TEM-assisted dynamic scanning force microscope imaging of (001) antigorite: Surfaces and steps on a modulated silicate

Palacios-Lidón, E.; Grauby, Olivier; Henry, Claude R.; Astier, Jean-Pierre; Barth, Clemens; Baronnet, Alain

doi:10.2138/am.2010.3219

Cited by 8 publications

(6 citation statements)

References 53 publications

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“…The large superstructure of antigorite along the [100] direction is a result of this repeating wave structure (Zussman 1954;Kunze 1956Kunze , 1958Kunze , 1961Uehara 1988). In this study, the supercell repeat-unit in antigorite is approximately 3.1 nm, which is determined by the selected-area electron diffraction (SAED) patterns (see HRTEM observation and EDS analysis) (Whittaker and Zussman 1956;Zussman et al 1957;Kunze 1961;Uehara and Shirozu 1985;Uehara 1988;Palacios-Lidon et al 2010).…”

Section: Starting Materialsmentioning

confidence: 91%

“…The structural unit of serpentine has a polar layer with a thickness of 0.72 nm, which is composed of one tetrahedral sheet and one octahedral sheet (Wicks and Whittaker 1975;Mellini 1982;Grobéty 2003;Palacios-Lidon et al 2010;Evans et al 2013). Lizardite and antigorite have similar theoretical formula of Mg 3 Si 2 O 5 (OH) 4 but with different extents and types of isomorphous substitution (e.g., lizardite is rich in Al and Fe, and antigorite is rich in Si) (Uehara and Shirozu 1985;O'Hanley and Dyar 1993).…”

Section: Transformation Mechanismmentioning

confidence: 99%

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Conversion of serpentine to smectite under hydrothermal condition: Implication for solid-state transformation

Zhu

et al. 2018

American Mineralogist

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Understanding clay mineral transformation is of fundamental importance to grasping phyllosilicate crystal chemistry and unraveling geochemical processes. In this study, hydrothermal experiments were conducted on lizardite and antigorite, to investigate the possibility of the transformation from serpentine to smectite, the effect of precursor minerals' structure on the transformation and the transformation mechanism involved. The reaction products were characterized using XRD, TG, HRTEM, and 27 Al MAS NMR. The results show that both lizardite and antigorite can be converted to smectite, but such conversion is much more difficult than that of kaolinite group minerals. The successful transformation is mainly evidenced by the occurrence of the characteristic (001) reflection of smectite at 1.2-1.3 nm in the XRD patterns and smectite layers with a thickness of 1.2-1.3 nm in HRTEM images of hydrothermal products as well as the dehydroxylation of the newly formed smectite at a higher temperature in comparison to that of the starting minerals. The difficulty for the transformation of serpentine to smectite may be due to the lack of enough available Al in the reaction system, in which the substitution of Al 3+ for Si 4+ in the neo-formed tetrahedral sheet is critical to control the size matching between the neo-formed tetrahedral sheet and octahedral sheet in starting minerals. Since the neighboring layers in antigorite are linked by the strong Si-O covalent bonds, the transformation only takes place at the edges of an antigorite layer rather than the whole layer, and the neo-formed smectite is non-swelling due to the inheritance of such Si-O covalent bonds. The conversion of lizardite to smectite is more feasible than that of antigorite, accompanied by exfoliation. This leads to a prominent decrease of the particle size in the hydrothermal products and the number of phyllosilicate layers contained therein. Two dominant pathways were observed for the transformation of lizardite and antigorite into smectite, i.e., conversion of one serpentine layer to one smectite layer via attachment of Si-O tetrahedra onto the octahedral sheet surface of the starting minerals and two adjacent serpentine layers merging into one smectite layer. In the case of the latter, dissolution of octahedra and inversion of tetrahedral sheets took place during the transformation. Besides these two dominant pathways, precipitation and epitaxial growth of smectite were also observed in the cases of lizardite and antigorite, respectively. The present study suggests that solid-state transformation is the main mechanism for conversion of serpentine minerals to smectite, similar to the transformation of kaolinite group minerals to beidellite.

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Section: Starting Materialsmentioning

confidence: 91%

Section: Transformation Mechanismmentioning

confidence: 99%

Conversion of serpentine to smectite under hydrothermal condition: Implication for solid-state transformation

Zhu

et al. 2018

American Mineralogist

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“…Some pertinent examples include diamond,115 and binary oxides, such as MgO (001)110 and bulk α‐Al 2 O 3 (0001) 111, 116. There has also been recent progress in imaging polar oxides, such as ZnO (0001),113, 117 and minerals, such as mica,112, 118 antigorite,114 and calcite (10–14) 119…”

Section: Non‐contact Atomic Force Microscopymentioning

confidence: 99%

Section: Non‐contact Atomic Force Microscopymentioning

confidence: 99%

Recent Trends in Surface Characterization and Chemistry with High‐Resolution Scanning Force Methods

et al. 2010

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The current status and future prospects of non-contact atomic force microscopy (nc-AFM) and Kelvin probe force microscopy (KPFM) for studying insulating surfaces and thin insulating films in high resolution are discussed. The rapid development of these techniques and their use in combination with other scanning probe microscopy methods over the last few years has made them increasingly relevant for studying, controlling, and functionalizing the surfaces of many key materials. After introducing the instruments and the basic terminology associated with them, state-of-the-art experimental and theoretical studies of insulating surfaces and thin films are discussed, with specific focus on defects, atomic and molecular adsorbates, doping, and metallic nanoclusters. The latest achievements in atomic site-specific force spectroscopy and the identification of defects by crystal doping, work function, and surface charge imaging are reviewed and recent progress being made in high-resolution imaging in air and liquids is detailed. Finally, some of the key challenges for the future development of the considered fields are identified.

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“…These range from biomineralisation [17,18], to rock-forming silicates such as feldspars [11,19,20], natural and synthetic garnets (e.g., [21,22], or minerals of secondary origin such as phosphates and phyllosilicates [23][24][25][26]. Rare materials such as carbonado diamonds and meteorites have also been addressed (e.g., [27][28][29][30][31][32]).…”

Section: Research Topics Addressed By Integrated Fib-sem and Tem Micrmentioning

confidence: 99%

Focused Ion Beam and Advanced Electron Microscopy for Minerals: Insights and Outlook from Bismuth Sulphosalts

et al. 2016

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This paper comprises a review of the rapidly expanding application of nanoscale mineral characterization methodology to the study of ore deposits. Utilising bismuth sulphosalt minerals from a reaction front in a skarn assemblage as an example, we illustrate how a complex problem in ore petrology, can be approached at scales down to that of single atoms. We demonstrate the interpretive opportunities that can be realised by doing this for other minerals within their petrogenetic contexts. From an area defined as Au-rich within a sulphosalt-sulphide assemblage, and using samples prepared on a Focused Ion Beam-Scanning Electron Microscopy (SEM) platform, we identify mineral species and trace the evolution of their intergrowths down to the atomic scale. Our approach progresses from a petrographic and trace element study of a larger polished block, to high-resolution Transmission Electron Microscopy (TEM) and High Angle Annular Dark Field (HAADF) Scanning-TEM (STEM) studies. Lattice-scale heterogeneity imaged in HAADF STEM mode is expressed by changes in composition of unit cell slabs followed by nanoparticle formation and their growth into "veins". We report a progressive transition from sulphosalt species which host lattice-bound Au (neyite, lillianite homologues; Pb-Bi-sulphosalts), to those that cannot accept Au (aikinite). This transition acts as a crystal structural barrier for Au. Fine particles of native gold track this progression over the scale of several hundred microns, leading to Au enrichment at the reaction front defined by an increase in the Cu gradient (several wt %), and abrupt changes in sulphosalt speciation from Pb-Bi-sulphosalts to aikinite. Atom-scale resolution imaging in HAADF STEM mode allows for the direct visualisation of the three component slabs in the neyite crystal structure, one of the largest and complex sulphosalts of boxwork-type. We show for the first time the presence of aikinite nanoparticles a few nanometres in size, occurring on distinct (111) PbS slabs in the neyite. This directly explains the non-stoichiometry of this phase, particularly with respect to Cu. Such non-stoichiometry is discussed elsewhere as defining distinct mineral species. The interplay between modular crystal structures and trace element behaviour, as discussed here for Au and Cu, has applications for other mineral systems. These include the incorporation and release of critical metals in sulphides, heavy elements (U, Pb, W) in iron oxides, the distribution of rare earth elements (REE), Y, and chalcophile elements (Mo, As) in calcic garnets, and the identification of nanometre-sized particles containing daughter products of radioactive decay in ores, concentrates, and tailings.

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TEM-assisted dynamic scanning force microscope imaging of (001) antigorite: Surfaces and steps on a modulated silicate

Cited by 8 publications

References 53 publications

Conversion of serpentine to smectite under hydrothermal condition: Implication for solid-state transformation

Conversion of serpentine to smectite under hydrothermal condition: Implication for solid-state transformation

Recent Trends in Surface Characterization and Chemistry with High‐Resolution Scanning Force Methods

Focused Ion Beam and Advanced Electron Microscopy for Minerals: Insights and Outlook from Bismuth Sulphosalts

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