J. Appl. Phys.
125
, 145902 (2019);
https://doi.org/10.1063/1.5055398
125
, 145902
© 2019 Author(s).
Application of Al-Cu-W-Ta graded density
impactors in dynamic ramp compression
experiments
Cite as: J. Appl. Phys.
125
, 145902 (2019);
https://doi.org/10.1063/1.5055398
Submitted: 07 September 2018 . Accepted: 26 March 2019 . Published Online: 11 April 2019
James P. Kelly
, Jeffrey H. Nguyen
, Jonathan Lind
, Minta C. Akin
, Brian J. Fix
, Cheng K. Saw
, Elida R.
White
, Waldi O. Greene
, Paul D. Asimow
, and
Jeffery J. Haslam
Application of Al-Cu-W-Ta graded density
impactors in dynamic ramp compression
experiments
Cite as: J. Appl. Phys.
125
, 145902 (2019);
doi: 10.1063/1.5055398
View Online
Export Citation
CrossMar
k
Submitted: 7 September 2018 · Accepted: 26 March 2019 ·
Published Online: 11 April 2019
James P. Kelly,
1
,
a)
Jeffrey H. Nguyen,
1
Jonathan Lind,
1
Minta C. Akin,
1
Brian J. Fix,
1
Cheng K. Saw,
1
Elida R. White,
1
Waldi O. Greene,
1
Paul D. Asimow,
2
and Jeffery J. Haslam
1
AFFILIATIONS
1
Lawrence Livermore National Laboratory, Livermore, California 94551, USA
2
Division of Geological and Planetary Sciences, California Institute of Technology, Pasadena, California 91125, USA
a)
Author to whom correspondence should be addressed:
kelly70@llnl.gov
ABSTRACT
Graded density impactors (GDIs) are used to dynamically compress materials to extreme conditions. Two modi
fi
cations to a previously devel-
oped Mg-Cu-W GDI are made in this work before using it in a dynamic compression experiment: Mg is replaced with Al and a Ta disk is
glued to the back. The Mg phase is replaced by Al because FCC Al remains solid to higher pressure along its Hugoniot compared to Mg. The
addition of the Ta disk creates a constant particle velocity regime and facilitates a de
fi
nition of peak pressure states. Microstructure analysis,
pro
fi
lometry, and ultrasonic C-scans of the Al-Cu-W GDI all con
fi
rm excellent uniformity. We evaluated signal variation in the radial direc-
tion of a dynamically compressed Al-LiF bilayer target to evaluate the contribution of spatial nonuniformity to errors. Velocity traces from
fi
ve photon Doppler velocimetry (PDV) probes located at di
ff
erent radial distances from the center of the target varied at most by 1.1% with
a root mean square of 0.3% during the compression ramp, demonstrating low PDV measurement error over a relatively large experimental
area. The experimental PDV data also agrees well with 1D simulations that use inputs from predictive characterization models developed for
the material properties resulting from tape casting, laminating, and powder consolidation processes. Low measurement error during quasi-
isentropic compression, leading to better precision, ensures a robust platform to reach extreme compression and low-temperature recovery
states and facilitates discovery via synthesis, quenching, and preservation of new high-pressure phases.
Published under license by AIP Publishing.
https://doi.org/10.1063/1.5055398
I. INTRODUCTION
Dynamic compression experiments are used to study matter at
extreme conditions in
fi
elds as diverse as aerospace, biology, chemistry,
geophysics, and planetary science. The physical state of matter in the
Earth
’
s core or the evolution of matter in a bolide impact target can
be explored.
1
,
2
An overview of the dynamic compression of materials
that includes general considerations, experimental methods to generate
dynamic compression, experimenta
ldiagnosticsathighdynamicpres-
sures, and error propagation is given elsewhere.
3
Interesting chemistry
and physics that emerge under extreme conditions are of general inter-
est and have also been reviewed elsewhere.
4
,
5
The report from the Basic Research Needs Workshop on
Synthesis Science for Energy Relevant Technology
4
identi
fi
ed four pri-
ority research directions (PRDs) for realizing the vision of predictive,
science-directed synthesis. Two of the four PRDs are (1) to achieve
mechanistic control of synthesis to access new states of matter and
(2) to accelerate materials discovery by exploiting extreme condi-
tions, complex chemistries and molecules, and interfacial systems.
Many future discoveries are expected to come from relatively unex-
plored parameter spaces that push the boundaries of synthesis
science. The latter PRD speci
fi
cally highlights the ability to synthe-
size matter under extreme conditions, providing access to previously
unknown phase space of new, metastable compounds. Shock
physics and dynamic compression enable access to these extreme
conditions for short periods of time, which may help quench new
metastable phases. Nanosecond synthesis of diamond by shock
compression is one of the most widely known examples of metasta-
ble phase synthesis,
1
and other examples exist in the literature. Our
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recovery experiments after dynamic compression demonstrate a varying
crystal defect structure evolution with loading paths,
6
which could
in
fl
uence phase transitions.
The use of customized loading paths in dynamic compression,
including intervals of quasi-isentropic compression, enables access
to a wider range of extreme pressure and temperature conditions
than can be achieved with traditional static or shock compression
experiments. Compared to conventional shock compression, exper-
iments with designed impedance pro
fi
les and ranges of impact
velocity provide access to periods of quasi-isentropic compression
that, in turn, allow temperature and pressure to be tuned, which
—
among other applications
—
presents an exciting opportunity to
quench new high-pressure phases to ambient conditions by exploit-
ing lower temperatures that inhibit the kinetics of forward or back-
ward transformations. Discovery and characterization of such novel
recovered phases may have implications in condensed-matter
physics, chemistry, materials science, planetary science, and various
applications. Methods for achieving quasi-isentropic loading and
other designed loading paths include gas gun,
7
–
9
laser,
10
–
12
and
magnetically driven compression.
13
–
17
Early quasi-isentropic compression experiments used cylindrical
compression geometries,
18
–
21
plane wave compressions with bu
ff
er
layers,
22
–
27
or conversion of a shock impact into a ramp before it
enters the specimen.
28
,
29
The use of a graded density impactor
(GDI) for quasi-isentropic loading began with Barker
30
in the 1980s.
At that time, the fabrication of high-quality GDIs was recognized as
the major challenge in creating quasi-isentropic compression with a
well-controlled input wave. Tape casting, laminating, binder burnout,
and hot pressing are highly e
ff
ective methods of tailoring GDIs to
control the thermodynamic path during an experiment because the
GDI design can be controlled by the tape-stacking sequence.
7
,
8
,
31
–
33
Such tailored GDIs can be designed to provide unique thermody-
namic paths that include sequential combinations of shock,
quasi-isentropic compression, constant pressure, and controlled
release regimes
—
all in a single experiment
—
enabling mechanistic
control of synthesis to access new states of matter.
The quali
fi
cation of a new GDI design prepared by tape casting
and laminating is lengthy and generally has three aspects.
31
–
33
The
fi
rst aspect is tape characterization, which is used to determine the
tape-stacking sequence. As many as 100 tape layers stacked within a
few millimeters may be required by the GDI design, which necessi-
tates several months of characterization. Replication of quali
fi
cation
experiments can reduce common-cause variation (inherent process
variation) and facilitate assigning and reducing special causes of vari-
ation, but at the expense of adding several more months onto the
quali
fi
cation time. GDI variation is of interest because a sensitivity
study has demonstrated that pressure ramp uncertainty from the
impactor is likely to generate more uncertainty in information
extracted from dynamic ramp compression experiments than align-
ment and diagnostic uncertainties.
34
The second and third aspects of
quali
fi
cation include process veri
fi
cation and deployment to verify
that there are no processing or application-speci
fi
climitations.
High-impedance GDIs have recently been prepared by func-
tionally grading Mg, Cu, and W.
33
In this work, we describe the
fabrication and quali
fi
cation of new high-impedance GDI prepared
by functionally grading Al, Cu, and W, followed by gluing Ta to
the back of the GDI. One advantage of replacing Mg with Al is that
the FCC Al phase melts at higher pressure along its Hugoniot com-
pared to the HCP Mg phase. Microstructure analysis, ultrasonic
C-scans, and pro
fi
lometry of GDIs alongside photon Doppler
velocimetry (PDV) signals recorded during a dynamic ramp com-
pression experiment all con
fi
rm excellent GDI uniformity.
Velocity traces from
fi
ve PDV probes located at di
ff
erent radial
distances from the center of a dynamically compressed target
varied by less than 1.1% of nominal in the functionally graded
section with a root mean square of 0.3%, indicating low PDV
measurement uncertainty. Low measurement uncertainty during
quasi-isentropic compression, leading to better precision, ensures
a robust experimental platform to facilitate the discovery and syn-
thesis of new high-pressure phases that can be quenched to
ambient conditions by exploiting extreme compression and low-
temperature recovery states.
II. MATERIALS AND METHODS
A. Tape characterization and root cause analysis of
variation
At least 20 nominally two-phase metal composites span-
ning the full composition range of Al-Cu and Mg-Cu systems
were fabricated by tape casting powder mixtures, stacking and
laminating 50 layers of tapes, binder burnout, hot pressing, and
characterization methods tha
t have been described in detail.
31
–
33
One of the systems consisted of aluminum (98%, APS 10
–
14
μ
m,
Alfa Aesar, Ward Hill, MA) and copper (99.9%, 3
–
5
μ
m, Alfa
Aesar). The other system consisted of magnesium (99.8%,
−
325
mesh, Alfa Aesar) and copper (99%,
−
325 mesh, Alfa Aesar).
The Mg-Cu composites were prepared and characterized for
comparison purposes.
The length of the binder burnout cycle was two days longer and
the
fi
nal temperature was 25 °C higher (i.e., 400 °C) for the Al-Cu
system compared to the binder burnout cycle for the Mg-Cu system.
The extended binder burnout cycle was necessary to prevent compact
defects. All other parameters were controlled to the maximum extent
possible. Samples were hot pressed at 370 °C for 66 min under a uni-
axial stress of 250 MPa using a Carver 30-ton Autoseries press
(Carver, Wabash, IN). Tape layer thicknesses reported are the mean
from measuring 5 blanks with a digital caliper. Consolidated layer
thicknesses and composite densities were measured from the cylindri-
cal geometry and masses of the hot pressed compacts. The 10-MHz
longitudinal acoustic velocities through the height of the compacts
were measured in four approximately equidistant locations around
the compact perimeter and in the center of the compact. A
time-of-
fl
ight cross correlation method was used to calculate acoustic
velocities. Reported values are an average of values obtained at the
fi
ve measurement locations.
Three replicate samples of select Mg-Cu composites (
n
=3)
were also prepared to evaluate the e
ff
ect of secondary phases by
X-ray di
ff
raction (XRD) analysis and using Jade software (v.9.7,
Materials Data, Inc., Livermore, CA). The XRD data were collected
with a conventional Phillips vertical goniometer, utilizing Cu-K
α
radiation. Step scans were performed from 20° to 100° 2
θ
with a
step size of 0.02° and an acquisition time of 2 s per step. Rietveld
re
fi
nement,
35
,
36
a whole pattern
fi
tting technique, was applied to
the XRD data to extract estimates of the weight percentage of each
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Published under license by AIP Publishing.
phase with better accuracy than typical peak intensity comparison.
The weight percent estimates were converted to volume percent
using the theoretical density of the phases.
B. GDI process veri
fi
cation
An Al-Cu-W GDI was designed and built in two steps
because of di
ff
erent processing requirements for Al-Cu mixtures
compared to Cu-W mixtures, as noted by Yep
et al.
33
The Cu-W
tapes were prepared from Cu (1.5
–
5
μ
m, ACuPowder International,
Union, NJ) and W (99.9%, 1
–
5
μ
m, Alfa Aesar) and stacked in a
compositional sequence that varied from 100% Cu to a mixture of
50:50 volume percent Cu:W. This composition has impedance
close to Ta and provides a good impedance match to the Ta disk
that will be bonded to the back of the GDI. The binder burnout
pro
fi
le was similar in length to that of the Al-Cu pro
fi
le, but 50 °C
lower (i.e., 350 °C). The samples were vacuum hot pressed in a
graphite punch and die set for 2 h at 1000 °C and 70 MPa uniaxial
stress (typical vacuum levels 10
−
5
–
10
−
6
Torr). The Al-Cu sequence,
from 100% Al to 100% Cu, was prepared as described in Sec.
II A
and hot pressed together with the
fi
nished Cu-W sequence,
arranged in the die, and hot pressed to bond the Cu-Cu interface.
The Al-Cu-W GDI was characterized by surface pro
fi
lometry
with a wide-area 3D measurement system (VR 3100, KEYENCE
Corporation, Itasca, IL). Ultrasonic testing with an UltraPAC
™
instrument (UPK-T10, MISTRAS Group, Inc., Princeton, NJ) was
conducted in the pulse-echo mode using a 15-MHz transducer
(0.375 in. diameter and 1.50 in. focal length) on a GDI immersed
in mineral oil. The microstructure was also evaluated using stan-
dard microscopy techniques (sectioning, polishing, and imaging).
C. GDI deployment
A Ta disk was bonded to the back of a GDI fabricated by the
procedure outlined in Sec.
II B
with STYCAST® epoxy. The GDI
and the Ta disk were
fi
rmly pressed into contact to squeeze out
excess epoxy. The Ta disk
—
a high-purity, high-impedance metal
standard in shock physics studies
—
provides a constant particle
velocity regime after the ramped compression and prevents a
release wave from interfering with the compression ramp. To assess
the radial uniformity of a nominally 1D impact, one assembled
GDI was mounted on a Lexan sabot and launched on the two-stage
light gas gun facility at the California Institute of Technology (Shot
#530) to dynamically compress an aluminum target backed with
a LiF window and observed by eight PDV probes located at di
ff
erent
radial distances from the target center (1, 2, 3, 4, 5, 6, 7, and 8 mm).
A schematic of the experimental con
fi
guration is illustrated in
Fig. 1
.
The edges were machined o
ff
the GDI to form a 25 mm diameter.
The measured velocity of the projectile prior to impact by double-
fl
ash X-ray and dual magnetic loop pickups was 3.85 ± 0.04 km/s.
Only PDV probes with response signal-to-noise ratios (S/N) greater
than or equal to 5 were analyzed, corresponding to 5 out of 8 chan-
nels (
r
=2,3,4,5,6mm),becausesmallerS/Ncreateddiscontinuities
in the PDV trace when transforming the raw signals into particle
velocities. Apparent velocities measured by PDV were corrected to
account for LiF properties and give true velocities.
37
Complementary simulations were performed to compare to
experimental data and expand the opportunity for expedited GDI
development and quali
fi
cation. Simulations were performed in
ALE3D, a
fi
nite element code developed at the Lawrence Livermore
National Laboratory.
38
Inputs included model layer thicknesses and
initial densities from tape characterization. A Mie
–
Grüneisen equa-
tion of state was used for all materials in the simulation with material
parameters from Steinberg.
39
Cubic hexahedral mesh elements were
used with a side length of 200 nm resulting in 2 × 2 × 10
5
elements.
The time at impact was de
fi
ned as
t
= 0 ns (shock breakout time and
ramp compression times are relative to the impact time) and simula-
tions continued up to 1
μ
s after impact. Material composition of any
given element was assigned based on probability equal to the volume
fraction of constituents within a given layer in the GDI.
FIG. 1.
(a) Side view schematic of a dynamic compression experiment where a
25-mm diameter GDI impacts a 32.5-mm diameter, 1.5-mm thick Al baseplate
and a 19-mm diameter, 10-mm thick LiF window. (b) Back view schematic of
the LiF window showing PDV probe locations that observe the Al-LiF interface
at positions 1, 2, 3, 4, 5, 6, 7, and 8 mm from the center.
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III. RESULTS AND DISCUSSION
A. Tape characterization and root cause analysis of
variation
Tape characterization for GDI quali
fi
cation has been described
elsewhere.
31
–
33
Important characterization metrics include the consol-
idated thickness, density, and acoustic velocity. Layer thickness analy-
sisforAl-Cucompositesisshownin
Fig. 2
. The mean tape thickness
is 81.12 ± 0.06
μ
m based on a 95% con
fi
dence interval [solid line in
Fig. 2(a)
] and the observed thickness range is within ±8.09
μ
mofthe
mean [bound by the dotted lines in
Fig. 2(a)
].
Figure 2(a)
also dem-
onstrates that the mean thickness, after binder burnout and consoli-
dation, is 48.02 ± 0.05
μ
m based on a 95% con
fi
dence interval and
the observed thickness range is within ±7.99
μ
mofthemean.Similar
thickness variation from mean values (about 8
μ
m) and similar thick-
ness variation patterns of the two data sets observed in
Fig. 2(a)
suggest that the consolidated thickness is correlated with tape thick-
ness; this correlation is linear, as shown in
Fig. 2(b)
.Theconsolidated
layer thickness can be predicted from the original tape thickness to
within ±9% based on this correlation.
Tape and consolidated thicknesses for Mg-Cu composites are
shown in
Fig. 3(a)
. The mean tape thickness is 85.16 ± 0.08
μ
m
FIG. 2.
(a) Experimental thicknesses of Al-Cu composite tapes (closed circles)
and consolidated thickness (open circles). (b) Correlation between the Al-Cu
tape thickness and the consolidated thickness (R
2
= 0.56) that enables the pre-
diction of consolidated layer thicknesses from the tape thickness measurements
to within ±9% of experimental observations. Mean thickness values or predic-
tions (solid lines) and observed limits from the mean or predictions (dashed
lines) are superimposed onto the plots.
FIG. 3.
(a) Experimental thicknesses of Mg-Cu composite tapes (closed circles)
and consolidated thickness (open circles), (b) consolidated shrinkage of Mg-Cu
tapes, and (c) correlation (R
2
= 0.82) that enables the prediction of the consoli-
dated layer thickness from tape thickness measurements and knowledge of the
tape formulation to within ±9% of experimental observations. A predicted con-
solidation shrinkage line (solid line) and observed limits from the prediction
(dashed lines) are superimposed onto the correlation plot in (c).
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based on a 95% con
fi
dence interval and the observed thickness
range is within ±15.17
μ
m of the mean. The average consolidated
thicknessis34.31±0.06
μ
m based on a 95% con
fi
dence interval
and the observed thickness range is within ±15.95
μ
mofthe
mean. The observed thickness range is about twice as much for
Mg-Cu tapes as it is for Al-Cu tapes, and the consolidated thick-
ness is not correlated with the tape thickness in the Mg-Cu tapes
(R
2
= 0.06 and not shown for brevity). The absence of correlation
suggests an additional source of variation, which is explored in
the next paragraph.
The calculated shrinkage during hot pressing of each Mg-Cu
tape is shown in
Fig. 3(b)
. The consolidation shrinkages for
Mg-Cu tapes are generally greater than for Al-Cu tapes. Several
factors (e.g., powder characteristics, additives) can cause di
ff
eren-
ces in the powder packing density that result in di
ff
erent consoli-
dation behaviors.
40
Without establishing individual contributions,
there is a reasonably tight linear correlation (R
2
= 0.82) between
the volume of polymers in Mg-Cu tapes and the consolidation
shrinkage [
Fig. 3(c)
]. This suggests that the slurry formulation
used to produce the tapes is a root cause for di
ff
erences in the
powder packing density and thus consolidation shrinkage. The
correlation can also be used to predict the consolidated layer
thickness of the Mg-Cu tapes to within ±9% from the tape formu-
lation and tape thickness measurements. It was not necessary to
consider the e
ff
ect of the polymers for Al-Cu tapes because there
was better control over the binder formulation (polymer fraction
within ±5 vol. % for all Al-Cu tapes compared to ±9 vol. % for
Mg-Cu tapes). The thickness data are summarized in
Table I
.
Consolidated thickness predictions based on the initial tape thick-
ness and polymer content can now be made with ±9% uncertainty
for both tape systems at the current level of process control. The
results suggest that better control over slurry formulations and
tape casting thickness will reduce this aspect of uncertainty.
Density after hot pressing is the second metric for characteriz-
ing the tapes. The measured densities and relative densities of the
composites are shown in
Fig. 4
. The theoretical densities of com-
posites were determined by a rule of mixtures:
ρ
th
¼
X
i
f
i
ρ
th
,
i
,
(1)
where
ρ
th
is the theoretical density of the composite,
f
i
is the
volume fraction of phase
i
, and
ρ
th,i
is the theoretical density of
phase
i
(e.g., Al, Cu, Mg). Theoretical densities of composites were
used to determine relative densities from measured densities. The
relative densities are measured densities expressed as a percent of
theoretical density. The
ρ
th,i
values for Al, Cu, and Mg phases used
in calculations were 2.70, 8.93, and 1.867 g/cm
3
, respectively.
49
The
ρ
th,i
value used for Mg is intentionally higher than the theoretical
FIG. 4.
Composite density (
ρ
c
) and density relative to theoretical (
ρ
rel
)for(a)
Al-Cu composites and (b) Mg-Cu composites. Mean density relative to theoretical
(dotted line), predicted composite density based on the mean relative density (solid
line), and observed density limits (dashed lines) are superimposed onto the plots.
Density can be predicted to be within ±2% of observed values for Al-Cu compos-
ites and ±4% for Mg-Cu composites using a rule of mixtures. (c) Phase estimates
from X-ray diffraction data were used to correct theoretical and relative densities of
Mg-Cu composites in part (b);
fi
ts are superimposed onto the plot to guide the eye
(n.b., no secondary phases were observed in the Al-Cu
system).
TABLE I.
Summary of thickness data and observed limits compared to predictions.
Metric
Al-Cu
Tapes
Consolidated
Al-Cu
Tapes
Mg-Cu
Tapes
Consolidated
Mg-Cu
Tapes
Mean thickness (
μ
m) 81
48
85
34
Observed range (
μ
m) ±9
±8
±15
±16
Mean shrinkage (%) NA
41
NA
60
Observed limits (%) NA
±9
NA
±9
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density of Mg (1.74 g/cm
3
) to account for signi
fi
cant MgO contam-
ination with 3.58 g/cm
3
theoretical density.
49
The MgO in Mg
determined by XRD measurements was 13.23 ± 0.12 wt. % based on
a 95% con
fi
dence interval, or 6.92 ± 0.07 vol. % using theoretical
densities. Thus, Eq.
(1)
predicts a density of 1.867 ± 0.001 g/cm
3
for
the Mg-MgO composite, which is used in place of the pure Mg
density. Although Mg
2
Cu and MgCu
2
intermetallic phases were
observed, such intermetallic phases are insigni
fi
cant to the density
because the compound densities are very close to the weighted
density of the pure metals with the same atomic proportions. No
additional phases were found in the Al-Cu system.
The measured and relative densities of Al-Cu composites are
shown in
Fig. 4(a)
. The mean relative density of the Al-Cu compos-
ites is 95.31% ± 0.01% of theoretical density based on a 95% con
fi
-
dence interval and the observed relative density range is within
±1.79% of the mean. The relative density variation appears nor-
mally distributed around the mean value. The measured and rela-
tive densities of Mg-Cu composites are shown in
Fig. 4(b)
. The
mean relative density of the Mg-Cu composites is 95.85% ± 0.02%
based on a 95% con
fi
dence interval and the observed relative
density range is within ±3.89% of the mean. There is more varia-
tion in the relative density for the Mg-Cu composites compared to
that for the Al-Cu composites. Unlike the Al-Cu system, there is a
systematic variation in the relative densities with composition in
the Mg-Cu system. The relative density is biased toward lower
values with increasing copper, as observed in prior studies.
31
,
32
This is an important point because uncertainties in mean density
values propagate to uncertainty in using and modeling Mg-Cu
GDIs. The volume fractions of the additional phases calculated
from XRD measurements of the weight fractions are given in
Fig. 4(c)
for reference.
The compact density,
ρ
c
, can be estimated from the mean rela-
tive density,
ρ
rel
, and the theoretical density:
ρ
c
¼
ρ
rel
ρ
th
:
(2)
All measured density data for Al-Cu composites are within ±2%
of values predicted using Eq.
(2)
, whereas measured density data
for Mg-Cu composites vary from the predictions by about twice
as much, ± 4%. The higher uncertainty for Mg-Cu composites is
most likely due to the relative density bias discussed previously.
Copper cannot be directly implicated for the bias toward lower
density with increasing copper because the bias is not observed in
the Al-Cu system. Factors like initial powder packing density and
reactions can in
fl
uence densi
fi
cation.
40
A lower powder packing
density due to a higher volume of polymers in the tape formula-
tion [see Fig.
3
] can contribute to the bias. Alternatively, reac-
tions forming the additional phases [see
Fig. 4(c)
] can contribute
to the enhanced densi
fi
cation in the Mg-rich compositions. The
formation of secondary phases involves temperature-dependent
reaction kinetics and so hot pressing thermal parameters
(e.g., heating/cooling rates, hold temperatures, hold times) are root
causes that can impact the quantities of additional phases and con-
tribute to additional uncertainty for the Mg-Cu system. Better
control over the slurry formulations and the hot pressing parame-
ters could reduce this aspect of modeling uncertainty. A summary
of the density data is provided in
Table II
.
The third metric is acoustic velocity through the hot pressed
compacts. A model of longitudinal acoustic velocity based on the
Reuss approximation of aggregate elastic moduli has been described
in detail and works quite well despite being considered a lower
limit.
31
,
32
The Reuss model assumption of stress continuity among
phases appears to describe the aggregate elastic behavior of GDIs
more closely than the alternative Voigt model assumption of equal
strain in both phases. The model for acoustic velocity of a two-
phase composite is given by
E
¼
ρ
v
2
,
(3)
and
E
12
¼
E
1
E
2
(
E
1
f
2
þ
E
2
f
1
)
,
(4)
where
E
is the elastic modulus,
ρ
is the density,
v
is the acoustic
velocity,
E
12
is the elastic modulus of a two-phase composite
made from phase 1 and phase 2,
E
1
is the elastic modulus of
phase 1,
E
2
is the elastic modulus of phase 2,
f
1
is the volume
fraction of phase 1, and
f
2
isthevolumefractionofphase2.
E
1
and
E
2
are usually determined from Eq.
(3)
with density and
acoustic velocity data on the pure phases, prepared under suit-
able processing conditions. Then,
E
12
is estimated from Eq.
(4)
and, with the measured density of the two-phase composite,
Eq.
(3)
yields a model prediction for the acoustic velocity of the
two-phase composite,
v
12
.Wewillmakeaslightmodi
fi
cation
to this approach to account for process variation by replacing
measured density and acoustic velocity values of phase 1 and
phase 2 with values that correspond to the mean relative
density. Approximating acoustic velocity at the mean relative
density requires elaboration.
Relative density is lower than theoretical because of porosity.
Accounting for the e
ff
ect of porosity on the model is not straight-
forward because there is no universal equation relating porosity to
elastic modulus; neither stress nor strain compatibility between the
matrix and the voids applies, and the aggregate properties depend
on pore morphology and spatial distribution in addition to volume
fraction. MacKenzie
41
derived an equation to estimate the elastic
modulus of a solid with a given radii distribution of spherical
pores. Other studies have con
fi
rmed a complex dependence on
pore morphology parameters that may be unknown
42
–
45
and on a
residual stress state, which can a
ff
ect acoustic velocity by up to
30%.
46
,
47
MacKenzie
41
noted that an empirical approach incorpo-
rating experimentally determined values enables reliable estimates
of porosity corrections in the presence of such combined e
ff
ects.
TABLE II.
Summary of composite densities and observed limits compared to
predictions.
Metric
Al-Cu
Composites
Mg-Cu
Composites
Mean relative density (%)
95.31
95.85
Observed limits (%)
±2
±4
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The dependence of acoustic velocity on porosity can be
described generically as
v
(
P
)
¼
v
o
F
(
P
),
(5)
where
v
(
P
) is the acoustic velocity as a function of porosity,
v
o
is
the acoustic velocity without porosity, and
F
(
P
) is a porosity func-
tion that corrects the acoustic velocities to the appropriate mean
relative density, 1
−
P
avg
, where
P
avg
is the mean pore fraction.
F
(
P
)
is calibrated at the measured porosity level,
P
exp
(e.g., 1
−
ρ
rel
),
v
o
¼
v
(
P
exp
)
F
(
P
exp
)
,
(6)
and substituting
v
o
from Eq.
(6)
into Eq.
(5)
gives the following
expression:
v
(
P
avg
)
¼
v
(
P
exp
)
F
(
P
avg
)
F
(
P
exp
)
:
(7)
Equation
(7)
yields the acoustic velocity of the two phases at the
mean relative density once the experimental and mean relative densi-
ties of the two phases are known. Equations
(5)
and
(7)
are written
generically so that any porosity function can be applied. In the
absence of a universal porous elasticity model, the porosity function
used here is derived from Kingery
’
ssimpli
fi
cation
48
of MacKenzie
’
s
derivation and the following expression for density:
E
(
P
)
¼
E
o
(1
1
:
9
P
þ
0
:
9
P
2
),
(8)
and
ρ
(
P
)
¼
ρ
th
(1
P
),
(9)
where
E
(
P
) is the elastic modulus as a function of pore fraction,
E
o
is
the elastic modulus without porosity, and
ρ
(
P
) is the density as a
function of pore fraction. Using Eqs.
(8)
and
(9)
to derive the acous-
tic velocity model from Eqs.
(3)
and
(4)
and comparing to Eq.
(5)
results in the following porosity function:
F
(
P
)
¼
1
1
:
9
P
þ
0
:
9
P
2
1
P
1
2
:
(10)
Table III
shows the data and results of the application of these
equations to obtain the mean density and mean acoustic velocity
of phase 1 (Mg or Al) and phase 2 (Cu), to be used as the
Reuss-derived model inputs for acoustic velocity of the composites
[see Eqs.
(3)
and
(4)
].
The measured and predicted acoustic velocities of Al-Cu com-
posites are shown in
Fig. 5(a)
; values agree within ±3%.
Corresponding values of Mg-Cu composites [
Fig. 5(b)
] agree
within ±4%. Like the density predictions from which the acoustic
velocity model is derived, acoustic velocity prediction errors for
Mg-Cu composites are higher than for Al-Cu composites, most
likely because of the same root causes. Thus, better control over the
slurry formulations and hot pressing parameters is likely to reduce
acoustic velocity prediction uncertainty. A summary of the
observed acoustic velocity prediction limits is given in
Table IV
.
The purpose of characterizing density and acoustic velocity
is to calculate acoustic impedance. The acoustic impedance,
z
,
FIG. 5.
Longitudinal acoustic velocities through (a) Al-Cu composites and (b)
Mg-Cu composites. Acoustic velocity predictions (solid lines) can be made to
within ±3% of experimental observations (open circles) and within ±4% for
Mg-Cu composites using a Reuss-bound model (observed limits from predic-
tions are given as dashed lines).
TABLE III.
Measured and mean densities, porosity fractions, and acoustic velocities
used to predict acoustic velocities of composites.
System Phase
Data
ρ
rel
(%)
P
ρ
(g/cm
3
)
v
(km/s)
Al-Cu
Al Measured 94.37 0.0563 2.55
5.83
Mean
95.31 0.0469 2.57
5.85
Cu Measured 95.44 0.0456 8.52
3.87
Mean
95.31 0.0469 8.51
3.86
Mg-Cu Mg Measured 94.53 0.0547 1.77
5.41
Mean
95.85 0.0415 1.79
5.44
Cu Measured 93.45 0.0655 8.35
4.13
Mean
95.85 0.0415 8.56
4.17
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is given by
31
–
33
z
¼
ρ
v
:
(11)
Acoustic impedance predictions can be made using density predic-
tions [Eq.
(2)
] and acoustic velocity predictions [Eq.
(7)
] as inputs
to Eq.
(11)
. Impedance values calculated from experimental data
and from this prediction scheme are shown in
Fig. 6
; impedance
predictions are accurate to ±4% for Al-Cu composites and ±6% for
Mg-Cu composites. These observed limits are consistent with the
propagation of the errors on density and acoustic velocity and so,
again, better control over slurry formulations and hot pressing
parameters should reduce acoustic impedance prediction uncer-
tainty. All aspects of tape characterization are now complete. The
second step of GDI quali
fi
cation is process veri
fi
cation.
B. GDI process veri
fi
cation
Section
III A
focused on a comparison between the Al-Cu and
Mg-Cu systems because we are substituting Al for Mg in previously
developed Mg-Cu-W GDIs.
33
We applied a similar analysis to the
Cu-W system to establish uncertainties, which is only summa-
rized here for brevity (
Table V
). The uncertainty in predicting
thickness, density, and acoustic velocity was 12%, 1%, and 1%,
respectively. There is greater uncertainty in thickness arising from
the tape casting process and lesser uncertainty in density and
acoustic velocity arising from both tape casting and thermal pro-
cessing compared to those in the Al-Cu and Mg-Cu composites.
However, these limits were inferred from a more limited data set
(only 8 composite samples compared to at least 20 in each of the
Al-Cu and Mg-Cu systems).
The prediction methods that have been developed in this work
can be used to model the acoustic impedance pro
fi
le of any GDI
tape-stacking sequence, which is typically done via a lengthy
process (months of e
ff
ort) that determines the thickness and acous-
tic impedance of each individual layer.
31
–
33
,
50
The predicted imped-
ance pro
fi
le (with calculated uncertainty) of a 52-layer Al-Cu-W
GDI are compared to data from the traditional experimental tape
characterization process in
Fig. 7
. The limits shown are extreme
limits for GDI-to-GDI impedance pro
fi
le variation (e.g., the upper
limit assumes that each consolidated layer has the minimum pre-
dicted thickness and the maximum predicted impedance). The
modeled and measured impedance pro
fi
les agree to within ±4%.
This agreement represents a major progress in the practical applica-
tion of new GDI designs, reducing the time for the
fi
rst stage of
GDI quali
fi
cation from months to weeks since only tape thick-
nesses and full characterization of the pure phases are required
(as opposed to full characterization of each individual compositional
layer), which reduces the number of tapes to characterize by 90%.
The predicted thickness of a GDI having the impedance
pro
fi
le depicted in
Fig. 7
is 2.40 ± 0.23 mm. This corresponds to an
estimated 10% uncertainty in the length or rate of the compression
ramp that will result from the use of the GDI in a dynamic com-
pression experiment.
30
This level of uncertainty is comparable to
the reported current input accuracy of Sandia
’
s Z machine.
51
Although the input wave may therefore vary from one GDI to
another, the thickness of each GDI is known before it is used in a
given experiment and the input wave (i.e., drive) for each experi-
ment is directly measured. Hence, the selection of a subset of
TABLE IV.
Observed limits for acoustic velocity compared to predictions.
System
Observed limits (%)
Al-Cu
3
Mg-Cu
4
TABLE V.
Observed limits compared to predictions for thickness, density, acoustic
velocity, and acoustic impedance for Cu-W composites.
Parameter
Observed limits (%)
Thickness
12
Density
1
Acoustic velocity
1
Acoustic impedance
2
FIG. 6.
Acoustic impedance of (a) Al-Cu composites and (b) Mg-Cu compos-
ites. Acoustic impedance predictions (solid lines) can be made to within ±4% of
experimental observations (open circles) for Al-Cu composites and within ±6%
for Mg-Cu composites using the density and acoustic velocity models (observed
limits from predictions are given as dashed lines).
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fi
nished GDIs with a narrower thickness range allows a series of
experiments with nearly identical compression ramps.
We have fabricated 13 GDIs with the nominal impedance
pro
fi
le demonstrated in
Fig. 7
to demonstrate the bene
fi
t of GDI
selection criteria. The mean thickness of the 13 GDIs is 2.42 ± 0.06
mm (95% con
fi
dence interval) and ranged from 2.21 to 2.59 mm.
The measured range is in excellent agreement with the predicted
limits (2.40 ± 0.23 mm). Selecting a subset of 5 GDIs from the orig-
inal 13 yields a thickness range from 2.42 to 2.45 mm and reduces
variations in pressure ramp uncertainty to 1%.
We so far focused on GDI-to-GDI variation, but the unifor-
mity of a given GDI is also important for dynamic compression
experiments. Each fabricated GDI is a cylinder with 31.75 mm
diameter and the microstructure should be as uniform as possible
over the entire area of the GDI to allow
fl
exible placement of mea-
surement probes. Next, we explore the microstructure and compo-
sition gradient on a full-depth, full-radius cross section of a GDI,
pro
fi
lometry to check surface height variation, and ultrasonic
testing to con
fi
rm uniformity.
Figure 8
shows a representative microstructure cross section of
an Al-Cu-W GDI. It is di
ffi
cult to decipher the original tape layer
boundaries, demonstrating a smooth compositional gradient.
Overall, the Al-Cu-W GDI appears to have good microstructure
uniformity. There are rare instances of abnormally large Al grains
in the microstructure, which could be eliminated by better control
of the Al particle size distribution.
Height images of two Al-Cu-W GDIs are shown in
Fig. 9
. The
white arrow across the height image in
Fig. 9(a)
depicts the direc-
tion of maximum side-to-side thickness variation across the
surface, which causes the maximum convex bow height (closed
circle) to shift from the center (open circle). The mean side-to-side
thickness variation from measurements on seven GDIs was 20 ± 10
μ
m (95% con
fi
dence interval) and ranged from 0 to 40
μ
m. The
mean bowing height from measurements on seven GDIs was 30 ±
10
μ
m (95% con
fi
dence interval) and ranged from 20 to 40
μ
m.
The extent of bowing and side-to-side thickness variation is com-
parable to previously developed GDIs.
32
,
33
Bowing and side-to-side
thickness variation cause local compression or dilation of the
impedance pro
fi
le at di
ff
erent points on the impacting surface that
can contribute to PDV measurement variation.
The extent of side-to-side thickness variation or bowing
(
≤
40
μ
m) compared to the thickness of the GDI (
≥
2.17 mm) sug-
gests that these factors may contribute up to about 1.8% to PDV
measurement uncertainty at di
ff
erent probe locations. However, this
may be an overly conservative limit because the e
ff
ects of bowing
and side-to-side thickness variation can be partially mitigated by
strategic selection of probe locations. For example,
Fig. 9(b)
demon-
strates a GDI that is bowed, but without a signi
fi
cant side-to-side
thickness variation. For this GDI, probes located at the same radial
distance from the center (e.g., at the positions of the arrows along
the dotted curve) would be minimally a
ff
ected by GDI side-to-side
thickness variation and bowing due to symmetry.
Nondestructive evaluation of each GDI with ultrasonic testing
is performed before it is considered for use in a dynamic compres-
sion experiment.
32
,
33
Such an evaluation is demonstrated by the A-,
B-, and C-scans in
Fig. 10
. An A-scan records the amplitude of
echoes returned to the transducer as a function of time; the front-
side and backside re
fl
ections can be picked and yield a transit time
through the GDI. This can be compared to a prediction from the
tape characterization data. The waveform of an Al-Cu-W GDI is
depicted in
Fig. 10(a)
. The time between the peak amplitudes of
the re
fl
ections from the front Al surface and the back Cu/W
surface is 0.90
μ
s. This precisely matches the acoustic time-of-
fl
ight
expected from thickness and acoustic velocity data (0.90
μ
s for the
2.36 mm thickness of this GDI).
A B-scan is given in
Fig. 10(b)
, which represents the waveform
(A-scan) as a function of position as the transducer is scanned
FIG. 7.
Impedance pro
fi
le of an Al-Cu-W GDI as a function of thickness deter-
mined by predictions and experimental validation (open circles). The predicted
impedance pro
fi
le is given as a solid line and limits derived from thickness and
impedance prediction limits are given as dashed lines. The predicted GDI thick-
ness based on the speci
fi
c tape-stacking sequence is 2.40 ± 0.23 mm when
considering the prediction limits, which agrees well with the observed thick-
nesses of 13 of these GDIs (the mean thickness of 13 GDIs is 2.42 ± 0.06
based on a 95% con
fi
dence interval and ranged from 2.21 to 2.59 mm).
FIG. 8.
Optical micrograph of the graded section of an Al-Cu-W GDI, which
demonstrates the transformation of a series of discrete compositional layers into
a smoothly graded structure as well as good microstructure uniformity.
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along a line, in this case a 31.75 mm grand diameter of the GDI.
The color scale in the B-scan represents the echo amplitudes
returned to the transducer as a function of time (the waveform
from an A-scan is drawn in the center of the B-scan to help clarify
this visualization). The uniformity of the color bands over the
inner 29 mm of the scan length shows that the waveform is
uniform across the scan length except where there are edge e
ff
ects
(i.e., about 1
–
2 mm from each edge). There are no major re
fl
ections
between the signals from the front and back surfaces anywhere
along the scan length, and both the position and the intensity of
the re
fl
ections are uniform. The parallel dotted lines drawn in
Fig. 10(b)
show that deviations from surface parallelism are too
small to be observed by this method.
A C-scan represents the spatial uniformity over the entire GDI
surface, typically by plotting either the acoustic time-of-
fl
ight or
the amplitude of the largest re
fl
ection in a speci
fi
ed time frame as a
function of scan position. For example, the C-scan in
Fig. 10(c)
depicts the amplitude of the back Cu-W surface re
fl
ection from the
GDI across the scan area. Any abnormalities in the GDI that cause
excessive acoustic scattering or re
fl
ection would decrease the ampli-
tude of the back surface re
fl
ection. However, the amplitude of the
back surface re
fl
ection is about 57% ± 1% over the entire surface
and demonstrates excellent radial uniformity of the GDI.
C. GDI deployment
Experimental diagnostics have rarely been used to explore the
uniformity of a dynamic compression response in the radial direc-
tion because such measurements are easily a
ff
ected by lateral
release waves.
3
Here, we carefully designed an experiment to evalu-
ate radial uniformity using a large-diameter, thin target that keeps
lateral release waves away from the probed region. The results can
be used to evaluate the intrinsic uniformity of the drive provided
by the GDI. As noted above, the GDI used was typical of the
selected group of most uniform GDIs, with 30
μ
m bowing, 30
μ
m
side-to-side thickness variation, and 2.36 mm thickness, implying
thickness variations of up to 1.3% of the total GDI thickness. The
GDI diameter is turned down before mounting into the sabot; the
diameter reduction of about 20% suggests up to 1.1% thickness var-
iation across the
fi
nal
fl
yer plate.
The plot in
Fig. 11
shows the apparent particle velocity traces
from
fi
ve PDV probes located at 2, 3, 4, 5, and 6 mm from the
center of an Al-LiF target (see
Fig. 1
). All particle velocity traces
show the shock breakout, followed by velocity stabilization at about
2500m/s for about 200 ns because of the constant impedance Al
section at the front of the GDI. The particle velocity then rises to
about 3600m/s over another 200 ns. There is a minor release due to
the slight separation between the Al-Cu-W GDI and the Ta
backing, where there is a glue line, followed by a rise back to about
3700m/s. The particle velocity stabilized to a plateau for about
300 ns due to the constant impedance of the Ta plate glued onto
the back of the GDI, followed
fi
nally by target decompression. The
release wave from the glue layer is acceptable if the goal of the
experiment is achieved before the release occurs or if the release
does not directly a
ff
ect data of interest beyond the release.
However, in some applications, the glue release could a
ff
ect the
thermodynamic path and path-dependent variables. In such cases,
the release wave may be eliminated by di
ff
usion bonding rather
than gluing the constant impedance backing to the GDI (this
method has been used in other GDIs, not shown here). Since the
primary goal of this experiment is to test radial uniformity of the
compression ramp, it was not necessary to eliminate this release
wave from this shot.
Bastea
et al.
suggested that properly diagnosed PDV measure-
ment variations can be minimized by time corrections to the
FIG. 9.
(a) Height image of the back surface of an Al-Cu-W GDI with a 31.75
mm diameter, a side-to-side thickness variation of about 20
μ
m, and a bow
height of about 30
μ
m [the white arrow depicts the direction of maximum
side-to-side thickness variation, which causes the maximum convex bow height
(closed circle) to shift from the center (open circle)]. (b) A height image of a
GDI without a side-to-side thickness variation, but with a similar bow height,
shows that strategically placed probes at a constant radial distance from the
center could exploit the symmetry of this GDI to minimize geometric
trace-to-trace differences in PDV pro
fi
les.
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Published under license by AIP Publishing.
particle velocity traces.
34
Time shifts between PDV traces might be
due to GDI factors (nonuniform impedance, bowing, side-to-side
thickness variation, and tilt between projectile and target surfaces
due to sabot mounting or in-
fl
ight rotation), target factors (varia-
tions in thickness, nonplanarity), or diagnostic factors (cables car-
rying current to the recording oscilloscopes, etc.). Diagnostics are
designed or calibrated to minimize the timing o
ff
set and the target
thickness is usually controlled to be within 1
μ
m, so GDI and pro-
jectile factors are most likely responsible for timing o
ff
sets.
The maximum timing o
ff
set of the shock breakout between
the di
ff
erent particle velocity traces is 65 ns. This corresponds to a
linear distance of 250
μ
m based on the projectile velocity (3.85 km/s).
This distance is greater than the extent of side-to-side thickness varia-
tion or bowing within the GDI, which can account only for o
ff
sets of
about ±4 ns and indicates that tilt between the projectile and the
target surfaces due to sabot mounting and/or in-
fl
ight rotation is
most likely responsible for the timing o
ff
sets.
Figure 12(a)
depicts results from an analysis of projectile tilt.
Two of the probes yielded equal shock breakout times, each o
ff
set
by +10 ns from the average shock breakout time. We therefore
developed a model for tilt of a planar projectile with a tilt rotation
axis parallel to the line between these two probe locations.
Assuming that the timing o
ff
sets are due to a simple tilt of a planar
projectile only, we obtain the timing o
ff
set for each other point by
projecting parallel timing o
ff
set contours through those points (red
lines).
Figure 12(b)
shows that the measured timing o
ff
sets are
linear when plotted against the distance between the o
ff
set contours
in the assumed tilt direction. The strong correlation of the linear
fi
t
(R
2
= 0.998) suggests that indeed tilt is the primary cause for shock
breakout timing di
ff
erences. The slope of 5.37 ns/mm, for a
FIG. 10.
Ultrasonic (a) A-scan, (b)
B-scan, and (c) C-scan of an Al-Cu-W
GDI. The A-scan waveform measures
the acoustic time-of-
fl
ight between the
front and back surface re
fl
ections
(0.90
μ
s), which is consistent with the
expected transit time for the 2.36 mm
thick GDI. The B-scan demonstrates
that the waveform is consistent across
a grand diameter of the GDI with no
major internal re
fl
ections. The C-scan
plots the back surface re
fl
ected ampli-
tude in two dimensions, showing no
major internal scattering or re
fl
ections
from defects.
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J. Appl. Phys.
125,
145902 (2019); doi: 10.1063/1.5055398
125,
145902-11
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