Title: MAIC newsletter
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Permanent Link: http://ufdc.ufl.edu/UF00091100/00004
 Material Information
Title: MAIC newsletter
Series Title: MAIC newsletter
Physical Description: Serial
Language: English
Creator: Major Analytical Instrumentation Center, College of Engineering, University of Florida
Publisher: Major Analytical Instrumentation Center, College of Engineering, University of Florida
Place of Publication: Gainesville, Fla.
Publication Date: January 2003
 Record Information
Bibliographic ID: UF00091100
Volume ID: VID00004
Source Institution: University of Florida
Holding Location: University of Florida
Rights Management: All rights reserved by the source institution and holding location.

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Grazing Incidence X-ray
By V Craciun

The X'Pert MRD system in MAIC can
be used to perform grazing incidence x-
ray diffraction (GIXD) studies of thin
films grown on various substrates. The
advantages of this technique are: (i)
higher sensitivity due to a larger
interaction volume (ii) absence of strong
diffraction lines from the substrate
material and (iii) depth profiling of
various crystalline phases present.
The first step in GIXD measurements is
the determination of the critical angle
(0c) of the film (see the previous MAIC
newsletter for the definition and
measurement of the critical angle; for
typical materials 0o is approximately
from 0.1 to 1, hence the name of the
technique, grazing incidence). If the
radiation incidence angle Q is smaller
than the critical angle then the x-rays
penetrate into the material as an
evanescent wave with a typical
penetration of around 1-2 nm.
counts/s

ooo-00. XRD


Diffraction (GIXD)


For incidence angles greater than 09, x-
ray radiation penetrates deeper into the
layer allowing for sampling at
increasing depths with increasing angle.
However, since the penetration depth
initially increases exponentially with the
increase of the incidence angle, the
depth profiling is not very accurate.
An example of the usefulness of the
GIXD technique is presented below.
Because the thickness of the deposited
film was rather small, the XRD
measurement in the usual Bragg-
Bretano geometry (0-20) didn't reveal
the crystalline structure of the film and
was dominated by the substrate peak.
On the other hand, the GIXD
measurement performed at an incidence
angle of 1 revealed much more
information about the crystalline
structure and lattice parameters of the
deposited film by reducing the signal
from the substrate.


X-ray diffraction patterns of a -25 nm thick LixMn2-xO4 film grown by the pulsed laser deposition
technique on a (100) Si substrate; upper trace: 0-20 geometry; lower trace: grazing angle incidence
(incidence angle Q10). The 0-20 spectrum was vertically shifted for clarity.




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Newsletter

Major Analytical Instrumentation Center
107 MEL, PO Box 116400, Gainesville, FL 32611
Phone:(352) 392-6985 Fax:(352) 392-0390









Kerry Siebein, M.S.
Electron Microscopy
Analysis

Kerry Siebein has joined the staff of the
MAIC to work in the areas of
Transmission Electron Microscopy
(TEM) and Scanning Electron
Microscopy (SEM). She earned her
Master of Science in Materials
Engineering at the Worcester
Polytechnic Institute in Worcester, MA.
She has held several positions as a
Materials Research Engineer before
joining the Particle Engineering
Research Center (PERC) at UF. Thus
she has significant experience working
with steels and experimental armor
materials, characterization of ceramic
materials for wear applications,
coatings, thin films and polymer blends
using TEM and SEM. Kerry is currently
dividing her hours between the PERC
and the MAIC performing materials
characterization using SEM and TEM.
At the MAIC, Kerry is in charge of
training students in the operation of the
FEG-SEM and services provided using
this instrument. She is also in charge of
the new Ultracryo-microtome and is
coordinating training and services using
this instrument.


Surface Analysis in the
21st Century
By Eric Lambers


Surface analysis at MAIC has entered a
new era in user friendliness with the
addition of RBD Enterprises PC
Upgrades for the PHI 660 Auger
Electron Spectrometer (AES) and the
PHI 5100 X-ray Photoelectron
Spectrometer (XPS/ESCA). While
preserving the functionality of the
previous software the biggest advantage
of the new implementation is the ease at
which the data can now be incorporated
into other Windows@ based programs
and documents. Using the "copy" and
"paste" commands the graphical data
can be added to manuscripts written
with Windows based word processing
programs (Figures 1&2) or
presentations put together for the
classroom or conferences using
programs such as Power Point. The
data can also be easily exported in an
ASCII format and then entered in a
spreadsheet program for further analysis
in any manner the user wishes. A free
copy of the RBD software can be
downloaded from their website at:
www.rbdenter.com and with this demo


version one can also change the
appearance of the graphed data.
Characteristics such as line types or
widths as well type faces on axis labels
can be adjusted to your personal
preferences. The PC 147 control unit is
also part of the upgrade and enables the
new software to control the instrument
with state of the art electronics which in
the case of the AES system replaced
five printed circuit boards with a single
board thereby discarding electronic
control architecture which was now
more than 15 years out of date.
Originally developed for older
generations of PHI equipment the
software is constantly being updated as
other equipment and new techniques are
being added to the programs
capabilities. We are currently involved
in "beta" testing of the software for our
instruments as well as working with
RBD and Microfabritech on the
addition of PHI 6600 SIMS capabilities
to the program. An additional feature of
this software is the ability of the
engineers at the company offices in
Bend, Oregon to monitor and control
our instruments over the Internet using a
program similar to Net Meeting. This
means maintenance and trouble
shooting is much faster and cheaper
saving both time and money.


Figure 1
Auger Depth Profile of 1000A
layers of Ag and Ta on a Si
substrate annealed at 600C
for 30 minutes showing O at
the Ag/Ta interface.



Sil


160 200 240 280
es


40 80 120
Cycl


Seminars: Using Size Exclusion/Gel Permeation Chromatography and Tetra Detection for the
Characterization of Proteins and Natural and Synthetic Polymers
Please join Dr. Max Haney of Viscotek for a discussion of the use of SEC/GPC and tetra detection for the characterization of proteins and
polymers. The seminar will cover the characterization of macromolecules using Low Angle Light Scattering, GPC-Viscometry, Refractive
Index, and UV-absorbance. This multi-detector approach provides comprehensive information on absolute molecular weight distributions,
molecular size, aggregation, branching, and copolymer composition.
The seminar will be held at 11 AM, February 19, 2003, in the J. Wayne Reitz Union Room 282 at the University of Florida.
Refreshments will be provided. Please call 352-392-6985 to register.


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Figure 2
XPS survey
spectra of an "as
received"
stainless steel
sample.


Binding Energy (eV)


Min: 0 M- :310786




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