High temperature hydrothermal synthesis of rare-earth titanates: synthesis and structure of RE5Ti4O15(OH) (RE = La, Er), Sm3TiO5(OH)3, RE5Ti2O11(OH) (RE = Tm–Lu) and Ce2 Ti4O11

Fulle, Kyle; Sanjeewa, Liurukara D.; McMillen, Colin D.; Kolis, Joseph W.

doi:10.1039/c7dt04810f

Title: High temperature hydrothermal synthesis of rare-earth titanates: synthesis and structure of RE₅Ti₄O₁₅(OH) (RE = La, Er), Sm₃TiO₅(OH)₃, RE₅Ti₂O₁₁(OH) (RE = Tm–Lu) and Ce₂ Ti₄O₁₁

Journal Article · Wed May 02 00:00:00 EDT 2018 · Dalton Transactions

DOI:https://doi.org/10.1039/c7dt04810f· OSTI ID:1596442

Fulle, Kyle ^[1]; Sanjeewa, Liurukara D. ^[1];

^[1]; Kolis, Joseph W. ^[1]

Clemson Univ., SC (United States). Center for Optical Materials Science and Engineering Technologies (COMSET)

Reactions of rare-earth oxides with TiO₂ were performed in high temperature (650–700 °C) hydrothermal fluids. Two different mineralizer fluids were examined, 20 M KOH and 30 M CsF, and their respective products analyzed. When concentrated KOH fluids were used, single crystals of a variety of new OH^- containing species were isolated and structurally characterized: RE₅Ti₄O₁₅(OH) (RE = La, Er) I, Sm₃TiO₅(OH)₃II and RE₅Ti₂O₁₁(OH) (RE = Tm–Lu) III. La₅Ti₄O₁₅(OH) I crystallizes in the orthorhombic space group Pnnm with unit cell dimensions of a = 30.5152(12) Å, b = 5.5832(2) Å, c = 7.7590(3) Å and V = 1321.92(9) Å³, Z = 4. Sm₃TiO₅(OH)₃II crystallizes in the monoclinic space group P21/m with unit cell parameters of a = 5.6066(2) Å, b = 10.4622(4) Å, c = 6.1258(2) Å and β = 104.7390(10)°, V = 347.50(2) Å3, Z = 2. Lu5Ti2O11(OH) III crystallizes in the monoclinic space group C2/m with unit cell dimensions of a = 12.1252(9) Å, b = 5.8243(4) Å, c = 7.0407(5) Å, β = 106.939(3)° and V = 475.65(6) Å3, Z = 2. When concentrated fluoride solutions are used, mostly RE₂Ti₂O₇ type compounds were isolated in either cubic or monoclinic phases. In the case of cerium, Ce2Ti4O11IV was isolated that crystallizes in the monoclinic space group C2/c with unit cell parameters of a = 13.6875(7) Å, b = 5.0955(3) Å, c = 12.8592(7) Å, β = 108.964(2)° and V = 848.18(8) Å³, Z = 4. The synthesis, structural characterization, and supporting characterization are reported for all compounds. The work highlights the complementary nature of hydroxide and fluoride fluids in studying the reactivity of refractory oxides.

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Research Organization:: Clemson Univ., SC (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0014271

OSTI ID:: 1596442

Alternate ID(s):: OSTI ID: 1435657

Journal Information:: Dalton Transactions, Vol. 47, Issue 19; ISSN 1477-9226

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 4 works

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Hydrothermal
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CSD 1886581: Experimental Crystal Structure Determination Fulle, Kyle; Sanjeewa, Liurukara D.; McMillena, Colin D. https://doi.org/10.25505/fiz.icsd.cc21b4g0 The current record is supplemented by this dataset	dataset	January 2018
CSD 1886582: Experimental Crystal Structure Determination Fulle, Kyle; Sanjeewa, Liurukara D.; McMillena, Colin D. https://doi.org/10.25505/fiz.icsd.cc21b4h1 The current record is supplemented by this dataset	dataset	January 2018
CSD 1886583: Experimental Crystal Structure Determination Fulle, Kyle; Sanjeewa, Liurukara D.; McMillena, Colin D. https://doi.org/10.25505/fiz.icsd.cc21b4j2 The current record is supplemented by this dataset	dataset	January 2018
CSD 1886584: Experimental Crystal Structure Determination Fulle, Kyle; Sanjeewa, Liurukara D.; McMillena, Colin D. https://doi.org/10.25505/fiz.icsd.cc21b4k3 The current record is supplemented by this dataset	dataset	January 2018
CSD 1886585: Experimental Crystal Structure Determination Fulle, Kyle; Sanjeewa, Liurukara D.; McMillena, Colin D. https://doi.org/10.25505/fiz.icsd.cc21b4l4 The current record is supplemented by this dataset	dataset	January 2018

Title: High temperature hydrothermal synthesis of rare-earth titanates: synthesis and structure of RE5Ti4O15(OH) (RE = La, Er), Sm3TiO5(OH)3, RE5Ti2O11(OH) (RE = Tm–Lu) and Ce2 Ti4O11

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Title: High temperature hydrothermal synthesis of rare-earth titanates: synthesis and structure of RE₅Ti₄O₁₅(OH) (RE = La, Er), Sm₃TiO₅(OH)₃, RE₅Ti₂O₁₁(OH) (RE = Tm–Lu) and Ce₂ Ti₄O₁₁