Synthesis and characterization of a series of nickel( ii ) alkoxide precursors and their utility for Ni(0) nanoparticle production
Abstract
We synthesized a series of nickel(II) aryloxide ([Ni(OAr)2(py)x]) precursors from an amide-alcohol exchange using [Ni(NR2)2] in the presence of pyridine (py). The H-OAr selected were the mono- and di-ortho-substituted 2-alkyl phenols: alkyl = methyl (H-oMP), iso-propyl (H-oPP), tert-butyl (H-oBP) and 2,6-di-alkyl phenols (alkyl = di-iso-propyl (H-DIP), di-tert-butyl (H-DBP), di-phenyl (H-DPhP)). Furthermore, the crystalline products were solved as solvated monomers and structurally characterized as [Ni(OAr)2(py)x], where x = 4: OAr = oMP (1), oPP (2); x = 3: OAr = oBP (3), DIP (4); x = 2: OAr = DBP (5), DPhP (6). The excited states (singlet or triplet) and various geometries of 1–6 were identified by experimental UV-vis and verified by computational modeling. Magnetic susceptibility of the representative compound 4 was fit to a Curie Weiss model that yielded a magnetic moment of 4.38(3)μB consistent with a Ni2+ center. Compounds 1 and 6 were selected for decomposition studied under solution precipitation routes since they represent the two extremes of coordination. The particle size and crystalline structure were characterized using transmission electron microscopy (TEM) and powder X-ray diffraction (PXRD). Finally, the materials isolated from 1 and 6 were found by TEM to form irregular shape nanomaterials (8–15 nm), which by PXRDmore »
- Authors:
-
[1];
- Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Advanced Materials Lab.
- Louisiana State Univ., Baton Rouge, LA (United States). Dept. of Physics and Astronomy
- Publication Date:
- Research Org.:
- Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
- Sponsoring Org.:
- USDOE National Nuclear Security Administration (NNSA)
- OSTI Identifier:
- 1360928
- Report Number(s):
- SAND2017-5498J
Journal ID: ISSN 1477-9226; ICHBD9; 653577
- Grant/Contract Number:
- AC04-94AL85000
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Dalton Transactions
- Additional Journal Information:
- Journal Volume: 46; Journal Issue: 18; Journal ID: ISSN 1477-9226
- Publisher:
- Royal Society of Chemistry
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 36 MATERIALS SCIENCE
Citation Formats
Treadwell, LaRico J., Boyle, Timothy J., Phelan, W. Adam, Parkes, Marie V., and Young, David P. Synthesis and characterization of a series of nickel( ii ) alkoxide precursors and their utility for Ni(0) nanoparticle production. United States: N. p., 2017.
Web. doi:10.1039/c6dt04083g.
Treadwell, LaRico J., Boyle, Timothy J., Phelan, W. Adam, Parkes, Marie V., & Young, David P. Synthesis and characterization of a series of nickel( ii ) alkoxide precursors and their utility for Ni(0) nanoparticle production. United States. doi:10.1039/c6dt04083g.
Treadwell, LaRico J., Boyle, Timothy J., Phelan, W. Adam, Parkes, Marie V., and Young, David P. Wed .
"Synthesis and characterization of a series of nickel( ii ) alkoxide precursors and their utility for Ni(0) nanoparticle production". United States. doi:10.1039/c6dt04083g. https://www.osti.gov/servlets/purl/1360928.
@article{osti_1360928,
title = {Synthesis and characterization of a series of nickel( ii ) alkoxide precursors and their utility for Ni(0) nanoparticle production},
author = {Treadwell, LaRico J. and Boyle, Timothy J. and Phelan, W. Adam and Parkes, Marie V. and Young, David P.},
abstractNote = {We synthesized a series of nickel(II) aryloxide ([Ni(OAr)2(py)x]) precursors from an amide-alcohol exchange using [Ni(NR2)2] in the presence of pyridine (py). The H-OAr selected were the mono- and di-ortho-substituted 2-alkyl phenols: alkyl = methyl (H-oMP), iso-propyl (H-oPP), tert-butyl (H-oBP) and 2,6-di-alkyl phenols (alkyl = di-iso-propyl (H-DIP), di-tert-butyl (H-DBP), di-phenyl (H-DPhP)). Furthermore, the crystalline products were solved as solvated monomers and structurally characterized as [Ni(OAr)2(py)x], where x = 4: OAr = oMP (1), oPP (2); x = 3: OAr = oBP (3), DIP (4); x = 2: OAr = DBP (5), DPhP (6). The excited states (singlet or triplet) and various geometries of 1–6 were identified by experimental UV-vis and verified by computational modeling. Magnetic susceptibility of the representative compound 4 was fit to a Curie Weiss model that yielded a magnetic moment of 4.38(3)μB consistent with a Ni2+ center. Compounds 1 and 6 were selected for decomposition studied under solution precipitation routes since they represent the two extremes of coordination. The particle size and crystalline structure were characterized using transmission electron microscopy (TEM) and powder X-ray diffraction (PXRD). Finally, the materials isolated from 1 and 6 were found by TEM to form irregular shape nanomaterials (8–15 nm), which by PXRD were found to be Ni0 hcp (PDF: 01-089-7129) and fcc (PDF: 01-070-0989), respectively.},
doi = {10.1039/c6dt04083g},
journal = {Dalton Transactions},
number = 18,
volume = 46,
place = {United States},
year = {2017},
month = {2}
}
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Structural Diversity in Solvated Lithium Aryloxides. Syntheses, Characterization, and Structures of [Li(OAr)(THF) x ] n and [Li(OAr)(py) x ] 2 Complexes Where OAr = OC 6 H 5 , OC 6 H 4 (2-Me), OC 6 H 3 (2,6-(Me)) 2 , OC 6 H 4 (2-Pr i ), OC 6 H 3 (2,6-(Pr i )) 2 , OC 6 H 4 (2-Bu t ), OC 6 H 3 (2,6-(Bu t )) 2
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The preparation of organically functionalised chromium and nickel nanoparticles
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Laser-Driven Aerosol Synthesis of Nickel Nanoparticles
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Synthesis, Alignment, and Magnetic Properties of Monodisperse Nickel Nanocubes
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Isolation, structural and spectroscopic investigations of complexes with tridentate [O,P,O] and [O,O,O] donor ligands
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CCDC 1510803: Experimental Crystal Structure Determination: XARWOF : bis(2,6-di-t-butylphenolato)-bis(pyridine)-nickel(ii)
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Structural and magnetic properties of hcp and fcc Ni nanoparticles
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Monodisperse nickel nanoparticles prepared from a monosurfactant system and their magnetic propertiesElectronic supplementary information (ESI) available: XPS of Ni nanoparticles; plot of magnetization vs. applied field. See http://www.rsc.org/suppdata/jm/b3/b303226d/
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Catalytic activity of nickel nanoparticles in hydrogenation of p-nitrophenol to p-aminophenol
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- Catalysis Communications, Vol. 10, Issue 15
Synthesis and structural characterization of Groups 10 and 11 mononuclear fluoroaryloxide complexes
journal, October 2005
- Kim, Miki; Zakharov, Lev N.; Rheingold, Arnold L.
- Polyhedron, Vol. 24, Issue 14
hcp and fcc Nickel Nanoparticles Prepared from Organically Functionalized Layered Phyllosilicates of Nickel(II)
journal, February 2007
- Richard-Plouet, Mireille; Guillot, Murielle; Vilminot, Serge
- Chemistry of Materials, Vol. 19, Issue 4
Controlled Design of Size-Tunable Monodisperse Nickel Nanoparticles
journal, February 2010
- Carenco, Sophie; Boissière, Cédric; Nicole, Lionel
- Chemistry of Materials, Vol. 22, Issue 4, p. 1340-1349
Synthesis and Structure of Three Unusual Homoleptic Aryloxides of Nickel and Palladium
journal, March 2002
- Cámpora, Juan; Reyes, Manuel L.; Mereiter, Kurt
- Organometallics, Vol. 21, Issue 6
Controllable Synthesis and Magnetic Properties of Cubic and Hexagonal Phase Nickel Nanocrystals
journal, March 2007
- Han, M.; Liu, Q.; He, J.
- Advanced Materials, Vol. 19, Issue 8
Synthesis and characterization of a family of solvated sodium aryloxide compounds
journal, August 2013
- Boyle, Timothy J.; Velazquez, Andrew T.; Yonemoto, Daniel T.
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Self‐consistent molecular orbital methods. XXIII. A polarization‐type basis set for second‐row elements
journal, October 1982
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- The Journal of Chemical Physics, Vol. 77, Issue 7, p. 3654-3665
Synthesis and Magnetic Properties of Nickel Nanorods
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- Cordente, Nadège; Respaud, Marc; Senocq, François
- Nano Letters, Vol. 1, Issue 10
Ab initio effective core potentials for molecular calculations. Potentials for K to Au including the outermost core orbitals
journal, January 1985
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Chemical synthesis and characterization of hcp Ni nanoparticles
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CCDC 1510808: Experimental Crystal Structure Determination: XARXOG : bis(pyridine)-bis(1,1':3',1''-terphenyl-2'-olato)-nickel(ii)
dataset, October 2016
- Treadwell, LaRico; Boyle, Timothy; Phelan, W. Adam
- Cambridge Structural Database (CSD)
Synthesis of dodecanethiol monolayer-stabilized nickel nanoparticles
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- Chen, Lei; Chen, Jianmin; Zhou, Huidi
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Adiabatic time-dependent density functional methods for excited state properties
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cclib: A library for package-independent computational chemistry algorithms
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CCDC 1510807: Experimental Crystal Structure Determination: XARXIA : bis(2-methylphenolato)-tetrakis(pyridine)-nickel(ii) pyridine solvate
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Synthesis, Characterization, and Electrochemical Properties of a Series of Sterically Varied Iron(II) Alkoxide Precursors and Their Resultant Nanoparticles
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Structural Variations of Potassium Aryloxides
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Size- and Structure-Controlled Synthesis and Characterization of Nickel Nanoparticles
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Advances in Structurally Characterized Lanthanide Alkoxide, Aryloxide, and Silyloxide Compounds
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CCDC 1510806: Experimental Crystal Structure Determination: XARXEW : bis(2-isopropylphenolato)-tetrakis(pyridine)-nickel(ii)
dataset, October 2016
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- Cambridge Structural Database (CSD)
Cadmium Amido Alkoxide and Alkoxide Precursors for the Synthesis of Nanocrystalline CdE (E = S, Se, Te)
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