POLYTYPE IDENTIFICATION IN TRIOCTAHEDRAL 1:1 LAYER SILICATES USING ELECTRON DIFFRACTION WITH APPLICATION TO A CHRONSTEDTITE THAT WAS SYNTHESIZED USING METALLIC IRON-CLAY INTERACTIONS

The present study presents a generalized procedure to accurately identify trioctahedral 1:1 layer silicates. The reciprocal space (RS) sections were obtained by the precession method by “unwarping” frames that were recorded using diffractometers with area detectors or from electron diffraction tomography (EDT) patterns. Distributions of subfamily reflections along the reciprocal lattice rows [21l]* / [11l]* / [12l]* in (2hhlhex)* / (hhlhex)* / (h2hlhex)* RS planes were used to determine OD (Ordered — Disordered) subfamilies (Bailey’s groups A, B, C, D). The distributions along the [10l]* / [01l]* / [11l]* rows in the (h0lhex)* / (0klhex)* / (hhlhex) RS planes allow determination of the polytypes. The use of traditional identification diagrams for the determination of OD subfamilies and polytypes was generalized in order to identify monoclinic and orthorhombic MDO (Maximum Degree of Order) polytypes. In these polytypes, the distribution of characteristic reflections along rows is different in RS sections that are perpendicular and diagonal to the symmetry plane of the polytype. The identification diagram of non-MDO polytype 6T2 is also presented. The method was applied to the identification of single crystals of cronstedtite that were synthesized during interactions of Fe metal with a natural claystone during experiments over a temperature range of 90-60°C. Conical and pyramidal crystals with a maximum size of a few micrometers were studied using electron diffraction tomography (EDT). The following polytypes were identified: 1M, 2M1, an apparently ninetuple polytype that was interpreted as triclinic 3A (group A), 1T (group C), and disordered crystals of group D. The 1M polytype was the most abundant. Some 1M crystals were twinned by reticular merohedry with a 120° rotation along the chex axis as the twin operation. The 2M1 occurred as isolated crystals as well as in mixed crystals. Intergrown 1T and 1M polytypes of the C and A group, respectively, were identified in one mixed crystal. The possible stacking sequence and the 3A polytype identification diagram was presented and discussed. Example RS sections of all polytypes were identified and demonstrated.