High Resolution Microprobe XPS

The Physical Electronics Instruments (PHI) Quantum 2000 X-ray photoelectron spectrometer (XPS) is a unique system that uses a focused monochromatic aluminum K X-ray beam that can be varied in size from as small as 10 μm in diameter to approximately 200 μm. The beam can be rastered over larger areas (about 0.5 mm2).

The PHI Quantum 2000 XPS features:

  • A focused X-ray beam (10 μm to 200 μm)
  • Beam raster capability to millimeter sizes
  • Optical- (charge-coupled diode camera) and X-ray-generated electron images (scanned X-ray image-SXI) to select areas of analysis
  • A special specimen holder for angle-resolved analysis (non-destructive depth profiles)
  • Mapping capability
  • A sputter gun (Model 11-066) for specimen cleaning and depth profiles (allows sputter rates up to approximately 50 nm/min)
  • Sample rotation to allow "Zalar" rotation during sputtering
  • The ability to set up multi-sample automated analysis (overnight data collection)
  • A charge neutralization system that uses both low-energy ions and low-energy electrons
  • Compatibility with the EMSL Sample Transfer System
  • A large platen size for either "large" single or multiple samples.

Performance Specifications

Performance conditions of the PHI Quantum 2000 XPS depend on operation mode; however, the following are characteristic of the instrument:

Beam Size: 20μm (4 watts) measured for Ag 3d 5/2
Energy Resolution High Medium Low
0.55 eV 0.7 eV 1 eV
Counts per second (cps) 15,000 cps 40,000 cps 70,000 cps

The best energy resolution achieved is approximately 0.45 eV. In the high-power mode at approximately 0.8 eV resolution, a count rate for the Ag 3d 5/2 photopeak of over 106 cps can be achieved.

Systems Configuration and Operational Overview

Sample Prep and Handling

This XPS is equipped to handle both the standard PHI Quantum 2000 holder and the EMSL sample platens. The standard PHI holder is approximately 3-inch × 3-inch square. Almost any vacuum-compatible sample that fits within the x-y dimensions of the holder and is less than 0.5-inch thick can be analyzed. Samples can be solid or powder, conducting or insulating.

The EMSL sample platen can hold samples up to 1 inch in diameter, although smaller samples are preferred. This holder interconnects with other parts of the EMSL Sample Transfer System and allows samples to be prepared and altered in several unique ways, including by electrochemical and liquid exposure, plasma treatment, coating deposition, optical exposure, and processing by heating and cooling.

The laboratory where the instrument is housed is equipped with a variety of ways to cut, polish, and clean samples prior to analysis or experiment. All work with this instrument must be performed in compliance with EMSL practices and permits.

PHI Quantum 2000 Scanning ESCA Microprobe

Analyzer and Optics
Spherical Capacitor Energy Analyzer
Mean Diameter 279.4 mm (11.0 in.)
Input Slit 4 x 10 mm
Scan Range 0 to 3200 eV
Detector
Type MultiChannel Detector
Number of Channels 16
Input Bias 0 to 200 V
Multiplier Voltage 500 to 2400 V
X-ray Generation
The PHI Quantum 2000 XPS is equipped with a quartz crystal monochromator and a scanning electron source that excites the aluminum anode to produce a focused X-ray beam.
Monochromator
Diameter of Rowland Circle 200 mm
Crystals Quartz (100) crystals on an ellipsoidal substrate
Electron Gun
Filament material LaB6
Lenses Electrostatic condenser, magnetic objective
Selection of electron beam diameter Variable from 5 μm to 100 μm
Large area 100 w, 1500 μm × 200 μm
Ion Sputter Gun and Gun Control
Beam Voltage Variable, 1 kV to 5 kV
Maximum Beam Current > 5 μA at 5 kV
Minimum Beam Diameter 150 μm at 5 kV
Beam Raster Size Center of raster pattern can be fixed at the focal point or varied about the focal point
Fixed Center Position At the focal point; raster up to ± 1.5 mm in x and y.
Variable Center Position Center can be varied by ± 0.7 mm about the focal point
Neutral Suppression 5-degree bend between the condenser and objective lenses; electrically adjustable
Source Type Argon
Leak Valve Integral; computer controlled
Pressure (In Operation) < 5 × 10-8 Torr in chamber, with differential pumping
Specimen Dimensions
x and y Up to 7.5-cm square or 100-mm diameter
z Up to 2.5-cm thick

Instrument ID:
1023
Availability: 10 hours a day, 5 days a week

Custodians

Publications

The ability to tune the atomic-scale structural and chemical ordering in nanoalloy catalysts is essential for achieving the ultimate goal of high...
This paper describes the results of an investigation of the synthesis of PtIrCo nanoparticles (2&ndash;3 nm) for electrocatalytic oxygen...
The ability to control the nanoscale size, composition, phase, and facet of multimetallic catalysts is important for advancing the design and...
The heterogeneous reduction of UVI to UIV by ferrous iron is a potentially key process influencing the fate and transport of U in the environment....
Nanostructured carbon (ns-C) films fabricated by stabilization and pyrolysis of di-block copolymers are of interest for a variety of electrical/...
Laser Raman spectroscopy and x-ray photoelectron spectroscopy were used to study the evolution of composition of oxide films in the presence of...
The ability to harness the metal-metal and metal-oxygen coordination structures of nanoalloy catalysts is critical for catalyzing the oxygen...
A simple method for creating self-assembled nanostructures using a single polymer system is reported. When spin-coated polystyrene thin films were...
This work was conducted to clarify the influence of the type of metal and support on the sulfur tolerance and carbon resistance of supported noble...
The mechanism involved in the photochemical immobilization of poly(4-vinylphenol) (PVP) thin films was investigated. The films were fabricated by a...
This report demonstrates a molecule&ndash;solid duality concept for nanoscale control of size, shape and alloying by showing novel evolution of...
Metal and metal oxide nanoparticles supported on high surface area materials are widely used in industry for fuel and chemical production and for...
In this study, we cultivated from subsurface sediments an anaerobic Clostridia 25 consortium that was composed of a fermentative Fe-reducer...
In this report we show that the size, shape, and composition of pre-synthesized metal nanoparticles can be engineered through exploiting concurrent...
Theoretically predicted effect of odd-even pattern of electron pairing on behavior of gold clusters in polyaniline/AuN (N = 0 to 8) has been...
This report describes a novel strategy of chromium-assisted shape control in the synthesis of platinum nanocubes with high monodispersity. The use of...
Under precisely controlled conditions, atomic gold electrodes with even or odd number of Au atoms per polyaniline repeat unit (Pt/PANI/AuN for 0 <...
The formation of water-induced cobalt oxides by re-oxidizing the metallic cobalt in the pre-reduced 10% Co/CeO2-ZrO2 catalyst was verified by in-situ...
The exploration of the magnetic properties of bimetallic alloy nanoparticles for various technological applications requires the ability to control...
The design and preparation of active and robust bimetallic catalysts require the understanding of the nanoscale alloying and phase-segregation...
Alloying palladium (Pd) with other transition metals at the nanoscale has become an important pathway for preparation of low-cost, highly-active and...
Electrochemically active LiMnPO4 nanoplates have been synthesized via novel single step solid state reaction in molten hydrocarbon. The LiMnPO4...
Plyaniline (PANI) has been shown to be an effective matrix for hosting metal nanoclusters. In the case of gold, the tetrachloroaurate anion (AuCl...
Here we report a nanoparticle label based on apoferritin nanovehicle loaded internally with markers for sensitive electrochemical DNA detection. The...
While transition metal-doped ferrite nanoparticles constitute an important class of soft magnetic nanomaterials with spinel structures, the ability...
How the composition of nanoscale surface oxides formed on complex metal alloys affects their passive state is a problem of great interest both from...
We report a flow injection amperometric choline biosensors based on the electrostatic assembly of an enzyme of choline oxidase (ChO) and a bi-enzyme...
In this article, we reported a spin successive ionic layer adsorption and reaction (SILAR) method for the first time. ZnS thin films were deposited...
Abstract Non-invasive biomonitoring approaches are being developed using reliable portable analytical systems to quantify dosimetry utilizing readily...
Raman microprobe spectroscopy was applied in studies of high-temperature air oxidation of a ferritic alloy (HT-9) in the absence and presence of...
Nanoporous, high-surface area films of TiO2 are synthesized by reactive ballistic deposition of titanium metal in an oxygen ambient. Auger electron...
This report describes findings of the correlation between the atomic scale structure and the electrocatalytic performance of nanoengineered PtNiFe/C...
A prototype high throughput operando reactor, that integrates FT-IR imaging for rapid reaction product analysis and parallel Raman imaging for...
A novel electrochemical immunosensor for the detection of tumor necrosis factor-alpha (TNF-a) based on poly(guanine)-functionalized silica...
Colloidal carbon spheres have been prepared from aqueous alpha-, beta-, and gamma-cyclodextrin (CD) solutions in closed systems under hydrothermal...
Surface and interface properties are important in controlling the yield and efficiency of the photochemically initiated immobilization. Using a...
The ability to use cellulosic biomass as feedstock for the production of fuels and chemicals currently derived from petroleum depends critically on...
High quality doped zinc oxide and mixed transition metal spinel oxide films have been deposited by means of sputter deposition from metal and metal...
Black carbon (BC) is a quantitatively important C pool in the global carbon cycle due to its relative recalcitrance against decay compared with other...
Phosphate-based mesoporous TiO2 materials were prepared by surfactant-directed method using an alkylphosphate surfactant, which produced a mesoporous...
The intensities of X-Ray absorption peaks at core-level edges are considered in terms of Russell-Saunders multiplets. The contributions of different...
The silicified L3-poly(N-sopropylacrylamide)/hydroxyapatite nanocomposites by the integration of thermosensitive polymer and heterogenious continuity...
A prototype operando high throughput (OHT) reactor designed and built for catalyst screening and characterization combines Fourier transform infrared...
Multiwall carbon nanotubes (MWNTs) form spontaneously upon graphitization of organic precursors bound to the internal surfaces of a high porosity...
The photodecomposition of acetone and butanone were examined on the (110) surface of rutile TiO2 using temperature programmed desorption (TPD) and...
The B9- cluster was found previously to be an unprecedented molecular wheel containing an octacoordinate planar boron with D8h symmetry in a combined...
Upcoming regulations regarding diesel engine emissions require substantial reduction in particulate matter and nitrogen oxides through aftertreatment...
Ag-doped mesoporous titanium oxide was prepared using non-ionic surfactants and easily handled titanium precursors, under mild reaction conditions....
Laser Raman spectroscopy was evaluated as a tool for studying fuel-cladding chemical interactions at elevated temperatures. Materials and conditions...
Many nanoporous Si structures, including those formed by common electrochemical etching procedures, produce a uniformly etch nanoporous surface. If...
The effect of nitrogen additives like urea, guanidine carbonate and melamine formaldehyde on the flame retardant efficacy of tributyl phosphate (TBP...
A novel prototype high throughput operando (OHT) reactor designed and built for catalyst screening and characterization is presented in this article...
Silver hollandite, Ag1.8Mn8O16, has been synthesized by ion exchange of cryptomelane in AgNO3 melt. Compared to the previously described synthesis...
Reactivity of adsorbates with titania is typically influenced by the presence of surface oxygen vacancy defects. For alcohols, it is well-established...
A completely "green" synthetic approach has been developed for the reduction and stabilization of Pt nanoparticles followed by self-...
The amount of electronic charge transferred between gold particles and polyaniline depends not only on the electron affinity of the two materials but...
Joints prepared using a silver-copper oxide based reactive air brazing (RAB) technique is known to experience a significant decrease in joint...
Core samples taken from a zero-valent iron permeable reactive barrier (ZVI PRB) at Cornhusker Army Ammunition Plant, Nebraska, were analyzed for...
A magnetic beads-based bioelectrochemical magnetic immunosensor was developed for the fast and sensitive determination of the trichloropyridinol (TCP...
Polyaniline forms a strong complex with chloroaurate at the protonated imine sites. Here we report on electrochemical procedure that allows...
The photodecomposition of acetone and butanone were examined on the (110) surface of rutile TiO2 using temperature programmed desorption (TPD) and...
Hydrogen bubbles trapped around lithographically formed etch pits on silicon single crystal surfaces were used to guide the formation of patterned...
Ab initio, fully relativistic four component theory was used to determine atomic and interatomic many-body effects for the 4f X-ray photoelectron...
A novel electrochemical immuno-biosensor based on poly(guanine)-functionalized silica nanoparticle labels and mediator-generated catalytic reaction...
The ability to regulate how molecular chirality of enantiomeric amino acids operates in biological systems constitutes the basis of drug design for...
The objectives of this study were to quantify the relative importance of either biotic or abiotic oxidation of biomass-derived black carbon (BC) and...
The aim of this work was to investigate changes in molecular form and surface charge of black carbon (BC) due to longtermnatural oxidation and to...
W have introduced template-synthesized metal phosphate nanoparticle labels for electrochemical immunoassay. Such use of an apoferritin template...
Black carbon (BC) may play an important role in the global C budget, due to its potential to act as a significant removal (sink) of atmospheric CO2....
This communication describes a novel method for detecting of matrix metalloproteinase-7 activity using a peptide substrate labeled with a ferrocene...
Uniform Au-Ag alloy nanoparticles have been synthesized on cellulose nanocrystal (CNXL) by co-reduction method of corresponding metal ions. CNXL that...

Quick Specs

    • Focused X-ray beam of 10 μm to 200 μm
    • Multi-sample automated analysis
    • Optimal energy resolution of 0.45 eV
    • Accomodates samples 7.5-cm thick, 100-mm diameter, and 2.5-cm wide

Science Highlights

Posted: Tuesday, September 13, 2016 - 14:07
The Science Sodium-ion batteries are an attractive alternative to lithium-ion batteries due to their high efficiency and low cost, but development...
Posted: Thursday, March 10, 2016 - 08:47
An international research team created a composite of a metal-organic framework, or MOF, and a helper molecule that efficiently separates oxygen...
Posted: Tuesday, January 13, 2015 - 09:06
The Science Lithium (Li) metal has long been considered one of the most attractive anode materials, but large-scale application of high-energy...
Posted: Tuesday, April 15, 2014 - 17:00
Scientists at EMSL and Pacific Northwest National Laboratory are studying energy storage devices to make them last longer and be able to be...

Projects

Zeolites are microporous aluminosilicate materials with a wide range of applications including catalysis, water purification, agriculture, and...
The aim of this proposal is to build upon our initial success in the exploration of the 3-D location and distribution of the Al and Si atoms in...
This proposal aims to provide molecular insight into elementary reaction steps and their kinetics in condensed phases at an atomic and molecular...
Biomass burning aerosols (BBA) are one of the most ubiquitous organic aerosol types with a source strength on the same order of magnitude as fossil...
Three related research programs at PNNL focus on developing bioinspired electrocatalysts for energy storage, energy production, or carbon fixation...