X-ray Diffraction Facility
X-ray Diffraction Facility
Make
Empyrean
Facility Status
Working
Facility Management Division
Institute Central Research Facilities (ICRF)

Category

  • Diffraction » X-ray Diffraction

Booking Details

Slot Booking Link
Click here for Booking!
Booking available for
Internal and External Both

Facility Management Team and Location

Faculty In Charge
Prof. Abhijeet L. Sangle
Facility Manager
Mr. Hitesh Thakur
Co-convenors
Prof. Abhijeet L. Sangle
Prof. MJNV Prasad
Prof. T R S Prasanna
Prof. Sushil Mishra
Prof. Arindam Sarkar
Prof. Subramaniam Chandramouli
Department
MEMS
LAB Email ID
xrdatmems@iitb.ac.in
Facility Location
Room No -G022 ,Ground Floor, Department of Metallurgical Engineering and Materials Science.
Lab Phone No
02221593603

Facility Features, Working Principle and Specifications

Features Working Principle
  1. Phase analysis of sample with flat surface of solid samples and powder samples.
  2. Thin film (Grazing Incidence) XRD measurements.
  3. Small Angle X-ray Scattering (SAXS)  measurements
  4. X-rays and their generation: X-rays are high energy electromagnetic radiation with both wave and particle nature in the wavelength range of 0.01-10 nm. X-rays are produced when electrons generated from a metal cathode at high negative potential are accelerated towards a metal anode (target) at ground potential. A small percentage (< 1%) of the total loss of kinetic energy due to the impact of the electron on the metal is manifested in the form of x-rays. A spectrum of x-rays consists of continuous radiation whose wavelength is inversely proportional to applied voltage. At sufficiently high voltages, electron in the inner shell of the atom in target metal is ejected and that position is filled by other electron from outer shell associated with a release of an x-ray photon. This results in higher intensity characteristic radiation (Kα, Kβ etc.) along with continuous radiation in spectrum and is specific to the target metal. The Kα characteristic radiation is specifically separated using filters from rest of the radiation and is used for diffraction.  
  5. Diffraction: The bending of waves around the edges of an object is called diffraction. It is noticeably visible when spacing between the objects is of the same order as the incident wavelength, resulting in constructive and destructive interference. The prime reason for using x-rays in crystallography is the wavelength of x-rays being of the order of inter-planar spacing (typically ~20-30 nm) of the metals. When characteristic x-rays are incident on any metal, the electrons in the atoms of the metal oscillate about their mean position and act as new sources of electromagnetic radiation in all directions with the same frequency as of incident x-rays. This absorption and reemission of radiation is called scattering. The scattering occurs in all the planes of atoms in the metal but leads to constructive interference in specific directions resulting in diffracted beams. The intensity of the successfully diffracted beam of x-rays is extremely small compared to the incident x-rays and is captured using special detectors. The condition for successful constructive interference of x-rays is derived by Sir W. H. Bragg and his son Sir W. L. Bragg as, the path difference between diffracted beams should be an integral multiple of wave length, given by the equation:
  6. nλ=2dsinθ
  7. Where n- an integer indicating the order of diffraction; λ- wavelength of x-rays used; d- spacing between planes of atoms; θ- angle of incidence. The position of the peaks in the intensity of diffracted beams versus 2θ plot is material characteristic and is used for various analyses.
  8. X-ray diffraction techniques is used in various applications like determining crystal structure, lattice parameters, phase analysis, quantitative phase composition, macro and micro strains, defect concentration, phase diagrams, and amorphicity, and to characterize polymorphs, DNA etc.
Body Specification

X-ray tube: Cu; long fine focus; spinner stage

Pixcel 1D detector with prefix interface

X’pert highscore plus; reflectivity software; easysaxs software

Instructions for Registration, Sample Preparation, User Instructions, Precautionary Measures and Charges

Instructions for Registration
  • A maximum of six samples will be accepted at a time.
  • Only One registration will accepted at a time.
  • Maximum two samples will be accepted for half an hour sample scan.
  • Collect the samples and the XRD results within 30 days of your registration.
  • If user will not collect samples within 30 days then lab person will not responsible for missed samples
Instruction for Sample Preparation

Please follow the sample preparation methods below, according to the nature of your analysis.

For Powder XRD

Samples should be submitted in the form of fine powder (preferably less than 10 μm) to completely fill the rectangular cavity of the sample holder of dimension of 0.6 cm3.

i.e. l = 2 cm, b = 1.5cm, h = 0.2 cm.

For Pallet Samples, the sample should have diameter of 2 cm and height 1 cm (maximum).

For Thin Film XRD and GIXRD

Sample size should be minimum 5 cm ´ 2.5 cm.

For SAXS

Details will be provided upon consultation.

Applications

  • Phase Identification of unknown crystalline materials.
  • Characterization of crystalline materials.
  • Determination of crystal structures using Rietveld refinement.
  • Thin film characterization.
  • SAXS method is useful for the structural characterization of nanomaterials. The samples may be solid objects, powders, gels or liquid dispersions, and they may be amorphous, crystalline or semi-crystalline.
  • Complete Functional system for Phase Analysis & Crystallography.
  • Thin film attachment (GIXRD) & reflectivity measurements.
  • Small angle and wide angle X-ray scattering (SAXS/WAXS) measurements & accessories for solids, composites as well as powder as per technical specifications.

Sample Details

SOP, Lab Policies and Other Details

Publications

Publications
NA