High-Surface-Area Antimony Sulfide Chalcogels

Kota Surya Subrahmanyam; Christos D. Malliakas; Saiful M. Islam; Debajit Sarma; Jinsong Wu; Mercouri G. Kanatzidis

doi:10.1021/acs.chemmater.6b02913

High-Surface-Area Antimony Sulfide Chalcogels

Kota Surya Subrahmanyam, Christos D. Malliakas, Saiful M. Islam, Debajit Sarma, Jinsong Wu, Mercouri G. Kanatzidis^*

^*Corresponding author for this work

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

18 Scopus citations

Abstract

Chalcogels are a new class of aerogel materials with diverse properties relevant to catalysis, ion-exchange, and gas adsorption. We report the synthesis of high-surface-area antimony sulfide chalcogels through the sol-gel process followed by supercritical drying. Four different synthetic routes were employed: (1) hydrolysis of sodium thioantimonite (Na₃SbS₃); (2) ligand metathesis between Sb³⁺ metal linker and SbS₃^3- anion; (3) reaction of Sb₂S₃ with Na₂S·9H₂O; and (4) reaction of Sb₂S₃ with KOH. All these reactions enable the formation of antimony sulfide gels. The aerogels derived after supercritical drying exhibit high porosity with Brunauer-Emmett-Teller (BET) surface areas up to 300 m² g^-1. The oxidation state of antimony in these chalcogels has been assigned by X-ray photoelectron spectroscopy (XPS) to be +3. Pair distribution function analysis suggests that the local environment around the Sb atoms is very similar to that of crystalline Sb₂S₃. All the antimony sulfide chalcogels possess the band gap of ∼1.75 eV, and they are thermally stable even up to 600 °C.

Original language	English (US)
Pages (from-to)	7744-7749
Number of pages	6
Journal	Chemistry of Materials
Volume	28
Issue number	21
DOIs	https://doi.org/10.1021/acs.chemmater.6b02913
State	Published - Nov 8 2016

Funding

These studies were supported primarily by a NEUP grant from the Department of Energy, Office of Nuclear Energy. K.S.S. acknowledges the Indo?U.S. Science and Technology Forum (IUSSTF) for a postdoctoral fellowship. M.S.I. thanks the MRSEC program (NSF DMR-1121262) at the Materials Research Center. SEM, TEM, STEM and XPS were performed at the EPIC facility of the NUANCE Center at Northwestern University. The NUANCE Center is supported by NSF-NSEC, NSF-MRSEC, the Keck Foundation, the State of Illinois, and Northwestern University. This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357.

ASJC Scopus subject areas

General Chemistry
General Chemical Engineering
Materials Chemistry

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10.1021/acs.chemmater.6b02913

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title = "High-Surface-Area Antimony Sulfide Chalcogels",

abstract = "Chalcogels are a new class of aerogel materials with diverse properties relevant to catalysis, ion-exchange, and gas adsorption. We report the synthesis of high-surface-area antimony sulfide chalcogels through the sol-gel process followed by supercritical drying. Four different synthetic routes were employed: (1) hydrolysis of sodium thioantimonite (Na3SbS3); (2) ligand metathesis between Sb3+ metal linker and SbS33- anion; (3) reaction of Sb2S3 with Na2S·9H2O; and (4) reaction of Sb2S3 with KOH. All these reactions enable the formation of antimony sulfide gels. The aerogels derived after supercritical drying exhibit high porosity with Brunauer-Emmett-Teller (BET) surface areas up to 300 m2 g-1. The oxidation state of antimony in these chalcogels has been assigned by X-ray photoelectron spectroscopy (XPS) to be +3. Pair distribution function analysis suggests that the local environment around the Sb atoms is very similar to that of crystalline Sb2S3. All the antimony sulfide chalcogels possess the band gap of ∼1.75 eV, and they are thermally stable even up to 600 °C.",

author = "Subrahmanyam, {Kota Surya} and Malliakas, {Christos D.} and Islam, {Saiful M.} and Debajit Sarma and Jinsong Wu and Kanatzidis, {Mercouri G.}",

note = "Funding Information: These studies were supported primarily by a NEUP grant from the Department of Energy, Office of Nuclear Energy. K.S.S. acknowledges the Indo?U.S. Science and Technology Forum (IUSSTF) for a postdoctoral fellowship. M.S.I. thanks the MRSEC program (NSF DMR-1121262) at the Materials Research Center. SEM, TEM, STEM and XPS were performed at the EPIC facility of the NUANCE Center at Northwestern University. The NUANCE Center is supported by NSF-NSEC, NSF-MRSEC, the Keck Foundation, the State of Illinois, and Northwestern University. This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357. Publisher Copyright: {\textcopyright} 2016 American Chemical Society.",

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AU - Subrahmanyam, Kota Surya

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AU - Islam, Saiful M.

AU - Sarma, Debajit

AU - Wu, Jinsong

AU - Kanatzidis, Mercouri G.

N1 - Funding Information: These studies were supported primarily by a NEUP grant from the Department of Energy, Office of Nuclear Energy. K.S.S. acknowledges the Indo?U.S. Science and Technology Forum (IUSSTF) for a postdoctoral fellowship. M.S.I. thanks the MRSEC program (NSF DMR-1121262) at the Materials Research Center. SEM, TEM, STEM and XPS were performed at the EPIC facility of the NUANCE Center at Northwestern University. The NUANCE Center is supported by NSF-NSEC, NSF-MRSEC, the Keck Foundation, the State of Illinois, and Northwestern University. This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357. Publisher Copyright: © 2016 American Chemical Society.

PY - 2016/11/8

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N2 - Chalcogels are a new class of aerogel materials with diverse properties relevant to catalysis, ion-exchange, and gas adsorption. We report the synthesis of high-surface-area antimony sulfide chalcogels through the sol-gel process followed by supercritical drying. Four different synthetic routes were employed: (1) hydrolysis of sodium thioantimonite (Na3SbS3); (2) ligand metathesis between Sb3+ metal linker and SbS33- anion; (3) reaction of Sb2S3 with Na2S·9H2O; and (4) reaction of Sb2S3 with KOH. All these reactions enable the formation of antimony sulfide gels. The aerogels derived after supercritical drying exhibit high porosity with Brunauer-Emmett-Teller (BET) surface areas up to 300 m2 g-1. The oxidation state of antimony in these chalcogels has been assigned by X-ray photoelectron spectroscopy (XPS) to be +3. Pair distribution function analysis suggests that the local environment around the Sb atoms is very similar to that of crystalline Sb2S3. All the antimony sulfide chalcogels possess the band gap of ∼1.75 eV, and they are thermally stable even up to 600 °C.

AB - Chalcogels are a new class of aerogel materials with diverse properties relevant to catalysis, ion-exchange, and gas adsorption. We report the synthesis of high-surface-area antimony sulfide chalcogels through the sol-gel process followed by supercritical drying. Four different synthetic routes were employed: (1) hydrolysis of sodium thioantimonite (Na3SbS3); (2) ligand metathesis between Sb3+ metal linker and SbS33- anion; (3) reaction of Sb2S3 with Na2S·9H2O; and (4) reaction of Sb2S3 with KOH. All these reactions enable the formation of antimony sulfide gels. The aerogels derived after supercritical drying exhibit high porosity with Brunauer-Emmett-Teller (BET) surface areas up to 300 m2 g-1. The oxidation state of antimony in these chalcogels has been assigned by X-ray photoelectron spectroscopy (XPS) to be +3. Pair distribution function analysis suggests that the local environment around the Sb atoms is very similar to that of crystalline Sb2S3. All the antimony sulfide chalcogels possess the band gap of ∼1.75 eV, and they are thermally stable even up to 600 °C.

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JF - Chemistry of Materials

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ER -

High-Surface-Area Antimony Sulfide Chalcogels

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