MSE 421/521 Structural Characterization
MSE 421/521 STRUCTURAL CHARACTERIZATION
Brief syllabus:
The theory and practice of x-ray diffraction and analytical electron microscopy; the principles of modern diffractometers and electron-beam instruments, both scanning and transmission, including electron optics, imaging modes, the interaction of electrons and x-rays with matter, diffraction theory, contrast mechanisms, and basic techniques for determining chemical composition, crystal structure, orientation, and defects in crystals.
Aims:
This course will introduce students to the theory of diffraction and electron microscopy as well as the basic techniques for phase identification, microstructural characterization, chemical analysis, crystal-structure determination, and defect analysis in crystals.
Course value:
3 cu
Semester:
2
Pre-requisites (MSE 421):
Overlap courses:
MSE 305
Lectures:
Tutorials:
24
6
Limits on number:
N/A
Examinations/Coursework Marks:
Homework
Quizzes
Video Report
Participation
Final Exam
MSE 421
40% (10% x4)
36% (12% x3)
N/A
4%
20%
MSE 521
36% (9% x 4)
30% (10% x 3)
15%
4%
15%
Texts:
D. Brandon & W.D. Kaplan, “Microstructural Characterization of Materials” 2 nd
B.D. Cullity & S.R. Stock, “Elements of X-Ray Diffraction” 3 rd
ed., Wiley, 2008.
ed., Prentice Hall, 2001.
Course organizer:
Teaching Assistant:
Time
:
Location
:
Dr. R. Ubic
MEC
403K
ENGR 238
Mon & Wed, 12:00 – 1:15
A+
A
A-
B+
B
B-
C+
C
C-
97%
90%
87%
85%
78%
75% D+
71% D
63% D-
60% F
55%
45%
40%
0%
Waves and particles
Electro-magnetic radiation, structure of atoms, wave/particle duality, interaction of x-rays and electrons with atoms, diffraction
X-Ray Diffraction
X-ray generation/detection, Bragg’s Law, diffractometers, phase identification/quantification, calculation of lattice parameters, texture, residual stress, and crystallite size.
Microscopy with Light and Electrons
: Methods of image formation, optical microscopy, magnification, resolution, depth of field, lens aberrations, electrons vs light
Syllabus
Transmission Electron Microscopy
: Electron generation, magnetic lenses, scattering, secondary effects, instrument, contrast mechanisms, HVEM,
STEM, sample preparation, Electron diffraction
(geometry, reciprocal lattice, kinematical vs dynamical theory, spot patterns, Kikuchi patterns)
Scanning Electron Microscopy
: Instrument, optics, performance, resolution, sample preparation, topographical/compositional images,
EBSD, low-voltage microscopy, ESEM, EBIC
Chemical Analysis:
EDS, WDS, AES, CL, quantitative analysis, EELS
R. Ubic, Spring 2016

MSE 421/521 Structural Characterization
Reading Assignments
A reading assignment is given for almost every lecture period. The content will have a significant overlap with the lecture but will also contain additional complimentary material.
Homework
Seven homework assignments will be assigned throughout the semester. Students are encouraged to collaborate on homework assignments, but copying
is not acceptable
.
4.
5.
6.
7.
Rules for Homework
1. All homework is to be done individually.
2.
3.
Physical quantities should be reported with both the numerical value
and unit
Diagrams and drawings must be labeled. Axes should have names and units.
.
Mark formal and numerical results clearly by double-underlining or boxing. Do NOT so mark anything else
in your answer.
Do not use red ink in drawings or diagrams.
Use of textbooks, lecture notes, and calculators is allowed for homework.
Show ALL your work. Do NOT submit electronically-generated results (MS Word,
8.
Excel, etc.
) unless otherwise instructed.
Homework sheets will be marked and returned within one week of their due date.
Late Homework
Homework assignments will be posted at least one week before they are due; therefore, students should plan accordingly. Late homework will not be accepted
under any circumstances.
Quizzes
Four quizzes will be scheduled throughout the semester. Apart from the first one, which will only cover the content of the course syllabus, all quizzes will generally cover the content of previous lectures and reading assignments. Each of these quizzes will cover roughly one third of the course. One quiz may be dropped from the final quiz mark.
Missing Quizzes
Quizzes cannot be taken late without a doctor's note and, in any event, never later than one week after the original quiz date. The doctor’s note must clearly indicate the name of the patient, the symptoms/diagnosis, and dates affected. The note must be delivered to either Dr. Ubic or your course advisor as soon as possible and, in any event, within one week of the date of the quiz.
Final Exam
There will be a comprehensive final exam for this course on Monday,
2 May 2016, 12:30 – 2:30
.
It will cover the entire content of the course.
Academic Honesty
The BSU policy on academic honesty is covered on p. 22 of the 2015-16 undergraduate catalog: http://registrar.boisestate.edu/undergraduate/files/2015/08/2015-2016-undergraduate-catalog.pdf
and p. 20 of the 2015-16 graduate catalog: http://graduatecatalog.boisestate.edu/wp-content/uploads/2015/07/2015-2016-Catalog.pdf
R. Ubic, Spring 2016

MSE 421/521 Structural Characterization
Presentation – Just a Minute
On Monday,
25 April 2015
, an exercise will be played like a panel game in which students will be challenged to speak on a subject for one minute
without hesitation
, repetition, or deviation.
Subjects relevant to the content of MSE 421/521 will be chosen by the instructor and/or other members of the class. Students score a point for making a correct challenge against whomever is speaking, while the speaker wins a point if the challenge is deemed incorrect by the instructor; however, if a particularly insightful, obscure, or witty remark sufficiently enlightens or amuses the class, even if not a correct challenge, both the challenger and speaker may gain a point, at the instructor’s discretion. A student who makes a correct challenge takes over the subject for the remainder of the minute, or until he or she is correctly challenged. The person speaking when the 60 seconds expires also scores a point. An extra point is awarded when a student speaks for the entire minute without being challenged.
For the purposes of this exercise:
•
•
•
"Hesitation" can be a momentary pause before resumption of the subject, tripping over one's words, pausing for dramatic/comic effect, or waiting during laughter (or applause!).
"Repetition" means the repeating of any word or phrase, although challenges based upon very common words such as "and" will generally be rejected except in extreme cases.
Words contained in the given subject are exempt unless repeated many times in quick succession.
"Deviation" means straying from the subject but can also be interpreted as deviation from the English language as we know it, deviation from grammar as we understand it, deviating from the truth, or deviation from logic, although leaps into the surreal may sometimes be allowed.
Points scored during
Just a Minute
will be included in the course participation mark.
Participation
Credit will be awarded for attendance and participation during class and for submitting all required coursework. In order to receive full credit for participation, a student must be present
to participate in the
Just a Minute
exercise when called upon to do so. In addition, extra credit will be given to the whole class if a 100% response rate is achieved in the end-of-term course evaluations.
Office Hours
MEC 403K or as indicated on whiteboard
Mondays 11:00 – 12:00
Tuesdays 10:00 - 11:00
Wednesdays 3:00 – 4:00
I am usually able to help you at other times as well. Just stop by my office or email me for an appointment to be sure I'll be in.
R. Ubic, Spring 2016

MSE 421/521 Structural Characterization
Learning Outcomes:
By the end of this course, students should be able to:
1.
Demonstrate a working knowledge of x-ray diffraction techniques and applications
2.
Demonstrate an understanding of the fundamentals of optics, including magnification, resolution, aberrations, and depth of field.
3.
Describe the generation of x-rays and electrons and their interactions with matter.
4.
Index diffraction patterns including x-ray diffractograms, electron spot patterns, and
Kikuchi patterns and explain variations in intensity in terms of structure factors.
5.
Explain the operating principles and construction of XRDs, SEMs, and TEMs.
6.
Explain the generation of x-rays in a specimen and compare/contrast various chemical analysis techniques, including EDS, WDS, Auger, and EELS.
Practical Training
All students will be allowed up to three hours of time, fully subsidized by the MSE department, in which to train on XRD, SEM, or TEM instruments within the BSCMC with BSCMC personnel; however, this training must be done in student groups of at least two but no more than three. If two students train together, their total time is six hours. If three students train together, then a total of nine hours is allowed. Students are not allowed to use this class subsidy to train individually
, although they may make such arrangements outside of class at the expense of their research advisor.
MSE 521 - Report
Students registered for MSE 521 will additionally be expected to create a five-minute video presentation on a topic that demonstrates an application of either electron microscopy or x-ray diffraction and answer questions about the topic during class on
27 April
. Further details of the assignment will be discussed later in the semester.
The video must be submitted in electronic format by 4:00pm on
Monday, 25 April.
Repeats/Withdrawals
Effective Spring 2014, students may register for a course a maximum of two times. Graded courses and withdrawals (Ws) count as attempts. If you need to enrol in a course for a third time, you are required to seek approval from the academic advisor of your major and the chair of the department offering the course. The approval form is available at: http://registrar.boisestate.edu/wp-content/uploads/2011/07/Exceed-Max-Registrations.pdf
The university allows for a maximum number of six repeats on your official academic record.
Courses you have repeated prior to Spring 2014 do not apply to the maximum. The official count of repeats begins Spring 2014.
The university allows for a maximum number of ten Ws on an academic record exclusive of
Complete Withdrawals (CWs). If you have withdrawn from a course prior to Spring 2014, it does not apply to the maximum. The official count of Ws begins Spring 2014.
R. Ubic, Spring 2016

MSE 421/521 Structural Characterization
When ordered to evacuate or when alarms are activated, always leave immediately.
Exit quickly and calmly using nearest emergency escape routes and marked exits and proceed to safe assembly locations as identified in the evacuation map for your classroom.
Do not use elevators.
Be alert for trapped, injured or other persons needing assistance. See
EVACUATION ASSISTANCE below.
Do not return to an evacuated building unless directed to do so by authorities.
Be alert for mobility-impaired, trapped, injured or other persons needing assistance.
Help those persons requiring assistance to get to a designated Evacuation
Assistance Area if it is safe to do so. These areas are identified in the
EDUCATION BUILDING EVACUATION AND SAFETY EQUIPMENT MAP on following page. First responders will tend to those in evacuation assistance areas as soon as possible after arriving.
Transporting of individuals requiring evacuation assistance up or down stairwells must be avoided unless imminent life-threatening conditions exist.
Notify emergency personnel immediately upon their arrival of the exact location of any injured or trapped persons, those waiting in designated Evacuation Assistance
Areas and any others who may be anywhere in the building.
If first responders are summoned and you have specific knowledge relating to the emergency, meet with them upon arrival outside the building on S. Manitou Ave.
The Boise State Emergency Response Guide can be found on-line at: http://coen.boisestate.edu/safety/coen-emergency-response/
R. Ubic, Spring 2016

MSE 421/521 Structural Characterization
Evacuation & safety-equipment map
ET Building 2 nd floor
*
You are here.
Fire Alarm Pull
Station
Fire Extinguisher
AED- MEC 2 nd
Floor, Opposite
Elevator
Emergency Phone
Evacuation
Assistance Area
R. Ubic, Spring 2016

MSE 421/521 Structural Characterization
Avogadro’s number
Symbol
Speed of light in vacuum c
Planck’s constant h e
Charge on an electron
Rest mass of an electron m o
N A
Value
6.62606876
×
10 -34
Units
2.99792458 × 10 8 ms -1
Js
1.602176462 × 10 -19 C
9.10938188 × 10 -31 kg
6.02214199 × 10 23 mol -1
λ wavelength
ν
E m v
V potential difference
Units of convenience
(not SI but sometimes used)
Hz Hertz = cycles per second, same as s –1 but easier to say eV electron volts = energy in Joules divided by the charge on an electron, often used with electron beam instruments as it gives numbers that are easier to handle, e.g.
, 2.4 × 10 -16 J = 1.5 keV
Å frequency energy mass velocity angstrom units = 10 -10 m, i.e.
. 0.1 nm often used as it is similar to atomic dimensions, e.g.
, radius of gold atom = 1.442 Å (0.1442 nm)
R. Ubic, Spring 2016

MSE 421/521 Structural Characterization
Acronym Meaning: Associated with:
AES Auger electron spectroscopy Specialised surface analysis technique
BEI
CA
EBSD
ECP
Backscattered electron imaging
Condenser aperture
Electron backscatter diffraction
Electron channelling pattern
Image mode in SEM
Microscopy
Crystallographic information in SEM
Crystallographic information in SEM
EDS
EELS
Energy dispersive x-ray spectroscopy
Electron energy loss spectroscopy
Chemical analysis mode in EMs
Chemical analysis mode in TEM
EM Electron microscopy Microscopy techniques
EMPA Electron microprobe analysis (aka microprobe) Specialised SEM (=EPMA)
EPMA Electron probe microanalysis (aka microprobe) Specialised SEM (=EMPA)
ESCA
FEG
FIB
HR
OA
OM
SAD
Electron spectroscopy for chemical analysis
Field emission (electron) gun
Focused ion beam
High resolution
Objective aperture
Optical microscopy
Selected area diffraction
Specialised surface analysis (=XPS)
Type of electron source in HR EM
Electron microscopes (spec. prep.)
In EM, i.e.
, HRSEM, HRTEM
Microscopy
Microscopy technique
Type of diffraction pattern in TEM
SAM
SEI
SEM
Scanning Auger microscopy
Secondary electron image
Scanning electron microscope
Specialised surface analysis technique
Image mode in SEM
Electron microscope
STEM
TEM
WDS
Scanning transmission electron microscope
Transmission electron microscope
Electron microscope
Electron microscope
Wavelength dispersive spectroscopy (of X-rays) Chemical analysis mode in SEMs
WEDS Windowless EDS
XPS X-ray photoelectron spectroscopy
XRD
ZAF
X-ray diffraction
Atomic number, absorption and fluorescence
Chemical analysis mode in EMs
Specialised surface analysis (=ESCA)
Crystallographic analysis technique
Correction for quantitative EDS, WDS
R. Ubic, Spring 2016