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Characterization of microstructure and residual stress in a 3D H13 tool steel

component produced by additive manufacturing

Article  in  Journal of Materials Research · September 2014

DOI: 10.1557/jmr.2014.190

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 Characterization of microstructure and residual stress in a 3D H13
tool steel component produced by additive manufacturing
Ryan Cottama) and James Wang
Industrial Laser Applications Laboratory, IRIS, Faculty of Science, Engineering and Technology, Swinburne
University of Technology, Victoria 3122, Australia
Vladimir Luzin
Bragg Institute, Australian Nuclear Science and Technology Organisation, Lucas Heights, New South Wales 2232, Australia

(Received 29 March 2014; accepted 25 June 2014)

H13 tool steel was deposited using the additive manufacturing technique Direct Metal Deposition
to produce a part having a wedge geometry. The wedge was characterized both in terms of
microstructure and residual stress. It was found that phase transformations were significantly
influencing the microstructure, which was then linked to the residual stress distribution as seen in
Fig. 8. The residual stress distribution was found to be opposite to that reported in the literature.
This was attributed to the low temperature martensitic phase transformation of the H13 tool steel
and the subsequent tempering of the microstructure with an increasing number of layers of
deposited material. The high hardness and compressive residual stress of the top 4 mm of the wedge
are ideal in die casting and forging dies, as it will resist thermal fatigue. It also has a hardness higher
than that produced by typical heat treatment processes.

I. INTRODUCTION is built. The advantage of this technology over DMD is

Additive Manufacturing (AM) is a group of technolo- support structures can be built allowing for overhanging
gies that builds near net shaped components by a track-by- features to be produced. Also the dimensional accuracy of
track, layer-by-layer method. There are two main this approach is superior.
approaches to the technology for metallic materials1; the One of the strengths of AM processes is their low cost
Direct Metal Deposition (DMD) approach and the powder for producing prototypes or low volume production runs
bed approach. In the DMD approach the substrate is melted of metallic components. This has led to applications in
by a heat source, which can be a Tungsten Inert Gas (TIG) aerospace,2,3 rapid tooling,4 and biomedical implants.5
torch, laser, or an electron beam, and when powder or a wire The other major strength of AM is the production of
is fed into the melt pool, this melts, Fig. 1(a). This formed complex shapes such as spline curves, hollow sections,
track of material is controlled in length and position by and lattice structures,6 which is changing the way compo-
a computer robotic system. Tracks of material are placed nents can be designed. Another advantage of AM DMD
side by side in such a fashion as to build a layer of a desired technology is the production of parts made from dissimilar
shape. The next layer is then built on top of the previous materials such as copper backed tool steel for increasing
layer and this is repeated until the component has been built. cycle times in die casting and injection molding.7 The
The major limiting factor with this technology is that production of tooling using AM draws on many of the
overhanging features cannot be produced. The powder advantages of AM and as such is the topic of this
bed approach uses a substrate plate initially, which sits on investigation.
a table that can be moved vertically, Fig. 1(b). A layer of H13 tool steel is one of the most commonly used tool
powder is swept over the substrate (typically as thick as the steels for producing die casting and forging dies. The
powder being used) and is melted to the substrate. The heat production of these dies involves the machining of the
source is computer controlled and the layers are melted in dies from large blocks of material after which a heat
such a fashion that a layer of the part is produced much like treatment is used to achieve the full strength of the
the DMD technology. The bed is then lowered and a new material. This process is costly and time consuming and
layer of material is swept over. The heat source then melts AM offers the ability to reduce the amount of machining
the next layer together. This is repeated until the desired part and hence wastage of this expensive material. DMD is
the main technology that has been used to produce blocks
of material for evaluation of the process. Hofmeister
a)
Address all correspondence to this author.
et al.8 evaluated the effect of laser parameters on the
e-mail: [email protected] thermal aspects of the processing, in particular, the cooling
DOI: 10.1557/jmr.2014.190 rate and its effect on the microstructure. It was found that

1978 J. Mater. Res., Vol. 29, No. 17, Sep 14, 2014 Ó Materials Research Society 2014
R. Cottam et al.: Characterization of microstructure and residual stress in a 3D H13 tool steel component produced by additive manufacturing

FIG. 1. Schematics of AM processes showing the key components; (a) DMD where (1) the laser beam, (2) nozzle shielding gas, (3) powder feeding
nozzle, (4) deposited track, (5) substrate; (b) selective laser melting (SLM) where (1) laser, (2) double rotating mirror system, (3) beam focus lens,
(4) powder feeding system, (5) building platform, (6) recoater, (7) powder recovery/recycle.

the cooling rate produced by the DMD process for H13 is that the effect of transformation plasticity and tempering of
around 3 K/s, which is quite fast and as such produces the microstructure were not taken into account in the
a cellular microstructure. For the range of laser parameters model. It is clear that H13 tool steel residual stresses are
tested, the dimension of the cellular structures only varies important for their use in making forming dies from
by several micrometers. Maziasz et al.9 evaluated the a fatigue point of view, this appears to be connected to
residual stress of spray formed and DMD deposited H13 the microstructure produced. These effects on a simple
and found that a tensile stress is produced during DMD in 3D build/component have not been evaluated and this is
the deposited region, which was balanced with a compres- the next step in developing the technology for this
sive stress in the substrate. It was also noted that the DMD material/application.
process produced an over tempering of the previous tracks,
which is undesirable. Pinkerton and Li10 evaluated the
effect of the powder morphology on the deposition of H13 II. EXPERIMENTAL
and found that the main difference was a rougher surface A POM DMD 505 equipped with a 5 kW CO2 laser
finish for the water atomized powder due to its irregular was used to manufacture the H13 tool steel wedge shape,
shape. Spray forming of H13 has also been studied11 and it Fig. 2. The STEP file of the wedge was open in the DMD
was found that process parameters influenced the micro- CAM software where a raster strategy was produced. The
structure produced, but more importantly, the compressive 90° cross-hatched path was used, Fig. 3, where the raster
residual stress state of the formed material increased tool moves through 90° between each layer, as this has been
life due to its ability to resist fatigue cracking. found to produce good material properties by the equip-
An understanding of residual stress formation in DMD ment manufacturer. The DMD processing parameters use
AM is still lacking. To date much of the work has a laser power of 2500 W, a traversing speed of 300 mm/min,
focused on simple structures such as walls12–14 and and a powder feed rate of 4.5 g/min. These parameters were
square pillars.13,15 The residual stress is compressive in developed in a previous trial and produced track
the center of all these structures and tensile is near the dimensions of 2 mm in width and 1 mm in height.
edges for both Waspaloy and stainless steel. A comparison Two layers were deposited sequentially followed by
between the wall and the pillar13 reveals that the magni- a 5 min interval, which was repeated six times giving
tude of the stress does not change significantly and the a build height of 12 mm.
distribution of stress is dictated by the geometry, which Residual strain through-sample-thickness scanning
can be linked to the cooling rates. For H13 there has been was carried out by neutron diffractometry at ANSTO in
a comprehensive study of residual stress, including full Kowari, NSW, Australia. The residual stress of the
thermal and mechanical modeling of the process,16 that wedge was measured down its center thus allowing for
were compared with experimental results. However, an the influence of section thickness to be resolved as
agreement between the experimental results and modeling a function of position. Three cross-sections were mea-
was missing. The difference can be attributed to the fact sured to ascertain the distribution of stress across the

J. Mater. Res., Vol. 29, No. 17, Sep 14, 2014 1979
R. Cottam et al.: Characterization of microstructure and residual stress in a 3D H13 tool steel component produced by additive manufacturing

polished down to 0.5 lm using colloidal silica. To reveal the

microstructure the sample was etched in 5% Nital solution for
5 min. The microscopic image was taken using a digital
camera set up on a stage where the height could be adjusted.
Scanning electron microscopy (SEM) was conducted on
a field emission gun microscope using the secondary electron
detector. Images were taken to show the changing micro-
FIG. 2. Dimensions of the AM wedge in mm.
structure as a function of position through the sample.
Temperature measurements were taken using K type
thermocouples supplied by Omega. To ensure a fast
response time of the thermocouple a 0.005 mm gauge
wire was used. The two wires were spot welded together
and inserted into a 1.5 mm OD alumina tube. Holes
1.5 mm in diameter were drilled into the back of the mild
steel substrate 2 mm from the top surface. A thermally
conductive ceramic glue was placed on the end of the
thermocouple and alumina sheath and pushed into the
hole to attach the thermocouple to the plate. Three
thermocouples were used and spaced 15 mm apart where
the central thermocouple was placed in the middle of the
wedge, thus allowing the temperature in the different
regions of the wedge to be monitored simultaneously.
The data were logged using Data Translator data logger
model number DT302. The data were logged at 200
points/s where each data set ran for 10 min.

III. RESULTS AND DISCUSSION

Figure 4(a) shows the temperature measured with the
FIG. 3. Schematic of raster pattern used in the production of H13 three thermocouples for the first two layers built. In the
wedge with the DMD system; (a) initial raster pattern, (b) alternate raster first layer the raster of the laser is up and down the length
pattern.
of the wedge, Fig. 3(a), hence there is a large variation in
the thermal profile as the laser passes the three thermo-
wedge and were also used to derive the variation of d0 couples. Initially the laser starts at the rear corner (the thick
(the unstrained lattice parameter) based on a stress bal- end) of the wedge and builds parallel to the thermocou-
ance. A 6  15 grid of measurement points were used ples. Each time the laser passes the thermocouple the
across the length of the wedge, a 7  6 grid across the end temperature rises and quickly decreases due to cooling
of the wedge, a 5  6 grid 2/3 of the total length of the from the substrate. The peak temperatures reached
wedge, and a 3  6 grid in the front section of the wedge. increases from track to track up to the point where the
A gauge volume of 2 mm was used to measure each point, laser runs over the thermocouples. Beyond this point the
and the wave length for the measurement was adjusted in laser is moving away from the thermocouples, therefore,
such a way that the (311) reflection could be used for the a decrease in the peak temperature is observed because the
stress measurement because this plane gives the best heat has further to travel to reach the thermocouples which
diffraction signal. Each point in the sample was measured increases thermal losses due to the thermal resistance of
in three orientations, thus allowing the calculation of the the material. The peak temperature reached is around
stress in three orthogonal orientations of the wedge. 600 °C, which is reasonable given that the thermocouples
Microstructural characterization was carried out by sec- were 2 mm below the top of the substrate. By the end of the
tioning the sample along the long axis in the same first layer the average temperature in the block has reached
orientation as the main neutron diffraction measurements. 150 °C, which is not that significant in terms of its effect on
The sample was then ground flat to a 600 grit size and the the microstructure. The laser then puts a track of material
microhardness measurements were conducted. A map of the around the edge of the build to increase dimensional
hardness was developed by taking microhardness measure- accuracy, which produces the second small trend in the
ments every 0.5 mm through the thickness of the sample and temperature data.
1 mm along its length. A load of 500 g was used to make the The laser then moves to the tip of the wedge and
hardness impressions. The sample was then ground and starts to build in an orthogonal orientation, Fig. 3(b).

1980 J. Mater. Res., Vol. 29, No. 17, Sep 14, 2014
R. Cottam et al.: Characterization of microstructure and residual stress in a 3D H13 tool steel component produced by additive manufacturing

FIG. 4. Temperature measurements in three thermocouples placed 2 mm below the surface of the substrate, where the central thermocouple was
positioned in the middle of the wedge and the other two were 15 mm either side; (a) layers 1&2; (b) layers 3&4; (c) layers 5&6; (d) layers 7&8;
(e) layers 9&10; (f) layers 11&12.

The thermocouple near the tip immediately spikes due to it temperature begins to rise more gradually than the pre-
being close to the tip and then falls as the laser moves vious thermocouple measurements when the laser is on top
down the wedge away from the thermocouple. Because of the thermocouple, and cools as the laser moves away.
the wedge is thinner at the tip, the rate at which it moves The rate of cooling is slightly slower than the central
down the wedge decreases with processing time. There- thermocouple because the length of the tracks increases
fore, as the laser approaches the middle thermocouple, the with the wedge thickness, and hence more heat is put into

J. Mater. Res., Vol. 29, No. 17, Sep 14, 2014 1981
R. Cottam et al.: Characterization of microstructure and residual stress in a 3D H13 tool steel component produced by additive manufacturing

the structure reducing the cooling rate. The laser then

approaches the thermocouple in the thick section. Like the
middle thermocouple its temperature rises due to the heat
from the approaching laser at a rate that is slower than the
middle thermocouple. This is due to the increasing length
of the tracks as the wedge thickens. Small spikes appear in
the thermocouple data as the laser passes the thermocouple
similar to the temperature profiles of the previous layer.
The laser then deposits a track of material around the edge
of the wedge, which leads to the final thermal temperature
excursions. The sample was then cooled for 5 min after the
two layers resulting in the temperature decay.
The trends in the thermal data are essentially the same
for Figs. 4(b)–4(f) with the only difference being that with
each increasing layer the distance between the thermo- FIG. 5. Macroscopic image of H13 tool steel wedge in cross-section
couple and the laser increases. The major effect this has on where the image was taken in the central cross-section of the wedge. The
the measurement is that it decreases the peak temperature dots on the image indicate the regions where close up SEM images were
reached due to thermal resistance of the material. This taken.
effect increases as the number of layers increases and it is
due to the heat from the laser diffusing from the meltpool. the wedge. The top layer shows a very fine martensitic
This produces a more even temperature as the heat from microstructure, which appears to have regions of retained
the different points combines and the thermal resistance of austenite between the martensite laths. This has not been
the material decreases the temperature measured. Interest- confirmed with x-ray diffraction. This is a reasonable
ingly by the fifth layer the average temperature reached assumption, however, as H13 has a very low martensitic
and stabilizes at around 200 °C for the rest of the build. transformation temperature.16 Figure 6(b) shows a coars-
The fact that the temperature remains elevated even in the ening of the microstructure but essentially the microstruc-
substrate during the build would be the cause of the ture is still the same. Figure 6(c) shows that the
tempering in the microstructure observed. microstructure has coarsened further and is dominated
Potentially the temperature in the wedge would be by martensitic laths, implying that the retained austenite in
higher and perhaps would exceed the tempering temper- the other images has been transformed. The formation of
ature of H13 of 565 °C. The thermal excursion of the first austenite and its subsequent transformation to martensite
layer only reaches a maximum temperature of 600 °C, in tool steels by the heat from a laser was observed by
which is low considering that the melting point of H13 is Colaco and Vilar.17 This is a reasonable assumption since
around 1430 °C, depending on composition. The steep this material has spent time at elevated temperature. Figure
temperature gradient is due to the low thermal conductiv- 6(d) shows that some of the martensite in the structure is
ity of H13 (24.5 W/m K). This illustrates the very localized being broken down and is similar to a microstructure of
heating during DMD processing. This coupled with the tempered H13 where carbide precipitation has occurred.
complex thermal excursion the underlying material expe- Figures 6(e)–6(h) all show this tempered microstructure
riences makes the analysis of the temperature reached in with prior austenite grain boundaries evident, which
the wedge difficult to calculate without the use of suggests the temperature in this region of the billet is
a complex finite element model, which is beyond the lower and has less impact on the structure.
scope of this study. The hardness map shown in Fig. 7 supports the
The macroscopic image of the cross-section of the H13 changing microstructure discussed above. The hardness
wedge is shown in Fig. 5. The pattern in this image of the top of the wedge is consistent at between 580 and
alternates, which is a result of the change in raster 650 Vickers and corresponds to the dull region of the
orientation between layers. Essentially one layer is the macroscopic image of Fig. 5. The coarsening of the
track in cross-section and the next is the track along its microstructure and the transformation of the austenite to
length. It is also noticeable that the top layer has a different martensite with increased depth in this top zone negates
hue to the rest of the sample, which is due to the fact that each other in terms of mechanical properties, resulting in
the top region of the samples did not etch as much as the this region having consistent hardness with changing
layers below, which can be attributed to a changing microstructure. At between 6 and 8 mm the hardness
microstructure. The white dots labeled a to h indicate the drops off significantly down to as low as 278 Vickers,
position of the SEM images in Fig. 5. which is the hardness of fully annealed microstructure.18
SEM of the etched microstructure in Fig. 6 shows how This reduction in hardness is exaggerated near the top of
the microstructure changes with position from the top of the wedge where it is conceivable that a high temperature

1982 J. Mater. Res., Vol. 29, No. 17, Sep 14, 2014
R. Cottam et al.: Characterization of microstructure and residual stress in a 3D H13 tool steel component produced by additive manufacturing

FIG. 6. SEM of the H13 tool steel wedge taken from the central cross-section. The positions of the images correspond to the position of the white dots
in Fig. 5.

has been reached due to the smaller cross-section of the the compression zone in the top and bottom regions of the
material. Beyond this the hardness is relatively unchanged, wedge does not match in depth. The compressive stress is
which is consistent with the microstructure not changing around 250 MPa in magnitude in both the top and bottom
and suggests that temperatures reached in the initial layers regions and there is a thin band of tensile stress just above
are not enough to change the microstructure further due to the central region of the sample that is around 150 MPa in
the heat from the upper layers. This result emphasizes magnitude. However, the stress distribution is compres-
the fact that the section thickness does play a role in the sive near the top and bottom surface and tensile near the
mechanical properties produced, particularly when the center, which is the opposite to that reported by other
microstructure can transform due to heat. investigations.12,14,15 They found the opposite trend where
The residual stress distributions for the H13 wedge are the center was in compression and the surface was in
shown in Fig. 8. The distribution of stress is not tension like an inverse quench.
symmetrical like a quenching stress,19 in that the side The compressive stress at the very top of the wedge
walls of the wedge are not in compression and the size of can be attributed to the low martensitic transformation

J. Mater. Res., Vol. 29, No. 17, Sep 14, 2014 1983
R. Cottam et al.: Characterization of microstructure and residual stress in a 3D H13 tool steel component produced by additive manufacturing

FIG. 7. Micro-Vickers microhardness map of H13 tool steel wedge, measured in the central cross-section, where the start of the hardness map is the
thick end of the wedge.

FIG. 8. Residual stress map of H13 tool steel wedge showing results of four different orientations where measurements were made. The units of the
scale are MPa.

temperature of this steel.16 It is well known in the welding the material, the size of the dilation component of the
literature that steels with a low martensitic transformation transformation, and the elastic modulus of the material.21
temperature produce compressive residual stresses in their This phenomenon is the cause of the compressive residual
martensitic regions. The formation of the compressive stress stress in the top layer of the wedge. Then further down it was
is due to the contraction (dilation) of the material during the observed that retained austenite was transforming to mar-
transformation.20 When this occurs at a low temperature tensite again, and this transformation exerts a compressive
tensile stresses that have formed during cooling are either stress on the structure resulting in the region of compressive
reduced or they become compressive. The final stress stress existing up to 2 mm into the structure. This corre-
magnitude and sign depends on the thermal expansion of sponds to the dull region of the macrostructure in Fig. 5.

1984 J. Mater. Res., Vol. 29, No. 17, Sep 14, 2014
R. Cottam et al.: Characterization of microstructure and residual stress in a 3D H13 tool steel component produced by additive manufacturing

The residual stress then transitions into a tensile re- manufacturing. Therefore, it is possible to use the tool
sidual stress just above the center of the wedge. This steel in the as-deposited condition, hence removing the
region corresponds with the change in hardness and also heat treatment step and saving time and money in
the tempering of the microstructure. Essentially the production. The compressive stress in this top layer is
tempering of martensite to form ferrite and iron carbide also desirable as this will resist fatigue of the die during
causes tension in the microstructure due to the lattice service, adding another advantage over the traditional
spacing decreasing with the precipitation of the iron machining method. However, tempering of the struc-
carbide.22 No further microstructure changes occur and ture below a 4 mm depth is undesirable. Perhaps this
as such, the stress transitions back to compressive to could be avoided by making the bulk of the die with
balance the tensile stress in the center of the wedge. Due to a cheap material like mild steel and then using H13 for
the layered nature of the wedge construction, the stress in the final 4 mm of the die. While this idea needs to be
plane is largely unaffected by the metallurgical trans- proven, it would considerably benefit AM production
formations and therefore the changes in residual stress of tool steel dies over conventional machining and heat
occur in the N direction and not the L and T directions, treatment.
Fig. 8.
The residual stress distribution of the wedge is the IV. CONCLUSIONS
opposite of that found in other studies where the center
was in compression and the exterior was in tension. The Characterization of the H13 tool steel wedge has
work of Moat et al.12 used Waspalloy, which does not revealed the complex relationship between the effect of
undergo a martensitic phase transformation during cooling heat from the laser, the metallurgical characteristics of
and has very low thermal expansion and conductivity. the H13, and their effects on the microstructure and
Rangaswamy et al.13,14 evaluated Inconel, another nickel residual stress formed. The compressive stress state at
based alloy, and austenitic stainless steel, both of which do the top of the wedge can be attributed to the low
not undergo a martensitic phase transformation during martensitic transformation temperature of the H13 ma-
cooling. Therefore, the residual stress produced is due terial. The significant depth of the compressive stress
only to the cooling of the component once built. As region was attributed to retained austenite transforming
confirmed by the finite element modeling of Wang23 this is to martensite due to the heat from the laser. The region
the cause of the residual stress distribution observed in of tensile stress was attributed to the martensite being
these studies. However, as shown above there are three tempered by the heat from the laser causing the carbon
metallurgical factors that influence the residual stress trapped in solution to precipitate out as iron carbide.
distributions formed in the H13 wedge, which have While the residual stress was not influenced by the
a greater influence on the residual stress formed than just geometry, the tempering of the H13 was. It was
the cooling rate alone being the cause of the residual stress suggested that lower laser power levels should be used
distribution of the previous studies. to produce thin sections of H13. The as-deposited
The wedge shape of the construction has had almost no hardness and the compressive stress state in the top
effect on the residual stress distribution formed, which 4 mm of the wedge are ideal for use in die casting and
is illustrated by the fact that the magnitude and sign of forging dies and this illustrates the potential of the
the residual stress changes in the N orientation and not the AM process as a method to produce tooling.
T and L. Again this supports the explanation that the
stresses have arisen due to metallurgical effects, which ACKNOWLEDGMENTS
are consistent through the different layers of the material.
The authors would also like to thank Mr. Girish
However, the hardness map in Fig. 7 shows that tempering
Thipperudrappa for his help with conducting the DMD
effects are more pronounced at the tip of the wedge than
experiments, Mr. Andrew Moore for his help with the
the thick end of the wedge. This can be attributed to the
thermal measurements, and AINSE for supplying funding
temperatures reached in the tip of the wedge being higher
for neutron proposal 2747.
for longer compared to the thick end. This is reasonable as
the volume of material is small and as such requires less
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1986 J. Mater. Res., Vol. 29, No. 17, Sep 14, 2014

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