n anoscale m aterials c haracterization f acility

Nanoscale Materials Characterization Facility

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 materialsElemental analysisElemental mapping and energy-filtered imaging Dynamic experiments utilizing heating, cooling and straining holders Orientation mapping of materials Microstructural characterizationComputer acquisition and processing of images and spectra

Operational Summary

Michal Sabat: X-Ray Diffraction Specialist, Senior Staff Scientist University Of Virginia

Depts. Chemistry and Materials Science & EngineeringPhone: 434-924-7862Email: [email protected]

Richard R. White: Facility Manager, Staff Scientist University Of Virginia Department of Materials Science & Engineering Phone: 434-982-5657 Email: [email protected]


NMCF Staff

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.


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

-------------- -------------- 0.1 wt% 50 nm - 5 µm Yes Sample Dependent > 30 nm

CL: Cathodoluminescence on 6700F SEM EDS: Energy dispersive spectroscopy FIB: Focused Ion Beam SEM: Scanning electron microscopy TDS: Temperature Desorption. Optical: Conventional and 3-D imaging systems AES: Scanning Auger electron Spectroscopy (August 2010) TEM: Transmission electron microscopy (STEM August 2010)XRD: X-ray diffraction (single crystals, powders, texture) SAXS/WAXS: Small/Wide angle X-ray scattering


Technique Application AreasAES: 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 filmsE-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.


Instrument Training

Instrument Room # Capabilities Training Time1,2FEI FIB MSE 112 Sectioning / SEM 8-10 Sessions (@2 hrs each)FEI Titan WDH B13 STEM / EDS / EELS 4-6 Sessions (pre req. JEOL 2000FX)JEOL 2000FX MSE 108 TEM / EDS 8-10 Sessions (@ 3 hrs each)JEOL 6700F MSE 116 SEM / EDS / CL 8-10 Sessions (@ 2hrs each, not EDS and CL)JEOL 840 MSE 115 SEM / EDS / EBSD 4 Sessions (@ 2hrs each, not EDS and EBSD)General Optical MSE 117 General Metallurgy, Stereo 1 Session (@ 2 hours)Hirox KH 7700 MSE 117 Optical: 3-D, Movie, 360 rotation 2 sessions (@ 2 hrs each)Scintag X1 XRD MSE 102 Powder XRD / Texture 1 Session (2 hours)Scintag XDS XRD MSE 102 Powder XRD / General Use 1 Session (2 hours)Rigaku 3000 SAXS MSE 114 Small-Angle X-Ray Scattering 5 Sessions (@ 1hour each)Bruker Apex II XRD MSE 100 Crystal Structure Determination 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.


HIROX KH 7700 Digital Microscope

Magnification Range: 0-7000x (optical)Auto Calibration2D & 3D Measurement Analysis2D & 3D Image TilingDynamic Image Focus for Rough SurfacesStill Image and Video Recording3D Rotation during Live ImagingLarge Depth of FieldIntegrated Illumination System


Perkin Elmer PHI 600 Scanning Auger Electron Microprobe

• Elemental Analysis of Thin Films• Depth Profiling• Conducting Samples• Light Element Detection• Secondary Electron Imaging

(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.

(a)

(b)


FEI FIB 200 Focused Ion Beam

Bob Benoit operating the FIB.

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 SpectrometerSecondary Electron / Ion Imaging Cooling / Heating (77 to 700 K)Minimum spot size ~ 10 nmIon current density > 10 A/cm2

Ion currents 1 pA to 10 nAIon energies 3 keV to 30 keVCharge NeutralizationDepth of focus ~ 200 m

Pt deposited pillars onto polystyrene micro-spheres using the FIB-200 ion beam induced deposition (IBID) system.


A second SEM, a JEOL JSM-840A, is equipped with a LaB6 filament and a PGT EDXS system for high-resolution 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.

JEOL JSM 840 Scanning Electron Microscope

Alex Traviss operating the JSM 840.


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.

JEOL 6700F Scanning Electron Microscope


Carbon “Nano Horns”

JEOL 2000FX Transmission Electron Microscope

Conventional TEM studies are performed on a JEOL 2000FXII 200kV TEM equipped with a LaB6

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.


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


X-Ray Powder Diffractometers

The Scintag XRD 2000 Powder

The Scintag X1 Texture


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 search-match 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.

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.

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.


Small-Angle X-Ray Scattering (SAXS)

Rigaku S-MAX 3000 SAXS Instrument

FeaturesThree 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

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 X-ray 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.


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.


SAXS Measurements for Polymers

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

•X-ray source-ceramic Mo tube

•APEX II CCD detector

•PC computer for data collection control and structure determination

•Oxford Cryosystems 700 low temperature device

Single-Crystal CCD Diffractometer

3 25

1

4

5

1

2

34

5


Typical single-crystal data collection and structure determination include the following steps:Selection of a single crystalDetermination of the unit cell and crystal symmetryData collection usually performed at -120oC on a Bruker APEX II CCD diffractometerData reductionStructure solution by heavy atom techniques or direct methods of the SHELXTL program suiteLeast-squares refinement of the structural parametersInterpretation 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.


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.


Bruker APEX II Single-Crystal CCD Diffractometer

GATAN Etching and Coating System

Sample Preparation Instruments

Southbay Plasma Cleaner

Other Services include: General and metallurgical sample preparation, chemical etching, electro-polishing, compound and stereo optical microscopes, and hardness measurements.


Cut-Off Saws Mounting Hand Polishing

Machine Polishing Chemical Etching

Sample Preparation Instruments


Electron MicroscopesCustomer Machine Time With Staff ScientistUniversity of Virginia $40/hr $90/hr (5pm - 8am, and weekends) $28/hr NA

External Universities NA $110/hrIndustrial Affiliates NA $300/hr

XRDCustomer Machine Time With Staff ScientistUniversity of Virginia $15/hr $65/hrExternal Universities $25/hr $90/hrIndustrial Affiliates $130/hr $230/hr

Sample Preparation InstrumentsCustomer PECS Plasma-Cleaner Hummer Ion Mill University of Virginia $5/use $5/use $5/use $15/hrExternal Universities $10/use $10/use $10/use $20/hrIndustrial Affiliates $20/use $20/use $20/use $60/hr

Current Fee Schedule


n anoscale m aterials c haracterization f acility

Documents

luminescent materials

electron beam lithography

diffracted electron

xray diffraction specialist

imaging mode20

facility manager

smallwide angle xray

mapping of defects