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National Facility for Neutron Beam Research [NFNBR]14.139.62.172/mumbai/nfnbr-book-R.pdfBhabha Atomic Research Centre, Mumbai, India 1 National Facility for Neutron Beam Research 2

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  • 1Bhabha Atomic Research Centre, Mumbai, India

    National Facility for Neutron Beam Research 2

    Neutrons for Condensed Matter Resarch 4

    Single Crystal Diffractometer 6

    Powder Diffractometer-1 8

    Powder Diffractometer-2 10

    Powder Diffractometer-3 12

    Polarized Neutron Spectrometer 14

    High-Q Diffractometer 16

    Small-Angle Neutron Scattering Diffractometer 18

    Double Crystal based SANS Instrument 20

    Polarized Neutron Reflectometer 22

    Spin Echo and Polarized Small Angle Neutron Scattering Instrument 24

    Triple Axis Spectrometer 26

    Quasi Elastic Neutron Spectrometer 28

    Filter Detector Spectrometer 30

    Neutron Radiography Facility 32

    Neutron Detectors 34

    Sample Environment Facilities 37

    Contact Scientists 38

    C o n t e n t s

  • 2 Bhabha Atomic Research Centre, Mumbai, India

    Neutron scattering at Trombay started

    with the facility at Apsara reactor

    (1 MW) in 1956, and then continued

    with CIRUS (40 MW), which became

    available in 1960 and then with the

    present reactor Dhruva. Dhruva is a

    100 MW natural uranium reactor with

    peak thermal neutron flux of 1.8x1014

    neutrons cm -2 s-1, tailor-made for

    neutron scattering experiments with

    tangential beam holes, through-tube,

    provision for separate moderators for

    cold and hot neutrons, guide-tube, etc.

    Advanced instruments, fully automatic

    in instrument control and data

    acquisition modes have been installed

    on various beam ports. State of the art

    technology was used to design and

    fabricate the spectrometers. 1-D and

    2-D position sensitive detectors (PSD),

    and associated electronics have also

    been developed indigenously.

    National Facility for Neutron Beam

    Research (NFNBR) has been created as

    a part of the Solid State Physics

    Division (SSPD) during early nineties

    to cater to the needs of the Indian

    scientific community in the field of

    neutron beam research. Scientists from

    BARC, other DAE units, universities and

    national laboratories are welcome to

    use this facility through collaborative

    reseach projects with SSPD scientists.

    Many of these collaborations are being

    supported by UGC-DAE Consortium

    for Scientific Research, Board of

    Research in Nuclear Sciences (BRNS)

    and other agencies.

    NationalFacility for

    Neutron BeamResearch

    International collaboration between neutron

    beam research at BARC and other countries is

    over four decades old. The first such

    agreement was the “Indian-Philippines-IAEA

    Agrement” signed during sixties, under

    which BARC-built neutron instrument was

    installed at Phillipines, and their scientists

    were trained to use it. A more recent example

    is the installation of a neutron spectrometer

    at Bangladesh through IAEA in nineties.

    Scientists from Phillipines, Korea, Indonesia,

    Bangladesh, Vietnam, Malaysia and Egypt

    have visited BARC to work on the neutron

    instruments. A neutron instrument was

    installed at the spallation neutron source at

    Rutherford Appleton Laboratory in UK.

    Scientists from SSPD avail advanced sources at UK, USA, Germany, France, Switzerland, Japan and other countries to carry

    out front line research, and keep themselves up to date in this field.

    Fig. 1. A panoramic view of CIRUS and DHRUVA reactors at BARC

  • 3Bhabha Atomic Research Centre, Mumbai, India

    General layout in the reactor hall and the guide-tube laboratory is shown in Fig. 2. There are four spectrometers at the

    tangential beam lines, three at the ends of the through tube, two at the beam lines looking at the hot source, and four

    instruments in the guide laboratory.

    The present-day facilities include, single-crystal and powder diffractometers, polarization analysis spectrometer, Hi-Q

    diffractometer, triple-axis & filter-detector spectrometers, quasi-elastic scattering spectrometer, all installed in the reactor

    hall, and two small-angle scattering instruments, spin-echo spectrometer and reflectometer in the guide-tube laboratory.

    80 K ice based cold neutron source and graphite at 1800 K hot source are under advanced stages of development.

    Fig. 2. A layout of the neutron scattering instruments at Dhruva reactor

    Fig. 3. A view of neutron scattering facilities inside the Dhruva reactor hall

  • 4 Bhabha Atomic Research Centre, Mumbai, India

    Neutrons forCondensed

    MatterResearch

    The existence of a neutral particle

    similar to the mass of a proton, was

    hypothesized by Rutherford in 1920

    and this was proved by the discovery

    of neutron by J. Chadwick, a student

    of Rutherford, in 1932. Since its

    discovery, neutrons have been used

    as a great probe for research in

    condensed matter.

    Due to its various special properties,

    neutrons provide an insight about the

    microscopic structures and dynamics

    in a wide class of materials. When get

    scattered by the materials, neutrons

    can not only tell about the position of

    an atom in that material but also

    atomic movement with time.

    Particle nature

    • Mass = 1.67x10-27 Kg

    • Spin = 1/2 Acts as a tiny magnet

    • Magnetic moment = -1.913 μN

    • Velocity [2200m/s for thermal

    neutrons of energy 25 meV]

    Neutron’s properties which make all these possible

    . Wave-particle duality

    . Compatible wavelength with the inter-atomic distances for thermal

    neutrons

    . Compatible energy with atomic excitation energies

    . Deep penetration due to the charge neutrality

    . Scattering contrasts between neighbouring elements in the periodic table

    . Isotope specific scattering and absorption

    . Magnetic moment and thus can interact with magnetic materials

    . Simple interaction with nuclei (isotropic s-wave scattering). No angular

    dependence of scattering amplitude for nuclear scattering unlike in the case

    of x-ray.

    Wave nature

    • Diffraction and interference

    pattern

    • Measurable wavelength

    • Measurable scattering length

  • 5Bhabha Atomic Research Centre, Mumbai, India

    Unlike for x-rays, the neutron

    scattering power of elements

    varies in a zigzag fashion with

    respect to the atomic mass. Due

    to this special property, neutron

    can differentiate neighbouring

    elements in a material and even

    sees differently the different

    isotopes of an element.

    Neutrons also allow to probe

    light atoms that are barely visible

    with x-rays. The scattering

    length of neutron for a few

    isotopes of some elements

    are negative. Hydrogen has a

    negative scattering length

    ( -3.739 fm) while Deuterium

    possess a positive scattering

    length (6.671fm). Suitable

    combination of materials with positive and negative scattering length can be used to tune the neutron scattering contrast.

    Contrast matching experiments are used to obtain multi-level structures.

    As the neutron does not carry any

    electric charge, the neutron has no

    electrostatic interaction with the

    electron cloud of an atom. For this

    reason, the neutron has a higher

    penetration power comparable to

    x-ray or electrons.

    Neutron has a spin ½ and is sensitive

    to the magnetic fields created by

    unpaired electrons. In the magnetic

    materials, the order in magnetic

    structures and the interactions can be

    obtained using neutron scattering.

  • 6 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole no. T1011

    Monochromator Cu220

    Wavelength 0.995

    Scattering angle 0 o < 2θ < 90o

    Flux at sample 5x105 n/cm2/sec

    Detector BF3

    Counter

    The instrument is used to study a high

    precision 3-dimensional structure of

    materials, where hydrogen plays a

    major role in either the stereochemistry

    or the physical properties of the

    materials. These include hydrates,

    biomolecules, ferro-electrics, electro-

    optic materials, etc.

    The single crystal diffractometer is

    located at T1011 beam line of the

    Dhruva reactor. The crystal is rotated

    about three Eulerian axes χ, φ and ω,and the detector is rotated about the

    2θ axis. These four axes meet at a point,which is the centre of the sample

    crystal. The χ circle is mounted on theω axis, while the φ circle is mountedon the χ-axis as shown in Figure.The crystal is mounted on the φ-axis.The geometry of axes mounting

    enables any reciprocal lattice point to

    be brought into the equatorial plane

    of the diffractometer.

    Single CrystalNeutron

    Diffractometer

    This Four Circle Eulerian geometrybased Single Crystal NeutronDiffractometer is used forthe studies on hydrogen-bondedcrystal structures.

    Å

  • 7Bhabha Atomic Research Centre, Mumbai, India

    Selected examples

    . Hydrogen bonding studies in bis(glycinium) oxalate

    Fig.1. Showing the short hydrogen bond between glycinium and oxalate moiety

    Single-crystal neutrondiffraction investigation ofbis(glycinium) oxalate wasundertaken in order to studyits hydrogen bondingnetwork, particularly the veryshort hydrogen bondbetween the glycinum andoxalate ions, indicated by theX-ray diffraction study. Thenon-existence of any phasetransition in these crystals wasattributed to the fact that theshort hydrogen bond inbis(glycinium) oxalate is asymmetric in nature, with no hydrogen disorder (Fig. 1). The potential energy landscape for theabove-mentioned H atom was found to have a single minimum closer to the glycinium ion. IR and Raman investigations ofthe title complex supported the above result.

    Some references:

    1. R. Chitra and R. R Choudhury, Acta Cryst. B 63, 497 (2007).2. R.Chitra, R.R. Choudhury and M.Ramanadham, Appl. Phys. A 74 (suppl.), S1576 (2002).3. R.R. Choudhury, R.Chitra and M.Ramanadham, Appl. Phys. A 74 (suppl.), S1667 (2002).

    . Thiourea doped ammoniun dihydrogen phosphate

    Fig. 2. Packing of the thiourea dopeddihydrogen phosphate

    Thiourea Doped ADP (TADP) exhibits nonlinear optical property and thesecond harmonic generation efficiency of these crystals is three timesthat of pure ADP crystal. The single crystal neutron diffraction (Fig. 2)study of TADP gave cell parameters (a=b=7.531(3)Å,c=7.544(5)Å),which were found to be significantly greater from that of pure ADP atRT (a=b=7.502(1)Å,c=7.546(1)Å). This indicates that the dopantconcentration in the crystals is small but enough to bring changes in theoverall average structure. There is a significant lengthening of N-H—Ohydrogen bond in the Thiourea Doped ADP crystal.

  • 8 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole No. TT1015

    Monochromator Si (422)

    Monochromatortake –offangle (2θ

    M) 60°

    Wavelength 1.094 Å

    Detector One linear He3

    PSD, covers 30°in one PSDsetting

    (Sin θ/λ )max 0.64 Å-1

    Flux at sample 5x105 n/ cm2/sec

    Scattering angle 5o < 2θ < 90o

    Resolution (Δd/d) 1 %

    The diffractometer is extensively used

    for studying crystal and magnetic

    structures in a large variety of systems.

    These studies include titanates and

    zirconates showing ferro/anti-

    ferro-electric properties, alloys of

    transition metals, rare-earths and

    actinides (UCu2Ge

    2, ErFe

    2D

    x etc.)

    showing exotic magnetic properties,

    ferrites exhibiting disordered

    magnetic ordering, manganites

    showing CMR behaviour, and

    cobaltates showing coexistence of

    ferro- and antiferromagnetism, etc.

    PowderDiffractometer-1

    This instrument is installed atThrough-tube beam hole no TT1015and has been used to carry out medium-resolution powder diffractionmeasurements on a variety ofmagnetic and nonmagnetic systems.

    S.K. Paranjpe and Y. D. Dande, Pramana-J. Phys. 32, 793 (1989).S.K. Paranjpe and S. M. Yusuf, Neutron News 13, 36 (2002).

  • 9Bhabha Atomic Research Centre, Mumbai, India

    Neutron powder diffraction patterns of CaTiO3 (CT)

    and Sr1-x

    CaxTiO

    3 (SCT) with x = 0.04 and 0.50. For

    the CT and SCT (x=0.50) samples, superlattice linesare observed.

    Temperature variation of I531

    / I006

    for Sr1-x

    CaxTiO

    3 (SCT) with

    x = 0.06 and 0.12. The antiferrodistortive phase transition isobserved around 300 K and 375 K for x = 0.06 and 0.12,respectively.

    Some references:

    1. V. G. Sathe et al., J. Phys.-Cond. Matter 10, 4045 (1998).2. R. Ranjan et al., J. Phys.-Cond. Matter 11, 2233 (1999).3. P. Raj et al., Phil. Mag. B 79, 1185 (1999).4. A. Das et al., J. Magn. Magn. Mat. 237, 41 (2001) .5. S. M. Yusuf et al., Phys. Rev. B 68, 104421(2003).

    Selected examples

    . Mixed Ferrites: Disordered Magnetic Systems: Magnetic ordering in Zn0.5

    Co0.5

    FeCrO4

    The evolution of themagnetic structure factorwith temperature for (a)the (220) reflection and(b) the (222) reflectionfor Zn

    0.5Co

    0.5FeCrO

    4.

    Solid curves: The Brillouinfunctions

    Difference neutron diffraction patterns at 40,20, and 15 K with respect to 200 K forZn

    0.5Co

    0.5FeCrO

    4 showing the buildup of the

    diffuse hump at ~20 K around a Q-value wherethe (200) Bragg peak is expected.

    . Structural phase transition in ferroelectric materials

  • 10 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole no. T1013

    Monochromator Ge (331)

    Wavelength 1.249 Å

    Beam size 4.0 cm x1.5 cm

    Flux at sample 8.5x105 n/cm2/sec

    Scattering angle 4o < 2θ < 140o

    Q range 0.4 – 9.4 Å-1

    Δd/d ~ 0.8 %

    Detector 5 PSDs (to beupgradedto 15 PSDs)

    Sampleenvironment 10 – 300 K

    PowderDiffractometer-2

    This Powder diffractometeris a conventional medium resolutionneutron diffractometer. It is mainly used tostudy stuctural and magnatic ordering inpolycrystalline materials.

    Powder diffractometer is a multi-PSD

    based instrument covering Q-range

    up to 9.4 Å-1. This instrument is being

    extensively used by researchers all over

    the country to study structural and

    dimensional magnetic materials,

    molecular magnetic materials and also

    in studies of local structure

    determination from disordered

    crystalline systems.

    magnetic transitions in alloys and

    compounds. It has been used for

    structural studies of a number of CMR

    materials, ferro-electric materials, high

    Tc materials, SOFC materials, low

  • 11Bhabha Atomic Research Centre, Mumbai, India

    Selected examples

    . Low temperature structural phase transitions in NaNbO3

    Material engineering of alkaline niobates like potassium sodium niobate and lithium sodium niobate with ultralarge piezo

    response comparable to PZT have evoked considerable interest as the next generation eco-friendly lead free piezo ceramics

    required for applications as transducers in cell phones, medical implants, etc. The end member NaNbO3 has an antiferroelectric

    (AFE) structure at room temperature and exhibits an unusual complex sequence of temperature and pressure driven

    structural phase transitions which are not clearly understood. Accurate characterization of the phase diagram of NaNbO3 is

    essential for the design of new sodium niobate based ceramics required for applications. Powder neutron diffraction

    studies have been used to understand the complex sequence of low temperature phase transitions of NaNbO3 in the

    temperature range between 12 and 350 K. Our studies present unambiguous evidence for the presence of the ferroelectric

    (R3c) phase (FE) of NaNbO3 coexisting with an antiferroelectric phase (Pbcm) over a wide range of temperatures. (S.K.

    Mishra et al., (2007).

    The physical properties in charge ordered manganites are influenced by magnetic

    field, pressure, and substitution effects. Here we study the effect of change in

    ionic radii on the magnetic structure and its influence on the measured physical

    properties. The figure shows a section of the neutron diffraction pattern of

    La0.5

    Ca0.5-x

    SrxMnO

    3 at 15 K. With increase in Sr concentration the magnetic

    structure evolves from a CE-type antiferromagnet to ferromagnet with an

    intermediate A-type antiferromagnetic structure. The magnetic structure

    influences the magnetic and transport properties .

    Some references:

    1. S.K. Mishra et al., Phys. Rev. B 76, 024110 (2007).

    2. I. Dhiman et al., Solid State Communications 141, 160 (2007).

    3. S. Taran et al., J. Phys. Cond. Matter (in press).

    4. Brajendra Singh et al., J. Appl. Phys. 101, 09G518 (2007).

    5. S. N. Achary et al., J. Alloys and Compounds 438, 274 (2007).

    Structure of NaNbO3

    913 K (PE)300 K (AFE) 12 K (FE)

    . Evolution of magnetic structures in charge ordered manganites

  • 12 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole no. TT1015

    Monochromator Bent perfect Si

    Wavelength 1.48 Å(standard)

    Beam size 15 × 25 mm2

    Flux at sample 7×107 n/cm2/sec

    Scattering angle 6 – 123O

    Q range 0.4 – 7.4 Å-1

    (1.48 Å)

    Δd/d ~ 0.3%

    Detector 4 Linear 3HePSDs (to beupgraded to12 nos.)

    PowderDiffractometer-3

    This diffractometer, installed recently,with focusing monochromator,is expected to be widely used in thearea of chemical and magnetic structuresof novel materials.

    This powder diffractometer developed

    and installed by UGC-DAE

    Consortium for Scientific Research, is

    a multi-PSD high throughput

    diffractometer. It employs a bent

    perfect crystal monochromator at a

    take-off angle of 90

    degrees and it is

    designed for a

    highly focused

    neutron beam of

    about 15 x 25 mm2

    in size. This would

    enable high flux

    at sample position

    and also use of

    small samples

    (~1 cc in volume).

    The resolutions obtained are up to

    Δd/d ~ 0.3%.

    The monochromator can be rotated or

    flipped to give a range of wavelengths

    from 1.1 to 2.3 Å. The sample

    environment consists of a 4 K CCR for

    standard measurements as a function

    of temperature and a cryogen-free

    7 Tesla magnet with VTI for in-field

    measurements down to 1.4 K. An

    oscillating radial collimator (under

    installation) will be used to suppress

    extraneous contributions from the

    magnet and CCR shrouds. The data

    acquisition system, developed locally,

    has an input for up to 16 PSDs and

    the software enables recording various

    sequences of measurements with

    respect to incident neutron flux and

    sample temperature.

  • 13Bhabha Atomic Research Centre, Mumbai, India

    . Monochromator Rocking Curve and Beam Profiles

    Rocking curve of bent perfect Si monochromator at a take-off angle of 90º

    and λ = 1.48 Å. Figures on right show the horizontal and vertical beamprofiles measured at sample position.

    Some references:

    1. A.V. Pimpale, B.A. Dasannacharya, V. Siruguri, P.D. Babu, P.S. Goyal, Nucl. Instrum. Meth.A481 (2002) 615

    2. S. Patnaik et al (unpublished)

    . Neutron diffraction pattern of YMnO3 taken at room temperature [2] at λ = 1.48 Å.

  • 14 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole No. T1009

    Wavelength 1.201 Å

    Beam polarization 98.83%

    Flipper RF flipper /DC flipper

    Flux at sample 3.6x105

    n/cm2/sec

    Scattering angle 0o < 2θ < 120o

    Analyzer efficiency 97.36% /99.89%

    Detector BF3 counter

    Available T range 1.5 – 300 K

    Available H 1.2 kOe

    The polarized neutron spectrometer (PNS) is used for magnetic

    scattering studies. This spectrometer can be used in different

    modes, such as (a) diffraction mode (2-axis configuration), (b)

    polarization analysis mode (3–axis configuration in scattering

    geometry), and depolarization mode (3-axis configuration in

    transmission geometry). The instrument has been used for

    studying mixed ferrites, 3d-based alloys, uranium / thorium /

    cerium based intermetallic compounds, amorphous magnets,

    CMR perovskites, quasi 1-D spin chain compounds, etc.

    PolarizedNeutron

    Spectrometer

    This PNS instrument is installedat the end of the tangential beamhole No. T1009. The spectrometeris used for magnetic correlation studies.

    S. M. Yusuf and L. Madhav Rao, Neutron News 8, 12 (1997).S. M. Yusuf and L. Madhav Rao, Pramana- J. Phys. 47, 171 (1996).

  • 15Bhabha Atomic Research Centre, Mumbai, India

    Selected examples

    . Magnetic and Electronic Phase Transitions-Ionic Size Effect in (La1-x

    Dyx)0.7

    Ca0.3

    MnO3

    CMR Perovskites

    Increasing Dy concentration drives the system first into a local cantedferromagnetic (LCF) state with a reduced metal-insulator transition temperature(for x = 0.114 and 0.243) and then (for x = 0.347) to an “insulating”cluster-spin glass state .

    . Neutron Depolarization Study on CMR Perovskites (Nd1-x

    Tbx)0.55

    Sr0.45

    MnO3

    Some References:

    1. S. M. Yusuf, L. Madhav Rao and P. Raj, Phys. Rev. B 53, 28 (1996).2. S. M. Yusuf et al., Solid State Commun. 112, 207 (1999).3. S. M. Yusuf, M. Sahana, K. Dorr, U.K. Röbler and K. H. Müller, Phys. Rev. B 66, 064414 (2002).4. S. M. Yusuf et al., Phys. Rev. B 68, 104421 (2003).5. S. M. Yusuf et al., J. Magn. Magn. Mater. 272-276, 1288 (2004).

    The crossover from long-range to short-range magnetic ordering in the CMR perovskites is studied by complementaryneutron scattering techniques. A canted ferromagnetic state for x < 0.5 with large domains (> 1000 nm), ferromagnetic-like spin clusters of ~ 100 nm size for 0.5< x < 0.6 and only short range correlation of ~ 5 nm for x > 0.6 compositions havebeen observed.

  • 16 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole no. HS1019

    Monochromator Cu (220): λ = 0.783ÅCu (111): λ = 1.278Å

    Flux at sample 2x106 (λ = 1.278 Å(n/cm2/sec) 3x105 (λ = 0.783 Å)

    Sample size 40 mm high &5-10 mm dia

    Scattering angle 3o < 2θ < 140o

    Detector 10 (1-d PSDs)at 5 positions

    Q range 0.3 – 15 Å-1

    ΔQ/Q 2.5 %

    Hi-Q diffractometer is a multi-

    PSD based instrument covering

    Q-range up to 15 Å-1. It has been used

    for structural studies of a number of

    molecular fluids, chalcogenide

    glasses,borate glasses, phosphate

    High - QDiffractrometer

    This High-Q diffractometer is a conventionalneutron powder diffractometer with highQmax (=15 Å-1) with λ = 0.783 Å and isused mainly to understand short rangeorder in glasses, liquids and disorderedcrystals.

    glasses, tellurite glasses, sulphide

    glasses, amorphous carbon and also

    in studies of local structure

    determination from disordered

    crystalline systems. This diffractometer

    has also been used to study high

    pressure structural phase transitions

    in α-Resorcinol, NbO2F etc., using a

    home made piston cylinder type

    pressure cell using EN45 steel as the

    cell material.

  • 17Bhabha Atomic Research Centre, Mumbai, India

    Selected examples

    . H-bonded simple alcohols

    Simple alcohols like CD3OD, t-butanol

    and 2-propanol show intermediate

    range order characterized by

    a pre-peak which is due to molecular

    clusters (mainly hexamer) through

    H-bond association. On the other

    hand 1-propanol does not show any

    pre-peak and the H-bonded

    association of the molecules lead to

    open chain clusters instead of closed

    cyclic chain clusters. The main reason

    is that the first group of alcohols all

    have methane like structure where as

    1-propanol is a linear molecule. The

    top right hand side figure shows

    schematic of the cyclic chain clusters

    . Rare earth phosphate glasses: Radioactive waste storage materials

    T(r) shown for R=Ce glass showing

    the P-O, R-O & O-O distances. PO4

    tetrahedra are the basic building blocks in

    these glasses

    Glasses with general formula 0.1La2O

    3 - 0.1R

    2O

    3 - 0.05Al

    2O

    3 – 0.75P

    2O

    5 are candidates of radioactive waste storage

    materials as they are chemically durable and pouring temperatures are low. Some phosphate glasses have low leachingrates compared to the alternative borosilicate glasses. We found that these glasses have mainly PO

    4 tetrahedral units. R-O

    co-ordination is about 6 to 8. A 3D-hand built model is displayed with the intention of confirming the feasibility ofconstructing a continuous random network. Some of these glasses are found to be good candidates as UV filters anda patent has been obtained for the same.

    Some References:

    1. A.G. Shikerkar et al., J. Non-Cryst. Solids. 270, 234 (2000).2. A.K. Karmakar et al., Phys. Lett. A 253, 207 (1999).3. P.P. Nath et al., Z. naturforschungs 56a, 825 (2001).4. A. Sahoo et al., Pramana – J. Phys. 63, 183 (2004).5. Keka R. Chakraborty et al., Pramana – J. Phys. 63, 245 (2004).

    n 2-propanol whereas the bottom one shows open chain clusters in 1-propanol.

  • 18 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam port Guide G1

    λ* (guide cut-off) 2.2 Å

    Monochromator BeO Filterat 77 K

    λcut-off 4.7 Å

    λaverage 5.2 Å

    (Δλ/λ) ~15 %

    Flux at sample 2.2×105 n/cm2/sec

    Source slit (S1) 3 cm × 2 cm

    Sample slit (S2) 1.5 cm × 1 cm

    Distance S1 & S2 2 m

    Angular divergence ± 0.5o

    Detector (D) linear He3-PSD

    Distance S2 & D 1.85 m

    Q range 0.017 – 0.35 Å-1

    The SANS diffractometer is widely

    used to investigate the structure(shape and size) of different kinds of

    mesoscopic systems such as micellarsolutions, magnetic fluids, protein

    solutions and colloidal suspensions.

    Small-angleNeutron

    ScatteringDiffractometer

    This SANS diffractometer isinstalled at the end of one ofthe guides. The diffractometeris suitable for studies ofinhomogeneities of the sizesin the range 10 – 200 Å.

    This is a conventional slit-geometry SANS diffractometer. It makes use of BeOfilter as a monochrometer. The beam passes through two slits S1 and S2 before

    it is incident on the sample. The angular distribution of neutrons scattered by thesample is recorded using a 1-m linear positive sensitive detector.

    V.K. Aswal and P.S. Goyal, Current Science 79, 947 (2000)

  • 19Bhabha Atomic Research Centre, Mumbai, India

    Selected examples

    . Protein crystallization in aqueous salt solutionThe process of proteincrystallization is of interestfrom both scientific andbiological aspects.Structural evolution amongprotein macromolecules isan important step inunderstanding the processthat the system isundergoing duringcrystallization. It has beenobserved that the effect ofsalt concentration as well

    as that of different salts on protein crystallization is markedly different (Fig. 1). SANS data suggest that difference in thecrystallization on varying concentration/type of salt is related to the differences in structures in these samples in terms of thepopulations of monomers and dimmers (Fig. 2). Higher-mers are not observed as they are formed in very small numberstowards the process that leads to crystallization.

    . Tuning gelation of block copolymer/surfactant mixed systemsS e l f - a s s e m b l ybehavior of theP E O - P P O - P E Obased triblockcopolymers havebeen studied quiteextensively in viewof their richs t r u c t u r a lp o l y m o r p h i s mand numerousapplications in theindustries. In manyapplications, they

    are used in combinations with ionic surfactants like SDS, CTAB etc. Fig. 4 shows lower (T1) and upper (T2) meltingtemperature of cubic gels formed by 25% of block copolymer (EO)20(PO)70(EO)20 solutions as a function of SDS concentration.The gel phase can be tuned by the ratio of the two components. Contrast variation SANS studies show that the blockcopolymer and SDS form mixed micelles comprising a uniform distribution of the respective molecules (Fig. 4).

    Some references

    1. V.K. Aswal and P.S. Goyal, Phys. Rev. E 6161616161, 2947 (2000).2. J. Sharma, V.K. Aswal, P.S. Goyal and H. Bohidar, Macromolecules 3434343434, 5215 (2001).3. J. Haldar, V.K. Aswal, P.S. Goyal and S. Bhattacharya, Angew. Chem. Int. Ed. 4040404040, 1228 (2001).4. S. Chodankar and V.K. Aswal, , , , , Phys. Rev. E 7272727272, 041931 (2005).5. R. Ganguly et al., J. Phys. Chem. B 110110110110110, 9843 (2006).

    Fig. 4Fig. 4Fig. 4Fig. 4Fig. 4Fig. 3Fig. 3Fig. 3Fig. 3Fig. 3

    Fig. 1Fig. 1Fig. 1Fig. 1Fig. 1 Fig. 2Fig. 2Fig. 2Fig. 2Fig. 2

  • 20 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam port Guide G1

    Monochromator Si(111)

    Wavelength (λ) 3.12 Å

    (Δλ/λ) ~1 %

    Flux at sample 500 n/cm2/sec

    Analyser Si(111)

    Q range 0.0003-0.0173 Å-1

    Real space 200 - 10000 Åresolution

    Detector BF3 Counter

    This facility is widely used toinvestigate the mesoscopicinhomogeneties in ceramics,metallurgical alloys, naturallyoccuring porous media like rock etc.

    In this kind of double crystal basedinstruments, unlike pinholecollimation instruments, thecollimation is performed in thereciprocal space only and theresolution in wave vector transfer Q isindependent of the beam crosssection. Because of the non-dispersive setting of both the crystals,the width of the rocking curve isindependent of the divergenceof the incoming beam.

    DoubleCrystal based

    SANSInstrument

    This is a double crystal based mediumresolution small-angle neutron scatteringinstrument built and commissioned at theguide tube laboratory. The instrumentconsists of a non-dispersive (1, -1) setting of(111) reflections of silicon single crystals withsample between the two crystals.

    S. Mazumder, D. Sen, T. Saravanan and P. R.Vijayaraghavan,J. Neutron Research 9, 9, 9, 9, 9, 39 (2001)

  • 21Bhabha Atomic Research Centre, Mumbai, India

    Selected examples

    . Effect of pore structure on low frequency dielectric response in ZrO2-8 %Y2O3 ceramic compact

    Yttria stabilized zirconia is

    a potential candidate forsolid oxide fuel cell

    applications. SANS data forZrO2-8 % Y2O3 pellet

    samples with identicalporosity but prepared from

    finer and coarser grain areshown (left). Scattering

    experiments have beencarried out for

    two different samplethicknesses in order to

    correct for multiple scattering. The real and the imaginary components of the dielectric response forthese samples are depicted (right). The variation in the dielectric response has been explained by a pore

    structure dependent interfacial polarization, ion hopping and conduction.

    . Carbide precipitates in solution quenched PH 13-8 Mo stainless steelPH13-8 Mo, because of itshigh strength andtoughness, coupled with

    good corrosion resistance, isoften used in aircraft, nuclear

    reactor, petrochemical plantsand many other challenging

    applications. SANS data fromsolution quenched (from

    1000oC) sample for twodifferent sample thickness

    are shown (left). Theestimated single scattering profile is also shown in the inset. TEM (left inset) shows the presence block like precipitates. The

    size distribution of the parallelepiped block precipitates, estimated from SANS, is shown (right).

    Some references

    1. D. Sen, S. Mazumder and S. Tarafdar; J. Mat. Sci 3737373737, 941 (2002).2. S. Mazumder et al. Phys. Rev. Lett. 9393939393, 255704 (2004); S. Mazumder, et al Phys. Rev. B 7272727272, 224208 (2005).3. D Sen, T. Mahata, A K Patra, S Mazumder and B P Sharma; J. Phys.: Condens. Matter 1616161616, 6229 (2004).4. D. Sen et al. Mat. Sci. & Eng A 397397397397397, 370 (2005); J. Mittra et al. Scripta Materilia 5151515151, 349 (2004).5. A.K. Patra, S. Nair, A.K. Tyagi, D. Sen, S. Mazumder, S. Ramanathan; J. Alloys and Comp. 403403403403403, 288 (2005).

  • 22 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Monochromator Si(113)

    Wavelength 2.5 Å

    ΔQ/Q 0.141 - 0.411

    Polarizer FeCo/TiZrsupermirror

    Flux at sample 104 n/cm2/sec

    D.C. flipper 92 %efficiency

    Detector linear He3 PSD

    Reflectivity 1 – 10-4

    The reflectometer uses a linear position sensitive detector, which helpsto collect the off-specular reflectivity data in addition to specular

    reflectivity data from the thin film samples, in a single setting.

    This facility has been widely used for structural and magneticcharacterization of thin film samples, using specular and off-specular

    techniques.

    Reflectivity is intrinsically sensitive to the difference of the refractiveindex (or contrast) across any interface. For the case of specular

    reflection, the intensity of the reflected beam is related to the depthdependence of the index of refraction averaged over the lateral

    dimensions of the sample. Polarized neutron reflectometry is a uniquetechnique to study the depth profile of magnetic moment in multilayer.

    Off-specular or diffuse neutron reflectivity is a widely used techniqueto understand surface (interface) morphology.

    PolarizedNeutron

    Reflectometer

    The polarized neutron reflectometeris located in Guide Tube laboratory.The reflectometer has been designed forvertical sample geometry. It utilizes ahighly collimated monochromatic:polarized or unpolarized beamof neutrons.

    Saibal Basu and Surendra Singh, J. Neutron Research 1414141414, 109 (2006).

  • 23Bhabha Atomic Research Centre, Mumbai, India

    Selected examples

    . Investigation of interface magnetic moment in Fe/Ge multilayer

    Metal-semiconductor interfaces display transport and magnetic properties which strongly depend on interface quality viz.roughness, alloying at interfaces, and magnetic moment at interface. Polarized neutron reflectivity data on Fe/Ge multilayers(left and right) have been used to clearly demonstrate that there is overall reduction in magnetic moment of Fe atoms as wellas asymmetry of moments at the Fe/Ge interfaces.

    . Corrosion-induced morphology in Ni Film: a study in off-specular reflectometry

    The microscopic fractal morphology of corrosion front at the exposed air-film interface of a Ni film as well as the morphologyof an interface buried below the affected surface layer have been used to determine off-specular neutron reflectivity (right)and specular neutron reflectometry (left) in unpolarized mode. Differences in morphology, of a hidden interface vis-à-visthe exposed surface under corrosion (middle), at microscopic length-scales have been quantified in terms of fractaldimension of these two surfaces.

    Some references

    1. Surendra Singh, Saibal Basu, M. Vedpathak, R. H. Kodama, R. Chitra and Y. Goud, Appl. Surf. Sci. 240240240240240,251 (2005).

    2. Surendra Singh, Saibal Basu, A.K. Poswal and M. Gupta, Solid State Comm. 136136136136136, 400 (2005).3. Surendra Singh and Saibal Basu, Surf. Sci. 600600600600600, 493 (2006).4. Surendra Singh, S.K. Ghosh, Saibal Basu, M. Gupta, P. Mishra and A.K. Grover, Electrochem. & Solid State Lett.

    99999, J5 (2006).5. Surendra Singh, Saibal Basu, Mukul Gupta, Mahesh Vedpathak, and R.H. Kodama, J. Appl. Phys. 101101101101101,

    33913 (2007).

  • 24 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam port Guide G2

    λ∗ (guide cut-off) 3.1 Å

    Monochromator BeO Filter (77 K)

    λcut-off 4.7 Å

    λaverage 5.2 Å

    (Δλ/λ) ~15 %

    Flux at sample ~105 n/cm2/sec

    Detector (D) linear He3-PSD

    Real space length 20-400 Åscale

    Q range (SANS) 0.015 – 0.3 Å-1

    Spin Echoand

    Polarized SANSInstrument

    This instrument consistsof two arms,i) Spin echo andii) polarised neutronssmall angle scattering.

    The spin echo technique is used tostudy stochastic dynamics of polymers,

    macromolecules etc. BeO filterproduces a quasi-monochromatic

    neutron beam. A focusing soller-typemulti-segment supermirror based

    polarizer and analyzer are used topolarize and analyze the neutrons.

    Similar π and π/2 flippers are used tochange the direction of neutron

    polarization. A multilayer copper wiresolenoid is used as guide field to

    initiate Larmor precession of theneutrons. A 3He detector is used to

    detect the neutrons. The maximumq-range is 1 Å-1. Dynamical systems

    of real space correlations of about10 Å and a time scale of 1 ns can be

    investigated.

    The small angle scattering instrument is a slit geometry configuration, using BeO

    filter cooled at liquid nitrogen temperature. The incident neutrons are polarizedusing a multi-segment soller type

    supermirror polarizer (Co/Ti coatedwith anti-reflecting Gd coating). The

    distance between the sample and thedetector is 2.21 m which may be

    increased to about 3 m. This setup canbe used to investigate shape and size

    of different mesoscopic systems likemicellar solutions, proteins and the

    study of magnetic inhomogeneties.

  • 25Bhabha Atomic Research Centre, Mumbai, India

    Some references

    1. S. L. Chaplot, R. Mittal, Prabhatasree Goel, Appl. Phys. A7474747474 (suppl). S280 (2002).2. S. L. Chaplot, R. Mittal, K. N. Prabhatasree, Neutron spin echo spectroscopy, eds. F. Mezei, C. Pappas and T.

    Gutberlet (Springer verlag, Berlin 2003) p 48.

    Selected examples

    . Surfactants in aqueous solution

    Surfactants are amphiphilic molecules with water repelling and water loving ends, they self-assemble to form micelles inaqueous solutions. SANS data on 0.2 M micellar solution of anionic surfactant Sodium Dodecyl Sulphate prepared in D2Oare shown. SANS distribution shows a correlation peak at Qmax ~ 0.07 Å

    -1, which is due to a peak in the interparticlestructure factor S(Q). This corresponds to average distance (~2π/Qmax) between micelles of about 90 Å.

    . Cobalt precipitates in Copper annealed at 560O CSmall angle neutronscattering studies on diluteCu alloy with 0.8 at %Co havebeen carried out. Cobalt formsprecipitates whose sizesdepend on reaction kinetics.The sample studied wassolution treated at 950OC for3 hrs in a vertical furnace inargon atmosphere, followedby rapid quench into waterat room temperature andannealed at 560OC for 80minutes.

  • 26 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole no. T1007

    Monochromator Cu(111)

    ΔE range 3 – 200 meV

    Q range 1 – 10 Å-1

    lncident 0.6 – 2.3 Åwavelength range

    Flux at sample 106 n/cm2/sec

    Analyzer PG(0002)

    Filter PG

    Scattering angle 10o – 100o

    Detector BF3 Counter

    Triple AxisSpectrometer

    This instrument is used tostudy inelastic Neutron Scatteringfrom single crystals andpolycrystalline samples.

    This instrument has been successfullyemployed for measurement of phonondispersion curves, phonon density ofstates, crystal field excitations andquasielastic scattering.

    The geometry of the triple axisspectrometer allows measurements ofthe scattering function S(Q,E) in singlecrystals at well defined values ofmomentum transfer Q and energytransfer E.

    Principal components of thisinstrument are:

    (i) Monochromator that producesthe mono-energetic neutronbeam.

    (ii) Positional spectrometer that setsthe angles φ and ψ.

    (iii) Analyzer that measures theoutgoing energy.

    Various arms of the spectrometer canbe moved at angular speeds of severaldegrees/ minute by means of wormgear assemblies.

    The shielding wedges of the monochromator shield are lifted automatically toallow for continuous variation of the monochromator settings.

    S.L. Chaplot, R. Mukhopadhyay, P.R. Vijayaraghavan, A.S. Deshpande andK.R. Rao, Pramana - J. Phys. 3333333333, 595 (1989).

  • 27Bhabha Atomic Research Centre, Mumbai, India

    Selected examples. Al2SiO5: Andalusite, a polymorph having five-coordinated aluminiumAl2SiO5 exists in threepolymorphic forms: sillimanite,

    andalusite and kyanite with onealuminium in tetrahedral, five-

    coordination and octahedralcoordination respectively. These

    display unique phase transitionswith pressure and temperature

    and the phase diagram hasextensive applications in

    geophysics. Experiments on allthree phases validated a

    transferable interatomic potentialto explain vibrational and

    thermodynamic properties of these polymorphs. (Left) Polyhedral representation of andalusite crystal structure with AlO6octahedra in red, five-coordinated Al in blue, SiO4 tetrahedra in yellow. (Right) Measured (solid squares) and calculated

    (solid line) phonon dispersion curves along the Σ direction in andalusite. The (zone centre) phonon frequencies knownfrom Raman (open triangle) and infrared (open diamond) measurements are also shown.

    . M2O (M=Cu, Ag): Negative Thermal Expansion materialsM2O (M=Cu, Ag)

    exhibits negative thermalexpansion (NTE).

    Experiments helped todevelop lattice dynamical

    model which identifiedlibrational mode related

    to NTE, explainedbond length variation

    in agreement withpublished EXAFS data, and stabilized lattice with a single M-M potential. (left) Experimental and calculated phonon spectra

    for Cu2O. (centre) Structure of M2O. The solid circles denote M and O atoms in decreasing order of size. (right) Polarizationvector of T2u mode shows rotation of M4O (M=Cu,Ag) tetrahedra about the aaaaa axis.

    Some references

    1. R. Mittal, S.L. Chaplot, S.K. Mishra, Preyoshi P. Bose, Phys. Rev. B75 (2007) 174303.2. A. Sen, Mala N. Rao, R. Mittal, and S.L. Chaplot, J. Phys.: Condens. Matter, 17 (2005) 6179.3. R. Mukhopadhyay, A. Sayeed, Mala N. Rao, A.V. Anilkumar, S. Mitra, S. Yashonath, S.L. Chaplot, Chem.Phys.

    292 (2003) 217.4. R. Mittal, S.L. Chaplot, A. Sen, S.N. Achary, A.K. Tyagi, Phys. Rev. B 67 (2003) 134303.5. P. Goel, Mala N. Rao, N. Choudhury, S.L. Chaplot, Subrata Ghose, M. Yethiraj, Appl. Phys. A 74 [Suppl.]

    S1149 (2002).

  • 28 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole no. TT1004

    Monochromator (2 nos. in tandem)crystals (2nd one vertically focused): PG(0002) (100 × 80 mm2)

    λincident 1.3 – 4.7Å

    Scattering angle 2θ< 80O

    Flux at sample 5 ×105 n/cm2/sec

    Analyser PG(0002)(MARX Mode)

    ΔE range 2.3 meV(for Ei=4 meV)

    ΔE/E 4 %

    QuasiElastic Neutron

    Scatteringinstrument

    This instrument is used to studyStochastic Motion (like Diffusion) inCondensed Matter. ‘Quasi’ means nearelastic (≤ 2 meV). Provides informationabout the time scale and geometry ofdiffusive motion as also the potentialexperienced by the species.

    Some distinct features of thisinstrument are mentioned below:

    • Virtue of Double Monochromator,neutrons of different incident

    energy can be obtained at a fixedsample position

    • The instrument works in Multi

    angle Reflecting X-tal mode (MARX)thereby facilitating complete energy

    spectrum for one instrumentalconfiguration.

    • Provision to change in the distance

    between different axes to obtaindifferent energy resolutions.

    • The out-of-pile portion of the

    instrument is on a ‘tanzboden’facilitating easy maneuvering

    R. Mukhopadhyay et al. , Nucl. Instr. Meth. A 474 474 474 474 474, 55 (2001).S. Mitra and R. Mukhopadhyay, Current Science 8484848484, 653 (2003)

  • 29Bhabha Atomic Research Centre, Mumbai, India

    Selected examples. Alkyl Chain Dynamics in Monolayer Protected Metal nano-Clusters (MPCs)

    Schematic of MPCs system

    A) Isolated MPCs (Au-clusters): Chains are dynamic only above Tc (340 K: chain melting) and all the chains are dynamic.B) Superlattice MPC (Ag-clusters): Only chains (50 %) are dynamic < Tc (393 K: Superlattice melting) Others held due to

    interdigitation . T> Tc all the chains dynamics.

    . Diffusion of Molecular absorbed in Zeolite

    MD Simulation results show translational motion exists in three differenttime scales. Only one contributes to QENS-data (Red circle). Rotational motion

    is much faster and measurable in Triple axis spectrometer with a wider energywindow.

    Rotational Diffusion coefficient

    of propane in Na-Y zeolite

    Some references

    1. T. Pradeep, S. Mitra, A. Sreekumaran Nair, R. Mukhopadhyay, J. Phys. Chem. B 108108108108108, 7012 (2004).2. A. Sayeed, S. Mitra, A. V. Anil Kumar, R. Mukhopadhyay, S. Yashonath, S. L. Chaplot, J. Phys. Chem. B 107107107107107,

    527 (2003).3. R. Mukhopadhyay, A. Sayeed, S. Mitra, A. V. Anil Kumar, Mala N. Rao, S. L. Chaplot, S. Yashonath Phys.

    Rev. E 6666666666, 061201 (2002).4. Siddharth Gautam, S. Mitra, R..Mukhopadhyay, S. L. Chaplot, Phys. Rev. E 7474747474, 041202 (2006).5. S. Mitra, R. Mukhopadhyay, A. K. Tripathi, N. M. Gupta, Applied Physics A 7474747474, S1308 (2002).

  • 30 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole no. HS1017

    Monochromator Doubly focusingCu(111)

    ΔE range 15 – 250 meV

    Q range 1 – 10 Å-1

    Incidentwavelength range 0.6 – 2.3 Å

    Flux at sample 106 n/cm2/sec

    Analyzer Be filter

    Scattering angle 10O – 100O

    Detector BF3 Counter

    FilterDetector

    Spectrometer

    This instrument is usedto study inelastic neutron scatteringfrom condensed matter.

    Principal components of thisinstrument are:

    (i) Monochromator that producesthe mono-energetic neutronbeam

    (ii) positional spectrometer that setsthe scattering angle.

    (iii) Analyzer that measures theoutgoing energy.

    Continuous variation of the incidentneutron energy is allowed for by liftingof the shielding wedges of themonochromator shield.

    The scattered neutron beam from thesample is filtered by polycrystalline Bemade of beryllium blocks interleavedwith cadmium, intended to capture anyBragg diffracted neutrons. Theneutron scattering cross section of Beexhibits a sharp drop at a neutronenergy of 5 meV. Thus, neutronswhose energy is less than 5 meV areallowed to pass through the filter andall others are scattered out of thebeam.

    C.L. Thaper, B.A. Dasannacharya,, and P.K. Iyengar, Nucl. Instr. Meth. 113(1973) 15.

  • 31Bhabha Atomic Research Centre, Mumbai, India

    Selected examples. Libration of NH4+ ion in NH4Cl at RT (CsCl Phase)Ammonium chloride NH4Cl is a simple ionic crystal containing distinctNH4

    + tetrahedra. At atmospheric pressure, three phases of ammonium chloridehave been found to exist. Above 243 K (i.e. in the CsCl (disordered) phase), theNH4

    + ions are randomly distributed between two possible orientations,with N-H bonds lying along threefold axes (body diagonals). Ammonium ions inthis room temperature phase may be considered torsional oscillators withfrequency ~ 359 cm-1 (~45 meV). This libration mode exhibits a ratherflat dispersion in the Brillouin zone, with the next branch occurring at least15 meV away.

    . Vibration of Hydrogen in Zirconium Hydride (ZrH2)The thermal vibration spectrum ofzirconium hydride includes (in additionto the band of acoustical frequencies)a sharp “optical” frequency νcorresponding approximately tovibrations of the individual hydrogenatoms in an isotropic harmonic well.This implies a set of optical energylevels for the lattice En=nhν. Peakscorresponding to transitions betweenthese optical energy levels will be seenin the spectrum of neutrons scatteredfrom zirconium hydride. The firsttransition is observed as a peak at anenergy transfer of about 140 meV.

    The data shown on this page have been taken on an instrument with a PG (0002) monochromator.

  • 32 Bhabha Atomic Research Centre, Mumbai, India

    Instrument parameters

    Beam hole No. 6 of Apsara,a swimming pool type Reactor

    Useful beam size: 15 cm dia.

    Thermal NeutronFlux: (n/cm2/sec) 1 x 106

    Gamma level: 4R/h

    Cadmium ratio: 6.3

    Neutron/gammaratio: (n/cm2/mR) 9 x 105

    NR Techniques used:converter screens : Gd (25 μm), Dy(100 μm), CCD- based imagingsetup, Neutron Imaging plate

    NeutronRadiography

    Applications

    Non-Destructive Testing andEvaluation of :Nuclear fuel pins,fuel plates,ControlRods, INSAT-pyrovalves & cable cutters,electric detonator, marker shells, boralcomposites

    Hydride blisters in zircaloy-2 and Zr-2.5%Nb PT coupons (lab generatedand from power reactor).

    Hydrogen Sensitive EpithermalNeutron Radiography

    Real time imaging, Two-phase flowstudy, Neutron tomography.

    NR Facility At Beam Hole No. 6, Apsara reactor.

    Schematic (above) Photograph of the Facility (below).

    NR Album : Neutron radiographs of various objectsrecorded using film techniques

    (1) INSAT Cable cutters

    (2) INSAT Pyro valve(3) Fuel pins

    (4) Flower plant through lead brick(1) (2) (3) (4)

    ←←←←←

  • 33Bhabha Atomic Research Centre, Mumbai, India

    Selected examples. Study of zirconium Hydride blister formation in zirconium based PHWR pressuretube materials.

    A zirconium hydride blister of nearly 0.35% of job thickness could be detected using neutron radiography.

    (1) (2)Hydride blisters in zircaloy-2

    (1) and Zr-2.5%Nb(2) PT coupons

    (Lab.generated)

    Zr-Nb(R) PT coupon from a powerreactor. Enlarged view of the

    blister shown at RHS

    Neutron radiograph of burst tested Zr-2.5%Nb pressure tube piece containing

    laboratory generated hydride blisters(B).The axial crack is seen passing through two

    blisters at position 4 on the tube.

    . Hydrogen SensitiveEpithermal Neutron(HYSEN) radiographytechnique

    . CCD based Electronic imaging

    HYSEN radiograph of 1-, 2-, 3-, 4- layers of cellophane adhesive tape as object.Calculated hydrogen sensitivity: 0.1 mg/cm2.

    Neutron images of (1) carburetor, (2) spark plug, (3) INSAT cable cutter &

    U-tube filled with wax recorded using electronic imaging system.

    Some references

    1. A.M. Shaikh, P.R. Vaidya, B.K. Shah, S. Gangotra and K.C. Sahoo, J. Non Destr Test. & Eval. 22222(3), 9-12, 2003.2. A.M. Shaikh, Suparna Bannerji and D.N. Sah The e-Journal & Exhibition of nondestructive

    Testing-ISSN1435-4934, URL:www.ndt.net/article/nde-india2006/files/tp- 58-pap.pdf3. Amar Sinha, A.M. Shaikh, A. Shyam , Nucl. Instr and Meth. in Phys. Res. B 142142142142142, 425- 431, 1998.

    (1) (2) (3)

    1 2 3 4 ←←←←←

  • 34 Bhabha Atomic Research Centre, Mumbai, India

    A large variety of neutron detectors both BF3 and 3He gas–filled and X-ray detectors with excellent characteristics and long

    shelf life are routinely fabricated. They range from

    . Small beam monitors (0.2c/nv) to. Large size signal detectors (200c/nv),. Single wire & multiwire 1-D position sensitive detectors (1-D PSDs). A curvilinear multiwire 1-D PSD and. A large area multiwire 2-D PSD.Typical energy resolution of these detectors is 8 % 25 % (FWHM) for BF3 and 5%-15% for

    3He-filled detectors.

    The detectors developed are of various dimensions, sensitivity and efficiency as per requirements,

    Applications: Neutron scattering, flux monitoring, area monitoring and nuclear waste monitoring.

    Developmentof NeutronDetectors

    Fig.1. Various types of neutron andFig.1. Various types of neutron andFig.1. Various types of neutron andFig.1. Various types of neutron andFig.1. Various types of neutron andXXXXX-ray detectors developed by Solid-ray detectors developed by Solid-ray detectors developed by Solid-ray detectors developed by Solid-ray detectors developed by SolidState Physics DivisionState Physics DivisionState Physics DivisionState Physics DivisionState Physics Division

    AAAAA : 2-D Position Sensitive NeutronDetector,

    BBBBB : 1-D Position Sensitive NeutronDetectors,

    C C C C C : Neutron Proportional Counters,

    DDDDD : 1-D Curvilinear Position SensitiveNeutron Detector

    EEEEE : 2-D Position Sensitive X-raydetector,

    F:F:F:F:F: Microstrip Detector for X-rays andNeutrons,

    G G G G G : X-ray Proportional counters,

    HHHHH : 1-D Position Sensitive X-rayDetector.

  • 35Bhabha Atomic Research Centre, Mumbai, India

    . 3He-filled 1-D position sensitive neutron detector

    Fig. 2. Picture of some of the high resolution 1-D PSDs developed.36DHP1 : 3He + Kr (8 + 4 bar), sensitive length 89 cm.

    36CHP1 : 3He + iso-C4H10 (8 + 2 bar), sensitive length 89 cm.36CHP2 : 3He + Kr (10 + 4 bar), sensitive length 89 cm.

    8E : 3He + Kr (3 + 1.5 bar), Anode: CCQF, sensitive length 17 cmPosition resolution: 4 mm – 7 mm, Efficiency: 60 % to 90 %

    Fig.3. Neutron diffraction patterns of Nickel with

    36DN2 and 36DHP1 obtained at high-Qdiffractometer at Dhruva (λ=0.783 Å.).

    Sensitive area of 345 mm x 345 mm,pixel size: 5mm x 5mm and efficiency

    of 70% for 4 Å neutrons has beendeveloped.

    Fig. 4. Schematic of 2-D PSD for neutrons. The PSD is shown in photograph

    (Fig.1.) as Å

    Fig. 5. Position spectrum of 1″ φ directneutron beam (λ ≥ 4Å) (LHS) and thatof scattered beam with alumina sampleplaced in direct beam (RHS). Sample

    to detector distance ∼1.5m.

    . 3He-filled 2-D multiwire position sensitive neutron detector:

  • 36 Bhabha Atomic Research Centre, Mumbai, India

    . 3He-filled 1-D PSD based on microstrip geometry:with anode : 12 μm, cathode:300 μm, pitch : 612 μm and active area of 20 mm x 15 mm is developedand tested for Neutron and X-rays.

    Fig. 6. Schematic of designed microstrip pattern on insulating substrate(LHS)

    A, anode; C, cathode; B, bonding pad; R,meandering resistive strip Photograph(RHS) of rectangular chamber containing the Microstrip plate (top plate not

    shown),

    Fig.7. Response of microstrip detector

    to 1.5mm wide, , , , , 4Å neutron beam.Position resolution ~ 1.8 mm

    . Neutron Detector Development and Testing Facilities:

    Fig.8. Facility for Testing 1-D Position Sensitive Neutron Detector at Beam Hole

    No. 9, Apsara. Schematic of Neutron Beam Collimator and Detector Shielding,Experimental Setup (left). The BF3-gas generation, purification and fillingBF3-gas generation, purification and fillingBF3-gas generation, purification and fillingBF3-gas generation, purification and fillingBF3-gas generation, purification and filling

    stationstationstationstationstation is shown above.

    Design of neutron detectors,Assembly of detector components,anode assemblyEvacuation and gas filling systems,Facility for performance Testing ofdetectors with laboratory andreactor sources

    Some references

    1. S. S. Desai and A.M. Shaikh, Rev. Sci. Instr. 7878787878, 023304 (2007).2. S.S. Desai and A.M. Shaikh, Nucl. Instr. and Meth. in Phy. Res. A 557557557557557,

    607 (2006).3. S.S. Desai and A.M. Shaikh, J. of Neutron Research 1414141414, 121 (2006).4. A.M. Shaikh, S.S. Desai and A.K. Patra, Pramana: J. of Phys. 6363636363, 465

    (2004).5. V.Radhakrishna, S.S. Desai, A.M. Shaikh and K. Rajanna, Curr. Sci. 8484848484,

    1327 (2003).

  • 37Bhabha Atomic Research Centre, Mumbai, India

    Sample Environment Facilities

    Low Temperature: CCR- 1.5 - 300 K

    High Temperature: Furnace: 300-1800 K

    High Pressure Apparatus: A piston-cylinder type high-pressure cell with pressure range up to 25 kbar.

    Magnetic Field: 12 kOe at Room Temperature

    1.5 kOe and 2 kOe in vertical and horizontal direction with CCR

    Up to 7 Tesla and T=1.5 to 300 K

  • 38 Bhabha Atomic Research Centre, Mumbai, India

    Contact Scientists

  • 39Bhabha Atomic Research Centre, Mumbai, India

    For further information about facilities and proposals for experiments contact:

    Dr. S.L. Chaplot

    Head, Solid State Physics Division

    Bhabha Atomic Research Centre, Trombay

    Mumbai 400085, India

    Telephone: +91 22 25595376, 25593754

    Fax: +91 22 25505151, 25519613

    E-mail: [email protected]

    Published by:

    DrDrDrDrDr. Vijai K. Vijai K. Vijai K. Vijai K. Vijai Kumarumarumarumarumar,,,,,

    Associate Director, Knowledge Management Group &

    Head, Scientific Information Resource Division,

    Bhabha Atomic Research Centre,

    Trombay, Mumbai 400 085, India

    [email protected]

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