GRAZING INCIDENCE X-

RAY DIFFRACTION
 X-RAY DIFFRACTION
• XRD IS A NON-DESTRUCTIVE TECHNIQUE FOR CHARACTERIZING
CRYSTALLINE MATERIALS.
• DETERMINE THE ORIENTATION OF SINGLE CRYSTAL OR GRAIN.
• FIND THE CRYSTAL STRUCTURE OF AN UNKNOWN MATERIAL.
• MEASURE THE SIZE,SHAPE AND INTERNAL STRESS OF SMALL
CRYSTALLINE REGIONS.
 XRD ANALYSIS

PRINCIPLE:
IT IS BASED ON CONTRUCTIVE INTERFERENCE OF
MONOCHROMATIC X-RAYS AND A CRYSTALLINE SAMPLE. THE X-
RAYS ARE GENERATED BY A CATHODE RAY TUBE, FILTERED TO
PRODUCE MONOCHROMATIC RADIATION, COLLIMATED TO
CONCENTRATE AND DIRECTED TOWARD THE SAMPLE.
• X-RAY DIFFRACTON CONSISTS OF THREE ELEMENTS; AN X-RAY
TUBE,A SAMPLE HOLDER AND AN X-RAY DETECTOR
• X-RAY ARE GENERATED IN A CATHODE RAY TUBE BY HEATING A
FILAMENT TO PRODUCE ELECTRONS, ACCELERATING THE
ELECTRONS TOWARD A TARGET BY APPLYING A VOLTAGE,AND
BOMBARDING THE TARGET MATERIAL WITH ELECTRONS.
• WHEN ELECTRONS HAVE SUFFICIENT ENERGY TO DISLODGE INNER
SHELL ELECTRONS OF THE TARGET MATERIAL,CHARACTERISTICS OF
X-RAY SPECTRA ARE PRODUCED.
 CONT...
• THESE X-RAYS ARE COLLIMATED AND DIRECTED ON THE SAMPLE.AS
THE SAMPLE AND DETECTOR ARE ROTATED, THE INTENSITY OF THE
REFLECTED X-RAYS IS RECORDED.
• WHEN THE GEOMETRY OF THE INCIDENT X-RAYS SATISFIES THE
BRAGG EQUATION CONSTRUCTIVE INTERFERENCE AND A PEAK IN
INTENSITY OCCURS.
• A DETECTOR RECORDS AND PROCESSES THIS X-RAY SIGNAL AND
CONVERTS THE SIGNAL TO A COUNT RATE WHICH IS THEN OUTPUT
TO A DEVICE SUCH AS A PRINTER OR COMPUTER MONITOR
GLANCING INCIDENT X-
RAY DIFFRACTION
 WORKING PRINCIPLE OF GIXRD

• GRAZING INCIDENCE X-RAY AND NEUTRON DIFFRACTION, TYPICALLY

FROM A CRYSTALLINE STRUCTURE USES SMALL INCIDENT ANGLES
FOR THE INCOMING X-RAY, SO THAT DIFFRACTION CAN BE MADE
SURFACES SENSITIVE.
• IT IS USED TO STUDY SURFACES AND LAYERS BECAYSE WAVE
PENETRATION IS LIMITED.
 WORKING
• WHEN AN X-RAY DIFFRACTION EXPERIMENT IS PERFORMED IN AN
ASYMMETRIC GEOMETRY EMPLOYING A LOW FIXED GRAZING INCIDENCE,
IT IS REFERRED TO AS GIXRD.
• THE INCIDENT ANGLE IS KPT A LOW VALUE NEAR THE CRITICAL ANGLE
AND THE DETECOR SCANS THE 2θ CIRCLE.
• THE CRYSTALLINE PLANES SCATTERING X-RAYS ARE NO LONGER
THE PLANE PARALLEL TO THE SAMPLE SURFACE, BUT
PERPENDICULAR TO THE Q-VECTOR.
INSTRUMENTATION...
X-RAY PATH LENGTH AND FOOT PRINT IN
GIXRD
 THIN FILM ANALYSIS

*PREPARED BY:

v COATING OR DEPOSITON
vCHEMICAL OR PHSYICAL
REACTION

*CHARACTERISTICS:

v
THICKNESS,ROUGHNESS,DENSITY,
POROSITY,RESIDUAL
STRESS,TOPOLOGY,STRUCTURES.
vCRYSTALLINITY,ORIENTATION,OR
DERING,COMPOSITION,DEFECTS,EPI
AXIAL STRAIN
 INSTRUMENTAL SET UP;

ü IT REQUIES A PARALLEL BEAM SET

UP. A PARALLEL BEAM GOEBEL
MIRROR (CU USED). A SMALL SLIT
WOULD ALSO WORK AT THE COST
OF INTENSITY.
ü A STAGE ABLE TO PRECISELY
ADJUST THE SAMPLE HEIGHT
ü A PARALLEL BEAM ATTACHMENT
ON SECONDARY SIDE (SOLLER
PLATE COLLIMNATOR, DEFINING
THE INSTRUMENTAL
RESOLUTION).
GIXRD DATA COLLECTION:
 SPECIFICATIONS

• IT FEATURES A HIGH PRECISION VERTICAL θ-θ GONIOMETER AND

ABLE TO HANDLE SAMPLES UP TO W400*D500*H400MM.
• IT HANDLES CRYSTALLITE SIZE,CRYSTAL STRAIN CALCULATION,
CRYSTAL SYSTEM DETERMINATION,AND OTHEER SOFTWARE
BASED CRYSTAL STRUCTURE.
• THE ADDITION ATTACHMENT PERMITS STRESS
MEASUREMENT,AND ON AMBIENT CONDITONS AND THIN FILMS
• THE NEWLY DEVLOPED R-θ STAGE PERMITS AUTOMATIC
STRESS MAPPING OF AN ENTIRE SAMPLE UP TO 350NM IN
DIAMTER.
 FEATURES:

• HIGH-PRECISION VERTICAL GONIOMETER

• COMPREHENSIVE RANGE OF OPTTIONS EXPAND THE SYSTEM
• WINDOWS 7 COMPATIBLE
• SAFETY FIRST DESIGN
 PRINCIPLE

X-RAY FOCUSED ON A SAMPLE FIXED ON THE

AXIS OF THE GONIOMETER ARE DIFFRACTED BY
THE SAMPLE.THE CHANGES IN THE DIFFRACTED
X-RAY INTENSITIES ARE MEASURED,RECORDED
AND PLOTTED AGAINST THE ROTATION ANGLES
OF THE SAMPLE
 CONT...

• COMPUTER ANALYSIS OF THE PEAK POSITIONS AND INTENSITIES

ASSOCIATED WITH THIS PATTERN ENABLES QUALITATIVE
ANALYSIS,LATTICE DETERMINATION AND STRESS.
• PEAK ANGLES USED TO DETERMINE PARTICLE DIAMETERS AND DEGREE
OF CRYSTALLISATION AND STRUCTURAL ANALYSIS.
 APPLICATIONS
oMEASUREMENT OOF SNO2 NANOPARTICLES COATING ON TITANIUM DIXOIDE NANOTUBE
ARRAYS USING GRAZING INCIDENCE X-RAY DIFFRACTION.
oBY GIXRD ANALYSIS,THE PHASE COMPONENTS OF THE COATING ON TIO2 NANOTUBE
WERE DISCLOSED, AND A MULTILAYER STRUCTURE IS ESTABLISHED.SNO2 CRYSTAL PHASE,
TIO2 CRYSTAL PHASE AND AMORPHOUS PHASE WITH O2 COMPOSITION, FROM THE TOP
DOWN, RESPECTIVELY.
oIT IS SHOWN FROM THE GIXRD RESULTS THAT, THERE IS OBVIOUS DIFFRACTION PEAK
BROADENING PHENOMENON CORRESPONDING TO THE DECREASING X-RAY INCIDENCE
ANGLES DUE TO THE CRYSTALS ON THE SURFACE,WHICH IS CAUSED BY THE NON-
PARALLEL X-RAYS SCATTERING ON THE SAMPLE SURFACE, WHULE FOR THE CRYSTAL
UNDER THE SURFACE THERE IS NO PHENOMENON OBSERVD,EVEN FOR CRYSTALS MUCH
CLOSER TO THE SURFACE. THIS PROVIDES A METHOD FOR DISTINGUISHING THE CRYSTAL
ON THE SURFACE OR UNDER THE SURFACE
 CONT...

• FERROUS METALS AND NON FERROUS METALS

• MACHINARY, AUTOMOBILES,SHIPBUILDING
• CHEMICAL AND CATALYSIS
• CERAMICS
• ELECTRONIC AND ELECTRICAL MATERIALS
• ENVIRONMENT AND INDUSTRIAL WASTES
• RESOURCES AND ENERGY
 MALVERN PANALYTICAL
• BENCHTOP X-RAY DIFFRACTOMETER
• EMPYREAN RANGE
• X'PERT3 (VERSATILE X-RAY DIFFRACTION SYSTEM)
• MEASUREMENT TYPE
Ø PARTICLE SHAPE AND SIZE
Ø CRYSTAL STRUCTURE
Ø PHASE IDENTIFICATION AND QUANTIFICATION
Ø CONTAMINANT DETECTION AND ANALYSIS
Ø EPITAXY ANALYSIS
Ø 3D STRUCTURE AND IMAGING
BENCHTOP AND EMPYREAN RANGE
 ADVANTAGES;

üPORE SIZE
üPARTICLE SIZE
üSURFACE ATOMIC DETAILS
üRESIDUAL STRESS
üNON DESTRUCTIVE TECHNIQUE
 DISADVANTAGES

• LIMITED IN PLANE SPATIAL RESOLUTIONS.

• VERY EXPENSIVE
 REFERENCES:

• https://www.slideshare.net>mobile gixrd
• https://en.m.wikipedia.org>wiki(gixrd)
• https://www.researchgate.net>post(gixrd)
• https://pdfs.semanticsholar.org>
• https://ec.europa.eu>article books