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Government of India | Department of Atomic Energy
Raja Ramanna Centre for Advanced Technology

Angle Dispersive X-Ray Diffraction Beamline (BL-12)

Introduction

X-ray diffraction (XRD) is a powerful technique for studying the structure of materials - both crystalline as well as amorphous. The combination of high brightness and fine vertical collimation of synchrotron radiation with the added advantage of broad range of wavelength tunability as compared to conventional laboratory x-ray sources makes it an ideal source for XRD characterization of materials.

An angle dispersive X-ray diffraction (ADXRD) beamline has been setup and installed on BL-12 bending magnet port of the Indus-2 synchrotron. The electron source size at this port is approximately 0.5 mm (H) X 0.5 mm (V). The beam acceptance of the beamline is 2 mrad(H) x 0.15 mrad(V). The first optical element is a platinum coated pre-mirror (M1) which is plane and bendable and is used for vertical focusing/collimation of the x-ray beam. Double Crystal Monochromator (DCM) with Si(111) crystals is the second optical element of the beamline and is used for monochromatization of photon beam. Second crystal of the DCM is also used for the sagittal focusing of the beam. For high energy resolution Si(311) crystal pair is also available which requires approximately 3 days for being replaced and aligned. The third optical element is a platinum coated bendable post mirror (M2) used for vertical focusing/collimation of the beam (Post mirror has been removed temporarily).

Optical Layout of the Beamline
Optical layout of The Beamline


Photograph of The Beamline
Photograph of the Beamline


Photon Beam Parameters
  • Spectral Range: 5-20keV
  • Energy Resolution: 1eV at 10keV [measured value ~ 7000 (ΔE/E) at Cu K-edge]
  • Flux: 1010 photons/sec at 10keV
  • Beam Size: 0.7mm (H) x 0.5mm (V)
  • Angular Resolution:
    • 15 arc sec (single crystal in rocking curve open detector geometry)
    • 0.03 degree (2σ in 2θ) for powder LaB6 (NIST) on diffractometer
    • 0.06 degree ((2σ in 2θ) powder sample on Image Plate)


Flux at 2.5 GeV, 100mA

Flux at 2.5 Gev,100 mA

Experimental Stations Available

There are two experimental stations in tandem. The adaptive focusing optics allows us to focus the photon beam on one or the other experimental station. The first experimental station consists of a six circle diffractometer (Huber-5020) with NaI scintillation detector. The four circles consist of θ, 2θ,φ and X rotations.φ and X rotations are used to adjust single crystal samples. The second experimental station consists of an area detector (Image Plate Mar-345) for fast recording of XRD data on powder sample.


Photographs of the Experimental Stations
Six circle Diffractometer Huber-5020
Image Plate Mar 345
Six circle Diffractometer Huber-5020
Image plate Mar 345


Features of the Huber-5020 diffractometer

Angular range

0 – 100°

Sample environment
  1. Air, Powder sample with provision for sample rotation
  2. High temperature ( up to 800K) See Photograph below

Higher order suppression

Possible with detuning of the second crystal

Various scan modes
  1. θ-2θ scan
  2. detector scan
  3. rocking curve scan
  4. φ and χ scans

Incident flux monitoring

On line measurement using Ionization Chamber

Q Range

4.66 Å-1 (6 keV) - 14.74 Å-1 (19keV)

Angular Resolution

15 arc seconds


High Temperature X-ray Diffraction Set-up

High Temperature X-ray diffraction Set-up


Details of the Image plate setup

Diameter

345mm

Sample environment
  1. Air
  2.  High pressure (Diamond anvil cell based)
  3. Low Temperature (3K – 450K) . Efforts are being made to reduce /eliminate Be peaks generated from Be domes.

Higher order suppression

Possible with detuning of the second crystal

Sample mounting
  1. Powder sample in a capillary with provision for sample rotation
  2. Powder sample sandwiched between kapton sheets

Q Range

up  to  10.88 Å-1 (at 20keV)

Angular Resolution

0.06 degree (2σ in 2θ)


High Pressure X-ray diffraction Set-up on Image Plate

Picture of the DAC on an automated X-Y scanner developed at RRCAT
A view of the X-Ray beam locator software developed at RRCAT
Picture of the DAC on an automated X-Y scanner developed at RRCAT
A view of the X-Ray beam locator software developed at RRCAT
Note : Users need to bring their own DAC and accessories. Microscope required for loading the sample in DAC is available
 
 
Data from Image Plate, DCM 17.0 Kev
Test Data: XRD pattern of LaB6 as a function of pressure.
Low Temperature XRD set-up (3K to 450K) on Image Plate

  • Liquid He based flow type cryostat
  • Temperature Range - 3K – 450K
  • PID Temperature Controller (Lakeshore 331)
  • Temperature stability ≈ 0.15K
Cryostat mounted on Image Plate setup
XRD pattern for BaTiO3
Cryostat mounted on Image Plate setup
Test Data : XRD pattern for BaTiO3


Detectors available on experimental stations
  • NaI (Tl) Scintillation point detector
  • Ionization Chambers
  • Low resolution x-ray CCD for x-ray beam viewing (20x onscreen)
  • Image plate (Mar 345) area detector
  • Vortex-EX SDD energy dispersive detector

Research Highlights
  1. X-ray diffraction studies of Gd1-xCaxBaCo2O5.5 system (0 <= x <= 0.30)
    		2.


  2. Determination of concentration of Eu valence states in EuCu2Ge2 using XANES
  3. Ordering of a'-Fe,Co nanocrystalline phase in soft magnetic FeCoNbB alloy

  4. XRD study of correlation of the magnetic properties of Cu free FINEMET alloys with air annealing at various temperatures.

  5. Investigation of charge states and multiferroicity in Fe doped h-YMnO3


    Low level Fe-substitutions on Mn site in YMnO3 multiferroic clearly contrast the roles of magnetic versus non-magnetic B-site dopants. The doped magnetic Fe ions weaken the Mn-Mn interaction. Doping driven enhanced charge disorder (Mn+3 / Mn+4) quenches the spin frusration (f); this affects the biferroicity minutely, but alters their coupled magneto-electric features hugely.


  6. X- ray Diffraction study of Low Temperature Phase transition in LiMn2O4 system

User List :

User

Affiliation

A K Sinha

ISUD, RRCAT, Indore

Amol

Anuj Upadhyay

Harish

M K Tiwari

M N Singh

Manas

S R Kane

Shailendra Kumar

Vishal Dhamgaye

 

Archna Sagdeo

MRL, ISUD, RRCAT, Indore

Ashok Bhakar

Kamini

Madhusmita Baral

Pooja Gupta

Pragya Tiwari

Ravindra Jangir

Soma Banik

Shreyaskar Dev Singh

 

Adityanarayan H Pandey

RRCAT, Indore

Amita Chaturvedi

Ashish Khandelwal

Debabreta Saha

G J Singh

J Khare

M K chattopadhya

Md. Matin

Pankaj Mishra

Parul Arora

Pramod Radheyshyam

R Kaul

Rajeev Bhatt

S B Roy

S M Gupta

S Satpathy

Saleem Khan

Sangeeta

Shyamsundar

Sunil Verma

V Shukla

 

A P Srivastva

BARC, Mumbai

Atul

H P U

Meenakshi

N L Mishra

Nilesh

Rekha Rao

S N Achary

S Neogy

Wishvanath

 

Anthony Arulraj

IGCAR, Kalpakkam

Balmukund Shukla

Bharthi A

R. Kalavathy

Kishan

M Sekar

Mahadevan

R Asuvathraman

R N Sarguna

N V Chandrashekhar

Ravi Kirna

S Murugesan

Sabeena

Shabana

Shilpam

Sorb

Soumee Chakraborty

Sridharan

Srinu

Subramanium

Vinod

 

Bishnu Pandey

Allahabad, University

S Deshpandey

Aurangabad University

Ranvijay Yadav

BHU, Varanasi

Ratnesh Gupta

DAVV, Indore

S N Kane

DAVV, Indore

Sheetal Soni

DAVV, Indore

H M Rai

IIT - Indore

Kaustav

IIT - Kharagpur

Sujoy KAR

IIT - Kharagpur

Chandan Upadhyay

IIT BHU, Varanasi

Mukesh Kumari Dahiya

IIT Delhi

Anvita

IIT Indore

Anjali Deotale

IPS Academy, Indore

Kavita

IUC, Indore

Sonu Namdeo

IUC, Indore

Sarika

Jiwaji University

Shobha Kulshreshta

Jiwaji University

Deeptikant Pathy

JNCASR, Bangaluru

Jaideo

JNCASR, Bangaluru

Rajeev Ranjan

JNCASR, Bangaluru

Subhajit Kundu

JNCASR, Bangaluru

Shweta Rajawat

MANIT, Bhopal

R Nandini Devi

NCL, Pune

Rajesh

NCL, Pune

Manas Ranjan Panda

Pondichery University

R Murugan

Puducherry University

Debaleen Biswas

SINP

S K Abdul Farque

SINP

Anirban Pal

TIFR

Selected Publications
  1. Electron-irradiation induced changes in structural and magnetic properties of Fe and Co based metallic glasses
    S. N. Kane, M. Satalkar, A. Ghosh, M. Shah, N. Ghodke, Pramod R., A. K. Sinha, M. N. Singh, J. Dwivedi, F. Celegato, F. Vinar, P. Tiberto, L. K. Verga
    Journal of Alloys and Compounds (2014) In press.

  2. Spectroscopic and structural studies of isochronally annealed cobalt oxide nanoparticles.
    Harishchandra Singh, A. K. Sinha, M. N. Singh, Pragya Tiwari, D. M. Phase, S. K. Deb
    Journal of Physics and Chemistry of Solids     75 (2014) 397

  3. Spin-fluctuations in Ti{0.6}V{0.4} alloy and its influence on the superconductivity.
    Md. Matin, L.S. Sharath Chandra, Radhakishan Meena, M. K. Chattopadhyay, A. K. Sinha, M. N. Singh, S. B. Roy;
    Physica B: Physics of Condensed Matter 436 (2014) 20.

  4. Structural modification of poly (methyl methacrylate) due to electron irradiation
    Pragya Tiwari, A.K. Srivastava, B.Q. Khattak, Suveer Verma, Anuj Upadhyay, A.K. Sinha, Tapas Ganguli, G.S. Lodha, S.K. Deb;
    Measurement (2014) (Accepted for publication)
    http://dx.doi.org/10.1016/j.measurement.2014.01.017.

  5. Investigation of charge states and multiferroicity in Fe doped h-YMnO3.
    Sonu Namdeo, A. K. Sinha, M. N. Singh and A. M. Awasthi;
    J. Appl. Phys. 113 (2013) 104101

  6. Magnetic irreversibility and pinning force density in the Ti-V alloys.
    Md. Matin, L. S. Sharath Chandra, M. K. Chattopadhyay, R. K. Meena, Rakesh Kaul, M.N.Singh, A. K. Sinha, and S. B. Roy;
    J. Appl. Phys. 113 163903 (2013)

  7. Angle dispersive X-Ray Diffraction beamline on Indus-2 Synchrotron radiation source: commissioning and first results.
    A. K. Sinha, Archna Sagdeo, Pooja Gupta, Anuj Upadhyay, Ashok Kumar, M.N.Singh, R.K.Gupta, S.R.Kane, A.Verma, S.K.Deb;
    J. Phys.: Conf Series 425, 072017(2013).

  8. A high pressure XRD setup at ADXRD beamline (BL-12) on Indus-2.
    Tapas Ganguli, A.K.Sinha, Chandrabhas Narayana, Anuj Upadhyay, M.N.Singh, P.Saxena, V.K.Dubey, I.J.Singh, Sendhil Raja, H.S.Vora, S.K.Deb;
    J. Phys.: Conf series 425, 112001 (2013).

  9. Characterisation of Sb doped Bi2UO6 solid solutions by x-ray diffraction and x-ray absorption spectroscopy.
    N. L. Misra, A. K. Yadav, Sangita Dhara, Rohan Phatak, S. K. Mishra, A. K. Poswal. S. N. Jha, A. K. Sinha and D. Bhattacharya;
    Analytical Sciences 29, 579 (2013).

  10. Correlation of microstructural and physical properties in bulk BiFeO3 prepared by rapid liquid- phase sintering.
    Archna Sagdeo, Puspen Mondal, Anuj Upadhyay, A. K. Sinha, A. K. Srivastava, S. M. Gupta, P. Chowdhury, Tapas Ganguli and S. K. Deb;
    Solid State Sciences 18 (2013) 1.

  11. High pressure structural investigation of LaGa.
    M. Sekar, Chandra Sekar, S. Chandra, P. Sahu, A. K. Sinha, A. Upadhyay and M. N. Singh;
    Philosophical Magazine,(2013); dx.doi.org/10.1080/14786435.2013.826880

  12. Magnetic Properties of Termary Aluminide TbFeAl10
    A. Khandelwal, V. K. Sharma, L. S. Sharath Chandra, M.N.Singh, A. K. Sinha, M. K. Chattopadhyay;
    Physica Scripta (2013) (Accepted for publication)

  13. Optical Properties of Cd(OH)2 Nanoparticles by Pulse Laser Ablation in Aqueous Environment.
    A. K. Shahi, B. K. Pandey, J. K. Pandey, A. K. Sinha, and R.Gopal;
    Mater. Focus 2, 342-345

  14. Electronic structure of EuCu2Ge2 studied by resonant photoemission and x-ray absorption spectroscopy.
    Soma Banik, Azzedine Bendounan, A. Thamizhavel, A. Arya, P. Risterucci, F. Sirotti, A. K. Sinha, S. K. Dhar, S. K. Deb;
    Phys. Rev. B86, 085134 (2012).

  15. A correlation between structural and optical properties of cobalt oxide nanoparticles for various annealing conditions.
    A. K. Sinha, R. K. Gupta and S. K. Deb;
    Appl. Phys. A (2012), in press (Online: DOI 10.00339-012-6938-y).

  16. Influence of isochronal annealing on the microstructure and magnetic properties of Cu-free HITPERM Fe40.5Co40.5Nb7B12 alloy.
    Pooja Gupta, Tapas Ganguly, A. Gupta, A. K. Sinha, P. Svec Jr., V. Franco and S. K. Deb;
    J. Appl. Phys. 111 (2012) .

  17. Magnetic property of novel cobalt sulfate nanoparticles synthesized by pulsed laser ablation.
    B. K. Pandey, A. K. Shahi, R. K. Swarnkar and R. Gopal;
    Sc. Adv. Mater. 4 (2012) 1

  18. Growth of CsI:Tl crystals in carbon coated silica crucible by the gradient freeze technique.
    S. G. Singh, D. C. Desai, A. K. Singh, M. Tyagi, Shashwati Sen, A. K. Sinha, S. C. Gadkari and S. K. Gupta;
    J. Cryst. Growth, 351, 88 (2012).

  19. Synthesis and characterization of various phases of cobalt oxide nanoparticles using inorganic precursor.
    R. K. Gupta, A. K. Sinha, B. N. Raja Sekhar, A. K. Srivastava, G. Singh and S. K. Deb.
    Appl. Phys. A 103, 13 (2011).

  20. Oxidation state of chromium in (Na0.5Bi0.5TiO3)(1-x)(BiCrO3)x solid solution investigated by XAS and Impedance spectroscopy.
    Rachna Selvamani, Gurviderjit Singh, A. K. Sinha and V. S. Tiwari;
    J. Mat. Sci. 47, 2011 (2011).

  21. Temperature-dependent index of refraction of monoclinic Ga2O3 single crystal.
    Indranil Bhaumik, S. Ganesamoorthy, R. Bhatt, A. Saxena, A. K. Karnal, P. K. Gupta, A. K. Sinha and S. K. Deb;
    Appl. Optics, 50, 6006 (2011).

  22. Structural evaluation and the kinetics of Cu clustering in the amorphous phases of Fe-Cu-Nb-Si-B alloys.
    Pooja Gupta, Ajay Gupta, Anuj Shukla, Tapas Ganguly, A. K. Sinha, G. Pricipi and A. Maddalena;
    J. Appl. Phys. 110, 033537 (2011).

Contact Number : 244 2512/ 244 2125

Contact Details Dr. A.K. Sinha (anil(at)rrcat.gov.in)
Mr. Anuj Upadhyay

(anuj(at)rrcat.gov.in)

Last Modification on : February 2014
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