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Materials Analysis SEF

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Analytical techniques available include Auger spectroscopy, X-ray photoelectron spectroscopy, atomic force microscopy, Quartz Crystal Microbalance with Dissipation, Thermal Analysis techniques and Profilometry. A wide array of spectroscopy techniques, including UV-visible-near IR spectrophotometry, Fourier transform infrared spectroscopy, Raman spectroscopy.

Personnel

Elisabeth (Libby) L. Shaw, Research Specialist
Room 13-4149
Phone: (617) 253-5045
Fax: (617) 258-6478
E-mail: elshaw@mit.edu

Tim McClure, Project Technician
Room 13-4149
Phone: (617) 258-6470
Fax: (617) 258-6478
E-mail: mtim@mit.edu

Location:

Building 13, Rooms 4137, 4139, 4148 and 4151 (4th floor)

Instruments Available:

Please note the initials following each instrument name for specific contact.
TM = Tim McClure
LS = Libby Shaw

Surface Analysis:

Physical Electronics Model 700 Scanning Auger Nanoprobe (LS)
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 6 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.

CMSE's 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.

Physical Electronics Versaprobe II X-ray Photoelectron Spectrometer (LS)
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.

CMSE's 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.

Scanned Probe Microscopes (LS)
Scanned probe microscopy (SPM) 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.

CMSE has three SPM controllers and four SPMs which can be used together in various configurations, as follows:

  1. Veeco/Digital Instruments Nanoscope IIIa Scanned Probe Microscope Controller with Dimension 3000 SPM (LS)

    The Dimension 3000 is a large stage microscope operable in many SPM modes, with a vacuum chuck allowing mounting of full wafers for analysis.

  2. Veeco Metrology Nanoscope IV Scanned Probe Microscope Controller with Dimension 3100 SPM (LS)The Dimension 3100 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, NanoMan software, and Dimension 3100's XY closed loop scanner can be used together for nanomanipulation.

  3. Veeco Metrology Nanoscope V Scanned Probe Microscope Controller with Dimension 3100 SPM, Hybrid Scanner, and Electrical Characterization Application Modules (LS)

    The Dimension 3100 is a large stage microscope operable in many SPM modes, with a vacuum chuck allowing mounting of full wafers for analysis. The Hybrid scanner is closed-loop in X, Y and Z dimensions, permitting precise positional control for nanolithography and nanomanipulation. The Nanoscope V controller permits calibration of cantilever spring constant, high resolution force measurements, and very high digital image resolution. The electrical characterization application modules permit imaging sample capacitance and conductance on the nanoscale, in standard tapping and contact modes and in Torsional Resonance mode.

  4. Veeco/Digital Instruments MultiMode SPM (LS)

    The MultiMode is a small stage high-resolution microscope with vertical engage D scanner, operable in many SPM modes, for use with either the Nanoscope IIIa or the Nanoscope IV controller. Closed fluid cell and heat stages accessories are available for this microscope.

Thin Film Instrumentation:

Gaertner Scientific 3-Wavelength Variable Angle Ellipsometer (LS)
Ellipsometry is used to determine the thickness of thin films and to find the complex index of refraction (n & k) of materials, by analyzing the polarization of light reflected at an angle from a sample surface. CMSE's ellipsometer probes the sample with a single wavelength laser, with a wavelength choice of red (633 nm), blue (488 nm) or near-IR (830 nm). The analysis area is about 1 mm x 3 mm. The minimum measurable film thickness is a few Ångstroms with an accuracy of +/- 3 Å, and the maximum measurable thickness is about 10 µm.

Bruker DXT Stylus Profilometer (TM) 
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.

Sopra Spectroscopic Elliposmeter (TM) Used to characterize the optical properties of materials from 2um to 25um. The polarization and incident angles can varied depending on your sampling needs. Winnelli Data Analysis software is available for modeling the data.

Filmetrics Reflectometer (LS)
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.

CMSE's 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 two stages: a large-sample stage with a spot size on the order of 1 mm, and a microscope stage with a 100 um analysis spot size.

Quartz Crystal Microbalance with Dissipation, QCMD (TM)
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.

Vibrational Electronic and Emission Spectroscopy:

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.

Oriel Instaspec II UV-Vis Spectrograph with Photo Diode Array Detector (LS)
The Oriel's photodiode array permits spectral analysis of light transmitted through solid or liquid samples.  Either Xenon or a quartz halogen lamp can be installed as a source.  The detector has a spectral range from 180 nm to 1100 nm.

Thermo Fisher FTIR6700 Fourier Transform Infrared Spectrometer (TM)
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.

Thermo Fisher Continuum Fourier Transform Infrared Microscope (TM)
This is an FTIR microscope that is attached to the FTIR6700 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.

Kaiser Optical Hololab 5000R Raman Microscope (TM)
This is an optical microscope with attached laser and spectrometer. 785nm & 514.5nm Excitation are available.

Renishaw Invia Reflex Micro Raman (TM)
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.

Agilent 5100 DVD Inductively Coupled Plasma-Optical Emission Spectrometer (TM)
Used to quantify the elements in a sample. Typical concentrations of 1-100ppm. Radial or Axial view emission spectrometer. Autosampler.

Quantum Design Inc. Magnetic Property Measurement Systems (MPMS-5S, MPMS-XL and MPMS SQUID-VSM)
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 1000 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.
*For inquiries on this instrument, please contact Patrick Boisvert at pboisver@mit.edu.

Support Instrumentation (TM)
Optical Microscopes, Balances and a Plasma Cleaner.

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