Laser synthesis of nanoparticles in organic solvents – products, reactions, and perspectives

• Theo Fromme,
• Sven Reichenberger,
• Katharine M. Tibbetts and
• Stephan Barcikowski

Beilstein J. Nanotechnol. 2024, 15, 638–663, doi:10.3762/bjnano.15.54

• reactions and radical species [43]. Besides the reactions involving metal salts during LRL, gas formation [44][45][46][47] and solvent decomposition [48][49][50][51] have also been reported, highlighting the importance of chemical reactions during the processes, although LSPC is often considered to be a

• example, polyynes or alkanes, or permanent gases forming persistent gas microbubbles. There have been various reviews regarding nanoparticle synthesis (mainly addressing findings reported for aqueous media) [7][54][55][56], fundamental physical processes during LSPC [57][58][59], and the potential use of

• nanoparticle synthesis in water is always accompanied by the production of gases [66][67]. Although gas formation has often been attributed to the vaporization of water, the formation of hydrogen and oxygen also occurs. Additionally, the formation of hydrogen peroxide was observed during LAL [50][51] and LRL

Exfoliation of titanium nitride using a non-thermal plasma process

• Priscila Jussiane Zambiazi,
• Dolores Ribeiro Ricci Lazar,
• Larissa Otubo,
• Rodrigo Fernando Brambilla de Souza,
• Almir Oliveira Neto and
• Cecilia Chaves Guedes-Silva

Beilstein J. Nanotechnol. 2024, 15, 631–637, doi:10.3762/bjnano.15.53

• , Brazil 10.3762/bjnano.15.53 Abstract In this study, we present a novel approach for the exfoliation of titanium nitride (TiN) powders utilizing a rapid, facile, and environmentally friendly non-thermal plasma method. This method involves the use of an electric arc and nitrogen as the ambient gas at room

• synthesized utilizing a non-thermal plasma apparatus, as previously developed by de Souza et al. [17]. In this process, similarly as reported in [4], TiN powder with a particle size of approximately 1.0 μm and a purity of 98% (Alfa Aesar) was exposed to a 60 kV electric arc in the presence of a nitrogen gas

AFM-IR investigation of thin PECVD SiO_x films on a polypropylene substrate in the surface-sensitive mode

• Hendrik Müller,
• Hartmut Stadler,
• Teresa de los Arcos,
• Adrian Keller and
• Guido Grundmeier

Beilstein J. Nanotechnol. 2024, 15, 603–611, doi:10.3762/bjnano.15.51

• films on polypropylene substrates. Polypropylene is widely used as packaging material [11] and in other industrial applications [12][13][14]; however, it is commonly known for its poor gas barrier properties [11][13]. Therefore, silicon oxide coatings are used to improve the gas barrier properties [13

• between 0.2 and 0.5 mbar. As the gas mixture, argon, oxygen, and HMDSO (98.5% purity, Sigma-Aldrich) were used in different ratios. First, the surface was pretreated for five seconds with an oxygen-rich plasma. For this step, the argon-to-oxygen ratio was set to 1:2. For the deposition of silicon oxide

• Si 2p peaks. The O 1s–Si 2p distance is 429.6 eV for the 50 nm film and 429.9 eV for the 5 nm film. This is in good agreement with values found in the literature for the PECVD deposition of SiOx films from HMDSO/O2/Ar gas mixtures [21]. A comparison of the relative intensities of the O 1s and Si 2p

Directed growth of quinacridone chains on the vicinal Ag(35 1 1) surface

• Niklas Humberg,
• Lukas Grönwoldt and
• Moritz Sokolowski

Beilstein J. Nanotechnol. 2024, 15, 556–568, doi:10.3762/bjnano.15.48

• , one-dimensional aggregates are also used for gas sensing and carbon-capturing materials [8][9]. A group of surfaces that is very appealing for the growth of 1D structures are vicinal surfaces [10] because the step edges break the rotational symmetry of the surface further and add a periodic 1D grating

Electron-induced deposition using Fe(CO)₄MA and Fe(CO)₅ – effect of MA ligand and process conditions

• Hannah Boeckers,
• Atul Chaudhary,
• Petra Martinović,
• Amy V. Walker,
• Lisa McElwee-White and
• Petra Swiderek

Beilstein J. Nanotechnol. 2024, 15, 500–516, doi:10.3762/bjnano.15.45

• of the desired material, typically a metal, are dosed via a gas inlet system onto a surface placed in a scanning electron microscope (SEM). There, the precursor is decomposed by the tightly focused electron beam to form a solid deposit. To provide the precursor with sufficient volatility, the metal

• FEBID, where the precursor is typically present at submonolayer coverage [29]. However, to the best of our knowledge, cryo-FEBID has not yet been applied to the fabrication of iron deposits. Numerous fundamental studies have investigated the electron-induced fragmentation of isolated Fe(CO)5 in the gas

• )4MA. For reference, data for Fe(CO)5 are included in Figures S1–S3 of Supporting Information File 1. Figure 2a shows mass spectra acquired during ESD from a condensed multilayer of Fe(CO)4MA during irradiation with an energy of 50 eV. For comparison, the gas phase mass spectrum (MS) of Fe(CO)4MA

Sidewall angle tuning in focused electron beam-induced processing

• Sangeetha Hari,
• Willem F. van Dorp,
• Johannes J. L. Mulders,
• Piet H. F. Trompenaars,
• Pieter Kruit and
• Cornelis W. Hagen

Beilstein J. Nanotechnol. 2024, 15, 447–456, doi:10.3762/bjnano.15.40

• ; FEBIP; side wall angle; Introduction Focused electron beam-induced processing (FEBIP) is a technique in which a focused electron beam is directed onto a substrate with an adsorbed layer of precursor molecules. The precursor molecules are supplied from a gas injection system through a nozzle at close

• the etching takes place is unknown. It was noticed that a small change in the pressure of water vapour led to a significant change in the etching rate, suggesting that the process is gas-limited (see Supporting Information File 1, section S3). The role of diffusion could therefore be significant. The

• Dual beam system equipped with two gas injection systems (GISs) for precursor delivery. The GIS nozzles were adjusted to be 150 μm above the sample and at a distance of 100 μm from the centre of the field of view. The precursors chosen were the same as in an earlier study to remove carbon interconnects

Unveiling the nature of atomic defects in graphene on a metal surface

• Karl Rothe,
• Nicolas Néel and
• Jörg Kröger

Beilstein J. Nanotechnol. 2024, 15, 416–425, doi:10.3762/bjnano.15.37

• by noble-gas ion irradiation [6][13][14][17][19][21][24], represents an opportunity for systematic defect studies. The work presented here was stimulated by the lack of experimental data on the actual geometry of atomic-scale defects in graphene. So far, scanning tunneling microscope (STM

• molecular precursor C2H4 (purity: 99.9%) at a partial pressure of 10−5 Pa for 120 s [25][26]. Atomic-scale defects were created by bombarding graphene-covered Ir(111) with low-energy (140 eV) Ar+ ions (purity of the Ar gas: 99.999%) [27][28][29][30] at room temperature for 5 s followed by annealing (900 K

• in graphene on Ir(111) induced by rare-gas ion bombardment. Defects that are assigned to alleged monatomic vacancy sites by STM measurements represent an intact graphene lattice in AFM topographies. Possibly, a defect in the Ir(111) surface is the origin of the STM-derived contrast. The smallest

Controllable physicochemical properties of WO_x thin films grown under glancing angle

• Rupam Mandal,
• Aparajita Mandal,
• Alapan Dutta,
• Rengasamy Sivakumar,
• Sanjeev Kumar Srivastava and
• Tapobrata Som

Beilstein J. Nanotechnol. 2024, 15, 350–359, doi:10.3762/bjnano.15.31

• ultrapure Ar gas (99.99%) using a mass flow controller at 30 sccm flow rate. The substrate holder was kept 12.5 cm away from the target at a glancing angle of 87° and 50 W rf power (Advanced Energy) was applied to the target, keeping the substrate holder grounded. Pre-sputtering was carried out for a

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

• is performed with only a few hundred or a few thousands of particles, whereas 1 g of titanium dioxide used in gas absorption experiments typically contains about 1014 particles, thus expanding the parent population and increasing statistical significance. The method for comparing the SSA with the

Determining by Raman spectroscopy the average thickness and N-layer-specific surface coverages of MoS₂ thin films with domains much smaller than the laser spot size

• Felipe Wasem Klein,
• Jean-Roch Huntzinger,
• Vincent Astié,
• Damien Voiry,
• Romain Parret,
• Houssine Makhlouf,
• Sandrine Juillaguet,
• Jean-Manuel Decams,
• Sylvie Contreras,
• Périne Landois,
• Ahmed-Azmi Zahab,
• Jean-Louis Sauvajol and
• Matthieu Paillet

Beilstein J. Nanotechnol. 2024, 15, 279–296, doi:10.3762/bjnano.15.26

Design, fabrication, and characterization of kinetic-inductive force sensors for scanning probe applications

• August K. Roos,
• Ermes Scarano,
• Elisabet K. Arvidsson,
• Erik Holmgren and
• David B. Haviland

Beilstein J. Nanotechnol. 2024, 15, 242–255, doi:10.3762/bjnano.15.23

• ], or to realize laterally grown high-aspect ratio nanopillars [36]. We realize sharp, vertically grown conductive tips at the apex of the Si-N cantilever using FEBID with a Pt precursor gas. Figure 6 shows the resulting structure. We obtain the conical shape by stacking multiple depositions with

Graphene removal by water-assisted focused electron-beam-induced etching – unveiling the dose and dwell time impact on the etch profile and topographical changes in SiO₂ substrates

• Aleksandra Szkudlarek,
• Jan M. Michalik,
• Inés Serrano-Esparza,
• Zdeněk Nováček,
• Veronika Novotná,
• Piotr Ozga,
• Czesław Kapusta and
• José María De Teresa

Beilstein J. Nanotechnol. 2024, 15, 190–198, doi:10.3762/bjnano.15.18

• electrons at a given process time. From the pressure P inside the SEM chamber one can calculate the number of impinging molecules by using the formula J = PNA/(2πMRT)1/2, given in the reference [31], where NA is the Avogadro number, M is the molar mass of impinging molecules, R is the universal gas constant

• using electron beams and gas precursors was not widely recognized at the time when earlier studies regarding morphological changes in silica upon the electron irradiation were performed [24]. Therefore, neither of the electron-beam-induced changes into the SiO2 surface during the water purification of

• less likely to oxidize quartz, where Si–O–Si bonds dominate on the surface. It is also consistent with other results, where oxygen gas was used for FEBIE of graphene and no etching of SiO2 substrate was detected by AFM. Although our studies already untangle some phenomena accompanying the graphene

Modification of graphene oxide and its effect on properties of natural rubber/graphene oxide nanocomposites

• Nghiem Thi Thuong,
• Le Dinh Quang,
• Vu Quoc Cuong,
• Cao Hong Ha,
• Nguyen Ba Lam and
• Seiichi Kawahara

Beilstein J. Nanotechnol. 2024, 15, 168–179, doi:10.3762/bjnano.15.16

• , and the system was bubbled with N2 gas for 1 h to remove residual dissolved oxygen. Then, 0.51 g of TEPA and 0.34 g of TBHPO initiators were added to the reaction to initiate the radical reaction between GO-VTES and the rubber particles. The reaction was carried out for 3 h with constant stirring

TEM sample preparation of lithographically patterned permalloy nanostructures on silicon nitride membranes

• Joshua Williams,
• Michael I. Faley,
• Joseph Vimal Vas,
• Peng-Han Lu and
• Rafal E. Dunin-Borkowski

Beilstein J. Nanotechnol. 2024, 15, 1–12, doi:10.3762/bjnano.15.1

• layer on the resist, creating fences on the edge of the structure and contaminating the silicon nitride membrane. A possible solution is replacing IBE with reactive ion etching (RIE). Using RIE, there would be less redeposition since the reaction between gas and etched metal will form a gaseous compound

Determination of the radii of coated and uncoated silicon AFM sharp tips using a height calibration standard grating and a nonlinear regression function

• Perawat Boonpuek and
• Jonathan R. Felts

Beilstein J. Nanotechnol. 2023, 14, 1200–1207, doi:10.3762/bjnano.14.99

• to left across two pristine grating structures within a scan size of 10 µm × 10 µm. The calibration grating was cleaned with DI water and dried with nitrogen gas before the experiments. For each tip, we performed a step-to-step linewidth scan pass (without repeating at the same scanline) in contact

A combined gas-phase dissociative ionization, dissociative electron attachment and deposition study on the potential FEBID precursor [Au(CH₃)₂Cl]₂

• Elif Bilgilisoy,
• Ali Kamali,
• Thomas Xaver Gentner,
• Gerd Ballmann,
• Sjoerd Harder,
• Hans-Peter Steinrück,
• Hubertus Marbach and
• Oddur Ingólfsson

Beilstein J. Nanotechnol. 2023, 14, 1178–1199, doi:10.3762/bjnano.14.98

• composition and morphology of FEBID deposits fabricated in an ultrahigh-vacuum (UHV) chamber were explored on different surfaces and at varied beam currents. In the gas phase, dissociative ionization was found to lead to significant carbon loss from this precursor, and about 50% of the chlorine was on average

• the potential to widen the scope of applicable nanomaterials. In FEBID, a focused electron beam is directed onto the surface of a substrate in close proximity to a gas inlet, through which a precursor compound is supplied to deliver the material for the nanostructures to be built. For metallic

• -vacuum (UHV) surface science studies and mass spectrometry in high-vacuum (HV) gas-phase investigations [27][28]. In this context, surface science experiments allow for electron-dose-dependent studies of the elemental composition of the deposit, and desorbing ligands may be monitored by means of mass

Properties of tin oxide films grown by atomic layer deposition from tin tetraiodide and ozone

• Kristjan Kalam,
• Peeter Ritslaid,
• Tanel Käämbre,
• Aile Tamm and
• Kaupo Kukli

Beilstein J. Nanotechnol. 2023, 14, 1085–1092, doi:10.3762/bjnano.14.89

• have been studied from many perspectives. For example, one can mention anodes for Li-ion batteries [1], gas sensors [2], catalytic activities [3], and stable buffer [4] or base [5] layers in solar cells. More applications can be found, when SnO2 is considered as constituent of a nanostructure or a

• glass boat inside the reactor. Nitrogen, N2 (99.999%, AS Linde Gas), was applied as the carrier and purging gas. Ozone, produced from O2 (99.999%, AS Linde Gas), was used as oxidizer, with a concentration of 220–250 g/m3. The ALD process was carried out in the temperature range of 100–600 °C when

• film thickness profile along the gas flow direction. Analysis of oxygen and iodine contents in the films revealed that above a substrate temperature of 200 °C, the oxygen content remained stable. At temperatures below 200 °C, the oxygen content was significantly higher than that expected from a

Experimental investigation of usage of POE lubricants with Al₂O₃, graphene or CNT nanoparticles in a refrigeration compressor

• Kayhan Dağıdır and
• Kemal Bilen

Beilstein J. Nanotechnol. 2023, 14, 1041–1058, doi:10.3762/bjnano.14.86

• in this study was selected in accordance with the R1234yf as the refrigerant. Superheating, which was applied to ensure that the refrigerant enters the compressor in gas phase, was approximately 6 °C. The superheating was controlled by an electronic expansion valve. The refrigerant was gradually

• were measured at 25 °C and shown in Figure 12. The measurement results were compatible with the National Institute of Standards and Technology (NIST) data [37] at 25 °C. Results of compressor electrical power measurements Compressors are devices used to compress any fluid that has a gas phase, and that

Nanoarchitectonics of photothermal materials to enhance the sensitivity of lateral flow assays

• Elangovan Sarathkumar,
• Rajasekharan S. Anjana and
• Ramapurath S. Jayasree

Beilstein J. Nanotechnol. 2023, 14, 988–1003, doi:10.3762/bjnano.14.82

• are likely to occur, namely (i) the relaxation of electrons from non-Fermi levels to the Fermi level (electron–electron scattering), (ii) the cooling of hot electron gas through electron–phonon scattering, and (iii) the emission of heat to the surrounding (phonon–phonon scattering) (Figure 4A,B). The

Fragmentation of metal(II) bis(acetylacetonate) complexes induced by slow electrons

• Janina Kopyra and
• Hassan Abdoul-Carime

Beilstein J. Nanotechnol. 2023, 14, 980–987, doi:10.3762/bjnano.14.81

• attachment. The reported data may contribute to a better understanding of the physical chemistry underlying the electron–molecule interactions, which is crucial for potential applications of these molecular systems in the deposition of nanoscale structures. Keywords: dissociative electron attachment; gas

• , 0.498, 0.44, and 0.16 eV for CuL2, NiL2, and CoL2, MnL2, and ZnL2, respectively [15][16][17][18][19]. As the molecules are sublimated, the pressure of the molecular beam, P, that is, the number of precursors in the gas phase, follows the Clausius–Clapeyron relation (log(P) = C − ΔHsub/T), where C is a

• scale was calibrated using a flow of SF6 gas through the oven that produced the well-known SF6− resonance near 0 eV. The measurements were performed without the presence of the calibration gas, avoiding potentially unwanted reactions such as dissociative electron transfer with the investigated molecules

Metal-organic framework-based nanomaterials for CO₂ storage: A review

• Ha Huu Do,
• Iqra Rabani and
• Hai Bang Truong

Beilstein J. Nanotechnol. 2023, 14, 964–970, doi:10.3762/bjnano.14.79

• facile post-synthetic modifications, which allow for diverse strategies towards efficient adsorption and separation of gas molecules [15]. Among the nanosized MOFs, MOF-210 has demonstrated a remarkable ability to adsorb CO2 (54.5 mmol·g−1 at 50 bar, 298 K) owing to its large surface area of 6240 m2·g−1

• adsorption ability with OMSs ranging from 5.5 to 8.0 mmol·g−1 at 296 K and 1 bar [21]. Moreover, acid Lewis sites within these MOFs effectively interact with CO2, leading to increased adsorption. The pore size plays a vital role in the adsorption and separation of CO2 from gas mixtures because of the

• different kinetic diameters of gas molecules. Herein, we present a comprehensive examination of the current scientific literature pertaining to the utilization of metal-organic framework (MOF)-based nanomaterials in the context of CO2 storage and conversion. This account focuses on the introduction of MOFs

Low temperature atomic layer deposition of cobalt using dicobalt hexacarbonyl-1-heptyne as precursor

• Mathias Franz,
• Mahnaz Safian Jouzdani,
• Lysann Kaßner,
• Marcus Daniel,
• Frank Stahr and
• Stefan E. Schulz

Beilstein J. Nanotechnol. 2023, 14, 951–963, doi:10.3762/bjnano.14.78

• under inert gas atmosphere. The bubbler was heated to 30 °C, which will result in a vapour pressure of 15.7 mbar according to the published Antoine parameters of Georgi and co-workers [23]. Pure argon (6N) was used as carrier gas for bubbling. The depositions in CVD mode were done with a continuous

• time of 6 s has been chosen to reach the saturation state safely. The purging time after the precursor pulse also may affect the deposition rate. Insufficient purging may result in an increased deposition rate as the remaining precursor can directly react in the gas phase within the hydrogen plasma

Ni, Co, Zn, and Cu metal-organic framework-based nanomaterials for electrochemical reduction of CO₂: A review

• Ha Huu Do and
• Hai Bang Truong

Beilstein J. Nanotechnol. 2023, 14, 904–911, doi:10.3762/bjnano.14.74

• implemented to address the issue of CO2 emissions. Among these, the carbon capture and storage (CCS) technique plays a crucial role in curtailing the release of CO2 into the air. By capturing and containing approximately 90% of the CO2 gas generated through the combustion of conventional fuels utilized for

• from metal ions and organic linkers, and have been identified as prospective materials for CO2RR [21]. Therefore, a multitude of MOFs structures have been explored in experimental studies [22][23], exhibiting diverse applications such as gas storage [24], electrocatalysis [25][26][27], glucose sensing

N-Heterocyclic carbene-based gold etchants

• Robert B. Chevalier,
• Justin Pantano,
• Matthew K. Kiesewetter and
• Jason R. Dwyer

Beilstein J. Nanotechnol. 2023, 14, 865–871, doi:10.3762/bjnano.14.71

• % nitrogen gas. Electron micrographs were recorded using the SE2 detector of a Zeiss SIGMA VP field emission scanning electron microscope (SEM). Energy dispersive X-ray spectroscopy (EDS) spectra were obtained for each sample using an Oxford Instruments X-max 50 mm2 EDS attachment. Peaks were identified

Ultralow-energy amorphization of contaminated silicon samples investigated by molecular dynamics

• Grégoire R. N. Defoort-Levkov,
• Alan Bahm and
• Patrick Philipp

Beilstein J. Nanotechnol. 2023, 14, 834–849, doi:10.3762/bjnano.14.68

• depths. Yet, low-energy ion beams come with a variety of challenges. When such low energies are used, the residual gas molecules in the instrument chamber can adsorb on the sample surface and impact the ion beam processes. In this paper we pursue an investigation on the effects of the most common