A humidity-controlled precipitation technique enabling discovery of Rb3(H1.5PO4)2

Sheel Sanghvi; Sossina M. Haile

doi:10.1016/j.jssc.2020.121951

A humidity-controlled precipitation technique enabling discovery of Rb₃(H_1.5PO₄)₂

Sheel Sanghvi, Sossina M. Haile^*

^*Corresponding author for this work

Materials Science and Engineering

Research output: Contribution to journal › Article › peer-review

2 Scopus citations

Abstract

The previously unknown compound Rb₃(H_1.5PO₄)₂ is successfully synthesized here using a newly developed variant of aqueous precipitation crystal growth. The approach exploits the phenomenon of boiling point elevation in concentrated solutions. Crystals of the title compound were obtained upon heating a stoichiometric solution from 110 to 150 °C under a high steam partial pressure of 0.83 atm. Single crystal X-ray diffraction studies revealed Rb₃(H_1.5PO₄)₂ crystallizes in space group C2/m and is isostructural to Cs₃(H_1.5PO₄)₂. As evidenced by thermal analysis, Rb₃(H_1.5PO₄)₂ does not undergo a phase transition to a trigonal superprotonic phase upon heating. Even under a steam partial pressure of 0.82 atm, under which dehydration is suppressed to a temperature of 263 °C, no polymorphic transition is detected. The behavior parallels that of Cs₃(H_1.5PO₄)₂ and contrasts that of several structurally and chemically similar selenate compounds. The crystal growth approach developed here may prove particularly useful for obtaining water soluble compounds which are thermodynamically or kinetically disfavored at temperatures close to ambient.

Original language	English (US)
Article number	121951
Journal	Journal of Solid State Chemistry
Volume	296
DOIs	https://doi.org/10.1016/j.jssc.2020.121951
State	Published - Apr 2021

Funding

Financial support has been provided by National Science Foundation ( DMR 1807234 ). SCXRD experiments made use of the Integrated Molecular Structure Education and Research Center (IMSERC) at Northwestern University , which has received support from SHyNE, the State of Illinois and International Institute for Nanotechnology (IIN) . The authors thank Charlotte Stern for single crystal data collection. Financial support has been provided by National Science Foundation (DMR 1807234). SCXRD experiments made use of the Integrated Molecular Structure Education and Research Center (IMSERC) at Northwestern University, which has received support from SHyNE, the State of Illinois and International Institute for Nanotechnology (IIN). The authors thank Charlotte Stern for single crystal data collection.

Keywords

Crystal Growth
Cs(HPO)
CsH(SeO)
Humidity
Precipitation
Solid Acid

ASJC Scopus subject areas

Electronic, Optical and Magnetic Materials
Ceramics and Composites
Condensed Matter Physics
Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/j.jssc.2020.121951

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title = "A humidity-controlled precipitation technique enabling discovery of Rb3(H1.5PO4)2",

abstract = "The previously unknown compound Rb3(H1.5PO4)2 is successfully synthesized here using a newly developed variant of aqueous precipitation crystal growth. The approach exploits the phenomenon of boiling point elevation in concentrated solutions. Crystals of the title compound were obtained upon heating a stoichiometric solution from 110 to 150 °C under a high steam partial pressure of 0.83 atm. Single crystal X-ray diffraction studies revealed Rb3(H1.5PO4)2 crystallizes in space group C2/m and is isostructural to Cs3(H1.5PO4)2. As evidenced by thermal analysis, Rb3(H1.5PO4)2 does not undergo a phase transition to a trigonal superprotonic phase upon heating. Even under a steam partial pressure of 0.82 atm, under which dehydration is suppressed to a temperature of 263 °C, no polymorphic transition is detected. The behavior parallels that of Cs3(H1.5PO4)2 and contrasts that of several structurally and chemically similar selenate compounds. The crystal growth approach developed here may prove particularly useful for obtaining water soluble compounds which are thermodynamically or kinetically disfavored at temperatures close to ambient.",

keywords = "Crystal Growth, Cs(HPO), CsH(SeO), Humidity, Precipitation, Solid Acid",

author = "Sheel Sanghvi and Haile, {Sossina M.}",

note = "Publisher Copyright: {\textcopyright} 2021 Elsevier Inc.",

year = "2021",

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doi = "10.1016/j.jssc.2020.121951",

language = "English (US)",

volume = "296",

journal = "Journal of Solid State Chemistry",

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AU - Haile, Sossina M.

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N2 - The previously unknown compound Rb3(H1.5PO4)2 is successfully synthesized here using a newly developed variant of aqueous precipitation crystal growth. The approach exploits the phenomenon of boiling point elevation in concentrated solutions. Crystals of the title compound were obtained upon heating a stoichiometric solution from 110 to 150 °C under a high steam partial pressure of 0.83 atm. Single crystal X-ray diffraction studies revealed Rb3(H1.5PO4)2 crystallizes in space group C2/m and is isostructural to Cs3(H1.5PO4)2. As evidenced by thermal analysis, Rb3(H1.5PO4)2 does not undergo a phase transition to a trigonal superprotonic phase upon heating. Even under a steam partial pressure of 0.82 atm, under which dehydration is suppressed to a temperature of 263 °C, no polymorphic transition is detected. The behavior parallels that of Cs3(H1.5PO4)2 and contrasts that of several structurally and chemically similar selenate compounds. The crystal growth approach developed here may prove particularly useful for obtaining water soluble compounds which are thermodynamically or kinetically disfavored at temperatures close to ambient.

AB - The previously unknown compound Rb3(H1.5PO4)2 is successfully synthesized here using a newly developed variant of aqueous precipitation crystal growth. The approach exploits the phenomenon of boiling point elevation in concentrated solutions. Crystals of the title compound were obtained upon heating a stoichiometric solution from 110 to 150 °C under a high steam partial pressure of 0.83 atm. Single crystal X-ray diffraction studies revealed Rb3(H1.5PO4)2 crystallizes in space group C2/m and is isostructural to Cs3(H1.5PO4)2. As evidenced by thermal analysis, Rb3(H1.5PO4)2 does not undergo a phase transition to a trigonal superprotonic phase upon heating. Even under a steam partial pressure of 0.82 atm, under which dehydration is suppressed to a temperature of 263 °C, no polymorphic transition is detected. The behavior parallels that of Cs3(H1.5PO4)2 and contrasts that of several structurally and chemically similar selenate compounds. The crystal growth approach developed here may prove particularly useful for obtaining water soluble compounds which are thermodynamically or kinetically disfavored at temperatures close to ambient.

KW - Crystal Growth

KW - Cs(HPO)

KW - CsH(SeO)

KW - Humidity

KW - Precipitation

KW - Solid Acid

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A humidity-controlled precipitation technique enabling discovery of Rb₃(H_1.5PO₄)₂

Abstract

Funding

Keywords

ASJC Scopus subject areas

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CSD 2008480: Experimental Crystal Structure Determination

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A humidity-controlled precipitation technique enabling discovery of Rb3(H1.5PO4)2

Abstract

Funding

Keywords

ASJC Scopus subject areas

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Datasets

CSD 2008480: Experimental Crystal Structure Determination

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A humidity-controlled precipitation technique enabling discovery of Rb₃(H_1.5PO₄)₂