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Extreme conditions AD/ED-XRD (BL-11) [an error occurred while processing this directive]

Beamline overview

Material investigations under extreme conditions (high pressure/ temperature) provide vital information about microscopic interactions through structural evolution and/or realization of new phases which may have unusual properties. To serve this purpose, the in-situ structural determinations under extreme conditions are primarily performed using x-ray diffraction (XRD), a versatile non-destructive technique. There are two main variants of x-ray diffraction technique viz. angle dispersive x-ray diffraction (ADXRD) and energy dispersive x-ray diffraction (EDXRD). Both the techniques have their own merits. EDXRD technique is advantageous in case of constrained geometries and kinetics investigations whereas ADXRD provides high resolution diffraction data for detailed structural refinement. An ED/AD-XRD beam line, incorporating both these variants and especially optimized for material investigations under extreme conditions has been developed and commissioned at port no. BL-11. This beam line is being routinely used by several national and international users.

Beamline specifications

EDXRD ADXRD
SR source: Bending Magnet 1.5T Bending Magnet 1.5T
Energy range: 10-70 KeV @ 2.5 GeV, 300 mA Monochromatic tunable 10 Kev to 30 KeV
Angular range for diffraction ±25° Depends on sample to detector distance, typically ± 45 °
Q Range: 1.3 to 15 Å-1 (for 2θ =25° ) ~Up to 12 Å-1 at 30 keV
Detector resolution 145 eV at 5.9 KeV; 475 eV at 122 KeV Mar345 area detetctor with 0.1 * 0.1 mm2 pixel
Resolution 2% (Geometrical) 4.7 * 10-4 @ 17 KeV (calculated)
Spot size at sample ~100*100 μm (which can be increased up to 5*5 mm) ~ 50x30 μm (using compound refractive lens)
Total Flux at sample 1011 photons/s (for 300 mA @ 2.5 GeV and 100*100 μm spot size) 1010 photons/s (for 300 mA @ 2.5 GeV and 1x1 mm2 spot size)

Experimental setup

The front end for the Extreme conditions ED/AD-XRD beamline delivers a 1 mrad white beam. This beam is transported to the experimental station through various components viz. beam stopper, primary slit and precision slit. Primary slit and precision slit cut down the size of synchrotron radiation (SR) to 100μm * 100μm at the sample. There are two variants at the experimental station viz. the EDXRD variant and the ADXRD variant.

1) EDXRD variant

A custom made 8-axis sample stage goniometer from Huber is installed for sample mounting. This goniometer has maneuverability of XYZ translation, rotation and tilt. The data acquisition system comprises of a high resolution HPGe detector mounted on a detector arm attached to the 2θ stage of the goniometer. The detector is preceded by a cleaning slit and a point slit. Diffraction angle is defined by cleaning slit and point slit within the precision of ~0.001°. Cleaning slit also helps in reducing the background arising from the Compton scattered x-rays. Main features of EDXRD variant are tabulated below.

8 axis motorized goniometric stage

Bottom XY- stage ; Θ-2Θ stage; Sample XYZΧ stage

2Θ detector arm with travel range ±25°

Detector: High Purity Ge detector



EDXRD beamline experimental station
Fig. EDXRD variant at BL-11

2) ADXRD variant

To complement the utilization of EDXRD beamline, it has been adapted for ADXRD measurements. This has been achieved by monochromatizing white synchrotron beam using Si (111) channel cut monochromator. This adaptation has been ergonomically conceived using the existing infrastructure at the beam line and switching between the two variants is easily achieved. In order to avoid diffraction peaks from gasket material used for high pressure measurements, a compound refractive lens (CRL) based micro-focusing arrangement has also been incorporated at the beamline. These CRL's have been indigenously developed at x-ray lithography (BL-7) of INDUS-2 synchrotron source.

Monochromatization using single crystal Si (111) channel cut monochromator
Fig. Monochromatization using single crystal Si (111) channel cut monochromator



Fig. Micro-focusing using indigenously developed Compound refractive lens (CRL)
Fig. Micro-focusing using indigenously developed Compound refractive lens (CRL)



Fig. Diffraction image collection at MAR345 imaging plate
Fig. Diffraction image collection at MAR345 imaging plate

Beamline capabilities

  1. Energy dispersive x-ray diffraction measurements
    1. High pressure powder diffraction (Up to Megabar)
    2. High temperature powder diffraction (inside capillary up to 1500° K)

  2. Energy dispersive grazing incidence x-ray diffraction
    1. Ambient and High temperature (up to 700°K)
    2. Angle dispersive x-ray diffraction
    3. High pressure powder diffraction (Up to Megabar)
    4. High pressure single crystal diffraction
    5. High temperature powder diffraction (inside capillary up to 1500° K)
    6. Total x-ray scattering measurements for pair distribution function analysis


Fig. Grazing incidence EDX adaptation for thin films
Fig. Grazing incidence EDX adaptation for thin films



Fig. Adaptation of ED/ADXRD setup for high temperature measurement up to 1500° K
Fig. Adaptation of ED/ADXRD setup for high temperature measurement up to 1500° K



Fig. Off-line ruby pressure measurement setup
Fig. Off-line ruby pressure measurement setup

A few recent studies performed using BL-11

  1. High pressure study on α⇔ω⇔β transition sequence in several pure and impure samples of Hf metal
    Journal of Applied Physics, 115, 233513 (2014)

    Fig. Evolution of volume fraction of alpha, omega and beta phases of Hf as a function of pressure
    Fig. Evolution of volume fraction of alpha, omega and beta phases of Hf as a function of pressures


  2. Ex-situ in-plane and out-of-plane diffraction measurements revealing the growth of Co on oxidized interface with preferential orientation of c-axis perpendicular to the film plane
    Journal of Physics D: Applied Physics, 47, 105002 (2014)

    Fig. Grazing incidence x-ray diffraction of Co/CoO/Co thin film
    Fig. Grazing incidence x-ray diffraction of Co/CoO/Co thin film


  3. Stability of ambient rhombohedral structure of CuCrO2 upto ~ 23 GPa however with large anisotropy in axial compression with c-axis compressibility, kc = 1.26 * 10-3 GPa-1 and a-axis compressibility, ka = 8.9 * 10-3 GPa-1
    Journal of Applied Physics, 116, 133514 (2014). )

    Fig. Evolution of lattice parameters of CuCrO2 as a function of pressure.
    Fig. Evolution of lattice parameters of CuCrO2 as a function of pressure.


  4. X-ray diffraction studies confirm two phase transformations in NaZr2(PO4)3 around 5 and 6.6 GPa conjectured through Raman scattering measurements
    Journal of Solid State Chemistry, 221,285-290 (2015). )

    Fig. Structural transition in NaZr2(PO4)3
    Fig. Structural transition in NaZr2(PO4)3



    Fig. Equation of state of different phases of NaZr2(PO4)3
    Fig. Equation of state of different phases of NaZr2(PO4)3





Recent users at BL-11 (2012-14)

S. No.

Name

Affiliation

1

Dr. M. Somayazulu

Geophysical laboratory, CDAC, Carnegie Institute of Washington, Washington DC, USA

2.

Dr. Ajay Gupta and team members

UGC-DAE Consortium for Scientific, Indore

3.

Dr. Pushan Ayyub

Department of Condensed Matter Physics and Materials Science, TATA INSTITUTE OF FUNDAMENTAL RESEARCH, Mumbai

4.

Dr. Usha Chandra

Department of Physics, University of Rajasthan, Jaipur

5.

Dr. T R Ravindran

Solid state Physics and Materials science IGCAR, Kalpakkam

6.

Dr. Sunil D Deshpande

Department of Physics, Dr Babasaheb Ambedkar Marathwada University, Aurangabad

7.

Dr. Pankaj Misra

Department of Physics, University of Puerto Rico San Juan, PR, USA

8.

Dr. S. Karmakar

High Pressure & Synchrotron Radiation Physics Division, BARC, Mumbai

9.

Dr. Alka Garg

High Pressure & Synchrotron Radiation Physics Division, BARC, Mumbai

10.

Dr. R. H. Naina

Thermal and Surface Analytical Methods, ACD, BARC, Mumbai

11.

Mr. Abhishek Bhardwaj

Research Scholar center of Environmental Science, University of Allahabad, Allahabad

12.

Dr. Atul Khanna

Guru Nanak Dev University, Amritsar

13

Mr. Praveen Kumar Yadav

ISUD, RRCAT, Indore

14

Mr. Himanshu Srivastava

ISUD, RRCAT, Indore

15

Mr. Nishant Patel

High Pressure & Synchrotron Radiation Physics Division, BARC, Mumbai

Publications related to Bl-11

Peer reviewed journal articles:

  1. Energy dispersive x-ray diffraction beamline at Indus-2   Synchrotron source;
    K. K. Pandey, H. K. Poswal, A. K. Mishra et. al; Pramana –
    J. Phys., Vol. 80, No. 4,607-619 (2013).

  2. In-situ energy dispersive x-ray diffraction study of the growth of CuO nanowires by annealing method;
    H Srivastava, T Ganguli, SK Deb, T Sant, HK Poswal, SM Sharma;
    Journal of Applied Physics 114(14), 144303 (2013).

  3. Influence of ion-to-atom ratio on the microstructure of evaporated molybdenum thin films grown using low energy argon ions;
    Praveen Kumar Yadav, Tushar Sant, Chandrachur Mukherjee, Maheswar Nayak, Sanjay Kumar Rai, Gyanendra Singh Lodha and Surinder Mohan Sharma;
    J. Vac. Sci. Technol. A 32, 021509 (2014).

  4. Interface induced perpendicular magnetic anisotropy in Co/CoO/Co thin  film structure: An in-situ MOKE investigation ;
    Dileep Kumar,  Ajay Gupta,  P. Patidar,  K.K Pandey, T. Sant  and Surinder M. Sharma;
    Journal of Physics D: Applied Physics, 47, 105002 (2014).

  5. Reinvestigation of high pressure polymorphism in Hafnium metal;
    K. K. Pandey, Jyoti Gyanchandani, M. Somayazulu, G. K. Dey, Surinder M. Sharma and S. K. Sikka;
    Journal of Applied Physics, 115, 233513 (2014).

  6. Multiferroic CuCrO2 under high pressure: In situ X-ray diffraction and Raman spectroscopic studies;
    Alka B. Garg, A. K. Mishra, K. K. Pandey and Surinder M. Sharma;
    Journal of Applied Physics, 116, 133514 (2014).

  7. Pressure induced phase transformations in NaZr2(PO4)3 studied by X-Ray diffraction and Raman spectroscopy ;
    K. Kamali, T. R. Ravindran, N. V. Chandra Shekar, K. K. Pandey, S. M. Sharma;
    Journal of Solid State Chemistry, 221,285-290 (2015).



    Conference proceedings:

  8. Energy Dispersive X-ray Diffraction Beamline at Indus-2 Synchrotron Source; 
    H. K. Poswal, K. K. Pandey, A. K. Mishra, et. al.;
    BARC news Letters (founder’s day issue), (2011).

  9. High Pressure phase transitions in Nd2O3;
    K.K. Pandey, Nandini Garg and Surinder M. Sharma;
    147, AIRAPT-23(2011).

  10. GIXRD Measurements at EDXRD beamline at Indus-2  Synchrotron; 
    K. K. Pandey, Dileep Kumar, Abhilash Dwivedi, Ajay Gupta  and Surinder M. Sharma;
    AIP conference proceedings 1447,483 (2012).

  11. Textured Growth of Co on CoO (fcc) layer; structural studies at EDXRD Beamline INDUS-2, RRCAT;
    Dileep Kumar, Tushar Sant, K. K. Pandey, Ajay Gupta and Surinder M. Sharma,
    AIP conference proceedings 1447,721 (2012).

  12. Oxidized interface induced perpendicular magnetic anisotropy in Co/CoO/Co thin film         
    structure; Dileep Kumar, P. Patidar, A. Gupta, T. Sant et al.;
    12th international SXNS (2012).

  13. Depth sensitive structural information of thin films from energy dispersive grazing incidence diffraction;
    T. P. Sant, K. K. Pandey, Dileep Kumar, Surinder M. Sharma;
    12th international SXNS (2012).

  14. High pressure phase transition in Nd2O3;
    K. K. Pandey, Nandini Garg, A. K. Mishra and Surinder M. Sharma;
    Journal of Physics: Conference Series 377, 012006 (2012).

  15. In-situ study of the growth of CuO nanowires by energy dispersive X-ray diffraction;  
    H. Srivastava, T. Ganguli, S.K.Deb, T. Sant, H.K. Poswal, Surnider M. Sharma;
    AIP Conference Proceedings, 1512, 306-307 (2013).

Contact Number : 244 2511

Contacts:

Name

Email

Phone No.

Mr. K. K. Pandey

kkpandey(at)barc.gov.in

022-25592753

Dr. A. K. Mishra

akmishra(at)barc.gov.in

022-25591312

Dr. H. K. Poswal

himanshu(at)barc.gov.in

022-25592753

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