Nanoscale Materials Characterization Facility
Nanoscale Materials Characterization Facility
Operational Summary
The Nanoscale Materials Characterization Facility (NMCF) is a state-of-the-art user
facility located with the Materials Science and Engineering Dept (MSE). The facility is
dedicated to materials characterization, available for use by all qualified faculty,
students and researchers at UVa, as well as by researchers from other universities
and industries.
Scheduling is handled on a first-come first-serve basis by our web-based sign-up
system. Technicians, students and faculty are available to assist researchers using
the instruments, and courses in electron microscopy and materials characterization
are offered each year.
Capabilities Include:
Atomic imaging of materials
Elemental analysis
Elemental mapping and energy-filtered imaging
Dynamic experiments utilizing heating, cooling and straining holders
Orientation mapping of materials
Microstructural characterization
Computer acquisition and processing of images and spectra
Nanoscale Materials Characterization Facility
NMCF Staff
Michal Sabat:
X-Ray Diffraction Specialist, Senior Staff Scientist
University Of Virginia
Depts. Chemistry and Materials Science & Engineering
Phone: 434-924-7862
Email: ms5c@virginia.edu
Richard R. White:
Facility Manager, Staff Scientist
University Of Virginia
Department of Materials Science & Engineering
Phone: 434-982-5657
Email: rrw3q@virginia.edu
Nanoscale Materials Characterization Facility
Education
Prof. Jiwei Lu and Ph.D. Candidate Matthew Steiner
discussing X-ray diffraction during an undergraduate
lab experience. Currently, NMCF staff and
instrumentation are utilized in (6) classes taught at
both the undergraduate and graduate levels.
Nanoscale Materials Characterization Facility
Analytical Technique Summary
Technique
Application
Signal
Detected
Element
Detected
Organic
Detection
Limits
Depth
Resolution
Imaging /
Mapping
Lateral
Resolution
SEM
High
Magnification,
Topography
Secondary and
Backscattered
Electrons
--------------
--------------
--------------
Dependent on KV and
Imaging Mode
(20 Ǻ to a few μm )
Yes
10 to 500 Ǻ for S.E.
S-TEM
Microstructural /
Crystallographic
Information
Transmitted and
Diffracted
Electron
--------------
--------------
--------------
<2000 Ǻ
Yes
3.5 - 10 Ǻ
FIB
Micromachining,
Deposition: SiO2
or Pt
Secondary
Electrons,
Secondary Ions
--------------
--------------
--------------
--------------
Yes
10 nm w/ 1pA beam
current
S-AES
Surface Analysis
Auger Electrons
Li – U
--------------
0.1 – 1 at %
5 -50 Ǻ
Yes
5000 Ǻ
XRD, SAXS,
WAXS
ID of Crystalline
Phases
Scattered X-rays
Not Element
Specific
Yes
Typically 1-3%
10 µm - 60 µm
No
Typically 10 - 12 mm
EDS
Elemental
Analysis
X-rays
C-U
(2010F: B-U)
Yes
0.1 - 3.0 wt% for
Material and Voltage
Dependent
(50 nm - 5 µm)
Yes
Technique
Dependent
Optical
3-D Optical
Imaging
Photons
---------------
Yes
Optical
Yes
400 nm
CL
Light Emitting
Materials
Photons
200 to 800 nm
--------------
--------------
50 nm - 5 µm
Yes
Sample Dependent >
30 nm
CL: Cathodoluminescence on 6700F SEM
FIB: Focused Ion Beam
TDS: Temperature Desorption.
AES: Scanning Auger electron Spectroscopy (August 2010)
XRD: X-ray diffraction (single crystals, powders, texture)
0.1 wt%
EDS: Energy dispersive spectroscopy
SEM: Scanning electron microscopy
Optical: Conventional and 3-D imaging systems
TEM: Transmission electron microscopy (STEM August 2010)
SAXS/WAXS: Small/Wide angle X-ray scattering
Nanoscale Materials Characterization Facility
Technique Application Areas
AES: Scanning Auger Electron Spectroscopy: Surface analysis and depth profiling, semi-conducting or
conducting samples.
CL: Cathodoluminescence: Luminescent materials, mapping of defects and measurement of their densities,
impurity segregation studies; Electronic band structure (band gap); Measurement of the dopant concentration
and of the minority carrier diffusion length and lifetime
EBL: Electron Beam Lithography: Patterning of polymeric substrates and polymer thin films
E-Beam Lithography (EBL): http://www.jcnabity.com/
EBSD: Electron Backscatter Diffraction: Phase identification, orientation, mapping.
EDS: Energy Dispersive Spectroscopy: Elemental analysis
OM: Optical Light Microscopy: Morphology; Size; Transparency; Color (reflected and transmitted), Refractive
Indices, Dispersion of Refractive Indices, Pleochroism, Crystal System, Birefringence, Extinction Angle,
Fluorescence (UV, V, IR), Melting Point, Polymorphism, Eutectics.
SEM: Scanning Electron Microscopy: Topography; Morphology; Composition; Crystallographic Information.
STEM / TEM: Scanning / Transmission Electron Microscopy: Microstructural and crystallographic
information; Composition.
XRD: X-ray Scattering and Diffraction: Measure the average spacings between layers or rows of atoms;
Determine the orientation of a single crystal or grain; Find the crystal structure of an unknown material; Measure
the size, shape and internal stress of small crystalline regions. Determine the properties of chain packing in
natural and synthetic polymers.
Nanoscale Materials Characterization Facility
Instrument Training
Instrument
FEI FIB
FEI Titan
JEOL 2000FX
JEOL 6700F
JEOL 840
General Optical
Hirox KH 7700
Scintag X1 XRD
Scintag XDS XRD
Rigaku 3000 SAXS
Bruker Apex II XRD
Room #
MSE 112
WDH B13
MSE 108
MSE 116
MSE 115
MSE 117
MSE 117
MSE 102
MSE 102
MSE 114
MSE 100
Capabilities
Sectioning / SEM
STEM / EDS / EELS
TEM / EDS
SEM / EDS / CL
SEM / EDS / EBSD
General Metallurgy, Stereo
Optical: 3-D, Movie, 360 rotation
Powder XRD / Texture
Powder XRD / General Use
Small-Angle X-Ray Scattering
Crystal Structure Determination
Training Time1,2
8-10 Sessions (@2 hrs each)
4-6 Sessions (pre req. JEOL 2000FX)
8-10 Sessions (@ 3 hrs each)
8-10 Sessions (@ 2hrs each, not EDS and CL)
4 Sessions (@ 2hrs each, not EDS and EBSD)
1 Session (@ 2 hours)
2 sessions (@ 2 hrs each)
1 Session (2 hours)
1 Session (2 hours)
5 Sessions (@ 1hour each)
Operated by Michal Sabat
Notes:
Users need to be trained and "checked out" before they can utilize the machines solo during day and evening hours.
This listing will be made available to users, as those proficient can train each other as well. However, all new users will
have to go through a final check out with a staff member, regardless of who trained them.
Please consider as many potential aspects of your research as possible when meeting with the staff, the staff is
available to sit down with all involved to give input.
Use is monitored - you will be required to show sufficient use on the instruments otherwise a refresher with a staff
member to maintain your training level and evening hours use. This is performed to maintain the high quality of
research data that both faculty and users are expecting and requiring from these instruments.
Nanoscale Materials Characterization Facility
HIROX KH 7700 Digital Microscope
Magnification Range: 0-7000x (optical)
Auto Calibration
2D & 3D Measurement Analysis
2D & 3D Image Tiling
Dynamic Image Focus for Rough Surfaces
Still Image and Video Recording
3D Rotation during Live Imaging
Large Depth of Field
Integrated Illumination System
Nanoscale Materials Characterization Facility
Perkin Elmer PHI 600 Scanning Auger Electron Microprobe
(a)
(b)
(a) An AES depth
profile of a sputter
deposited thin film
structure consisting of
a Au film on Si. The Cr
layer was intended to
be a diffusion barrier to
prevent the Au and Si
from inter-diffusing. (b)
AES depth profile of
the previous thin film
structure after heat
treatment ( 2 hrs at 300
ºC). The TFA shows
that the barrier has
failed.
• Elemental Analysis of Thin Films
• Depth Profiling
• Conducting Samples
• Light Element Detection
• Secondary Electron Imaging
Nanoscale Materials Characterization Facility
FEI FIB 200 Focused Ion Beam
The focused ion beam (FIB) employs rastering of a Ga+ ion beam, imaging is accomplished with
either secondary electrons or secondary ions. For milling, the high energy (30 keV) Ga+ ions are
focused into spots as small as 10 nm to form pixel-by-pixel images.
Specifications:
Pt, SiO2 deposition sources (organic platinum, Si) Secondary Ion Mass Spectrometer
Secondary Electron / Ion Imaging Cooling / Heating (77 to 700 K)
Minimum spot size ~ 10 nm
Ion current density > 10 A/cm2
Ion currents 1 pA to 10 nA
Ion energies 3 keV to 30 keV
Charge Neutralization
Depth of focus ~ 200 m
Bob Benoit operating the FIB.
Pt deposited pillars onto polystyrene micro-spheres using the FIB200 ion beam induced deposition (IBID) system.
Nanoscale Materials Characterization Facility
JEOL JSM 840 Scanning Electron Microscope
A second SEM, a JEOL JSM-840A, is equipped with a LaB6 filament and a PGT EDXS system for highresolution imaging (4 nm) and microanalysis of elements down to Be. This instrument has SEI and BEI,
as well as HKL Technology electron backscattered pattern (EBSP) hardware and software for
orientation imaging and mapping of specimens. It also has a NPGS electron-beam lithography system.
The microscope has extensive automation, image storage and processing capabilities.
Alex Traviss operating the JSM 840.
Nanoscale Materials Characterization Facility
JEOL 6700F Scanning Electron Microscope
The facility recently acquired a completely digital JEOL JSM-6700F cold field-emission gun SEM. This
microscope operates at accelerating voltages ranging from 0.5 to 30 kV in 0.1 kV steps and has a
guaranteed resolution of 1.0 nm at 15 kV and 2.2 nm at 1.0 kV. It has secondary electron imaging (SEI)
capability utilizing both through-the-lens and in-chamber secondary electron detectors and
backscattered electron imaging (BSE). The microscope is equipped with a scanning
cathodoluminescence system and a PGT IMIX-SPIRIT energy-dispersive X-ray spectroscopy (EDXS)
detector with an ultra-thin window for light element detection down to boron.
Carbon “Nano Horns”
Nanoscale Materials Characterization Facility
JEOL 2000FX Transmission Electron Microscope
Conventional TEM studies are performed on a JEOL 2000FXII 200kV TEM equipped with a LaB 6
filament, high-angle Gresham EDXS detector, Gatan slow-scan and wide-angle TV-rate cameras and a
variety of specimen holders, including heating, cooling and straining stages with tilting capability. This
instrument has a high-tilt pole-piece with a point resolution of 0.3 nm and ± 60° double-tilt capability
using the Gatan low-background double-tilt holder.
Dr. Chi-Chin Wu operating the JEOL
2000FX.
Nanoscale Materials Characterization Facility
FEI Titan Scanning Transmission Electron Microscope
• 80 - 300kV S-TWIN platform
• STEM system for FEG configuration, 300 kV kit, (Resolution:
STEM: 0.135 nm; TEM: 0.205 nm).
• r-TEM retractable detector unit for Titan S-TWIN (0.13 Sr
collection angle)
• Low-Dose Exposure Technique
• Low-Background, Double-Tilt Specimen Holder
• Cold Stage, Double-Tilt Specimen Holder
• Titan Smart Tilt
• Gatan 794 Mult-scan Camera (EFTEM)
• EFTEM, EELS
• EDAX Spectroscopy
• Gatan Model 863P Tridiem GIF
• HAADF Detector
• Titan Compucentricity
• Titan Free Lens Control
Nanoscale Materials Characterization Facility
X-Ray Powder Diffractometers
The Scintag X1 Texture
The Scintag XRD 2000 Powder
The
Scintag
XRD
2000
automated
X-ray
powder
diffractometer consists of a 3.5
kW x-ray generator, a biplane
vertical/horizontal theta/theta
goniometer, and a Peltier
cooled Si(Li) detector. Besides
controlling data collection in a
variety of modes, computer
software capabilites include:
data
reduction
and
manipulation, JCPDS searchmatch system, quantitative
analysis, particle size and
residual stress analysis. High
and
low
temperature
attachments provide a wide
range
of
measurement
temperatures. The Scintag X1
instrument is a fully computer
–controlled texture goniometer
and diffraction system.
Nanoscale Materials Characterization Facility
Small-Angle X-Ray Scattering (SAXS)
In comparison with X-ray diffraction techniques, small-angle X-ray scattering (SAXS)
offers only modest resolution (1-3 nm) which is not sufficient to reveal the atomic
structure of materials, However, SAXS measurements are superior when applied to
establish the size, shape and degree of aggregation of nanoparticles and large
molecules such as polymers. SAXS has been applied to a variety of materials,
including metal alloys, synthetic polymers in solution and in bulk, proteins in solution,
emulsions, porous materials, gels, nanoparticles and several other systems.
Nanoscale Materials Characterization Facility
Rigaku S-MAX 3000 SAXS Instrument
The Rigaku S-MAX 3000 SAXS system is
equipped with a MicroMAX-007 rotating
anode generator, a three-pinhole camera
system and a two-dimensional multi-wire Xray area detector. A three-meter, fully
evacuated camera provides both high
intensity and high resolution. Coupled with a
fully integrated two-dimensional multi-wire
proportional counter, the system is capable
of making highly sensitive measurements
from both isotropic and anisotropic
materials.
Features
Three pinhole collimation
Two sample chambers for long and mid-range SAXS
Simultaneous wide angle X-ray scattering (WAXS) capability
Complete vacuum environment
Sample temperature control available
SAXS analysis software
Nanoscale Materials Characterization Facility
SAXS Measurements for Polymers
Small-angle X-ray scattering measurements
can provide the following information:
Lamellar repeat distance: the distance from
the center of one bilayer to the center of its
neighbor, which includes the thickness of
associated water layers.
Radius of gyration: the first moment of
the scattering center distribution function.
Particle size and shape: from Guinier's
and Porod's Laws.
Large-scale structure and long-range
order: distances between
similar structures.
This technique has been used extensively in
polymer industries to characterize the
morphological effects of drawing, rolling, and
annealing on mechanical properties.
Nanoscale Materials Characterization Facility
Single-Crystal CCD Diffractometer
The Bruker APEX II single-crystal diffractometer is one of the best tools for accurate
crystal structure determination. The most important parts of the Bruker instrument:
•X-ray generator 1
•X-ray source-ceramic Mo tube 2
•APEX II CCD detector 3
•PC computer for data collection control and structure determination 4
•Oxford Cryosystems 700 low temperature device 5
4
1
5
3
5
2
Nanoscale Materials Characterization Facility
Single-Crystal CCD Diffractometer
Typical single-crystal data collection and structure
determination include the following steps:
Selection of a single crystal
Determination of the unit cell and crystal symmetry
Data collection usually performed at -120oC on
a Bruker APEX II CCD diffractometer
Data reduction
Structure solution by heavy atom techniques or
direct methods of the SHELXTL program suite
Least-squares refinement of the structural
parameters
Interpretation of the results.
Crystal structure of a rhodium complex used in
homogenous catalysis experiments by the Gunnoe
group (Department of Chemistry). Atomic thermal
vibrations are represented by 30% probability
ellipsoids.
Nanoscale Materials Characterization Facility
Bruker APEX II Single-Crystal CCD Diffractometer
Joanna Webb (a PhD student in the Gunnoe group of the Chemistry Department ) is working
on the Bruker APEX II CCD single-crystal diffractometer.
Nanoscale Materials Characterization Facility
Sample Preparation Instruments
GATAN Etching and Coating System
Southbay Plasma Cleaner
Other Services include: General and metallurgical sample preparation, chemical etching,
electro-polishing, compound and stereo optical microscopes, and hardness measurements.
Nanoscale Materials Characterization Facility
Sample Preparation Instruments
Cut-Off Saws
Machine Polishing
Mounting
Hand Polishing
Chemical Etching
Nanoscale Materials Characterization Facility
Current Fee Schedule
Customer
University of Virginia
(5pm - 8am, and weekends)
Electron Microscopes
Machine Time
$40/hr
$28/hr
External Universities
Industrial Affiliates
NA
NA
With Staff Scientist
$90/hr
NA
$110/hr
$300/hr
XRD
Customer
University of Virginia
External Universities
Industrial Affiliates
Machine Time
$15/hr
$25/hr
$130/hr
With Staff Scientist
$65/hr
$90/hr
$230/hr
Sample Preparation Instruments
Customer
University of Virginia
External Universities
Industrial Affiliates
PECS
$5/use
$10/use
$20/use
Plasma-Cleaner
$5/use
$10/use
$20/use
Hummer
$5/use
$10/use
$20/use
Ion Mill
$15/hr
$20/hr
$60/hr