INTRODUCTION - Chalmersfy.chalmers.se/gsms/Intro.pdfe.g. XPS, AES, SIMS MICROSCOPY An introduction to AP-FIM, AFM and electron microscopy ... Physics 1986, Ernst Ruska Electron Microscopy

CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155

INTRODUCTION

Materials Science:Characterisation

Bending a silicon nano-whisker inside the TEM-STM instrument.

90 nm

[email protected]


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

[email protected]

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




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


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


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.


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.



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.



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.


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


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


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)



Thermodynamicssegregation energiesbond strengthsphase transtions

Time evolutionkineticsdynamics

Compositionelemental compositionchemical compositionand bonding

Structuredefectscrystalline orientation

Microstructure andTopography

Which property of the material do we want tocharacterise?



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?



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


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



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!!



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.



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.



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.



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



Physics 1986, G. Binnig, H. RohrerScanning tunneling microscopy

Physics 1986, Ernst RuskaElectron Microscopy

Chemistry 1991 Richard ErnstDevelopment of NMR

Physics 1994, G. ShullNeutron diffraction


INTRODUCTION- ”Physics”

Detection

Raman,XRF,XRD,NMR

PIXEEPMAPhotons

SNMSSALI

Neutrals

LAMMALIMA(AP-FIM)

FABMSSIMSRBS,ISS,FIB

ESDESDIAD

Ions

UPS,XPS

INSAES,SEMEELS

Electrons

PhotonsNeutralsIonsElectronsExcitation


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

Documents

INTRODUCTION - Chalmersfy.chalmers.se/gsms/Intro.pdfe.g. XPS, AES, SIMS MICROSCOPY An introduction to AP-FIM, AFM and electron microscopy ... Physics 1986, Ernst Ruska Electron Microscopy