Scanning Electrochemical Microscopy (SECM)
Scanning Electrochemical Microscopy (SECM) is a four-electrode electrochemical imaging technique that permits spatial measurement of individual REDOX processes. The working electrode potential, EWE, and the tip potential, Etip, can be tuned independently, with EWE driving the electrochemical system, and Etip monitoring REDOX species. The INL SECM is home-built and modeled after the White Group’s (University of Utah). It is based upon the Burleigh Stepper Motors and National Instruments LabView softeware control.
Contact: Dr. Tedd Lister, Send E-mail
Microelectrode Array Microscope (MEAM)
This instrument is a homebuilt instrument that is based upon the INL SECM. As an alternative to the single microelectrode, the MEA-ECM uses an array of 100 independent microelectrodes arranged in a simple 10 x 10 array. Each of these microelectrodes is controlled and monitored via the Scribner Model 900 MMA. The working electrode is controlled by the Cypress Systems Omni-101 Potentiostat.
Contact: Dr.Tedd Lister, Send E-mail
Capillary Microelectrochemical Cell
Design modeled after Thomas Suter and Hans Bohni, courtesy of Prof. Rudolph Buccheitt (Ohio State University). The system operates about a three-electrode design, working electrode (WE), counter electrode (CE), and reference electrode (RE). The novelty is that all of the electrolyte volume is contained within a small capillary that is sealed above a site of interest on the specimen. This configuration allows site selective reaction between the electrolyte and the area of the specimen which it is in contact.
Contact: Dr. Patrick Pinhero, Send E-mail
Digital Instruments Multimode Nanoscope IIIa
The Digital Instruments (DI) Nanoscope is our workhorse SPM. Like the MI, it possesses STM, contact AFM, and Tapping-Mode AFM. Experiments can be set up in ambient air, solution, and inert atmospheres. We possess both electrochemical and electrical conductivity capabilities for this instrument. The DI instrument is much easier to use than the MI and it has a larger scan range (125 mm).
Contact: Ms. Tammy Trowbridge, Send E-mail, Dr. Patrick Pinhero, Send E-mail or Dr. Tedd Lister, Send E-mail
Molecular Imaging PicoSPM
The INL Molecular Imaging (MI) PicoSPM possesses a variety of capabilities. One can image surfaces with either scanning tunneling microscopy (STM), contact atomic force microscopy (AFM), non-contact AFM, magnetically-coupled (MAC mode) non-contact AFM, pulsed force modulated (PFM) non-contact AFM. For STM, there are three scan sizes available:1 mm, and 50 mm. For AFM scan sizes include 1 mm, 6 mm, and 30 mm. There are many variants that one can select a number of variants for each of the mentioned modes. The INL MI can image both adhesion and stiffness, lateral force, electrical conductivity, current-sensing, etc. We can operate the instrument in ambient air, in inert atmospheres, in controlled vapors, in solution, and in low vacuum. There are full temperature capabilities (-30C to 250C), an electrochemistry component, and additional techniques that we have developed at the INL.
Contact: Dr. Patrick Pinhero, Send E-mail, or Dr. Tedd Lister, Send E-mail
FEI Environmental Scanning Electron Microscope (ESEM)
The ESEM is a workhorse support instrument for the INL. It can operate in either high vacuum for routine microstructural analysis of conductive materials or in a low vacuum (environmental) mode for less conductive materials or vacuum sensitive biological organisms. The ESEM possesses secondary electron imaging (SEI), backscatter electron (BSE) imaging, and energy dispersive spectroscopy (EDS). It also has temperature stages (-10C to 1000C) and a mini load frame stage. Sample preparation via critical-point drying, carbon coating, or precious metals coatings are available.
Dr. Patrick Pinhero, Send E-mail
Perkin-Elmer Phi 5300 X-ray Photoelectron Spectrometer (XPS)
XPS is an ultra-high vacuum (UHV) technique that measures elemental composition of the outermost layers (~ 50 nm) of a material’s surface. In addition to elemental composition, XPS can help resolve the chemical environment surrounding the element by virtue of changes in its binding energy. UHV instruments typically operate at pressures of 2 x 10-10 Torr (or better). Our XPS is fitted with a dual anode (MgKa> & AlKa) excitation source and a single channel analyzer. It can be operated as in conventional XPS, angle-resolved XPS, and depth profile modes. The XPS has been recently upgraded with a RBD Enterprises acquisition system and fast-entry load-lock sample entry port. There is a multi-port (Ar+, He+, Ne+, Kr+) differentially-pumped ion gun for sample cleaning, depth-profiling, and ion scattering spectroscopy (ISS). ISS, or more precisely, low-energy ion scattering (LEIS), is a technique whereby the elemental composition of the outermost atomic layer can be assessed. The INL XPS also has a removable catalysis chamber/reaction chamber.
Contact: Dr. Patrick Pinhero, Send E-mail
Perkin-Elmer Phi 4300 Scanning Auger Microprobe (SAM)
The Phi 4300 SAM provides a more spatially resolved elemental composition than the XPS because it uses a focused electron gun as the excitation source. This allows the instrument to be operated as a scanning electron microscope (SEM) to image surfaces and pick out inhomogeneities. These inhomogeneities can then be chemically assayed with Auger electron spectroscopy (AES) to determine their elemental composition. AES is a secondary electron technique whereby the primary core electron is ionized by high energy (2 to 10 KV) electron irradiation. In order to quench this highly excited electronic state, a valence electron will ‘drop’ into the core of an element, and either an x-ray or electron (Auger) will be emitted to release excess internal energy. The energy of this Auger electron is resolved by a cylindrical mirror analyzer (CMA) to identify the atom from which it originated. Our SAM has been upgraded with RBD Enterprises acquisition system (AugerScan & AugerMap) and fast sample entry load lock. It also possesses a fracture chamber.
Contact: Dr. Patrick Pinhero, Send E-mail
First Ten Ångstroms Dynamic Contact Angle Instrument
The INL Contact Angle Measurement Instrument offers an easy-to-measure indication of the chemical bonding of the uppermost surface layers of a solid. This bonding determines wettability and adhesion, and also allows prediction of coating properties and detection of trace surface contaminants. Contact angles are an easily seen physical manifestation of the more fundamental concepts of surface energy and surface tension. In a theoretical approach, you can calculate surface energy values from contact angle data, or you can take an empirical approach and deal only with contact angles. Either approach may be more useful for your situation — the important concept is that contact angles are related to surface energy and tension.
Contact: Mr. Alan Wertsching, Send E-mail, or Dr. Patrick Pinhero, Send E-mail
EG&G PAR Scanning Reference Electrode Technique (SRET)
SRET is a scanning electrode technique that monitors variations in the micropotential gradients about localized elctroactive sites in solution. We modified the INL SRET with an optical system for better determination of probe displacement from the specimen surface. Our major use of the SRET was in our Biocorrosion project.
Contact: Dr. Patrick Pinhero, Send E-mail
PRP Electrochemical Noise (ECN) System
ECN is a potentially valuable technique for field implementation. The keys to ECN are that it is relatively inexpensive, fairly robust, and real time. The downside is that the signals, though simple to acquire, are fairly complex to analyze. At the INL, our goal is to take a commercial ECN instrument and software and apply it to systems of interest to the INL, as well as the entire DOE complex.
Contact: Mr. Ron Mizia, Send E-mail
- Contact:
- Patrick Pinhero, (208) 526-2285, Send E-mail