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Manuscript_75f481f7be60c62f2bcc4e6f9737f5ca

Fracture Characteristics and Heat Treatment of Laser Powder Bed Fusion

Additively Manufactured GRCop-84 Copper
A. H. Seltzman*, S. J. Wukitch
Massachusetts Institute of Technology, Plasma Science and Fusion Center, 190 Albany St, Cambridge, MA, 02139
(Received dd month 2020; published dd month 2020)
Laser Powder Bed Fusion (LPBF) of Glenn Research Copper 84 (GRCop-84), a Cr2Nb (8 at. % Cr, 4 at. %
Nb) precipitation hardened alloy, produces a fully dense high conductivity alloy with a yield strength of 500
MPa and ultimate tensile strength (UTS) of 740 MPa, superior to other competing copper alloys, and 20%
elongation at fracture for material stressed perpendicular to the build direction. The high thermal stability of
the Cr2Nb precipitate in the copper matrix reduces coarsening and maintains a 300 MPa yield, 520 MPa UTS
and 26% elongation after a 900°C, 5-hour heat treatment, while a 3h 450°C heat treatment increases yield to
810 MPa, UTS to 970 MPa with 9% elongation at fracture, for samples stressed perpendicular to the build
direction. Tensile strength anisotropy based on print direction was attributed to internal stress and columnar
grain formation. Void nucleation during tensile fracture was initiated by brittle fracture of precipitate particles
within the copper matrix. Fracture cusps contain matching precipitate fragment geometry on opposing sides
located near the cusp center in at least 80% of fracture cusps. An optimal precipitate size of 100 nm is
predicted for maximum tensile strength from precipitates on fracture surfaces, while tensile testing with
varying heat treatments shows maximum strength with 100 nm and smaller precipitates. Cr2Nb precipitates
are shown to transition between polycrystalline and monocrystalline structures at high temperature.
DOI: PACS numbers:

I. Introduction
Glenn Research Copper 84 (GRCop-84) [1], a
Niobium Chromide (Cr2Nb) 8 at. % Cr, 4 at. % Nb [2]
precipitation hardened alloy, has shown suitability for
additive manufacture (AM) [3], [4], [5], [6], [7], [8] with
Laser Powder Bed Fusion (LPBF), also known as Selective
Laser Melting TM (SLM). High thermal conductivity and
poor laser coupling to Nd:YAG and fiber lasers in the 1030-
1080 nm wavelength range [9] have presented challenges in
AM of traditional copper alloys [10], such as oxygen free
copper (C10100), CuCrZr (C18150), GlidCop (C15715).
These attributes often result in poor surface quality and sub-
unity density in the bulk material that degrades thermal and
mechanical properties, requiring Hot Isostatic Pressing
(HIPing). Improved density and reduced surface roughness
in LPBF GRCop-84 were attributed to the higher absorption
of near-IR laser light at low temperatures due to the 14 vol
% Cr2Nb [6]. GRCop-84 prints at densities exceeding
>99.9% [3] with surface roughness of Ra=3-4 μm [11]; for
comparison LPBF pure copper achieves Ra=18-30 μm with
95% density [12], and CuCrZr achieves Ra=10-16 μm with
99.8% density [13]. Minimal internal voids in As Printed
GRCop-84 eliminated post-print HIPing preventing high
temperature exposure that coarsens precipitates, allowing
flexibility in heat treatment to select desired mechanical
properties. High tensile strength and a precipitate structure
stable at high temperatures, allowing use in applications
requiring high strength and high temperature tolerance, such
as rocket engine combustion chambers and fusion reactor
components.
The high temperature stability and coarsening
resistance of Cr2Nb precipitates within the copper matrix
allows GRCop-84 to achieve superior performance at high
temperatures. Oxidation resistance in air is improved an
order of magnitude over oxygen free copper (OFC) at up to
650°C by formation of a durable Nb0.6Cr0.4O2 oxide layer
[14]. LPBF GRCop-84 has a thermal conductivity of 260
W/m∙K [4] to 300 W/m∙K [5] (75%-84% of OFC),
resistivity of 2.5 µΩ∙cm [15] (140% of OFC), and typical
yield strength of 470 MPa and UTS of 710 MPa in as-printed
condition [3]. Elongation depended on print direction
ranging from 20-25% in As Printed condition. Ductility
increased after a 900°C 5h heat treatment with elongation
increasing to ~26-37%.
We propose LPBF AM of GRCop-84 for
development of high field side (HFS) lower hybrid current
drive (LHCD) multijunction RF launcher on the DIII-D
tokamak [16], where high temperature bakeouts and
electromagnetic loads during disruptions prevent the use of
OFC due to annealing. LPBF allows AM of LHCD launcher
components in configurations difficult to achieve with
conventional machining, such as tapering sections within
phase shifters, or RF tuning elements within power dividers.
In contract to stainless steel or Inconel, the high conductivity
of copper reduces RF losses and the high thermal
conductivity increases permissible first-wall heat loading.
Although the build area in most commercially available
LPBF printers is smaller than the volume of an LHCD
launcher, brazing, laser and electron beam welding have
demonstrated joining thin sheets of GRCop-84 [17] typical

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of LHCD launcher septa. Similar precipitate and grain size
to copper alloys with neutron damage resistance imply
suitability in a fusion reactor environment [18]. Surface
roughness [19] in AM GRCop-84 RF components may be
reduced to Ra<~0.3 μm for low loss at 4.6 GHz by choice of
an acceptable a mass finishing step [11].
In this paper we present studies of the fracture
surfaces of heat treated LPBF printed GRCop-84, and
analyze variations in precipitate structure and tensile
strength. Yield and UTS of LPBF printed GRCop-84 was
greater than extruded or hot isostatic pressed GRCop-84.
Precipitate coarsening saturates during high temperature
exposure, allowing GRCop-84 to maintain a substantial
fraction of its initial strength after 900°C heat treatment or
brazing. Tensile strength is optimized by selecting a suitable
heat treatment schedule. Fracture surfaces showed brittle
fracture of Cr2Nb precipitate nucleated voids during the
fracture process, an effect not previously observed in
GRCop-84. This effect is an emergent property of AM
GRCop-84: void nucleation by precipitate fracture under
tensile stress. Studies of tensile strength and fracture of
GRCop-84 manufactured by hot isostatic pressing and
extrusion from powder and showed no detectable correlation
between fracture cusp and precipitate location during
material fracture. In contrast, AM GRCop-84 showed
cleaving of precipitate crystals under tensile stress that
nucleated the voids that coalesced and resulted in material
fracture. Identification of this failure mechanism is critical
for further improvement of this material since the tensile
strength of AM GRCop-84 is substantially greater than that
of HIPed or extruded material. The distribution of ratio
between fracture cusp and precipitate diameter was used to
predict the optimum precipitate diameter for maximum
material strength and compared to precipitate sizes in heat
treated GRCop-84.
II. GRCop-84 Material Properties
GRCop-84 is a copper alloy with a sub-micron Cr2Nb
precipitate structure formed by rapid solidification of a melt
(8 at. % Cr, 4 at. % Nb, bal. copper) with chill block melt
spinning (CBMS) of ribbon or gas atomization of powder to
prevent large precipitate growth that would otherwise reach
up to 1 cm during slow cooling. The resulting precipitate
distribution confers high mechanical strength through both
the Hall-Petch mechanism by pinning grain boundary
growth at high temperature with larger precipitates and the
Orowan mechanism by providing dislocation obstacles with
small precipitates. The low solubility of the Cr2Nb
precipitate in the copper matrix results in superior high
temperature stability compared to other precipitation
hardened copper alloys. Grain and precipitate structures in
as-extruded, HIPed, and brazed material did not exhibit
significant coarsening at high temperature [20].
Consolidation of GRCop-84 powder into a fully-
2
dense material must utilize a process at either a sufficiently
low temperature to prevent coarsening of the precipitate
structure, or a process where the melt and re-solidification
time is sufficiently fast. Processes that operate below the
melting point of the copper matrix and use high pressure to
consolidate GRCop-84 powder, such as hot isostatic pressing
(HIP) from powder between 945-1010°C at 208MPa for 1-4
hours [21] or direct extrusion from powder [14] at 830-
885°C (857°C recommended) with a minimum 6:1 reduction
ratio by area. Processes utilizing re-melting must use a rapid
melt/re-solidification cycle to prevent precipitate coarsening
such as LPBF [3], Electron Beam Melting (EBM) [22], or
Vacuum Plasma Spraying.
a. Cr2Nb Precipitate Properties
GRCop-84 is similar to dispersion strengthened (DS),
precipitation hardened (PH), and metal matrix composite
(MMC) materials. Unlike traditional PH materials, Cr2Nb
primary precipitates form during rapid solidification of gas
atomized powder rather than during aging. Precipitates as
small as tens of nanometers exist like a DS material and a
large volume (~14%) of Cr2Nb exists within a copper matrix
like an MMC [23]. Cr2Nb precipitates form a C15 (cF24)
Laves phase, a close packed binary intermetallic with the
approximate formula AB2, where the A atom (Nb) is the
larger element [24]. B atoms (Cr) form layers of stacking
tetrahedra linked corner to corner while A atoms fill the
space within the B atom tetrahedra in a diamond shaped
lattice. The C-15 phase resembles a f.c.c., however the four
interpenetrating atomic layers inhibit slip dislocation
movement at ambient temperature. Cr2Nb unit cells contain
24 atoms with a lattice parameter of 6.98 Å [25] compared
to the 4 atoms per unit cell f.c.c structure of copper with a
lattice parameter of 3.6 Å [26].
Non-stoichiometric Laves phases result in antisite
substitution crystallographic defects where the more
prevalent atom replaces the less prevalent in the lattice. In
certain Laves phases, such as Cr2Nb, antisite substitutions
form for both Nb rich and Cr rich configurations; larger Nb
atom substitutes in smaller Cr atom sites [24]. An atomic
ratio of Cr:Nb=2.05:1 prevents hydrogen embrittlement [21]
due to the affinity of niobium for hydrogen in both rocket
engine and fusion reactor environments. Cr2Nb melts
between 1620°C (Cr rich) and 1650 °C (Nb rich) depending
on the ratio of Cr to Nb [27], while Cu melts at 1084°C. The
ductile-brittle transition for Laves phases occurs at 60% of
the melting temperature [24], 870 °C in Cr2Nb.
Cr2Nb precipitate remains stable within the copper
matrix over a wide temperature range with minimal
coarsening or growth at elevated temperatures. Pinned grain
boundaries in HIPed or extruded GRCop-84 inhibited further
grain growth during long duration 800°C exposure with little
reduction in tensile strength after exposure to 1000°C, unlike
most precipitation hardened alloys which were weakened
after high temperature exposure. High temperature stability
and resulting inhibition of growth of the copper grain, allows
GRCop-84 HIPed or extruded from powder to retain most of
its strength after exposure to temperatures as high as 1000°C
for an extended time, as precipitate coarsening had saturated
during the gas atomization process and was subsequently
maintained during condensation using HIPing or extrusion
processes. A simulated 1000°C braze cycle reduced the
tensile strength of extruded GRCop-84 by 75 MPa [28] due
to particle coarsening. Thermal stability of the precipitate
depends on solubility, low for both Cr and Nb in liquid
copper below 1750°C, and negligible in solid copper [36].
Low mobility in the base metal inhibits agglomeration.
Precipitates in gas atomized powder with 102 to 103 Ks-1
cooling rates have a bimodal distribution composed of
primary particles up to ~0.5 µm in diameter formed during
the initial rapid solidification process, and secondary
particles in the 24-76 nm range formed during subsequent
aging [36]. Cooling rates of 106 K/s were insufficient to
suppress Cr2Nb precipitate [2]. Heat treatment between
500°C and 700°C resulted in secondary precipitates in the 30
nm range that saturated in population after 1 h, then began to
slowly coalesce while grain size remained constant up to the
end of the 100 h test. At temperatures above 827°C, these
small precipitates began to dissolve back into the copper
matrix [36]. Cr2Nb precipitates range from 20 nm to 0.5 µm;
the molten phase of GRCop-84 contains a percentage of co-
soluble Cr and Nb that precipitates during solidification [23].
b. Precipitation Strengthening Mechanism
Cr2Nb precipitates pin grain boundaries to prevent
growth at elevated temperature and provide Orowan
dislocation obstacles [36]. GRCop-84 extruded from powder
had grain size is on the order of 1-5 µm [23],[29], with
submicron Cr2Nb precipitates with a bimodal size
distribution. Larger irregularly shaped primary precipitates
form during gas atomization within the molten copper and
were mainly located on grain boundaries, while smaller
spherical precipitates form within the solid solution as it
cools below the solvus point or during aging. The boundary
between primary and secondary precipitates in extruded
GRCop-84 is 300±100nm [29]. Aging below the solvus
temperature precipitates additional secondary particles and
generates a trimodal size distribution.
Orowan strengthening depends on precipitate size and
volume fraction and within the copper matrix.
 f 1/ 2   r 
 y  0.538Gb   ln   (1)
 2r   b 
The Ashby-Orowan equation (1) gives increase in tensile
strength, Δσy, where b is the Burgers vector in the slip
direction (0.255 nm for copper), Gb is the Burgers vector –
shear moduli product (12.3 MPa∙µm for copper), f is the
precipitate volume fraction, and r is precipitate radius [30].
3
Tensile strength increases as precipitate radius decreases,
assuming hard particles with a constant volume fraction.
This trend is bounded at low radii when bypass slip
transitions from Orowan looping to particle sheering.
Maximum strengthening occurs at a critical radius where
particle sheering transitions to Orowan looping.
Yield strength depends on grain size, described by
the Hall-Petch equation (2), where σ0=26 MPa is the Hall-
Petch constant of pure copper, ky=0.12 [MPa∙m1/2] is the
material specific strengthening coefficient of copper, and d
is the grain diameter.
 y   0  k y  d 1/2 (2)
Assuming a pure copper matrix with grain size of 2.7 µm,
the calculated grain boundary strengthening due to the Hall-
Petch mechanism was 99 MPa [29]. Yield strength of copper
continues to increase as grain size decreases down to ~20-30
nm; yield strength up to 800-900 MPa is observed in pure
copper with a 20 nm grain [31]. Grain size reduction in LPBF
GRCop-84 would further increase tensile strength.
The bimodal precipitate size distribution gives
extruded GRCop-84 its high strength and resistance to
softening at high temperatures. Larger precipitates pin grain
boundaries, maintaining Hall-Petch strengthening by
preventing growth. Pinned grain boundaries did not grow
larger than 2.6 μm when exposed to 800°C for 100 h [36].
The low solubility of Cr2Nb in copper confers high
temperature stability. Unlike other precipitation hardened
copper alloys that soften permanently when exposed to
brazing temperatures, larger Cr2Nb precipitates do not
dissolve into the copper matrix and grain boundaries
remained pinned.
Smaller precipitates dominate strengthening of
extruded GRCop-84 by producing dislocation obstacles
through the Orowan mechanism. Decreased strength was
observed when small particles coarsened with prolonged
high temperatures. Aging at 500°C for 100 h increased
strength due to precipitation of new secondary particles as
the existing ones coarsen [28]. Strengthening from particles
~1 μm in diameter is 10 times less than from small particles
and considered negligible [36]. Increasing smaller secondary
precipitates will increase tensile strength as the Orowan
mechanism dominates, however, larger primary precipitates
pin grain boundaries and prevent loss of strength during
brazing.
c. Prior Studies on LPBF printing of GRCop-84
LPBF printing of GRCop-84 was developed at NASA
Marshall Space Flight Center (MSFC), Quadrus Corp.
(formally ASRC Federal Astronautics LLC prior to May
2020) [32], and Special Aerospace Services (SAS) [3].
GRCop-84 was printed on an EOS M290 at Visser
Precision for Special Aerospace Services (SAS) [3] from gas
atomized powder produced by ATI powder metals. No stress
relief, anneal, or heat treatment was applied. Rocket engine
combustion chambers, tensile test bars, and cylindrical test
samples were produced. Unsupported cooling channels ~140
mm in length and 1 mm in diameter were sufficiently wide
for powder removal. Sagging in cooling channels was
minimized for overhanging angles greater than 45° from the
horizontal XY plane of the build plate (see Figure 4 for
coordinate system). Hexagonal bars were turned on a lathe
to create tensile test specimens with a reduced cross section.
Cylinders 2mm in diameter were printed along the Z axis and
removed from the build plate with wire EDM.
Micro Computed Tomography (μCT) scanning on a
Zeiss Xradia 520 Versa μCT with a 3.7 μm voxel size
measured voids within as printed GRCop-84 cylinders. Most
of the porosity (99%) was located at 100 μm below the
surface on a 2 mm diameter test cylinder which had 99.875%
total density. Porosity was concentrated at the overlap
between the shell perimeter scan and the infill hatch pattern.
The bulk material, excluding the surface layer, had >99.9%
density in as printed material without requiring HIPing to
achieve full density.
Light microscopy and scanning electron microscope
images of etched cross sections in the XY plane showed
Cr2Nb precipitates pushed to the boundaries of the laser melt
pools. Small grains in the copper matrix located in the melt
pool center were surrounded by long columnar grains 6 μm
in width that grew across the boundaries of adjacent melt
pools. The outer surface of LPBF printed parts consisted of
a network of 30 μm Cu grains with un-melted or partially
melted powder particles adhered to the surface. Energy-
dispersive X-ray spectroscopy indicated a composition of
8.43 at. % Cr, 4.35 at. % Nb (Cr/Nb ratio=1.94).
Tensile testing of LPBF printed samples showed a
0.2% yield strength anisotropy due to print orientation.
Samples printed parallel to the applied stress had a 392 MPa
yield strength and 710 MPa UTS with 16.6% elongation,
while samples printed perpendicular to the applied stress had
a 472 MPa yield strength and 714 MPa UTS with 15.4%
elongation [3]. No anisotropy was observed in UTS.
Fracture surfaces typical of ductile rupture on the
microscopic scale exhibited LPBF hatch patterns in tensile
bars printed parallel to the pull direction (bar length along Z
axis, see Figure 4) and build layers in tensile bars printed
perpendicular to the pull direction (bar length in XY plane).
Hatch pattern laser weld tracks in the fracture plane were cut
through by the fracture surface implying minimal separation
at the weld seams [3].
GRCop-84 LPBF printing developed at NASA
Marshall Space Flight Center in 2014 followed prior work
on wrought GRCop-84 fabrication at NASA Glenn Research
Center [5]. LPBF on a Concept Laser M2 utilized the
following settings [33]:
 Laser power: 180 W
 Laser scan speed: 600 mm/s
 Layer thickness: 30 µm
 Hatch Width: 105 µm
LPBF GRCop-84 consolidated from gas atomized
powder from different vendors had minor differences in
mechanical properties [5]. Inclusion of fine gas atomized
powder particles <10 μm in diameter while limiting the
maximum diameter to 45 μm improved elongation and
tensile strength [5]. Powder re-use by blending virgin
powder into a working stock of re-used powder that did not
have excessive oxidation resulted in a 2% reduction in UTS,
however tensile and elongation properties remained
unchanged [6]. All powder stocks mixed must meet specified
contaminant levels independently [4]. The melt for gas
atomization required elemental charges with minimum
purities of 99.99% Cu, 99.8% Cr, and 99.5% Nb; significant
quantities of oxygen can be absorbed into Nb, and Fe was
found to be a common contaminant in the Cr charge [4]. 200-
250 appm Fe contamination from the Cr charge reduced the
thermal conductivity of GRCop-84, while <50 appm was
considered acceptable [4], [15]. Powder removal from
cooling channels can be aided by Alcohol, >500 psi air or
N2, and tapered cooling channels, and inhibited by narrow
channels, or oil contamination; mallet blows for powder
removal prior to HIPing created microcracks [5]. Powder
removal from channels was verified by water flow testing or
CT scanning [5].
Anisotropy in As-Printed bars increased tensile strength
by ~10% in bars printed perpendicular to the stress direction
compared to those printed parallel to the stress direction [5].
Faster laser scan speeds increased porosity in the bulk of
LPBF GRCop-84, however this increased porosity was
reduced by HIPing [5]. Coolant channels 25.4 mm in length
have been pressure tested to 13.8 MPa with no signs of
leakage due to through porosity [5]. As-printed samples had
higher strength and lower ductility than HIPed samples,
implying compressive residual stresses [5]. Post HIP
material had similar strength to extruded GRCop-84
implying full annealing [5]. Elongation at fracture of HIPed
LPBF GRCop-84 were greater than extruded material due to
finer Cr2Nb precipitates allowing increased strain in the
copper matrix before failure [5].
HIPed LPBF GRCop-84 had a 208 MPa yield strength
and 390 MPa UTS with 30% elongation [8]. High residual
stress in as printed GRCop-84 resulted in low elongation at
fracture; a stress relieving heat treatment ductility improved
ductility but lowered tensile strength [5]. A UTS of 674 MPa
in as build condition reduced to 390 MPa after HIP treatment
[4]. Tensile strength of GRCop-84 exceeded almost all other
copper alloys in the 500-700°C range [5]. In parts requiring
HIPing, high temperature heat treatment, or brazing,
GRCop-84 exceeded the tensile strength of all other
precipitation strengthened copper alloys at all temperatures
if subsequent solution and precipitation heat treatments were
not allowed [5].
III. Additive Manufacturing of Test Samples
4
 LPBF GRCop-84 samples tested in this paper were SEM were taken at 0° or 45° angles, as shown in Figure 2 (a).
produced by Quadrus Corp. [32] (Formerly ASRC Federal A 45° angle increases secondary electron (SE) detector
Astronautics LLC prior to May 2020). LPBF production signal and enhances surface topographic features [34]. A 52°
utilized the following settings: angle was used for FIB cross-section micrographs (b,c). FIB
 Machine type: Concept Laser M2 (p/n: SL400W) images were digitally stretched on the vertical axis to
 Max build area: 250 mm by 250 mm compensate for the cross-section tilt angle. A platinum mask
 Max build height: 350 mm applied to the top surface reduces vertical line artifacts on
 Laser power: 180 W the milled cross-section due to variability in milling rate.
 Laser scan speed: 600 mm/s The FIB uses a magnetic immersion lens that
 Layer thickness: 30 µm immerses the sample in a magnetic field parallel to the
electron beam. FIB mill micrographs of Cr2Nb precipitates
 Hatch Width: 100 µm
had the best contrast between the copper and precipitate in
Components were printed under an argon atmosphere to
SE mode. Low electron beam energy results in superior
prevent oxidation. Laser scanning projected a 3 mm by 3 mm
square hatch pattern with patterns within adjacent squares resolution on fracture surfaces compared to high energy due
to reduced penetration and diffraction through the thin septa
rotated by 90 degrees. Hatches are spaced 100 μm peak to
between fracture cusps.
peak. A single hatch line is scanned around part cross section
perimeters resulting in smoother external surfaces. Printed
GRCop-84 was cleaned with compressed air and ultrasonic
cleaning in water. Heat treatments, discussed later in this
paper, were applied after cleaning.
Build plate containing LPBF poloidal RF power
dividers and phase shifters are shown in Figure 1 (a) and (b),
respectively. Chemical / chemical mechanical finishing of
power dividers are shown in (c), reducing surface roughness
for low RF loss. Waveguide segments that would have been
Figure 2. Imaging angles for SEM and FIB systems. SEM images
impossible to produce by conventional machining and
were taken at a 0° or 45° angle to vertical (a). FIB images were
difficult to produce through bending or drawing are shown taken at a 52° angle (sample surface was normal to the ion beam
in (d,e). Wide bandwidth reflectometer horn antennas are used for milling (b)). FIB cross-sections were oriented 90° to the
shown in (f). sample surface (c); a platinum (Pt) mask improves cross-section
uniformity.

V. Gas Atomized GRCop-84 Powder

LPBF AM samples were produced from gas atomized

GRCop-84 powder from ATI Powder Metals and Carpenter
Powder Products. Size distributions are shown in a
histogram Figure 3 (a) and CDF (b) of powder (c) size
produced by ATI Powder Metals [35]. ATI powder
diameters are quoted between 10 µm and 45 µm with an
average of 25 µm. Laser diffraction particle size analysis by
Ellis et.al [28] indicated gas atomized powders typically
have a log normal distribution; ATI powder had a log-normal
distribution.

Figure 1. LPBF waveguides and LHCD launcher parts on build

plate (a-f). Photos (a,b,d,e) courtesy of Quadrus Corp. [32].

IV. Electron Microscopy and Focused Ion

Beam Milling of GRCop-84

Micrographs of precipitate size and fracture surfaces

were imaged with a Zeiss Merlin scanning electron
microscope (SEM) and a FEI Helios Nanolab 600 Dual
Beam Focused Ion Beam (FIB) mill. Micrographs on the

5

Figure 3. Histogram (a) and CDF (b) of gas atomized powder from
ATI Powder Metals [35]. A mixture of powder from Carpenter
Powder Products and ATI Powder Metals is shown in (c). Cr2Nb
precipitates appear as dark areas, grain boundaries were visible as
changes in contrast in FIB sectioned 40 µm diameter (d,e) and 5 µm
(f,g) powder particles. Vertical striations were an artifact of the FIB
milling process. Imaged at 52° angle (tilt corrected), at 5 kV 86 pA.
GRCop-84 particle diameter controls cooling rate
during the gas atomization process, and thus effects
precipitate size. A crucible melt temperature of 1750°C was
required to dissolve Cr2Nb into the copper as Cr and Nb have
low solubility in liquid copper at lower temperatures
[21],[36]. During gas atomization, the molten metal solution
is aspirated from a crucible by the supersonic flow of an inert
gas (argon is used for GRCop-84 as nitrogen reacts to form
nitrides) surrounding an atomization nozzle. Contact with
the gas jet breaks up the metal film into initial ~500 µm
droplets which subsequently break up into secondary
spherical droplets between 10 and 150 µm in diameter [37].
dT 6h
 T  T0  (3)
dt  Cd
k spectrometry. GRCop-84 tensile bars were produced from
h
d
 2  0.6 Re1/2 Pr1/3  (4)
The cooling rate, assuming Newtonian cooling
conditions (rate proportional to temperature difference), is
given by (3), where ρ is the metal density, C is the specific
heat, d is the metal droplet diameter, (T-T0) is the
temperature difference between the droplet and the
surrounding gas, an h is the heat transfer coefficient given by
the Ranz-Marshall correlation (4), where Re is the Reynolds
number, Pr is the Prandtl number, and k is the thermal
conductivity of the surrounding gas. The cooling rate is
therefore inversely proportional to the square of the droplet
diameter [37].
Cr2Nb particles precipitate out of the molten copper
solution before solidification of the copper matrix [38] due
to low solubility. During the time between primary
precipitation and solidification of the copper matrix at
1084°C, precipitate agglomeration occurs, resulting in larger
precipitate diameters in larger powder particles that cooled
at a slower rate. FIB milling of powder particles through their
diameter illustrates precipitate distribution in a 40 µm Figure
3 (d,e) diameter powder particle and a 5 µm (f,g) diameter
powder particle that cooled 64 times faster exhibiting a
comparatively smaller precipitate size.
During LPBF, the rapid melting and cooling by the
scanning laser reduces precipitate size resulting in increased
strength. Precipitates are either re-melted and subsequently
re-precipitate as the melt pool rapidly cools or are broken
apart during the LPBF process [39]. As ~2/3 of the tensile
strength in GRCop-84 was from the Orowan mechanism
[28], LPBF results in a stronger material compared to HIPing
or extruding from powder, where the precipitate structure of
the powder was maintained during condensation into a solid
material. Precipitate size distributions within gas atomized
GRCop-84 powder particles therefore do not to effect
precipitate sizes within LPBF material. Refinement of
precipitate size also means that unlike HIPed or extruded
material, LPBF GRCop-84 will lose a noticeable amount of
tensile strength during stress relief heat treatment as
precipitates begin to coarsen towards saturation. This
coarsening will begin at a lower temperature then that of the
HIPed or extruded material, however as the final heat-treated
material will have a tensile strength higher than HIPed or
extruded GRCop-84, this effect should not be considered
detrimental, particularly as the heat treatment improved
ductility.
VI. Material and Powder Composition
Analysis
Composition of GRCop-84 powder and LPBF printed
material was measured with x-ray fluorescence and with X-
ray florescence (XRF) using a Fischerscope XRAY
XDAL237SDD, by inductively coupled plasma (ICP)
atomic emission spectroscopy (AES), and ICP mass
the powder working stock at Quadrus Corp. The working
stock consisted of powder not consolidated during previous
prints that was recycled and sieved following use, then
blended with new powder to maintain required volume.
Powder loaded into the printer was additionally sieved
preceding any build [40]. Previous tests in blending virgin
powder into a recycled working stock resulted in a 2%
reduction in UTS, but no difference in yield or elongation
properties [6].
Prior to 2017, Quadrus Corp. purchased powder from
Carpenter Powder Products, receiving the last batch of
Carpenter powder in February 2018; purchasing of powder
from ATI Powder Metals began after February 2017.
Material certifications for gas atomized GRCop-84
powder from ATI Powder Metals measured with ICP AES at
the time of production between February 2017 and March
2020 are shown in Table 1. In tabulated data, composition
6
 Table 1 ATI Argon Atomized Powder Composition as Delivered to Quadrus Corp.

Production 24-Feb 5-Jun 5-Jun 16-Nov 19-Mar 26-Jun 26-Jun 16-Aug 5-Mar 5-Mar 6-Mar
Date 2017 2017 2017 2018 2019 2019 2019 2019 2020 2020 2020
ATI Batch # 1112 1806 1807 5760 6576 7641 7642 8006 10216 10217 10214
ATI Heat # 522758 522810 522801 522909 522907 522896 522897 522903 523098 523099 523098
Element Units AVG STD Units
Cu at% 87.8 87.8 87.7 87.7 87.7 87.7 87.7 87.7 88.1 87.8 88.1 87.80.15 at%
Cr at% 8.2 8.2 8.2 8.1 8.2 8.2 8.2 8.2 7.9 8.1 7.9 8.10.12 at%
Nb at% 4 4 4.1 3.9 4.1 4 4 4.1 3.8 4 3.8 4.00.11 at%
Al appm 118 ND ND 118 165 472 213 142 778 142 778 325 279 appm
B appm ND ND ND ND ND ND ND ND ND ND ND appm
Ca appm 80 ND ND 80 80 79 80 80 79 80 79 80 0.5 appm
Fe appm 57 57 46 57 57 57 57 57 57 57 57 56 3.3 appm
Hf appm ND ND ND ND ND ND ND ND ND ND ND appm
Si appm 136 ND ND 113 114 113 114 114 680 318 680 265 245 appm
Y appm 36 ND ND 36 36 36 36 36 36 36 36 36 0 appm
Zr appm 35 ND ND 35 35 35 35 35 230 35 230 78 86 appm

was listed in atomic % or appm, and “ND” specifies no data measured Cr and Nb than ICP/MS. Prior studies on LPBF
for the specified element was measured. Heat numbers GRCop-84 produced with powder from different vendors
indicate powder atomized from a single crucible melt, while had minor differences in mechanical properties [5], therefore
a heat may be divided into several batches for packing and bars printed on different build plates at different times were
shipping purposes. Composition across batches was nearly expected to have comparable tensile results.
identical with a Cr:Nb ratio in slight excess of 1:1.
Table 2 Composition Analysis of Gas Atomized Powder
Composition analysis by NSL analytical using ICP mass
and LPBF GRCop-84 Tensile Bars
spectrometry (MS) of the Quadrus Corp. powder working
stock sampled in Feb. 2019, new ATI powder sampled in Sample ATI/Carp ATI LPBF LPBF LPBF LPBF LPBF LPBF
March 2020, and LPBF tensile bars printed in Oct 2018, Oct Powder Powder GRCop84 GRCop84 GRCop84 GRCop84 GRCop84 GRCop84
2019 and Dec 2020 are shown in Table 2. Composition of Method ICP/MS ICP/MS ICP/MS ICP/MS ICP/MS XRF XRF XRF
LPBF tensile bars printed in Oct 2018, Oct 2019 and Dec Date 2019 2020 2018 2019 2020 2018 2019 2020
2020 were analyzed by XRF at MIT for comparison, Element Feb March Oct Oct Dec Oct Oct Dec
showing similar composition results. Units
Cu at% 88.3 88.83 87.9 88.0 88.6 87.54 87.44 87.65
Purity of powders and tensile bars increased between
Cr at% 7.69 7.44 7.84 8.13 7.51 8.43 8.43 8.36
Oct 2018 and Dec 2020 implying improved purity of gas Nb at% 4.0 3.7 4.06 3.85 3.89 4.03 4.13 3.99
atomized powder produced by of ATI Powder Metals Al appm 330 90 500 120 70 ND ND ND
compared to the powder produced from Carpenter Powder B appm <60 <10 <60 <60 <60 ND ND ND
Products. In powders from both suppliers, Aluminum and Ca appm <80 <10 80 <80 <80 ND ND ND
Silicon were common impurities. Increased iron impurities Fe appm 50 20 110 20 <50 ND ND ND
(110 appm Fe) in bars produced in 2018 would decrease Hf appm <10 <10 <10 <10 <10 ND ND ND
thermal conductivity compared to bars produced in 2020 Si appm 250 110 950 160 <110 ND ND ND
Y appm <10 <10 <10 <10 <10 ND ND ND
(<50 appm Fe), however this finding was incidental and
Zr appm <10 <10 <10 <10 <10 ND ND ND
would only effect thermal conductivity, which was not
examined in this paper. ATI powder had 20 appm Fe, and
<10 appm B. Low Fe content yields high thermal and
electrical conductivity, while low B impurities results in low VII. Grain and Laser Hatch Pattern in LPBF
swelling in a nuclear environment, important characteristics Material
for use in a fusion reactor. Oxygen content of powder stock
measured by ATI with inert gas fusion was 0.067% by mass Tensile bars shown in Figure 4 were produced
at time of manufacture. including a “parallel printed” bar printed along the long axis
Tensile bars labeled Perp1,2 and Para1,2 that (a), and a “perpendicular printed” bar printed along the one
receiving the 900°C 5h heat treatment were built with the of the short axis (b). A cross-section of the interior (d) was
working powder stock in October 2018, all other tensile bars removed from each type of bar. The top surface of each bar
in this paper were built with the working powder stock exhibits a laser hatch pattern from the LPBF process visible
during October 2019, September 2020, and December 2020. on the perpendicular printed bar (d,e).
XRF of GRCop-84 bars demonstrated good batch to batch Etched cross-sections of sample bars show
uniformity of composition, though XRF resulted in higher characteristic patterns of the laser hatch. Samples were

7
etched until melt pools were visible with a 1:1 mixture of
30% NH4OH, 3% H2O2 following a 3 μm diamond polish.
VIII.
Figure 4. Sample LPBF printed GRCop-84 bars. Bar (a) was
printed along its length (z axis during print left to right in lower
picture), bar (b) was printed along its width (z axis during print out
of page in lower picture). Bars were cut across their width ~3 mm
from the end (c) to produce an internal sample (d). The laser hatch
pattern was visible on the top surface of a printed part (b). Bar
dimensions are 89mm x 12.7mm x 9.5mm.
The internal melt pool structure in LPBF printed
GRCop-84 corresponding to the laser hatch pattern and build
direction indicates that the laser scanning affects the internal
structure of LPBF produced material. Prior studies of LPBF
printed GRCop-84 fracture surfaces by Hayes et al. [3] show
that the fracture cuts through most of the laser weld tracks
implying that failure of the material does not occur by
separation at the weld seams, however the hatch pattern
remained visible on the fracture surfaces.
Cross sections in the XY plane of the print, shown in
Figure 5 (a,d), exhibited the characteristic hatch pattern of
the laser melt pools matching the laser hatch observed on the
top surface of LPBF printed material (c). Hatches in (a,d)
have 100 μm width and are shown to overlap. A single hatch
scanned around the perimeter of the consolidated cross
section was evident on the left and top of (d). Cross sections
with the z-axis lying vertically within the cross section plane,
shown in (b,e), show lines along the print direction
corresponding to the cross-section of the layers of hatches.
The cross section of the scanned perimeter hatch was visible
on the left of (e). LPBF GRCop-84 exhibits evidence of
internal structure due to the AM process in both cross
sections, an effect also visible on the fracture surfaces
discussed later in this paper.
8
Figure 5. Etched cross-section surface of GRCop-84 bars with print
direction into / out of the page (a) and print direction upward along
the page (b). SEM micrograph of top surface of print showing laser
hatch pattern (c). Magnified micrographs of etched cross sections
printed into / out of the page (d) and upward along the page (e)
Cr2Nb Precipitate Structure in LPBF
Material
Variation in precipitate size distributions with heat
treatment determine the mechanical properties of AM
GRCop-84. Distributions were measured in FIB sections
shown in Figure 7 and plotted in Figure 6 from the equivalent
area of a spherical particle cross section contained within the
precipitate outline. The equivalent diameter of a precipitate
is calculated from the area, A, of the precipitate in the image
(5).
Dcirc  2  A /  
1/ 2
(5)
The LPBF process reduces precipitate sizes in as-
printed material as shown in Figure 7 (a) compared to the gas
atomized powder shown in Figure 3 (d,e) which extend up to
1 µm in diameter. The largest precipitates in as-printed LPBF
printed material remain under 200 nm. The reduction in
precipitate size implies that larger agglomerations in the gas-
atomized powder were either dissolved into the melt pool
and re-precipitate during rapid solidification or broken apart
during the LPBF process. Precipitate diameter distribution in
as-printed material had a single peak at ~85 nm with most
precipitates remaining below 150 nm in diameter.
Occasional precipitates up to ~200 nm are observed due to
precipitate boundaries touching, though these are not
considered true agglomerations and the two precipitates
retain a geometrically distance dumb-bell shape. Larger
precipitates do not agglomerate due to the rapid cooling of
the laser melt pool, while this same rapid cooling rate inhibits
precipitation of smaller particles from solution. No
precipitates below 35 nm in diameter are observed.
Table 3 Heat Treatment Schedules for GRCop-84
(b) 450°C 3h Heat Treatment Schedule
Time (hh:mm) 0:00 0:10 0:20 0:30 0:40 1:25 1:45 1:55 2:15 2:25 4:25 4:55
Temp. (°C) 30 100 100 200 200 450 450 450 450 450 450 20
(c) 600°C 20min and 450°C 2h20min Heat Treatment Schedule
Time (hh:mm) 0:00 0:10 0:20 0:30 0:40 1:25 1:45 1:55 2:15 2:25 4:25 4:55
Temp. (°C) 30 100 100 200 200 450 450 600 600 450 450 20

(d) 880°C 20min Cusil-ABA Braze Schedule

Time (hh:mm) 0:00 0:10 0:20 0:25 0:55 1:55 2:25 2:40 3:00 3:15 3:45 4:45
Temp. (°C) 30 100 100 200 200 760 760 880 880 700 700 20
(e) 900°C 5h Vacuum Furnace Anneal Schedule
Time (hh:mm) 0:00 0:10 0:20 0:25 0:35 1:55 6:15 6:30 6:30 6:30 6:30 6:30
Temp. (°C) 30 100 100 200 200 900 900 30 30 30 30 30

Heat treatment temperature and duration controlled

precipitate size distribution, and therefore tensile properties
in LPBF GRCop-84. Heat treatment may cause coarsening
or agglomeration of existing precipitates, or additional
precipitation from solid solution. Heat treatments applied in
this paper were done within a vacuum furnace, except for the
“Perp 1,2,6” and “Para 1-10” tensile bars that received a
900°C 5h heat treatment at atmospheric pressure under an
inert argon at Quadrus Corp. Furnace temperature control
had positive temperature control authority (heating) only;
free cooling time to the water-cooled shell temperature Figure 6. Density plot of GRCop-84 precipitate sizes in as-printed
exceeded the decreasing temperature ramp at the end of (a), heat treated 450°C for 3h (b), heat treated at 600°C for 20min
followed by 450°C for 2h and 20min (peak value of 163 on plot cut
programed temperature cycles, particularly at low
off for clarity, located at 15 nm) (c), heat treated for the schedule in
temperatures. (c) followed by a CUSIL-ABA braze cycle (d), and heat treated at
A 450°C 3h heat treatment cycle as per the schedule 900°C for 5h (3) illustrating changes in precipitate size. Boxplot
shown in Table 3 (b), resulted in a bimodal distribution of (top) indicates statistical distribution of precipitate sizes. Whiskers
precipitates. The 85 nm diameter peak present in the as- extend at most up to q3+1.5×(q3 – q1) or down to q1–1.5×(q3 – q1),
printed GRCop-85 remains along with the formation of an where qn is the nth quartile. Particle sizes outside whiskers are
additional peak at 40 nm. Minimal formation of precipitates marked as outliers “+”. Mean “○” of precipitate size include
in the 5-35nm range was observed. No observable outliers. Notch indicates 95% CI of median. Data (a-d) from 25kX
coarsening of existing precipitates occurs, however, the images in Figure 7 center column, data (e) from 8kX image data
precipitate edge morphology changes, as shown in Figure 7 (not shown). Data (e) normalized to equivalent image area in (a-d)
to compensate for difference in magnification.
(b). Precipitates become elongated and exhibit rougher edges
that in as-printed GRCop-84. This bimodal distribution had
Application of a simulated Cusil-ABA braze
been observed in extruded/HIPed GRCop-84 [29] composed
schedule peaking at 880°C for 20min, as given in Table 3
of primary particles formed during the initial rapid
(d), to LPBF GRCop-84 previously heat treated with the
solidification process, and secondary particles in the 24-76
schedule given in Table 3 (c), resulted in elimination of the
nm range formed during subsequent aging [36].
population of 5-30 nm range precipitates, indicating either
A 600°C 20min heat treatment followed by a 450°C
coarsening and agglomeration, or re-dissolution back into
2h 20min heat treatment as per the schedule shown in Table
the copper matrix [36], shown in Figure 7 (d). Distribution of
3 (c), resulted in formation of a large population of secondary
precipitates greater than 60 nm in diameter is equivalent to
precipitates in the 5-30 nm range, increase in precipitates in
that in the annealed and heat-treated material prior to the
the 40nm range, and decrease in precipitates in the 85 nm
braze cycle with minimal coarsening of precipitates.
range, as shown in Figure 7 (c). The sharp decrease in 85 nm
Morphological differences in precipitate structures are
precipitates occurs due to agglomeration of existing primary
observed with post braze cycle precipitates spherical in
precipitates in the as-printed GRCop-84, while new
shape with smooth edges.
precipitates form from dissolved Cr2Nb within the copper
A 900°C, 5-hour heat treatment of the as-printed
matrix [36]. The formation of large precipitates with a 600°C
material illustrates coarsening of the precipitates at high
20min heat treatment implies that agglomeration and
temperature, as shown in Figure 7 (e). Absence of small
coarsening from precipitate sizes in the As Printed condition
precipitates in the sub 30nm range indicates either
occur rapidly with even brief high temperature exposures.
coarsening and agglomeration, or re-dissolution of small
precipitates into the copper matrix. The number of

9
precipitates between 5nm and 150nm are substantially but will coarsen precipitate structure in LPBF copper in As-
reduced due to agglomeration into fewer larger precipitates. Printed condition due to the refined precipitate size. As
A few small precipitates are observed and are attributed to approximately two thirds of the tensile strength in GRCop-
precipitation during the cool down ramp of the heat 84 was based on precipitate size through the Orowan
treatment furnace. Morphological differences in precipitate mechanism, brazing, or other high temperature exposure of
structures are observed with precipitates condensing into a LPBF will result in a decrease in tensile strength.
spherical shape with smooth edges. In contrast to HIPed or direct extruded GRCop-84
Heat treatment schedules control the precipitate where tensile strength was minimally changed after exposure
distribution in LPBF printed GRCop-84. In as-printed to high temperatures up to 935°C, LPBF produced material
material, the distribution has a single peak at 85 nm diameter. exhibits rapid coarsening of pre-existing precipitates at
Heat treatment at 450°C for 3h creates a secondary peak at temperatures as low as 600°C and possibly lower, though not
40 nm in diameter with no agglomeration of existing at or below 450°C. This should not be taken as a detriment
precipitates. Application of a brief 600°C 20min heat of LPBF GRCop-84; even with precipitates fully coarsened
treatment at the beginning of the 450°C heat treatment cycle to a saturated value by a 900°C 5h heat treatment, tensile
produced noticeable coarsening and agglomeration of pre- strength of LPBF material exceeded that of HIPed or
existing precipitates and formation of new precipitates in the extruded (228 MPa yield, 414 MPa UTS) material. LPBF
5-30nm range. The absence of large precipitates after the GRCop-84 previously exposed to a 900°C 5h heat treatment
450°C 3h heat treatment, but presence of large precipitates to relieve stress and improve ductility was not expected to
when a 600°C 20min exposure was added showed that As exhibit major changes in tensile strength after a brazing cycle
Printed material was susceptible to agglomeration and as precipitate structure would have been coarsened during
coarsening at lower temperatures than HIPed or extruded the first high temperature exposure. These attributes of
GRCop-84, and that this effect occurred rapidly. This LPBF GRCop-84 should be considered when evaluating the
agglomeration at 600°C, as well as during 880°C and 900°C high temperature response. Tensile strength changes
cycles, contrasts with observations during high temperature resulting from heat treatments are discussed in a later
exposure of GRCop-84 produced by HIPing or direct section.
extrusion from powder [20], where negligible reduction in
yield and UTS occurred after a simulated braze cycle (935°C
for 22.5min, followed by a ramp from 935°C to 871°C for
38min), implying minimal changes in precipitate structure.
This difference was attributed to the prior high temperature
exposure of GRCop-84 produced by HIPing (945-1010°C at
208MPa for 1-4 hours [21]) or direct extrusion from powder
(830-885°C [14]) which would result in an agglomerated
precipitate structure in the as-HIPed or as-extruded material
prior to the brazing cycle.
In GRCop-84 produced by HIPing or extrusion
from powder, the precipitate structure of the powder was
maintained during condensation into a solid material, while
in LPBF material, precipitate size was refined during the
LPBF process [5]. This refined precipitate size was shown to
have average diameters of μ=95 nm in As Printed material,
which coarsened to μ=128 nm after a 900°C 5h heat
treatment, at which point coarsening was considered
saturated, however, precipitate diameters are still smaller
than those in gas atomized powder which range between
200-600 nm [39]. As the precipitate size in gas atomized
powder was larger than that of LPBF GRCop-84 that
received a 900°C 5h heat treatment, it was also considered to
have saturated precipitate coarsening, and hence HIPed or
extruded material which maintain precipitate sizes during
material condensation also have saturated coarsening. Any
small precipitates within gas atomized powder likely also
coarsen during the high temperature exposure during HIPing
(945-1010°C [21]) or extrusion (830-885°C [14]), therefore
subsequent high temperature exposure during a braze cycle
will not significantly coarsen HIPed or extruded GRCop-84,

10
Figure 7. FIB milled cross sections of GRCop-84 in as-printed (a), heat treated at 450°C for 3h (b), heat treated at 600°C for 20min
followed by 450°C for 2h and 20min (c), heat treated at 600°C for 20min followed by 450°C for 2h and 20min followed by a CUSIL-
ABA braze cycle (d), and heat treated at 900°C for 5h (e), illustrating coarsening of precipitates. Precipitates in images with a 2μm scale
bars (center column, precipitates highlighted in red on left half of image) are used to generate histograms of precipitate size. In the center
column of images precipitates on the left half of the column are marked in red, however all precipitates are used for histogram generation.

11

IX. Tensile Strength Testing and Heat
Treatment
a. Tensile Test Setup
Tensile strength anisotropy based on print direction
was observed in GRCop-84. Rectangular “parallel printed”
(long axis of the bar aligned with the Z axis build direction)
and “perpendicular printed” (long axis of the bar in the XY
plane perpendicular the build direction) bars, shown in
Figure 4 (a) and (b) respectively, were machined per ASTM
E8/E8M – 16a sect. 6.14 [41], for powder metallurgy
specimens. LPBF printed bars were machined to the nominal
dimensions listed in Figure 8. Thickness variation in the
reduced cross-section does not exceed 25 μm between ends
with a nominal thickness of 9.53 mm by 6.35 mm.
Dimensions may vary due to machining tolerances, this was
compensated for in measurement of the bar cross-section
prior to the pull test.
Figure 8. Nominal dimensions (mm [in]) of GRCop-84 tensile
stress test specimens.
Figure 9. Tensile stress test specimens (a) were machined from
LPBF printed bars. Stress was applied with a hydraulic pull tester
(b) while strain was measured with an extensometer affixed to the
center of the broad side of the test bar (c).
Tensile test samples, shown in Figure 9 (a), were
gripped by serrated fixtures (b) in an Instron 850I hydraulic
testing system at room temperature; a MTS model 632.13C-
12
20 extensometer was mounted to the side of the tensile bars
to measure engineering strain. Crosshead rate was constant
at 2.12x10-2 mm/s (0.05 inches/min). Elongation and
reduction in cross-section were measured with calipers on
fractured bars. Yield strength, UTS, and elastic modulus
were calculated from engineering stress and do not
compensate for reduction in cross-section. Within this paper
the terms “stress” and “strain” denoted measurements of
engineering stress and engineering strain.
b. Tensile Strength of LPBF GRCop-84
Tensile properties of GRCop-84 varied with
application of heat treatment which altered precipitate size
distribution contributing to tensile strength through the
Orowan mechanism and print orientation which controlled
columnar grain orientation and internal stress. Tensile
strength was increased by heat treatment at 450°C at the
expense of ductility, and decreased with heat treatment at
900°C with improved ductility. Tensile strength anisotropy
was observed based on print direction; samples printed
parallel to the applied stress had higher tensile strength than
bars printed perpendicular to the applied stress. Samples
denoted as “parallel printed”, “Para<n>” are built with with
the long axis of the bar aligned with the Z axis build direction
Figure 4 (a), while bars denoted as “perpendicular printed”,
“Perp<n>” are built with the long axis in the XY plane
perpendicular to the build direction Figure 4 (b). Tensile tests
of GRCop-84 printed parallel to the applied stress in As-
Printed condition are shown in Table 5 while samples
subjected to a 900°C 5h heat treatment are shown in Table 4.
Stress-strain curves for parallel printed bars are plotted in
Figure 10. Calculation of 0.2% yield strength utilized the
offset line fitted between 10 and 150 MPa. Bars printed
parallel to the stress direction (a-c) had an average 257 MPa
0.2% yield strength and 462 MPa UTS with 34% elongation
after a 900°C 5h heat treatment, bars in ad printed condition
(d) had a 350 MPa 0.2% yield strength and 717 MPa UTS
with 25% elongation. Heat treatment was shown to improve
ductility in exchange for reduced tensile strength.
Samples were analyzed from two separate batches of
printed tensile bars; the first batch (a), printed in 2018 (see
composition analysis section), and the second batch (b,c)
were printed separately in 2020. Measurements (b) utilized a
cyrogenic type extensometer with suspected incorrect
calibration resulting in scaling of measured strain; values for
0.2% yield strength and elastic modulus (marked in red) are
assumed incorrect and removed from average and standard
deviation (STD) calculations, all other values for (b) bars are
unaffected. Measurements (c) utilized the MTS
extensometer and are comparable to the results in (a). Tensile
strengths are similar between bars with slight variation
between batches. Bars printed in 2018 perpendicular the
stress direction (d) had a 300 MPA 0.2% yield strength and
a 519 MPA UTS, as shown in Table 7 (e); these bars were
printed in the same batch as Table 4 (a). Printing
perpendicular to the stress direction increased yield strength
and UTS. LPBF GRCop-84 produced by Hayes et al. [3] and 600
Gradl et al. [5] demonstrated a similar anisotropy in strength
with samples printed perpendicular to the stress direction, 500
shown in Table 6 (e,f) having increased yield strength over
400
samples printed parallel to the stress direction (b,c).
Comparisons to GRCop-84 extruded from powder in as- 300
extruded condition (j), and HIPed after LPBF printing (g) are
listed for comparison. LPBF+HIPed GRCop-84 has 210 200 (a) Para[1,2] 900C 5h
MPa yield strength, 390 MPa UTS, 112 GPa elastic modulus, (b) Para[3-6] 900C 5h
30% elongation, and 28.9% reduction in area [42], a 100 (c) Para[7-10] 900C 5h
reduction in tensile strength from As Printed condition, but (d) Para[1-6] AP
an increase in ductility, similar to GRCop-84 that received a 0
0 0.5 1 1.5 2
stress relieving heat treatment.
Strain [%]
Figure 10. GRCop-84 stress strain curves for parallel printed
Table 4 Tensile Test Data for LPBF GRCop-84 Heat (a,b,c), samples after a 900°C 5h heat treatment and in As-Printed
Treated at 900°C for 5 hours condition (d).

Sample Print Extens 0.20% UTS Elong Red. Elastic

Date Type Yield ation in Area Mod.
[MPa] [MPa] % % [GPa]
(a) Para1 2018 MTS 268.7 498.3 34.13 38.97 102.0
(a) Para2 2018 MTS 277.4 478.5 33.33 41.51 113.1
(b) Para3 2020 Cryo 230.6 455.7 33.50 52.06 61.9
(b) Para4 2020 Cryo 227.9 460.4 33.00 45.61 64.8
(b) Para5 2020 Cryo 230.3 460.0 36.44 53.32 60.2
(b) Para6 2020 Cryo 233.4 446.5 36.20 54.86 66.2
(c) Para7 2020 MTS 245.9 454.6 31.74 39.87 109.8
(c) Para8 2020 MTS 248.9 458.3 29.65 47.34 118.2 Figure 11. GRCop-84 powder was melted (a) onto the top surface
(c) Para9 2020 MTS 256.9 454.2 36.60 48.16 109.6 of solid underlying layers in small overlapping melt pools (b). The
(c) Para10 2020 MTS 247.7 458.5 38.10 47.93 116.0 rapid cooling of each melt pool (light blue), induces internal stress
AVG 257.6 462.5 34.27 46.96 111.5 (red) that is isotropic within the plane normal to the build direction
STD 12.87 14.95 2.57 5.55 5.72 (b), but anisotropic in the build direction. This anisotropy was
caused the underlying material restraining the horizontal
(d) Perp1 2018 MTS 293.0 518.4 26.13 27.63 122.1
contraction of the top melt pool during cooling while contraction
(d) Perp2 2018 MTS 288.6 520.9 25.07 25.18 124.5
was unrestricted in the vertical direction (c). This internal stress
(d) Perp3 2020 MTS 258.5 465.5 37.62 43.75 136.8
anisotropy results in a lower yield strength when oriented
(d) Perp4 2020 MTS 263.3 428.4 36.50 47.70 159.2
perpendicular to the external tensile force (d) than when external
AVG 275.8 483.3 31.33 36.07 135.6
force was applies within the plane normal to the build direction (e).
STD 17.48 44.61 6.65 11.31 16.97
290.80 519.62 25.60 26.41 123.29
Anisotropy in yield strength was attributed to a
combination of internal stress [43] [44] produced by rapid
Table 5 Tensile Test Data for Parallel Printed LPBF solidification of the laser melt pools, and columnar grain
GRCop-84 in As-Printed Condition growth. During the formation of each layer in LPBF, a thin
layer of powder, Figure 11 (a), was melted into overlapping
Sample Print Heat 0.20% UTS Elong Red. Elastic
pools arranged in a laser hatch pattern (b) and fused into an
Date Treat Yield ation in Area Mod.
underlying solid surface (c). During the rapid solidification
Type [MPa] [MPa] % % [GPa]
and cooling of the melt pools, the thermal contraction results
(d) Para1 2020 As print 345.6 722.7 26.48 27.23 122.0
in each pool contracting relative to the underlying material
(d) Para2 2020 As print 357.6 716.1 22.51 27.32 119.5
(b,c) which constrains the cooling melt pool in the horizontal
(d) Para3 2020 As print ND 709.8 22.41 29.37 141.2
direction, but not the vertical direction. This process results
(d) Para4 2020 As print 364.5 716.6 31.84 27.71 117.7
in anisotropic stress concentrated in the plane normal to the
(d) Para5 2020 As print 342.0 714.9 23.45 27.58 116.4
build direction (d,e). Internal stresses were minimized
(d) Para6 2020 As print 340.1 721.2 25.21 26.99 117.2
parallel to the build direction as each subsequent vertical
AVG 350.0 716.9 25.32 27.70 122.3
layer was free to contract in the vertical direction as it cools
STD 10.6 4.6 3.57 0.86 9.5
(c), while restrained in the horizontal direction by the
underlying material. This anisotropic stress concentration
within the LPBF printed material acts to stiffen the tensile

13
bar when external tensile stress was applied perpendicular to 700
the build direction Figure 11 (e), resulting in an increase in
yield strength. This effect persists after a 900°C 5h heat
treatment implying the LPBF material retains internal 600
anisotropy after annealing.
Etching of fracture surface cross-sections [3] show
that the fracture cuts through melt pools of the laser hatch 500
implying the bulk material does not fracture due to weld
delamination, UTS was slightly enhanced by printing

Stress [MPa]
perpendicular to the applied tensile stress and fracture along 400
some weld seams was observed. A possible explanation of
this effect was that a small number of welds delaminate
while the majority were sheared by the fracture. Hatch 300
patterns in the stress direction are up to the length of the 3
(a) Para1 AP
mm square pattern for perpendicular printed samples, while (b) Para(Hayes V2) AP
layers in the stress direction are 30 μm thick in parallel 200 (c) Para (Gradl DB-12) AP
printed samples. This effect implies that the additive effects (d) Perp2 AP
(e) Perp (Hayes H4) AP
of numerous abutting laser hatches increases the statistical (f) Perp (Gradl DB-06) AP
probability that a weld will delaminate at the seam. 100 (g) Gradl (DB-10) LPBF-HIPed
Columnar grain growth within an LBFF printed (h) Para7 900C 5h
material contributes to tensile strength anisotropy. Slip is (i) Perp3 900C 5h
(j) Ellis Extruded
impeded across grain boundaries and grain shape generates 0
anisotropy when a fiber texture is oriented on long axis of a 0 1 2 3 4 5
columnar grain structure [45]. Columnar grain growth is Strain [%]
driven by thermal gradients in the LPBF process as heat from Figure 12. GRCop-84 stress vs strain curves comparison between
the melt pool is drawn into the underlying substrate resulting measurements in this paper and prior measurements by Hayes et al
[3] and Gradl et al [5] for parallel printed (a,b,c), and perpendicular
in columnar grains oriented in the build direction [46].
printed (d,e,f) samples in As Printed condition, and after a 900°C
Columnar grain growth across hatch boundaries was 5h heat treatment (h,i) or HIP process (g). Extruded (j) GRCop-84
observed by Hayes et.al [3] with small even grains in the [28], measured by Ellis et al shown for comparison.
center of laser hatches and greater precipitate density at hatch
perimeters. Small even grains in cross sections by Hayes is Table 6 LPBF GRCop-84 Tensile Test Data Compared to
attributed to a transverse cut through a columnar grain in the Previous Publications
vertical direction, while columnar grain growth across hatch
boundaries is attributed to transverse thermal gradients at Sample
Heat 0.2% UTS Elong Red. Elastic
hatch boundaries as heat is transferred into adjacent hatches Treat Yield ation in Area Mod.
transverse to the build direction. This columnar grain Type [MPa] [MPa] % % [GPa]
structure likely contributes to the strength anisotropy (a) Para[1-6] As Print 350.0 716.9 25.3 27.7 122.3
resulting in lower tensile strength in bars stressed parallel to (b) Hayes Para As Print 391.6 710.2 15.4 22.0 121.8
the build direction. (c) Gradl Para As Print ND 674.0 ND ND ND
LBPF GRCop-84 printed by Quadrus Corp. and (d) Perp[1-2] As Print 492.0 742.4 19.6 15.6 150.4
specimens produced for Hayes et al [3] at Visser Precision (e) Hayes Perp As Print 471.6 714.3 16.6 22.0 119.5
and Gradl et al [5] at NASA MSFC showed similar stress strain (f) Gradl Perp As Print ND 709.0 ND ND ND
curves and tensile properties as shown in Table 6 and Figure (g) Gradl LPBF HIPed 208.0 390.0 30.0 ND ND
12 for a given print orientation and heat treatment (a-c) and
(h) Para[1-10] 900C 5h 257.6 462.5 34.3 47.0 111.5
(d-f). Stress strain curves nearly overlay for LPBF GRCop-
(i) Perp[1-2] 900C 5h 290.8 519.6 25.6 26.4 123.3
84 printed from different powder stock on different machines
implying the exact composition of the powder stock and (j) Ellis Ext Extruded 227.5 413.7 22.0 41.0 ND
machine choice only modestly effects tensile strength.
Strength anisotropy was observed from all three c. Tensile Strength of Heat Treated LPBF
manufacturers; perpendicular printed bars had improved GRCop-84
yield and UTS compared to parallel bars. Heat treatment at
900C for 5h, HIPing, and extrusion from powder resulted in Heat treatment of LPBF GRCop-84 alters
lower yield and UTS, but improved ductility (g-j). precipitate size distribution through precipitation or

14
agglomeration, as shown in Figure 7 and plotted in Figure 6, strength and ductility may be selected with choice of heat
that determine tensile properties of the material. Tensile treatment.
properties of samples printed perpendicular to the stress 900
direction subjected to different heat treatment schedules are
tested, shown in Table 7 and plotted in Figure 13. Heat 800
treatment schedules are listed in Table 3. Calculation of
0.2% yield strength utilized the offset line fitted between 10 700
and 250 MPa (except (e,f) fitted from 10-150 MPa due to
lower yield strength and (g), fitted from 100-150 MPa due to 600
low end extensometer noise). Bars in As Printed condition
without heat treatment (a) are comparable to similar bars
500
tested by Hayes et al (h) even though a different laser hatch
pattern was used. Maximum strength for the heat treatment
400
schedules tested occurred for 450°C 3h (b). 0.2% yield and
modulus values for bars 1 and 2 (marked in red in Table 7)
were measured with the cryogenic extensometer and are 300
assumed inaccurate, bars 3 and 4 are plotted in Figure 13.
Even short durations at high temperatures such as 20 min at 200 (a) Perp[1,2] As Printed
(b) Perp[3,4] 450C 3h
600°C at the beginning of a 450°C heat treatment reduced (c) Perp[1,2] 600C 20min, 450C 2h20min
tensile strength, and corresponding agglomeration was seen 100 (d) Perp[1,2] Cusil-ABA
(f) Perp[3,4] 900C 5h
in Figure 7 (c). Although a large population of fine (h) Hayes Perp (H4) As Printed
precipitates forms during a 600°C heat treatment as plotted 0
in Figure 6, the strength was still less that observed for the 0 0.5 1 1.5
450°C 3h heat treatment that did not produce observable fine Strain [%]
precipitates, though precipitates smaller then observable in Figure 13. GRCop-84 engineering stress vs engineering strain
curves for perpendicular printed GRCop-84 samples with different
the FIB cross sections may have been generated. The
heat-treatment schedules.
formation of additional fine precipitates in the 5-30 nm range
therefore does not guarantee an increase in tensile strength if Table 7 Tensile Test Data for Perpendicular Printed
larger precipitates in the 100 nm range agglomerate during LPBF GRCop-84 with Different Heat Treatments
heat treatment. Heat treatment of a simulated Cusil-ABA
Sample Print Heat 0.20% UTS Elong Red. Elastic
braze (d) and 900°C 5h (e,f), generate precipitate
Date Treat Yield ation in Area Mod.
agglomeration and corresponding reduction in tensile Type [MPa] [MPa] % % [GPa]
strength. Samples Perp[1,2], shown in Table 7 (e), printed in (a) Perp1 2019 As print 497.7 741.8 23.33 16.88 145.8
2018, and Perp6 (g) printed in 2020, were heat treated in (a) Perp2 2019 As print 486.3 743.0 15.87 14.24 155.0
atmospheric pressure argon, while Perp[3,4] (f) printed in (b) Perp1 2019 450C 742.1 973.9 7.75 4.24 109.9
2020 was heat treated in a vacuum. Difference in tensile (b) Perp2 2019 450C 767.7 964.3 8.95 8.10 99.3
properties may be attributed in part to different composition (b) Perp3 2020 450C 814.0 970.9 10.27 9.17 113.0
between batches, as listed in Table 2, as a ~30MPa reduction (b) Perp4 2020 450C 814.5 969.4 9.20 10.81 102.2
in yield and UTS was observed in parallel bars printed in (c) Perp1 2019 600/450C 561.0 780.1 16.53 16.51 148.0
2018 vs 2020, see Table 4 (a) vs (b,c). Negligible difference (c) Perp2 2019 600/450C 559.2 781.0 14.67 14.68 135.8
in UTS was observed between bars printed in 2019 and 2020, (d) Perp1 2019 ABA/880C 334.4 553.7 26.67 30.73 135.1
as shown in Table 7 (b). Modest tensile differences in bars (d) Perp2 2019 ABA/880C 338.2 554.3 25.33 34.70 169.2
heat treated under vacuum, Table 7 (f), vs in argon (g) imply (e) Perp1 2018 900C 293.0 518.4 26.13 27.63 122.1
potential contribution of precipitation differences during (e) Perp2 2018 900C 288.6 520.9 25.07 25.18 124.5
(f) Perp3 2020 900C 258.5 465.5 37.62 43.75 136.8
furnace cool down at different rates.
(f) Perp4 2020 900C 263.3 428.4 36.50 47.70 159.2
Heat treatment at 450°C increased tensile strength
(g) Perp6 2020 900C 287.1 489.5 32.86 38.73 108.0
but decrease ductility, while a 900°C 5h heat treatment
(h) Hayes Perp NA As Print 472 714 16.6 22.0 120
reduced tensile strength but improved ductility. GRCop-84
had typical elongation values ranging from between 20% for
perpendicular printed to 25% for parallel printed directions LPBF GRCop-84 is thus more sensitive to loss of
in As Printed condition. Elongation increased to ~26-37% peak strength capability at lower temperatures than HIPed or
for perpendicular printed and 34% for parallel printed extruded GRCop-84. This effect exists due to the inherent
direction after a 900°C 5h heat treatment. A balance of initial fine precipitate structure present in the material which

15
subsequently agglomerates. The agglomeration of printed specimens the characteristic fracture pattern exhibits
precipitates saturates and tensile strength of LPBF GRCop- striations parallel and perpendicular to the print direction (b).
84 exceeds that of HIPed or extruded GRCop-84 even after
a 900°C 5h heat treatment. Should absolute maximum tensile
strength of LPBF GRCop-84 be desired, maximum operating
temperature must be limited to prevent precipitate
agglomeration. This limit exists somewhere between 450°C
and 600°C; further testing will be required to determine the
precise value. An additional loss of ductility corresponding
to a less pronounced reduction in cross section and lower
elongation at fracture is also observed on material receiving
the 600°C and 450°C heat treatments.

X. Fracture Surface Analysis

Fracture surfaces of tensile test bars showed dimple

characteristics typical of ductile rupture on the microscopic Figure 15. Fracture surface of 900°C 5h HT GRCop-84 tensile
level, however macroscopic fracture patterns demonstrated stress test specimens post fracture for parallel printed (T1) sample
(a) and perpendicular printed (W1) sample (b). Image stacking was
internal material anisotropy. Tensile bars printed parallel to
used to generate a composite with enhanced depth of field.
tensile stress fracture on a flat plane normal to applied stress
in a manner typical of ductile rupture, while tensile bars
printed perpendicular to the applied stress fracture on a plane
inclined to the applied stress, as shown in Figure 14. Samples
of both print directions displayed necking and rough fracture
surfaces typical of ductile rupture. Necking length was more
concentrated in the parallel printed specimens than in the
perpendicular printed specimens. Both top and perpendicular
printed samples display microvoid formation and
coalescence perpendicular to the pull direction on the surface
of the tensile specimens concentrated in the necking area, a
property typical of GRCop-84 [28].

Figure 16. Fracture surface GRCop-84 tensile stress test specimens

printed perpendicular to the pull direction following several heat
treatment schedules. All fracture surfaces exhibit laser scanning
hatch like texture independent of heat treatment.
Figure 14. 900°C 5h HT GRCop-84 tensile stress test specimens
post fracture (a) for parallel printed and perpendicular printed
samples. Fracture line occurs at ~45° to pull direction for
perpendicular printed bars, and ~90° for parallel printed bars.

Fracture surfaces show characteristic patterns of the

laser hatch based on print direction in optical micrographs;
on parallel printed tensile bars, the hatch pattern was seen on
the fracture surface, Figure 15 (a), while on perpendicular

16

Figure 17. 900°C 5h HT GRCop-84 tensile stress test specimen
post fracture for parallel printed bar (a) and perpendicular printed
bar (b), imaged at a 45° angle to the macroscopic fracture plane.
Print direction indicated by 3D arrow.
Macroscopic fracture patterns do not change with
heat treatment as shown in Figure 16, except for scaling of
size observed in fractures where increased ductility resulted
in greater reduction in fracture cross section on Cusil-ABA
and 900C 5h heat treatments. Similar patterns were observed
in the GRCop-84 grain in etched cross sections shown in
Figure 5 (b,e) implying that the hatch scanning results in an
internal grain structure that controls fracture properties. In
contrast to macroscopic fracture surface characteristics,
cusps on the ~1 µm scale, shown in Figure 17, demonstrated
no difference in characteristics based on material print
direction. Fracture cusps for GRCop-84 were typical of
ductile rupture where microvoid growth and coalescence
were present. Fracture characteristics on the 100 µm scale
were determined by the melt geometry of the laser hatch
pattern, while fracture cusp characteristics on the sub-micron
scale resemble traditional ductile rupture in the copper
material.
a. Fracture Cusps and Precipitate
Characteristics
Analysis of fracture cusps and Cr2Nb precipitates
on 900°C 5h heat treated GRCop-84 fracture surfaces
indicates that void nucleation was initiated by brittle fracture
of Cr2Nb precipitate within the copper matrix. Fractured
precipitates bounding voids exist below the fracture surface.
The high fraction of cusps (80%) with a single Cr2Nb
precipitate at their center indicates precipitate fracture where
parts remaining in opposing cusps and opposing fracture
cusps have similar shaped Cr2Nb precipitates in similar
locations.
SEM micrographs of the fracture surface, shown in
Figure 18 (a), show a distribution of cusp sizes with a distinct
precipitate near the center of each cusp. EDX analysis,
17
shown in Figure 19, indicates that Cr2Nb particles were
located near the center of the fracture cusps, Figure 18 (b),
within the surrounding copper matrix, Figure 18 (c).
Figure 18. Fracture surface of 900°C 5h HT GRCop-84 parallel
printed tensile stress test specimen imaged at a 0° angle (a) showing
presence of Cr2Nb precipitate at the apex of each fracture cusp.
EDX spectra measured on the Cr2Nb precipitate at Point 1 (b), and
on the copper matrix at the edge of the fracture cusp at Point 2 (c).
The presence of a single precipitate near each cusp
center implies that void nucleation initiated on a precipitate
and expanded outward from the nucleation point. The result
was a strong correlation of precipitates and voids rather than
precipitates randomly distributed throughout the fracture
surface. Cusps with more than one precipitate were not
typically seen. Cusps with two adjacent precipitate
fragments in the center were likely produced by the fracture
of two partially agglomerated precipitates. Similar
precipitate are seen near the center of most cusps where the
cusp bottom was visible. Shadowing of the secondary
electron detector by the depth of small cusps obscures
visibility for cusp diameters less than ~100 µm.
Figure 19. EDX spectra measured at Point 1 and Point 2 using a
20keV electron beam. EDX spectra of the Cr2Nb precipitate
indicates a higher Cr peak than the spectra at the edge of the cusp;
Nb peaks were lower due to the higher atomic number.
Comparison of relative sizes, position, and quantity
of cusps and sheared Cr2Nb precipitates on a fracture surface
micrograph show that most cusps contain a single particle
near the center implying shearing or fracture of Cr2Nb
precipitates was the cause of void nucleation during the
fracture process. A SEM image of a fracture surface, shown
in Figure 20, was manually segmented by tracing Cr2Nb
particle (a) and cusp (b) boundaries; in certain cases, image
resolution, depth of field, or shadowing of the secondary
electron detector by the cusp depth obscures visibility of the
cusp bottom preventing observation of Cr2Nb particle
presence in the cusp (c). In this micrograph image intensity
was a mix of 75% from secondary electron detectors and
25% from in-lens detectors; the secondary detector improves
contrast of surface topography, while the in-lens detector
assists highlighting of cusp edges.
Figure 20. Fracture surface of a 900°C 5h HT GRCop-84 parallel
printed tensile bar imaged at a 0° angle showing Cr2Nb precipitate
outlined in blue (a), at the valley of each fracture cusp, outlined in
red (b). Cusps where obscured visibility of the bottom prevented
identification of precipitates locations were marked with green dots
(c). Image intensity is a mix of 75% from SE and 25% from in-lens
detectors.
Two mechanisms of void initiation are possible to:
Cr2Nb fracture, or delamination from the copper matrix. If
Cr2Nb fracture is the primary mechanism, Cr2Nb precipitate
should be found in a large majority of the cusps since part of
the precipitate remains within each cusp. Conversely,
precipitate delamination process is stochastic, with the
precipitate remaining in one side of the fracture surface or
the other, resulting in approximately 50% occupancy of
precipitates within cusps. From a total of 410 cusps in Figure
20, 119 cusps had obscured bottoms due to resolution or
shadowing of the secondary electron detector; 291 cusps had
clearly visible bottoms. Of these 291 cusps, 57 were not
occupied by an identifiable precipitate (19.6% of visible
cusps) while 234 were occupied by an identifiable precipitate
(80.4% of visible cusps). Cusps with obscured bottoms were
of a deeper variety, observed to often contain precipitates in
similar cusps with visible bottoms, while cusps counted with
no precipitate occupancy were scallop shaped and near the
top of intersecting ridges; the verifiable 80.4% precipitate
occupancy within cusps was considered a minimum bound.
The presence of precipitates within 80.4% of visible cusps
indicates that precipitate fracture was dominant.
Image processing of Cr2Nb precipitate and cusp
boundaries provide a statistical analysis of the fracture
surface. Cusps and precipitates in Figure 20 have size
distributions shown in Figure 21; the equivalent diameter of
18
a circular cusp or precipitate (6) is calculated from the area,
A, of the cusp or precipitate in the image.
Dcirc  2  A /  
1/ 2
(6)
Cusp diameters within Figure 20 have a mean of 434 nm and
a median of 374 nm, while precipitates have a mean of 174
nm and a median of 148 nm; a modest shift of towards larger
diameters occurs due to difficulty identifying small cusps
and precipitates. The precipitate size distribution on the
fracture surface shown in Figure 21 matched the distribution
in a pre-fracture FIB cross section shown in Figure 6 (e).
25
Cusp [ m]
Cr2Nb [ m]
20
15
10
0
0 0.2 0.4 0.6 0.8 1
1/2
Dcirc=2(A/ ) [ m]
Figure 21. Histogram of Cusp and Cr2Nb particle diameters on
fracture surface for 900°C 5h HT, assuming circular cross-sections
of Cr2Nb particle and cusp.
Relative positions between Cr 2Nb precipitates and
the center of the containing fracture cusp indicates that the
particle was approximately located at the cusp center; growth
of the cusp from the center during the fracture process
implies that void nucleation and growth initiated at the
Cr2Nb particle. Displacement of a fractured precipitate from
the cusp center, shown in Figure 22, was calculated as the
distance between cusp and precipitate centroids,
Δcentroid=|Cprecipitate-Ccusp|, where C is centroid if the outlined
cusp of precipitate. The centroid distance is normalized to
cusp diameter Δcentroid/Dcusp assuming the equivalent area of
a circular cusp, where D given by (6) due to the irregular
shape of cusp and precipitate edges. Normalized centroid
differences that exceed (Δcentroid/Dcusp >0.5) implying
precipitate location outside of a cusp were due to the
assumption of circular cusps and precipitates, (eg. a
precipitate with a large offset on the major axis of a highly
elliptical cusp is calculated as outside the diameter of a
circular cusp with equivalent area); all precipitates are
located within the cusp for these calculations. Precipitate
locations in Figure 22 have a mode of 0.1∙Dcusp, a median of
0.21∙Dcusp and a mean of 0.26∙Dcusp, where values used to
calculate the mean were restricted to Δcentroid/Dcusp<1 to
reduce skew contribution from values far on the histogram
tail. Fractured precipitates were located near the cusp center
indicating that void formation initiates at the precipitate
location and grows outward.
 Median
Mean
N
Figure 22. Histogram of distance between centroids of Cr2Nb
particle and containing cusp in fractions of cusp diameter for 900°C
5h HT assuming circular cross-sections of Cr2Nb particle and cusp.
Figure 23. Simplified diagram of fracture process involving void
nucleation by fracturing of Cr2Nb precipitates resulting in a
precipitate to cusp diameter ratio indicating relative fracture time.
Precipitates do not necessarily fracture under tensile loading,
shearing is also common.
The ratio of cusp to precipitate diameter plotted
against precipitate diameter is used to estimate the transition
between Orowan looping and precipitate fracture given that
void growth is initiated by a fracturing Cr2Nb precipitate and
void size is correlated with growth time, eg. voids that were
nucleated early in the fracture process will be larger than a
void nucleated later. This process is illustrated in a simplified
diagram shown in Figure 23. A distribution of precipitates
exists within a copper matrix under stress which fractures a
precipitate thereby nucleating the growth of a void (A), as
the material is stressed further, the void grows outward from
the precipitate location; subsequent precipitates were also
fractured (B). These voids continue to grow outward from
fractured precipitates and eventually coalesce as the void
surfaces touch (C). The fracture surface separates at
locations where void surfaces touch forming the cusp edges;
voids that were nucleated early in the fracture process had a
longer growth time and have a proportionally larger ratio of
cusp to precipitate diameter (D).
19
1/2
)
Cr Nb
2
/A
Cusp
(A
Figure 24. Ratio of cusp to Cr2Nb particle diameter plotted vs
Cr2Nb particle diameter for cusps containing a Cr2Nb particle.
Figure 25. FIB cross-section of 900°C 5h HT GRCop-84 in pre-
fractured (a) and post-fractured (b) condition. Large grain
formations seen in the pre-fractured material (a) were broken up
into smaller grains by work hardening or Orowan looping (b). Small
voids nucleated by the fracture of a Cr2Nb precipitate were
observed (c) in the boxed area in (b); two halves of a fractured
Cr2Nb precipitate were located abutting the voids on opposing
sides.
The ratio of cusp to precipitate diameter increases
sharply in the 100 nm to 200 nm range as shown in Figure
24, indicating that precipitates smaller diameters fracture
first, while larger precipitates fracture later when growth of
adjacent voids concentrates stress into the remaining
material. Maximum strengthening occurs at the precipitate
diameter where particle fracture transitions to Orowan
looping, the 100 nm to 200 nm range is estimated as the
optimal precipitate size. Nucleation of voids by precipitate
fracture is shown in Figure 25, in a FIB cross-section of pre-
fracture (a) and post fracture (b) material. Pre-fracture
material is void free with grain boundaries on the order of
several micron. Grain size is substantially reduced during the
fracture process, possibly by a combination of work
hardening and Orowan looping. A magnified view of the
fracture nucleated voids in the boxed area is shown in (c),
where a pair of fractured precipitate precipitates bound voids
in roughly the direction of applied tensile stress.
Fractured precipitates on opposing surfaces have
matching shapes and opposing cusps have matching surface
morphology. Micrographs of opposing left (L) and right (R)
fracture surfaces on a parallel printed tensile test bar were
located at positions shown in Figure 26 100X (top) and 5kX
(bottom) magnification. Two slightly overlapping regions,
denoted “Bear Paw” (boxed in white) and “Mystery Lake”
(boxed in red) were further examined in Figure 28 and Figure
27 at 15kX magnification.
Cusp and precipitates in the Bear Paw (Figure 28)
and Mystery Lake (Figure 27) regions were outlined in red
(cusp) and blue (precipitate). Opposing fracture surfaces of
a GRCop-84 parallel printed tensile test specimen imaged at
a 0° (normal) angle are shown in Figure 28 and Figure 27.
Image intensity is a mix of 75% from a SE detector (provides
improved contrast of height variations) and 25% from in-lens
detectors (highlights cusp edges). Right images were
mirrored horizontally for comparison. For clarity, not all
cusp and precipitate edges were outlined. Not all precipitate
particles in the cusp valleys were visible due to secondary
electron shadowing of the bottom of the cusp. Due to
metallic deformation during the fracture process and position
variations in the SEM, the left and right fracture surfaces
were not geometrically identical and do not directly overlay,
however the surfaces were morphologically equivalent with
respect to the relative positions, number, and shapes of cusps
and precipitates. Opposing fracture surfaces shown in Figure
28 and Figure 27 have fractured precipitates in similar places
within opposing cusps indicating brittle fracture of Cr2Nb
precipitates consistent with the characteristics of Cr2Nb as a
hard, low ductility, brittle precipitate [47]. Several large
fractured precipitate pairs with easily identifiable shapes
were labeled A,A’, B,B’, C,C’, D,D’, and E,E’. Faces of
sheared Cr2Nb precipitates appear smooth, implying
cleaving on a crystal plane. FIB sectioning of the particle
labeled A indicates no delamination of the particle surface
embedded in the fracture cusp from the copper matrix, as
seen in Figure 29.
The fracture characteristics of GRCop-84 samples
indicate that void nucleation during the fracture process is
initiated by fracture of the Cr2Nb precipitates within the
copper matrix. The supporting evidence is that:
1. Cusps contain a single Cr2Nb particle (Figure 20)
located near the center (Figure 22) indicating void
nucleation and growth initiated at the precipitate.
2. Void nucleation by precipitate fracture was
observed below the fracture surface (Figure 25).
3. The fraction of cusps with Cr2Nb precipitate at their
center (80%) indicates precipitate shearing with
parts remaining in opposing cusps.
4. Opposing fracture cusps have similar shaped Cr2Nb
precipitates in similar locations indicating void
growth around the nucleation point of the fractured
particle (Figure 28 and Figure 27).
Maximum strengthening of a precipitate hardened material
occurs when precipitate size is concentrated at the transition
between Orowan looping and particle shearing. This size is
estimated to be ~100 nm for GRCop-84. As the nucleation
of voids within the material is caused by fracture of
precipitate, choice of a Laves-phase based precipitate with
higher shear or tensile strength will increase material
strength in future precipitation hardened copper alloys.
b. Comparison of Fracture Characteristics
of Heat Treated and As Printed GRCop-
84
Differences in precipitate fracture characteristics
between as-printed and 900°C 5h heat treated GRCop-84
imply a transition between polycrystalline and
monocrystalline precipitate structure at high temperatures.
As seen in FIB cross sections of as-printed material where
high cooling rates occurred during the remelt-solidification
process, shown in Figure 7 (a), precipitates have a rough
perimeter with a structure composed by closely packed sub-
granules. Precipitates in as-printed material are distinctly
different in morphology than agglomerated precipitates
exposed to a 900°C 5h heat treatment or Cusil-ABA braze
cycle, shown in Figure 7 (d,e), where smooth perimeters
exist, implying full agglomeration into a monocrystalline
precipitate.
The effect of this transition between a
polycrystalline and monocrystalline structure is evident in
the fracture characteristics of the precipitates. Opposing
fracture surfaces for a tensile specimen in As-printed
condition is shown in Figure 30. Compared to Fracture
surfaces from material exposed to a 900°C 5h heat treatment
shown in Figure 27, cusp sizes are reduced, corresponding to
the higher density of smaller precipitates initiating void
formation during the fracture process. Comparison of
precipitates between As-printed and 900°C 5h heat treated
material, shown in Figure 31, illustrates differences in the
fracture surfaces of the precipitates. While precipitates in the
900°C 5h heat treated material exhibit a smooth surface
typical of a monocrystalline material cleaving along a crystal
plane, precipitates in As-printed material exhibit a rough
surface typical of a polycrystalline material undergoing
brittle fracture. This change in precipitate fracture
morphology implies a transition between polycrystalline and
monocrystalline Cr2Nb occurs at sufficiently high
temperature.

20
 Figure 26. SEM images of opposing fracture surfaces of GRCop-84 parallel printed tensile stress test specimen heat treated at 900°C
for 5h imaged at a 0° (normal) angle. Two select regions containing a distribution of large and small fracture cusps and precipitate
particles, called “Bear Paw” and “Mystery Lake”, and imaged at high magnification in subsequent figures.

Figure 27. SEM images of opposing fracture surfaces in the “Mystery Lake” region of specimen heat treated at 900°C for 5h.

21
 Figure 28. SEM images of opposing fracture surfaces in the “Bear Paw” region of specimen heat treated at 900°C for 5h.

Figure 29. FIB cross-section of fracture surface in the left “Bear Paw” region cut across the line indicated on the left image through the
Cr2Nb particle indicated at location “A”. A platinum mask, shown in the middle image, was applied to the fracture surface before milling
in the region indicated in dashed red; ion beam damage to the surface extends into the area marked in dashed green. The cross-section,
shown in the right image, was imaged at a 30° angle with vertical dimensions tilt corrected on the cross-section. The Cr 2Nb particle
precipitate locate at “A” has undergone brittle fracture, but did not delaminate from the copper matrix. Specimen was heat treated at
900°C for 5h.

22
Figure 30. SEM images of opposing fracture surfaces in specimen in as-printed condition without application of heat treatment. Only
outlines of major cusps and cusp groups are shown for clarity. All visible precipitates are marked.

Figure 31. FIB images of pre-fracture material and SEM images of opposing fracture surfaces for specimens in as-printed condition
(top) and with 900°C 5h heat treatment (bottom) from Figure 27. 900°C heat treatment results in both coarsening of precipitate, and
corresponding fracture cusp size, as well as transition from a polycrystalline precipitate with a rough fracture surface (F) to a
monocrystalline precipitate exhibiting smooth cleaving of a single crystal (E)

23
XI. Conclusions and Recommendations
LPBF of GRCop-84 (8 at. % Cr and 4 at. % Nb) from
gas atomized powder results in a fully dense copper alloy
with a yield strength of 500 MPa and UTS of 740 MPa
(increasing to 810 MPa yield 970 MPa UTS with heat
treatment), exceeding existing wrought coper alloys and
GRCop-84 produced through HIP and extrusion from
powder. The LPBF process was enabled by the improved
coupling of the powder to lasers in the 1060 nm range
compared to OFC. LPBF allows AM of components with
fine detail and good dimensional tolerances [48]. GRCop-84
is 3D printable as vacuum-compatible full density parts with
no additional HIP step required to achieve full density. The
rapid melting and re-solidification during the LPBF process
produces a fine-grained copper alloy with small precipitates.
Heat treatment at 900°C for 5h to relive internal stress results
in precipitate agglomeration that reduces tensile strength
compared to as-printed material. The low solubility of Cr2Nb
precipitate in the copper matrix prevents further coarsening
of precipitates during subsequent exposure high
temperatures. Heat treatment at 450°C for 3h significantly
improves tensile strength, while exposure to 600°C results in
modest precipitate agglomeration and loss of strength even
during short duration exposures in the 10s if minutes.
Brazing near 900°C results in similar tensile strength loss as
the 900°C for 5h heat treatment. FIB sectioning of heat
treated GRCop-84 illustrates agglomeration of precipitates
with sufficiently high temperature and allows calculation of
precipitate size distributions. Although a 600°C heat
treatment results in formation of many fine precipitates, the
tensile strength was still less than that of the 450°C heat
treatment where no fine precipitate formation was observed
implying that maximum strength requires larger precipitates.
Etched LPBF samples indicated an internal melt
pattern controlled by the LPBF laser hatch. Hatch patterns
consistent with the melt pool pattern observed on the top
surface were observed in etched samples of the internal
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XII. Acknowledgements
Work supported by the U.S. Department of Energy,
Office of Science, Office of Fusion Energy Sciences, using
User Facility DIII-D, under Award No. DE-FC02-
04ER54698. This work made use of the MRSEC Shared
Experimental Facilities at MIT, supported by the National
Science Foundation under award number DMR-14-19807.
The authors would like to thank David Ellis for proofreading
this manuscript. The authors would like to acknowledge
Quadrus Corp. (formerly ASRC Federal Astronautics LLC)
for their work in printing samples used in this paper. The
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