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Structural Characterization of Methanol Substituted Lanthanum Halides.

Timothy J Boyle¹, Leigh Anna M Ottley, Todd M Alam

¹Sandia National Laboratories, Advanced Materials Laboratory, 1001 University Boulevard, SE, Albuquerque, NM 87106.

Polyhedron

|June 2, 2010

Summary

This study explored alcohol solvation of lanthanum halides using methanol (MeOH) to reduce processing temperatures for LaBr(3) scintillators. Researchers successfully isolated various solvated lanthanum complexes, with concentration influencing the final structure.

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Preparation, Purification, and Characterization of Lanthanide Complexes for Use as Contrast Agents for Magnetic Resonance Imaging

Preparation, Purification, and Characterization of Lanthanide Complexes for Use as Contrast Agents for Magnetic Resonance Imaging

Published on: July 21, 2011

Area of Science:

Inorganic Chemistry
Materials Science
Coordination Chemistry

Background:

Lanthanum halide (LaX(3)) derivatives are crucial for producing LaBr(3) scintillators.
Lowering processing temperatures is key to efficient scintillator production.
Alcohol solvation offers a potential route to modify LaX(3) properties.

Purpose of the Study:

Investigate the alcohol solvation of lanthanum halide derivatives using methanol (MeOH).
Determine the effect of solvation on the structure and properties of LaX(3) compounds.
Explore methods to lower processing temperatures for LaBr(3) scintillator production.

Main Methods:

Dissolution of lanthanum halide precursors in methanol (MeOH) under various conditions (room temperature, reflux).
Isolation and characterization of solvated metal complexes using X-ray diffraction (XRD) and multinuclear NMR ((139)La).
Thermal analysis using thermogravimetric analysis (TGA) and differential thermal analysis (DTA) to assess de-solvation temperatures.

Main Results:

Successfully isolated mixed solvate monomeric [La(H(2)O)(7)(MeOH)(2)](Br)(3) and fully substituted [LaBr(3)(MeOH)(5)] complexes.
Identified a salt derivative {[LaBr(2.75)*5.25(MeOH)](+0.25) [LaBr(3.25)*4.75(MeOH)](-0.25)} where crystallization solution concentration dictated the structure.
Other LaX(3) derivatives, including [(MeOH)(4)(Cl)(2)La(micro-Cl)](2) and [La(MeOH)(9)](I)(3)*MeOH, were also isolated and characterized.
XRD analysis confirmed structural integrity for some compounds, while NMR indicated a lack of structural retention in MeOD.
TGA/DTA data showed slightly higher de-solvation temperatures for MeOH derivatives compared to hydrated counterparts.

Conclusions:

Alcohol solvation, specifically with methanol, can effectively modify lanthanum halide structures.
Crystallization conditions significantly influence the resulting solvated complex.
These findings contribute to understanding LaX(3) chemistry and offer insights for optimizing scintillator production processes.