dilution from the substrate does
influence the chemical composition in first few deposited layers (as identified from the
measurements in Figure 7 and also the existence of the solid dissolved carbide precipitates), the
dilution-affected height is limited to 7mm when using the parameters listed in Table 1 and 2. The
dilution-affected height can potentially be reduced by adjusting the welding parameters and
preheating temperature to reduce the weld pool depth and/or layer height.

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3.4 Tensile test

Sample 2

Sample 3

Average

MPa
MPa
%

927
845
3.2

971
851
3.4

944.319.2
847.72.5
3.270.1

Unit

Sample 1

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The ultimate tensile strength (UTS), 0.2% offset yield strength (0.2% YS) and elongation results
collected at room temperature of the 3 specimens extracted from the middle section of the buildup
wall are listed in Table 3. As calculated from the stress-strain curves of the 3 specimens (Figure 8),
the 0.2% YS of the built up material is approximately 847MPa. As expected, the
room-temperature ductility of the specimens as shown in Table 3 are relatively low. In comparison
to tensile testing results in previous research for material produced by conventional methods, the
yield strength of the present as fabricated Fe3Al wall is approximately 50MPa higher. The room
temperature ductility is comparable but slightly lower than that of conventionally-produced
material, which is reported at 3.7% for annealed Fe3Al at 28at% [31]. The fracture surfaces of all 3
specimens (Figure 9) exhibit brittle transgranular cleavage fractures with lamellar stream-shaped
patterns and no dimples. Such behavior is same as the fracture modes shown in previous literature
for this material [10]. T-shaped cracks appear in all 3 specimens (Figure 9a, b, c) and Figure 9a
also shows some bifurcated cracks. The existence of secondary cracks indicates the low ductility
of the material.
Ultimate Tensile Strength
Yield Strength (0.2% offset)
Elongation

935
847
3.2

Table 3: Tensile test results at room temperature

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Figure 8: Stress-strain curves

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Figure 9: SEM micrographs of fracture surfaces (500) of: (a) Sample 1; (b) Sample 2; (c)
Sample 3

4. Conclusions

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It is feasible to produce Fe3Al-based iron aluminide, exhibiting consistent composition and

full density, by using the wire-arc additive manufacturing (WAAM) process incorporating
in-situ alloying of the elemental iron and aluminum components.
The yield strength at room temperature of the additively manufactured Fe3Al intermetallic
material is 50MPa higher than comparable material fabricated by conventional methods in
previous research, although the room temperature elongation is approximately 0.5% less.
Future researches will focus on manufacturing Fe-Al intermetallics with different aluminum
composition and different fabrication parameters. And more mechanical tests such as tensile
and fatigue tests will be performed in all three directions (longitudinal, transverse and
normal) of the buildup wall since the orientations of the large columnar grains may lead to
significant metallurgical changes.

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Acknowledgement
The authors gratefully acknowledge financial support from China Scholarship Council (CSC),
University of Wollongong (UOW), and Welding Technology Institute of Australia (WTIA), and
use of the facilities within the UOW Electron Microscopy Centre.

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Tables

Parameter
Unit
Current
A
Voltage
V
Travel speed
mm/min
Aluminum wire feed rate
mm/min
Iron wire feed rate
mm/min
Table 1: Details of welding parameters

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25
20.6
6
24
12
25

Sample 1
935
847
3.2

Unit
MPa
MPa
%

Sample 2
927
845
3.2

Sample 3
971
851
3.4

Average
944.319.2
847.72.5
3.270.1

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Parameter
Ultimate Tensile Strength
Yield Strength (0.2% offset)
Elongation

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Parameter
Unit
Aluminum content
at%
Specific deposition energy
kJ/mm
Deposition rate
g/min
Wall build height
mm
Wall width
mm
Number of layers
-Table 2: Resultant deposition parameters

140
12.7
100
695
1000

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Table 3: Tensile test results at room temperature

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