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Characterization of shielding materials used in neutron

scattering instrumentationI

M. B. Stone∗
Neutron Scattering Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831,
USA

L. Crow∗
Neutron Technologies Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee
37831, USA

V. R. Fanelli∗
Neutron Scattering Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831,
USA

J. L. Niedziela∗
Nuclear Nonproliferation Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee
37831, USA

Abstract

The nuclear cross-sections of certain isotopes make some materials excellent


candidates for neutron shielding. We have performed a series of measurements
examining the transmission, reflection, and nuclear Bragg scattering of a series of
common materials used for neutron shielding. We concentrate on characterizing
the materials most likely to be used in neutron scattering instrumentation.
Keywords: Neutron absorption, Thermal neutron cross sections, Neutron

I This manuscript has been authored by UT-Battelle, LLC under Contract No. DE-

AC05-00OR22725 with the U.S. Department of Energy. The United States Government
retains and the publisher, by accepting the article for publication, acknowledges that the
United States Government retains a non-exclusive, paid-up, irrevocable, world-wide license
to publish or reproduce the published form of this manuscript, or allow others to do so, for
United States Government purposes. The Department of Energy will provide public access to
these results of federally sponsored research in accordance with the DOE Public Access Plan
(http://energy.gov/downloads/doe-public-access-plan).
∗ Corresponding author

Email address: stonemb@ornl.gov (M. B. Stone)

Preprint submitted to NIM: A August 28, 2019


powder diffraction, Inelastic neutron scattering

1. Introduction

Understanding effective neutron absorbing materials has been a pursuit since


Chadwick surmised and demonstrated the existence of the neutron.[1, 2] Indeed
the large nuclear cross-section of hydrogen played a key role in the discovery.[3]
5 Exploration of materials specifically for moderation, reflection, and absorption
of neutrons would all be made in the second half of the twentieth century as the
study of the neutron and its interaction with matter developed.[4] One result
of this effort was the construction and operation of the X-10 Graphite Reactor
at Oak Ridge National Laboratory. It was built as a pilot reactor during the
10 Manhattan Project for the production of transuranic material. With several
scientific missions developing after the war, the X-10 reactor became one of the
incubators for the new field of neutron scattering.[5]
An early publication concerning the neutron scattering instruments at the
X-10 reactor includes descriptions of the neutron absorbing materials used to
15 improve measurements: plastic impregnated with boron carbide for beam defin-
ing slits and a series of 0.010 inch thick cadmium sheets for an incident beam
collimator.[6] In fact, this instrument was used to measure the energy dependent
cross-sections of materials. Such measured and calculated cross-sections assem-
bled since the 1940s are now available in tabulations in on-line databases.[7]
20 Figure 1 shows a series of calculated total neutron cross-sections as a function
of energy and wavelength. The total cross-section, σTotal is a sum of the total
scattering, σS , and absorbing, σabs. , neutron cross-sections. The total scattering
cross section is the sum of the incoherent, σI , and coherent, σC , nuclear cross
sections:

σTotal = σS + σabs. (1)

σTotal = σI + σC + σabs. . (2)

25 For slow neutrons, the absorption cross-section is typically inversely propor-


tional to the neutron velocity. Cross-sections in Fig. 1 are shown for typical

2
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Figure 1: Cross-section of common elements and isotopes used for neutron absorption. Cross-
sections, shown in units of barns (10−24 cm2 ), are obtained from Ref. [7]. Unless noted, these
calculations are for the material with its natural abundance of isotopes. Temperature values
on top axis are located at the energy of the peak of the probability distribution of neutrons
moderated at the given temperature.

isotopes and elements used for absorbing materials in neutron scattering instru-
mentation. Non-relativistic neutron energies are inversely proportional to the
81.81
square of the neutron wavelength: E = λ2 where E is in units of meV and λ
30 is in units of Ångstroms. We also show calculations for hydrogen, carbon and
aluminum. Unless otherwise noted, these calculations are for the material with
its natural abundance of isotopes taken into consideration.
Neutron scattering instruments are used to examine the properties of materi-
als with neutron wavelengths between approximately 0.25 and 8 Å.[8, 9] Neutron
35 scattering measurements most often consist of samples of materials mounted to
sample environment equipment which provides temperature control and/or con-
trol over other external parameters such as magnetic field or pressure.[10] The
neutrons for the experiment are generated in a reactor or spallation based neu-

3
tron source. A beam of monochromatic neutrons or a wide wavelength band
40 of neutrons is used to irradiate the sample. The resulting scattered neutrons
are then counted by neutron detectors as a function of their final direction and
energy. From these measurements, one can determine the structure or dynamic
properties of the samples that were placed in the neutron beam.
Shielding and masking neutrons in the incident and scattered beams is done
45 to reduce the background of the measurements in order to improve measure-
ment quality. Biological shielding is also used in these instruments to shield the
personnel working in the vicinity of the neutron beams from radiation due to
the neutron source or from the prompt gamma radiation produced by neutrons
interacting with the sample or other instrument components. This manuscript
50 does not consider the design of biological shielding. Rather, this manuscript
quantifies the use of practical shielding materials within neutron scattering in-
struments. A similar manuscript concentrated on the properties of materials
used for SANS instrumentation.[11] Absorbing materials may be used in the di-
rect beam of neutrons to define beam geometry or they may be used to provide
55 incident beam collimation.[12] They may also be used in the vicinity of samples
to shield the instrument from measuring multiple scattering effects within com-
plicated sample environments. Scattered neutron beams can also be shielded
or collimated using neutron absorbing materials to reduce the background from
sample environments and multiple scattering.[13]
60 Although one can use tabulated wavelength dependent nuclear cross-sections
to calculate a materials absorption, the reflective properties or albedo of com-
posite materials or elemental absorbers are not as easy to predict. This can lead
to unintended consequences in neutron scattering measurements. For example,
one may use a very good neutron absorber in a furnace sample environment.
65 Materials may absorb neutrons and not melt at high temperatures, but there
may be a number of nuclear Bragg peaks which may be present in the back-
ground of the shielding material. Alternatively, neutron shielding may be placed
in a cryostat sample environment in locations that would potentially impact the
cooling power of the cryostat depending upon the thermal properties of the ab-

4
70 sorber. Other issues can arise when absorbers are used at instruments that
operate over a large range of neutron wavelengths. Measurements employing
gadolinium oxide paint as shielding with neutron energies less than 20 meV
will be potentially well shielded. However, when extending these measurements
to 200 meV the absorption cross-section of gadolinium quickly decreases and a
75 hydrogenous binder in these paints can cause the background to dramatically
increase. A recent survey of adhesives used in sample mounts for neutron scat-
tering has also been completed.[14] The authors provide an excellent reference
in order to determine which adhesives are most appropriate to use in a mea-
surement. To help guide choices and avoid unintended consequences of shielding
80 materials in the vicinity of neutron scattering instrumentation, we provide here
a series of measurements examining commonly used materials in neutron scat-
tering facilities and instrumentation. Measurements are shown for transmission
and reflection geometries at fixed values of neutron wavelength for a large range
of scattering angles. Transmission of some of these materials is also measured
85 as a function of neutron wavelength.

2. Experimental Techniques

A series of samples were measured using the CG1B beam line at the High
Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL). The
samples all had a flat plate geometry with a length and width of approximately
90 50 mm. The thickness of the samples varied between the materials measured,
however a thickness dependence was not characterized in these measurements.
Details of the samples composition and thickness are listed in Table 1. Mea-
surements were also performed using the SEQUOIA chopper spectrometer at
the Spallation Neutron Source (SNS) at ORNL.

95 2.1. Materials

Table 2 lists additional properties of some of the traditional materials used


for shielding in neutron scattering instrumentation. We use the inorganic crystal

5
structure database[15] to determine the three strongest Bragg peaks for these
materials. The melting point is also listed because materials may be placed in
100 high temperature sample environments. We also calculate the thickness value to
absorb 99.75 percent of the neutrons, z3σ (E), for three commonly used energies
in neutron scattering instruments. Scattering cross-sections are not included in
the calculation of absorption. These values are calculated by considering the
absorption of neutrons following the Beer-Lambert law,

−z
A = 1 − exp( ), (3)
δp

105 where A is the fraction of neutrons absorbed, z is the thickness of the material,
and δp is the penetration depth due to absorption. The penetration depth can
be determined in terms of the unit cell volume, V , the absorption cross section
per formula unit, σabs./f.u. , and the packing fraction ,

V
δp = . (4)
σabs./f.u. 

For solid materials, the packing fraction is  = 1. For powder samples the
110 packing fraction can be between approximately 0.25 and 0.8 depending upon
the particle size distribution of the system being studied. The absorption cross-
section per formula unit is assumed to be proportional to the inverse of the
neutron velocity. This corresponds to the linear portions of the data shown in
q
Fig. 1. This velocity dependence results in a EEm term in the absorption cross-
115 section per formula unit where Em is the energy at which the nuclear absorption
cross section is tabulated or calculated, and E is the neutron energy at which
one is calculating the absorption cross-section such that,
r
Em X
σabs./f.u. = σabs.n , (5)
E n

where the summation is over the n nuclei in the unit cell and σabs.n is the
tabulated absorption cross section of the nuclei in dimensions of area.[16] Prior
120 to detailed discussion of individual materials, we note that the decay prod-
ucts from the neutron absorption should also be considered in any shielding

6
design. Gamma ray and other decay products are potential byproducts of neu-
tron absorption. High energy prompt production of gamma rays are especially
concerning if the instruments neutron detectors are sensitive to gamma radi-
125 ation. Another concern is the generation of gamma radiation areas and their
potential impact on personnel. Online databases are available for the prompt
gamma spectra of individual isotopes.[17]
Materials with boron content have the potential to be good shielding ma-
terials. These materials are often enriched to increase the abundance of the
10
130 highly absorbing boron-10, B, isotope relative to the other isotopes. Figure 1
illustrates that borated materials are especially useful in shielding neutrons with
energies above approximately 200 meV. Boron nitride, BN, is sometimes used for
neutron shielding. Because of its structure and its lubricant properties, boron
nitride is sometimes referred to as white graphite. It is able to be machined
135 into simple parts, but it is brittle. Machining should be done with care because
of the slippery environment the swarf produces. Borated aluminum (B-Al) is
typically made from 1100 alloy Al with 10 B incorporated. The starting material
is available in sheets or plates. Several manufacturers provide this material with
varying percentages of boron content. The 1100 alloy version of B-Al should not
140 be considered as a structural material. Borated polyethelene is available from
several manufacturers. The standard color of this material is green. It is usually
available in large sheets with a 5% natural boron content. Other grades and
boron levels of this material are available from vendors. It is easy to machine
and cut into shapes. Lithiated polyethelene is also available commercially, but
145 this product was not tested in the present study. Boron carbide (B4 C) is avail-
able in several formats. Boron carbide is typically sold as a powder industrial
abrasive. RBBC refers to reaction bonded boron carbide. This material is a
ceramic composite of B4 C and Si that is used in armor applications.[18] It is
available in limited shapes and is difficult to cut or machine. CBBC (carbon-
150 bonded boron carbide) is the starting material that is made before the reaction
process is performed to produce RBBC. CBBC is available in limited shapes,
typically sheets. It is brittle, abrasive, and friable. ZHIP stands for zero hy-

7
drogen in product. It is a boron carbide based composite material made with a
non-hydrogenous binder. It is most often used in rectangular sheets with a thin
155 aluminum backing to provide structural support. Curved and custom shapes
are available from a very limited number of manufacturers. ZHIP is often used
to line neutron scattering instrument vacuum tanks with neutron shielding.[19]
Cadmium and gadolinium foils are often used as shielding materials for
neutrons in the vicinity of sample mounts. Although inexpensive and easily
160 malleable or cut into shapes, cadmium produces high energy gamma radiation
upon absorption of a neutron. This is an additional biological shielding issue
and an issue for detectors that have a significant gamma sensitivity. The use
of cadmium as a neutron absorber may therefore be restricted depending upon
the configuration of the beams in the instrument and the biological shielding in
165 place. The prompt gamma produced by cadmium when it absorbs a neutron can
also lead to the generation of additional neutron background radiation. This
was recently documented at a neutron scattering beamline. The high energy
gamma radiation from the cadmium interacted with beryllium components via
a photoneutron process to generate an additional fast neutron background.[20]
170 Another difficulty in using cadmium is its toxicity and high vapor pressure. Cad-
mium should be avoided in high vacuum environments at elevated temperatures.
Gadolinium foil is much more expensive than cadmium (approximately 8 to 13
times), although gadolinium oxide paints have been used in small quantities for
shielding complicated sample mounts. Gadolinium and cadmium are available
175 from chemical and industrial suppliers as sheets with a range of thicknesses and
purity levels.
The high density concrete (HCONC) and concrete (CONC) examined in
this study are samples of concrete produced at the Spallation Neutron Source
at ORNL. The HCONC here has a hematite aggregate (nonmagnetic iron ore)
180 chosen for its high atom density. The resultant density of the HCONC is 3.92
g/cm3 . The CONC is a standard sand aggregate concrete used for structural
purposes at SNS. It conforms to Standard Specification for Concrete Aggre-
gates ASTM 33 and has a density of 2.3 g/cm3 . These materials are typically

8
used for biological shielding around neutron scattering instruments and rarely
185 placed in the vicinity of the direct neutron beam. Polyethylene (HDPE) is a
a high proton density plastic that is sometimes used in the vicinity of neutron
instrumentation. The aluminum alloy examined in this study (6061) is very
commonly used in manufactured parts or cryostats that are used with neutron
scattering instruments.
190 Sometimes absorbing coatings are applied to structural materials to provide
some neutron shielding. We examine Coraflon coatings mixed with boron car-
bide powders. Coraflon is a commercial fluoropolymer that can be rolled or
brushed onto surfaces to provide a lower hydrogen content coating that incor-
porates boron carbide material. Boron nitride is also available in an aerosol with
195 proprietary binder materials. These products are often used for mold releases
or lubricant applications. We applied a layer of this material to an aluminum
substrate to test the neutron absorbing properties of this product. Paints and
coatings as absorbers can sometimes be problematic due to flaking and deterio-
ration with age. This should be considered prior to application of such material.
200 Lithium carbonate (Li2 CO3 ) can also be combined with Coraflon to provide a
shielding material that can be painted.
Flexible sheets of boron carbide in silicone (Bflex) [Shieldwerx 238] provide
a relatively low hydrogen content material that is commercially available. The
same manufacturer has also produced a custom material with 6 Li2 CO3 in sili-
205 cone (LiSiO). Lithium-6 carbonate or boron carbide powder in an epoxy (LiEP
and B4 CEp respectively) may be cast into simple shapes. The commercial epoxy
used for this purpose is Stycast W-19 red with catalyst 9. The LiEP is useful
for neutron shutters and beamstops in instrumentation that has detectors that
are highly gamma sensitive. The lithium-6 (n, alpha) absorption produces very
210 few gamma rays. The B4 CEp product is often cast to make masks and other
shielding pieces.

9
Table 1: Table of samples measured, their thickness (t), and the corresponding instrument
used for the measurement.
Material t (mm) instrument
BN 3.29 CG1B, SEQ
Borated Aluminum (B-Al)a 1.16 CG1B, SEQ
b
Borated Polyethelene (B-HDPE) 25.4 CG1B, SEQ
B4 C (CBBC) 7.94 CG1B
B4 C (RBBC) 2.2 CG1B, SEQ
B4 C (ZHIP) 12.8 CG1B
c
Gd foil 0.1 CG1B, SEQ
Cd foild 0.4 CG1B, SEQ
High Density Concrete (HCONC) 25.4 CG1B
Concrete (CONC) 25.4 CG1B
Polyethylene (HDPE) 10.6 CG1B
Aluminum-6061 (thin plate) 1.74 CG1B
Aluminum-6061 (thick plate) 5.19 SEQ
Borated coraflon(1 layer) on Ale 0.14 SEQ
e
Borated coraflon(3 layers) on Al 0.42 SEQ
BN paint on Alf 1.74(Al)/0.05(coating) SEQ
Lithiated coraflon on Al 1.44(Al)/0.2(coating) SEQ
Bflex 3.2 CG1B
LiSiO 3.2 CG1B
Li2 CO3 in epoxy (LiEP) 6.4 CG1B
B4 C in epoxy (B4 CEp) 6.4 CG1B

a 10
4.5% B in 1100 Al.
b
5% borated
c
Alfa Aesar 99.9%
d
Alfa Aesar 99.997%
e
Fine B4 C powder mixed with coraflon and painted onto a 5.19 mm thick
6061-Al substrate
f
BN lubricant in aerosol form sprayed onto a 1.74 mm thick 6061-Al sub-
strate
10
Table 2: Table of material properties for select neutron absorbers and materials used in
neutron scattering instrumentation. Q values are wave-vectors of the first three most intense
nuclear Bragg peaks and their indices for Q < 7 Å−1 , MP is the melting point, and z3σ is the
thickness of material required to absorb 99.75% of incident neutrons. Scattering effects are
not included in this calculation. Boron nitride (BN) has a hexagonal structure with lattice
constants a = b = 2.504 Å, c = 6.6612 Å, α = β = 90◦ , and γ = 120◦ .[21] Boron carbide (B4 C)
has a hexagonal structure with lattice constants a = b = 5.61 Å, c = 12.14 Å, α = β = 90◦ ,
and γ = 120◦ .[22] Gadolinium (Gd) has a hexagonal crystal structure with lattice constants
a = b = 3.63 Å, c = 5.78 Å, α = β = 90◦ , and γ = 120◦ .[24] Cadmium (Cd) has a hexagonal
crystal structure with lattice constants a = b = 2.972 Å, c = 5.605, α = β = 90◦ and
γ = 120◦ .[25][26] Aluminum (Al) has a face-centered-cubic structure with lattice constants
a = b = c = 4.0975 Å.[35]. Vanadium (V) has a body-centered-cubic structure with lattice
constants a = b = c = 3.026 Å.[27] Copper (Cu) has a face-centered-cubic structure with
lattice constants a = b = c = 3.615 Å.[28] Li2 CO3 has a monoclinic structure with lattice
constants a = 8.359, b = 4.974, c = 6.194, Åand β = 114.79◦ .[29]
Compound Q (Å−1 ), (H K L)) MP (K) z3σ (3.5, 14.6, 81 meV) (mm)
BN 1.887 (0 0 2), 5.361 (1 1 2), 6.279 (1 1 4) 1663a 0.53, 1.08, 2.55
b
B4 C 2.638 (0 2 1), 4.290 (1 2 5), 4.480 (2 2 0) 2763 0.27, 0.55, 1.29
10
B4 Cc 0.06, 0.12, 0.29
Gd 2.273 (0 1 1), 4.085 (1 1 2), 5.393 (1 2 1) 1586 0.02, 0.03, NAd
Cd 2.437 (0 1 0), 3.310 (0 1 2), 2.239 (0 0 2) 594 0.19, 0.39, NAd
Al 2.687 (1 1 1), 5.146 (1 1 3), 4.388 (0 2 2)e 933 1600, 3300, 7800
V 2.936 (0 1 1), 1.235 (1 1 2), 6.566 (0 1 3) 2183 60, 120, 290
f
Cu 3.010 (1 1 1), 4.916 (0 2 2), 5.765 (1 1 3) 1358 70, 140, 340
Li2 CO3 1.510 (1 1 0), 2.393 (1 1 2), 2.235 (0 0 2) 996 9.3, 19, 45
6 g
Li2 CO3 0.78, 1.6, 3.7

a
BN sublimes at elevated temperatures.[30, 31, 32]
b
Above 1200 C oxidation weakens B4 C.[23]
c 10
Calculated with 90% of
B atoms.
q
d Em
Gd and Cd no longer have a E relationship in the absorption cross section above approxi-

mately 50 meV.
e
Additional aluminum peaks at low-Q are 3.103Å−1 (0 0 2), 6.763Å−1 (1 3 3), and 6.939Å−1 (0 2
4).
f
Additional copper peaks at low-Q are 3.476Å−1 (0 0 2), 6.021Å−1 (2 2 2), and 6.952Å−1 (0 0 4)
g
Calculated with 90% of 6 Li atoms. 11
2.2. Instrumentation
The CG1B instrument is a fixed wavelength (λ = 2.417 Å, Ei = 14.0 meV)
neutron diffractometer. Measurements were performed with the incident beam
215 defined by a 25.4 mm high and 6.35 mm wide slit before the sample position.
A 38.1 mm high and 6.35 mm wide boron carbide and epoxy beam mask was
placed 337 mm after the sample position. This was followed by a rectangular
cross section (95.3 mm high by 50.8 mm wide) 200 mm long borated aluminum
tube. A 24.4 mm by 25.4 mm opening in a boron carbide mask followed the
220 borated aluminum tube. A 149 mm long forty minute soller collimator was
placed 34.9 mm after the second mask. The CG1B detector was placed 810 mm
from the sample position. Additional ZHIP mix shielding was placed on the
sides of the incident beam and on the high angle side of the neutron detector to
reduce ambient background signal at larger scattering angles.
225 The scattering angle, 2θ, and the sample angle, θ, are able to be indepen-
dently adjusted with the CG1B instrument. Figure 2(a)-(b) illustrates these
angles and the two configurations of the instrument used for measurements. Ki
and Kf are the incident and final scattering vectors. S is the plate geometry
sample, 2θ is the scattering angle, θ is the orientation of the sample relative to
230 the incident beam, C is a collimator placed in front of the detector D for the
CG1B measurements. Figure 2(a) shows a sample being measured in reflection
(r), and Fig. 2(b) shows a sample being measured in transmission (t). Three
standard scans were measured for each sample. A θ − 2θ scan was measured in
transmission and reflection for 2 ≤ 2θ ≤ 90 degrees, and a θ scan was measured
235 with the scattering angle fixed at 90 degrees, i.e. a rocking curve. Higher point
density θ − 2θ scans were performed for some samples in the vicinity of the
calculated intense nuclear Bragg peak position for the sample for λ = 2.417 Å
neutrons.[15] To account for any variations of neutron flux from the reactor
source during the course of the measurement, the CG1B data were normalized
240 to the number of neutron counts measured in an incident beam monitor placed
upstream of the incident beam defining slits.
Additional measurements were made at SEQUOIA. SEQUOIA is a fine reso-

12
(a) S
Ki T
2T
Kf
C
D
(b) S
Ki T 2T
Kf
C
D
(c) D
S
Ki Kf
M1 M2

(d) Kf D
S 2T
Ki
M1 M2

Figure 2: Overview of measurements performed using the CG-1B diffractometer and the
SEQUOIA spectrometer. (a) Representation of the reflection geometry used in θ − 2θ scans
at CG1B. (b) Representation of the transmission geometry used in θ − 2θ scans at CG1B.
(c) Representation of the geometry used in the SEQUOIA transmission measurements. (d)
Representation of the geometry used in the SEQUOIA diffraction measurements. Ki and Kf
are the respective incident and final wave-vectors. S is the sample location. θ and 2θ are the
orientation of the sample and scattering angle, respectively. C is a collimator placed in front
of the detector D for the CG1B measurements. D represents the detector location(s). M1
and M2 are beam monitor locations at the SEQUOIA instrument.

13
lution thermal chopper spectrometer located at beamline 17 of the SNS.[33, 19]
The instrument most often operates by using a Fermi chopper to prepare a
245 monochromatic beam of incident neutrons on the sample. Neutron detectors
are arranged in a cylindrical configuration concentric with the sample position
for the primary purpose of performing direct-geometry spectroscopy measure-
ments. There are also two beam monitors at the instrument. One is located
in the incident beam between the Fermi chopper and the sample position, M1 ,
250 18.23 m from the moderator. The second one, M2 , is located in the beam-
stop (29 m from the moderator location) downstream from the sample position.
Transmission measurements, Fig. 2(c), were performed by removing the Fermi
chopper from the incident beam with the T-zero (prompt neutron) chopper
parked in the open position. M1 and M2 represent the beam monitors located
255 in the incident and transmitted neutron beam. The detectors D are arranged in
a cylindrical geometry around the sample position. This configuration of the in-
strument uses the entire spectrum of neutrons provided by the water moderator
of the beamline. Data presented here were normalized to the amount of pro-
ton charge on the target of the SNS during the measurement. Wide-bandwidth
260 diffraction measurements are able to be extracted in this configuration using
the detectors at finite scattering angles as shown in Fig. 2(d).

3. Results

We describe here the measurements performed at the CG-1B and SEQUOIA


instruments examining a series of neutron absorber materials. We first present
265 the angle dependent measurements performed using CG-1B, and then we ex-
amine the transmission and diffraction measurements at SEQUOIA.

3.1. Monochromatic measurements from CG-1B

Figure 3 illustrates θ − 2θ scans for no sample present, the Cd sample in


transmission and reflection geometries, and a measurement with the incident
270 beam blocked by a thick piece of boron carbide. The beam blocked data is a

14
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*@76,*A:%5B7>
*$>*=8?
*$>*=(?

.'-,*+*)('&%$
"!! *C%*)6,D:7

#!!

!
! #1 ! 31 2! 01 /!
456((78-'9*6'9:7;*"<*=>79.?

Figure 3: θ − 2θ scans with no sample, the cadmium (Cd) sample in a reflection (r) and
transmission (t) geometry, and measurements without a sample. The no sample data were
acquired with no sample present in the instrument, and shows the angular dependent air
scattering. The beam blocked data were acquired with a half inch thick boron carbide mask
covering the incident beam. Measurements were made using the CG-1B diffractometer with
λ = 2.417 Å, Ei = 14.0 meV, neutrons.

measure of the angular dependent background, also called the room background.
The no sample measurement illustrates the angular dependent air scattering
present at the instrument. The Cd measurements substantially reduce this air
scattering (at low 2θ values). The transmission measurement of Cd reduces
275 the air scattering contribution more than the reflection measurement. Both the
transmission and reflection measurements agree very well with one another for
scattering angles greater than thirty degrees.
Figure 4 shows the angular dependence of the scattering intensity as the
Cd sample is rotated with the scattering angle fixed at 2θ = 90 degrees. Not
280 surprisingly, there is no angular dependence in the no sample data. There is a
small peak at θ = 0 degrees in the Cd measurement. We fit this data to a simple
Gaussian function with the peak fixed at θ = 0. This small peak is due to the
increase in air scattering when the thin Cd sample is oriented longitudinal to
the incident beam. These orientations are illustrated in the insets of Fig. 4. The
285 value of the beam blocked data at 2θ = 90 degrees is also shown as a dashed line

15
150
ș 
No sample &G
%HDPEORFNHG

Counts / min.
100

50
Ki T= 0 Ki T= 90
Kf Kf

0
0 45 90 135
6DPSOHDQJOHș GHJ

Figure 4: θ scan of the cadmium (Cd) sample. The value of 2θ was fixed at 90 degrees. The
solid line through these data are a fit to a constant value. The beam blocked dashed line
corresponds to the fitted intensity at 2θ = 90◦ as shown in Fig. 3. The solid line through
the Cd measurement is a Gaussian fit with the peak location fixed at θ = 0. The insets
illustrate the sample orientation relative to the incident and scattered beams for θ = 0 and
θ = 90 degrees. Measurements were made using the CG-1B diffractometer with λ = 2.417 Å,
Ei = 14.0 meV, neutrons.

for comparison. Good neutron absorbers should have little to no orientation


dependence, and have less scattering intensity than the air scattering.
Figure 5 is a θ − 2θ scan in the vicinity of the calculated Cd (101) nuclear
Bragg peak (2θ = 62.22◦ ) for the Cd sample in transmission and reflection ge-
290 ometry. Compared to the no sample measurement there is a reduction in overall
scattering intensity, due to the absorption of the neutron beam by the Cd at the
sample position. We do not observe any nuclear Bragg peak scattering due to
the Cd. Bragg peak contributions should be considered when choosing shielding
materials to use in the vicinity of incident and scattered neutron beams.
295 Unless otherwise noted for the subsequent CG-1B data presented, we sub-
tract a polynomial fit of the angle dependent beam blocked data shown in Fig. 3
from the measured scattering intensity. Figure 6 shows the θ − 2θ scan for a
3.29 mm thick boron nitride (BN) sample, a 1.74 mm thick Al sample, and the

16
!"
>6477)?54@):A0:)(34&
)#<);6=))) )B$)(4+?85
)#<);'= )>54+)C8$3@5<

-&,+)*)('&%$#
""

!"

"
!1 ." .0 ./ ..
234''56,&7)4&7859)0:);<57-=

Figure 5: θ − 2θ scan of the cadmium (Cd) sample in transmission and reflection geometry.
Data were acquired in the vicinity of the calculated (101) nuclear Bragg peak for Cd. For
Ei = 14 meV, the scattering angle is calculated to be 2θ = 62.05◦ . The beam blocked dashed
line and datapoints correspond to the data shown in Fig. 3 and a linear fit of this data.
Measurements were made using the CG-1B diffractometer with λ = 2.417 Å, Ei = 14.0 meV,
neutrons.

Cd sample used for the measurements described earlier. After subtraction of


300 the beam blocked background, the Al measurements follow the no sample back-
ground except in the vicinity of nuclear Bragg peaks at approximately 62 and 72
degrees. The transmission and reflection measurement of the BN sample is al-
most identical to that of Cd. However, the BN reflection measurement observes
several weak nuclear Bragg peaks for scattering angles greater than 40 degrees.
305 Figure 7 shows higher point density scans in the vicinity of nuclear Bragg peaks
for (a) BN, (b) Al and (b) Cd. Although Fig. 6 indicates that BN is a good
neutron absorber, there are clear nuclear Bragg peaks visible in reflection ge-
ometry of the sample. No significant indication of a Bragg peak in BN can be
seen in the transmission measurement. The BN Bragg peak shown corresponds
310 to the (002) nuclear reflection. For comparison the nuclear Bragg peak of the
aluminum sample is shown in Fig. 6(b). Although the total cross-section of Al
is small, one can see a clear reduction in scattering intensity for the aluminum
measurement in transmission compared to the reflection measurement. Simple

17
#
" ,A',57.B;8
,CA,>*@,,,,, ,&?,>*@,,,,, ,D;,>*@
! ,CA,>9@ ,&?,>9@ ,D;,>9@

0)/.,-,+*)('&
$%%
#
"
!

% $3 4% !3 "% 23 1%
567**89/):,7):;8<, =,>?8:0@

Figure 6: θ − 2θ scan of the cadmium (Cd), boron nitride (BN) and aluminum (Al) sam-
ples in reflection and transmission geometry. Measurements were made using the CG-1B
diffractometer with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

Gaussian fits to these data are shown as solid lines in Fig. 7.


315 Figure 8 illustrates the orientation dependence of Cd, Al, and BN for 2θ = 90
degrees scattering angle. There is no significant orientation dependence to these
measurements. The scattering intensity of the Al sample is larger than that of
the absorbers, and larger than the no sample measurement. This is likely due
to a combination of the lack of absorption of Al, the elastic incoherent nuclear
320 scattering of Al, and inelastic scattering processes involved.
Figure 9 shows the θ − 2θ scan for the 25.4 mm thick borated polyethylene
(B-HDPE), the 10.6 mm thick polyethylene (HDPE), and the Cd sample for
comparison. Note that the scattering intensity is plotted on a logarithmic scale.
The B-HDPE and HDPE samples in reflection have large scattering intensities
325 due to the large incoherent nuclear cross section of hydrogen. In transmission
geometry, the B-HDPE sample performs as an absorber as well as the Cd sam-
ple. Figure 10 shows the orientation dependence of the B-HDPE, HDPE, and
Cd samples at 2θ = 90 degrees scattering angle. The scattering intensity of the
HDPE sample essentially varies as a function of how much material is intercept-
330 ing the incident beam. The B-HDPE data indicate a great deal of scattering

18
3
(a)
2
No Sample
BN (t) BN (r)
Counts / min.

100
7
6
5
4
3

2
(b) 40 42 44 46
1000 No Sample
8
6 Al (t) Cd (t)
Counts / min.

4 Al (r) Cd (r)

100
8
6
4

2
58 60 62 64 66
Scattering angle, 2θ (deg.)

Figure 7: θ − 2θ scan of the cadmium (Cd), boron nitride (BN) and aluminum (Al) samples
in reflection and transmission geometry. Data were acquired in the vicinity of the calculated
(101) nuclear Bragg peak for Cd, the calculated (111) nuclear Bragg peak for Al[34, 35], and
the calculated (002) nuclear Bragg peaks for BN. Measurements were made using the CG-1B
diffractometer with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

19
!"

-&,+)*)('&%$#
""

!"

)<$)12+345))) )#:
)=< )>4
"
" 0! /" .!
12+345)2&6457)8)9:56-;

Figure 8: θ scan of the cadmium (Cd), aluminum (Al) and boron nitride (BN) samples. The
value of 2θ was fixed at 90 degrees for these measurements. Measurements were made using
the CG-1B diffractometer with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

intensity for even shallow angles. Beyond θ = 90, B-HDPE is no longer in reflec-
tion and the scattering intensity matches very well with that of Cd. B-HDPE
should not be used as a neutron absorber in neutron scattering instrumentation
in a reflection geometry, only transmission. We especially caution against using
335 B-HDPE materials in the vicinity of the direct neutron beam.
Figure 11 shows the θ − 2θ dependence for a series of boron based absorbers:
B-Al, ZHIP, CBBC and RBBC. All of these materials perform well in both re-
flection and transmission geometries. The B-Al sample is less absorbing than
Cd in reflection for scattering angles below approximately 30 degrees. The
340 ZHIP, CBBC and RBBC samples are exceptional absorbers both in transmis-
sion and reflection. Figure 12 shows denser θ − 2θ scans in the vicinity of the
B4 C (104) nuclear Bragg peak, Fig. 12(a), and at the Al (111) nuclear Bragg
peak, Fig. 12(b). In order to improve counting statistics, we average the data
from the three B4 C based absorbers (ZHIP, CBBC and RBBC) together. There
345 is no Bragg scattering for these samples in transmission. There is a weak nu-
clear Bragg peak in the B4 C reflection measurements. This peak is still weaker
than the measurement with no sample in the beam and it is weaker than the

20
#
"
!!!
.'-,*+*)('&%$ #
"
!!
#
" *@%*46,A:7
! *$>*=(?*** *BCDE*=(?***** *FGBCDE*=(?
*$>*=8?*** *BCDE*=8? *FGBCDE*=8?
*
! 1 3! #1 2! 01 /!
456((78-'9*6'9:7;*"<*=>79.?

Figure 9: θ − 2θ scan of the cadmium (Cd), HDPE and borated HDPE (B-HDPE) samples in
reflection and transmission geometry. The Cd data are shown without error bars for compar-
ison to the other measurements. Measurements were made using the CG-1B diffractometer
with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

#
"
!!!
.'-,*+*)('&%$

#
"

!!
#
"
*=>?@*** *AB=>?@*** *C%*)3,456** *$;
!
! #0 1! /0
23,456*3'7568*9*:;67.<

Figure 10: θ scan of the cadmium (Cd), HDPE and Borated HDPE (B-HDPE) samples. The
value of 2θ was fixed at 90 degrees for these measurements. Measurements were made using
the CG-1B diffractometer with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

21
)@$)46+A:7
)BCD:)=8?)) )#BB#)=8?
!! )BCD:)='? )#BB#)='?

-&,+)*)('&%$#
)EFGH)=8? )IBB#)=8?
)EFGH)='? )IBB#)='?
)#>)=8? )#>)='?

"!!

!
! "0 3! 20 1! /0 .!
456''78,&9)6&9:7;) <)=>79-?

Figure 11: θ − 2θ scan of a series of boron based samples in reflection and transmission
geometry. For comparison, data for the cadmium sample are included without error bars
shown. Measurements were made using the CG-1B diffractometer with λ = 2.417 Å, Ei =
14.0 meV, neutrons.

scattering from BN shown in Fig. 7(a). We also observe a weak broad peak
in the B-Al reflection measurement. Again, this is less than the air scattering
350 measured with no sample present in the beam. The larger width of the B-Al
Bragg reflection is likely due to residual stress broadening. Figure 13 shows the
orientation dependence for a fixed scattering angle of 2θ = 90◦ . There is no
orientation dependence for these materials. The B4 C based absorbers perform
slightly better than the B-Al absorber, both materials are reasonable absorbers
355 for use both in transmission and reflection geometries. However, the borated
aluminum sample measured does have a higher cross-section for scattering an-
gles below 30 degrees.
Figure 14 compares the θ − 2θ scattering for Cd, Gd, and two types of con-
crete. The Gd sample performs comparably to the Cd sample in both reflection
360 and transmission geometry. The concrete samples behave very similarly to the
HDPE measurement shown in Fig. 9. We note that Figs. 14 and 9 are plotted on
identical intensity scales. The HCONC concrete absorbs slightly more neutrons
compared to the CONC sample. Figure 15 compares the orientation dependence

22
90 (a) No Sample B4C (r) B4C (t)
Counts / min.

60

30

90
54 56 58 60
Counts / min.

60

30

(b) No Sample B-Al (r) B-Al (t)


58 60 62 64 66
Scattering angle, 2θ (deg.)

Figure 12: θ − 2θ scan of the (a), boron carbide (B4 C) based samples and (b) the borated
aluminum (B-Al) sample in reflection and transmission geometry. Data in (a) were averaged
for the measurements of ZHIP, CBBC, and RBBC samples to improve the counting statistics.
Solid lines in panels are Gaussian fits for the reflection data, and constant fits for the trans-
mission data. Data were acquired in the vicinity of the calculated (014̄) nuclear Bragg peak
for B4 C and the calculated (111) nuclear Bragg peak for Al. Measurements were made using
the CG-1B diffractomete with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

23
!" )
)<$)12+345
)=>?4))) )#==#
)@ABC )D==#

-&,+)*)('&%$#
""

!"

"
" 0! /" .!
12+345)2&6457)8)9:56-;

Figure 13: θ scan of the boron carbide (B4 C) based samples and the borated aluminum (B-Al)
sample. The value of 2θ was fixed at 90 degrees for these measurements. Measurements were
made using the CG-1B diffractometer with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

of Gd and the two concrete samples for a scattering angle of 2θ = 90◦ . The
365 Gd samples shows no orientation dependence, however the concrete samples
show an increase in scattering for both transmission and reflection geometries,
with an overall maximum in reflection. High density and traditional concrete
are not appropriate neutron shielding very close to neutron beams. They are
necessary components of the biological shielding around neutron scattering in-
370 strumentation. We note that there are also nuclear Bragg peaks in the concrete
data shown in Fig. 14. Due to the aggregate nature of the material, we do not
attempt to index these peaks.
In Fig 16, we plot the θ − 2θ scattering intensity for additional boron and
lithium based absorbing materials: Bflex, LiSiO, LiEP, B4 CEp and Cd. All of
375 the samples measured perform better as absorbers in transmission compared to
reflection. The lithium carbonate in epoxy (LiEP) does not work well as an
absorber when in a scattering geometry. The LiSiO and Bflex materials work
fair in transmission, but do not reduce the air-scatter in reflection. The B4 CEP
works very well in transmission, but for large scattering angles, does not reduce
380 the air scattering in reflection geometry. The orientation dependence data shown

24
#
"
!!!
.'-,*+*)('&%$ #
"
!!
#
" *@%*46,A:7
*B>*=(?*** *C$D@$*=(?*** *$D@$*=(?** $>*=(?
! *B>*=8?*** *C$D@$*=8? *$D@$*=8? $>*=8?

! 1 3! #1 2! 01 /!
456((78-'9*6'9:7;*"<*=>79.?

Figure 14: θ − 2θ scan of the Gd, concrete (CONC) and hematite loaded concrete (HCONC)
for samples in reflection and transmission geometry. For comparison, data for the cadmium
sample are included without error bars shown. Data are shown with the identical vertical axis
range as Fig. 9. Measurements were made using the CG-1B diffractometer with λ = 2.417 Å,
Ei = 14.0 meV, neutrons.

# *
"
*=%*23,456
*>;
!!! *$?=$
*@$?=$
.'-,*+*)('&%$

#
"

!!
#
"
!
! #0 1! /0
23,456*3'7568*9*:;67.<

Figure 15: θ scan of gadolinium (Gd) and concrete samples, hematite concrete (HCONC) and
traditional concrete (CONC). The value of 2θ was fixed at 90 degrees for these measurements.
Measurements were made using the CG-1B diffractometer with λ = 2.417 Å, Ei = 14.0 meV,
neutrons.

25
*@%*46,A:7
BC:7D*=8?* E-4-F*=8?* E-GH*=8?* B#$GA*=8?* $>*=8?
BC:7D*=(? E-4-F*=(? E-GH*=(? B#$GA*=(? $>*=(?
#
"
!!!
.'-,*+*)('&%$
#
"
!!
#
"
!
! 1 3! #1 2! 01 /!
456((78-'9*6'9:7;*"<*=>79.?

Figure 16: θ − 2θ scan of the Bflex, Li in silicone, Li in epoxy and B4 C in epoxy for samples
in reflection and transmission geometry. For comparison, data for the cadmium sample are
included without error bars shown. Measurements were made using the CG-1B diffractometer
with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

in Fig. 17 further illustrates the difficulties of using these materials in a reflection


geometry. The scattering intensity peaks well above the no sample scattering
intensity for the LiEP, LiSiO, Bflex, and B4 CEp samples. These materials
should not be used in a reflection geometry in the vicinity of neutron scattering
385 instrumentation.

3.2. Time-of-flight measurements at SEQUOIA

The SEQUOIA measurements examined a selection of the materials studied


at the CG-1B diffractometer. The wavelength dependent intensity was measured
using the second beam monitor, shown in Fig. 2(c) as M2 . This was first done
390 with no sample installed in the instrument. This spectrum is shown in Fig. 18.
Measurements of the neutron counts at beam monitor M2 were made by placing
the absorbers in the neutron beam at the sample position. This is shown for
example in Fig. 18 for the Gd sample. The Gd foil is an excellent absorber
at smaller values of energy transfer. The energy dependent transmission was

26
#
" *=->?
*=-2-@
!!! *AB56C

.'-,*+*)('&%$
*A#$>4
# *D%*23,456
"

!!
#
"
!
! #0 1! /0
23,456*3'7568*9*:;67.<

Figure 17: θ scan of Bflex, Li based composites, and B4 CEp. The value of 2θ was fixed at 90
degrees for these measurements. Measurements were made using the CG-1B diffractometer
with λ = 2.417 Å, Ei = 14.0 meV, neutrons.

395 determined through the ratio of these two measurements. This is shown in
Fig. 19 for a series of materials. Because the transmission is calculated using a
ratio of measurements, the wavelength dependent detector sensitivity correction
is not included in the analysis.
Based upon the results shown in Fig. 19, several conclusions can be made.
400 The BN paint on an aluminum substrate does not provide any effective shielding
for the wavelengths examined. There is some shielding provided by the lithi-
ated coraflon paint on the aluminum substrate, but this is nearly identical to
the transmission of a simple 1/4 inch thick aluminum plate. Borated coraflon
paint on an aluminum substrate is somewhat effective at long wavelengths with
405 at least 3 layers of material applied. We estimate that five or six layers of this
material would be needed to provide comparable or better shielding than bo-
rated aluminum. Gadolinium and cadmium are excellent absorbers for longer
wavelengths. Note that the small deflection in the transmission of the gadolin-
ium sample at approximately 2660 meV agrees very well with the increase in
410 cross-section of Gd at this energy as shown in Fig. 1. A reasonable definition of
a cut-off energy for the Cd and Gd samples would be the point at which their

27
!!!
(9#(:*7;<4
(=>

/'&.%$(-,+*)('&%$#"
!!

0 1 2
! ! ! !
3%4+56()748/
(

Figure 18: Measured intensity as a function of neutron energy using the second beam monitor,
M2 , of the SEQUOIA instrument. Measurements are shown for no sample in the beam and
the gadolinium sample in the beam. Solid circle symbols are plotted for every five data points.

transmission is one-half their respective maximum values. These cut-offs are 80


meV (1.01 Å) for the gadolinium sample and 360 meV (0.48 Å) for the cadmium
sample. The BN and B4 C samples remain below 20 percent transmission for
415 energies less than 4300 meV. The borated polyethylene sample is nearly opaque
to neutrons. However, we again caution that this measurement only examines
the neutrons passing through the sample and scattering roughly within 1 degree
scattering angle. The CG-1B measurements in Fig. 9 and 10 clearly show that
using borated polyethylene near the direct beam of an instrument can cause
420 significant increase in background.
The polychromatic measurements at SEQUOIA also allow the chopper spec-
trometer to operate as a coarse resolution powder diffractometer. By using the
time-resolved scattering intensity along with the instruments dense detector cov-
erage one can measure a reasonable diffraction pattern.[36] Figures 20 and 21
425 show the scattering intensity as a function of wave-vector transfer, Q. The
time-of-flight data were first converted to be a function of d-spacing for each
detector. The spectra of all the detectors were then summed together and nor-
malized to the number of coulombs of charge accumulated on the target of the

28
945:7
&!8 "!8 "!&8 "! &8
4;E4F)-*<4.*4G@
!" 4$!/84,,4<H-IJ4G@
4K-<H-)<1=4>.()?@.*4F)-*<4.*4G@
"!# 4;.()<1=4>.()?@.*4 4@)31(
*.-++-,+*)('

"!$ L= 4;.()<1=4>.()?@.*4/4@)31(+
4;.()<1=4G@
"!%
4;%>
4;E
"!& >=

" 4;ABCD0
& / %
" " " "
0*1(2345,167
4

Figure 19: Energy dependent transmission for a series of materials examined using the SE-
QUOIA spectrometer. Thickness and composition of the materials are further described in
Tab. 1. The B4 C sample measured is the 2.2 mm thick RBBC sample.

SNS.[37] The measurement was not normalized for detector sensitivity. Because
430 of the polychromatic nature of the measurement and the absorbing nature of
the samples, one must keep in mind that the relative intensities of the Bragg
peaks may vary significantly from when monochromatic neutrons are used.
We first note the striking contrast between the transmission of the borated
polyethylene sample in Fig. 19 compared to the scattering intensity of this ma-
435 terial shown in Fig. 20. For some values of Q the scattering intensity is an entire
order of magnitude greater than the scattering intensity for the other materi-
als. Although, we note that this scattering is a smooth function of wave-vector
transfer. The absorbers which consist of a painted layer of absorbing material on
a substrate have significant scattering intensities despite their reduction in neu-
440 tron transmission. Borated aluminum is a reasonable absorber in comparison
to the other materials shown in Fig. 20.
In Fig. 21, we examine the materials which provided significant transmission
reduction of neutrons. The scattering intensity of the borated aluminum sample
is shown in this figure for comparison to the other results, however it is offset

29
<6
$
! <4=>?@

<7A8'(B,.7A8C;7&,#,;8+(A)
# <7A8'(B,.7A8C;7&, ,;8+(A
!
.,-,+'*)&('&%

J*'F*8'(B,.7A8C;7&,:8*&',7&,I;
0D#E,99,'F*GH,I;
" <6,:8*&',7&,I;
! <7A8'(B,I;
,67,)89:;(
!

!
!
! " $ 0 / ! " $
4
1,23 5

Figure 20: Measured scattering intensity per Coulomb as a function of Q using the SEQUOIA
detectors in the polychromatic beam configuration. The vertical axis is a logarithmic intensity
scale.

445 from the vertical axis and shown at one-fifth the measured intensity. At the top
of this figure, are the calculated nuclear Bragg peak positions of aluminum[35],
Gd[24] Cd[25], B4 C[22], BN[21] and Li2 CO3 [29]. As shown earlier, there are
advantages to using boron nitride for shielding, however, there are nuclear Bragg
peaks which may be significant when neutrons scatter from this material. The
450 Gd measurement also has a significant Bragg peak at smaller values of wave-
vector transfer. The Cd and B4 C samples have the weakest total scattering
observed in this measurement.

4. Conclusions

Both monochromatic and polychromatic measurements were used to exam-


455 ine the transmission and scattering from a series of materials. Boron carbide,
gadolinium, cadmium, and boron nitride are all reasonable choices of materials
for use in the vicinity of the direct beam in neutron instrumentation depending
upon the wavelengths of neutrons in use at the instrument. The prompt-gamma
present when cadmium is used should be considered when working in instru-
460 mentation with more open beams or in the vicinity of personnel. Painted layers
of absorbing material on substrates provides some shielding benefit, but should

30
E*#.F"
A9
.9
7.
78
=>
!!

"!!
.,-,+'*)&('&%

,78,,, ,.9,,, ,7:;<'(9,=>,?,!@#


,7 . ,A9 ,8:,B<CD>(
#!!

$!!

!
# " 1 0 /
5$
2,34 6

Figure 21: Measured scattering intensity per Coulomb as a function of Q using the SEQUOIA
detectors in the polychromatic beam configuration. The borated aluminum measurement is
shown at one-fifth the measured intensity scale and offset vertically for presentation. The
upper portion of the figure shows the calculated nuclear Bragg peak positions as a function of
Q. Tick marks represent Bragg peak positions of the materials written in the left margin of
the figure. The darkness of the tick mark is proportional to the relative intensity of the Bragg
peak for the neutron cross-section.

31
likely be kept out of the direct neutron beams of instruments. Borated polyethe-
lene has significant reduction of scattering intensity in a purely transmission
configuration; however, the amount of scattering from the hydrogen in this ma-
465 terial can increase neutron backgrounds by an order of magnitude. Polyethelene
shielding can be used to reduce the flux of epithermal and fast neutrons in re-
gions of the instrument far from the incident or potentially scattered neutron
beams. For the case of high-density polyethylene, it has been found that a
minimal thickness of approximately 100 mm is required to both thermalize and
470 attenuate the high energy neutrons at a reactor based neutron source.[38] Steel
shot and borated paraffin mixtures in appropriate ratios have also been used at
several neutron scattering facilities in locations far from the incident neutron
beam to reduce thermal, epithermal and fast neutron backgrounds.[39] The
presence of Bragg peaks in scattering from traditional neutron absorbers has
475 also been shown to be a reasonable concern. The boron carbide and cadmium
samples examined here have smaller cross-sections for Bragg peaks compared
to the boron nitride, borated aluminum and gadolinium samples. Examining
composite materials made of multiple layers of absorbers which would provide
effective shielding across a range of wavelengths is beyond the scope of the cur-
480 rent effort. However, such multilayers or composites should be considered in
future studies for applications. We emphatically note that the shielding choices
made for particular applications should be tested for both neutron transmission
and neutron scattering across the entire wavelength range which may be used
at the instrument and as a function of scattering angle. The gamma sensitivity
485 of the neutron detectors used at the instrument should also be considered when
choosing neutron shielding materials.
We have presented a series of measurements examining practical materials
for use as neutron shielding for neutron scattering instruments. Often these
instruments are co-located surrounding the neutron source at large facilities.
490 While it may be hackneyed to say, it is true that, good neutron absorbers make
good neighbors at these facilities. Good neutron shielding should also not add
to the background of a measurement. Likewise, it should be chosen to avoid

32
significant contamination of nuclear Bragg peak scattering in the measurement.
We also note that in choosing neutron shielding one should determine whether
495 one is shielding scattering in or shielding scattering out of the instrument. We
have not addressed methods of biological shielding, i.e. keeping scattering or
radiation within the instrumentation. Rather we focused our attention to char-
acterizing shielding materials which serve to shield detectors from scattering
that is not an intended cross-section of the measurement. The other important
500 point we would like to make is that one should not take shielding down until
one knows why it was put up, i.e installed. The life-cycle of neutron scattering
instruments can span beyond institutional memory. Removing shielding can
have unanticipated consequences to the quality of a measurement.

5. Acknowledgements

505 This research used resources at the High Flux Isotope Reactor and Spal-
lation Neutron Source, a DOE Office of Science User Facility operated by the
Oak Ridge National Laboratory. We acknowledge A. Savici for assistance in
generating the diffraction patterns from the SEQUOIA measurements.

[1] J. Chadwick, Possible Existence of a Neutron, Nature 129, 312 (1932)

510 [2] J. Chadwick, The existence of a neutron, Proc. Roy. Soc. A 136, 692 (1932).

[3] I. Joliot-Curie and F. Joliot-Curie, Emission de protons de grande vitesse


par les substances hydrogenees sous l’influence des rayons [lambda] tres
penetrnts Comptes Rendus 194, 273 (1932).

[4] V. Nesvizhevsky and J. Villain, The discovery of the neutron and its con-
515 sequences (1930-1940), Comptes Rendus Physique 18, 592 (2017).

[5] T. E. Mason, T. J. Gawne, S. E. Nagler, M. B. Nestor, and J. M. Carpenter,


The early development of neutron diffraction: science in the wings of the
Manhattan Project, Acta Crystallogr 69, 37 (2013).

33
[6] R. B. Sawyer, E. O. Wollan, S. Bernstein, and K. C. Peterson, A bent
520 crystal neutron spectrometer and its application to neutron cross-section
measurements, Physical Review 72, 109 (1947).

[7] V.V.Zerkina and B.Pritychenko, The experimental nuclear reaction data


(EXFOR): Extended computer database and Web retrieval system. NIMA,
888, 31 (2018).

525 [8] G. L. Squires, Introduction to the Theory of Thermal Neutron Scattering


(Cambridge University Press, Cambridge UK 2012).

[9] B. T. M. Willis, C. J. Carlile, Experimental Neutron Scattering (Oxford


University Press, Oxford UK 2009).

[10] I. F. Bailey, A review of sample environments in neutron scattering, Z.


530 Kristallogr. 218, 84 (2003).

[11] J. G. Barkera, and D. F. R. Mildner, Survey of background scattering from


materials found in small-angle neutron scattering, J Appl Crystallogr. 48,
1055 (2015).

[12] W. Soller, A new precision X-ray spectrometer, Phys. Rev. 24, 158 (1924).

535 [13] M. B. Stone, J. L. Niedziela, M. J. Loguillo, M. A. Overbay, and D. L.


Abernathy, A radial collimator for a time-of-flight neutron spectrometer,
Review of Scientific Instruments 85, 085101 (2014).

[14] K. C. Rule, R. A. Mole, D. Yu, Which glue to choose? A neutron scat-


tering study of various adhesive materials and their effect on background
540 scattering, Journal of Applied Crystallography 51, 1766 (2018).

[15] Mariette Hellenbrandt, The Inorganic Crystal Structure Database


(ICSD)Present and Future, Crystallography Reviews 1, 17 (2014).

[16] V. F. Sears, Neutron scattering lengths and cross sections, Neutron News
3, 26 (1992).

34
545 [17] G.L.Molnra, Zs. Rvay, T. .Belgy, R. B. Firestone, The new prompt gamma-
ray catalogue for PGAA, Applied Radiation and Isotopes, 53, 527 (2000).

[18] M. P. Dariel and N. Frage, Reaction bonded boron carbide: recent devel-
opments, Advances in Applied Ceramics 11 301 (2012).

[19] M. B. Stone, J. Niedziela, D. L. Abernathy,L. M. Debeer-Schmitt, G.


550 Ehlers, V. O. Garlea, G. E. Granroth, M. Graves-Brook, A. I. Kolesnikov,A.
A. Podlesnyak, and B. Winn, A comparison of four direct geometry time-of-
flight spectrometers at the Spallation Neutron Source, Review of Scientific
Instruments 85, 045113 (2014).

[20] M. M. Elcombe, R. A. Mole, D. H. Yu, Time dependent fast neutron back-


555 ground: Understanding the cause and identifying a solution for the PEL-
ICAN cold neutron spectrometer, Physica B: Condensed Matter 551, 347
(2108).

[21] R. S. Pease, An X-ray study of boron nitride, Acta Crystallographica 5,


356 (1952).

560 [22] H. K. Clark, J. L. Hoard, The crystal structure of boron carbide, Journal
of the American Chemical Society 65, 2115 (1943).

[23] F. Thevenot, Boron carbide - A comprehensive review, Journal of the Eu-


ropean Ceramic Society, 6, 205 (1990).

[24] M. Norman, I. R. Harris, and G. V. Raynor, The lattice spacings of


565 thorium-rich solid solutions with praseodymium, samarium, gadolinium,
and erbium, Journal of the Less-Common Metals, 11, 395 (1966).

[25] S. S. Lu and Y. L. Chang, The accurate evaluation of lattice spacings from


back-reflection powder photographs, Proceedings of the Physical Society of
London 53, 517 (1941).

570 [26] E. Rossmanith, X-ray measurements of the root-mean-square displacement


of the atoms in cadmium single crystals, Acta Crystallographica, Section
A, 34, 497 (1978).

35
[27] O. N. Carlson and C. V. Owen, Preparation of high purity vanadium by
the iodide refining process, Journal of the Electrochemical Society 108, 88
575 (1961).

[28] H. E. Swanson and E. Tatge, Standard X-ray diffraction powder patterns,


National Bureau of Standards Circular 1 539 (1953).

[29] Y. Idemoto, J. W. Richardson, N. Koura, S. Kohara, and C.-K. Loong,


Crystal structure of (Lix K1−x )2 CO3 (x=0, 0.43, 0.5, 0.62, 1) by neutron
580 powder diffraction analysis, Journal of Physics and Chemistry of Solids 59,
363 (1998).

[30] R. Lorenz, and J. Woolcock Z. anorg. allgem. Chem. 176, 289 (1928).

[31] T. Q. P. Vuong, G. Cassabois, P. Valvin, E. Rousseau, A. Summerfield, C.


J. Mellor, Y. Cho, T. S. Cheng, J. D. Albar, L. Eaves, C. T. Foxon, P. H.
585 Beton, S. V. Novikov, and B. Gil, Deep ultraviolet emmision in hexago-
nal boron nitride grown by high-temperatrure molecular beam epitaxy, 2D
Materials 4, 021023 (2017).

[32] L. H. Dreger, V. V. Dadape, and J. L. Margrave, Sublimation and decom-


position studies on boron nitride and aluminum nitride. The Journal of
590 Physical Chemistry, 66, 1556 (1962).

[33] G. E. Granroth, A. I. Kolesnikov,T. E. Sherline, J. P. Clancy, K. A. Ross, J.


P. Ruff, B. D. Gaulin, S. E. Nagler, SEQUOIA: a newly operating chopper
spectrometer at the SNS, Journal of Physics: Conference Series 251, 12058
(2010).

595 [34] H. E. Swanson and E. Tatge, Standard X-ray diffraction powder patterns,
National Bureau of Standards Circular (U.S.) 539, 1 (1953).

[35] A. S. Cooper, Precise lattice constants of germanium, aluminum, gallium


arsenide, uranium, sulphur, quartz and sapphire, Acta Crystallographica
15, 578 (1962).

36
600 [36] E. S. Bozin, P. Juhas, W. Zhou W, M. B. Stone, D. L. Abernathy, A. Huq,
S. J. Billinge, Atomic pair distribution function analysis from the ARCS
chopper spectrometer at the Spallation Neutron Source, Journal of Applied
Crystallography, 42, 724 (2009).

[37] Arnold O., Bilheux J., Borreguero J.M., Buts A., Campbell S.I., Chapon
605 L.C., Doucet M., Draper N., Leal R.F., Gigg M.A., Lynch V.E., Markvard-
sen A., Mikkelson D.J., Mikkelson R.L., Miller R.G., Palmen K., Parker
P., Passos G., Perring T.G., Peterson P.F., ”MantidData analysis and vi-
sualization package for neutron scattering and SR experiments”, Nuclear
Instruments and Methods in Physics Research Section A, 764, 156-166
610 (2014).

[38] K. C. Rule, F. Darmann, T. Oste, D. Bartlett, F. Franceschini, A. Berry,


A. McGregor, A. Ogrin, T. Ersez, A. Kafes, S. Pangelis, S. Danilkin, A. P.
J. Stampfl, and S. R. Olsen, Recent enhancements and performance gains
from upgrades to ANSTOs thermal neutron instrument TAIPAN and the
615 triple-axis and Be-filter spectrometers, Nuclear Instruments and Methods
in Physics Research Section A, 901, 140 (2018).

[39] S. A. Danilkin, G. Horton, R. Moore, G. Braoudakis, and M. Hagen, The


TAIPAN thermal triple-axis spectromater at teh OPAL reactor, Journal of
Neutron Research 15, 55 (2007).

37

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