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      Analysis of Fe nanoparticles using XPS measurements under d.c. or pulsed-voltage bias

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      Author(s)
      Süzer, Şefik
      Baer, D. R.
      Engelhard, M. H.
      Date
      2010
      Source Title
      Surface and Interface Analysis
      Print ISSN
      0142-2421
      Electronic ISSN
      1096-9918
      Volume
      42
      Issue
      6-7
      Pages
      859 - 862
      Language
      English
      Type
      Article
      Item Usage Stats
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      106
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      Abstract
      The impact of solution exposure on the charging properties of oxide coatings on Fe metal-core oxide-shell nanoparticles has been examined by sample biasing during XPS measurements. The Fe nanoparticles were suspended in relatively unreactive acetone and analyzed after particles containing solutions were deposited on SiO2/Si or Au substrates. The particle and substrate combinations were subjected to ±10V d.c. or ±5V a.c., biasing in the form of square wave (SQW) pulses. The samples experienced variable degrees of charging for which low-energy electrons at ∼1eV, 20 μA and low-energy Ar+ ions were used to minimize it. Application of d.c. bias and/or SQW pulses significantly influences the extent of charging, which is utilized to gather additional analytical information about the sample under investigation. This approach allows separation of otherwise overlapping peaks. Accordingly, the O1s peaks of the silicon oxide substrate, the iron oxide nanoparticles, and that of the casting solvent can be separated from each other. Similarly, the C1s peak belonging to the solvent can be separated from that of the adventitious carbon. The charging shifts of the iron nanoparticles are strongly influenced by the solvent to which the particles were exposed. Hence, acetone exhibited the largest shift, water the smallest, and methanol in between. Dynamical measurements performed by application of the voltage stress in the form of SQW pulses provides information about the time constants of the processes involved, which leads us to postulate that these charging properties we probe in these systems stem mainly from ionic movement(s).
      Keywords
      Casting from different solvents
      Fe nanoparticles
      XPS
      Adventitious carbon
      Charging property
      Charging shifts
      Different solvents
      Fe metal
      In-between
      Ionic movement
      Iron nanoparticles
      Iron oxide nanoparticle
      Low energy electrons
      Low-energy Ar
      Overlapping peaks
      Oxide coating
      Shell nanoparticles
      Silicon oxide substrates
      Square waves
      Time constants
      Voltage bias
      Voltage stress
      XPS measurements
      Acetone
      Ionization of liquids
      Iron oxides
      Methanol
      Protective coatings
      Silicon compounds
      Silicon oxides
      Solvents
      Substrates
      X ray photoelectron spectroscopy
      Nanoparticles
      Permalink
      http://hdl.handle.net/11693/28580
      Published Version (Please cite this version)
      http://dx.doi.org/10.1002/sia.3260
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      • Department of Chemistry 640
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