Solvothermal hot injection synthesis of core-shell AgNi nanoparticles

Vit Vykoukal; Jiri Bursik; Pavla Roupcova; David A. Cullen; Jiri Pinkas

doi:10.1016/j.jallcom.2018.08.082

Solvothermal hot injection synthesis of core-shell AgNi nanoparticles

Vit Vykoukal, Jiri Bursik, Pavla Roupcova, David A. Cullen, Jiri Pinkas

Materials MicroAnalysis

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Abstract

Silver-nickel core-shell nanoparticles (NP) were prepared by solvothermal hot injection synthesis by simultaneous thermolysis/reduction of AgNO₃ and Ni(acac)₂ precursors in the hot mixture of octadecene and oleylamine. Oleylamine decreases decomposition temperature of AgNO₃ to that of Ni(acac)₂ thus ensuring favorable reaction conditions. The prepared AgNi NPs with different Ag/Ni ratios were completely characterized. Dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) were used for particle size characterization of as-prepared AgNi colloids. There is no dependence of the particle size (13–21 nm by SAXS) on the Ag/Ni stoichiometric ratio, but the ultraviolet–visible spectroscopy (UV–vis) reveals that the intensity of the surface plasmon (SPR) decreases with increasing Ni content. Transmission electron microscopy (TEM) verified the results of DLS and SAXS and showed spherical nanoparticle shape. Distribution of individual elements in the nanoparticles was mapped by high resolution scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDS) and revealed their core-shell structure where an Ag nucleus is covered by a thin amorphous Ni layer. Upon heating to 400 °C, Ni crystallization is substantiated by appearance of diffractions in the high-temperature X-ray powder diffractograms (HT-XRD) and of a magnetic moment. Ultimate phase separation was proven by scanning electron microscopy and energy dispersive X-ray analysis (SEM-EDS) in samples heated to 1000 °C. The reaction course and nanoparticle formation studied by DLS, UV–vis, and Ag and Ni elemental analyses reveal an initial Ag seed formation with subsequent Ni overlayer deposition after 180 s.

Original language	English
Pages (from-to)	377-385
Number of pages	9
Journal	Journal of Alloys and Compounds
Volume	770
DOIs	https://doi.org/10.1016/j.jallcom.2018.08.082
State	Published - Jan 5 2019

Funding

The results of this research have been acquired within the CEITEC 2020 (LQ1601) project with financial contribution made by the MEYS CR within special support paid from the National Program for Sustainability II funds and by the Czech Science Foundation ( GA 17-15405S ). CIISB research infrastructure project LM2015043 funded by MEYS CR is gratefully acknowledged for the financial support of the measurements at the CF X-ray Diffraction and Bio-SAXS. The authors thank Dr. K. Novotny and L. Simonikova for ICP-OES analyses, Dr. O. Schneeweiss for magnetic and Dr. Z. Moravec for TG-DSC measurements. STEM-EDS analysis was performed as part of a user project through Oak Ridge National Laboratory's Center for Nanophase Materials Sciences , which is a U.S. Department of Energy (DOE) Office of Science user facility along with instrumentation provided by the DOE Office of Nuclear Energy, Fuel Cycle R&D Program, and the Nuclear Science User Facilities. The results of this research have been acquired within the CEITEC 2020 (LQ1601) project with financial contribution made by the MEYS CR within special support paid from the National Program for Sustainability II funds and by the Czech Science Foundation (GA 17-15405S). CIISB research infrastructure project LM2015043 funded by MEYS CR is gratefully acknowledged for the financial support of the measurements at the CF X-ray Diffraction and Bio-SAXS. The authors thank Dr. K. Novotny and L. Simonikova for ICP-OES analyses, Dr. O. Schneeweiss for magnetic and Dr. Z. Moravec for TG-DSC measurements. STEM-EDS analysis was performed as part of a user project through Oak Ridge National Laboratory's Center for Nanophase Materials Sciences, which is a U.S. Department of Energy (DOE) Office of Science user facility along with instrumentation provided by the DOE Office of Nuclear Energy, Fuel Cycle R&D Program, and the Nuclear Science User Facilities.

Funders	Funder number
Grantová Agentura České Republiky
Oak Ridge National Laboratory
U.S. Department of Energy
Office of Science
Ministerstvo Školství, Mládeže a Tělovýchovy
Grantová Agentura České Republiky	GA 17-15405S, LM2015043

Keywords

Chemical synthesis
Energy-dispersive X-ray spectroscopy
Magnetic measurements
Metals and alloys
Nanostructured materials
Transmission electron microscopy

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10.1016/j.jallcom.2018.08.082

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title = "Solvothermal hot injection synthesis of core-shell AgNi nanoparticles",

abstract = "Silver-nickel core-shell nanoparticles (NP) were prepared by solvothermal hot injection synthesis by simultaneous thermolysis/reduction of AgNO3 and Ni(acac)2 precursors in the hot mixture of octadecene and oleylamine. Oleylamine decreases decomposition temperature of AgNO3 to that of Ni(acac)2 thus ensuring favorable reaction conditions. The prepared AgNi NPs with different Ag/Ni ratios were completely characterized. Dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) were used for particle size characterization of as-prepared AgNi colloids. There is no dependence of the particle size (13–21 nm by SAXS) on the Ag/Ni stoichiometric ratio, but the ultraviolet–visible spectroscopy (UV–vis) reveals that the intensity of the surface plasmon (SPR) decreases with increasing Ni content. Transmission electron microscopy (TEM) verified the results of DLS and SAXS and showed spherical nanoparticle shape. Distribution of individual elements in the nanoparticles was mapped by high resolution scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDS) and revealed their core-shell structure where an Ag nucleus is covered by a thin amorphous Ni layer. Upon heating to 400 °C, Ni crystallization is substantiated by appearance of diffractions in the high-temperature X-ray powder diffractograms (HT-XRD) and of a magnetic moment. Ultimate phase separation was proven by scanning electron microscopy and energy dispersive X-ray analysis (SEM-EDS) in samples heated to 1000 °C. The reaction course and nanoparticle formation studied by DLS, UV–vis, and Ag and Ni elemental analyses reveal an initial Ag seed formation with subsequent Ni overlayer deposition after 180 s.",

keywords = "Chemical synthesis, Energy-dispersive X-ray spectroscopy, Magnetic measurements, Metals and alloys, Nanostructured materials, Transmission electron microscopy",

author = "Vit Vykoukal and Jiri Bursik and Pavla Roupcova and Cullen, {David A.} and Jiri Pinkas",

note = "Publisher Copyright: {\textcopyright} 2018 Elsevier B.V.",

year = "2019",

month = jan,

day = "5",

doi = "10.1016/j.jallcom.2018.08.082",

language = "English",

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T1 - Solvothermal hot injection synthesis of core-shell AgNi nanoparticles

AU - Vykoukal, Vit

AU - Bursik, Jiri

AU - Roupcova, Pavla

AU - Cullen, David A.

AU - Pinkas, Jiri

PY - 2019/1/5

Y1 - 2019/1/5

N2 - Silver-nickel core-shell nanoparticles (NP) were prepared by solvothermal hot injection synthesis by simultaneous thermolysis/reduction of AgNO3 and Ni(acac)2 precursors in the hot mixture of octadecene and oleylamine. Oleylamine decreases decomposition temperature of AgNO3 to that of Ni(acac)2 thus ensuring favorable reaction conditions. The prepared AgNi NPs with different Ag/Ni ratios were completely characterized. Dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) were used for particle size characterization of as-prepared AgNi colloids. There is no dependence of the particle size (13–21 nm by SAXS) on the Ag/Ni stoichiometric ratio, but the ultraviolet–visible spectroscopy (UV–vis) reveals that the intensity of the surface plasmon (SPR) decreases with increasing Ni content. Transmission electron microscopy (TEM) verified the results of DLS and SAXS and showed spherical nanoparticle shape. Distribution of individual elements in the nanoparticles was mapped by high resolution scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDS) and revealed their core-shell structure where an Ag nucleus is covered by a thin amorphous Ni layer. Upon heating to 400 °C, Ni crystallization is substantiated by appearance of diffractions in the high-temperature X-ray powder diffractograms (HT-XRD) and of a magnetic moment. Ultimate phase separation was proven by scanning electron microscopy and energy dispersive X-ray analysis (SEM-EDS) in samples heated to 1000 °C. The reaction course and nanoparticle formation studied by DLS, UV–vis, and Ag and Ni elemental analyses reveal an initial Ag seed formation with subsequent Ni overlayer deposition after 180 s.

AB - Silver-nickel core-shell nanoparticles (NP) were prepared by solvothermal hot injection synthesis by simultaneous thermolysis/reduction of AgNO3 and Ni(acac)2 precursors in the hot mixture of octadecene and oleylamine. Oleylamine decreases decomposition temperature of AgNO3 to that of Ni(acac)2 thus ensuring favorable reaction conditions. The prepared AgNi NPs with different Ag/Ni ratios were completely characterized. Dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) were used for particle size characterization of as-prepared AgNi colloids. There is no dependence of the particle size (13–21 nm by SAXS) on the Ag/Ni stoichiometric ratio, but the ultraviolet–visible spectroscopy (UV–vis) reveals that the intensity of the surface plasmon (SPR) decreases with increasing Ni content. Transmission electron microscopy (TEM) verified the results of DLS and SAXS and showed spherical nanoparticle shape. Distribution of individual elements in the nanoparticles was mapped by high resolution scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDS) and revealed their core-shell structure where an Ag nucleus is covered by a thin amorphous Ni layer. Upon heating to 400 °C, Ni crystallization is substantiated by appearance of diffractions in the high-temperature X-ray powder diffractograms (HT-XRD) and of a magnetic moment. Ultimate phase separation was proven by scanning electron microscopy and energy dispersive X-ray analysis (SEM-EDS) in samples heated to 1000 °C. The reaction course and nanoparticle formation studied by DLS, UV–vis, and Ag and Ni elemental analyses reveal an initial Ag seed formation with subsequent Ni overlayer deposition after 180 s.

KW - Chemical synthesis

KW - Energy-dispersive X-ray spectroscopy

KW - Magnetic measurements

KW - Metals and alloys

KW - Nanostructured materials

KW - Transmission electron microscopy

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DO - 10.1016/j.jallcom.2018.08.082

M3 - Article

AN - SCOPUS:85051760988

SN - 0925-8388

VL - 770

SP - 377

EP - 385

JO - Journal of Alloys and Compounds

JF - Journal of Alloys and Compounds

ER -

Solvothermal hot injection synthesis of core-shell AgNi nanoparticles

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