Abstract
A new phosphate, Ca9FeD(PO4)7, with a whitlockite-like structure was synthesized by treating Ca9Fe(PO4)7 with D2 at 820 K. Mossbauer spectroscopy showed that the oxidation state of Fe in Ca9FeD(PO4)7 is +2. Ca9FeD(PO4)7 was paramagnetic in a temperature range from 5 to 300 K with an effective magnetic moment of 4.97 μB per Fe2+ ion. The infrared spectrum of Ca9FeD(PO4)7 exhibited a broad absorption band due to an O−D stretching vibration at 2225 cm-1 in addition to bands assigned to PO4 groups. Ca9FeD(PO4)7 was stable under an Ar atmosphere up to 840 K. Above this temperature, it decomposed to a β-Ca3(PO4)2-like phase, Ca9.333Fe1.167(PO4)7, as well as β-Ca2P2O7 with releasing D2O and keeping the oxidation state of +2 for Fe. Ca9FeD(PO4)7 liberated D2O in air above ca. 720 K to produce Ca9Fe(PO4)7. Second-harmonic-generation signals, I2ω/I2ω(SiO2), in Ca9FeD(PO4)7 (ca. 0.15) were by a factor of ca. 17 less than ca. 2.5 in Ca9Fe(PO4)7. Rietveld analysis of time-of-flight neutron diffraction data for Ca9FeD(...
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