HIGH PRESSURE BEHAVIOR OF FEOOH

Understanding the stability and properties of simple hydroxides at high pressures and temperatures offers an important first step toward quantifying more complex hydrogen-bearing compounds relevant to the Earth’s interior. We focus on iron-oxy-hydroxides because they may be an important Fe and water bearing component in the deep Earth. Goethite (α-FeOOH) transforms to a high-pressure phase, ε-FeOOH, which is isostructural with δ-AlOOH, a material which may transport hydrogen to the core-mantle boundary. Here we present XES spectroscopy data of powder samples of synthesized alpha-FeOOH, beta-FeOOH and gamma-FeOOH monitoring their electronic spin transition. The samples was loaded into a Beryllium gasket, where a 50 mm hole served as the sample chamber with 300 mm culet diamond paired with a beveled 150 mm diamond in a diamond-anvil cell (DAC) without a pressure transmitting medium. Pressure was determined using ruby fluorescence (Mao et al. 1978). Using the incident X-ray energy centered at 11.3 KeV from the Advanced Photon Source, beam line HPCAT 16-ID-D, we measured Fe K-β 13 emission to pressures greater than 73 GPa. For alpha-FeOOH, we saw a clear shift in the main peak to lower energy, and an increasingly diminishing K beta prime peak intensity, indicating the sample was undergoing an electronic spin transition. The K beta prime peak completely disappeared at a pressure greater than 73 GPa. Beta-FeOOH showed no evidence of the beginnings of a spin transition, while Gamma- FeOOH underwent an incomplete transition.