Materials Analysis and X-ray Facility (MAX)

PRIMARY CONTACTS SECONDARY CONTACT
Elizabeth (Libby) Shaw
Research Specialist
Office: 13-4149
Phone: (617) 253-5045
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Tim McClure
Project Technician
Office:: 13-4149
Phone: (617) 258-6470
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Charles Settens, Ph.D.
SEF Operations Manager
Office: 13-4013
Phone: (845) 430-2584
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Training available: PHI 700 Scanning Auger Electron Spectrometer

Auger Auger Photo

With a small electron beam diameter, AES is especially useful when investigating particles and small areas, less than 25 nm. The depth resolution of AES can provide an alternative when films are too thin for quantitative EDS analysis (see interaction volume diagram above). AES can produce 2D chemical mapping or depth profiling of all elements except H and He with 0.1 to 1 at. % sensitivity.

Features

  • High Spatial Resolution: ≥11nm minimum spot size
  • Surface Sensitive; top 5nm
  • Ar ion gun for sputter cleaning or depth profiling
  • Identification of all elements except H and He
  • 2D elemental distribution mapping
  • Portable transfer vessel to allow samples to be loaded without exposure to air
  • Liquid nitrogen cooled impact fracture stage for intergranular fracture surface analysis

Limitations

  • Minimal chemical state information
  • Insulators are difficult, but charge mitigation strategies are possible
  • Samples must be vacuum compatible
  • Detection limits of ~0.1% to 1% atomic

Libby Shaw, Research Specialist
Room 13-4137
Email This email address is being protected from spambots. You need JavaScript enabled to view it. for training

 

INSTRUMENTS

Physical Electronics Model 700 Scanning Auger Nanoprobe

A scanning Auger microscope can be thought of as a scanning electron microscope with a specialized electron energy analyzer attached. Auger electron spectroscopy permits elemental and sometimes chemical analysis with high depth resolution (about 3 nm), good elemental sensitivity (1.0 to 0.1 atomic percent) and high lateral resolution (minimum 11 nm). The spatial distribution of elements on a surface can be mapped. Changes in elemental composition with depth can be documented by recording surface composition while using an ion gun to gradually remove surface layers. The sample is analyzed in an ultra high vacuum chamber.

PHI Model 700 Nanoprobe has a field emission electron source for high lateral resolution; a floating voltage argon gun for depth profiling and sample neutralization; a portable transfer vessel so that processed samples can be loaded into the instrument without exposure to air; and a nitrogen-coolable impact fracture stage for in situ preparation of intergranular fracture surfaces for analysis.
Contact: Libby Shaw    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.        Instrument Location: 13-4137

Physical Electronics Versaprobe II X-ray Photoelectron Spectrometer
X-ray photoelectron spectroscopy (XPS, aka ESCA) permits elemental and chemical spectroscopic analysis of both conductive and insulating samples, with high depth resolution (10 nm or less), good elemental sensitivity (0.1 to 0.01 atomic percent), and lateral resolution down to 10 µm. Changes in elemental composition with depth (to a maximum depth of about 10 nm) can be documented nondestructively by recording surface composition while varying sample tilt relative to the analyzer (this technique is called angle-resolved depth profiling). Compositional changes with depth down to a few hundred nm can be observed by recording surface composition while using an ion gun to gradually remove surface layers. The spatial distribution of elements or chemistries on a surface can be mapped with a lateral resolution of down to ten microns. The sample is analyzed in an ultra high vacuum chamber.

PHI Versaprobe II XPS has a C60 cluster-ion gun as well as a floating voltage argon single-ion gun for depth profiling. The cluster-ion gun permits depth profiling softer materials which would be too damaged by single-ion bombardment. Other features of this XPS are a portable transfer vessel so that processed samples can be loaded into the XPS without exposure to air; an in situ heat/cold stage (-120C to 500C); and X-ray induced secondary electron imaging (SXI), which aids significantly in setting up for small area analysis.
Contact: Libby Shaw    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4137

Scanned Probe Microscopes
Scanned probe microscopy (SPM) or atomic force microscopy (AFM) uses a tiny mechanical probe to record sample surface topography and explore forces between the probe tip and sample surface on a very fine spatial scale, tracking the surface with nanoNewtons of force or less. Vertical resolution is in the sub-nanometer range, and lateral resolution is typically in the nanometer range (limited by the probe radius). Magnetic and electrostatic domains, hydrophilic/hydrophobic regions, and other variations in surface property can be mapped along with surface topography. Electrical characterization and force characterization on the nanoscale can also be performed.

MIT MRL has three SPM microscopes with various configurations:

  1. Bruker Dimension Icon XR SPM
    The Icon XR has many SPM modes including contact and PeakForce tapping mode with ScanAsyst, Magnetic Force Microscopy, Piezo Force Microscopy, conducting atomic force microscopy (AFM). There are also additional features such as electrical characterization from 80 fA to 1 uA with 10 nm spatial resolution, Kelvin Force Probe Microscopy with amplitude or frequency feedback, and pixel-by-pixel quantitative force characterization to probe material properties.
     
  2. Veeco Dimension 3100 SPM / Nanoscope V SPM controller
    The Dimension 3100 SPM is a large stage microscope operable in many SPM modes, with a vacuum chuck allowing mounting of full wafers for analysis.  The Nanoscope V Controller permits topographic imaging, phase contrast imaging, magnetic and electrostatic force imaging, and Kelvin force imaging.  It also can perform piezo force mapping and characterization of variations in conductance or capacitance through the sample to ground. Additional Multimode SPM is used for closed fluid cell and heat stage accessories.
     
  3. Veeco Dimension 3100 SPM / Nanoscope IV SPM controller
    The Dimension 3100 SPM is a large stage microscope operable in many SPM modes, with a vacuum chuck allowing mounting of full wafers for analysis.  The Nanoscope IV Controller permits topographic imaging, phase contrast imaging, magnetic and electrostatic force imaging, and Kelvin force imaging. Additional Multimode SPM is used for closed fluid cell and heat stage accessories.

Contact: Libby Shaw    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4137

Scattering-type Near-field Scanning Optical Microscopy (s-NSOM or s-SNOM)

s-SNOM system integrates a Bruker Innova AFM with a quantum cascade infrared lasers (mid-IR, 4-6 micron and near-IR, 8-10 micron wavelengths). S-SNOM can be used to overlay both sample topography and local optical conductivity at infrared frequencies with sub-10 nm spatial resolution depending on laser wavelength used​. Alternatively, s-SNOM can be useful for mapping identification of chemical composition based on molecular vibration, routinely acquiring amplitude and phase images for refractive or absorptive properties, or mapping plasmon- or phonon- resonant materials.

MRL contact: Charles Settens     Email: This email address is being protected from spambots. You need JavaScript enabled to view it.
Contact: Prof. Long Ju     Office 13-2005     E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.
Instrument Location: 13-2011 (Ju Group lab space)

 

THIN FILM INSTRUMENTATION

Bruker DXT Stylus Profilometer
Provides high precision surface metrology measurements on a wide variety of substrates using a 2um radius diamond tipped stylus Step height, Roughness or Curvature of your sample can be measured. 2D and 3D Measurement Range: 50 Angstroms to 1mm. Stress measurements.
Click here to read more on this instrument.
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.     Instrument Location: 13-4139

Filmetrics Reflectometer
Spectroscopic reflectometry is used to determine the thickness and complex index of refraction (n & k) of thin films, by comparing the spectral amplitude and periodicity of light reflected at normal incidence from a thin film surface with light reflected from a known reference sample, and fitting the result to a mathematical model based upon proposed values for the parameters thickness, n and k.

The reflectometer has been optimized to enhance the spectral yield in the near-IR, with a consequent spectral range from 480 to 1700 nm. The measurable film thickness range is from about 100 nm to 25 µm, and the accuracy is +/-10 Å or 0.4%, whichever is larger.

The reflectometer has a large-sample stage with a spot size on the order of 1 mm.
Contact: Libby Shaw     E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.    Instrument Location: 13-4151


Quartz Crystal Microbalance with Dissipation, QCMD

The QCM-D is used to study molecular interactions and surface science.

Based on a vibrating quartz crystal sensor (an acoustic resonator). Measurements are made based on changes in vibration frequency in response to reactions that occur on the sensor surface. The measurements provide answers about mass and structural changes at the nanoscale level.

Common applications include measurements on proteins, polymers, surfactants and cells onto surfaces in liquid.

Measurement Cells available: Flow, static, window, electrochemistry and humidity.
Click here to read more on this instrument.
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.   Instrument Location: 13-4148

 


Perkin Elmer Lambda 1050 UV/VIS/NIR Spectrophotometer
Used to measure the Transmittance, Reflection or absorbance of a sample. Measurement Range: 175nm to 3300nm. Integrating Sphere.
Click here to read more about his instrument.
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.    Instrument Location: 13-4139

Thermo Fisher Nicolet iS50 Fourier Transform Infrared Spectrometer
This is an FTIR bench with available detectors, beam splitters and sources to allow data collection in the near, mid and far IR. Accessories are available that allow for Transmission, Reflection or Attenuated Total Reflection (ATR) measurements.
Click here to read more on this instrument.
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.    Instrument Location: 13-4139

Thermo Fisher Continuum Fourier Transform Infrared Microscope
This is an FTIR microscope that is attached to the FTIRiS50 bench. An FTIR spectra can be collected from spot sizes down to 20um (Typical is 100um). Data can be collected in Transmission, Reflection, Emission or Attenuated Total Reflection mode. This microscope is capable of FTIR mapping and ATR mapping.
Click here to read more on Materials Analysis Instruments.
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.    Instrument Location: 13-4139

Renishaw Invia Reflex Micro Raman
Microscope based raman system with three laser excitation and spectrometer with CCD detector. Motorized stage and software allows mapping or imaging. Temperature controlled microscope stage. Automated polarization. Open Sample compartment. Photoluminescence. Low wavenumber gratings.
Click here to read more on this instrument.
Click here to download the SOP
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.    Instrument Location: 13-4139

Agilent 5100 DVD Inductively Coupled Plasma-Optical Emission Spectrometer
Used to quantify the elements in a sample. Typical concentrations of 1-100ppm. Radial or Axial view emission spectrometer. Autosampler.
Click here to read more on this instrument.
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.   Instrument Location: 13-4148

Quantum Design Inc. Magnetic Property Measurement System (MPMS-3)
This apparatus is capable of measuring magnetic moments in the range +/-2 emu to a resolution of 10-7 emu. Measurements may be obtained in the temperature range 1.8 to 400 K with magnetic fields from -7 Tesla to +7 Tesla. The system is fully automated, accepting flexible user-programmed parameters that allow for unattended operation day and night.
Click here to read more on this instrument.
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.   Instrument Location: 13-4148

Support Instrumentation
Optical Microscopes, Balances and a Plasma Cleaner.
Contact: Tim McClure    E-mail: This email address is being protected from spambots. You need JavaScript enabled to view it.

 

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