Major Instrumentation

SPECTROSCOPY

SURFACE ANALYSIS

THERMAL ANALYSIS

SYNTHESIS

CRYSTALLOGRAPHY

POLYMER/PARTICLE ANALYSIS

GAS ANALYSIS

ELECTROCHEMISTRY

 

 

SPECTROSCOPY    
INSTRUMENT CAPABILITIES TYPICAL USE

Fourier Transform Infrared Spectrometer
(FT/IR-6300, Jasco)

Location:   132 Nieuwland Science Hall

ftir_website
View Examples of Results:
Far IR Spectra
Fitting of FTIR Spectrum
Near IR Spectra

Range: 350 -15,000 cm-1

Resolution: 0.07-16 cm-1

Detectors:

  • DLA-TGS (Peltier temp. control)
  • InSb (11500~1850 cm-1)

Single reflection micro-ATR

Interchangeable ATR crystal plates

Sampling capability for liquids, solutions, gels, pastes, powders and solid

Library with 10,000 compound data base

Molecules structure and composition

Surface active centers (adsorbents)

Reaction kinetics

Solutes concentration

 

 

Fourier Transform Infrared Spectroscopy Microscope (FTIR-6300, Jasco)
(Spotlight 200 Perkin Elmer)

Location:  132 Nieuwland Science Hall

Ftir Microscope Website





View Examples of Results:
FTIR results

Spectra can be recorded at a spatial resolution down to 10 um.

Transmission, reflectance, and automated-ATR modes

Spatially resolved FTIR

Micro-Raman Spectrometer (NRS-5100, Jasco)

Location:  132 Nieuwland Science Hall

raman_jasco_website
View Examples of Results:
Raman Spectrum of Volatile Liquids
Elimination of Fluorescence
X-Y Surface Profile Map
Z-X Depth Profile Map of Polymer Compositions

532 and 785 nm excitation lasers

Range 50 – 8000 cm-1

Dual Spatial Filtration (DSF) for enhanced spatial resolution and fluorescence rejection

Microscope with 5×, 20×, 100× objectives

High-Speed XYZ imaging capability

Simultaneous visual observation of laser spot and spectrograph measurement area

Materials and molecules structure and composition

Molecular imaging and nanostructures mapping

Observation of low frequency excitations in solids: plasmons, magnons, phonons, and superconducting gap excitations

 

 

Raman Spectrometer (Bruker) with in situ measurement capability for hydro- and solvothermal syntheses

Location:  305 Stinson-Remick Hall of Engineering

raman_bruker_website
View Example of Results:
In-situ Monitoring of Uranyl Cluster Formation

Spectral range 100-3100cm-1

Resolution 5cm-1

Working distance 60-70mm

Laser power 400mW

Max. power at sample 280mW

Video camera for in-situ observation

Temperatures up to 220°C

In-situ studies of reactive intermediates in solution phase syntheses

Ordinary Raman uses:

  • Solution Raman
  • Micro-Raman
Solar Simulators

Location:  132 Nieuwland Science Hall
 

Xe Lamp Housing

 

2 Xe lamps with AM1.5 filters

  • 150W ozone free
  • 300W
Beam turner, power meter, and other filters available

Photocatalyst and PV illumination

Anything requiring UV-Vis irradiation

UV-Visible-Near IR Spectrometer
(V-670, Jasco)

Location:  132 Nieuwland Science Hall

uv_vis_website
View Examples of Results:
Absorption of Near-IR Materials
Kubelka-Munk Transformed Powder Reflectance Spectra
Powder Reflectance Spectra
Spectrum Fitting
Total Transmittance Spectra of Colloids

Double-beam, dual grating monochromator utilizing PMT and PbS detectors

Range 190 to 3200 nm

Bandwidth: 0.1 – 10nm (UV/Vis) 0.4 – 40nm (NIR)

Scan rate: 10 – 4000nm/min (NIR)

Data interval: 10msec (time course)

Integrating Sphere (200-2500 nm) for colloids and powders

Solutes concentration

Sample composition

Reaction kinetics

Semiconductor and metallic nanoparticles shapes, sizes and compositions

SURFACE ANALYSIS    
INSTRUMENT CAPABILITIES TYPICAL USE

Adsorption Physi/Chemi
(BET, ASAP-2020 Micromeritics)

Location:  132 Nieuwland Science Hall

adsorption_websitwe
View Examples of Results:
CO2 Adsorption: Aerogels
Mesoporous Structures
Microporous Structures Adsorption Isotherm, T-plot and Pore Sizes

Pressure Measurement Specifications:

  • Range: 0 to 950 mmHg
  • Resolution: 10-mmHg Transducer - 0.00001 mmHg (Analysis) 1 mmHg (Degas)
  • Accuracy: Within 0.15% of reading

2 degas ports

Chemisorption & Vapor adsorption options

Surface area of adsorbents, fine powders, ceramics

Macro/Meso/Microporosity

Chemisorption (metal and oxide catalyst active surface area)

Pyridine adsorption (acidity /basicity of surface active centers)

Profilometer
(DektakXT, Bruker)

Location:  132 Nieuwland Science Hall

profilometer_website
View Examples of Results:
2D Line Scans of TiO2 Nanostructured Film by Different Styli
3D Surface Profile

Stylus radii: 0.2um, 2um, 12.5um

Minimum spacing between data points 3nm, allowing to scan nanostructured surfaces.

2D surface profile scans, 3D mapping

2D stress scans

Stylus force 1-15 mg

Max scan area 15x15 cm

Surface roughness

Film thickness

Advanced image processing for Volume and Surface area analysis, Grain analysis

Thin film stress

Atomic Force Microscope (AFM, Park XE7)

Location: Fitzpatrick Hall B31

130726 Park Systems Xe7 Atomic Force Microscope Afm








View Examples of Results:
Graphene Sample

0.03 nm resolution/noise limit

29.5 um z-travel range,

zero background correction
Nanosclae topological imaging through non-contact AFM

Also capable of basic contact, lateral force, and phase imaging

X-Ray Photoelectron Spectrometer
(XPS, PHI VersaProbe II)

Location:  132 Nieuwland Science Hall

xps










View Examples of Results:
Solder Ball Surface Chemistry by XPS Depth Profiling
XPS Mapping of Calcium Containing Stain Red- Ca, Green- Au

Monochromatic X-ray beam focusable to 9 um spot size (no satellite peaks, high spatial resolution).

Modes of operation:

  • General XPS spectrum
  • Element scan
  • Line scan
  • Element or chemical state map
  • Depth profile
  • Angle-resolved spectra

Microscope for coarse sample positioning

X-ray induced secondary electrons imaging for fine sample positioning

Argon ion gun for sample cleaning or depth profiling 

High pressure gas cell for sample activation and catalysis

Surface elemental analysis

Oxidation state of surface elements

Surface transformation during gas phase activation and catalysis

THERMAL ANALYSIS    
INSTRUMENT CAPABILITIES TYPICAL USE

Differential Scanning Calorimeter
(DSC-1, Mettler Toledo)

Location:  132 Nieuwland Science Hall

dsc_website
View Examples of Results:
Phase Diagrams of Binary Mixtures
Thermal Response of Polymers

Sensitivity 0.04 mW for the measurement of weak effects

Resolution ± 0.02 K allows measurement of rapid changes and close-lying effects

Temperature range: from –150 °C to 700 °C

Heating rate 0.02 - 300 K/min. Cooling rate 0.02 K - 50 K/min.

Star-shaped arrangement of 50 thermocouples compensates any possible temperature gradients, guarantees flat baselines and reproducible measurement results

Thermochemical reactions: Decomposition, Pyrolysis, Oxidation (transition enthalpies)

Phase changes: Melting, Crystallization, Vaporization, Crystalline & Glass transitions, Adsorption

Phase diagrams and composition

Calorimeter
(Setaram)

Location:  306 Stinson-Remick Hall of Engineering

calorimeter_website
View Example of Results:
Enthalpy of AI2O3 Formation

Isothermal Differential Heat Flow

Temperature range: 500 ˚C – 1000 ˚C.

Temperature Accuracy ± 0.1%

Enthalpy accuracy ± 1%

Resolution: 50 µW

Cells: 28 ml (quartz cell) - 20 ml (platinum crucible)

The heats of formation of complex actinide materials containing transuranic elements

Drop solution calorimetry with gas flow above the sample and/or gas bubbling through the molten solvent

Direct reaction calorimetry to form alloys and compounds

Aluminothermic and other oxidation-reduction reactions

Gas-solid, gas-liquid, and liquid-liquid reactions

Thermal Gravimetric Analyzer
(TGA/DSC-1, Mettler Toledo)

Location:  132 Nieuwland Science Hall

tga_dsc_website
View Examples of Results:
TGA/DSC of Thermolysis
Thermo-induced Reaction
 

Sub-microgram resolution over the whole measurement range

Analyze samples from 25 C - 1600 C

DSC option for simultaneous detection of  heat capacity of thermal events

Thermochemical reactions: Decomposition, Pyrolysis, Oxidation

Phase changes: Melting, Crystallization, Vaporization, Crystalline & Glass transitions

Adsorption

Specific heat capacity

Organic content / purity

Thermal Gravimetric Analyzer (TGA/DSC-1) coupled with Mass Spectrometer (Thermo Star, Pfeiffer)

Location:  132 Nieuwland Science Hall

tga_dsc_attached_massspec_website
View Example of Results:
TGA/DSC/MS of Thermal Decomposition and Reaction

(For Mass Spec):

Inlet heater, controllable to 200 ºC reduces condensation in the inlet.

Mass Spectral Library includes 72 common gasses / solvents - expandable

Molecules up to 300 amu can be monitored

Detection limit 8ppb

Data collection speed of 500 points per second

Same as TGA-DSC plus:

Analysis of the composition of vapours evolved during sample heating:               

  • gases
  • volatile organic compounds
  • adsorbates
  • surface ligands
CRYSTALLOGRAPHY    
INSTRUMENT CAPABILITIES TYPICAL USE

Powder XRD
(D8 Advance Davinci, Bruker)

Location:  303 Stinson-Remick Hall of Engineering

powder_xrd_website
View Examples of Results:
Composition of Nanomaterials
Crystal Structure of Hydrothermally Synthesized Inorganic Compounds

SOL-XE energy dispersive X-ray detector

Rotating sample stage. 

Vertical goniometer, Theta/2Theta or Theta/Theta geometry

Max. usable angular range: 2Theta ≤ 168°

Smallest addressable increment: 0.0001°

Maximum angular speed: 20/s

Routine crystallographic structure analysis

Single Crystal XRD
(ApexII, Bruker)

Location:  303 Stinson-Remick Hall of Engineering

sc_xrd_website
View Examples of Results:
Crystal Lattice Analysis and Unit Cell Parameter
Crystal Structure Modeling

CCD area detector

Low temperature (liquid nitrogen stream) device.

Microfocus sealed tube

Latest type of Montel mirror.

Mo Kα radiation (wavelength of  0.71073 Å). -SOL-XE energy dispersive X-ray detector

Determination of crystallographic structure of novel organic, inorganic, and organometallic materials

SYNTHESIS    
INSTRUMENT CAPABILITIES TYPICAL USE

Microwave Reactor
(Discover/Explorer12, CEM)

Location:  132 Nieuwland Science Hall

microwave_reactor_website
View Examples of Results:
Metal Nanoparticle Synthesis in Poor (Octadecene) and Good (Dioctyl Ether) Microwave Absorbers
PEG Film Decorated with Ag Nanoparticles
Temperature and Pressure Curves of MW Heating of High-boiling Solvents

Heating Rate: 2-6ºC/second

Max Temperature: 300ºC; Max Pressure 20 bar (300 psi); Max Power: 300 W

Open Vessel option included for reflux reactions

Operating Volume: 0.2 – 75 mL (0.2 – 50 mL pressurized)

Gas Purging kit

Synthesis and catalytic reactions:

  • at high solvent vapor pressure (allows to heat the reaction above solvent boiling point)
  • under microwave irradiation
  • in supercritical fluids
  • under  inert (e.g. N2, Ar) or reactive (e.g. H2, CO) gas pressure (with gas addition kit)

Thermal Evaporator
(Oerlikon Leybold UNIVEX 250)

Location:  132 Nieuwland Science Hall
 

thermal_evaporator

 

Two shuttered thermal sources available for sequential deposition

High vacuum system with a 345 L/s turbopump

Front loading door

Swappable stage configuration. One stage is water cooled with rotation, and the other stage can tilt and rotate.

Quartz crystal controller allows for automated deposition thickness control

Creation of thin metal films for:

  • electronic devices
  • solar cells
  • sensors
POLYMER / PARTICLE ANALYSIS    
INSTRUMENT CAPABILITIES TYPICAL USE

Size Exclusion Chromatography with Multiangle Light Scattering Detector
(SEC/MALS (+ FFF), Wyatt)

Location:  370 Stepan Chemistry Hall

Contact:   Dr. Haifeng Gao
at 574-631-8023 or hgao@nd.edu

sec_mals_website
View Examples of Results:
Chromatograms from WTC Columns for Protein
Polymer Mass Distribution

18-angle light scattering detector

Compatible with any Field Flow Fractionation

Supplied with 3 columns for complimentary SEC

Separation of macromolecules

Measurement of absolute molecular weight, size and conformation of macromolecules in solution

Zetasizer and Dynamic Light Scattering (DLS)
(Nano-ZS, Malvern)

Location:  370 Stepan Chemistry Hall

Contact:   Dr. Haifeng Gao
at 574-631-8023 or hgao@nd.edu

z_sizer_website
View Examples of Results:
Electrophoretic Mobility Distribution
Polymer Particle Size Distribution

Size of particles and molecules in a size range 0.3nm to 10 microns using NIBS technology and Dynamic Light Scattering

Zeta potential  in aqueous and non-aqueous dispersions (particles size range 3.8nm - 100µm)

Macromolecule weight in Static Light Scattering operation mode using Debye plot

Molecular weight range 980 Da – 20 MDa

Compatible with any SEC system

Particles size distribution (hydrodynamic radius) for colloids and emulsions

Colloid nanoparticles surface charge and stability

Protein crystal screening

2nd virial coefficient determination

Oligomer identification

Protein-melting point

GAS ANALYSIS    
INSTRUMENT CAPABILITIES TYPICAL USE

ISQ Gas Chromatograph with Mass Spectrometry
(Thermo Scientific Trace GC Ultra with Mass Spectrometer)

Location:  215 Radiation Research Building

gcms_2_
View Examples of Results:
Gas Chromatograph with Mass Spectrometry

Dual injector ports capable of running distinct carrier gases

Autosampler for high throughput

Equipped with 4 detectors:  TCD, ECD, FID, and Mass Spec

ISQ Mass Spec with 1.2-1100 amu range and gas fingerprinting match to library

Gas Analysis:

  • Separation
  • Detection
  • Identification
  • Quantification
ELECTROCHEMISTRY    
INSTRUMENT CAPABILITIES TYPICAL USE

Solar Fuels and Electrocatalyst Testing Stations
(Autolab Potentiostat, Thermo Trace Ultra Gas Chomatograph, AM1.5 solar simulated light)

Location:  132 Nieuwland Science Hall
electrochem_suite

 

Potentiostat/Galvanostat with rotating disc electrode (RDE) and electrochemical impedance spectroscopy (EIS) capabilities

AM1.5 solar simulated light with a variety of spectral filters

In-line GC with automated gas sampling loop for produced gas analysis for extended stability testing

General and specialized electrochemical cells for photo and electrocatalysis studies

General electrochemical measurements

Performance and stability testing of electro and photoelectrocatalysts

Water splitting and carbon dioxide reduction catalysts