Research Paper

Journal of Nanoparticle Research

, Volume 13, Issue 5, pp 1937-1952

First online:

Recovery of iron/iron oxide nanoparticles from solution: comparison of methods and their effects

  • James T. NurmiAffiliated withDivision of Environmental and Biomolecular Systems, Oregon Health & Science University
  • , Vaishnavi SarathyAffiliated withDivision of Environmental and Biomolecular Systems, Oregon Health & Science University
  • , Paul G. TratnyekAffiliated withDivision of Environmental and Biomolecular Systems, Oregon Health & Science University Email author 
  • , Donald R. BaerAffiliated withEnvironmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory Email author 
  • , James E. AmonetteAffiliated withFundamental and Computational Sciences Directorate, Pacific Northwest National Laboratory
  • , Abhi KarkamkarAffiliated withFundamental and Computational Sciences Directorate, Pacific Northwest National Laboratory

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Abstract

Most methods currently being used to recover Fe0-core/oxide-shell nanoparticles from solutions (including the solvents they are synthesized or stored in) are potentially problematic because they may alter the particle composition (e.g., depositing salts formed from solutes) or leave the particles prone to transformations during subsequent storage and handling (e.g., due to residual moisture). In this study, several methods for recovery of nanoparticles from aqueous solution were studied to determine how they affect the structure and reactivity of the recovered materials. Simple washing of the nanoparticles during vacuum filtration (i.e., “flash drying”) can leave up to ~17 wt% residual moisture. Modeling calculations suggest this moisture is mostly capillary or matric water held between particles and particle aggregates, which can be removed by drying for short periods at relative vapor pressures below 0.9. Flash drying followed by vacuum drying, all under N2, leaves no detectable residue from precipitation of solutes (detectable by X-ray photoelectron spectroscopy, XPS), no significant changes in overall particle composition or structure (determined by transmission electron microscopy, TEM), and negligible residual moisture (by thermogravimetric analysis, TGA). While this improved flash-drying protocol may be the preferred method for recovering nanoparticles for many purposes, we found that Fe0-core/oxide-shell nanoparticles still exhibit gradual aging during storage when characterized electrochemically with voltammetry.

Keywords

Recovery Flash drying Weight loss Colloids Thermogravimetric analysis Transmission electron microscopy X-ray diffraction X-ray photoelectron spectroscopy Linear sweep voltammetry