Matching the organic and inorganic counterparts during nucleation and growth of copper-based nanoparticles – <i>in situ</i> spectroscopic studies

Staniuk, Malwina; Zindel, Daniel; Beek, Wouter van; Hirsch, Ofer; Kränzlin, Niklaus; Niederberger, Markus; Koziej, Dorota

doi:10.1039/c5ce00454c

Cited by 34 publications

(47 citation statements)

References 61 publications

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“…Staniuk et. al . have also used MCR‐ALS to study the growth of Cu based nanoparticles in organic solvents and predicted the nucleation of Cu 2 O and its consecutive reduction to Cu.…”

Section: Resultsmentioning

confidence: 99%

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In Situ XAS Study on Growth of PVP‐Stabilized Cu Nanoparticles

et al. 2018

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Cu nanoparticles have been synthesized from copper acetate using NaBH4 as a reducing agent and poly(N‐vinyl‐2‐pyrrolidone) (PVP) as a stabilizing agent under an inert ambience. In‐situ time‐resolved X‐ray absorption spectroscopy (XAS) measurement, which include both X‐ray near edge structure (XANES) and extended X‐ray absorption fine structure (EXAFS) techniques, have been carried out in a specially designed measurement cell during the formation of Cu nanoparticles using a specialized computer controlled flow setup. Principal Component Analysis (PCA) and Multivariate Curve Resolution with Alternating Least Squares (MCR‐ALS) analysis have been successfully applied to the time‐resolved Cu K‐edge XANES data recorded during the growth of Cu nanoparticles. PCA of the XANES spectra predicted three chemical species present in the reaction solution including an intermediate species apart from the initial and the product species. From MCR‐ALS analysis of the Cu K‐edge XANES spectra, the oxidation state of the reaction intermediate species and the concentration profile of the constituents during the reactions have been determined. Finally the EXAFS spectra of the intermediate species has been extracted and analyzed to predict the local structure of Cu cations in this species.

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“…Staniuk et. al . have also used MCR‐ALS to study the growth of Cu based nanoparticles in organic solvents and predicted the nucleation of Cu 2 O and its consecutive reduction to Cu.…”

Section: Resultsmentioning

confidence: 99%

“…al. have studied in situ the nucleation and growth of Cu based nanoparticles in organic solvents and applied MCR‐ALS to predict intermediate species for copper based nanoparticles . Boita et.…”

Section: Introductionmentioning

confidence: 99%

In Situ XAS Study on Growth of PVP‐Stabilized Cu Nanoparticles

et al. 2018

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“…Typically, only completely dissolved species are visible in the IR spectra . However, if the nanoparticles are in close contact with the IR probe, for example, if they grow on the probe, then it is possible to get information about their surface functionalization . An instructive example was reported by Garnweitner and Grote, who studied the molecular kinetics and particle formation of water‐dispersible titania nanocrystals from TiCl 4 in a benzyl alcohol‐ethanol mixture by in situ ATR‐FTIR .…”

Section: Spectroscopymentioning

confidence: 99%

“…Metal acetylacetonates are viable alternatives to metal halide or alkoxide precursors due to their stability and better availability. The solvothermal reaction between metal acetylacetonates and benzyl alcohol allows the preparation of nanocrystalline Fe 3 O 4 , ZnO, as well as metallic copper nanoparticles . In comparison to BaTiO 3 and yttria, the organic byproduct is not 4‐phenyl‐2‐butanol, but 4‐phenyl‐2‐butanone.…”

Section: Chemical Formation Mechanismsmentioning

confidence: 99%

“…Staniuk et al. studied the reaction between Cu(II) acetylacetonate and benzyl alcohol for the synthesis of copper nanoparticles . In situ FTIR, UV/Vis and in situ XAS studies indicated that the nucleation of Cu 2 O co‐occurred with the formation of benzyl acetate through the reaction of acetylacetonate with benzyl alcohol and formation of benzaldehyde through the oxidation of benzyl alcohol with concurrent reduction of Cu 2+ to Cu + .…”

Section: Chemical Formation Mechanismsmentioning

confidence: 99%

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Mechanistic Aspects in the Formation, Growth and Surface Functionalization of Metal Oxide Nanoparticles in Organic Solvents

Deshmukh

Niederberger

2017

Chemistry A European J

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112

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The synthesis of metal oxide nanoparticles in organic solvents, so-called nonaqueous (or nonhydrolytic) processes represent powerful alternatives to aqueous approaches and have become an independent research field. 10 Years ago, when we published our first review on organic reaction pathways in nonaqueous sol-gel approaches, the number of examples was relatively limited. Nowadays, it is almost impossible to provide an exhaustive overview. Here we review the development of the last few years, without neglecting pioneering examples, which help to follow the historical development. The importance of a profound understanding of mechanistic aspects of nanoparticle crystallization and formation mechanisms can't be overestimated, when it comes to the design of rational synthesis concepts under minimization of trial-and-error experiments. The main reason for the progress in mechanistic understanding lies in the availability of characterization tools that make it possible to monitor chemical reactions from the dissolution of the precursor to the nucleation and growth of the nanoparticles, by ex situ methods involving sampling after different reaction times, but more and more also by in situ studies. After a short introduction to experimental aspects of nonaqueous sol-gel routes to metal oxide nanoparticles, we provide an overview of the main and basic organic reaction pathways in these approaches. Afterwards, we summarize the main characterization methods to study formation mechanisms, and then we discuss in great depth the chemical formation mechanisms of many different types of metal oxide nanoparticles. The review concludes with a paragraph on selected crystallization mechanisms reported for nonaqueous systems and a few illustrative examples of nonaqueous sol-gel concepts applied to surface chemistry.

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Electrochemical Mechanism Investigation of Cu₂MoS₄ Hollow Nanospheres for Fast and Stable Sodium Ion Storage

Chen

Mohrhusen

Ali

et al. 2019

Adv Funct Materials

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Sodium ion batteries (SIBs) are promising alternatives to lithium ion batteries with advantages of cost effectiveness. Metal sulfides as emerging SIB anodes have relatively high electronic conductivity and high theoretical capacity, however, large volume change during electrochemical testing often leads to unsatisfactory electrochemical performance. Herein bimetallic sulfide Cu 2 MoS 4 (CMS) with layered crystal structures are prepared with glucose addition (CMS1), resulting in the formation of hollow nanospheres that endow large interlayer spacing, benefitting the rate performance and cycling stability. The electrochemical mechanisms of CMS1 are investigated using ex situ X-ray photoelectron spectroscopy and in situ X-ray absorption spectroscopy, revealing the conversion-based mechanism in carbonate electrolyte and intercalation-based mechanism in ether-electrolyte, thus allowing fast and reversible Na + storage. With further introduction of reduced graphene oxide (rGO), CMS1-rGO composites are obtained, maintaining the hollow structure of CMS1. CMS1-rGO delivers excellent rate performance (258 mAh g −1 at 50 mA g −1 and 131.9 mAh g −1 at 5000 mA g −1 ) and notably enhanced cycling stability (95.6% after 2000 cycles). A full cell SIB is assembled by coupling CMS1-rGO with Na 3 V 2 (PO 4 ) 3 -based cathode, delivering excellent cycling stability (75.5% after 500 cycles). The excellent rate performance and cycling stability emphasize the advantage of CMS1-rGO toward advanced SIB full cells assembly.

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Matching the organic and inorganic counterparts during nucleation and growth of copper-based nanoparticles – in situ spectroscopic studies

Abstract: Closing the loop: initially, the reactivity of benzyl alcohol determines the nucleation of Cu nanoparticles, but as soon as they start to form they begin to catalyze the condensation of benzyl alcohol to dibenzylether.

Cited by 34 publications

References 61 publications

In Situ XAS Study on Growth of PVP‐Stabilized Cu Nanoparticles

In Situ XAS Study on Growth of PVP‐Stabilized Cu Nanoparticles

Mechanistic Aspects in the Formation, Growth and Surface Functionalization of Metal Oxide Nanoparticles in Organic Solvents

Electrochemical Mechanism Investigation of Cu₂MoS₄ Hollow Nanospheres for Fast and Stable Sodium Ion Storage

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Matching the organic and inorganic counterparts during nucleation and growth of copper-based nanoparticles – in situ spectroscopic studies

Abstract: Closing the loop: initially, the reactivity of benzyl alcohol determines the nucleation of Cu nanoparticles, but as soon as they start to form they begin to catalyze the condensation of benzyl alcohol to dibenzylether.

Cited by 34 publications

References 61 publications

In Situ XAS Study on Growth of PVP‐Stabilized Cu Nanoparticles

In Situ XAS Study on Growth of PVP‐Stabilized Cu Nanoparticles

Mechanistic Aspects in the Formation, Growth and Surface Functionalization of Metal Oxide Nanoparticles in Organic Solvents

Electrochemical Mechanism Investigation of Cu2MoS4 Hollow Nanospheres for Fast and Stable Sodium Ion Storage

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Product

Resources

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Electrochemical Mechanism Investigation of Cu₂MoS₄ Hollow Nanospheres for Fast and Stable Sodium Ion Storage