Precursor Routes to Complex Ternary Intermetallics: Single-Crystal and Microcrystalline Preparation of Clathrate-I Na8Al8Si38 from NaSi plus NaAlSi

Yongkwan Dong; Ping Chai; Matt Beekman; Xiaoyu Zeng; Terry M. Tritt; George S. Nolas

doi:10.1021/acs.inorgchem.5b00348

Precursor Routes to Complex Ternary Intermetallics: Single-Crystal and Microcrystalline Preparation of Clathrate-I Na8Al8Si38 from NaSi plus NaAlSi

Yongkwan Dong, Ping Chai, Matt Beekman, Xiaoyu Zeng, Terry M. Tritt, George S. Nolas

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

19 Scopus citations

Abstract

Single crystals of the ternary clathrate-I Na8Al8Si38 were synthesized by kinetically controlled thermal decomposition (KCTD), and microcrystalline Na8Al8Si38 was synthesized by spark plasma sintering (SPS) using a NaSi + NaAlSi mixture as the precursor. Na8AlxSi46-x compositions with x ≤ 8 were also synthesized by SPS from precursor mixtures of different ratios. The crystal structure of Na8Al8Si38 was investigated using both Rietveld and single-crystal refinements. Temperature-dependent transport and UV/vis measurements were employed in the characterization of Na8Al8Si38, with diffuse-reflectance measurement indicating an indirect optical gap of 0.64 eV. Our results indicate that, when more than one precursor is used, both SPS and KCTD are effective methods for the synthesis of multinary inorganic phases that are not easily accessible by traditional solid-state synthesis or crystal growth techniques.

Original language	English (US)
Pages (from-to)	5316-5321
Number of pages	6
Journal	INORGANIC CHEMISTRY
Volume	54
Issue number	11
DOIs	https://doi.org/10.1021/acs.inorgchem.5b00348
State	Published - 2015
Externally published	Yes

Bibliographical note

KAUST Repository Item: Exported on 2021-10-15
Acknowledged KAUST grant number(s): KAUST Faculty Initiated Collaboration grant
Acknowledgements: Y.D., P.C., and G.S.N. gratefully acknowledge support from the U.S. Department of Energy, Basic Energy Sciences, Division of Materials Science and Engineering, under Award DE-FG02-04ER46145 for single-crystal and microcrystalline syntheses; structural analyses; and PXRD, SEM, and EDS measurements and analyses. X.Z. and T.M.T. acknowledge support, in part, from a KAUST Faculty Initiated Collaboration grant and also some funding from Clemson University.
This publication acknowledges KAUST support, but has no KAUST affiliated authors.

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

Access to Document

10.1021/acs.inorgchem.5b00348

Cite this

@article{8be60769e1fe4e39b7ed40ed786d581d,

title = "Precursor Routes to Complex Ternary Intermetallics: Single-Crystal and Microcrystalline Preparation of Clathrate-I Na8Al8Si38 from NaSi plus NaAlSi",

abstract = "Single crystals of the ternary clathrate-I Na8Al8Si38 were synthesized by kinetically controlled thermal decomposition (KCTD), and microcrystalline Na8Al8Si38 was synthesized by spark plasma sintering (SPS) using a NaSi + NaAlSi mixture as the precursor. Na8AlxSi46-x compositions with x ≤ 8 were also synthesized by SPS from precursor mixtures of different ratios. The crystal structure of Na8Al8Si38 was investigated using both Rietveld and single-crystal refinements. Temperature-dependent transport and UV/vis measurements were employed in the characterization of Na8Al8Si38, with diffuse-reflectance measurement indicating an indirect optical gap of 0.64 eV. Our results indicate that, when more than one precursor is used, both SPS and KCTD are effective methods for the synthesis of multinary inorganic phases that are not easily accessible by traditional solid-state synthesis or crystal growth techniques.",

author = "Yongkwan Dong and Ping Chai and Matt Beekman and Xiaoyu Zeng and Tritt, {Terry M.} and Nolas, {George S.}",

note = "KAUST Repository Item: Exported on 2021-10-15 Acknowledged KAUST grant number(s): KAUST Faculty Initiated Collaboration grant Acknowledgements: Y.D., P.C., and G.S.N. gratefully acknowledge support from the U.S. Department of Energy, Basic Energy Sciences, Division of Materials Science and Engineering, under Award DE-FG02-04ER46145 for single-crystal and microcrystalline syntheses; structural analyses; and PXRD, SEM, and EDS measurements and analyses. X.Z. and T.M.T. acknowledge support, in part, from a KAUST Faculty Initiated Collaboration grant and also some funding from Clemson University. This publication acknowledges KAUST support, but has no KAUST affiliated authors.",

year = "2015",

doi = "10.1021/acs.inorgchem.5b00348",

language = "English (US)",

volume = "54",

pages = "5316--5321",

journal = "INORGANIC CHEMISTRY",

issn = "1520-510X",

publisher = "American Chemical Society",

number = "11",

}

TY - JOUR

T1 - Precursor Routes to Complex Ternary Intermetallics: Single-Crystal and Microcrystalline Preparation of Clathrate-I Na8Al8Si38 from NaSi plus NaAlSi

AU - Dong, Yongkwan

AU - Chai, Ping

AU - Beekman, Matt

AU - Zeng, Xiaoyu

AU - Tritt, Terry M.

AU - Nolas, George S.

N1 - KAUST Repository Item: Exported on 2021-10-15 Acknowledged KAUST grant number(s): KAUST Faculty Initiated Collaboration grant Acknowledgements: Y.D., P.C., and G.S.N. gratefully acknowledge support from the U.S. Department of Energy, Basic Energy Sciences, Division of Materials Science and Engineering, under Award DE-FG02-04ER46145 for single-crystal and microcrystalline syntheses; structural analyses; and PXRD, SEM, and EDS measurements and analyses. X.Z. and T.M.T. acknowledge support, in part, from a KAUST Faculty Initiated Collaboration grant and also some funding from Clemson University. This publication acknowledges KAUST support, but has no KAUST affiliated authors.

PY - 2015

Y1 - 2015

N2 - Single crystals of the ternary clathrate-I Na8Al8Si38 were synthesized by kinetically controlled thermal decomposition (KCTD), and microcrystalline Na8Al8Si38 was synthesized by spark plasma sintering (SPS) using a NaSi + NaAlSi mixture as the precursor. Na8AlxSi46-x compositions with x ≤ 8 were also synthesized by SPS from precursor mixtures of different ratios. The crystal structure of Na8Al8Si38 was investigated using both Rietveld and single-crystal refinements. Temperature-dependent transport and UV/vis measurements were employed in the characterization of Na8Al8Si38, with diffuse-reflectance measurement indicating an indirect optical gap of 0.64 eV. Our results indicate that, when more than one precursor is used, both SPS and KCTD are effective methods for the synthesis of multinary inorganic phases that are not easily accessible by traditional solid-state synthesis or crystal growth techniques.

AB - Single crystals of the ternary clathrate-I Na8Al8Si38 were synthesized by kinetically controlled thermal decomposition (KCTD), and microcrystalline Na8Al8Si38 was synthesized by spark plasma sintering (SPS) using a NaSi + NaAlSi mixture as the precursor. Na8AlxSi46-x compositions with x ≤ 8 were also synthesized by SPS from precursor mixtures of different ratios. The crystal structure of Na8Al8Si38 was investigated using both Rietveld and single-crystal refinements. Temperature-dependent transport and UV/vis measurements were employed in the characterization of Na8Al8Si38, with diffuse-reflectance measurement indicating an indirect optical gap of 0.64 eV. Our results indicate that, when more than one precursor is used, both SPS and KCTD are effective methods for the synthesis of multinary inorganic phases that are not easily accessible by traditional solid-state synthesis or crystal growth techniques.

UR - http://hdl.handle.net/10754/672863

UR - https://pubs.acs.org/doi/10.1021/acs.inorgchem.5b00348

UR - http://www.scopus.com/inward/record.url?scp=84930632508&partnerID=8YFLogxK

U2 - 10.1021/acs.inorgchem.5b00348

DO - 10.1021/acs.inorgchem.5b00348

M3 - Article

SN - 1520-510X

VL - 54

SP - 5316

EP - 5321

JO - INORGANIC CHEMISTRY

JF - INORGANIC CHEMISTRY

IS - 11

ER -

Precursor Routes to Complex Ternary Intermetallics: Single-Crystal and Microcrystalline Preparation of Clathrate-I Na8Al8Si38 from NaSi plus NaAlSi

Abstract

Bibliographical note

ASJC Scopus subject areas

Access to Document

Other files and links

Fingerprint

Cite this