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Clay Minerals; September 2001; v. 36; no. 3; p. 381-387
© 2001 Mineralogical Society of Great Britain and Ireland
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Research Paper

HRTEM study of freeze-dried and untreated synthetic ferrihydrites: consequences of sample processing

C. GREFFIÉ1,*, M. AMOURIC2 and C. PARRON3

1 BRGM, Ressources Minérales, B.P. 6009, 45060 Orléans Cedex 02, 2 CRMCC, Campus de Luminy, 13288, Marseille, and 3 CEREGE, UMR CNRS 6635, B.P. 80, 13545 Aix en Provence Cedex 04, France

* E-mail: c.greffie{at}brgm.fr

(Received 20 December 1999; revised 15 November 2000)

Two-line ferrihydrite samples were synthesized following conventional procedure. Detailed characterizations of freeze-dried and untreated samples – prepared from direct inclusion of the fresh precipitates in hydrophilic resin – were made by high resolution transmission electron microscopy to investigate in detail their structural organization and to compare the two types of preparations.

Only highly disordered chain-like aggregates of 2–5 nm diameter size nano-particles were revealed within the untreated samples. Conversely, in freeze-dried samples, domains with different degrees of order were recognized, from poorly ordered 2-line ferrihydrite to 3-line ferrihydrite particle aggregates that revealed lattice fringes. Associated with these aggregates, a goethite phase with a modified crystal morphology was also observed.

These HRTEM observations revealed that freeze-drying techniques induce artifacts by disturbing ferrihydrite aggregates while direct inclusion in hydrophilic resin preserves the primary organization of such poorly ordered phases.

KEYWORDS: ferrihydrite, goethite, hydrophilic resin inclusions, Fe oxy-hydroxide, synthesis, transmission electron microscopy






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