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Title: 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 » were found to be Ni0 hcp (PDF: 01-089-7129) and fcc (PDF: 01-070-0989), respectively.« less

Authors:
 [1]; ORCiD logo [1];  [2];  [1];  [2]
  1. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Advanced Materials Lab.
  2. 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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    Works referencing / citing this record:

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    journal, August 2010

    • Pascu, Oana; Caicedo, José Manuel; Fontcuberta, Josep
    • Langmuir, Vol. 26, Issue 15
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    Oleic Acid/Oleylamine Cooperative-Controlled Crystallization Mechanism for Monodisperse Tetragonal Bipyramid NaLa(MoO 4 ) 2 Nanocrystals
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    • Boyle, Timothy J.; Bunge, Scott D.; Andrews, Nicholas L.
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    Catalytic activity of nickel nanoparticles in hydrogenation of p-nitrophenol to p-aminophenol
    journal, September 2009


    Synthesis and structural characterization of Groups 10 and 11 mononuclear fluoroaryloxide complexes
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    hcp and fcc Nickel Nanoparticles Prepared from Organically Functionalized Layered Phyllosilicates of Nickel(II)
    journal, February 2007

    • Richard-Plouet, Mireille; Guillot, Murielle; Vilminot, Serge
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    • DOI: 10.1021/cm062521c

    Controlled Design of Size-Tunable Monodisperse Nickel Nanoparticles
    journal, February 2010

    • Carenco, Sophie; Boissière, Cédric; Nicole, Lionel
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    • DOI: 10.1021/cm902007g

    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
    • DOI: 10.1021/om010918e

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    journal, March 2007


    Synthesis and characterization of a family of solvated sodium aryloxide compounds
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    • 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
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    Synthesis and Magnetic Properties of Nickel Nanorods
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    • Cordente, Nadège; Respaud, Marc; Senocq, François
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    Ab initio effective core potentials for molecular calculations. Potentials for K to Au including the outermost core orbitals
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    • Hay, P. Jeffrey; Wadt, Willard R.
    • The Journal of Chemical Physics, Vol. 82, Issue 1, p. 299-310
    • DOI: 10.1063/1.448975

    Chemical synthesis and characterization of hcp Ni nanoparticles
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    dataset, October 2016


    Synthesis of dodecanethiol monolayer-stabilized nickel nanoparticles
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    Synthesis of Nickel Nanoparticles in Water-in-Oil Microemulsions
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    • Chen, Dong-Hwang; Wu, Szu-Han
    • Chemistry of Materials, Vol. 12, Issue 5
    • DOI: 10.1021/cm991167y

    Adiabatic time-dependent density functional methods for excited state properties
    journal, October 2002

    • Furche, Filipp; Ahlrichs, Reinhart
    • The Journal of Chemical Physics, Vol. 117, Issue 16
    • DOI: 10.1063/1.1508368

    cclib: A library for package-independent computational chemistry algorithms
    journal, January 2008

    • O'boyle, Noel M.; Tenderholt, Adam L.; Langner, Karol M.
    • Journal of Computational Chemistry, Vol. 29, Issue 5
    • DOI: 10.1002/jcc.20823

    Large Scale Synthesis of NiCo Layered Double Hydroxides for Superior Asymmetric Electrochemical Capacitor
    journal, January 2016

    • Li, Ruchun; Hu, Zhaoxia; Shao, Xiaofeng
    • Scientific Reports, Vol. 6, Issue 1
    • DOI: 10.1038/srep18737

    Ab initio effective core potentials for molecular calculations. Potentials for main group elements Na to Bi
    journal, January 1985

    • Wadt, Willard R.; Hay, P. Jeffrey
    • The Journal of Chemical Physics, Vol. 82, Issue 1
    • DOI: 10.1063/1.448800

    Block copolymer mediated stabilization of sub-5 nm superparamagnetic nickel nanoparticles in an aqueous medium
    journal, September 2009


    CCDC 1510807: Experimental Crystal Structure Determination: XARXIA : bis(2-methylphenolato)-tetrakis(pyridine)-nickel(ii) pyridine solvate
    dataset, October 2016


    Synthesis and magnetic properties of face-centered-cubic and hexagonal-close-packed Ni nanoparticles through polyol process
    journal, May 2005

    • Chinnasamy, C. N.; Jeyadevan, B.; Shinoda, K.
    • Journal of Applied Physics, Vol. 97, Issue 10
    • DOI: 10.1063/1.1851951

    Synthesis, Characterization, and Electrochemical Properties of a Series of Sterically Varied Iron(II) Alkoxide Precursors and Their Resultant Nanoparticles
    journal, July 2011

    • Boyle, Timothy J.; Ottley, Leigh Anna M.; Apblett, Christopher A.
    • Inorganic Chemistry, Vol. 50, Issue 13
    • DOI: 10.1021/ic200423m

    Structural Variations of Potassium Aryloxides
    journal, August 2003

    • Boyle, Timothy J.; Andrews, Nicholas L.; Rodriguez, Mark A.
    • Inorganic Chemistry, Vol. 42, Issue 17
    • DOI: 10.1021/ic034222k

    Size- and Structure-Controlled Synthesis and Characterization of Nickel Nanoparticles
    journal, September 2009

    • Chen, Yuanzhi; Luo, Xiaohua; She, Houde
    • Journal of Nanoscience and Nanotechnology, Vol. 9, Issue 9
    • DOI: 10.1166/jnn.2009.1206

    Advances in Structurally Characterized Lanthanide Alkoxide, Aryloxide, and Silyloxide Compounds
    journal, June 2008

    • Boyle, Timothy J.; Ottley, Leigh Anna M.
    • Chemical Reviews, Vol. 108, Issue 6, p. 1896-1917
    • DOI: 10.1021/cr0401063

    Controlling the crystal structure of Ni nanoparticles by the use of alkylamines
    journal, September 2009

    • Mourdikoudis, S.; Simeonidis, K.; Vilalta-Clemente, A.
    • Journal of Magnetism and Magnetic Materials, Vol. 321, Issue 18
    • DOI: 10.1016/j.jmmm.2009.03.076

    CCDC 1510806: Experimental Crystal Structure Determination: XARXEW : bis(2-isopropylphenolato)-tetrakis(pyridine)-nickel(ii)
    dataset, October 2016


    Cadmium Amido Alkoxide and Alkoxide Precursors for the Synthesis of Nanocrystalline CdE (E = S, Se, Te)
    journal, March 2005

    • Boyle, Timothy J.; Bunge, Scott D.; Alam, Todd M.
    • Inorganic Chemistry, Vol. 44, Issue 5
    • DOI: 10.1021/ic0485155