CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION
Materials Science:Characterisation
Bending a silicon nano-whisker inside the TEM-STM instrument.
90 nm
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION
Aims of the course Course lectures Course examination Course projects Seminars Course literature Survey over Materials Characterisation
Bending a silicon nano-whisker inside the TEM-STM instrument.
90 nm
CHALMERS / Göteborg UniversityGraduate School in Materials ScienceCharacterisation FTF155
Organization
The course has three parts:
• Lectures (appr. 10x2 hours)• Project work (total extent about 3
weeks)• Seminars
CHALMERS / Göteborg UniversityGraduate School in Materials ScienceCharacterisation FTF155
INTRODUCTION- Aims
The course is directed to Ph.D studentsand Masters and Undergraduate studentsin the 4th year at CTH and GU, with interestin materials science.
The aim is to give a basic knowledge ofexperimental techniques used forcharacterisation of structural and electronicproperties in materials science
To develop experimental skills and abilitiesfor critical analysis and scientific reporting
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- Lectures
DIFFRACTIONA short theoreticalintroduction todiffraction of x-rays,neutrons andelectrons by solidmatter
SURFACE ANALYSISTechniques forsurface and interfaceanalysis are reviewede.g. XPS, AES, SIMS
MICROSCOPYAn introduction to
AP-FIM, AFM andelectron microscopy
SPECTROSCOPYBasic concepts ofNMR, Raman andInfrared spectroscopy
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- Examination
The examination has two components
a) A written project report
b) An oral presentation of the project work
Graduate students: Only grade”passed” and ”non-passed”Undergraduate and mastersstudents: grades 3 - 5 or theequivalent ETCS.
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- Projects(1)
A compulsory project work is included inthe course.The aim of the project is tocharacterise, as completely as possible,a given material with some (at least two)of the techniques presented in the course.
It is recommended that two students worktogether.
Some projects will be proposed by thelecturers, but it is also recommended thatstudents use material from their ownresearch.
Use preferably analytical techniqueswhich are not used in own research.
Obtained results must be scrutinized andpresented orally and in a written report.
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- Projects(2)
PROJECT ABSTRACTA written abstract (1-2 pages) describingthe project should be submitted beforeanalysis work is started.Deadline is Dec. 4.
Firstly discuss your idea with theresponsible person (lecturer) for therelevant analytical technique(s).
Describe the material and the propertiesthat are to be characterised.
Describe which techniques you want to useand why they were chosen.
Explain shortly why other techniquespresented in the course are not suitable.
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- Projects(3)
PROJECT REPORT (deadline Dec. 29)
Describe the results of the analysis in awritten report
Describe each of the analytical techniquesnot used in the analysis project butpresented in this course, in relation toyour own project.
Propose and describe a second project tostudy a material using at least 3 of thetechniques not used in your presentproject.
The oral presentation is planned to be a12 minutes presentation and 3 minutesdiscussion of each project.
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- Seminars
Three seminars will be given after thelecture presentations with invited guestsfrom academy and industry ;
Jan-Olov Nilsson (Sandvik /CTH):Industrial use of characterisationtechniques in the Sandvik materialslaboratory
Jukka Lausmaa (SP Borås):Presentation of applications using TOF-SIMS and MALDI
Magnus Hellsing (Högskolan Dalarna):Presentation of AES-use in consulting work
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- Literature
The essential part of the course will besummarized by review papers in thecompendium and by complementinghandouts 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, ISBN0471953407
3. Surface Characterization;a users handbook.Ed. D. Brune et al, John Wiley, ISBN 3-527-28843-0, 1996
4.Encyclopedia of Materials Characterisation, Ed C.R,BrundleManning Publ. Co., ISBN 0-7506-9168-9, 1992
WEB-SITE; Charles Evans and Ass.www.eaglabs.com/en-US/index.html
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
A widespread applicability of materialscharacterisation in manufacturing industry
Motor vehicles(lubrication, wear, corrosion,)
Aircraft (superalloy oxidation, adhesives) Metal goods (joining, welding, soldering, casting) Electronics (thin films, dopants, adhesion, failure) Mechanical Engineering (hard metals, oxidation) Chemicals(catalysis, plastics, pigments) Gas, electricity, water (steel failures) Food, drink (canning, corrosion)
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
Thermodynamicssegregation energiesbond strengthsphase transtions
Time evolutionkineticsdynamics
Compositionelemental compositionchemical compositionand bonding
Structuredefectscrystalline orientation
Microstructure andTopography
Which property of the material do we want tocharacterise?
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
Surfaceconcentrations,maps,profiles and sections
Bulk
Interface
Which part of the material do we want tocharacterise?
How to select the appropriate method/s tocharacterize the material in question?
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
Are quantitative results needed,or is qualitative identification sufficient?Quantitative analysis with high precision is difficultand expensive
Is an identification of the chemical compoundneeded or is the elemental composition sufficient?
What is the detection limit needed for qualitativeidentification?
If quantitative results are required, what is theaccuracy and resolution needed?
Accurate quantitative results require carefulanalysis, well documented standards and carefulcalibration procedures
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
Characterisation survey-Quality assurance and safeguards
Modification induced by the analytical procedure
Quality Assurance: according to ISO-8402Quality is the totality of characteristics of an entity thatbear on its ability to satisfy stated and implied needs
Quality control concerns the operational means to fulfil thequality requirements,while quality assurance aims atproviding confidence in this fulfilment.
Limitations imposed by the analysis environment
Surface-layer-induced limitations
Other limitations
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
LIGHT MICROSCOPY (LM)The interpretive use of Light Microscope.Should be used initially in all analytical work
Is not included explicitly in this course!
The technique involves, at its very basiclevel, to observe features that are beyondthe resolution of the human eye(100mm).The direct visual observation of a samplewith white-light has a resolution of about0.2 mm for LM.
The morphology, colour, opacity and opticalproperties are often sufficient tocharacterise and identify a material!!
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
SIMS(Secondary Ion MassSpectrometry)Surface and layercompostion
NMR(Nuclear Magneticresonance)Chemical state
AFM and STM(Atomic ForceMicroscopy)Atomic surfacestructure
Ions and ionized clusters ejected froma surface during ion bombardment aredetected with a mass spectrometer.Surface chemical composition andsome information on bonding can beextracted from SIMS ion fragmentdistributions
NMR is not an explicit surface-sensitive technique,but NMR data onlarge surface area samples haveprovided usful information onmolecular adsorbtion geometries.This method is limited to the analysisof magnetically active nuclei
The topography of a surface ismeasured by mechanically scanning aprobe over a surface. The distancefrom the probe to the surface ismeasured by the probe-surfacetunneling current. Angstrom resolutionof surface features is routinelyobtained.
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
ElectronMicroscopy
AES(Auger electronSpectroscopy)Near-surface chemicalcomposition
XPS (”ESCA”)(X-ray PhotoelectronSpectroscopy, )Composition,oxidationstates
Core-hole excitations arecreated, usually by 1-10 keVincident electrons and Augerelectrons of characteristicenergies are emitted through atwo-electron process as excitedatoms decay to their groundstate
Electrons photoemitted fromthe atomic core levels aredetected as a function ofenergy. The shifts of core-levelenergies give information onthe chemical environment ofthe atoms.
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
Atom Probe- FieldIon Microscope
X-Ray DiffractionCrytstallographicstructure
Neutron Diffractionmagnetic structuremolecular structure
X-ray diffraction has beencarried out at extremeglancing angles ofincidence where totalreflection ensures surfacesensitivity..
Neutron diffraction is rathercharacterising bulkproperties. Neutrondiffraction can providestructural information onadsorbed molecules andsurface phase transitions.
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
NOBEL PRIZE Awards 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 (XPS) Physics 1930, Venketa Raman
The scattering of light,Raman-effect Physics 1981, Kai Siegbahn
HR electron microscopy 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, G. Shull
Neutron diffraction Chemistry 2002 K. Wüthrich Development of NMR for structural determination
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRO.-Characterisation survey
Physics 1986, G. Binnig, H. RohrerScanning tunneling microscopy
Physics 1986, Ernst RuskaElectron Microscopy
Chemistry 1991 Richard ErnstDevelopment of NMR
Physics 1994, G. ShullNeutron diffraction
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- ”Physics”
Detection
Raman,XRF,XRD,NMR
PIXEEPMAPhotons
SNMSSALI
Neutrals
LAMMALIMA(AP-FIM)
FABMSSIMSRBS,ISS,FIB
ESDESDIAD
Ions
UPS,XPS
INSAES,SEMEELS
Electrons
PhotonsNeutralsIonsElectronsExcitation
CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155
INTRODUCTION- MAL AT CTH
CLPL,RamanEllipsom,FTIR
Opticalproperties
SEM,AFM, STM
Surfacestructure
XRD,Raman,FIR, AP
BulkStructure
Raman,XRF,AESSAM,ESCA
SIMS,RBS TOF-SIMS, FIB
Chemicalcomposit.
Hall, CV-IV, DLTS
Electricalproperties
MBEMOCVD
Material-growth
Spectro-scopy
Micro-scopy
Ion beamtechnique
Opticalcharact.
Electricalcharact.Epitaxy
Top Related