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Corrosion Analysis


Materials and Chemistry Laboratory, Inc. (MCLinc) offers a unique combination of experience and instrumental capability to the field of corrosion analysis.  The value of these capabilities can best be recognized when studies are performed in order to obtain a fundamental understanding of corrosion mechanism under a variety of existing conditions with a view to formulating an efficient and cost effective control strategy.  Conduct of such corrosion studies requires experience and instrumentation capability in both physical and chemical analysis.

MCLinc experience dates back to the 1980’s when our investigators began corrosion study on cylinders containing depleted uranium hexafluoride.  During the past 20 years MCLinc scientists have investigated corrosion mechanisms for a variety of materials.  In 1998, MCLinc became a fully commercial facility.  As a private, employee-owned, small business, MCLinc offers this extensive experience in the solution of corrosion problems.

MCLinc’s 25,000 square-foot laboratory is equipped with instruments needed for the chemical analysis of corrosion products, corrosion films, and deposits.  Four large environmental chambers are available for simulating corrosive conditions.  Modern optical microscopy and scanning electron microscopy equipment is utilized to observe and characterize corrosion material and associated substrates and to define corrosive rates.  Capabilities of these instruments are summarized in a following table.

SEM analysis allows definitive evaluation of corrosion rates and provides significant information about the corrosion mechanism.  This technique includes elemental analysis of corrosion products and visualization of the location of different constituent elements.  SEM characterization of the corrosion products can be done either as cut pieces of the substrate material placed in the SEM directly or, more typically, pieces of the substrate prepared by metallographic techniques (embedding in epoxy, grinding and polishing).  After polishing, the substrates still have the coating and corrosion products intact and all parts of the corroding material can be imaged, measured, and elemental components identified by energy dispersive spectroscopy (EDS).  Images can be collected from all areas of the corroding part and converted to a digital image.  SEM magnification range is from 20x to 1,000,000x and elemental analysis is possible for all elements of the periodic table with atomic number ≥ boron.  Often SEM analysis identifies the impact on the corrosion of:  coating, coating thickness, the effect of pinholes in the coating, the presence of previously unknown materials, different corrosion rates in areas of the substrate, etc..

The ESEM (environmental scanning electron microscope) is a unique SEM instrument that allows the sample to be subjected to the dry, high-vacuum conditions normally present in SEM’s as well as low-pressure gas conditions (water vapor and other gases) at pressures up to 15 torr.  This allows the observation of any reaction between a substrate or its corrosion products with water vapor or other selected gases.

 
OM allows the observation and recording of the appearance of the corroded material at magnifications from 20x to 400x.  Observations of substrates that are three to five millimeters in diameter fall into this size range.  In addition to observation, digital photographic images of the observed material can be recorded.  Thickness measurements can be done on the substrate also, although SEM is probably better qualified to do this determination.

X-ray Photoelectron Spectrometry (XPS) can be used for identification of:  compound formation, oxidation states of constituents etc.  This is complementary to the elemental analysis capability of SEM instruments.  Ion milling of the sample surface can be done in order to evaluate material beneath the surface as well.

Materials and Chemistry Laboratory, Inc. (MCLinc) has the equipment and staff to successfully perform corrosion study.  MCLinc is a fully integrated laboratory that incorporates staff experienced in both physical and chemical analysis.  A list of several instruments used in previous corrosion studies and available at MCLinc follows:

   Instruments Applicable to Corrosion Studies

Instrument

         Capabilities

X-ray Photoelectron Spectrometer (XPS)

  • Surface analysis at 20-40Å
  • Chemical speciation
  • Depth profiling

Scanning Electron Microscope/

Electron Probe Microanalyses, SEM/EPA

  • Energy Dispersive X-ray Spectroscopy (EDS)
  • Wavelength Dispersive X-ray Spectrometry (WDS)
  • Sample composition and microstructure
  • Elemental analysis
  • Backscattered Electron Imaging (BEI) (distinguishes high atomic numbered elements)
  • Elemental mapping

Field Emission Scanning Electron Microscope (FESEM)

  • Energy Dispersive X-ray Spectroscopy (EDS)
  • Ultra high resolution microscopy identifies extremely small particles
  • 0.6 nanometer resolution

Environmental Scanning electron Microscopy (ESEM)

  • Operates at 20 TORR
  • Capable of EDS
  • Large sample holder
  • Heating and cooling stage

Transmission Electron Microscopy (TEM)

  • Small area electron diffraction of submicron crystalline phases
  • Chemistry of interfaces at high magnifications and ultra small particles (EDS)

X-ray Diffractometer (XRD)

  • Identifies crystalline phases
  • Can be used to determine phase concentrations
  • Determine crystallite sizes
  • Uses a zero diffractions sample mount

X-ray Fluorescence Spectroscopy (XRF)

  • Chemistry of sample
  • Can be used to identify elements in the parts per million range

Fourier Transform Infrared Spectroscopy

  • Monitor reactions in the various states


Special Expertise with Highly Corrosive Materials

MCLinc as a prior member of the K-25 (Gaseous Diffusion Plant) at Oak Ridge, Tennessee was involved in several corrosion studies.  For example, a constant threat to the enrichment facilities was the maintenance of the numerous cylinders containing depleted UF6.  Studies involved a) materials of construction exposed to destructive environments and b) analyzing the UF6 cylinder surfaces and associated leakage from the cylinder valves.  Since commercialization, this experience has proven valuable in investigations involving many types of highly corrosive environments.

 

Materials and Chemistry Laboratory, Inc.
East Tennessee Technology Park, Bldg. K-1006 • Oak Ridge, TN 37830-1702
Voice: (865) 576-4138 • FAX: (865) 576-8558
Contact:
Barry A. Stephenson
, President

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