Ultrathin aluminum sample cans for single crystal inelastic neutron scattering

M. B. Stone, M. J. Loguillo, and D. L. Abernathy

Citation: Review of Scientific Instruments 82, 055117 (2011); doi: 10.1063/1.3593374

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 REVIEW OF SCIENTIFIC INSTRUMENTS 82, 055117 (2011)

Ultrathin aluminum sample cans for single crystal inelastic

neutron scattering
M. B. Stone, M. J. Loguillo, and D. L. Abernathy
Neutron Scattering Sciences Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831, USA
(Received 24 March 2011; accepted 3 May 2011; published online 27 May 2011)
Single crystal inelastic neutron scattering measurements are often performed using a sample environ-
ment for controlling sample temperature. One difficulty associated with this is establishing appropri-
ate thermal coupling from the sample to the temperature controlled portion of the sample environ-
ment. This is usually accomplished via a sample can which thermally couples the sample environment
to the sample can and the sample can to the sample via an exchange gas. Unfortunately, this can will
contribute additional background signal to one’s measurement. We present here the design of an
ultrathin aluminum sample can based upon established technology for producing aluminum bever-
age cans. This design minimizes parasitic sample can scattering. Neutron scattering measurements
comparing a machined sample can to our beverage can design clearly indicate a large reduction in
scattering intensity and texture when using the ultrathin sample can design. We also examine the pos-
sibility of using standard commercial beverage cans as sample cans. © 2011 American Institute of
Physics. [doi:10.1063/1.3593374]

I. INTRODUCTION material relative to the mass of the can. In contrast, single

Neutron scattering is used for probing the excitations and
structure of materials.1 The utility of the neutron as a scat-
tering probe stems from its fundamental properties of mass,
nuclear spin, and a highly variable cross section as a function
of the scattering nuclei. The constant development of neutron
sources and neutron scattering instrumentation using neutron
beams since the conception of the technique is further testa-
ment to the usefulness of the neutron as a probe of materials.
For nearly all neutron scattering measurements, there is
a container for holding the sample in the neutron beam. This
container or sample can resides within a sample environment
which provides an additional independent variable to study
the material of interest.2 The sample environment may be a
furnace,3, 4 pressure-cell,5, 6 magnet,7, 8 cryostat,9, 10 etc., or a
combination of these.11 The sample can and sample environ-
ment also scatter neutrons and contribute to the measured
scattering intensity during an experiment. It is possible to
measure the scattering intensity of an empty sample can and
use this as a measure of the background for the measurement.
This is a reasonable approximation; however the empty can
measurement does not account for the absorption of the sam-
ple or multiple scattering events between the sample and the
sample can and sample environment. If the scattering inten-
sities from the empty can and sample environment are large,
then the subtraction technique will deteriorate the ratio of sig-
nal to noise. Furthermore, time and effort measuring an empty
sample can often be better spent examining other materials
with the neutron scattering instrumentation. A clear way to
improve the measurement is to reduce the cross section of the
sample can and sample environment through a proper choice
of materials and reducing the amount of these materials in
the neutron beam. Powder inelastic neutron scattering mea-
surements are often performed in small diameter aluminum
sample cans and often with a significant amount of sample
crystal measurements are very often sample mass limited, and
require much larger diameter cans to accommodate sample
mounting hardware. This paper focuses upon improving the
sample can used for single crystal inelastic neutron scattering
measurements.
II. DESIGN
There are two common choices of material used for con-
struction of sample cans for neutron scattering: vanadium
and aluminum. These are used because of their availability,
machinability, good thermal conductivity, and the specifics of
their cross sections. Aluminum has a relatively small cross
section compared to vanadium. For 1 Å neutrons the ratio of
the total scattering cross section is σ T (Al)/σ T (V) = 1.631 b
/ 7.925 b = 0.206 (1 b = 10−24 cm2 ).12 However, vanadium
has almost no coherent cross section σ coh (V) = 0.0184, σ inc
(V) = 5.08, σ coh (Al) = 1.495, and σ inc (Al) = 0.0082 b,
and thus has very little contribution from Bragg scattering,
making it especially useful as a sample can for structural
studies of powder materials.13 Figure 1 illustrates the mea-
sured integrated scattering intensity as a function of scatter-
ing angle (2θ ) for vanadium and aluminum normalized per
mole of material. While vanadium has a very smooth signal,
integrating the entire measured cross section indicates that
vanadium’s cross section is a factor of 1.33 times larger than
aluminum’s with a significant inelastic contribution. How-
ever, because the density of vanadium is 2.22 times that of alu-
minum, this measurement indicates that comparable sample
cans of vanadium will contribute a background which is ap-
proximately three times that of a comparable aluminum can.
Because of its smooth wave vector, Q, dependent cross sec-
tion vanadium sample cans are often used for neutron diffrac-
tion measurements, while aluminum cans are more often used
for inelastic neutron scattering measurements. Our focus is to

0034-6748/2011/82(5)/055117/5/$30.00 82, 055117-1 © 2011 American Institute of Physics

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 055117-2 Stone, Loguillo, and Abernathy Rev. Sci. Instrum. 82, 055117 (2011)

1
6
4
Intensity (arb. units / mol.)

0. 1
6
4

2
Aluminum
0.01
Vanadium
6
4

0 40 80 120
Scattering angle (deg.)

FIG. 1. (Color online) Scattering intensity plotted as a function of scattering

angle for a vanadium and aluminum sample. A machined aluminum can typ-
ically used for powder neutron scattering measurements (12.7 mm (0.5 in.)
inner diameter and 0.381 mm (0.015 in.) wall thickness) and a 6.35 mm
(0.25 in.) diameter vanadium rod were used for the measurement. Data have
been normalized per mole of material in the incident neutron beam. Data
are integrated for energy transfers between −50 and 50 meV. Measurements
were made using the ARCS instrument with an incident energy of 80 meV.

improve the sample can used for inelastic neutron scattering

measurements, thus we choose to focus upon the use of alu-
minum as a sample can material.
Our primary goal is to reduce the amount of aluminum in
the neutron beam while providing good thermal conductivity
to the sample. The thermal conductivity from the sample en-
vironment to the sample will be provided by an atmosphere
of helium exchange gas sealed within the sample can along
with the sample. Exchange gas sample cans for single crys-
tal inelastic measurements are typically cylindrical in shape
to provide a uniform background within a strong container.
Typical limits for machined aluminum wall thicknesses are
between 0.25 and 0.51 mm (0.01 and 0.02 in.) with increas-
ing difficulty as the height and width of the cylindrical sample
can increases. Another approach to achieving a thin-walled
aluminum vessel is to press the can from a single flat sheet
of aluminum. This “deep-draw” procedure is currently used
by the beverage industry to produce aluminum cans.14 Wall
thicknesses of 0.076 mm (0.003 in.) are typically used for
these cans, a factor of 3 to 7 times less than a typical ma-
chined sample can. Because of their availability, thickness,
and variety of sizes, we chose to base our sample can design
around the use of an aluminum beverage can.
Our can design incorporates a beverage can which has
been provided without interior or exterior varnish coatings or
a crimped top, known as “washer cans.” To this raw polished
aluminum can, we attach a machined aluminum flange. The
flange is carefully machined to tight tolerances such that a
mating re-sealable lid can be attached using machine screws
and an indium seal o-ring. Figure 2(a) shows a rendering of
our design with a sample holder mounted in the center of
the can.
We have tested two methods of attaching the can flange
to the can body. The simplest method is to use an epoxy
adhesive.15 Using this epoxy requires a gap of 0.051 mm to
0.076 mm (0.002 to 0.003 in.) between the flange and can
body. We find that joining reliability improves if both mating
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FIG. 2. (Color online) Our aluminum beverage exchange gas sample can
used for inelastic neutron scattering measurements of crystalline materials.
(a) Rendering of sample can with suspended post and plate mounted within
the can. Samples are typically mounted to such plates for measurements.
(b) Dimensioned cross section of our sample can design. (c) Expanded view
of the location of the interfaces between the can, the flange, and the lid. The
can is shown as a solid red line. The electron beam weld is located where the
can meets the flange at the top portion of the flange. The blue horizontal lines
are the location of indium grooves used for the indium o-ring seals.
surfaces are scuffed with a fine emery cloth and are wet with
epoxy before carefully assembling and baking at a tempera-
ture of 74 ◦ C for 2 h to cure the epoxy.
The second and preferred method requires a more com-
plicated machined flange and must be made from a compati-
ble aluminum alloy such as Al-5083. This method uses elec-
tron beam welding to fuse the flange to the aluminum can. A
detail of the interface is shown in Fig. 2(c). This process pro-
duces a flawless leak tight all-aluminum seam. This welding
process requires the use of an expanding mandrel inside the
can to prevent the can from shrinking away from the flange.
Additionally, the can flange inner diameter must be machined
oversized by no more than 0.025 mm (0.001 in.) of the can’s
outer diameter.
With this can assembly, we use a machined lid which can
be repeatedly sealed using an indium wire o-ring. There are
two indium wire o-rings, one in the lid of the can and one
located in the flange. These are illustrated in Fig. 2(c). We
find that placing indium in both of these positions distributes
indium over the electron beam weld and also the flange-lid
interface improving the sealing reliability of the can. The lid
has a 6.35 mm (0.25 in.) diameter socket used for suspend-
ing samples on an aluminum post into the beam center po-
sition. Using these cans with a helium exchange gas we reg-
ularly obtain leak rates less than 6.7 × 10−9 Pa m3 /s (5.0
× 10−8 torr-l/s) at pressures of 1.3 × 10−1 Pa (1 × 10−3 torr)
 055117-3 Stone, Loguillo, and Abernathy Rev. Sci. Instrum. 82, 055117 (2011)

as measured with a helium leak detector. Cans made using the
electron beam welding method have proven reliable to use re-
peatedly and have been in regular use for more than a year.
Typical measurements range between T = 4 K and T = 325 K
with the can suspended in a cryogenic vacuum of 2.6 × 10−4
Pa (2.0 × 10−6 torr).
III. MEASUREMENTS
Although readily available, commercial beverage (cb)
cans are often painted on the exterior and the interior is lined
with a food-grade hydrocarbon to prevent interactions be-
tween the can and the contents. We obtained unlined bever-
age cans direct from a can manufacturer. These washer-cans
or unlined beverage (ub) cans were pressed and washed, but
did not have any external paint, internal coating, or lid ap-
plied. We present here measurements comparing the cb and
the ub cans. We then present a comparison between a typ-
ical machined aluminum sample can (mac) (outer diameter
51.38 mm (2.023 in.) and wall thickness 0.28 mm (0.011 in.))
and our ub sample can.
Inelastic neutron scattering measurements were per-
formed using the wide Angular-Range Chopper Spectrome-
100
(a)
75
ω (meV)
ter (ARCS) at the Spallation Neutron Source at Oak Ridge
National Laboratory.16 This instrument is a direct geometry
time-of-flight neutron spectrometer. It measures scattering in-
tensity as a function of energy transfer, ¯ω, and wave vector
transfer, Q. The incident neutron beam of the instrument was
set to the fully open size of 50 mm wide by 50 mm tall (1.97
by 1.97 in.), and incident neutron energies of 60, 100, and
700 meV were used for the measurements. All data shown
were acquired at room temperature.
Figure 3 illustrates the measured scattering intensity17 as
a function of energy and wave vector transfer for the cb can
(a) and the ub can (b) for an incident energy of 100 meV. The
data in Fig. 3(b) clearly shows the aluminum phonon spec-
tra; although in (a) this spectra is obscured by a large scat-
tering intensity due to the organic molecule coating the in-
terior of the commercial can. Hydrogen has a large neutron
cross section σ T (H) = 82.353 barns. The molecule coating
the interior of the cb can is very likely a polycarbonate resin
with both CH3 and OH groups. The large hydrogen cross sec-
tion (both elastic incoherent and inelastic vibrational modes)
is thus overwhelming the signal due to the aluminum lattice
excitations. Figure 3(c) illustrates the wave-vector integrated
scattering intensity for these two samples for an incident en-
ergy of 700 meV. Here one can clearly see two higher energy
modes. These are most likely a stretching CH3 –C mode at
172(2) meV and an OH stretching mode at 370.1(7) meV.18
Clearly, a cb can is not appropriate for neutron scattering mea-
surements.

50
Figure 4 shows the measured scattering intensity for a
25 typical machined aluminum sample can (a) and our ub can (b).
0
These data were acquired with an incident energy of 60 meV.

-25
100
(b) 0.01
(a)
75
40
0.005
ω (meV)

50
20
ω (meV)

25 0
0 0

-25
-20
0 4 8 12
-1
Q (Å ) -40
(b) 0.02
0.012
(c) 40
Intensity (arb. units)

unlined can 0.01

20
ω (meV)

0.008 commercial can

0 0

0.004
-20

0 -40
-600 -400 -200 0 200 400 600 0 2 4 6 8 10 12
-1
ω (meV) Q (Å )

FIG. 3. (Color online) Inelastic neutron scattering measurements of an (a)
commercial beverage can (cb) and a (b) unlined beverage can (ub). Spectra
from the ub and cb can were measured with an incident energy of 100 meV.
Both panels are shown on the identical intensity scale. (c) Wave- vector in-
tegrated scattering intensity of the ub and cb can measured with an incident
energy of 700 meV.
FIG. 4. (Color online) Inelastic neutron scattering spectra of the (a) ma-
chined aluminum can (mac) and (b) unlined beverage can (ub) sample can
as a function of energy and wave vector transfer. Measurements were per-
formed with an incident energy of 60 meV using the ARCS instrument as
described in the text. Color bar in panel (b) indicates intensity scale of the
two measurements.

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 055117-4 Stone, Loguillo, and Abernathy Rev. Sci. Instrum. 82, 055117 (2011)

(a) (111) 2 θ=22.4±0.7 deg.

-1 2
10 4 (c)
Ψ

Q (Å )
-1
Intensity (arb. units)

0
-2
10 3

-2
-4 -2 -1
0 2
10
-3 2 Q (Å )

Machined can

Intensity (arb. units)

Unlined Beverage can
10
-4 1

-40 -20 0 20 40
ω (meV) 0
(b) (002) 2 θ=25.9±0.7 deg.
FIG. 5. (Color online) Intensity as a function of energy transfer for the two machined can
sample cans: the machined aluminum sample can and the unlined beverage unlined beverage can
can sample can. Data correspond to inelastic neutron scattering spectra shown 1.5
in Fig. 4 integrated between Q = 4 and 6.5 Å−1 . Note that the vertical axis is
a logarithmic scale.

1.0

Both measurements clearly show the nuclear Bragg peaks at

the ¯ω = 0 position, and the phonon excitations for both
neutron energy gain (¯ω < 0) and neutron energy loss (¯ω
> 0). These data are normalized to the incident flux of neu-
trons and thus represent a true comparison of the background
for using these two different sample cans. Figure 5 shows
the wave-vector integrated scattering intensity based upon
the data shown in Fig. 4. Again, both spectra show the alu-
minum phonon density of states extending out to ∼38 meV.
The offset between the two measurements is essentially mul-
tiplicative; scaling with the mass of each can. The machined
can has approximately a factor of three times more scattering
intensity. Figure 6 shows the intensity as a function of wave
vector transfer for these two sample cans. The ratio of the
thicknesses of the machine sample can and the ub can is ∼3.7,
and the ratio of the total integrated scattering intensity for the
two measurements shown in Fig. 4 is 2.8. The machined sam-
ple can has broader nuclear Bragg peaks than the ub can, for
0.5
0
0 45 90
Ψ (deg.)
FIG. 7. (Color online) Characterization of sample can texture for both mea-
sured sample cans: the machined aluminum sample can and the unlined bev-
erage can sample can. Data were acquired using an incident neutron energy
of 100 meV using the ARCS instrument as described in the text. The data
have been integrated between energy transfers of ¯ω = −1 and 1 meV. Panel
(a) shows the scattering intensity of the (111) aluminum Bragg peak as a
function of azimuthal angle . Panel (b) shows the scattering intensity for
the (002) aluminum Bragg peak. Panel (c) shows the scattering intensity of
the machined sample projected onto the cylindrical detector geometry of the
ARCS instrument. The horizontal and vertical axes are in Å−1 , and the angle
 is defined in panel (c). Higher scattering intensities are shown as darker
shades of gray. Solid lines in (a) and (b) are simple Gaussian fits to further
illustrate the texture measurement.

10
Machined can example, in the vicinity of Q = 2.5 Å−1 . There also appears
Unlined Beverage can to be additional Bragg peaks near Q = 4.0 and 5.8 Å−1 . These
Intensity (arb. units)

broader and potentially additional structural peaks may be a

1 consequence of the alloy used to produce the mac (6061-T6)
0.1
0.01
0 2 4 6
Q (Å )
-1
FIG. 6. (Color online) Intensity as a function of wave vector transfer for the
two sample cans: the machined aluminum sample can and the unlined bev-
erage can sample can. Data correspond to inelastic neutron scattering spectra
shown in Fig. 4 integrated between ¯ω = −0.5 and 0.5 meV. Note that the
vertical axis is shown using a logarithmic scale.
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compared to the alloy used for the ub can (3xxx series).
The large detector coverage of the ARCS instrument,
allows us to characterize the texture of the nuclear Bragg
peaks for both cans. Figure 7 shows data corresponding to
a texture measurement for Ei = 100 meV. Figure 7(c) shows
the first several powder rings of aluminum. These are, from
smallest to largest Q, the (111), (002), (220), (311) etc. nu-
8 10 clear Bragg peaks. The angle  is the angle between the in-
strument horizontal, and the detector of interest:  = 90o
corresponds to the detectors located above the Q = (0, 0)
position in Fig. 7(c). We integrate the scattering intensity
for the (111) and (002) Bragg peaks and plot this scatter-
ing intensity as a function of  in Figs. 7(a) and 7(b), re-
spectively. Once again, the scattering intensity due to the
 055117-5 Stone, Loguillo, and Abernathy
unlined beverage can is less than the machined can. The an-
gular dependence of the (111) peak is very similar for these
two cans, c.f. Fig. 7(a). However, the angular dependence of
the (002) peak is quite different, c.f. Fig. 7(b). There are two
peaks in the texture measurement of the machined sample can,
and only one significant texture peak in the measurement of
the unlined beverage can.
IV. CONCLUSIONS
We have designed and constructed a re-sealable ultrathin
aluminum exchange gas sample can based upon the unlined
aluminum beverage can. These cans are especially useful for
inelastic neutron scattering measurements of single crystal
samples. We find that the commercial beverage cans are not
appropriate for this purpose because of the large scattering
cross section of the interior liner of the can. We also made
comparisons to a typical aluminum sample can produced from
machining a solid piece of aluminum. In addition to the added
background due to the greater mass of material in the ma-
chined can, there were additional structures in the texture of
the machined aluminum can and its diffraction pattern. Based
upon the amount of scattering intensity and the reduction in
texture, the ub can is an excellent choice of material to build a
single crystal exchange gas can. We are currently developing
a single axis goniometric mount which will be built into the
interior lid of our can. We are also planning on adding electri-
cal feedthroughs to the lid of the can. This will allow one to
mount a thermometer within the exchange gas and provide a
more accurate measure of sample temperature. One may also
use these feedthroughs for simultaneous electrical19 or ther-
mal transport measurements or application of electric fields
or light to the sample being measured in the neutron beam.
ACKNOWLEDGMENTS
The authors would like to thank John Brock and Dwayne
Griffith of the machine shop at Oak Ridge National Labora-
tory (ORNL); K. Herwig for suggestions concerning adhe-
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Rev. Sci. Instrum. 82, 055117 (2011)
sives; Alan Fredrick and Roger Miller at the ORNL Materi-
als Joining Lab; and the Custom Can sales department of the
Ball Corporation of America. This Research at Oak Ridge Na-
tional Laboratory’s Spallation Neutron Source was sponsored
by the Scientific User Facilities Division, Office of Basic En-
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