MSE 206-Materials Characterization I INTRODUCTION MSE 206-Materials Characterization I

Course Syllabus Aim: The aim of this course is to familiarize the students with the fundamentals of microstructural characterization, basics of geometric optics and light microscopy. Both theoretically and practically, the students will have the chance to learn how to work on an optical microscope and determine typical microstructures of ferrous as well as nonferrous metallic materials. Methods of Instruction Theor. Appl. Lab. Total Credit ECTS Credit 42 - (2 4 4) 6 Semester Spring 2016 – 2017 Instructor Assoc Prof. Dr. Ziya Esen, Materials Science and Engineering Dept. Room: NB-16, e-mail: ziyaesen@cankaya.edu.tr Assistant Ezgi Bütev, Materials Science and Engineering Dept., NC-09; e-mail: ebutev@cankaya.edu.tr Emre Yılmaz, Materials Science and Engineering Dept., NC-08; e-mail: emreyilmaz@cankaya.edu.tr Schedule Lecture Hours : Wednesday 09:20-11:10 Laboratory Hours : Wednesday 13:20-17:10 (section 01) Friday 09:20-13:10 (section 02) Friday 13:20-17:10 (section 03)

Textbook Textbook: There is no recommended specific textbook in metallography in the English language. For this reason the students are asked to attend the lectures regularly and take notes. Relevant class material will be posted on www.mse206.cankaya.edu.tr Book Author Pub. Inf. Introduction to Optical Microscopy Jerome Mertz Roberts and Company Publishers, 2009 Metallography Principles and Practice George F. Vander Voort ASM International, 1999 Optics Eugene Hecht Addison Wesley, 4th Edition 2002. Encyclopedia of Materials Characterization R. Brundle, C. Evans, S. Wilson Butterworth-Heinemann, 1992 Experimental Techniques in Materials and Mechanics C. Suryanarayana CRC Press, Taylor and Francis Group, 2011 Optical Techniques for Solid State Materials Characterization Rofit P. Prasankumar and Antoinette J. Taylor CRC Pres, Taylor and Francis Group, 2011 Fundamentals of Light Microscopy and Electronic Imaging Douglas B. Murphy Wiley-Liss; 1st edition, 2001 Microstructural Characterization of Materials David Brandon, Wayne D. Kaplan Wiley, 2008 Physical Principles of Electron Microscopy: An Introduction to TEM, SEM, and AEM R.F. Egerton Springer, 2010 Fractography: Observing, Measuring and Interpreting Fracture Surface Topography Derek Hull Cambridge University Press, 1999

Laboratory In the metallography lab, each student is assigned to a microscope and she/he will be held responsible to look after it well. Lab schedule is handed out in the class. Pop quizzes will be given in each lab hour. In addition to this, students are required to complete lab reports each week. Term Project: Each student will be given a metallic sample of unknown composition and microstructure. Using the necessary characterization tools available in our department the student will try to determine the alloy composition, microstructure, hardness etc. of the unknown sample. Based on the obtained information the student will comment on the processing as well as possible heat treatment history of the sample and typical applications of the alloy with the determined properties. The term projects are due the last day of classes.

Attendance&Grading Attendance 70% attendance of all lecture hours and 80% attendance of all laboratory hours is required by the university’s regulations. Absence from a quiz, lab. or an examination will result in zero grade. Grading Policy Laboratory work(Quiz+ HW) & Lab exam.......................…................... 20% Term Project………………………………....................................………. 10% Midterm s (I&II).................……………...............................…………...... 40% Final………………………………………....................................………... 30%

Tentative Course Outline

Weekly Lab Topics Metallographic Specimen Preperation Optical Microscopes Macro-examination, Inclusions and Solidification Structures Equilubrium cooled Fe-C Structures Isothermal Transformation Fe-C Structures Non-Equilubrium Structures Cast Irons Plastically Deformed and Surface Treated Structures Nonferrous Metallography Scanning Electron Microscopy Transmission Electron Microscopy Quantitative Metallography

Introduction to Materials Characterization techniques

Materials Optimization Loop Material science is the investigation of the relationship among processing, structure, properties, and performance of materials.

Structure 1) Sub atomic – electrons and nuclei (protons and neutrons) 2) Atomic – organization of atoms or molecules 3) Microscopic – groups of atoms that are normally agglomerated together 4) Macroscopic – viewable with the un-aided eye 1 Ao = 10-10 m 1 nm = 10-9 m 1 m = 10-6 m 1 mm = 10-3 m 1 cm = 10-2 m

Property - A material trait expressed in terms of the measured response to a specific imposed stimulus Hardness Strength Ductility, etc. Resistivity Conductivity Mag. permeability Index of refraction Reflectivity Ther. conductivity Heat capacity + Deteriorative Properties: Relate to the chemical reactivity of materials

(mechanical, electrical&magnetic, optical, thermal) of materials Why Materials Characterization is Necessary ? Properties (mechanical, electrical&magnetic, optical, thermal) of materials depend on internal structure (in microscopic and atomic level ; bonding, crystal structure and composition) Characterization is needed to identify the material and predict material properties, as well as processing conditions Some characterization techniques are qualitative, such as providing an image of a surface, others yield quantitative information such as the relative concentrations of atoms that comprise the material. Qualitative – what is present? Quantitative – how much is present?

Categories of Materials Characterization Techniques 1) Image 2) Surface 3) Structural 4) Organic 5) Elemental

SPM – Scanning Probe Microscopy AFM – Atomic Force Microscopy 1)Image Analysis Optical microscopy Confocal microscopy SEM/EDX – Scanning Electron Microscopy with Energy Dispersive X-Ray detector SPM – Scanning Probe Microscopy AFM – Atomic Force Microscopy TEM – Transmission Electron Microscopy

1)Image Analysis p-n ZnO nanowires by SEM

AES – Auger Electron Spectroscopy Surface Analysis AES – Auger Electron Spectroscopy XPS – X-Ray Photoelectron Spectroscopy TOF-SSIMS – Time of Flight Static Secondary Ion Mass Spectroscopy LEED – Low Energy Electron Diffraction

Surface Analysis XPS – X-Ray Photoelectron Spectroscopy: gives information from 1-10 nm depth. XPS results of Titanium surface Binding Energies (eV) Sample

XRD – X-Ray Diffraction Structural Analysis XRD – X-Ray Diffraction XAX/EXAFS - X-ray Absorption Spectroscopy  and Extended X-Ray Absorption Fine Structure Raman spectroscopy TEM – Transmission Electron Microscopy EELS – Electron Energy Loss Spectroscopy (typically combined with TEM)

FTIR – Fourier Transform Infrared Spectroscopy Organic Analysis FTIR – Fourier Transform Infrared Spectroscopy GC/MS – Gas Chromatography with Mass Spectroscopy (detector) HPLC – High Performance Liquid Chromatography Raman spectroscopy (structural organic)

ICP – Inductively Coupled Plasma XRF – X-Ray Fluorescence Elemental Analysis ICP – Inductively Coupled Plasma XRF – X-Ray Fluorescence PIXE - Particle-Induced X-ray Emission Optical atomic spectroscopy CHN (Carbon / Hydrogen / Nitrogen)

Scope of ‘’Materials Characterization I’’ Course Some Image Characterization Techniques: 1-Light (optical) microscopy (LM) or (OM) 2-Scanning electron microscopy (SEM) Energy dispersive X-ray spectroscopy (EDS) 3-Transmission electron microscopy (TEM)

Electron Microscopes vs. Optical Microscope Optical Microscope uses visible light (photons, 0.4-0.7 m wavelength). Contrasts in the image produced result from differences in reflectivity of the various regions of the microstructure. Transmission Electron Microscope (TEM) uses a wide beam of electrons passing through a thin sliced specimen to form an image. Scanning Electron Microscope (SEM) uses focused beam of electrons scanning over the surface of thick or thin specimens.. Images are produced one spot at a time in a grid-like raster pattern. (will be discussed in a later lecture)

Electron Microscopes vs. Optical Microscope

Electron Microscopes vs. Optical Microscope Transmission Electron Microscope, TEM Optical Microscope Scanning Electron Microscope, SEM

Resolution Scale of Different Methods

Resolution Scale of Different Methods XRD,TEM,STM SEM OM Grain I Grain II Valve Turbo charge Atomic atomic Large defects, voids, inclusions by OM; grain and size distribution by either OM and SEM depending scale; Grain boundary and interface by TEM, Crystal structure by XRD and TEM.

IMAGES: OM vs SEM Optical Microscope image of a polycrystalline material BaTiO3 Depth of field 50m Scanning Electron Microscope image of a polycrystalline BaTiO3 5m Optical microscopy provides 2-dimensional image whereas SEM is able to show 3-dimensional features

Identification of Fracture Mode by SEM Pores Cracks Cracks Grain boundary Processing-microstructure-property relationships! 4m 20m Intergranular fracture Intragranular fracture

SEM Images                           Pollen Butterfly Tongue Fire ant head Spider

SEM Images flue virus Snow crystals

Transmission Electron Microscopy Schematic view of carbon nanotubes TEM image of carbon nanotubes

Transmission Electron Microscopy TEM imaging of graphene

Transmission Electron Microscopy Dislocations TEM image of deformed 316 stainless steel showing dislocations and dipoles on (111) planes.

Transmission Electron Microscopy Close view of TEM images of some nano-catalysts.

Homework-I Write a short report about; Similarities and differences between optical (light), Scanning electron microscope (SEM) and Transmission Electron Microscopes (TEM)