Course Plan Aims of the course Course lectures Course examination Course projects Seminars

1. 90 nm Bending a silicon nano-whisker inside the TEM-STM instrument. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRODUCTION • Course Plan • Aims of the course • Course lectures • Course examination • Course projects • Seminars • Course literature • Survey over Materials Characterisation

2. CHALMERS / Göteborg UniversityGraduate School in Materials ScienceCharacterisation FTF155INTRODUCTION- Aims • The course is directed to Ph.D students andMasters 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

3. DIFFRACTIONA short theoretical introduction to diffraction of x-rays, neutrons and electrons by solid matter SURFACE ANALYSISTechniques for surface and interface analysis are reviewed, e.g.XPS, AES, SIMS MICROSCOPYAn introduction to AP-FIM, STM/AFM and electron microscopy SPECTROSCOPYBasic concepts of NMR, Raman and Infrared spectroscopy CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRODUCTION- Lectures

4. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRODUCTION- 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.

5. CHALMERS / Göteborg UniversityGraduate School of Materials Science Characterisation FTF155INTRODUCTION- Projects(1) • A compulsory project work is included in the courseThe 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.

6. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRODUCTION- 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. • 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. 

7. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRODUCTION- Projects(3) PROJECT REPORT (deadline Dec. 30) • 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 techniquesnot used in your present project. • The oral presentation is planned to be a 12 minutes presentation and 3 minutes discussion of each project.

8. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRODUCTION- Seminars Three seminars will be given after the lecture presentations with invited guests from academy and industry ; • Jan-Olov Nilsson (Sandvik /CTH): Industrial use of characterisation techniques in the Sandvik materials laboratory • Jukka Lausmaa (SP Borås): Presentation of applications using TOF-SIMS and MALDI • Magnus Hellsing (Högskolan Dalarna): Presentation of AES-use in consulting work

9. 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 Literature1. 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 04719534073. Surface Characterization;a users handbook. Ed. D. Brune et al, John Wiley, ISBN 3-527-28843-0, 19964.Encyclopedia of Materials Characterisation, Ed C.R,BrundleManning Publ. Co., ISBN 0-7506-9168-9, 1992 WEB-SITE; Charles Evans & Ass.http://www.cea.com CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRODUCTION- Literature

10. A widespread applicability of materials characterisation in manufacturing industry 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 UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey

11. Thermodynamicsenthalpiessegregation energiesbond strengthsphase transtions Time evolutionkinetics Compositionelementalchemical composition and bonding Structuredefectscrystalline orientation Microstructure and Topography CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey Which property of the material do we want to characterise?

12. Surfaceconcentrations, maps, profiles and sections Bulk Interfaces CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey Which part of the material do we want to characterise? How to select the appropriate method/s to characterize the material in question?

13. Are quantitative results needed, or is qualitative identification sufficient? Quantitative analysis with high precision is difficult and expensive CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey Is an identification of the chemical compound needed or is the elemental composition sufficient? 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

14. Modification induced by the analytical procedure CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155Characterisation survey-Quality 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. Limitations imposed by the analysis environment Surface-layer-induced limitations Other limitations

15. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey • LIGHT MICROSCOPY (LM)The interpretive use of Light Microscope.Should be used initially in all analytical workIs 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!!

16. SIMS(Secondary Ion Mass Spectrometry) Surface and layer compostion NMR(Nuclear Magnetic Resonance) Chemical state 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 distributionsNMR 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 UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey

17. TEM, SEM (Transmission/Scanning Electron Microscopy) AES(Auger Electron Spectr.) Near-surface composition, chemical state 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 UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey

18. AP - FIM (Atom Probe-Field Ion Microscopy) XRD(X-ray Diffraction)Crystallographic structure Neutron Diffractionmolecular structure, magnetic ordering X-ray diffraction has been carried out at extreme glancing angles of incidence where total reflection ensures surface sensitivity.. Neutron diffraction is rather characterising bulk properties. Neutron diffraction can provide structural information on adsorbed molecules and surface phase transitions. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey

19. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRO.-Characterisation survey NOBEL PRIZE Awards • Physics 1914, Max von LaueX-ray diffraction • Chemistry 1922, Francis AstonMass-spectroscopic separation of isotopes (”SIMS”) • Physics 1924, Manne Siegbahn X-ray spectroscopy • Physics 1930, Venkata RamanThe scattering of light,Raman-effect • Physics 1981, Kai SiegbahnHR photoelectron (ESCA) • Physics 1986, G. Binnig, H. RohrerScanning tunneling microscopy • Physics 1986, Ernst RuskaElectron Microscopy • Chemistry 1991 Richard ErnstDevelopment of NMR spectroscopy • Physics 1994, Clifford ShullNeutron diffraction

20. CHALMERS / Göteborg UniversityGraduate School of Materials ScienceCharacterisation FTF155INTRODUCTION- ”Physics”