Comparative electron microscopy particle sizing of TiO₂ pigments: sample preparation and measurement

• Ralf Theissmann,
• Christopher Drury,
• Markus Rohe,
• Thomas Koch,
• Jochen Winkler and
• Petr Pikal

Beilstein J. Nanotechnol. 2024, 15, 317–332, doi:10.3762/bjnano.15.29

• ; particle sizing; primary particles; Introduction Following the EU definition of nanomaterials as being materials in which more than 50% by number of their primary particles have at least one dimension smaller than 100 nm [1][2], the accurate measurement of particle size distributions (PSDs) has become

• because aggregates and primary particles start to be destroyed above 250 J/mL, but only at low rates [18][19]. However, dispersion energies of approximately 600 J/mL or higher may significantly break aggregates into primary particles, causing a shift in the particle size distribution towards a smaller

• median size (D50n) due to the detection of a higher number of liberated primary particles. After dispersion, the samples were transported to the Agilent laboratory. The following day, they were re-dispersed in two different ways just before measurement. This was done to evaluate the impact of sample

Biocatalytic synthesis and ordered self-assembly of silica nanoparticles via a silica-binding peptide

• Mustafa Gungormus

Beilstein J. Nanotechnol. 2023, 14, 280–290, doi:10.3762/bjnano.14.25

• particles and, in turn, stabilizing the early particles. The resulting high number of small particles with very large surface area results in the high OD at 45 min, which is higher than the plateau of the positive control group (Figure 4a). When the fraction of the peptide to primary particles exceeds a

• critical value, the primary particles rapidly aggregate into larger particles, which results in the rapid drop in the OD (Figure 4a,d). Further studies are underway to take advantage of this interesting effect in synthesizing colloidally stable approx. 10 nm SiO2 particles at high volume fractions. Self

A novel approach to pulsed laser deposition of platinum catalyst on carbon particles for use in polymer electrolyte membrane fuel cells

• Bogusław Budner,
• Wojciech Tokarz,
• Sławomir Dyjak,
• Andrzej Czerwiński,
• Bartosz Bartosewicz and
• Bartłomiej Jankiewicz

Beilstein J. Nanotechnol. 2023, 14, 190–204, doi:10.3762/bjnano.14.19

• approaching 1.0 is typical for particulate materials with extensive interparticle porosity and indicates the presence of large aggregates of particles. Such isotherms are typical for carbon black. As elucidated by Holdcroft et al. [40], the primary particles of carbon black materials coalesce into few-hundred

Sputtering onto liquids: a critical review

• Anastasiya Sergievskaya,
• Adrien Chauvin and
• Stephanos Konstantinidis

Beilstein J. Nanotechnol. 2022, 13, 10–53, doi:10.3762/bjnano.13.2

• species (Mz+) to metal atoms (M0), which aggregate until the critical nucleus size ((M0)n) is reached. The future growth of the formed nuclei is limited by the autocatalytic reduction of metallic species on their surface (Equation 5). NPs formed via these steps are called primary particles according to

• the colloid chemistry classification [97]. Controlling the ratio between the rates of the processes in Equation 4 and Equation 5 allows one to control the number and size of the primary particles. Fast nucleation leads to the formation of large amounts of nuclei and smaller final primary particles

• means that these primary particles were not stabilized well enough [79][83]. Despite the fact that the colloidal synthesis of NPs has been actively studied for decades because of the growing interest in nanomaterials, the majority of synthetic protocols were found and optimized by empirical procedures

Criteria ruling particle agglomeration

• Dieter Vollath

Beilstein J. Nanotechnol. 2021, 12, 1093–1100, doi:10.3762/bjnano.12.81

• of particles. Number of particles as function of the particle volume and the number of collisions. This simulation was started with 107 primary particles. The calculations were performed up to 4.7 × 106 collisions. For each number of collisions, the distribution function follows obviously an

Revealing the formation mechanism and band gap tuning of Sb₂S₃ nanoparticles

• Maximilian Joschko,
• Franck Yvan Fotue Wafo,
• Christina Malsi,
• Danilo Kisić,
• Ivana Validžić and
• Christina Graf

Beilstein J. Nanotechnol. 2021, 12, 1021–1033, doi:10.3762/bjnano.12.76

• the bristle-like shape, even after the growth stopped after 18 h reaction time, a merging process was excluded. The growth of individual particle fragments, such as bristles, has been described in the literature as a dendrite-like splitting or branching of primary particles in an autoclave synthesis

Fate and transformation of silver nanoparticles in different biological conditions

• Barbara Pem,
• Marija Ćurlin,
• Darija Domazet Jurašin,
• Valerije Vrček,
• Rinea Barbir,
• Vedran Micek,
• Raluca M. Fratila,
• Jesus M. de la Fuente and
• Ivana Vinković Vrček

Beilstein J. Nanotechnol. 2021, 12, 665–679, doi:10.3762/bjnano.12.53

• of AgNPs from primary particles or AgNO3 was shown in cellular fractions [52]. Also, biogenic synthesis was noted in bacterial cells and in many other organisms. It stands to reason that human intracellular or extracellular environments can provide similar conditions [53][54]. Secondary particles are

• etching process of AgNPs. The reformation of AgNPs from primary particles or released Ag+ was evidenced by the incubation of AgNO3 in liver and brain homogenates which led to the formation of small AgNPs. Moreover, NMR experiments demonstrated the crucial role of biothiols in this reformation process. Our

The preparation temperature influences the physicochemical nature and activity of nanoceria

• Robert A. Yokel,
• Wendel Wohlleben,
• Johannes Georg Keller,
• Matthew L. Hancock,
• Jason M. Unrine,
• D. Allan Butterfield and
• Eric A. Grulke

Beilstein J. Nanotechnol. 2021, 12, 525–540, doi:10.3762/bjnano.12.43

• , resulting in primary particles ca. 5 nm in diameter and with a predominance of surface Ce3+ (Supporting Information File 1, Table S1). Nanoceria are autocatalytically redox-active, cycling between Ce3+ (anti-oxidative) and Ce4+ (pro-oxidative) species. A higher temperature during nanoceria preparation is

Magnetic-field-assisted synthesis of anisotropic iron oxide particles: Effect of pH

• Andrey V. Shibaev,
• Petr V. Shvets,
• Darya E. Kessel,
• Roman A. Kamyshinsky,
• Anton S. Orekhov,
• Sergey S. Abramchuk,
• Alexei R. Khokhlov and
• Olga E. Philippova

Beilstein J. Nanotechnol. 2020, 11, 1230–1241, doi:10.3762/bjnano.11.107

• aggregation and recrystallization of primary particles was previously described for micrometer-sized rod-like magnetite particles synthesized by co-precipitation under different conditions [28]. In that case [28], the rods were composed of primary particles bound together. In our system, some primary

• the {220} and {200} planes of the Fe3O4 crystal, respectively. Hexagonal (blue circle) and cubic (green circle) primary particles are attached to the surface of the rod. HRTEM micrograph of hexagonal iron oxide nanoparticles synthesized at R = 2.1 under a magnetic field of 0.4 T and at 20 °C. TEM

• particles are attached to the surface of the rods; however, the main body of the rods is single-crystalline (Figure 7). Thus, at comparable amounts of OH− and iron ions (Fe3+ and Fe2+) (R = 2.1) in the mixture, the presence of a magnetic field has a direct influence on the morphology of the nanoparticles

Mechanism of silica–lysozyme composite formation unravelled by in situ fast SAXS

• Tomasz M. Stawski,
• Daniela B. van den Heuvel,
• Rogier Besselink,
• Dominique J. Tobler and
• Liane G. Benning

Beilstein J. Nanotechnol. 2019, 10, 182–197, doi:10.3762/bjnano.10.17

• describing the arrangement of primary particles within the composites, and A is a single collective fitting parameter in our model, which is proportional to the number density of aggregates, Nagg, and their specific surface area, SSAagg. Hence, it expresses indirectly the size/extent of the aggregates. In

• indirectly by the parameter A (see region II in Figure 4D–E). This means that aggregates grow through the accretion of individual primary particles to larger aggregates [52], where aggregates as such become denser as their size increases, which in consequence favours the eventual occurrence of the correlated

• structure factor function describing an arrangement of primary particles of a certain scattering length density (SLD), ρp, within an aggregate. The SLD of the space between the particles within the aggregate (the “template”) is ρt, while the SLD of the surrounding (“solvent”) is ρs. The average scattering

New micro/mesoporous nanocomposite material from low-cost sources for the efficient removal of aromatic and pathogenic pollutants from water

• Emmanuel I. Unuabonah,
• Robert Nöske,
• Jens Weber,
• Christina Günter and
• Andreas Taubert

Beilstein J. Nanotechnol. 2019, 10, 119–131, doi:10.3762/bjnano.10.11

• spherical primary particles are observed, but the materials produced at lower temperatures appear to consist of smaller particles (approximate diameter between ≈50 and 150 nm), while the samples produced at higher temperatures contain larger particles with approximate diameters of 200 to 300 nm. Moreover

A novel polyhedral oligomeric silsesquioxane-modified layered double hydroxide: preparation, characterization and properties

• Xianwei Zhang,
• Zhongzhu Ma,
• Hong Fan,
• Carla Bittencourt,
• Jintao Wan and
• Philippe Dubois

Beilstein J. Nanotechnol. 2018, 9, 3053–3068, doi:10.3762/bjnano.9.284

• showed that the silsesquioxane modified-LDH (OLDH) revealed an increase in the interlayer distance, nanoscale plate-like morphology of primary particles, and improved thermal stability. A synergistic effect between the siloxane moiety and Mg–Al hydroxide was found during thermal degradation, and

• important factor accounting for the “compact structure” of OLDH. TEM and SEM The morphology of the LDHs was investigated through TEM and SEM, and the images are shown in Figure 8 and Figure 9, respectively. As can be observed from the contrast in Figure 8a–b, the primary particles of NLDH exhibit plate-like

• geometries with sizes mainly ranging from 100 to 200 nm in diameter and without any defined outer shape. The irregular and arc-like edges of most particles might be an indication of the incomplete process of crystal growth. On the other hand, the primary particles of OLDH in Figure 7c–d are also found to be

Bombyx mori silk/titania/gold hybrid materials for photocatalytic water splitting: combining renewable raw materials with clean fuels

• Stefanie Krüger,
• Michael Schwarze,
• Otto Baumann,
• Christina Günter,
• Michael Bruns,
• Christian Kübel,
• Dorothée Vinga Szabó,
• Rafael Meinusch,
• Verónica de Zea Bermudez and
• Andreas Taubert

Beilstein J. Nanotechnol. 2018, 9, 187–204, doi:10.3762/bjnano.9.21

• (Figure 3). Although the primary particles roughly have the same size in all samples, there are differences in the inter-particle distances. While the NPs in the TS samples show a more open, cluster-like structure with small pore-like spaces up to 100 nm, the TPS samples always exhibit very densely packed

Needs and challenges for assessing the environmental impacts of engineered nanomaterials (ENMs)

• Michelle Romero-Franco,
• Hilary A. Godwin,
• Muhammad Bilal and
• Yoram Cohen

Beilstein J. Nanotechnol. 2017, 8, 989–1014, doi:10.3762/bjnano.8.101

• product meets the definition of “nano-relevant” using the European Union regulatory recommendation of 2011 [57]. According to this recommendation, a nanomaterial is defined as “an unknown material containing primary particles in an unbound state or as an aggregate or as an agglomerate and where, for 50

• % or more of the primary particles in the number size distribution, one or more external dimensions is in the size range 1–100 nm or if the number size distribution is unknown”. A material is also considered to be “nano-relevant” by this definition if its specific surface area per unit volume is

Formation and shape-control of hierarchical cobalt nanostructures using quaternary ammonium salts in aqueous media

• Ruchi Deshmukh,
• Anurag Mehra and
• Rochish Thaokar

Beilstein J. Nanotechnol. 2017, 8, 494–505, doi:10.3762/bjnano.8.53

• to the adsorption of TMAH, resulting in a disc-like aggregation. The assembly of these intermediate nanoclusters happens through continuous rotation and interactions of the primary particles. The translation and rotation occur until the primary particles find a suitable atomic site with compatible

• nanorods is the same as that of the flat surfaces of nanoplates obtained at room temperature (Figure 6c). But the crystalline nature is strikingly different. The surface of nanorods exhibits polycrystallinity. This can be understood from the fact that the primary particles are large (ca. 100 nm) and

• polycrystalline themselves, while the primary particles in the formation of nanoplates are single-crystalline. The thickness of the nanoplates is limited to two particles (size of monomers ca. 15 nm). The above discussion describes the similarity in the growth direction of nanoplates and nanorods. In both

Impact of ultrasonic dispersion on the photocatalytic activity of titania aggregates

• Hoai Nga Le,
• Frank Babick,
• Klaus Kühn,
• Minh Tan Nguyen,
• Michael Stintz and
• Gianaurelio Cuniberti

Beilstein J. Nanotechnol. 2015, 6, 2423–2430, doi:10.3762/bjnano.6.250

• , many of these laboratory-scaled apparatus are inappropriate to be applied in well-defined conditions, making the application with available pilot photoreactors challenging. Besides, such particles often form aggregates [5][13] whose properties differ from those of the primary particles, leading to

• of fine, primary particles (as a result of the larger surface area) has been investigated [4][16][17][18], the behavior and properties of the aggregates is not well understood. This paper shows an engineering approach to study the aggregation in photocatalysts. The first part presents the

An ISA-TAB-Nano based data collection framework to support data-driven modelling of nanotoxicology

• Richard L. Marchese Robinson,
• Mark T. D. Cronin,
• Andrea-Nicole Richarz and
• Robert Rallo

Beilstein J. Nanotechnol. 2015, 6, 1978–1999, doi:10.3762/bjnano.6.202

• [primary particle measurements]” column was designed to report whether or not the size measurements obtained were explicitly stated, in the publication from which they were extracted, to have been made for the primary particles: in principle, TEM might be used to provide information about agglomerates

Temperature-dependent breakdown of hydrogen peroxide-treated ZnO and TiO₂ nanoparticle agglomerates

• Sinan Sabuncu and
• Mustafa Çulha

Beilstein J. Nanotechnol. 2015, 6, 1897–1903, doi:10.3762/bjnano.6.193

• degree of the agglomeration is mostly governed by the synthesis method, which defines their surface properties. During the synthesis processes or in subsequent process steps, the agglomeration of primary particles occurs as a result of the weak bonding between NPs. These primary aggregates then form

• aggregates consisting of a few NPs. It is more clear from Figure 6c that when the hydroxylation and heating processes are combined, the hydrodynamic radius of the ZnO NPs is reduced. At 90 °C, most of the aggregates in the ZnO suspension are broken down and the primary particles are obtained. Figure 6c shows

Metal hydrides: an innovative and challenging conversion reaction anode for lithium-ion batteries

• Luc Aymard,
• Yassine Oumellal and
• Jean-Pierre Bonnet

Beilstein J. Nanotechnol. 2015, 6, 1821–1839, doi:10.3762/bjnano.6.186

• primary particles of 0.1–5 μm, Figure 12b) limits the reversibility of the conversion process. III.3 Effect of hydrogen sorption cycles on MgH2 The particle size of the hydride is also reduced through decrepitation during hydrogen desorption–absorption cycles. This solid–gas reaction not only reduces the

Nanotechnology in the real world: Redeveloping the nanomaterial consumer products inventory

• Marina E. Vance,
• Todd Kuiken,
• Eric P. Vejerano,
• Sean P. McGinnis,
• Michael F. Hochella Jr.,
• David Rejeski and
• Matthew S. Hull

Beilstein J. Nanotechnol. 2015, 6, 1769–1780, doi:10.3762/bjnano.6.181

• primary particles have at least one dimension between 1 and 100 nm, with no provisions for “novel properties” stemming from their small size [16]. Cosmetics that contain nanomaterials are also regulated by the European Commission, and although the use of nanoscale titanium dioxide is permitted, zinc oxide

The eNanoMapper database for nanomaterial safety information

• Nina Jeliazkova,
• Charalampos Chomenidis,
• Philip Doganis,
• Bengt Fadeel,
• Roland Grafström,
• Barry Hardy,
• Janna Hastings,
• Markus Hegi,
• Vedrin Jeliazkov,
• Nikolay Kochev,
• Pekka Kohonen,
• Cristian R. Munteanu,
• Haralambos Sarimveis,
• Bart Smeets,
• Pantelis Sopasakis,
• Georgia Tsiliki,
• David Vorgrimmler and
• Egon Willighagen

Beilstein J. Nanotechnol. 2015, 6, 1609–1634, doi:10.3762/bjnano.6.165

Tattoo ink nanoparticles in skin tissue and fibroblasts

• Colin A. Grant,
• Peter C. Twigg,
• Richard Baker and
• Desmond J. Tobin

Beilstein J. Nanotechnol. 2015, 6, 1183–1191, doi:10.3762/bjnano.6.120

• ± 2 nm (Figure 1a). The light scattering technique used to make these measurements cannot distinguish between primary particles, aggregates and agglomerates. This means that the primary pigment particles may be smaller than the distribution suggests, although they cannot be larger. However, the

Influence of gold, silver and gold–silver alloy nanoparticles on germ cell function and embryo development

• Ulrike Taylor,
• Daniela Tiedemann,
• Christoph Rehbock,
• Wilfried A. Kues,
• Stephan Barcikowski and
• Detlef Rath

Beilstein J. Nanotechnol. 2015, 6, 651–664, doi:10.3762/bjnano.6.66

• yet and can only be speculated about. In contrast to AuNP–ssO which attach to sperm as primary particles due to their good electrosteric stability in salt containing media, ligand-free AuNP attach as agglomerates because their electrostatical stabilisation is shielded once exposed to salt ions (Figure

A reproducible number-based sizing method for pigment-grade titanium dioxide

• Ralf Theissmann,
• Manfred Kluwig and
• Thomas Koch

Beilstein J. Nanotechnol. 2014, 5, 1815–1822, doi:10.3762/bjnano.5.192

•  1. As an example, Figure 1 shows five different projections of one agglomerate found in K2360. The number of obviously visible primary particles varies for the different projections, as well as the size of the projected area, which is generally evaluated. These TEM tomogram-based data illustrate the

• diameter (ECD) are summarised in Tables 1 to 4. The first column gives the number of detected primary particles, followed by mean and standard deviation. Meaningful quantiles (d10, d16, d25, d50 and d84) are given in the next columns. The data of the different samples are treated without any assumption of

• particles is used as a mask for the unified image. The final detection of the primary particles is done on the masked unified image, which allows for the detection of the particles, including their grey values. The grey values of the particles are important for the subsequent filtering of the results

The surface properties of nanoparticles determine the agglomeration state and the size of the particles under physiological conditions

• Christoph Bantz,
• Olga Koshkina,
• Thomas Lang,
• Hans-Joachim Galla,
• C. James Kirkpatrick,
• Roland H. Stauber and
• Michael Maskos

Beilstein J. Nanotechnol. 2014, 5, 1774–1786, doi:10.3762/bjnano.5.188

• industrial scale as well. By pyrolysis of, for example, silicon tetrachloride, primary particles with diameters less than 50 nm are obtained. These merge irreversibly into aggregates with diameters between 250 nm and a few tens of micrometers [58][59]. 3. The third synthesis route involves the hydrolysis and