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After dispersion in 1–0.5 M TiCl4 aqueous solutions and carefully drying, Na-montmorillonite showed a sharp X-ray powder diffraction (XRD) pattern. Such a pattern was obtained only when the TiCl4-treated montmorillonite was dried quickly in a stream of dry air without rinsing with water. If the sample was washed with water before drying or treated with dilute TiCl4 solutions (<0.05 M), only the broad diffraction pattern typical of montmorillonite was obtained. The use of TiOS04 instead of TiCl4 also resulted in a broad pattern. Most of the XRD peaks of the pattern were indexed on the basis of a monoclinic cell with a = 5.22(1) Å, b = 9.13(2) Å, c = 11.37(2) Å, and β = 93.7(1)°. The sharpening of the XRD peaks is probably caused by hydrogen bonded interlayer water molecules coordinated with the titanium ions, which restrict the relative orientation of the adjacent silicate layers, resulting in a highly crystalline product.

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