A laser powder bed fusion system for in

situ x-ray diffraction with high-energy

synchrotron radiation
Cite as: Rev. Sci. Instrum. 91, 075104 (2020); https://doi.org/10.1063/1.5143766
Submitted: 07 January 2020 • Accepted: 09 June 2020 • Published Online: 02 July 2020

Eckart Uhlmann, Erwin Krohmer, Felix Schmeiser, et al.

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Rev. Sci. Instrum. 91, 075104 (2020); https://doi.org/10.1063/1.5143766 91, 075104

© 2020 Author(s).
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A laser powder bed fusion system for in situ

x-ray diffraction with high-energy
synchrotron radiation
Cite as: Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766
Submitted: 7 January 2020 • Accepted: 9 June 2020 •
Published Online: 2 July 2020

Eckart Uhlmann,1 Erwin Krohmer,1,a) Felix Schmeiser,2 Norbert Schell,3 and Walter Reimers2

AFFILIATIONS
1
Institute for Machine Tools and Factory Management, Technische Universität Berlin, Pascalstraße 8-9, 10587 Berlin, Germany
2
Institute for Materials Science and Technology, Metallic Materials, Technische Universität Berlin, Ernst-Reuter-Platz 1,
10587 Berlin, Germany
3
Helmholtz-Zentrum Geesthacht, Max-Planck-Str. 1, 21502 Geesthacht, Germany

a)
Author to whom correspondence should be addressed: [email protected]

ABSTRACT
In Laser Powder Bed Fusion (LPBF), the highly localized energy input by the laser leads to high-temperature gradients. Combined with the
inherent cycles of re-melting and solidification of the material, they can result in high mechanical stresses. These stresses can cause distortion
and cracking within the component. In situ diffraction experiments with high-energy synchrotron radiation allow an analysis of the lattice
spacing during the LPBF process and provide insight into the dynamics of stress generation and texture evolution. In this work, an LPBF
system for the purpose of synchrotron x-ray diffraction experiments during the manufacturing process of multi-layer components with
simple geometries is described. Moreover, results from diffraction experiments at the HEMS beamline P07 at PETRA III, DESY, Hamburg,
Germany, are presented. Components with a length of ls = 20 mm and a width of ws = 2.5 mm consisting of 100 layers with a layer thickness
of Δz = 50 μm were produced using the nickel-base alloy Inconel 625 as the powder material. Diffraction experiments were carried out in
situ at sampling rates of f = 10 Hz with a synchrotron radiation beam size of 750 × 70 μm2 . The presented experimental setup allows for
the observation of arbitrary measuring positions in the sample in the transmission mode while gathering full diffraction rings. Thus, new
possibilities for the observation of the dynamic evolution of strains, stresses, and textures during the LPBF process are provided.
Published under license by AIP Publishing. https://doi.org/10.1063/1.5143766., s

I. INTRODUCTION knowledge considering their origins and a profound understand-

ing of the physical phenomena in melt-pool creation, solidification,
The market of additive manufacturing systems for metal com- and microstructural evolution is needed. At this point, simulation
ponents has been growing rapidly in recent years1 with a focus on models help us to understand and to predict residual stress,6 defect
powder-bed based manufacturing technologies, such as Laser Pow- formation,7 and microstructure.8 However, those models require
der Bed Fusion (LPBF), which is also referred to as Laser Beam experimental validation. Due to the small timescales of melting and
Melting (LBM) or Selective Laser Melting (SLM). LPBF offers the solidification processes during LPBF, highly dynamic monitoring
possibility to design and manufacture components with complex procedures are required to collect experimental data with sufficient
geometries while maintaining good mechanical properties. How- temporal resolution. Thermal metrology based melt-pool monitor-
ever, the process stability still needs improvement as the limited ing systems have been widely addressed in research,9 and some are
reproducibility inhibits the breakthrough of LPBF in fracture-critical state of the art in commercial LPBF systems. They provide impor-
applications.2 Current challenges include crack-inducing defects3 tant insights into the dynamics of the process. Yet, those are surface
or residual stresses4 and require non-destructive testing methods related measurement techniques with limited suitability to gather
and material qualification processes.5 In order to avoid the for- information about bulk properties. Hence, new in situ measure-
mation of defects and to control the residual stress states, further ment methods are necessary, especially in the challenging case of

Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766 91, 075104-1
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the investigation of residual stress evolution and varying metallic In this paper, an experimental system for in situ x-ray diffrac-
phase structure.10 With the development of the third-generation tion with high-energy synchrotron radiation is presented, which is
synchrotron light sources, in situ diffraction experiments during designed for the investigation of the evolution of textures and resid-
time-critical manufacturing processes became possible.11 Together ual stresses during the build process of three-dimensional parts.
with x-ray imaging data, x-ray diffraction with high-energy syn- With the presented setup, it is possible to produce multi-layer parts
chrotron radiation offers bulk sensitive insights into the melting and with conditions mostly similar to the industrial LPBF process. This
solidification process in LPBF. system’s key advantages are the possibility to gather full diffrac-
Only recently researchers presented their work on in situ x- tion rings to improve measurement accuracy, the free choice of the
ray diffraction and imaging in LPBF. Uhlmann et al.12 discussed measuring position in the sample, and the feasibility of various mea-
the complex implementation of such an experimental setup and surement modes that deliver a range of spatially and temporally
the requirements that the LPBF system should meet to simulate an resolved data. Further experimental results using the here described
industrial system. Bidare et al.13,14 presented a compact system with experimental setup have been discussed in depth by Schmeiser
access for x rays and suitable for several in situ imaging techniques et al.33
such as high-speed schlieren imaging. The first results from in situ x-
ray diffraction and in situ x-ray imaging experiments with a system II. SYSTEM DESCRIPTION AND SPECIFICATIONS
that mimics LPBF conditions were reported by Zhao et al.15 They
A. Instrument design
observed dynamic melt pool evolution, keyhole pore formation, and
the motion of ejected particles in the process of melting and solid- The experimental instrumentation consists of an LPBF system
ification of Ti6Al4V powder with a frame rate of f = 50 kHz. In positioned in the x-ray beam path of a synchrotron light source
addition, they showed the possibility to investigate phase transfor- such that a desired gauge volume in the sample is irradiated and
mations by means of x-ray diffraction. Subsequently, the described the diffracted x rays are detected by a 2D detector, e.g., scintillator-
LPBF system was upgraded and used in several further investiga- based. The experimental approach is depicted in Fig. 1. The cus-
tions so that high-speed x-ray imaging with a frame rate of up to tomized LPBF system, which allows for in situ x-ray diffraction
6.5 MHz proved possible to give profound insight into the transient corresponding to the described experimental geometry, is presented
dynamics of the LPBF process.16 Guo et al.17 continued the research below. The specified system was designed to operate at the HEMS
on powder spattering behavior and evaluated the dynamics of pow- beamline P07 at PETRA III.34 Hence, any diffraction related speci-
der spattering as a function of time, ambient pressure, and location. fications or described peripheral equipment refer to the beamline’s
Additional research on powder motion was conducted by Escano facilities.
et al.18,19 who designed a device to examine the powder deposition One of the main requirements during the design process was to
by a spreading wiper by means of high-speed x-ray imaging. Another reproduce the conditions of a commercial LPBF setup as precisely as
setup that allows the investigation of phase transformations and lat- possible while accounting for the required x-ray transparency. First,
tice expansion during cyclic heating and cooling using micro-x-ray attenuation of x rays throughout the experimental setup, besides
diffraction was introduced by Kenel et al.20 The setup simulates the in the sample, should be avoided in order to prevent noise in the
thermal behavior of a multi-layer LPBF process but under consid- measurement. Therefore, compared to a state of the art industrial
erably different conditions than in a common industrial system as LPBF system, the powder bed is elevated and unavoidable objects in
no powder material is involved. Nevertheless, the advantage of the the x-ray path are made of material with high x-ray transparency.
presented setup is the in situ gathering of surface temperature infor- Furthermore, the system features an additional linear axis, ensur-
mation.21 Leung et al.22 used a custom-built system called LAMPR, ing linear motion of the powder bed not only vertically but also
short for Laser Additive Manufacturing Process Replicator, for in horizontally, perpendicular to the incident synchrotron radiation
situ x-ray imaging experiments. Research with the LAMPR includes beam. Since the synchrotron radiation beam and the detector are
time-resolved melt track, spatter, and defect formation of different stationary, the powder bed, therefore, can be positioned relative to
materials.22–24 Calta et al.25 developed a system for the purpose of the measuring instrumentation without moving the whole process
in situ x-ray imaging and diffraction of single tracks. They reported chamber. Thus, free variation of the measuring position is facilitated,
experiments showing pore formation via in situ x-ray imaging and and different measurement modes can be implemented.
β-Ti–α-Ti phase transitions upon cooling in Ti6Al4V via x-ray The InSituLPBF system presented here is based on the mod-
diffraction. In further studies, utilizing the mentioned experimental ular industrial machine AconityMINI manufactured by ACONITY3D
systems, melting and solidification dynamics in single tracks of Alu- GMBH, Herzogenrath, Germany. The process chamber was designed,
minum 6061 and AISI 4140 steel26,27 and pore formation and spat- built, and integrated into the industrial system at the INSTITUTE FOR
ter dynamics in the laser–metal-interaction with solid and powdery MACHINE TOOLS AND FACTORY MANAGEMENT of TECHNISCHE UNIVERSITÄT BERLIN
Ti6Al4V28–31 were investigated. Finally, Hocine et al.32 presented in order to meet the requirements for in situ x-ray diffraction exper-
an advanced experimental instrumentation for in situ diffraction iments. The system consists of three modules. Control systems for
experiments. Their instrumentation adopts a hopper-based pow- media and energy supplies as well as the laser source are situated
der feeding system and a particle filter system for the inert gas in the first module, the control cabinet, which also serves as the
circulation and is therefore applicable for multi-layer experiments. human–machine interface. The second module is the process cham-
They analyzed the influence of laser processing parameters and ber itself. The third module contains the components for circulation
scanning strategies on the phase transformation and microstruc- and filtration of the inert gas atmosphere in the process chamber.
tural evolution in several Ti6Al4V samples in the reflection For in situ x-ray diffraction experiments, the process chamber is
mode. mounted on a heavy load hexapod from PHYSIK INSTRUMENTE (PI) GMBH

Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766 91, 075104-2
Published under license by AIP Publishing
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FIG. 1. Schematic of the experimental approach for x-ray diffraction with synchrotron radiation.

& CO. KG, Karlsruhe, Germany, which is part of the Experimental is mounted on a rigid guide rail, which is actuated in the z-axis
Hutch 3 at the HEMS beamline P07. The laser source is a single- direction by an EMC electromechanical cylinder, BOSCH REXROTH AG,
mode continuous wave Ytterbium fiber laser YLR-400-AC from IPG Lohr am Main, Germany. Additionally, the sample holder is actu-
LASER GMBH, Burbach, Germany, which emits radiation at a wave- ated in the x-axis direction by a C-shaped driver, which is mounted
length of λL = 1070 nm with a nominal power output of PL = 400 W. on a CKK-110 linear axis, BOSCH REXROTH AG, Lohr am Main, Ger-
The laser fiber is connected to the three-axis deflection unit many. The motion arrangement comprises a sliding contact between
Axialscan-30 from RAYLASE, Wessling, Germany, via a collimator. The the C-shaped driver and the sample holder such that the move-
installed deflection unit features a focus compensation and scanning ments of the two linear axes are decoupled. As a result, the C-shaped
speeds of vL = 3 m/s can be realized. A cooling unit SC11 from GLEN driver is fixed in the z-direction. This principle assures a constant
DIMPLEX DEUTSCHLAND GMBH, Kulmbach, Germany, provides the scan working plane, as the glassy carbon plates are mounted on the
head with coolant for the galvo mirrors. The laser beam has a Gaus- driver.
sian shape with an adjustable focus diameter between dL ≈ 60 μm and When the sample holder moves in the positive z-direction, the
500 μm (1/e2 ) and is deflected onto a powder bed with a length of glassy carbon plates stay in position, leading to a void between the
lb = 70 mm and a width of wb = 3 mm. The optical working dis- substrate plate and the edges of the glassy carbon. The fully auto-
tance of the setup is 455 mm. The powder bed is enclosed by two matic recoating mechanism fills the void with powder and levels
glassy carbon plates, HTW HOCHTEMPERATUR-WERKSTOFFE GMBH, Thier- it. The operating principle is demonstrated in Fig. 3. The powder
haupten, Germany, each with a thickness of 1 mm in the x-ray recoating mechanism is based on a funnel, which is actuated in the x-
transmission direction. The samples are built on a replaceable sub- axis direction by another CKK-110 linear motion axis. For recoating,
strate plate, which is sandwiched between the glassy carbon plates. the sample holder is moved to the recoating position [see Fig. 3(a)].
The material of the substrate is selected according to the powder Then, the funnel is moved over the sample holder up to its turning
material. The sample holder together with the glassy carbon mount point. During motion, the powder flows into the void due to gravity
is depicted in Fig. 2. Here, substrate plates with the dimensions of alone [see Fig. 3(b)]. On its way back, the elastomeric lip attached
70 × 10 × 3 mm3 are mounted in the groove of the stainless to the funnel levels the powder layer, as depicted in Fig. 3(c), and
steel build plate. The surrounding material is PAMITHERM 41140, scrapes the excess powder to the sides of the sample holder. The
VON ROLL DEUTSCHLAND GMBH, Augsburg, Germany, a high-temperature gap between the funnel and glassy carbon plates is usually set to
resistant silicone phlogopite mica laminate to thermally insulate the ∼100 μm but can be adjusted manually using the funnel height
carriage from the installed heating ceramic, BACH RC GMBH, Seefeld, adjustment and precision sheet-metal. Returned to its parking posi-
Germany, which is in contact with the bottom side of the build tion, the funnel orifice is sealed by the thick powder layer beneath.
plate. The substrate plate can be heated up to 300 ○ C. If the desired The funnel shape was tested and optimized for titanium and nickel-
gauge volume is in a lateral distance of more than 10 mm to either base alloys with a particle size distribution of 20 μm–63 μm and a
side of the glassy carbon mount, the sample holder allows for Bragg spherical particle shape. Note that, e.g., finer powder or different
angles 2θ ≤ 14○ without shadowing of the diffracted x rays. The materials could lead to bridging in the orifice due to cohesiveness
detailed view in Fig. 2(a) shows a schematic illustration of the of the powder. With the use of small vibration motors, which were
powder bed, which is confined between the two glassy carbon plates installed on the funnel and are not depicted in Fig. 3, the flowa-
and the substrate beneath during an experiment. The sample holder bility of the powder was improved and formerly clogging powders

Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766 91, 075104-3
Published under license by AIP Publishing
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FIG. 2. Sample holder: (a) rendering of the sample holder and schematic of the sample during the experiment, (b) linear axis for x-axis motion, and (c) linear axis for z-axis
motion.

could be processed as well, e.g., TNB-V5 powder. Using an exten- excess pressure during flooding and laser melting process is con-
sion, the powder capacity of the funnel can be increased as desired. stantly controlled by the proportional pressure regulator VVPM,
With a layer thickness of Δz = 50 μm, parts consisting of 120 lay- FESTO AG & CO. KG, Esslingen, Germany, while the gas flow is monitored
ers or approximately a height of hs = 6 mm were produced so far by the installed flow sensor SFAB, FESTO AG & CO. KG, Esslingen, Ger-
utilizing such a powder capacity extension. The motion limits of the many. Both components are part of the basic AconityMINI system.
z-axis allow for maximum part heights of hs = 10 mm or 200 layers The ambient conditions inside the process chamber are monitored
when using a layer thickness of Δz = 50 μm. by means of an oxygen sensor and a thermocouple. Oxygen values
For laser processing, the process chamber has to be sealed and and excess pressure and inert gas flow data are logged on the com-
purged with an inert gas, usually argon. For this purpose, the pro- puter besides other data such as axis positions and laser status. Two
cess chamber has an inlet and outlet port for inert gas flooding. The further ports in the process chamber walls serve as inlet and outlet

FIG. 3. Functionality of the powder recoating mechanism: (a) positioning, (b) filling with fresh powder, and (c) leveling the powder bed.

Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766 91, 075104-4
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for the continuous smoke gas extraction and filtration. The recir-
culation and filtration of the inert gas atmosphere ensures that the
process chamber is mostly free of welding fumes and particles that
might interfere with either laser or x-ray beam and cause distur-
bances during the measurement. The power of the circulation pump
can be regulated to adjust the flow speed.
The inlet and outlet windows of the process chamber for the
incident and diffracted x rays are made of Kapton foils, DUPONT, INC.,
Wilmington, USA, with a thickness of 50 μm. As diffuse laser radia-
tion might pass through the Kapton foil windows, laser safety mea-
sures need to be taken before emitting radiation. Besides the desired
metal sample, the synchrotron radiation beam passes through ambi-
ent air, Kapton foils, argon, and glassy carbon with distinguished
x-ray transparency and negligible noise.

B. Measurement modes
For the synchrotron x-ray diffraction experiments described
here, a two-dimensional area detector is used. In combination with
the use of monochromatic synchrotron radiation, the diffraction
images deliver no information about lattice plane spacings in the
transmission direction, which is therefore neglected in subsequent
explanations. Up to this point, three different measurement modes
are possible to conduct with the InSituLPBF system at PETRA III
(see Fig. 4). In measurement mode 1 (MM1), the gauge volume (GV)
is in a defined distance to the topmost layer. Relative to the sam-
ple, the vertical position of the gauge volume changes layer by layer,
whereas the lateral position is fixed throughout the buildup of one
sample.
In measurement mode 2 (MM2), the gauge volume corre-
sponds to a fixed volume in the sample, which can be monitored
during the melting and solidification of all the above layers. For this
mode, the z-axis translation of the beamline hexapod compensates
the z-axis translation of the powder bed and therefore ensures a fixed
measurement height. FIG. 4. Feasible measurement modes with the InSituLPBF system at PETRA
In the third measurement mode (MM3), the gauge volume is in III.
a defined lateral and vertical distance to the laser spot. This measure-
ment mode is limited to samples with scan tracks longitudinal to the
incident synchrotron radiation beam. After the laser scans a longitu-
dinal track, the sample holder is moved translationally according to one type of scan vector defined. However, using certain commercial
the hatch distance h, before the laser scans again. As a result, the pro- Computer Aided Manufacturing (CAM) software with the capability
cess time increases significantly compared to the other measurement to generate CLI files, the definition and production of more com-
modes. plex samples with several vector types would be possible, as long
as the powder bed size of the experimental system is not exceeded.
C. Data preparation For the sake of ease of interpretation, only unidirectional, paral-
lel scanning patterns were utilized in the experiments conducted so
The scan path of the laser is provided in a Common Layer Inter- far.
face (CLI) file, where the scan vectors are listed in sequence for each
layer separately. They are defined by their starting and ending coor-
dinates in the working plane. An algorithm to generate CLI-files of III. EXPERIMENTAL PROCEDURE
simple cuboid samples was implemented in MATLAB 2017b, The
MATHWORKS, INC., Natick, USA. Its input parameters are length ls , A. Sample and system preparation
width ws , height hs , layer thickness Δz, hatch distance h, and ori- In order to produce a new sample, a substrate plate has to be
entation of the scan vectors of the desired sample. In this study, the inserted into the groove of the build plate and fixed via two headless
laser scan tracks were oriented either parallel or perpendicular to the screws. After placing the two glassy carbon plates into the slots of
incident synchrotron x-radiation beam such that either transverse or the carriage and fixing them, the sample holder is ready for initial
longitudinal strains relative to the scan track can be evaluated in situ. powder coating. Although the recoating procedure runs fully auto-
Unlike in commercial data preparation for LPBF parts, there is only matic during the LPBF process, the initial layer has to be applied

Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766 91, 075104-5
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semi-automatically as thinly as possible to guarantee sufficient volumes of the solid Vs,irr and the powder Vp,irr . The irradiated vol-
bonding of the first layer with the substrate. Before each experi- umes Vs,irr and Vp,irr are calculated according to the chosen gauge
ment, the chamber is sealed and purged with the argon gas. With volume of 750 × 70 μm2 , the thickness of the sample ws , and
the installed oxygen sensor, the oxygen level is monitored through- the combined thickness of the powder gaps. They equal Vs,irr =
out the entire process. As soon as the oxygen content reaches a level 0.131 mm3 and Vp,irr = 0.026 mm3 . Including an error estimation
below 2000 ppm, the circulation pump can be turned on to remove of 3% for possibly varying values for the solidified material density
welding fumes from the laser beam path during the manufacturing ρs = 8.5 g/cm3 and the bulk density of the powder ρp = 4.5 g/cm3 , we
process. In order to set the measuring position, the left, right, and derive a maximum fraction of wp,irr = 13 wt. % of the irradiated mass
upper edge of the first layer are determined by incrementally collect- for the powder material,
ing diffraction patterns after laser scanning of the first layer. This can
be necessary as scan track widths and therefore sample geometries Vp,irr ⋅ ρp
may vary with changing laser scanning parameters. The measuring wp,irr = . (1)
Vp,irr ⋅ ρp + Vs,irr ⋅ ρs
position can then be set accordingly in relation to the first layer’s
edges by adjusting (a) the position of the process chamber to set the
vertical distance of the gauge volume to the top layer and (b) the The samples were manufactured using a laser power of PL = 55
position of the sample holder in the process chamber to set the lateral W, a scanning velocity of vL = 50 mm/s, a laser beam diameter of
measuring position. Eventually, the in situ diffraction experiment dL ≈ 60 μm (1/e)2 , and a unidirectional, longitudinal scanning
can be started. pattern with respect to the synchrotron radiation beam direction.
Furthermore, MM1 was employed, so the gauge volume stayed
in a constant distance to the top surface of the sample. The laser scan
B. X-ray diffraction experiments
time tL indicates the time during which the laser emits radiation, i.e.,
The x-ray diffraction experiments were conducted at the P07 exposes the current powder layer. With the given parameters, the
HEMS beamline at PETRA III at Deutsches Elektronen-Synchrotron total laser scan time tL,t , which is the duration of scanning of one
(DESY),34 where the process chamber module was mounted on the single layer, is tL,t = 7.8 s.
heavy load 6-axis positioning system (see Fig. 5). The material used For the experiments, an x-ray energy of 98.02 keV
in the experiments was Inconel 625 powder from M4P MATERIAL SOLU- (λ = 0.126 49 Å) was used, and the beam size was set to 750 × 70 μm2 .
TIONS GMBH, Magdeburg, Germany, with a particle size distribution The beam height of 70 μm ensured for sufficient spatial resolution
of 20 μm–63 μm. The layer thickness was set to Δz = 50 μm. Sam- close to the layer thickness. Combined with the chosen beam width
ples consisting of 100 layers, resulting in samples with a height of of 750 μm, it was ensured that enough grains were irradiated in
∼hs = 5 mm, a length of ls = 20 mm, and a thickness of ws = 2.5 mm order to collect full diffraction rings. The diffraction patterns were
in the transmission direction, were produced during the in situ mea- collected with the Perkin-Elmer XRD1621 2D detector with an expo-
surements. To account for the thermal boundary conditions in an sure time of t = 0.1 s and a sampling rate of f = 10 Hz. Furthermore, a
industrial scale LPBF machine, a powder-filled gap of 250 μm was calibration measurement was performed using a LaB6 powder sam-
left on either side of the sample and the powder-bed limiting glassy ple fixated between the glassy carbon plates in the process cham-
carbon plates. Regarding the synchrotron radiation beam, the irradi- ber. The collection of calibration diffraction patterns using the same
ated powder was factored in during the subsequent data analysis by x-ray diffraction exposure parameters as during the in situ experi-
excluding data points showing less than 40% of the respective maxi- ments enabled the precise determination of the sample-to-detector
mum peak intensity. In the described experiments, the powder con- distance and the detector tilt. The detector delivers 2D intensity dis-
tributes to about wp,irr = 10 wt. % of the irradiated mass, calculated tributions with a pixel resolution of 2048 × 2048 and a pixel size
using Eq. (1) with respect to the gauge volume and the irradiated of 200 × 200 μm2 . For polycrystalline materials such as metals, the
x-ray beam is diffracted as a number of cones onto the flat panel
detector, resulting in a diffraction pattern of a set of concentric rings.
The radius of the diffraction ring is proportional to the Bragg angle,
which, in turn, is used to calculate the interatomic spacing following
the Bragg equation,
2d ⋅ sin θ = n ⋅ λ. (2)

In case the interatomic spacing for a stress-free sample is known,

deviations from the measured spacing can be used to calculate
strains and stresses in the observed gauge volume.
During the in situ measurements, diffraction patterns are col-
lected continuously by using the post-trigger function of the beam-
line’s control software. Once the image acquisition is started, a single
dark image is taken, which is subsequently subtracted from all of the
diffraction patterns. During the LPBF process, the sample moves in
and out of the desired gauge volume as a consequence of the recoat-
FIG. 5. Experimental setup at HEMS beamline P07 at PETRA III, DESY, Hamburg,
ing procedure. Image collection during that time does not gener-
Germany.
ate useful data, which is why the simultaneously logged positioning

Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766 91, 075104-6
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information of the sample holder is used to select for the applicable a clear peak in the strains is visible in both TD and BD. At that point
images during post-processing. in time, the laser passes over the gauge volume, which is why the
peak occurs first in the left gauge volume, then in the center of the
sample and finally in the right edge gauge volume. The peak strains
during the laser passage vary by the measuring position. For the cen-
IV. EVALUATION OF EXPERIMENTAL RESULTS
ter and right edge gauge volume, the median strain in TD during the
The diffraction patterns are segmented into equal size cake peak is about ε311
TD = 0.8%, while in the left gauge volume, it reaches
pieces, which correspond to the principal directions of the sam- only about 0.4%.
ple geometry. Azimuthal angles of η = 0○ and η = 180○ equal the This is caused by differences in the heat flow rate, which is
transverse direction (TD) with respect to the synchrotron radiation illustrated in Fig. 7. The material in the left gauge volume is heated
beam direction, while the build-up direction of the sample (BD) first during the laser scan of a layer. All of the surrounding mate-
is characterized by η = 90○ and η = 270○ . These cake pieces are rial, i.e., powder, previously solidified layers below and the substrate
then integrated using the software Fit2D35 to gather 1D line pro- plate, is cold. Therefore, heat conduction happens rapidly, leading
files from the 2D data. The 1D line profiles are subsequently par- to a lower degree of lattice expansion. For the center and right edge
tially fitted by a Voigt function employing custom Python scripts gauge volumes, the surrounding material, on average, has a higher
utilizing the “lmfit” package.36 The fit function delivers a paramet- temperature than for the left gauge volume since the left side of the
ric description of the peaks and is used to extract the peak position, corresponding gauge volume was already heated up, reducing the
peak intensity, full width at half maximum (FWHM), and associated temperature gradients and, thus, slowing down the heat conduction.
errors. From the peak positions and the stress-free lattice parameter This type of lateral heat accumulation was also shown in simula-
d0 , the lattice strain ε is calculated and can be plotted over differ- tive results by Parry et al.6 The described effects lead to higher peak
ent timescales. The stress-free lattice parameter d0 was determined temperatures in the gauge volume, resulting in higher lattice strain
from stress-free cuboid samples in a separate experiment.33 For face- peaks.
centered cubic materials such as Inconel 625, generally the fourth While the peak itself is caused by a rise in temperature, the laser
diffraction ring, corresponding to the 311 lattice plane, is analyzed does not affect the two directions TD and BD in the same magni-
as its stress state correlates well with the macroscopic stress of the tude. For all of the measuring positions, the median strain values in
material.37 TD are higher than in BD. Since the strain values for TD and BD for
Due to the sample’s geometry, a triaxial stress state must be each point in time are calculated from the same diffraction pattern,
assumed. Therefore, the measured strains in TD and BD are affected they represent grains with the same temperature. Therefore, both
by the stress in the longitudinal direction (LD). The experimen- directions are affected by the temperature and the subsequent ther-
tal geometry used here, however, does not deliver any information mal expansion the same way, which implies that any strain disparity
regarding the longitudinal direction. Nevertheless, the argument in between the two is purely elastic. Hence, the difference between the
the following paragraphs is based on the differences in the strain directions has to be caused by mechanical stresses, which themselves
progressions in TD and BD. Since the contribution of LD is equal are a result of the thermal gradient mechanism.38 When the top layer
to both respective directions, the difference between TD and BD of the part is exposed to the laser, its temperature increases rapidly.
is unaffected by LD. Therefore, valuable conclusions can be drawn The material expands, but the colder material below hinders the
even without the knowledge of the full triaxial stress state. thermal expansion due to its lower temperature. As a consequence
In Fig. 6, the average strain progression during the produc- of the high temperature in the top layer, the material plasticizes and
tion of cuboid samples over the course of manufacturing is shown. is compressed plastically. After being exposed by the laser, the mate-
This figure illustrates three subplots (a)–(c), which show different rial cools down and contracts. Caused by the plastic compression
measuring positions according to Fig. 6(d). For each subplot, one during heating, the contraction is now hindered and tensile stresses
individual cuboid sample [Fig. 6(e)] was additively manufactured are introduced. This effect is much more pronounced in the work-
and measured layer after layer with a total number of layers of ing plane than out of plane, which results in higher tensile stresses
n = 100 using the parameters given in Fig. 6(f). One diagram sum- in TD. As a result, there is a transverse contraction in BD leading
marizes the data from layers 20 to 100 by plotting the lattice strains to lower lattice strains. Below the plasticized zone, the material is
ε311 in both TD and BD over the laser scan time tL . There are no data expanded by the hotter material above, which adds another tensile
before or after laser emission. For the diagrams presented here, the effect on the gauge volume. The gauge volume with a distance of
measurements from layer 1 to 19 were omitted in order to observe zGV = 150 μm to the top surface most likely experiences a combina-
stable process conditions. In LPBF, the effective layer thickness of tion of both effects.
the deposited powder layer and therefore also the solidified layer The magnitudes of this effect are dependent on the lateral posi-
typically varies over the first few layers.14 tion of the gauge volume. In the center of the sample, this effect is the
While the colored areas show the full range of strain values for strongest, resulting in the highest difference between the strains in
each point in time for the layers 20–100, the lines represent the cor- TD and BD. This holds true for both before and after the laser passes
responding median strain value. The number of measurements for over the gauge volume. The difference before the laser passes over
each diagram is about 80 × 78 = 6240 measurements, with 80 lay- the gauge volume originates from the manufacturing of the previous
ers consisting of 78 captures each. With respect to Fig. 4, the lateral layer, where the stresses were induced after the laser scan. Then, after
distance of the gauge volume was xGV = 1 mm, xGV = 10 mm, and the laser passage, the effect is repeated and stresses are induced again
xGV = 19 mm. Thus, the peripheral measuring positions were located due to the process discussed above. Close to the edges, the strain
1 mm away from the edge of the sample. In each measuring position, difference is smaller than in the center before the laser passes over

Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766 91, 075104-7
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FIG. 6. Strain progression in cuboid samples made from Inconel 625. Gauge volumes were located (a) close to the left edge, (b) in the center, and (c) close to the right edge
of the sample in three separate experiments. (d) Schematic diagram of the experiment. (e) Cuboid samples. (f) Process and measurement parameters.

the gauge volume. Due to the proximity of the edge gauge volumes over the gauge volume. Despite the free surfaces close to the left and
to both the top surface and side faces of the sample, the free sur- right edge gauge volumes, the energy input by the laser does still
face allows for free expansion and contraction in TD, resulting in have a noticeable effect, which is indicated by the increase in the
minimal stress build-up. This is further underlined by the median strain difference during cooling after the laser passed over the gauge
strain value in TD, which is close to ε311
TD = 0% before the laser passes volume.

Rev. Sci. Instrum. 91, 075104 (2020); doi: 10.1063/1.5143766 91, 075104-8
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FIG. 7. Schematic diagram of heat conduction from the melt pool and lateral heat accumulation in an LPBF sample.

3
V. CONCLUSIONS E. Uhlmann, G. Gerlitzky, and C. Fleck, in Proceedings of the 28th Annual
International Solid Freeform Fabrication Symposium, Austin, Texas (University of
An LPBF system for the realization of in situ x-ray diffraction Texas, 2017), p. 48.
experiments during the buildup of multi-layer samples was pre- 4
S. Leuders, M. Thöne, A. Riemer, T. Niendorf, T. Tröster, H. A. Richard, and
sented. It is based on an industrial system with a custom-built pro- H. J. Maier, Int. J. Fatigue 48, 300 (2013).
5
cess chamber in order to mimic the industrial process as closely as J. L. Bartlett and X. Li, Addit. Manuf. 27, 131 (2019).
6
possible while considering the special requirements to carry out in L. Parry, I. A. Ashcroft, and R. D. Wildman, Addit. Manuf. 12, 1 (2016).
7
situ x-ray diffraction experiments. The design of the process cham- A. M. Rausch, V. E. Küng, C. Pobel, M. Markl, and C. Körner, Materials 10, 1117
ber allows for observation of arbitrary measuring positions in the (2017).
8
sample in the transmission mode while gathering full diffraction T. M. Rodgers, J. D. Madison, and V. Tikare, Comput. Mater. Sci. 135, 78
(2017).
rings. First experiments conducted at PETRA III show promising 9
S. K. Everton, M. Hirsch, P. Stravroulakis, R. K. Leach, and A. T. Clare, Mater.
results and give insight into the dynamics of the lattice spacing Des. 95, 431 (2016).
during the build-up of Inconel 625 samples consisting of 100 lay- 10
M. Mani, B. M. Lane, M. A. Donmez, S. C. Feng, and S. P. Moylan, Int. J. Prod.
ers. Upcoming scientific publications will focus on the results of Res. 55, 1400 (2016).
extensive series of experiments using the here described experimen- 11
W. Reimers, in Neutrons and Synchrotron Radiation in Engineering Materi-
tal instrumentation. Further improvements of the instrumentation als Science: From Fundamentals to Material and Component Characterization,
will address the possibility to gather more temperature informa- edited by W. Reimers, A. R. Pyzalla, A. Schreyer, and H. Clemens (Wiley-VCH,
tion during the process in order to evaluate in-process stresses. The Weinheim, Chichester, 2008), p. 115.
12
instrumentation is not limited to the single use of Inconel 625 as E. Uhlmann, E. Krohmer, F. Hohlstein, and W. Reimers, in Proceedings of the
28th Annual International Solid Freeform Fabrication Symposium, Austin, Texas
the powder material but allows for in situ strain analysis during the (University of Texas, 2017), p. 1472.
manufacturing of other commonly used metals and alloys. Further- 13
P. Bidare, I. Bitharas, R. M. Ward, M. M. Attallah, and A. J. Moore, Acta Mater.
more, the examination of texture evolution and phase transforma- 142, 107 (2018).
tions during the LPBF process are possible future fields of research 14
P. Bidare, R. R. J. Maier, R. J. Beck, J. D. Shephard, and A. J. Moore, Addit.
that can be considered using the presented experimental setup. Manuf. 16, 177 (2017).
15
C. Zhao, K. Fezzaa, R. W. Cunningham, H. Wen, F. de Carlo, L. Chen, A. D.
Rollett, and T. Sun, Sci. Rep. 7, 3602 (2017).
16
ACKNOWLEDGMENTS N. D. Parab, C. Zhao, R. Cunningham, L. I. Escano, K. Fezzaa, W. Everhart,
A. D. Rollett, L. Chen, and T. Sun, J. Synchrotron Radiat. 25, 1467 (2018).
This paper, which is based on the results obtained in project 17
Q. Guo, C. Zhao, L. I. Escano, Z. Young, L. Xiong, K. Fezzaa, W. Everhart,
Nos. DFG UH 100/207-1 and DFG RE 688/73-1, was supported B. Brown, T. Sun, and L. Chen, Acta Mater. 151, 169 (2018).
by the Deutsche Forschungsgemeinschaft (DFG). Furthermore, we 18
L. I. Escano, N. D. Parab, L. Xiong, Q. Guo, C. Zhao, K. Fezzaa, W. Everhart,
acknowledge Helmholtz-Zentrum Geesthacht (HZG) for the sup- T. Sun, and L. Chen, Sci. Rep. 8, 15079 (2018).
19
port and the provision of experimental facilities at PETRA III and L. I. Escano, N. D. Parab, L. Xiong, Q. Guo, C. Zhao, T. Sun, and L. Chen,
the provision of peripheral equipment. Synchrotron Radiat. News 32, 9 (2019).
20
C. Kenel, D. Grolimund, X. Li, E. Panepucci, V. A. Samson, D. F. Sanchez,
F. Marone, and C. Leinenbach, Sci. Rep. 7, 16358 (2017).
21
C. Kenel, D. Grolimund, J. L. Fife, V. A. Samson, S. van Petegem, H. van
DATA AVAILABILITY Swygenhoven, and C. Leinenbach, Scr. Mater. 114, 117 (2016).
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