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Los Alamos National LaboratoryCenter for Integrated Nanotechnologies
Helping you understand, create, and characterize nanomaterials
DOE

II. CINT Experimental Capabilities: Characterization

Structure Measurements - Techniques that deliver real-space coordinate information;
Property Measurements - Methods that provide characteristic information;
Function/Response Measurements - Experiments that provide dynamic information under time-dependent conditions/stimulation.
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Structure Measurements

Low Energy Electron Microscope (LEEM)

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:
Dr. Taisuke Ohta, tohta@sandia.gov

Transmission Electron Microscopy Lab
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:
Dr. Katie Jungjohann, kljungj@sandia.gov

High Resolution Electron Microscope

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:
Dr. Nate Mara, namara@lanl.gov

In-situ Ion Irradiation Transmission Electron Microscopy (I3TEM) Facility

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:
Dr. Khalid Hattar, khattar@sandia.gov

High Resolution Scanning Electron Microscope, Focused Ion Beam, and Electron Beam Lithography

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, dvpete@sandia.gov

High-Resolution X-Ray Diffraction System
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:
Dr. John Reno, jlreno@sandia.gov

Atomic Force Microscopy

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

Contact:
Dr. Brian Swartzentruber, bsswart@sandia.gov

Scanning Tunneling Microscopy
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:
Dr. Brian Swartzentruber, bsswart@sandia.gov

Ion Beam Materials Laboratory
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:
Dr. Yongqiang Wang, yqwang@lanl.gov

Environmental Scanning Electron Microscope
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, darrick@lanl.gov

X-Ray Diffraction System

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, darrick@lanl.gov

Small-Angle / Wide-Angle X-Ray Scattering

Bruker Nanostar for wide q-range characterization of soft materials under controlled environments.

Contact:
Dr. Millie Firestone, firestone@lanl.gov

In Situ Dynamic Atomic Force Microscopy
An Asylum MFP-3D-SA AFM system allows for both standard and user-defined operation modes. A specific application focus of this new AFM is imaging and spectroscopic force measurements of dynamic biological and biomimetic assemblies and structure formation.

Contact:
Dr. Gabe Montano, gbmon@lanl.gov

XRD

The XRD instrument is comprised of a high-precision XRD platform with small-angle x-ray scattering, and variable temperature, thin-film, and microdiffraction accessories. It is capable of variable-temperature 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:
Dr. Gabe Montano, gbmon@lanl.gov

Super Resolution Imaging

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:
Dr. Jim Werner, jwerner@lanl.gov

Property Measurements

Electrochemistry of Nanoscale Structures
We have a microfabricated fluidic platform that permits the investigation of electrochemical energy storage processes in real time inside a transmission electron microscope (TEM).  This Electrochemical Discovery Platform is comprised of top and bottom micromachined chips that form a sealed, 100nm thick cavity that can contain liquids while exposed to high vacuum.  This electrochemical platform features 10 electrical leads with customizable passivation layers that converge at the center of the device and reside on an electron transparent (40nm thick) silicon nitride membrane. This device, which we combine with state-of-the-art electrochemical testing equipment capable of ~10fA current levels, allows users to perform controlled electrochemistry on small volumes (e.g., single nanowires or 10’s of nanoparticles) of precisely positioned nanomaterials, while visualizing microstructural changes in the material of interest via TEM.

Contact:
Dr. Tom Harris, ctharris@sandia.gov

MEMS and NEMS Characterization

Our Nanomechanics Discovery Platform features a variety of MEMS-based actuators (both thermal and electrostatic) and microscale cantilevers that enable one to understand phenomena associated with the motion, displacement, or vibration of nanoscale structures.  Our lab capabilities include multiple interferometers with temperature-dependent stages and a laser Doppler vibrometer for the detection of MEMS/NEMS resonator motion, resonance frequency, and quality factor.  The microcantilever arrays on the Nanomechanics Platform permit studies of the mechanical properties and of mechanical deformation and fracture in deposited thin-film materials.

Contact:
Dr. Tom Harris, ctharris@sandia.gov

Variable-Temperature Measurments of Nanostructure Transport Properties

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:
Dr. Tom Harris, ctharris@sandia.gov

Variable and Low Temperature Electronic Transport

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:
Dr. Mike Lilly, mplilly@sandia.gov

Hysitron PI-85 SEM Picoindenter

This in-situ SEM strain stage represents a significant capability enhancement in support of CINT’s signature efforts in in-situ nanomechanics. The system has a load range from 1μN to 30mN, offers in-situ indentation, bending, compression and tension testing capabilities, includes a heating stage rated to 400°C, an electrical characterization package, and has outstanding resolution of both load (<1μN) and displacement (<1nm).

Contact:
Dr. Nate Mara, namara@lanl.gov

Mechanical Properties from very Small Regions

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 two nanoindenters with continuous stiffness measurement up to 2 N, lateral force measurement, AFM scanning, nanopositioning, and a thermal stage.

Contact:
Dr. Nate Mara, namara@lanl.gov

Nanomanipulator for In Situ Nanostructure Electrical Characterization

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:
Dr. Brian Swartzentruber, bsswart@sandia.gov

Mid-Infared Time-Domain Spectroscopy

A system for measuring optical transients in the mid infrared (7-14 microns) is available. The system employs phase-matched electro-optic sampling for detection and difference frequency generation for creating the IR transients (~400fs). The system allows for characterization of phase and amplitude of optical fields in addition with time-resolution. This system can be used to obtain phase and amplitude response of optical samples in transmission or reflection in this IR optical range.

Contact:
Dr. Igal Brener, ibrener@sandia.gov

Optomechanics

Optomechanics capabilities will consist of advanced design, fabrication, and testing of optomechanical structures.  A test station capapable of coherent coupling light on and off chip at wavelenghts spanning all telecommunications bands as well as the near infrared will be constructed, as well as the RF equipment and software for mechanical and electrical readout.  New projection lithography techniques will be used to selectively metallize 3D surfaces and explore optomechanics at ultra-high frequencies sub-wavelength volumes.

Contact:
Dr. Ryan Camacho, rcamach@sandia.gov

Terahertz Spectroscopy

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 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 configured for transmission measurements, 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:
Dr. Hout-Tong Chen, chenht@lanl.gov

Carbon Nanotube and Nanomaterials Spectroscopy and Characterization

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:
Dr. Steve Doorn, skdoorn@lanl.gov

Near-IR Fluorescence Microscopy, Imaging, and Spectroscopy

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:
Dr. Steve Doorn, skdoorn@lanl.gov

Raman Spectroscopy, Microscopy, and Imaging

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:
Dr. Steve Doorn, skdoorn@lanl.gov

FTIR Spectroscopy and Microscopy

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:
Dr. Anatoly Efimov, efimov@lanl.gov

Ultrafast Broadband Characterization of Photonic Waveguides

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:
Dr. Anatoly Efimov, efimov@lanl.gov

Ultrafast Spectroscopy and Coherent Control

MilliJoule and microJoule 100-fs Ti:Sapphire lasers equipped with optical parametric amplifiers and a difference-frequency generator covering a wide range of wavelength (266-4000nm) are available for custom setups for various pump-probe configurations in materials, photonic and biophotonic research. Femtosecond interferometry and spectral interferometry are available in addition to standard lock-in detection techniques. Coherent control experiments with an amplitude/phase LC-SLM pulse shaper are possible.

Contact:
Dr. Anatoly Efimov, efimov@lanl.gov

NanoSight LM10-HSB Multi-Parameter Nanoparticle Characterization System

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:
Dr. Jennifer Hollingsworth, jenn@lanl.gov

Apertureless Near-Field Scanning Optical Microscopy and Spectroscopy

This capability is designed to perform high resolution, 3 dimensional mapping of plasmonic field of metallic nanostructures and exciton-plasmon interactions of metal-semiconductor hybrid nanostructures.

Contact:
Dr. Han Htoon, htoon@lanl.gov

Optical Spectroscopy of Individual Semiconductor Nanostructures

Optical spectroscopy has been utilized widely in studies of light-nanostructure interactions.  Conventional spectroscopic techniques however can only probe an average response of a large ensemble of nanostructures.  CINT house several capabilities that allow to perform wide variety of optical imaging and advanced spectroscopy studies on the individual nanostructures in the temperature range of 4⁰ to 340⁰ K.  In addition, CINT also possesses capability to directly correlate the optical properties of individual nanostructures with their structural properties.  This unique capability is achieved through performing optical spectroscopy studies and high resolution structural imaging including atomic force and scanning/transmission electron microscopies on the same nanostructures.

Advanced single nanostructure spectroscopy capabilities of CINT includes:

  • Photoluminescence (PL) and PL excitation spectrosocpy
  • Raman imaging and spectroscopy
  • Time resolved and time tagged PL spectroscopy
  • Photon correlation/cross-correlation spectroscopy
  • Single nanostructure, time resolved, spectro-electrochemistry

Contact:
Dr. Han Htoon, htoon@lanl.gov

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:
Dr. Han Htoon, htoon@lanl.gov

Time-Resolved Photoluminescence

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(fs)– milliseconds), wide temperature ranges (3K – 400K) and sample configuration (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 bsed 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-S laser and photon counting to obtain time-resolved PL from the visible to the near IR.

Contact:
Dr. Han Htoon, htoon@lanl.gov

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

Contact:
Dr. Sergei Ivanov, ivanov@lanl.gov

Simultaneous TGA/DSC Analyzer

Thermogravimetric Analysis and Differential Scanning Calorimetry (TGA/DSC) (Netzsch STA 449 F1 Jupiter) are complementary techniques to investigate 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 indispensible in the design of new metal precursors and understanding the structure/composition of nanocomposites.

Contact:
Dr. Sergei Ivanov, ivanov@lanl.gov

UV Micro Photoluminescence

A dedicated UV microphotoluminescence 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:
Dr. Ting (Willie) Luk, tsluk@sandia.gov

Variable Angle Spectral Ellipsometer (IR and UV-Visible)

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:
Dr. Ting (Willie) Luk, tsluk@sandia.gov

Ultrafast Broadband Optical Spectroscopy

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

Contact:
Dr. Rohit Prasankumar, rpprasan@lanl.gov

Optical Microscopy and Single Molecule Spectroscopy

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 hyper-spectral
  • 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
  • Near-field scanning optical microscopy, combined with both cw and transient absorption spectroscopy
  • Low temperature optical microscopy/spectroscopy in combination with various scanning probe techniques

Contact:
Dr. Peter Goodwin, pmg@lanl.gov

Simultaneous TGA/DSC Analyzer

Thermogravimetric Analysis and Differential Scanning Calorimetry (TGA/DSC) are complementary techniques to investigate 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 indispensible in the design of new metal precursors and understanding the structure/composition of nanocomposites.

Contact:
Dr. Dale Huber, dlhuber@sandia.gov

Holographic Optical Trapping and Force Measurement System

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 measure 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:
Dr. Wally Paxton, wfpaxto@sandia.gov

Function/Response Measurements

2D and 3D Single Molecule and Particle Tracking

Conventional 2D single molecule tracking via fluorescence microscopy with an EM-CCD camera. Also have unique 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:
Dr. Jim Werner, jwerner@lanl.gov

Biomolecular Transport Manipulation and Characterization

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:
Dr. George Bachand, gdbacha@sandia.gov

Multi-Photon Laser Scanning Confocal and Fluorescence Lifetime Imaging Microscope

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:
Dr. Gabe Montano, gbmon@lanl.gov

Sinlge-Molecule Manipulation, Biomolecular Motor Mechanics and Application of Calibrated Magnetic Forces

Instrumentation for parallel application of calibrated vertical magnetic forces with simultaneous evanescent wave scattering readout of polymer length.

Suitable for:

  • Unzipping individual short DNA molecules to monitor protein binding, measure equilibrium association constants, and probe binding kinetics with dynamic force spectroscopy (DFS).
  • Epi-illumination tethered particle motion (TPM) monitoring of single-molecule transcription with and without dynamic magnetic forces.
  • Characterizing unbinding forces of any receptor-ligand system that can be set up in the magnetic microsphere / planar glass slide configuration.

Instrumentation for application of calibrated horizontal magnetic forces or application of fields using customized magnetic pole piece configurations.

Suitable for:

  • Calibrating magnetic forces on polymer / superparamagnetic nanoparticle composites using micromachined piconewton force sensing spring; sensitive to 300 femtograms magnetite (or equivalent sat. moment), 1 pN force sensitivity, and >= 500 nm microsphere radius.
  • Laterally stretching / unzipping single molecule tethers (e.g. lambda DNA, chromatin) monitoring force-extension with cross-correlation video tracking.
  • Application of forces to molecular motor / shuttle systems via attached magnetic microspheres.
  • In-cell manipulation of functionalized magnetic nanoparticles.

Custom software applications for tethered particle motion (TPM) analysis, in-plane motion tracking, dynamic force spectroscopy (DFS) analysis and simulation, polymer force-extension modeling.

Contact:
Dr. Peter Goodwin, pmg@lanl.gov