CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION
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Course Plan
Aims of the course
Course lectures
Course examination
Course projects
Seminars
Course literature
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Survey over Materials Characterisation
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90 nm
Bending a silicon nano-whisker inside the TEM-STM instrument.
CHALMERS / Göteborg University
Graduate School in Materials Science
Characterisation FTF155
INTRODUCTION- Aims
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The course is directed to Ph.D students
and Masters and Undergraduate students
in the 4th year at CTH and GU, with
interest in materials science.
The aim is to give a basic knowledge of
experimental techniques used for
characterization of structure and dynamic
properties in materials science
To develop skills in
experimental techniques,
critical analysis, and
scientific reporting
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION- Lectures
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DIFFRACTION
A short theoretical
introduction to
diffraction of x-rays,
neutrons and electrons
by solid matter
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MICROSCOPY
An introduction to
AP-FIM, ST M/AFM
and electron
microscopy
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SURFACE ANALYSIS
Techniques for surface
and interface analysis
are reviewed, e.g.
XPS, AES, SIMS
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SPECTROSCOPY
Basic concepts of
NMR, Raman and
Infrared spectroscopy
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION- Examination
The examination has two components:
a) A written project report
b) An oral presentation of the project work
It is compulsory to attend at least 80% of the
lectures and seminars.
Only grades ”passed” and ”non-passed” will
be given for graduate students.
Undergraduate and masters students can get
3,4 or 5.
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION
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Projects(1)
A compulsory project work is included in
the course
The aim of the project is to characterize,
as completely as possible, a given material
with some of the techniques presented in
the course.
It is recommended that two students work
together.
Some projects will be proposed by the
lecturers, but it is also recommended that
students use material from their own
research
Students should use the analytical
techniques which are not used in their
research.
Obtained results must be scrutinized and
presented orally as well as in writing.
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION- Projects(2)
PROJECT ABSTRACT
A written abstract (1-2 pages) describing
the project should be submitted before
analysis work is started.
Deadline is Nov. 27.
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Firstly, discuss your idea with the
responsible person (Lecturer) for the
relevant analytical technique(s).
Describe the material and the properties
that are to be characterised.
Describe which techniques you want to use
and why they were chosen.
Briefly explain why other techniques
presented in the course are not suitable.
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION- Projects(3)
PROJECT REPORT
(deadline Dec. 30)
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Describe the results of the analysis in a
written report
Describe each of the analytical techniques
not used in the analysis project but
presented in this course, in relation to your
own project.
Propose and describe a second project to
study a material using at least 3 of the
techniques not used in your present
project.
The oral presentation is planned to be a
12 minutes presentation and 3 minutes
discussion of each project.
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION- Seminars
Three seminars will be given after the
lecture presentations with invited guests
from academy and industry ;
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Jan-Olov Nilsson (Sandvik /CTH):
Industrial use of characterisation techniques
in the Sandvik materials laboratory
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Jukka Lausmaa (SP Borås):
Presentation of applications using
TOF-SIMS and MALDI
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Magnus Hellsing (Högskolan Dalarna):
Presentation of AES-use in consulting work
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION- Literature
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The essential part of the course will be
summarized by review papers in the
compendium and by complementing
handouts at lectures.
Additional literature is recommended
Reference Literature
1. Analysis of Microelectronic Materials and Devices, Ed. M.
Grasserbauer, H.W. Werner, J. Wiley, ISBN 0471950130,1991
2. Practical Surface Analysis, ed. D. Briggs& M.P. Seah, J. Wiley, ISBN
0471953407
3. Surface Characterization;a users handbook.
Ed. D. Brune et al, John Wiley, ISBN 3-527-28843-0, 1996
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4.Encyclopedia of Materials Characterisation, Ed C.R,Brundle
Manning Publ. Co., ISBN 0-7506-9168-9, 1992
WEB-SITE; Charles Evans & Ass.http://www.cea.com
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
A widespread applicability of materials
characterisation in manufacturing industry
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Motor vehicles (lubrication, wear, corrosion)
Aircraft (superalloy oxidation, adhesives)
Metal goods (joining, welding, soldering, casting)
Electronics (thin film, dopants, adhesion, failure)
Mechanical Engineering (hard metals, oxidation)
Chemicals (catalysis, plastics, pigments)
Gas, electricity, water (steel failures)
Food, drink (canning, corrosion)
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
Which property of the material do we want to
characterise?
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Thermodynamics
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enthalpies
segregation energies
bond strengths
phase transtions
elemental
chemical composition
and bonding
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Composition
Structure
Time evolution
defects
kinetics
crystalline orientation
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Microstructure
and Topography
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
Which part of the material do we want to
characterise?
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Surface
concentrations, maps,
profiles and sections
Bulk
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Interfaces
How to select the appropriate method/s to
characterize the material in question?
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
Is an identification of the chemical compound needed or is
the elemental composition sufficient?
Are quantitative results needed,
or is qualitative identification sufficient?
Quantitative analysis with high precision is difficult
and expensive
What is the detection limit needed for qualitative
identification?
If quantitative results are required, what is the
accuracy and resolution needed?
Accurate quantitative results require careful
analysis, well documented standards and careful
calibration procedures
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
Characterisation surveyQuality assurance and safeguards
Quality Assurance: according to ISO-8402
Quality is the totality of characteristics of an entity that
bear on its ability to satisfy stated and implied needs
Quality control concerns the operational means to fulfill
the quality requirements,while quality assurance aims at
providing confidence in this fulfillment.
Modification induced by the analytical procedure
Limitations imposed by the analysis environment
Surface-layer-induced limitations
Other limitations
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
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LIGHT MICROSCOPY (LM)
The interpretive use of Light Microscope.
Should be used initially in all analytical work
Is not included in this course!
The technique involves, at its very basic
level, to observe features that are beyond
the resolution of the human eye (100mm).
The direct visual observation of a sample
with white light has a resolution of about
0.2 mm for LM.
The morphology, colour, opacity and optical
properties are often sufficient to
characterize and identify a material!!
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
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SIMS
(Secondary Ion Mass
Spectrometry)
Surface and layer
compostion
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NMR
(Nuclear Magnetic
Resonance)
Chemical state
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STM/AFM
(Scanning Tunneling
Microscopy/Atomic Force
Microscopy)
Atomic surface structure
Ions and ionized clusters ejected from a
surface during ion bombardment are
detected with a mass spectrometer.
Surface chemical composition and some
information on bonding can be extracted
from SIMS ion fragment distributions
NMR is not an explicit surface-sensitive
technique,but NMR data on large surface
area samples have provided usful
information on molecular adsorbtion
geometries. This method is limited to the
analysis of magnetically active nuclei
The topography of a surface is measured
by mechanically scanning a probe over a
surface. The distance from the probe to the
surface is measured by the probe-surface
tunneling current. Angstrom resolution of
surface features is routinely obtained.
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
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TEM, SEM
(Transmission/Scanning
Electron Microscopy)
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AES
(Auger Electron Spectr.)
Near-surface composition,
chemical state
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XPS (”ESCA”)
(X-ray Photoelectron Spectr.,
”Electron Spectr. for Chemical
Analysis”)
Near-surface composition,
chemical state
Core-hole excitations are
created, usually by 1-10 keV
incident electrons and Auger
electrons of characteristic
energies are emitted through a
two-electron process as excited
atoms decay to their ground
state
Electrons photoemitted from the
atomic core levels are detected
as a function of energy. The
shifts of core-level energies give
information on the chemical
environment of the atoms.
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
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AP - FIM
(Atom Probe-Field Ion
Microscopy)
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XRD
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X-ray diffraction has been
carried out at extreme
glancing angles of incidence
where total reflection
ensures surface sensitivity..
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Neutron diffraction is rather
characterising bulk
properties. Neutron
diffraction can provide
structural information on
adsorbed molecules and
surface phase transitions.
(X-ray Diffraction)
Crystallographic structure
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Neutron Diffraction
molecular structure,
magnetic ordering
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRO.-Characterisation survey
NOBEL PRIZE Awards
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Physics 1914, Max von Laue
X-ray diffraction
Chemistry 1922, Francis Aston
Mass-spectroscopic separation of isotopes (”SIMS”)
Physics 1924, Manne Siegbahn
X-ray spectroscopy
Physics 1930, Venkata Raman
The scattering of light,Raman-effect
Physics 1981, Kai Siegbahn
HR photoelectron (ESCA)
Physics 1986, G. Binnig, H. Rohrer
Scanning tunneling microscopy
Physics 1986, Ernst Ruska
Electron Microscopy
Chemistry 1991 Richard Ernst
Development of NMR spectroscopy
Physics 1994, Clifford Shull
Neutron diffraction
CHALMERS / Göteborg University
Graduate School of Materials Science
Characterisation FTF155
INTRODUCTION- ”Physics”
Input rad. Electron
Output
detected
Ions
Electron
AES,
SEM
EELS
INS
Ions
ESD
ESDIAD
SIMS
RBS,
ISS,FIB
Neutral
Photons/
X-rays
Neutrals
Photons/
X-rays
UPS,
XPS
FABMS
LAMMA
LIMA
(AP-FIM)
SNMS
SALI
EPMA
PIXE,
Raman,
XRF,
XRD,
NMR