Application of Small Angle Neutron

Scattering(SANS)
A case study
by

Karthik B. Kamath
1st Semester
Manufacturing Science & Engineering
Dept. of Mechanical Engineering
BMS College of Engineering
Contents
Introduction to SANS
Working of SANS
SANS Equipment
Application & Highlights
Case studies
References
Introduction
• Small-angle neutron scattering (SANS) is an experimental
technique that uses elastic neutron scattering at small scattering angles
to investigate the structure of various substances at a mesoscopic
scale of about 1–100 nm.
• During a SANS experiment a beam of neutrons is directed at a sample,
which can be an aqueous solution, a solid, a powder, or a crystal. The
neutrons are elastically scattered by nuclear interaction with the nuclei
or interaction with magnetic momentum of unpaired electrons.
• In neutron scattering, neutrons interact with nuclei and the interaction
depends on the isotope; some light elements like deuterium show
similar scattering cross section as heavy elements like Pb.
Working of SANS

• The information in elastic scattering experiments is contained in the

neutron intensity measured as a function of the momentum transfer
Q  ki  kf
kf →
Q  2k sin
2
Q
 4 
ki Q sin
  

• where Ki and Kf are the incoming and outgoing neutron wave vector, λ is
the neutron wavelength and 2θ the scattering angle
 SANS Equipmennt Schematic

Fig 1.0 Schematic of Small angle neutron scattering equipment

• Neutron guide: Allow neutron to travel large distance without suffering

intensity loss.
• Velocity selector: Allow neutron of defined velocity to pass while absorbing
other neutrons to produce monochromatic neutron beam.
• Collimator pinholes : Define the travel direction of neutron
• Detector: The scattered neutrons within a angular range, typically between
0.1° and 20° are detected.
 Application of SANS
• Identification of atomic structures and magnetic nature of metallic alloys
• Engineering geophysics , material science & forensic sciences
• Studying polymers , mechanism of molecular assembly in solutions
• Biological microsolutions, proteins, nucleic acids, membranes membrane
components, DNA etc
Highlights of SANS
• High penetrating ability of neutrons, wide range of wavelengths can be
achieved.
• Need nuclear reactor for supply of neutrons, hence high installation &
maintenance cost.
• Large sample are requires, less damage to samples.
 Case Study-1
Small-angle neutron scattering investigations of nanocrystalline alloy chips
obtained by machining
Elwyn Rebello, Frazer Vaz, Avino Colaco, Wellon Rodrigues, Geethalakshmi K, Debasis Sen, S. Mazumder & A.O. Surendranathan

• Studies have revealed that, nanocrystalline materials have enhanced

mechanical properties in terms of hardness and strength over the bulk
materials.
• Under Certain combinations of machining parameters, large shear strains can
be imposed in the machining process, resulting in nanoscale microstructures.
• In this study, small-angle neutron scattering (SANS) was employed to
investigate the modifications in the microstructure of the chips produced via
machining. .
• Significant scattering intensity at small enough angles reveals the presence of
mesoscopic density fluctuations produced because of the machining.
• Atomic force microscopy images also supported the existence of such small
length scale density fluctuations.
 Experimentation
• Material details :Steel and brass with near equivalent specification were used
• Machining details: Chips were produced by using with HSS and carbide tools
under controlled plain strain conditions with following parameters. Feed rate
= .2 mm/rev, Rake angle= +8° to −15°, DOC=40 μm, Cutting Speed= 15–20
mm/s to avoid the influence of temperature.
• The initial grain sizes of the bulk material in both case greater than 10 μm.
• The bulk hardness of steel and brass was 140 HV and 110 HV respectivley.
• Chip samples 50–80 μm in width, 40–60 μm in thick & 100–200 μm in length.
• The chips were characterized by SANS , determination of Vickers hardnesss
• Scattered intensities [I(q)] recorded as a function of wave vector transfer q.
• specimens were placed on a sample holder with a circular slit of 1.5 cm dia.
• Microstructural characterizations were done using an optical microscope,
SEM & AFM. For metallographic observation, chips were mounted , polished
followed by chemical etching.
 Results & Discussion
• SANS signal originates from density fluctuations in mesoscopic length scale.
• Because of the presence of the sub-micrometric structure after machining. It is
observed that the scattering profile becomes significantly broader due to small-
angle scattering after the machining.
• The estimated particle size distribution for the machined samples is plotted &
average radius of the grains in machined samples is nearly 45nm.
 Case Study-2
A Small-Angle Neutron Scattering Environment for In-Situ Observation of
Chemical Processes
Dominic W. Hayward, Leonardo Chiappisi, Sylvain Prévost, Ralf Schweins & Michael Gradzielski

• Small-angle neutron scattering (SANS) was introduced for observation of

chemical reaction which enables structural changes to be followed
continuously across a wide Q-range in response to changes in chemical
environment.
• The approach is demonstrated and validated by performing multiple titrations
with addition times varying from 1 s to 2 h.
• It is shown that the continuous flow set-up offers considerable advantages
over ‘static’ measurements with regards to sample throughput, compositional
precision and the ability to observe fast structural transitions.
• Finally, the capabilities and ongoing optimization of the sample environment
are discussed with reference to potential applications in the fields of biology,
colloidal systems and complex soft matter.
 Conclusion
• Fine microstructure, composed of grains even smaller than 100 nm, is found
to result from chip formation in commercial steel and brass due to the induced
shear strain leading to large strain deformation.
• The machined chips exhibit a remarkable increase in the hardness as
compared with the measured bulk hardness values in both materials. This
increase in hardness values is attributed to the reduced grain size and
dislocation substructures in the chips.
• The average particle size obtained from neutron scattering experiment is
found to be in corroboration with the particle size obtained from AFM.
• Furthermore, the presence of mesoscopic traces of shear bands in the
machined chips formed due to large strain deformation leads to the density
fluctuations during neutron scattering.
 Experimentation
• Setup consists of a reaction vessel, a pH
electrode, a peristaltic pump, an observation
cell , two syringe pumps SANS instrument,
controlled entirely from instrument control
platform.
Fig 2.0 Schematic of Experimental setup with connections(dotted lines)
• Undertaken to follow the structural evolution
of the self-assembled surfactant aggregates at a
high resolution with respect to the pD of the
solution.
• Changing pD from 2.5 to 12 via the slow,
continuous addition of 12 mL of 0.1 M NaOD
over 2 hours, at 0.1 mL/min. Performed three
times, sample-to-detector distance, follow
Fig 3.0 Photograph of Experimental setup
structural evolution over a broad Q-range.
 Results & Discussion
• The resulting SANS curves from the three different experiments are shown
combined according to the volume of titrant added to reduce number of data
points.
• The overlap between the detector configurations is very good, further
demonstrating the validity of this approach.
 Conclusion
• The presence of one or more organic components, structures (or features) in
the 1–100 nanometre size range and, crucially, structural transitions that occur
in response to compositional determine the use of Insitu SANS .
• Allows chemical reactions to be monitored in real time, providing insights into
mesoscopic structural changes and non-equilibrium structures that may occur
as the system evolves.
• ‘Static’measurements, whereby every composition is prepared and measured
individually, does not match the time-efficiency and compositional resolution
provided by the equivalent continuous-flow measurement.
• It is quick and straightforward to assemble and enables the efficient collection
of large amounts of data with respect to equivalent experiments conducted via
discrete reaction sampling which would require both more time and a larger
sample volume.
References
 https://en.wikipedia.org/wiki/Small-angle_neutron_scattering
 Fundamentals of Small Angle Neutron Scattering by Glinka NIST Center for Neutron
Research Gaithersburg, Maryland
 The basics of small-angle neutron scattering (SANS for new users of structural
biology) Cy M. Jeffries, Zuzanna Pietras, and Dmitri I. Svergun
 Small-angle neutron scattering investigations of nanocrystalline alloy chips obtained
by machining Elwyn Rebello, Frazer Vaz, Avino Colaco, Wellon Rodrigues,
Geethalakshmi K, Debasis Sen, S. Mazumder & A.O. Surendranathan
 A Small-Angle Neutron Scattering Environment for In-Situ Observation of
Chemical Processes Dominic W. Hayward, Leonardo Chiappisi, Sylvain Prévost, Ralf
Schweins & Michael Gradzielski.
Thank You