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LAB EQUIPMENT:

 

Tandem LASIS-GRR Set-up:

 

Location: Senter Hall 104, University of Tennessee, Knoxville, TN 37996

  1. Q-switched Nd:YAG pulsed laser (manufactured by Brilliant Inc.) of wavelengths 532 and 1064nm which provides 165 and 330mJ/pulse respectively at a repetition rate of 10Hz with laser pulse width of 4 nsec. The laser beam is focused at a metal target in a desired liquid medium inside a sealed stainless steel reactor cell.

  2. Reactor cell mounted with a high damage threshold laser window on the top as well as four side viewing windows to accurately adjusting the laser focus status, while a gas inlet and outlet is mounted to enable inert gas circulation. The metal target platform, mounted on a stepper motor, rotates continuously to enable uniform ablation from the surface. The reactor cell is also provided with heating coils and a thermocouple for temperature control, an injection unit for chemical injection rate control, as well as a sonic dismembrator for real-time de-aggregation of the synthesized nanoparticles.

  3. The aforementioned set-up is housed inside a caging shielded for class 4 laser safety requirements.

Laser Induced Breakdown Spectroscopy (LIBS): 

 

Location: Senter Hall 104, University of Tennessee, Knoxville, TN 37996.

 

Capabilities: TSI Inc. manufactured Insight™ is an integrated, turn-key LIBS platform capable of providing quantitative chemical characterization of atomic constituents in any sample in solid, liquid or aerosol form with ppb level of precision from atomic emission spectral signatures.

In order to analyze nanoparticle samples with high spatial and temporal resolution in real-time, the reactor cell was custom ordered. The system includes:

  1. In-house built reactor cell specifically designed for real-time in-situ characterization of air-borne nanoparticles with high spatial and temporal resolution. Atomic emission data for nanoparticles are collected in nsec timeframes with spectral resolution capable of detecting elemental compositions in nano-scaled particles (~ 10 - 20 nm).

  2. Q-switched Nd:YAG laser, of wavelength = 1064 nm and laser energy 200mJ/pulse with a pulse width of 8 nsec.

  3. Shamrock 303i Czerny-Turner spectrometer with triple-grating.

 

Direct Electrochemistry Experimental Set-up:

 

Location: Senter Hall 104 & 116, University of Tennessee, Knoxville, TN 37996

 

Scanning Probe Microscopy set-up with AFM and STM capabilities:

 

Location: Senter Hall 106, University of Tennessee, Knoxville, TN 37996.

Capabilities: NT-MDT manufactured SPM with AFM/STM/KPFM capabilities; Model Ntegra Prima BasicTM is capable of simultaneous surface topography/phase, local conductivity and surface potential measurements as well as electrochemical measurements in STM mode under liquid conditions.The system includes:

  1. Scanning Atomic Force Microscopy (AFM) head for measurements in liquid and air/gas environment in basic AFM modes

  2. Exchangeable universal Scanning Tunneling Microscopy (STM) head (NTEGRA version) that has been modified for use with high resolution optics ~ 1 um

  3. System capable of mounting samples in high vacuum conditions up to 0.001 torr vacuum compatibility

 

Spectroscopic Ellipsometer:

 

Location: Senter Hall 104, University of Tennessee, Knoxville, TN 37996.

Capabilities: Horiba manufactured Phase Modulated Spectroscopic Ellipsometer; Model: UVISEL is capable of ultra-high resolution and sensitivity characterizations of thin films, surfaces and interfaces from a few angstroms to several microns thickness and for single layer or complex multilayer stacks. The system is also capable of measuring refractive index, extinction coefficient and optical band gap along with film crystallinity and composition.

 

  1. Spectral Range of ~190 nm to 880 nm; Resolution: 0.4 nm.

  2. Measurements in Micro Spots of sizes: 80 μm, 100μm and 1 mm.

  3. Computer controlled variable angles of incidence from 55° to 90° by step of 0.01°.

  4. Low Stray Light DUV‐Visible Monochromator and Detector. Solar blind PMT to cover DUV and high sensitivity red PMT to cover visible‐NIR.

 

Scanning Mobility Particle Sizer (SMPS):

 

Location: Senter Hall 104, University of Tennessee, Knoxville, TN 37996.

Capabilities:  TSI Inc. manufactured scanning mobility particle sizer spectrometer; Model: 3936 is a high resolution nanoparticle sizer that uses a differential mobility analyzer (DMA) in conjunction with condensation particle counter (CPC) for nanoparticle size characterization and distributions. The technique is widely used for measuring airborne particle size distributions as well as nanoparticle size measurements of particles suspended in liquid. The method is independent of the refractive index of particle or fluid, and has a high degree of absolute sizing accuracy and measurement repeatability.

  1. High resolution data: up to 167 channels

  2.  Broad size range: from 2.0 nm to 1000 nm

  3.  Fast measurements: complete size distributions in 16 seconds

  4.  Wide concentration range from 1 to 107 particles/cm3 

  5. Ability to size select particles with narrow size distributions of geometric standard deviation < 1.05 

Dynamic Light Scattering (DLS):

 

Location: Senter Hall 116, University of Tennessee, Knoxville, TN 37996.

Capabilities: Malvern Instruments manufactured dynamic light scattering (DLS) equipment; Model: Zetasizer Nano ZS is capable of characterization of nanoparticles, colloids and proteins through the solution phase measurements of size, electrophoretic mobility of proteins and nanoparticles as well as zeta potential of colloids and nanoparticles. The instrument provides the following capabilities:

  1. Particle and molecular size measurements in the range of ~ 0.3nm – 10.0 mm with an accuracy and precision of ~ +/-2% (NIST traceable latex standards)

  2. Zeta potential and protein mobility measurements on particle sizes of ~ 3.8 nm – 100 µm with an accuracy of 0.12 µm.cm/V.s for aqueous systems (NIST SRM1980 standard reference)

  3. Molecular weight measurements in the range: ~ 980 Da – 20 MDa with +/- 10% accuracy

  4. Temperature control range: 0°C - 90°C +/-0.1

  5. Light source: He-Ne laser with 633 nm and maximum power ~ 4mW.

Nanometer Aerosol Sampler (NAS):

 

Location: Senter Hall 104, University of Tennessee, Knoxville, TN 37996.

Capabilities:  TSI Inc. manufactured NAS is an electrostatic precipitator that samples nanoparticles of different sizes; Model: 3089 enables uniform deposition of size selected nanoparticles by sampling charged aerosols onto substrates with control over the collection spot size using different electrode sizes, flow control, and voltage control. The system has the following features:

  1. Uniform particle deposition on various substrates: TEM grids, Mica and/or glass slides

  2. High collection efficiency of charged particles in the range: ~ 2 nm -100 nm

  3. Flow and voltage adjustment

  4. Suitable for sample preparation for electron microscopy (TEM/SEM) and scanning microscopy (AFM/STM) measurements.

Controlled Atmosphere Glove Box:

 

Location: Senter Hall 116, University of Tennessee, Knoxville, TN 37996.

Capabilities: MBraun manufactured controlled atmosphere glove box with gas purifier and dual user workstation; Model: Unilab 1950 is ideally suited for high purity sample preparation and storage especially to prevent any contamination to catalytic nanomaterials as well as to prevent oxidation and moisture adsorption during sample treatments and preparations. The system has the following provisions:

  1. Fully automated (PLC controlled) gas pressure and atmosphere controlled chamber allowing box pressure control of: -15 to +15 mbar

  2. PLC-controlled quick purge unit with gas flow control of ~ 200 l/min

  3. PLC controlled solid state H2O analyzer; Measuring range: 0-500 ppm.

  4. PLC controlled solid state O2 analyzer; Measuring range: 0-1000 ppm

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