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MATERIALS
CHARACTERISATION
TECHNIQUES
(MLZ 222, 229 & 230)
Prof. Dr. Servet Turan
Thanks to Doç.Dr. Hilmi Yurdakul
Thanks to Tayfun Koçak &
Cem Eren Özbilgin
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PROBLEMS: OVERLAPPING ENERGIES
Anadolu University, Materials Science & Engineering, Eskisehir, Turkey
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BASICS OF WDS
Crystal change
motor
Crystal
X- ray
Spectrometer mounting interface
X-ray diffracted
Extrance slit
X-ray counter
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ROWLAND CIRCLE (WDX)
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Specimen
Detector
Electron Beam Curved
Crystal
R
Rowland
Circle
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Wavelength dispersive spectroscopy (WDS)
WDS utilizes the wave properties of X-rays to discern emitted X-ray energies.
X-rays, like all wave energy, can be diffracted.
Some necessary background:
Diffraction of X-rays obeys Braggs law:
n=1, 2, 3, … , l=X-ray wavelength, d=the spacing between atomic planes in a
crystal, q=the diffraction angle
)sin(2 ql dn
q
incident X-rays in phasediffracted X-rays
out of phase
d
Suggested Curriculum Links
Physics: light diffraction, wave theory of matter
Anadolu University, Materials Science & Engineering, Eskisehir, Turkey
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Wavelength dispersive x-ray spectrometry (WDX)
EDX
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Wavelength dispersive x-ray spectrometry (WDX)
WDX
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COMPARISON OF EDX & WDX
WDX
EDX
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COMPARISON OF EDX-WDX
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TaW
Ni
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COMMON CRYSTALS USED IN WDX
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WDX vs EDX
Advantages
(i) high peak/background ratio
(ii) easy to detect low atomic number elements
(iii) high peak resolution
Disadvantages
(i) very expensive
(ii) a need to use several crystals for entire spectrum
Therefore, time consuming
Numunenin kesinlikle düz olması gerekliliği
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Electron beam - sample interaction
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Electron beam - sample
interaction 2: Effect of kV
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Electron beam - sample
interaction 2: Effect of atomic no.
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Electron beam - sample
interaction 3
K
L
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CHEMICAL ANALYSIS (MICROANALYSIS)
Analysis performed on a very small part of a large
specimen
In principle, one can determine two things from the
x-ray spectrum emitted by any specimen:
(i) measurement of wavelength or energy of each
characteristic x-ray enables us to find out which
elements are present, i.e., qualitative analysis
(ii) measurement of how many x-rays of any type are
emitted per second should tell us how much of the
element is present, i.e., quantitative analysis
However, due to instrumental and specimen
requirements quantitative analysis is not easy
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EDS is a parallel collection
technique
All X-ray energies are collected
simultaneously and X-ray
spectrum of energy vs number
of counts produced.
From the energy of peaks the
elements present can be deduced
From the size of the peaks the
relative amounts of elements in
the sample can be estimated
Qualitative Analysis
C
Ca
O
Mg
P
P
Ca
Ca
0.5 1 1.5 2 2.5 3 3.5 4
Full Scale 3644 cts Cursor: 2.743 keV (71 cts) keVFull Scale 3644 cts Cursor: 2.743 keV (71 cts) keVFull Scale 3644 cts Cursor: 2.743 keV (71 cts) keV
Spectrum 1
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QUANTITATIVE ANALYSIS
Two questions to answer:
(i) What is the smallest amount of element X which
could be detected
(ii) What is the amount of an element in a specimen
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Ni 18.3%
O 25.9%
Si 2.2%Ti 8.1%
Fe 45.4%
Quantitative Results (weight%)
QUANTITATIVE ANALYSIS
Ti
Ti
Fe
Fe
Ni
Ni
4 5 6 7 8
Full Scale 8635 cts Cursor: 6.023 keV (241 cts) keVFull Scale 8635 cts Cursor: 6.023 keV (241 cts) keVFull Scale 8635 cts Cursor: 6.023 keV (241 cts) keV
Mnpt1
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THE LIMIT OF DETECTABILITY
Should know minimum detectable concentration
(MDC)
If the count rate in the background is b counts per
second, if the counting time is t, then the background
level is bt and the smallest detectable peak is 2sqr(bt)
above the background.
What concentration of an element in the specimen
would give this peak. To answer this we must compare
our peak height with the peak height (P-B) given by a
standard specimen consisting of the pure element. MDC
is given by:
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Where p is the peak count rate on the pure element
standard. Simplifying this slightly we get:
To lower the MDC, reduce b, increase p and t. The
easiest is to increase the time of analysis.
EDX system have poorer peak-to-background ratios
than WDX,
Both systems have worse p/b ratios for the lighter
elements
THE LIMIT OF DETECTABILITY
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For the lighter elements, MDC is around 0.1% in EDX
and an order of magnitude lower for WDX.
The precise figure will depend on the atomic weight of
the trace element compared to that of the specimen
since the soft x-rays from a light element will be
strongly absorbed by a matrix of high atomic weight
THE LIMIT OF DETECTABILITY
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If one wants to quantify the relative amounts of different
elements present in a complex sample one has to account
for a number of factors and carry out a correction of the
data
QUANTITATIVE ANALYSIS
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SPATIAL
RESOLUTION
DIFFERENT TYPES OF RESOLUTIONS!
5
Å
IMAGE
RESOLUTION
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EYE
RESOLUTION
PEAK
RES.
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Sample
Preperation(Excl. SEM)
CHEMICAL
ANALYSIS
DEVELOPMENTS: 3 MAIN CONCEPTS!
5
Å
IMAGING
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WDS
Anadolu University, Materials Science & Engineering, Eskisehir, Turkey
Specimen
Scintillation
Counter
Electron Beam Curved
Crystal
R
Rowland
Circle
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EDS
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Specimen
Detector
Electron Beam
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EBSD
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Electron Beam
Back-scattered
Electron diffraction
Specimen
Detector
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EDS-WDS
Anadolu University, Materials Science & Engineering, Eskisehir, Turkey
Specimen
Electron Beam Curved
Crystal
R
Rowland
Circle
Detector
Scintillation
Counter
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XRF with WDS
Anadolu University, Materials Science & Engineering, Eskisehir, Turkey
Specimen
X-rays Curved
Crystal
Scintillation
Counter
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XRD
Anadolu University, Materials Science & Engineering, Eskisehir, Turkey
Target
Electron Beam Diffracting
Sample
Scintillation
Counter
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Kristal
Yapı
Üretim
Süreci
Özellik
Performans
Karak-ter-
izasyon
MALZEMELERİN KARAKTERİZASYONU NEDEN ÖNEMLİDİR?
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
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Faz
Analizi
Görüntü
Kimyasal
Analiz
Diğer
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
Karakter-izasyon
Teknikleri
Kalitativ
Kantitativ
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Nano
Piko
Mikro
Makro
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
60 karbon atomunun
sıralanmasıyla elde edilen
futbol topu şeklindeki
~1 nm çapında “fullerene”
molekülü, çelikten daha
güçlü, plastikten daha hafif,
elektrik ve ısıyı ileten
Uçucu kül~ 10-20 mm
Silikon atomlarıAtomlararası mesafe
0.078 nm
Karakter-izasyonun
Mertebeleri
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Elektron
Işık
İyon
Diğer
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Mikroskoplar
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2D
3D
Dinamik
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
Elde EdilenBilgi Türleri
Atomik
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Karakterizasyonu halka nasıl anlatırız?
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
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CHARACTERISATION TECHNIQUES
Non-Microscobic Tech.Microscobic Tech.
Light Microscopy
Scanning Electron Micr.
Transmission Electron Micr.
Other Tech.
Thermal Analysis
X-ray Diffraction
Spectroscopic Techniques
Other Tech.
Anadolu University, Materials Science & Engineering Department, Eskisehir, Turkey
MLZ 229MLZ 230
MLZ 222
https://www.facebook.com/groups/1657111924571465/
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WHAT IS THIS?
Energy (keV)
Inte
nsi
ty (
cps)
Anadolu University, Materials Science & Engineering Department, Eskisehir, Turkey
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nepheline syenite and 25% quartz
revealing quartz filler (Q), cuboidal
primary mullite (PM) and acicular
WHAT IS THIS?
Anadolu University, Materials Science & Engineering Department, Eskisehir, Turkey
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FATIGUE FRACTURED AIRCRAFT PART!
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5 Å
Yurdakul & Turan et al., Scripta Materialia, 65, 656 (2011)
WHAT IS THIS?
Anadolu University, Materials Science & Engineering Department, Eskisehir, Turkey
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MİKROYAPI NEDİR?
Anadolu Üniversitesi Malzeme Bilimi ve Mühendisliği Bölümü
Birim Hücre
Yer alan AtomArayer Atomu
Vida
Dislokasyonu
Taneler Arası
KırılmaTane İçi Kırılma
Tane Sınırı Fazı
TaneSınırı
Çökeltileri
Koherent
Çökeltiler
Koherent Olmayan
Çökeltiler
İkinci FazKayma
ÇizgileriKenar Dislo.
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MİKROYAPI NEDİR?
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
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PROBLEMLER-3D vs 2D
Numune
Mikroskop
Görüntü
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
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PROBLEMLER-3D vs 2D
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
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PROBLEMLER-3D vs 2D
Servet Turan, Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
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İnce Numune
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NUMUNE KALINLIĞININ ETKİSİ
Kalın Numune
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Problem Çözen İlk Mikroskopçular !!!
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It is a mammoth!
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ÖNERİLER
5 Å
-Si3N4 ‘de ve tane sınırlarında Ce!!
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66
Anadolu Üniversitesi, Malzeme Bilimi ve Mühendisliği Bölümü, Eskişehir
Görmeden İnanmam!
Gördüğüme de İnanmam!
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Phase rich in Zr
Görmeden İnanmam!
Gördüğüme de İnanmam!
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Kimyasal Analiz!
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Techniques
Properties
TG DTG DSC DTA STA
TG/DTA
Dilato-
meterXRD XRF MS FTIR
Atomic bonding
Qualitative elemental analysis
Quantitative elemental analysis
Qualitative phase analysis
Quantitative phase analysis
Crystallinity
Non-Crystallinity
Texture
Particle (or crystal) size
Particle shape
Crystal STructure
Bravais lattice
Lattice parameters
Elemental distribution
Phase distribution
Trace elements (less than 0.1 %)
Physical W….
Chemical W….
Phase Tran…… Te….
Dec…. Te….
Glass T… Te
Crys… Te….
For… Rea… Te
229 Final
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Techniques
Properties
TG DSC DTA STA
TG/DTA
Dilato-
meterXRD XRF LM SEM TEM EDS WDS SADP
Atomic bonding
Qualitative elemental analysis
Quantitative elemental analysis
Qualitative phase analysis
Quantitative phase analysis
Crystallinity
Non-Crystallinity
Texture
Particle (or crystal) size
Particle shape
Crystal STructure
Bravais lattice
Lattice parameters
Elemental distribution
Phase distribution
230 Final
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Techniques
Properties
TG DSC DTA STA
TG/DTA
Dilato-
meterXRD XRF LM SEM TEM EDS WDS SADP
Trace elements (less than 0.1
%)
Physical W….
Chemical W….
Phase Tran…… Te….
Dec…. Te….
Glass T… Te
Crys… Te….
For… Rea… Te
Me…… Te…..
Va… Te…
Powder sample
Bulk sample
Destructive
Non-Destructive
Please add a different
property
Please add a different
property
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What do I gain at the end of it ?
The student will be able to know how to characterise
any kind of sample
Anadolu University, Materials Science & Engineering Department, Eskisehir, Turkey
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Türk Elektron Mikroskopi Derneği (TEMD) üyeliğinin yanı sıra
European Microscopy Society (EMS), International Federation of
Societies for Microscopy (IFSM) ve International Federation of
Societies for Histochemistry and Cytochemistry (IFSHC) üyesi olma
ayrıcalığı kazanacaksınız. Bu sayede bu derneklerin vermiş olduğu
desteklerden faydalanabileceksiniz.
ÜYE OLMANIN AVANTAJLARI NELERDİR?
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