Chemical Synthesis and Characterization of Pd/SiO2: The Effect of Chemical Reagent

The size and shape distribution of metal nanoparticles (NPs) are important parameters that need to be tuned in order to achieve desired properties of materials for practical applications. In the current work, we present the synthesis of palladium NPs supported on silica by three different methods, a...

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Main Authors: Aram L. Bugaev, Vladimir A. Polyakov, Andrei A. Tereshchenko, Ashura N. Isaeva, Alina A. Skorynina, Elizaveta G. Kamyshova, Andriy P. Budnyk, Tatiana A. Lastovina, Alexander V. Soldatov
Format: Article
Language:English
Published: MDPI AG 2018-02-01
Series:Metals
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Online Access:http://www.mdpi.com/2075-4701/8/2/135
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author Aram L. Bugaev
Vladimir A. Polyakov
Andrei A. Tereshchenko
Ashura N. Isaeva
Alina A. Skorynina
Elizaveta G. Kamyshova
Andriy P. Budnyk
Tatiana A. Lastovina
Alexander V. Soldatov
author_facet Aram L. Bugaev
Vladimir A. Polyakov
Andrei A. Tereshchenko
Ashura N. Isaeva
Alina A. Skorynina
Elizaveta G. Kamyshova
Andriy P. Budnyk
Tatiana A. Lastovina
Alexander V. Soldatov
author_sort Aram L. Bugaev
collection DOAJ
description The size and shape distribution of metal nanoparticles (NPs) are important parameters that need to be tuned in order to achieve desired properties of materials for practical applications. In the current work, we present the synthesis of palladium NPs supported on silica by three different methods, applying reduction by sodium borohydride, hydrazine vapors, and polyethylene glycol (PEG). The synthesized materials were characterized by X-ray diffraction, X-ray fluorescence, transmission electron microscopy, surface area and porosity measurements, and thermogravimetric analysis. Similar nanoparticle sizes with narrow size distribution centered at 8 nm were obtained after reduction by sodium borohydride and hydrazine vapors, whereas the smallest particle size of about 4.8 nm was obtained after reduction by PEG. The effect of modification of the initial palladium chloride compound by ammonium hydroxide was found to lead to the formation of larger particles with average size of 15 nm and broader size distribution. In addition, the process of the reduction of palladium by PEG at different reduction stages was monitored by UV-Vis spectroscopy. CO-stripping voltammetry showed that reduction in hydrazine and in PEG allowed the preparation of Pd NPs with high electrochemically-active surface area. Such NPs are promising materials for electrocatalysis.
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spelling doaj.art-b86d1ced3e00470a8390ec506f471e182022-12-22T01:52:46ZengMDPI AGMetals2075-47012018-02-018213510.3390/met8020135met8020135Chemical Synthesis and Characterization of Pd/SiO2: The Effect of Chemical ReagentAram L. Bugaev0Vladimir A. Polyakov1Andrei A. Tereshchenko2Ashura N. Isaeva3Alina A. Skorynina4Elizaveta G. Kamyshova5Andriy P. Budnyk6Tatiana A. Lastovina7Alexander V. Soldatov8The Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe Smart Materials Research Center, Southern Federal University, 178/24 Sladkova, Rostov-on-Don 344090, RussiaThe size and shape distribution of metal nanoparticles (NPs) are important parameters that need to be tuned in order to achieve desired properties of materials for practical applications. In the current work, we present the synthesis of palladium NPs supported on silica by three different methods, applying reduction by sodium borohydride, hydrazine vapors, and polyethylene glycol (PEG). The synthesized materials were characterized by X-ray diffraction, X-ray fluorescence, transmission electron microscopy, surface area and porosity measurements, and thermogravimetric analysis. Similar nanoparticle sizes with narrow size distribution centered at 8 nm were obtained after reduction by sodium borohydride and hydrazine vapors, whereas the smallest particle size of about 4.8 nm was obtained after reduction by PEG. The effect of modification of the initial palladium chloride compound by ammonium hydroxide was found to lead to the formation of larger particles with average size of 15 nm and broader size distribution. In addition, the process of the reduction of palladium by PEG at different reduction stages was monitored by UV-Vis spectroscopy. CO-stripping voltammetry showed that reduction in hydrazine and in PEG allowed the preparation of Pd NPs with high electrochemically-active surface area. Such NPs are promising materials for electrocatalysis.http://www.mdpi.com/2075-4701/8/2/135palladium nanoparticleshydrazinewet-synthesissolvothermal polyol synthesis
spellingShingle Aram L. Bugaev
Vladimir A. Polyakov
Andrei A. Tereshchenko
Ashura N. Isaeva
Alina A. Skorynina
Elizaveta G. Kamyshova
Andriy P. Budnyk
Tatiana A. Lastovina
Alexander V. Soldatov
Chemical Synthesis and Characterization of Pd/SiO2: The Effect of Chemical Reagent
Metals
palladium nanoparticles
hydrazine
wet-synthesis
solvothermal polyol synthesis
title Chemical Synthesis and Characterization of Pd/SiO2: The Effect of Chemical Reagent
title_full Chemical Synthesis and Characterization of Pd/SiO2: The Effect of Chemical Reagent
title_fullStr Chemical Synthesis and Characterization of Pd/SiO2: The Effect of Chemical Reagent
title_full_unstemmed Chemical Synthesis and Characterization of Pd/SiO2: The Effect of Chemical Reagent
title_short Chemical Synthesis and Characterization of Pd/SiO2: The Effect of Chemical Reagent
title_sort chemical synthesis and characterization of pd sio2 the effect of chemical reagent
topic palladium nanoparticles
hydrazine
wet-synthesis
solvothermal polyol synthesis
url http://www.mdpi.com/2075-4701/8/2/135
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AT ashuranisaeva chemicalsynthesisandcharacterizationofpdsio2theeffectofchemicalreagent
AT alinaaskorynina chemicalsynthesisandcharacterizationofpdsio2theeffectofchemicalreagent
AT elizavetagkamyshova chemicalsynthesisandcharacterizationofpdsio2theeffectofchemicalreagent
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