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Materials Analysis SEF

Featured Equipment

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Analytical techniques available include Auger spectroscopy, X-ray photoelectron spectroscopy, atomic force microscopy, and several kinds of thermal analysis. A wide array of spectrophotometric techniques, including UV-visible-near IR spectrophotometry, Fourier transform infrared spectroscopy and Raman spectroscopy are also available.

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 4111, 4137, 4139 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.

Kratos AXIS Ultra Imaging 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 20 mm.  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 lateral resolution in the tens of microns.  The sample is analyzed in an ultra high vacuum chamber.

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.

CMSE has two 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/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 available.

  4. Veeco/Digital Instruments Tipview SPM (LS)

    The Tipview is a small stage high-resolution microscope with E and A scanners, operable in Contact AFM and STM modes only, for use with either the Nanoscope IIIa or the Nanoscope IV controller.

 

Thermal Analysis:

Perkin Elmer Diamond Differential Scanning Calorimeter (TM)
Power Compenated Differential Scanning Calorimeter that can be used to find heat flow, melting temperature, and glass transition temperature.

Perkin Elmer Pyris 1 Differential Scanning Calorimeter (TM)
Power Compenated Differential Scanning Calorimeter that can be used to find heat flow, melting temperature, and glass transition temperature.

Mettler FP900 Thermosystem Hot stage (TM)
This is a temperature controlled microscope stage that can be used to observe the thermal behavior of a sample under a microscope. Operating temperature range from RT. to 375° Celsius.

Oxford Instruments Liquid Helium Cryostat (TM)
This is a dynamic liquid helium optical cryostat with automated temperature controller. The temperature can be controlled from 1.6° to 320°Kelvin. This cryostat was purchased for use in the FTIR for transmission or emission experiments but can be used in any of the optical measurement instrumentation.

Linkum Scientific FTIR 600 Freezing/Hot stage (TM)
Temperature controlled microscope stage that can be used on any of the lab's microscopes (Optical, FTIR, and Raman).   Temperature scanning as well as isothermal experiments can be performed. Capable of operating from (-170) °C to 600°C. This stage has a sealed sample chamber that allows a vacuum to be maintained around the sample or a particular gas can be flowed through the chamber.

Thin Film Instrumentation:

Qsense E4 Quartz Crystal Microbalance with Dissipation (TM)
The QCM-D is used to study molecular interactions and molecular adsorption to many different types of surfaces. Applications include proteins, lipids, polyelectrolytes, polymers and cells, bacteria interacting with surfaces or with previously bound molecular layers.The change in frequency and dissipation of an oscillating quartz crystal is measured while a sample is introduced to the electrode of an oscillating quartz crystal. A sample chamber is specifically designed to flow a sample across the crystal surface at a controlled temperature. Measurement cells available: Electrochemistry, Static, Humidity, Optical Window.

Sharon Vacuum Thermal Co-Evaporator (TM)
Single materials can be evaporated or the deposition can be controlled from two separate crystal monitor controllers allowing for CO-Evaporation from two sources (2 KVA and 4 KVA) simultaneously. Includes three filament positions and a cryo-pumped vacuum system with an interlocked ion gauge controller and automatic valve sequencing controls. Substrate stage is water- cooled and temperature monitored.

Tencor FLX 2320 Thin Film Stress Measurement System (TM)
Measures the changes in the radius of curvature of a substrate caused by deposition of a stressed thin film. The change in radius of curvature can be measured over time and as a function of temperature (LN2 Temp to 500 degrees Celsius).

KLA Tencor P-16 Surface Profilometer (TM)
Provides high precision surface topography measurements on a wide variety of substrates using a 2um radius diamond tipped stylus. Maximum sample size is 355 X 355 mm (14" X 14") and a maximum scan length of 60mm. 3d Mapping software is available.

KLA Tencor P-10 Surface Profilometer (TM)
Provides high precision surface topography measurements on a wide variety of substrates using a 2um radius diamond tipped stylus. Maximum sample size is 355 X 355 mm (14" X 14") and a maximum scan length of 60mm. 3d Mapping software is available.

Sopra Spectroscpic Elliposmeter(TM)
The Spectroscopic Ellipsometer measures the change in polarization over a wide spectral range (0.25 - 2.0 um). The change in polarization is typically used to investigate the dielectric properties of single or multiple layered thin films.

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. 

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 analysis spot is 100 um in diameter, 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.

Ultraviolet, Visible, and Infrared Spectroscopic Analysis:

Cary 5E UV-Vis-NIR Dual-Beam Spectrophotometer (TM)
Solid, liquids or pastes can be measured from 175nm to 3300nm. Available sampling accessories are: Absolute Specular Reflectance Accessory (7° incident angle), Automated Variable Angle Specular Reflectance Accessory (20° to 70° incident angles), Diffuse Reflectance Accessory (PTFE coated integrating sphere range 250nm to 2500nm), Praying Mantis Reflection Accessory (Diffuse reflectance of small samples, 3mm measurement area, Range of 220nm to 3300nm), and Automated Multi-Cuvette Sampling Accessory with Temperature Controller.

Cary 500i UV-Vis-NIR Dual-Beam Spectrophotometer (TM)
Solid, liquids or pastes can be measured from 175nm to 1750nm. Available sampling accessories are: Absolute Specular Reflectance Accessory (7° incident angle), Automated Variable Angle Specular Reflectance Accessory (20° to 70° incident angles), Diffuse Reflectance Accessory (PTFE coated integrating sphere range 250nm to 2500nm), Praying Mantis Reflection Accessory (Diffuse reflectance of small samples, 3mm measurement area, Range of 220nm to 3300nm), and Automated Multi-Cuvette Sampling Accessory with Temperature Controller.

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.

Nicolet Magna 860 Fourier Transform Infrared Spectrometer (TM)
This is an FTIR bench with an attached Spectra Tech Nic Plan FTIR Microscope. Accessories are available that allow for Transmission, Reflection or Attenuated Total Reflection (ATR) measurements. Sample emissions can also be measured.

Thermo Nicolet 6700 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.

Harrick Scientific PDC-32G Plasma Cleaner (TM)
RF Plasma cleaner has a quartz sample chamber and two gas flow controller. Currently configured to flow oxygen and air. Applications include: contaminant removal, activation, prebond preparation, surface chemistry modification and polymeric grafting & coating.

 

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