The field of nanoparticle (NP) sizing encompasses a wide array of techniques, with electron microscopy and dynamic light scattering (DLS) having become the established methods for NP quantification; however, these techniques are not always applicable. A new and rapidly developing method that addresses the limitations of these techniques is the electrochemical detection of NPs in solution. The ‘nano-impacts’ technique is an excellent and qualitative in situ method for nanoparticle characterization. Two complementary studies on silver and silver bromide nanoparticles (NPs) were used to assess the large radius limit of the nano-impact method for NP sizing. Noting that by definition a NP cannot be larger than 100 nm in diameter, we have shown that the method quantitatively sizes at the largest limit, the lower limit having been previously reported as ∼6 nm.1
We
report the femtomolar detection of silver (Ag) nanoparticles
by direct-impact voltammetry. This is achieved through the use of
a random array of microelectrodes (RAM) integrated into a purpose-built
flow cell, allowing combined diffusion and convection to the electrode
surface. A coupled RAM-flow cell system is implemented and is shown
to give reproducible wall-jet type flow characteristics, using potassium
ferrocyanide as a molecular redox species. The calibrated flow system
is then used to detect and quantitatively size Ag nanoparticles at
femtomolar concentrations. Under flow conditions, it is found the
nanoparticle impact frequency increases linearly with the volumetric
flow rate. The resulting limit of detection is more than 2 orders
of magnitude smaller than the previous detection limit for direct-impact voltammetry (900 fM) [J. Ellison et al. Sens. Actuators, B2014, 200, 47], and is more than 30 times smaller than the previous detection
limit for mediated-impact voltammetry (83 fM) [T.
M. Alligrant et al. Langmuir2014, 30, 13462].
We report the tracking of atom count in individual nanoparticles during photochemical Ostwald ripening. The nano-impact technique, in conjunction with UV-Vis and TEM analysis, is used to follow the photochemical formation of silver nano-prisms from spherical seed particles. A mechanism of photochemical Ostwald ripening is deduced and key growth stages are identified.
Colloidal suspensions of Bi2 O3 nanoparticles were studied in aqueous solution using imaging and electrochemical techniques. Nanoparticle tracking analysis revealed the particles to be agglomerated. In contrast, electrochemical detection via the nano-impacts technique showed almost exclusive detection of monomeric nanoparticles. Comparison of the two techniques allows the conclusion to be drawn that the agglomeration/deagglomeration of the nanoparticles is reversible. A minimum rate constant for the deagglomeration process was estimated.
Mercury(I) chloride (Hg2Cl2) nanoparticles (NPs) are synthesised for the first time by using two different techniques. First, particles are formed by implosion of a calomel nanolayer, induced by partial electrolysis at a mercury hemisphere microelectrode. The resulting NPs are then characterised by the nanoimpact method, demonstrating the first time metal chloride NPs have been sized by this technique and showing the ability to form and study NPs in situ. Second, Hg2Cl2 NPs are synthesised by using the precipitation reaction of Hg2(NO3)2 with KCl. The NPs are characterised on both mercury and carbon microelectrodes and their size is found to agree with TEM results.
Agglomeration processes in non-interacting particle systems can be understood from a thermodynamic point of view. If the enthalpy of agglomeration is negligible, the distribution of agglomeration states adopts the state of highest entropy. Herein, we provide the exact analytical solution to the mole fractions of agglomerates comprising i monomers, x =2 .
We report the use of nano-impacts as a novel method for the study of photochemical reactions of individual nanoparticles (NPs). The conversion of gelatine stabilised silver bromide (AgBr) NPs to silver (Ag) NPs through photochemical reduction by ascorbic acid is studied mechanistically. Two mechanisms are proposed and investigated by monitoring the amount of electrochemically accessible AgBr against the time scale of conversion, measured through the use of the nano-impacts technique.
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