(X-Ray Characterization)
(XRD-XRF)
Environmental Laboratory
Environmental Engineering Study Program
Universitas Brawijaya
Spectrum Electromagnetic
Type
Frequency(Hz) Long Wave
Radiation
gamma-rays 1020-1024 < 1 pm
X-Rays 1017-1020 1 pm - 1 nm
ultraviolet 1015-1017 1 nm– 400 nm
visible 4-5.5x1014 400 nm- 800 nm
near-infrared 1x1014-4x1014 800 nm-2.5 m
infrared 1013-1014 2.5 m-25 m
microwaves 3x1011-1013 25 m-1 mm
radio waves <3x1011 > 1 mm
X-Ray Characterization
X-Ray
X-Ray
Fluoresce
Diffraction
nce
X-Ray Diffractometer
X-ray detector
Tube 2️
Sample
stage
Sample requirements:
1. The sample is a powder solid
2. Crystals samples
Diagramscheme tube ray -X
X-ray tube
The electrons come from the tungsten filament in
the vacuum area, accelerated by a high voltage
(30,000 V) against the target metal. Nuclear
electrons are ejected from the target metal: rays-X,
(characteristics of the target metalused). Ray-X exits
the beryllium window in the tube.
3p1s ; K️
Intensity
2p 1s ; K️ Metal Anode RadiationK️(️)
Cr 2.29️
Fe 1.94️
Long wave() Co 1.79️
Cu 1.54
The spectrum that comes out of the ray Mo 0.71
tube-X Ag 0.56️
Light experiment-X
To obtain a single wavelength, a single crystal monochromator is used. Generally lineK️1selected because
has the greatest intensity.
The principle of ray diffraction-X
Ray-X interacts with electrons in matter. When the light-X hits a material, the light will be
scattered in various directions by bound cloud of electron. Light wavelength-X used in ray
diffraction experiments-X, lies between 0.6 and 1.9 A.
Dray refraction-X
X-ray diffraction is used to determine the positions of atoms in molecules and solids.
In inorganic chemistry, distances are determined from structure and provide additional
information on the bonds into and between molecules.
Miller Index
Ray-X interacts with planes of atoms in a three-dimensional lattice exhibiting the translational symmetry of
the structure.
Each plane represents a member of a parallel set of planes of the same space, and each lattice point must lie
in one plane.
Labels to describe fields️Miller Index (h, k and l) whereh,k,lis a positive or negative integer or zero.
XRD characterization results analysis
Qualitative Quantitative
• Material identification • Determination of crystal size
• Identification of sample purity
• Determine the crystallinity of the
sample (crystalline or amorphous)
• Determination of atomic position and
structure (refining technique)
Characterization Results: Diffractogram Example
The refracted light will be captured by the detector and
then interpreted as a diffraction peak.
The more crystal planes there are in the sample, the
stronger the refraction intensity it produces.
The results of XRD measurements are intensity values
and gap length at an angle of 2θ
2θ is the angle between the incident ray and the
reflected ray. Meanwhile, intensity is the number of X-
Rays diffracted by the lattice formed by the atoms that
make up the crystal. If there are no atoms that make
up a lattice plane in the crystal, then the incoming X
Results measurement XRD in the form of rays cannot be diffracted or in other words there is no
price intensity and long gap on 2️θ intensity.
Qualitative Analysis
Identify unknown materials
Patern of diffraction ray-x character unique for each
material that character crystal.
More than 150,000 distinctive powder diffraction data sets
have been collected from samples and arranged in
database.
JCPDS (Joint Committee on Powder Diffraction Standards).
ICSD (International Crystallography Data Standard). For knowing phase the crystal formed,results
measurement matched with data diffraction
ICDD (International Center for Diffraction Data) standard.
Purity sample Sample crystallinity
Phase purity can be identified by looking at the A sample with high crystallinity will provide
peaks that appear on the diffractogram. a high and sharp diffraction intensity
The existence of conformity between the
standard and the sample indicates that the
sample is a single/pure phase without any other
compounds being formed
Quantitative Analysis
Crystal Size
Scherrer's formula connects size crystal with peak width diffraction,
and is widely used to determine the particle size distribution:
Decrease particle
size
D= Size crystal (nm)
B = FWHM value
Theta = Bragg Sudut angle
λ =X-ray wavelength.
k = constant “Shape Factor” (0.8-1)
Advantages
• Non-destructive technique Deficiency/Weakness
• Expensive tool and characterization costs
• Fast and easy sample turnaround time
• Unable to analyze organic samples
• Easily identify many inorganic compounds
by comparing standards • Samples can only be powder
X-Ray Fluorescence
X-Ray Fluorescence
The x-ray fluorescence (XRF) technique is an analytical technique that can analyze the
elements contained in a material
This technique can also be used to determine the concentration of elements based on
the wavelength and number of x-rays that are re-emitted after a material is
bombarded with high-energy x-rays.
XRF Working Principle
X-ray shooting from an x-ray tube for Secrete electron from skin part in for produce ray-Xnew
which characteristics from element-composing elements the sample in analysis
• For every atom in samples, intensity from
ray-X characteristics compared with
amount(concentration) atom in samples.
• Intensity ray–X characteristics from every
element, compared with something
standard which is known concentration,so
that concentration element in sample can
determined.
Radiation
shoot radiation electromagnetic
photon which emitted will
electromagnetic to interact with
material that electron which is at
researched. in skink something
element.
Electron whichis at in
skink will have energy
kinetic which enough for
release self from bond
core, so that electron that
will bounce go out.
Sample
Powder
⮚ Size powder< 400 mesh
⮚ A total of 1 gram
Solid
⮚ Surface which coated will minimize effect scattering
⮚ Sample must flat for produce analysis quantitative optimal
Fluid
⮚ Sample must fresh when analyzed and analysis conducted by fast if sample easy evaporate
⮚ Sample can’t contain sediment
Detector PIN Diode
FET
Window
Si(Li)Detector
Super-Cooled Cryostat
Cooling: Thermoelectrically cooled
(Peltier)
Si(Li)
Pre-Amplifier
Window: Beryllium
crystal
Count Rates: 3,000 – 20,000 cps
Cooling: LN2or Peltier Resolution: 170-240 eV atM Nk-alpha
Window: Beryllium or Polymer
Counts Rates: 3,000 – 50,000 cps
Resolution: 120-170 eV atM NK-alpha
Packaging: Similar to PIN Detector
Cooling: Peltier
Count Rates; 10,000 – 300,000 cps
Silicon Drift Detector
Resolution: 140-180 eV atM NK-alpha
Spectra XRF
Identification elements which contained
Qualitative Analysis in something material
Compare the fluorescence specific energy values of
each element.
Total X-Ray Intensity
Element Energy K️
V 4952 eV
Cr 5415 eV
MN 5899 eV
Fe 6403 eV
Co 6930 eV
Ni 7478 eV
Cu 8048 eV
elemental fluorescence
Quantitative Analysis
Concentration analysis elements which contained in material
C sample = K x C standard
K : X-ray intensity
Advantages Weakness
• Easy used and Sample could in the form of • Couldn’t knowing compound what which
congested,powder(details)and fluid formed by elements which contained in
• High Accuracy (relative) material
• Could determine element inmaterial without • Couldn’t determine structure from the atom
existence standard(comparedg. AAS)
• Lots element could analyzed at a time(Na-U)
• Could used for analysis element major (Si,Ti,
Al, Fe,M N, Mg, Ca, Na, K, P) nor trace
element(>1 ppm; Ba, Ce, Co, Cr, Cu, Ga,
La,Nb, Ni,rb,Sc,Sr, Rh, U, V, Y,Zr, Zn)
THANK YOU
Dielectric relaxati on behavior of
Li and La co-doped NiO ceramics
A ADakhel
Department of Physics, College of Science, University of Bahrain, PO Box 32038,
Bahrain
Trial Procedure NiO is doped with Li . cation+and La3+
NiO, Li(OH).H2O, LLNO-1 ️Li0.05La0.03Ni0.92O
Lanthanum
Acetylacetonate LLNO-2 ️Li0.05La0.05Ni0.90O
• Dstoichiometrically weigh
• Methanol was added and ground until homogeneous
• Calcined at 1000oC for 20 hours
For elemental analysis of samples
LLNO-1andLLNO-2
using spectroscopic measurements
• Dshaped into pellets with a thickness of 1-2 mm
• Calcined at 1200oC for 20 hours Energy Dispersive X-Ray Fluorescence
• Analysis using XRD and XRF (EDXRF)with Cu K . radiation️and
detector Amptek XR-100CR.
Data analysis
For structural analysis using the X-
Ray Diffraction (XRD) method with
Cu K . radiation️(0.15406 nm) with
scan step 0.02o.
XRF Analysis
The spectrum shows peaks:
Ni K️(7.47keV),
La L️(4.65keV),
La L️1 (5.04keV),
La L️2 (5.38keV)
The peak of Lithium is not detected in the
detector
XRD analysis All patterns show a single NiO crystalline
phase that is cubic FCC (Fm3m) structure.
The reflection (200) has the highest
intensity, as in the standard diffraction
pattern.
ICSD #92127(NiO)
Structural and magnetic
properties ofM N-doped ZnO
powders
M. El-Hilo n,AADakhel
Department of physics, College of science, University of bahraini, PO Box
32038,Kingdom of Bahrain
Trial Procedure
bus(acetylacetonato),zinc(II)hydrateand
Synthesize ZnO doped with Mn, 0% tris (acetyla-cetonato) manganese(III).
(undoped),3.9% (I), 3.3% (II) and 4.2% (II).
• Dstoichiometrically weigh
• Mixed and dissolved in methanol
Elemental analysis for samples using the
spectroscopic method Energy Dispersion X- Cingredients mix
ray Fluorescence (EDXRF).X-rays are formed • MEthanol is evaporated
using a Cu anode operated at15 kV and 5 • The mixture is put into an alumina crucible
mA,and detector AmptekXR-100CR. • Calcined at 400oC for 2 hours
Powder
• Dformed into pellets with a pressure of 750 MPa
• Calcined at 600oC for 2 hours
• Analysis using XRD and XRF
Data analysis
XRF Analysis
The EDXRF spectrum of the sample shows:
M N K️(5,898keV),
M N K️1 (6,490keV),
Zn K️(8.638keV),.
Zn K️1 (9,572keV)
AndsignalfromCuX-ray source
XRD analysis
The XRD patterns show that all the investigated samples
were polycrystalline with a hexagonalwurtzitestructure
(space group P63mc) of ZnO. Signals arising from Mn,
Mn-oxides, or any Mn related phases were not detected.
ICSD #157724
Laporan
• Sampul
• Daftar isi
• Pendahuluan (Latar Belakang, tujuan : XRD dan XRF)
• Studi kasus (SC 1 : nama sampel, mekanisme pembuatan, dan hasil, dan demikian
untuk SC2)
• Pembahasan
• Penutup (Kesimpulan : menjawab tujuan)
• Daftar Pustaka
Pengumpulan : pekan depan di hari yang sama pukul 20.00 WIB. Lewat G-Drive.
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