MSE 104 – Materials

Characterization
Instructor: Mary Scott (mary.scott@berkeley.edu)

316 HMMB | Wednesday 2-3PM and Friday 2-3PM

GSIs:
Ian Lin: ian.lin@berkeley.edu (Tuesdays, 9:30-10:30am, 240 HMMB)
Kirill Popov: popkir@berkeley.edu (Monday, 5-6pm, 240 HMMB)
Bethany Smith: bbsmith5@berkeley.edu (Fridays, 11am-12pm, 240 HMMB)
Important Info

• Read the syllabus! Most of your questions

can be answered there.
• Text: Text: B.D. Cullity and S.R. Stock,
Elements of X-ray Diffraction, 3rd Edition,
Prentice Hall, Upper Saddle River, NJ, 2001.
– There is a copy on reserve in the engineering
library
– There will be supplemental texts and
handouts for portions of the course
Homework..
• Homework (20% of total grade, 2% for each assignment)
• Homeworks may be completed in groups of 2 students (but no more than 2)
or you may choose to work independently
• Each individual student must turn in an individual version of each homework
online
• Homework pairs must clearly indicate partner
• Similarities and correlation of solutions within the homework pair are
expected, verbatim copying of one another solutions is not allowed
• If you work out how to do the problem together, then write-up your final
solutions separately
• Strong correlation between the solutions of different pairs’ homeworks will
lead to additional scrutiny. Cheating/identical solutions will result in zero
credit.
• Homeworks are to be turned in online (bCourses) by the start of class (12:10PM)
on each of the noted due dates
• Homeworks must be turned-in in .pdf format and done in word processor* with
equation editor, graphs done in graphing software
• No late homeworks will be accepted
Exams and final
• Exams (25% of total grade, 12.5% for each exam)
• There will be two (2) 50 minute, in-class exams, occurring
on Feb. 27, 2015 and the other on April 10, 2014
• No makeup exams: valid reason for missing an exam is
required
• Final Examination (20% of total grade)
• The final examination is cumulative
• The exam will take place on May 10, 2016 from
3:00-6:00PM
• There will be no makeup exams. If you have a valid reason
for missing an exam (e.g., doctor’s excuse, death in the
family, school-sponsored activity, etc.) I will work with you
to reach an acceptable time to take the exam. Cases will be
dealt with on a case-by-case process
Lab time and reports
• We will divide most sections into “A” and “B” weeks to allow
for more individual interaction with the lab equipment.
• Divisions will look like this:

MSE 104 Lab M Tu W Th F

Week A 8:00-11:00AM 105A 104A

2:00-5:00PM 101A 102A 103A

Week B 8:00-11:00AM 105B 107B

2:00-5:00PM 101B 102B 103B

Lab time and reports
• Reports must be completed following the guidelines
outlined in the Laboratory Guide (available online)
• Laboratory reports are submitted electronically through
bCourses and are due 1 week from the end of your
laboratory
• Example: if you are in laboratory section 105A, your
report will be due online by 11:00AM on the next
Tuesday (week B)
Course policies
• Late Assignments
• No late assignments will be accepted unless prior arrangements
are made with the instructor for valid excuses
• Valid excuses include, but are not limited to, deaths in the family,
jury duty, hospitalization for illness, etc. (documentation required)
• Non-valid excuses include, but are not limited to, “I didn’t get it
submitted to bCourses soon enough,” oversleeping, “my internet
was out,” “I wasn’t here when you assigned it,” etc.
• If you have concerns I am happy to discuss with you about your
specific situation and clarify any questions you have.
• Re-grading Policy
• The Instructor and University take this very seriously
• A complete process by which regarding should take place is
provided in the syllabus. It requires a written submission.
• Attendance: Lab attendance is mandatory. Justified absences will be
dealt with on a case-by-case basis.
Academic code of conduct
• This course will execute a “zero-tolerance” policy concerning
cheating and plagiarism
• Students are referred to the University of California, Berkeley
Student Code for complete details on the Student Code. Special
attention should be given to Section V and Appendix II of (http://
sa.berkeley.edu/code-of-conduct)
• Cheating and plagiarism will be dealt with according to established
campus policy
• Students caught cheating will receive a failing grade
• What is cheating?
• Copying from your classmate, Wikipedia, other references…
• Utilization of course materials from previous versions of this
course (i.e., homeworks, exams, laboratory reports, etc.)
• Having your homework partner do this week’s homework because
you will do the assignment next week
• Expectation of professional conduct – students, GSIs, staff, etc.
Laboratory expectations
• Be on time. Late is absent, and attendance is mandatory.
• Before you arrive in laboratory you should have read completely the
Laboratory Guide and the Laboratory Manual for that week’s lab section
• If you fail to follow this simple guideline, you will be asked to leave
the laboratory to assure the safety of yourself and others and efficient
utilization of the resources
• Work efficiently and effectively
• Work safely – if you aren’t sure what to do…STOP and ASK
• Carefully note down your actions, issues, challenges
• Understand the hazards around you and how to keep yourself and others
safe
• This is a chance to pick up GOOD habits
• Laboratory attire – Wear long pants, closed-toe shoes, no loose/baggy
things
• The Laboratory Guide is full of good tips and hints on how to make a good
laboratory report and notebook.
MSE 104 Course Goals
• In-depth knowledge of XRD
• Working knowledge of TEM and SEM
• Introduction and basic comfort level with scanning probe and
spectroscopic methods.
• Be excited about characterization!

Overall, I want you to be comfortable with a variety of

characterization methods. I want you to understand how
they are used and what their limitations are.
What is materials characterization?
Old school:
• Visual inspection – color, surface texture, size, shape…
• Other senses – smell of wood, sound of metal, feel of glass
• Weight, density
• For millennia materials were picked empirically for the task at
hand – what makes a good hammer?

Modern characterization:
• Atomic structure and composition
• Crystalline or amorphous?
• Crystal structure/orientation?
• Crystallite size/morphology?
• Defects types – point, line, planar, volume?
• Role of effects – residual stress, chemical?
• Real-time analysis
Modern materials characterization
Basic science
• What is the material?
• What is it made of?
• What is the arrangement of the atoms? Grains?
• How does that structure impact properties?

Engineering
• Was the material manufactured to spec?
(structure, composition)
• What caused the catastrophic failure in service?
• Residual stress? Flaws? Corrosion?
• How might one better engineer a material for a
specific application?
• Nanostructuring? Multi-functionality?
Atomic electron tomography: 3D
structures without crystals
Dr. Scott’s own research in characterization
Jianwei Miao,* Peter Ercius, Simon J. L. Billinge
Atomic resolution electron
BACKGROUND: To understand material prop-
erties and functionality at the most fundamen-
identical
ture determination of macromolecules with
or similar conformations at near-atomic seeing where atoms
live in 3D!
tal level, one must know the three-dimensional
resolution, this method cannot be generally applied
(3D) positions of atoms with high precision. For
to the physical sciences for the following three
crystalline materials, x-ray crystallography has
provided this information since the pioneering
work of Max von Laue, William Henry Bragg, and
William Lawrence Bragg around 100 years ago.
But perfect crystals are rare in nature. Real ma-
terials often contain defects, surface reconstruc-
tions, nanoscale heterogeneities, and disorders,
which strongly influence material properties and
performance. Completely different approaches
from crystallography are needed to determine
the 3D atomic arrangement of crystal defects
and noncrystalline systems. Although single-
particle cryo–electron microscopy (cryo-EM)
has been under rapid development for 3D struc-
tomography:
reasons. First, most materials do not have identical
copies and cannot be averaged to achieve atom-
ic resolution. Second, a priori knowledge of the
peptide sequence and stereochemistry in pro-
tein molecules greatly facilitates their 3D atomic
structure determination, but this knowledge is not
applicable to physical science samples. Third, un-
like in biological specimens, the presence of dif-
fraction and phase contrast in the transmission
electron microscopy images of most materials
poses a challenge for tomographic reconstruc-
tion. These difficulties have made the objective
of solving the 3D atomic structure of crystal de-
fects and noncrystalline systems a major chal-
ON OUR WEBSITE atom-tracing algorithms
have placed one method—
Read the full article
at http://dx.doi. atomic electron tomogra-
org/10.1126/ phy (AET)—on the cusp of
science.aaf2157 this breakthrough. In recent
..................................................
years, AET has been used
to image the 3D structure of grain boundaries
and stacking faults and the 3D core structure
of edge and screw dislocations at atomic reso-
lution. This technique has also revealed the
existence of atomic steps at 3D twin boundaries
Downloaded from http://science.sciencemag.org/ on January 18, 2017
that are hidden in conventional 2D projections.
Furthermore, the combination of AET and atom-
tracing algorithms has enabled the determination
of the coordinates of individual atoms and point
defects in materials with a 3D precision of ~19 pm,
allowing direct measurements of 3D atomic dis-
placements and the full strain tensor. Finally, the
single-particle reconstruction method developed
in cryo-EM has been applied for 3D structure de-
termination of small (≤2-nm) gold nanoparticles
and heterogeneous platinum nanocrystals at
atomic-scale resolution.
OUTLOOK: The future research frontiers of
AET involve increasing the sample complexity
(including real materials with different atomic
species and disordered systems), image contrast
(determining the 3D atomic positions of both
heavy and light elements), detection sensitivity
(revealing individual atoms at surfaces and in-
terfaces), and data acquisition speed (probing
the dynamics of individual atoms and defects).
The ability to precisely determine all atomic
coordinates and species in real materials with-
out assuming crystallinity will transform our
understanding of structure-property relation-
ships at the most fundamental level. For instance,
using atomic coordinates as inputs to first-
principles calculations, it is possible to compute
the effect on the material properties of each de-
fect and atomic reorganization, giving precious
clues about how to modify and engineer ma-
terials at the atomic level to yield better per-
formance in a device. Catalysis involves atoms
interacting on nanoparticle surfaces in poorly
FePt Grain Structure in 3D

Fe
Traced atomic positions of FePt nanoparticle.
Pt
FePt Grain Structure in 3D

Fe
Traced atomic positions of FePt nanoparticle.
Pt
FePt Grain Structure in 3D

Fe
Traced atomic positions of FePt nanoparticle.
Pt
Grains separated by phase.
FePt Grain Structure in 3D

Fe
Traced atomic positions of FePt nanoparticle.
Pt
Grains separated by phase.

Slices showing interior of grains.

Characterization methods
How do we learn about the structure and bonding of our
material?

• Diffraction: positions and intensities of scattered radiation

• Spectroscopy: energy dispersion of scattered radiation
• Microscopy: image reconstruction

Radiation Sample Radiation

In Out
Diffraction Diffraction: the phenomena of waves
encountering apertures or obstacles,
particularly concerning constructive and
destructive interference.
• Radiation scattered by the sample is collected
and analyzed with respect to its geometry of
scattering
• X-rays (and other photons)
• Neutrons
Double slit experiment, • Electrons
Wikipedia
• Quantitative evaluation of diffraction experiments
is performed in a diffractometer

• Many different types of diffraction (e.g., Laue,

Hall/Debeye-Scherrer, SANS, GIXS, etc.)- same
physics, different radiation source and collection
methods
All diffraction phenomena obey the
Diffraction pattern of SrTiO3
same laws
Spectroscopy
Separation of white light by a
prism – Welcome to the
Machine
X-ray photoelectron
spectroscopy of oxidized InAs
• Study of interaction between matter and radiated
energy
• Radiation scattered by the sample is collected
and analyzed with respect to its energy
(wavelength)
• X-rays (and other photons)
• Neutrons
• Electrons
• Quantitative evaluation of spectroscopy
experiments is performed in a spectrometer
• Many different types of spectroscopy (e.g., EDS,
XPS, WDS, XAS, etc.)- same physics, different
radiation source and collection methods
All spectroscopy phenomena obey the
same laws
 Microscopy
• The field of using microscopes to view samples
and objects that cannot be seen with the naked
eye (includes optical, electron, and scanning probe
microscopy)
• Radiation scattered by the sample is collected and
recombined through lens system to produce an
image
Optical microscope
• X-rays (and other photons)
• Electrons
• Quantitative evaluation of microscopy experiments
is performed in a microscope
• Many different types of microscopy (e.g., light, X-
ray, electron, etc.) -same physics, different
radiation source and collection methods
Highest resolution atomic All “true” microscopy techniques
microscope in the world obey the same laws of optics
21 (0.33 A)
So far…
Reading: Syllabus, Laboratory Guide, Laboratory 1,
Operating Procedures for MiniFlex, Chapter 1

Homework:
• Complete your EH&S X-ray Safety Training before you go to
Lab 1
• Homework 1 (Due Feb. 3, online by 12:10PM) will be posted
next week.

Important announcements:
Read the course documents!
Chapter 1: Properties of
X-rays

How are X-rays produced and what can we do with them?