MSE 421/521 INTRODUCTION TO ELECTRON MICROSCOPY

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MSE 421/521 Introduction to Electron Microscopy
MSE 421/521 INTRODUCTION TO ELECTRON MICROSCOPY
Brief syllabus:
The theory and practice of scanning electron microscopy (SEM) and transmission electron microscopy (TEM),
including electron optics, contrast mechanisms, diffraction theory, chemical analysis techniques, and sample
preparation. Applications of SEM and TEM in materials science and engineering will be covered.
Aims:
This course will introduce students to the use of a Hitachi S-3400N VP SEM and a JEOL 2100 HR TEM as well
as the basic techniques for microstructural characterization, chemical analysis, crystal structure determination,
and defect analysis in crystals.
Course value:
3 cu
Semester:
2
Pre-requisites:
MSE 305/505
Lectures:
Tutorials:
29
5
Overlap courses: MSE 305/505, PHYS 423
Limits on number: N/A
Examinations/Coursework Marks:
Homework
Quizzes
Report
Participation
Final Exam
Text:
MSE 521
28% (4% x 7)
27% (9% x 3)
15%
5%
25%
MSE 421
35% (5% x7)
33% (11% x3)
N/A
5%
27%
Brandon & Kaplan, “Microstructural Characterization of Materials” 2nd ed., Wiley, Chichester, 2008.
Course organizer:
Dr. R. Ubic
MEC 302H
Teaching Assistant:
Time:
Mon & Wed, 1:40 – 2:55
Location:
MEC 307
A+
A
AB+
B
BC+
C
C-
97%
90%
87%
85%
78%
75%
71%
63%
60%
D+
D
DF
55%
45%
40%
0%
Syllabus
Microscopy with Light and Electrons:
Methods of image formation, optical
microscopy, magnification, resolution, depth
of field, lens aberrations, electrons vs light
Interaction of Electrons with Matter:
Electrons, electron generation, magnetic
lenses, scattering, secondary effects, electron
microscopes
Electron Diffraction: geometry of diffraction,
spot patterns, reciprocal lattice, other types of
diffraction
Transmission
Electron
Microscope:
Instrument, contrast mechanisms, HVEM,
STEM, sample preparation
R. Ubic
Spring 2012
Scanning Electron Microscope: Instrument,
optics, performance, resolution, topographical
images,
compositional
images,
crystallographic information, other signals,
sample preparation, low-voltage microscopy,
ESEM
Chemical Analysis: generation of x-rays, xray detection, EDS, WDS, quantitative
analysis, EELS
Other Techniques: scanning tunneling
microscopy, AFM, FIM, holography,
tomography, RHEED & LEED, atom probe
FIM, SIMS, Auger spectroscopy, XPS,
confocal microscopy, Raman and IR
spectroscopy.
MSE 421/521 Introduction to Electron Microscopy
Homework
Homework is a "practical' aspect of the course. Students may work on homework problems
during the lab while instruments are occupied by other students. Seven homework assignments
will be assigned throughout the semester.
Rules for Homework and Quizzes
1.
Show ALL your work. Do NOT submit electronic results or results in spreadsheet form
unless otherwise instructed.
2.
Physical quantities have a numerical value and a unit. Numerical results without an SI
unit will not be graded (exceptions are dimensionless quantities).
3.
Mark formal and numerical results clearly by double-underlining or boxing.
4.
Diagrams and drawings must be labeled. Axes should have names and units. Diagrams
without sufficient labeling will not be marked.
5.
Do not use red ink in drawings or diagrams.
6.
Use of textbooks, lecture notes, and calculators is allowed for homework.
7.
All homework is to be done individually.
8.
Homework sheets will be marked and returned within one week of their due date.
Reading Assignments
A reading assignment is given each week. The content will have a significant overlap with the
lectures but will also contain additional material to compliment the lectures.
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 the
reading assignment due that day, but may also require knowledge of previous reading
assignments. One quiz may be dropped from the final quiz mark.
Late Homework or Missing Quizzes
Late homework assignments will only be accepted with a valid note from a doctor clearly
indicating the name of the patient, the symptoms/diagnosis, and dates affected. The note must be
delivered to Dr. Ubic as soon as possible and, in any event, within one week of the original due
date for the assignment. In other circumstances, penalty points will be deducted by applying the
following formula to the graded assignment: (1 - n/7)M, where n is the number of days late and
M is the un-penalised grade for the work. Likewise, quizzes cannot be taken late without a
doctor's note and, in any event, never later than one week after the original quiz date.
Final Exam
There will be a comprehensive final exam for this course on 7 May 2012, 3:30 – 5:30. It will
cover the entire content of the course.
Academic Honesty
The BSU policy on academic honesty is covered on p. 22 of the 2011-12 undergraduate catalog:
http://boisestate.edu/registrar/catalogs/ug2011-2012/catalog.pdf
and p. 18-19 of the 2011-12 graduate catalog:
http://registrar.boisestate.edu/catalogs/gr2011-2012/catalog.pdf
R. Ubic
Spring 2012
MSE 421/521 Introduction to Electron Microscopy
Participation
Credit will be awarded for attendance and participation during class and for submitting all
required coursework. Marks will also be given for participation in the Just a Minute exercise.
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.
Presentation – Just a Minute
On 30 April 2012, 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 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.
Office Hours
Mondays 3:00 – 4:00
Tuesdays 9:00 - 11:00
MEC 302H or as indicated on whiteboard
R. Ubic
Spring 2012
MSE 421/521 Introduction to Electron Microscopy
Physical constants
Symbol
Value
Units
Speed of light in vacuum
c
2.99792458 × 108
ms-1
Planck’s constant
h
6.62606876 × 10-34
Js
Charge on an electron
e
1.602176462 × 10-19 C
Rest mass of an electron
mo
9.10938188 × 10-31
kg
Avogadro’s number
NA
6.02214199 × 1023
mol-1
Other Symbols
λ
wavelength
ν
frequency
E
energy
m
mass
v
velocity
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
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 2012
MSE 421/521 Introduction to Electron Microscopy
Acronyms
Acronym
Meaning:
Associated with:
AES
BEI
CA
EBSD
ECP
EDS
EELS
EM
EPMA
ESCA
FEG
FIB
HR
OA
OM
SAD
SAM
SEI
SEM
STEM
TEM
WDS
WEDS
XPS
XRD
ZAF
Auger electron spectroscopy
Backscattered electron imaging
Condenser aperture
Electron backscatter diffraction
Electron channelling pattern
Energy dispersive x-ray spectroscopy
Electron energy loss spectroscopy
Electron microscopy
Electron probe microanalysis
Electron spectroscopy for chemical analysis
Field emission (electron) gun
Focused ion beam
High resolution
Objective aperture
Optical microscopy
Selected area diffraction
Scanning Auger microscopy
Secondary electron image
Scanning electron microscope
Scanning transmission electron microscope
Transmission electron microscope
Wavelength dispersive spectroscopy (of X-rays)
Windowless EDS
X-ray photoelectron spectroscopy
X-ray diffraction
Atomic number, absorption and fluorescence
Specialised surface analysis technique
Image mode in SEM
Microscopy
Crystallographic information in SEM
Crystallographic information in SEM
Chemical analysis mode in EMs
Chemical analysis mode in TEM
Microscopy techniques
Specialised SEM
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
Specialised surface analysis technique
Image mode in SEM
Electron microscope
Electron microscope
Electron microscope
Chemical analysis mode in SEMs
Chemical analysis mode in EMs
Specialised surface analysis (=ESCA)
Crystallographic analysis technique
Correction for quantitative EDS, WDS
R. Ubic
Spring 2012
MSE 421/521 Introduction to Electron Microscopy
MSE 521 - Report
Students registered for MSE 521 will additionally be expected to complete a written report on
the use of electron microscopy in their project work. The report should be formatted like a
standard scientific manuscript as per the instructions for Materials Research Bulletin:
http://www.elsevier.com/wps/find/journaldescription.cws_home/313/authorinstructions#20000
The page limit, excluding figures, references, and appendices is 5. It should be written in 12point Times New Roman font with 1.5 line spacing and single-sided.
The report is due by 4:00 on Wednesday 25 April 2012.
Publications and Presentations Beyond MSE 421 / 521
All presentations or publications which include data from the JEOL 2100 TEM must include an
acknowledgement to the effect that the work was supported by the National Science Foundation
Major Research Instrumentation Program, Award No. 0521315.
All presentations or publications which include data from the Hitachi S-3400N SEM must
include the following acknowledgement and disclaimer:
Acknowledgment:“This material is based upon work supported by the Department of Energy
[National Nuclear Security Administration] under Award Number DE-NE0000338.”
Disclaimer: “This report was prepared as an account of work sponsored by an agency of the
United States Government. Neither the United States Government nor any agency thereof, nor
any of their employees, makes any warranty, express or implied, or assumes any legal liability or
responsibility for the accuracy, completeness, or usefulness of any information, apparatus,
product, or process disclosed, or represents that its use would not infringe privately owned
rights. Reference herein to any specific commercial product, process, or service by trade name,
trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement,
recommendation, or favoring by the United States Government or any agency thereof. The views
and opinions of authors expressed herein do not necessarily state or reflect those of the United
States Government or any agency thereof.”
Learning Outcomes:
By the end of this course, students should be able to:
1. Demonstrate an understanding of the fundamentals of optical microscopes, including
magnification, resolution, aberrations, and depth of field.
2. Describe generation of electrons and their interactions with matter.
3. Index electron diffraction patterns including spot patterns, Kikuchi patterns, and EBSD
patterns and explain variations in intensity in terms of structure factor.
4. Explain the operating principles and construction of both SEMs and TEMs.
5. Explain the generation of x-rays in a specimen and compare/contrast various chemical
analysis techniques, including EDS, WDS, Auger, and EELS.
R. Ubic
Spring 2012
MSE 421/521 Introduction to Electron Microscopy
Marking Scheme for MSE 521 Written Report
Name of Student:
Examiner:
Criterion
Organisation and Structure:
20% of Total Mark
Are section headings listed and page
numbers given? Is the report set out in a
sensible order? Does the abstract
adequately convey the aims, outcomes and
conclusions of the project? Is the report
easy to follow? Are the references cited in
a consistent format?
Introduction/Literature Survey:
20% of Total Mark
Does the literature survey progress
logically from the general background to
the specific subject matter of the project?
Mark (%)/Comments
%
%
Is sufficient information given on how
SEM/TEM can advance the project? Are
different methods described?
Experimental Details:
20% of Total Mark
Are the sample preparation details given
sufficient to allow someone else to repeat
this work? Are they appropriate? Are the
models, manufacturers and locations of
manufacturers of equipment given? Are
the grades, purities and sources of
reagents cited?
Results:
25% of Total Mark
Are the results clearly set out? Are
sufficient results presented? Have they
been fully analysed?
Outlook:
15% of Total Mark
%
%
%
Is there a critical evaluation of the use of
electron microscopy for this project? Are the
next steps in the project discussed?
TOTAL
R. Ubic
Spring 2012
%
MSE 421/521 Introduction to Electron Microscopy
EVACUATION PROCEDURE
EVACUATING YOUR BUILDING OR WORK AREA:
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.
EVACUATION ASSISTANCE
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 COLLEGE OF
ENGINEERING BUILDING EVACUATION AND SAFETY EQUIPMENT MAPS on
following pages. 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.
MEETING FIRST RESPONDERS
If first responders are summoned and you have specific knowledge relating to the
emergency, meet with them upon arrival. The first responders will typically stop at the
following locations:
Engineering and Technology Building- University Dr.
Micron Engineering Center- Manitou Ave.
Harry Morrison Civil Engineering Building- Euclid Ave.
Construction Management Lab Bldgs- Belmont St. or Manitou Ave.
The College of Engineering Emergency Response Guide can be found on-line at:
http://coenintranet.boisestate.edu/Safety/COENEmergencyResponse/tabid/75/Default.aspx
R. Ubic
Spring 2012
MSE 421/521 Introduction to Electron Microscopy
*
R. Ubic
Spring 2012
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