CINT Capabilities: Characterization

A state-of-the-art image-corrected monochromated Titan Environmental Transmission Electron microscope (ETEM), 300 kV, provides the capability to resolve reactions between materials and gaseous environments during atomic-resolution (1 Å) imaging. CINT has developed their own gas delivery system to expose the sample within the objective lens of the TEM to gases of H₂, O₂, CO, CO₂, CH₄, N₂, Ar, He, air, or H₂O up to 100 mbar of pressure during TEM imaging. This equipment provides dynamic information on catalytic and nanomaterials under reaction conditions. Lorentz microscopy and piezo stage control are additional features of this tool. Imaging may be performed in TEM or Scanning TEM modes, with collection from a Ceta camera or bright-field and dark-field STEM detectors. The ETEM is compatible with our current variety of in-situ TEM holder for cryo-EM, high-temperature, mechanical straining, and electrical biasing (see TEM laboratory capability). The ETEM has also been equipped with the Gatan K2-IS camera for either high-speed imaging, up to 1,600 frames per second or low dose imaging, down to single electron sensitivity with direct electron counting. There are no analytical capabilities currently available on the ETEM.

Contact:
Katie Jungjohann

The TEM lab at CINT is equipped with a FEI Tecnai G(2) F30 S-Twin 300kV transmission electron microscope. The field emission gun offers a highly coherent electron beam with 0.2 nm point resolution in TEM and 0.19 nm in high angle annular dark field (HAADF) Scanning TEM. The accelerating voltage of the electron beam can also operate at 200 kV and 100 kV with resolutions of 0.25 and 0.32 nm, respectively. The microscope is equipped with an EDAX ECON x-ray detector, Gatan GIF Tridiem electron energy loss spectrometer, Gatan Ultrascan 1000 CCD camera, Gatan bright field, Gatan annular dark field, and Fischione Instruments HAADF STEM detectors. A variety of sample characterization and in situ studies may be conducted using FEI single tilt, low background single tilt, and double tilt holders; Nanofactory STM, AFM, NanoIndentation, 16 lead, and STM-X6 holders; Gatan 2.3 mm single tilt holder with a Faraday cup, and double tilt cyro holders; Protochips Aduro double tilt heating with biasing holder; and the Hummingbird Scientific liquid flow with biasing holder. The instrument functions for a range of experimental techniques for elemental analysis, energy-filtered imaging, and the structural characterization of nanomaterials with or without an external stimulus. Sample preparation of electron transparent samples for TEM analysis can be fabricated using a Leica EM UC7 ultramicrotome, tripod polisher, or mechanical thinning and ion milling.

Contact:
Katie Jungjohann

The cryogenic electron microscopy (cryo-EM) lab houses instruments for the imaging of soft matter, nanomaterials, and beam sensitive materials in their native, hydrated state. Included is a Talos L120C dedicated cryogenic transmission electron microscope (cryo-TEM) from Thermo Fisher Scientific. The TEM has user-switchable accelerating voltages from 20-120 keV and is equipped with a high speed camera (40 fps at 4k x 4k) optimized for imaging at low keV. It has a point resolution of 0.37 nm and is capable of electron diffraction and scanning transmission electron microscopy (STEM). The Talos L120C has a modified pole piece with a larger gap which allows for a wider angle of rotation for tomography experiments. It also accepts the insertion of a cryogenically cooled ‘cryo-box’, giving greater stability when imaging cryogenically frozen samples. Hydrated samples are frozen controllably and reproducibly using a Vitrobot rapid vitrification machine ion milling.

Also present in the lab is a Thermo Fisher Scientific Scios 2 Dual Beam scanning electron microscope with focused ion beam milling capability (SEM/FIB) optimized for the imaging and sectioning of soft matter. A specialized in-column T3 detector is included, which is optimized for low-kV, low energy secondary electron detection. It is equipped with a dedicated cryo-cooled SEM stage from Leica Microsystems providing the capability to section and image frozen samples, yielding information on internal microstructure. The Leica cryo-workflow is specially designed to allow sample preparation and transfer while maintaining a frozen state and includes a shuttle (VCT-500), sample transfer workstation (VCM) and sputter coater/freeze fracture unit (ACE-600). Cryogenic lift-out can therefore be performed on milled samples and transferred to the Talos L120C, thereby covering a wide range of length scales in the characterization of frozen, hydrated samples.

Contact:
John Watt

The I³TEM facility combines an 200 kV JEOL 2100 high-contrast TEM (2.5 Å point resolution) with an 10 kV Colutron and an 6 MV Tandem accelerator. The I³TEM facility can permit a wide breath of combined experiments in high temperature, flowing liquid, gas exposure, mechanical loading, displacement damage, gas implantation, and numerous sequential or simultaneous combinations thereof to evaluate the structural evolution that occurs during ion beam modification or overlapping combinations of extreme environments.

Specific capabilities of the I³TEM include:

1. Single electron sensitive 4k x4k camera
2. Video rate 1k x1k camera
3. Microfluidic mixing using a Protochips two channel fluid stage
4. High temperature and gas flow experiments using a custom Protochips stage
5. High temperature experiments using an 2.3 mm Hummingbird heating stage
6. Classical TEM straining experiments using a Gatan 654 ST qualitative strain stage
7. Quantitative straining environments using a Hysitron PI-95 with heating options
8. Detailed 3D tomographic reconstructions of samples using either
   • Gatan 925 DT double tilt-rotate stage
   • Hummingbird high tilt (±81°) tomography stage
9. A custom built stage with four electrical probes is available
10. Large variety of ion species in the range between protons and gold
11. Ion beam currents from single ion strikes up to 100 nA (Tandem) and 10 µA (Colutron)
12. Direct photoluminescence, cathodoluminescence, and ion beam luminescence from the entire TEM sample
13. Detailed orientation imaging microscopy (OIM) of texture and grain boundary information via the Nanomegas and ASTAR systems.

Contact:
Khalid Hattar

The I³SEM facility combines a 30 kV JEOL IT300HRLV SEM (1.5 nm spot resolution) with a 6 MV Tandem accelerator. The I³SEM facility can permit a wide breadth of combined experiments in high temperature, gas exposure, mechanical loading, displacement damage, gas implantation, and numerous sequential or simultaneous combinations thereof to evaluate the structural evolution that occurs during ion beam modification or overlapping combinations of extreme environments. Specific capabilities of the I³SEM include:

• Three in-situ SEM mechanical loading frames: Hysitron PI-85 nanoidenter, MTI/Fulham heat straining stage, custom-built fatigue stages.
• Large variety of ion species in the range between protons and gold.
• Ion beam currents from single ion strikes up to 100 nA (Tandem).
• Electron beam or ion beam induced current measurement (EBIC or IBIC).

Contact:
Khalid Hattar
Brad Boyce

The FEI Magellan 400 SEM provides sub-nanometer spatial resolution from 1kV to 30 kV. By using low voltages, only the surface of the sample interacts with the electron beam and thus insulators/beam sensitive samples can be imaged without the need for conductive coatings and the amount of surface data is maximized. These capabilities make this tool ideal for investigations of nanotubes, nanowires, nanocomposites, and other materials where workhorse SEMs do not have the low-voltage resolution required for sensitive surface imaging.

This system features:

• Schottky thermal emission source with UniColore mode to give a highly coherent beam (less than 0.2 eV energy spread)
• Spatial resolutions of 0.8 nm at 1kV and above in secondary electron mode
• EDAX Apollo XV Energy Dispersive Spectroscopy (EDS) detector for elemental analysis
• EDAX Hikari Electron Backscatter Diffraction (EBSD) detector for crystallographic orientation determination
• Nabity electron beam lithography patterning capability
• Annular STEM detector (spatial resolution of 0.7 nm)

Contact:
Chris Sheehan

The Quanta 400 FEG from FEI Company is a high resolution electron microscope that allows data collection from a variety of samples due to its ability to image at relatively high background pressures while reducing sample charging. The system is equipped with a cooling stage, solid-state STEM detector, BSE detector, and Genesis EDS.

Contact:
Darrick Williams

We have two FEI field-emission source SEMs in the Integration Lab at CINT. The Nova NanoSEM 450 includes a Nabity electron beam lithography (EBL) patterning capability. The Nova 600 Nanolab from FEI Company combines ultrahigh resolution SEM with FIB capabilities in one machine for sample analysis, 2D and 3D machining, and prototyping. The resolution of 1.1 nm at 15 kV in secondary electron mode is further enhanced when using the STEM detector.  This dual-beam machine also allows for electron and ion induced deposition of metals from gas source precursors (currently, Pt) with line widths of 50 nm (ion beam) and 20 nm (electron beam). An auto FIB, auto TEM, and pattern generation module is available for ion milling to provide automation of many tasks. The system also includes a Nabity EBL patterning capability.

Contact:
Doug Pete

The low energy electron microscope (LEEM) is a unique and versatile surface microscope that can be used to view dynamic processes on surfaces in real time with a spatial resolution of 7-8 nm and a depth resolution of one atomic layer. The LEEM provides high image contrast between regions on a surface with different atomic structures or chemical compositions. Because it is a non-scanning microscope, dynamic processes can be observed with a time resolution limited only by the video recording rate of the image acquisition system. The LEEM is also equipped with an in situ scanning tunneling microscope for acquiring atomic-scale images of the samples. Current interests for LEEM applications include: 1) studies of the fundamental mechanisms underlying self-assembly and pattern formation on solid surfaces, 2) studies of the evolution of surface morphology including thermal smoothing mechanisms, 3) studies of the fundamental aspects surface phase transitions and surface chemical reactions, 4) studies of doping distributions and surface oxide charging effects in microelectronic device structures, and 5) the development of LEEM-IV analysis to obtain 3-D compositional maps of the surface and near surface regions of crystalline solids. 

Specific capabilities of the LEEM include:

• Ultra-high vacuum (<1x10-10 Torr) in main chamber
• Sample cleaning by ion bombardment and thermal annealing
• Surface characterization by Auger Electron Spectroscopy
• Images can be recorded with the sample at temperatures from 200 K to 1800 K
• Images can be recorded with a flux of atoms or molecules impinging on the surface

Contact:
Taisuke Ohta

The XRD instrument is comprised of a high-precision XRD platform with small-angle x-ray scattering, and variable temperature/pressure, thin-film, and microdiffraction accessories. It is capable of variable-temperature and pressure crystal phase identification and quantification; size, size-distribution, and shape analysis of nanocrystals and crystalline domains; film thickness in single and multilayer films together with core and shell thickness determination in heterogeneous core/shell nanocrystals; stress analysis in films and heterogeneous nanomaterials; and quality control of epitaxial films and superlattices.

Contact:
John Reno

The Rigaku Ultima III is a powder diffractometer that operates in a theta/2theta mode that can analyze many different types of samples (bulk powders, thin-films and liquids). The system is equipped with a standard powder stage, a thin-film stage, a small angle X-ray scattering stage (SAXS), and a Differential Scanning Calorimetry-X-ray Diffraction Stage (DSC-XRD) stage. Also we have software to analyze bulk powders (Crystal Maker, Jade, GSAS), thin-film (diffraction, reflectivity, SAXS) and liquids that contain (Spherical, Core/Shell and Rods nanoparticles).

Contact:
Darrick Williams

The Bruker NANOSTAR is a state-of-the-art tool for characterization of nanostructures ranging from 1 nm to roughly 125 nm, and nanostructured surfaces by SAXS, GISAXS and Nanography.

The mirror-conditioned pinhole collimation system provides a highly intense, parallel X-ray beam so that short measuring times can be achieved. At the same time, the collimation system maintains the ideal circular beam shape and is very efficient in eliminating background, which allows analyzing very weakly scattering samples as well as large structures.

The NANOSTAR analyzes pure sample properties, even for non-isotropic sample systems. The modular design permits setting the detector-to-sample distance from 11.5 mm up to 1070 mm. Hence, the entire range from SAXS to WAXS can be covered.

Features:

• Modular setup for greatest flexibility
• Brilliant X-ray sources: IμS, TXS and METALJET
• MONTEL optics with exchangeable pinhole collimation system for high flux/high resolution
• Low background collimation system using traditional three-pinhole or new SCATEX two-pinhole setup
• Large sample chamber accommodating a variety of sample holders
• VÅNTEC-2000, large 2-D detector with true photon counting ability
• Variable sample-to-detector distance covering a vast q-range

Contacts:
Kyungtae Kim

We have two commercial ultra-high vacuum (UHV) RHK Instruments variable-temperature (~40K to 1000K) scanning tunneling microscopes (STM) and two home-built UHV STMs with custom data acquisition and control software and electronics. Three of these instruments are set up for atomic-scale lithography using hydrogen-passivated silicon surfaces. One RHK STM is available for general surface science experiments.

Contact:
Brian Swartzentruber

We have a Digital Instruments Atomic Force Microscope available for routine imaging.

The available capabilities include:

• Atomic force microscopy: topography and phase imaging
• Conducting tip atomic force microscopy: scanning capacitance, scanning Kelvin force, piezoelectric force, and scanning current-voltage microscopy

We also have a Bruker Dimension Icon Scanning Probe Microscope with many advanced imaging features, including:

• PeakForce® Quantitative nanomechanical mapping, with high-resolution high-stiffness upgrade
• Electrochemical scanned probe microscopy
• Kelvin probe (potential mapping) scanned probe microscopy
• Low-force nanoindentation
• Scanning tunneling microscopy
• Conductive/Photoconductive AFM: Peakforce Tunneling current AFM (PeakForce TUNA) with bottom illumination
• Piezoresponse force microscopy

Contacts:
Brian Swartzentruber
Peter Goodwin
Dan Hooks
Andy Jones

We have constructed a super-resolution microscope based upon single molecule detection and localization (e.g. PALM, STORM, or d-STORM), including both acquisition and analysis software. Can be used to image static cellular structure or selected nanomaterials.

Contact:
Jim Werner

Conventional 2D single molecule tracking via fluorescence microscopy with an EM-CCD camera. We also have unique in-house developed capabilities in active feedback for time-resolved 3D tracking of single nanoparticles, organic dyes, and fluorescent proteins. Can explore 3D transport in live cells or selected soft materials.

Contact:
Jim Werner

The core of the laboratory consists of a 3.2 MV Pelletron® tandem ion accelerator and a 200 kV ion implanter. The tandem accelerator has five beam lines with a series of experimental stations that support various research programs. The operation of IBML and its interactions with users are organized around core facilities and experimental stations. The IBML provides and operates the core facilities, while supporting the design and implementation of specific apparatus needed for experiments requested by users of the facility. This results in a facility with competencies in routine ion beam experiments and the versatility to cater to the individual researchers needs. Detailed information is available at http://www.lanl.gov/mst/ibml/.

Contact:
Yongqiang Wang

Some more demanding electron-beam and optical microscopy and nanomechanics characterization studies may require specialized sample preparation for optimal results. For such studies CINT maintains high-performance sample preparation tools to be used in conjunction with the characterization effort(s). These include the following:

• A Leica RES102 ion mill capable of the following four functions: (1) removing damage in TEM lamellae induced by focused ion beam tools, (2) thinning material to electron transparency for TEM inspection, (3) surface cleaning/polishing of planar surfaces for subsequent imaging and electron backscatter diffraction, and (4) cross-sectionional polishing for site-specific inspection of integrated circuits, printed circuit boards, etc. It is the only commercial ion mill capable of both TEM and SEM preparation.
• A Leica TXP target preparation tool: an all-in-one tool for sawing, milling, drilling, grinding, and polishing for rough preparation of sample surfaces for subsequent optical and electron microscopies.

Contact:
Brad Boyce

CINT provides a range of capabilities to characterize fundamental and quantum optical properties of individual nanoscale materials including colloidal nanocrystals, quantum dots, nanowires, carbon nanotubes, 2D materials and solitary quantum defects in wide variety of solid state hosts. Range of advance optical imaging and spectroscopy experiments includes resonance Raman, photoluminescence, (PL), time and frequency resolved PL spectroscopy, time tagged-time correlated single photon counting, electro-luminescence and photo-current imaging. Quantum Optical Experiments including single photon quantum interference, Hunbury-Brown-Twiss and Hong-Ou-Mandel experiments are also supported. Unique spectroscopy capabilities developed at the lab including single nanostructure spectroelectro chemistry experiment and direct correlation of optical properties and high resolution TEM images acquired on the same set of nanostructures are also available. These capabilities are built upon 4 confocal optical microscopes that can be coupled to continuous follow liquid helium cryostats covering 4 – 500 K temperature range. High resolution spectrometers and state of art low light level detectors allow to investigate any nanomaterials emitting in 400-1600 nm spectral range. Avalanched photodiodes, superconducting nanowire detectors, and single photon counting electronics enable detection of single photons with <60 ps time resolution with ultralow dark count, over 400 – 1600 nm spectral range. Multiple pulse and CW lasers covering 350 nm to 1400 nm spectral range are available as excitation sources.

Specific capabilities include:

• 3 Home-built micro-photoluminescence systems
• Trivista scanning confocal Raman microscope with a triple spectrometer (Acton Research)
• 2 Oxford Instrument’s continuous flow LHe cryostats (4-500 K)
• Acton Research 1/2 meter triple spectrometer and 2 1/3 meter spectrometers
• LN2 cooled CCD and TE cooled EMCCD array detectors covering 400-1000 nm (PI-Acton)
• 1D and 2D InGaAs Diode array covering 900 – 1600 nm spectral range.
• Time-correlated single-photon-counting electronics (B&H SPC 630 & Pico-quant Hydraharp); multiple Si avalanched photodiodes (Perkin Elmer SPCM-50 and id Quantique id100: 300 ps and 50 ps resolution, respectively)
• Single Quantum Eos 410, Four Channel Superconducting Nanowire Single Photon Detection System (>25% QE at 1.3 µm, <50ps timing resolution)
• Lasers (532 nm DPSS, 405 nm diode lasers and Coherent Mira OPO pumped by Chameleon fs Ti:Sapphire laser, Whitelase Supercontinuum Laser)

Contacts:
Han Htoon

This new facility allows us to perform a wide range of advanced optical imaging and spectroscopy studies on individual nanoscale materials at low temperature and under high magnetic field.  Nanoscale materials that can be investigated span from quantum dot, quantum wire, complex oxides, and colloidal nanocrystals, carbon nanotubes, and 2D layered semiconductors to individual defects/dopants implanted in those nano materials. The advanced optical imaging and spectroscopy studies include photoluminescence (PL), PL excitation, Raman spectroscopy and excitation profiling, polarization resolved imaging and spectroscopy, time and energy resolved PL spectroscopy, and photon correlation spectroscopies. The facility can also be expanded to perform low temperature electrical transport studies simultaneously with the advanced optical spectroscopies.  The facility is also coupled to a 2 channel superconducting nanowire detector and a supercontinuum white-light laser to enable time resolve PL and quantum optics experiment under high magnetic field. 

Specific capabilities include:

• 9T Superconducting magnet and microscopy cryostat.
• NIRvana 2D InGaAs diode array detector                                      
• Optical workbench, Opto-mechanics
• TE cooled CMOS camera
• LN cooled Roperscientific CCD camera & ½ meter Acton spectrometer
• Princeton Instruments IsoPlane High Throughput Imaging Spectrometer
• Princeton Instruments Triple Monochromator system with UV and red sensitive CCD detectors
• Superconducting nanowire detector pair
• Spectra-Physics Matisse Doubled Ti:Saph laser system
• Multiple CW diode lasers spanning excitation from 650 to 680 nm and 405 and 460 nm
• Quantum Opus, Two Channel Superconducting Nanowire Single Photon Detection System (> 85% QE at 1.55 µm, <50ps timing resolution)
• Whitelase Supercontinuum Laser

Contacts:
Han Htoon

As part of the Quantum Sensed Nuclear Magnetic Resonance Discovery Platform (QSNMR), scientists at CINT have assembled a Quantum Diamond Magnetometry Microscope. This new capability enables users to image magnetic fields with a noise floor of 1 µT/√(Hz) per pixel up to a 2x2 mm area with resolution down to a few 100 nm, from room temperature down to T = 3 K. This magnetometer utilizes the long quantum coherence of nitrogen vacancies in diamond—the same property that makes them a potential qubit platform—to detect small magnetic fields in a widefield mode. This is accomplished by integrating magnetic materials onto the surface of nitrogen vacancy-implanted diamond, pumping nitrogen vacancies with 532 nm laser excitation and high-power microwaves, and detecting the magnetic field through photoluminescence. This new capability will enable CINT scientist and users to, for example, rapidly image magnetic fields of magnetic materials, image current through fabricated devices, or even reveal the nature of superconductivity in materials.

Contact:
Andy Mounce

The neaSpec scattering type scanning near-field optical microscope (s-SNOM) provides high spatial resolution (<20 nm) imaging and spectroscopy (nano-FTIR) with ultrafast pump-probe capability. It is equipped with femtosecond laser sources at near-infrared 780 nm, 1560 nm, and mid-infrared ranging from 4.7 to 15.3 μm (by DFG), as well as a mid-IR quantum cascade laser unit covering wavelength ranging from 7.5 to 11 μm. This instrument allows to investigate complex physical behaviors in systems including, but not limited to, strongly correlated materials, plasmonic response and wave propagation in 2D materials, nano-wires and carbon nanotubes, resonances in metamaterials, and other nano-structured materials and functional photonic devices.

Contact:
Hou-Tong Chen

Simultaneous electrical and optical characterization of nano-photonic and -photovoltaic devices understanding the competition between recombination and separation/collection of photo generated electron-hole pairs across the interfaces of nanomaterials hold the key to successful development of nanomaterial based novel photonic/photovoltaic devices. CINT possesses unique capabilities to perform photo-current and other electrical transport measurements simultaneously with advanced single nanostructure optical spectroscopies.

Contact:
Han Htoon

Photoluminescence (PL) and its temporal dynamics constitute one of the most fundamental techniques for uncovering fundamental physical properties of nanomaterials and their coupling to the environment. CINT possess multiple time-resolved photoluminescence (TRPL) systems covering wide range of excitation and detection spectral range, a large span of time scale (150 femtoseconds – milliseconds), wide temperature ranges (3K – 400K) and sample configurations (single nanostructure and ensemble as well as different chemical and electrochemical environments).

State of the art equipment includes:

• Coherent Ti-sapphire laser oscillator (>3.5W average power) in conjunction with doubler and tripler attachments and pulse picker
• Coherent Chameleon Ti-Sapphire Laser coupled to Mira OPO
• Continuum ps light source (IChrome TVIS tunable from 480 to 650 nm, 3ps pulsewidth)
• Hamamatsu Streak Camera capable of time resolution and spectral range?)
• Multiple Si based single photon counting modules (time resolution: 50 ps, Spectral range: 400-1000nm)
• InGaAs based single photon counting modules
• Superconducting Nanowire Single Photon Detector (time resolution: <50 ps, Spectral range: 800-1500nm)
• Fluorescence upconversion system from Ultrafast Systems: mixes the fluorescence from the sample with an intense beam from the Ti-Sapphire laser and photon counting to obtain time-resolved PL from the visible to the near IR.

Contact:
Igal Brener

A dedicated UV microphotoluminescence system with CW or pulsed excitation is available. This system photoluminescence from 365nm to 500nm. Available excitation sources are pulsed 266nm and CW 325nm. The UV microscope objective available is a 50x Mitutoyo with numerical aperture of 0.4 and a working distance of 12mm.

Contact:
Ting (Willie) Luk

Ultrafast spectroscopy provides important information about the excitation and relaxation dynamics occurring in complex nanomaterials.  A suite of ultrafast excitation and diagnostic capabilities spanning wavelengths from the ultraviolet to the far-infrared are available for dynamic nanoscale characterization.  These capabilities enable coherent quantum control experiments, as well as experiments for dynamic materials characterization.

Tha abailable capabilities include:

• Femtosecond broadband transient absorption spectroscopy (infrared to ultraviolet) with microscopic spatial resolution
• Can be done at low temperatures (down to 4 K) and high magnetic fields (up to 8 T)
• Capability to both photoexcite and probe complex materials over a broad wavelength range
• Degenerate and non-degenerate four-wave mixing
• Static and time-resolved second harmonic generation
• Static and time-resolved magneto-optical Faraday and Kerr spectroscopy
• Ultrafast scanning tunneling microscopy
• Femtosecond spectral interferometry
• Coherent control with an amplitude/phase LC-SLM pulse shaper

Contact:
Rohit Prasankumar

Our carbon nanomaterials (nanotubes, graphene, graphene oxide) chemistry, processing, and synthesis, capabilities are supported by extensive optical characterization capabilities, including near-IR photoluminescence (PL) spectroscopy, microscopy, and imaging instrumentation.  Near-IR capabilities include wide-area direct imaging, spectroscopy, time-correlated single photon counting, and fluorescence correlation spectroscopy able to access a range of sample types from the single tube and flake level to ensemble measurements of solutions, bulk solids, devices, and films.  Capability for extensive Raman characterization also exists and encompasses  tunable and fixed wavelength Raman (tunable from 345 nm to 1000 nm exc., with fixed instrumentation at 785, 532, 514, and 633 nm). Tunable (700-1000 nm exc.) and fixed wavelength (514 nm) micro-Raman for single-nanostructure spectroscopy and imaging also exist.  Finally, standard UV-Vis-nearIR absorption capability is also available.

Contact:
Han Htoon

Near-IR microscopy capability is built around an inverted microscope system that offers both confocal (diffraction-limited) excitation for rastor-imaging and wide-area excitation for direct 2-D imaging enabled by 2-D InGaAs and EM-CCD camera imaging arrays.  This direct imaging capability allows simultaneous imaging over both arrays for real-time access of differing spectral regions.  The microscope is also integrated to a monochromator system for performing single-element/nanostructure spectroscopic measurements with either InGaAs or CCD linear arrays.  The microscope is also paired with a time-correlated single-photon counting (TCSPC) system for performing lifetime measurements and fluorescence correlation spectroscopy at the small ensemble and single nano-structure levels.  Excitation sources for the microscopy capability include CW diode laser excitation over a range of visible wavelengths and a ps (3 ps pulsewidth) fiber laser with excitations ranging from 480 nm to 650 nm.   Additionally, at the ensemble level we have available standard commercial instrumentation with tunable lamp source excitation for full near-IR photoluminescence excitation mapping.  We also have available for ensemble level measurements an FT-IR based system with tunable lamp and diode laser excitation for rapid spectral acquisition.

Contact:
Andy Jones

Extensive capability for ensemble level and single-nanostructure Raman spectroscopy is available.  Instrumentation includes broadly tunable (UV to near-IR) excitation sources paired to systems for ensemble measurements (tunable from 345 nm to 1000 nm exc., with fixed instrumentation at 785, 532, 514, 405, and 633 nm).  Micro-Raman capability is also available for imaging and single-element spectroscopy, and includes tunable excitation (700-1000 nm exc.) and fixed wavelength (514, 785 nm) confocal microscopy systems.   These systems are available for study of a wide range of materials ranging from solutions to bulk solids, thin films, and device structures.  Materials studies can include as just some examples carbon nanomaterials, bio and soft material composites, quantum dots, nanowires, complex oxides, etc.

Contact:
Andy Jones

Extensive Fourier-transform spectroscopy capabilities are available at CINT, covering a wide range of infrared spectral wavelengths. Two FTIR microscopes are available: a Nicolet Magna 860 for bigger spots and a Bruker FTIR microscope that allow transmission and reflection spectra of samples with 10-micrometer resolution, which is near diffraction-limited for the wavelengths used. The latter system also possesses a spatial mapping capability allowing to build full IR hyperspectral image of the sample. Timeresolved measurements are possible with a step-scan capability included with the system. In the near future, ultrashort-pulse laser will be coupled to the microscope allowing localized sample excitation. Future plans also include coupling ultrashortpulse mid-IR supercontinuum pulses into the system for the purpose of full pump-probe interferometric capability in an all-reflective microscopy setup. Additionally, a Bruker IFS 66 FTIR spectrometer with a low temperature cryostat is available allowing measurements of transmitance and reflectance from room temperature to 4K.

Contact:
Dmitry Yarotski

Broadband terahertz time-domain (THz-TDS) spectroscopy provides simultaneous amplitude and phase information, and becomes a powerful tool for the characterization of materials and devices including semiconductors, complex metal oxides, multiferroics, metamaterials, and fingerprints in many chemicals and biological tissues. Multiple in-house developed THz-TDS based capabilities are available for conventional THz-TDS, optical-pump THz-probe (OPTP), and high power nonlinear measurements.

These capabilities include:

• Fiber-coupled photoconductive conventional THz time-domain spectroscopy for angle resolved reflection, transmission, and scattering measurements
• Tilted wavefront high power THz-pump THz-probe spectroscopy
• Cryogenic capability (4 - 700K) in combination with these THz systems
• Optical-pump THz-probe spectroscopy, using 800 nm, 400 nm (SH) and 267 nm (TH) pump, with additional capability of magnetic field up to 8 T and temperature down to 1.5 K

Contact:
Hou-Tong Chen

An expertise exists to study complicated waveguiding structures including functionalized and nonlinear optical fibers, photonic crystal waveguides and plasmonic or hybrid systems. Capabilities include spectral interferometry for linear characterization and cross-correlation frequency-resolved optical gating for nonlinear processes. Tunable femtosecond lasers near 800 and 1550 nm are available with pulse shaping and derived supercontinua options. Continuous-wave Erbium-doped broadband sources and amplifiers are also available with gigahertz optional modulation.

Contact:
Dmitry Yarotski

Photoemission electron microscopy (PEEM) uses the photoemission process to image surfaces and nanomaterials, and to study the electronic structure locally. To enhance its capability, we have coupled various light sources: a helium discharge lamp (21.22 eV photons), a xenon lamp (tunable between 3.44 to 6.53 eV photons or 190 to 360 nm), an ultrafast laser (4.13 to 5.96 eV or 208 to 300 nm), and a high intensity continuous wave laser (5.82 eV or 213 nm). The PEEM instrument offers various measurement modalities including work function mapping, valence band edge mapping, band dispersion mapping (also known as angle-resolved photoemission spectroscopy, or ARPES), and linear and circular dichroisms.

Contact:
Taisuke Ohta

Two instruments are available: V-VASE and IR-VASE. The UV-Visible Variable Angle Spectroscopic Ellipsometer (VASE) has spectral coverage from 0.24-2.5um, is equipped for ellipsometric measurements on a small sample area, and can be used as scatterometer. These features are particularly useful for metamaterials, photonic crystals, gratings and nano-antenna arrayed with only a small patterned area. This instrument can also perform reflection and transmission measurements to yield absorption information, and attenuated total reflection measurements to study surface photonic states.  The IR Variable Angle Spectroscopic Ellipsometer (IR-VASE) covers a spectral range of 2-40um. For this instrument, the sample can be heated to maximum of 300C; when using this heater stage only a single angle of incidence of 70 deg is available. These instrument allow optical characterization of thin films and substrates in these spectral ranges, for example refractive index (n) and extinction (k) coefficients, or real and imaginary parts of permittivities.

Contact:
Ting (Willie) Luk

This instrument consists of Multi-Photon Laser Scanning Confocal Microscope (Olympus FV1000) with a Fluorescence Lifetime Imaging Attachment (Becker & Hickl). It is among the most advanced, commercially available optical imaging systems, and gives CINT a world-class capability for optical characterization of any array of biological, synthetic, and hybrid nanomaterials. Techniques enabled by this system include Fluorescence Recovery After Photobleaching (FRAP), Fluorescence Resonance Energy Transfer (FRET), Total Internal Reflectance Fluorescence (TIRF). The FLIA module will enable spatial mapping of fluorescence lifetimes.  MCP-PMT detector allows for lifetime resolution imaging in near-IR.

Contact:
George Bachand

Advanced spectroscopic techniques can be combined with optical microscopy to provide a suite of tools for characterizing the spatially dependent properties of nanoscale materials.

The available capabilities include:

• Microscopy: light, fluorescence, and high-resolution
• Single-molecule fluorescence detection, imaging and spectroscopy techniques including: confocal scanning microscopy (one- and two-photon excitation); wide-field, CCD camera imaging using epi-illumination or total internal reflection excitation; single-molecule fluorescence flow cytometry; time-correlated single-photon counting; fluorescence correlation spectroscopy; polarization anisotropy; single molecule tracking in two and three dimensions; high-throughput (~100,000 per image), four-color, single-molecule fluorescence imaging

Contact:
Peter Goodwin

Sensitive to 30 different nuclei, the 90MHz Anasazi multinuclear FT NMR spectrometer instrument is an invaluable and robust tool for a quick characterization of a variety of organic, inorganic, and organometallic precursors used in our laboratories.

Contact:
Sergei Ivanov

We have 7 closed-cycle cryostats set up for measuring the thermal and electrical transport properties of 1-D (i.e., nanowires and nanotubes) and 2-D (various thin films) nanostructures between 10K and 350K.  Using assembling techniques such as dielectrophoresis and nanomanipulation, we can position individual nanowires or tubes on our Transport Discovery Platforms, which permit temperature-dependent measurements of electrical conductivity, thermal conductivity, and Seebeck coefficient.  For thin-film thermal property measurements, we have built a time-domain thermoreflectance pump-probe system that is capable of measuring thermal transport in thin films ~10nm thick, from room temperature to 10K.

Contact:
Tom Harris

Capabilities for electrical transport characterization of nanoelectronic devices are an Oxford Heliox 3He system for 0.3 K to 30 K, an Oxford MX 400 dilution refrigerator for reaching 0.02 K and a Janis flow cryostat for 4K to 300K.  Magnetic fields up to 13 Tesla are available using a superconducting solenoid magnet.  Cryostats are wired with 24 DC and low frequency lines as well as 4 intermediate frequency coax lines.  Hall resistance measurements can be performed using the 4K flow cryostat and a 0.17 T electromagnet.

Contact:
Mike Lilly

We have a custom two-probe nanomanipulator inside of a JEOL 6701F field-emission source SEM. The two probes are controlled independently via piezo actuators with nanometer resolution and can be coarsely positioned within a 7 x 7 x 7 mm3 volume with stick-slip actuators. The two probes and sample are connected to an Agilent B1500A Device Parameter Analyzer to measure electrical conductivity of nanostructures. Typical experiments include measuring the conductivity of as-grown nanowires by passing current through a nanowire between a probe and the growth substrate or between the two probes.

Contact:
Brian Swartzentruber

The mechanical properties of thin films and layered materials or very small volumes of materials cannot be measured using conventional techniques. Nanoindentation methods have been developed to probe materials at depths of tens of nanometers over regions with dimensions of hundreds of nanometers. Using continuous stiffness measurement, we have the capability to measure changes in mechanical properties as a function of depth. Substrate or layering effects can also be examined. We have also measured material length scales and size effects resulting from dislocation concentrations and dislocation interactions with other structural defects. Changes in material properties resulting from impurities, second phase inclusions, or engineered nanostructures can also be measured. Specific capabilities include multiple Bruker/Hysitron SEM and TEM Picoindenters that represents a significant capability enhancement in support of CINT’s signature efforts in in-situ nanomechanics. These systems have a load range from 1 μN to 30 mN, offers in-situ indentation, bending, compression and tension testing capabilities, include a heating stage rated to 400°C, an electrical characterization package, and has outstanding resolution of both load (<1 μN) and displacement (<1 nm).

Contacts:
Nan Li
Dan Hooks
Brad Boyce

System and associated Nanoparticle Tracking Analysis (NTA) software suite automatically tracks, sizes and counts nanoparticles on an individual basis. Through direct observation of particle motion and scattering behavior, particles are simultaneously sized and different materials identified by their disparate scattering intensities. Results are displayed as a frequency size distribution graph and output to spreadsheet, and concentration is directly determined. The high-sensitivity (HS) camera affords a lower detection limit of ~10 nm (upper detection limit ~2000 nm), and an added fluorescence measurement capability allows facile assessment of dark/bright nanoparticle fractions (total number of nanoparticles determined under light-scattering mode and bright particles determined under fluorescence mode). Polydisperse populations can be accurately and quantitatively assessed without the "intensity-biasing" that is characteristic of DLS because size is calculated on a particle-by-particle basis. Ideal for time-dependent studies of particle aggregation (aqueous and non-aqueous-solvent compatible).

Contact:
Jennifer Hollingsworth

Thermogravimetric analysis and differential scanning calorimetry (TGA/DSC) (Netzsch STA 449 F1 Jupiter) are complementary techniques to investigate a material’s response to different temperatures: mass change (e.g., decomposition or sublimation temperatures) and thermal changes often unaccompanied by the mass change as a function of temperature (e.g., melting, glass transition, second order phase transition, enthalpy and heat capacity measurements). Both techniques have become indispensable in the design of new metal precursors and understanding the structure/composition of nanocomposites.

Contact:
Sergei Ivanov
Dale Huber

Waters Synapt G2 Mass Spectrometer featuring double quadrupole and time-of-flight ion separation for very high mass resolution. SYNAPT enables extensive characterization of complex mixtures and molecules with uncompromising qualitative and quantitative performance, streamlined workflows and unparalleled platform versatility. This system is available for characterization of both hard and soft materials.

Contact:
Lisa Phipps

Instrumentation to characterize transport of biomolecular motors and filaments including high contrast DIC, wide-field fluorescence, total internal reflectance microscopy (TIRF), and spinning disk confocal microscopy.

Contact:
George Bachand

The instrument is comprised of a modular optical trapping fluorescence microscope that enables the non-contact 3-dimensional manipulation of trapped objects and a force measurement module capable of measuring interaction forces on the order of 0.1-900 pN, allowing one to observe the unfolding of supramolecular structures, the action of molecular motors, and measurement of the surface adhesion forces of biological cells. This laser trapping system complements the suite of top down and bottom up fabrication and manipulation methods at CINT, and fills a gap in the mechanical characterization in fluidic environments of soft structures composed of nanocomponents, such as biological and biomimetic materials and nanoparticles. We expect that the versatility of the system will be of great benefit to members of our user community interested in addressing the challenges of manipulating and interrogating the interaction between hard and soft nanomaterials in their native environments and integrating these components into composite nanomaterials and functional devices.

Contact:
Jim Werner
Peter Goodwin