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

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

• instance. The images showed that the trend in the profile is reproduced, although a certain profile may occur at a different location each time the series is repeated. This means that, at least within a range of 100 nm on the sidewall, given a position, a suitable electron dose would result in a vertical

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

• nanopatterning, we have found significant morphological changes induced in the SiO2 substrate even at low electron dose values (<8 nC/μm2). We demonstrate that graphene etching and topographical changes in SiO2 substrates can be controlled via electron beam parameters such as dwell time and dose. Keywords

• : direct writing; dwell time; electron dose; etching; graphene; maskless lithography; nanopatterning; Introduction The discovery of extraordinary and controllable electrical conductivity in graphene back in 2004 made it the most recognized 2D material [1]. The newly discovered phenomena, such as

• , corresponding to three groups of patterns with given dwell times and varying electron doses, are presented in Figure 3. Already for the lowest electron dose D1 – 20 nC/μm2, one observes that graphene is effectively removed. From the profiles for the two lowest electron doses (D1 and D2), it is difficult to find

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

• -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

• , high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) was performed to analyze the morphology of the deposited nanoparticles. For this purpose, several FEBID structures were prepared on the SiO2 substrate with the size of 4 × 4 µm2 and an electron dose of 7.80 C/cm2. For

• currents The FEBID deposits were also prepared with [Au(CH3)2Cl]2 using beam currents of 0.4 nA (deposit size: 2 × 2 μm2), 1.5 nA (deposit size: 4 × 4 μm2), and 3 nA (deposit size: 4 × 4 μm2). The other deposition parameters (electron dose: 7.80 C/cm2 and acceleration voltage: 5 keV) were the same in all

Investigation of electron-induced cross-linking of self-assembled monolayers by scanning tunneling microscopy

• Patrick Stohmann,
• Sascha Koch,
• Yang Yang,
• Christopher David Kaiser,
• Julian Ehrens,
• Jürgen Schnack,
• Niklas Biere,
• Dario Anselmetti,
• Armin Gölzhäuser and
• Xianghui Zhang

Beilstein J. Nanotechnol. 2022, 13, 462–471, doi:10.3762/bjnano.13.39

• the initial stage of cross-linking, the SAMs are exposed to 50 and 1 keV electrons at very low doses and subsequently imaged by STM. The electron dose is then gradually increased up to doses of 25 mC/cm2 and the electron-induced structural changes were then determined. Results and Discussion The

Low-energy electron interaction and focused electron beam-induced deposition of molybdenum hexacarbonyl (Mo(CO)₆)

• Po-Yuan Shih,
• Maicol Cipriani,
• Christian Felix Hermanns,
• Jens Oster,
• Klaus Edinger,
• Armin Gölzhäuser and
• Oddur Ingólfsson

Beilstein J. Nanotechnol. 2022, 13, 182–191, doi:10.3762/bjnano.13.13

• its distinguishable EDX peak among the Mo, C and O elements at 5 keV primary beam energy. Cleanliness of the surface was probed by EDX prior to measurements, confirming the absence of C and O at the surface within the s/n level of the measurements. An electron dose of 8.33 × 1013 was applied on a

• allowing for a clear distinction between EDX peaks from the Mo, C and O elements from the original precursor. Deposition was carried out with an electron dose of 8.33 × 1013 applied on a scanning area of 1 μm2, which resulted in a 230 nm thick pad. EDX measurements were carried out with a ZEISS SEM system

• contribution alone should not make the carbon content more than 5% higher than that of oxygen. Carbon deposition from the background gas was also considered, but EDX measurements of the surface exposed to the same electron dose as in the Mo(CO)6 deposition experiments showed insignificant carbon deposition

Irradiation-driven molecular dynamics simulation of the FEBID process for Pt(PF₃)₄

• Alexey Prosvetov,
• Alexey V. Verkhovtsev,
• Gennady Sushko and
• Andrey V. Solov’yov

Beilstein J. Nanotechnol. 2021, 12, 1151–1172, doi:10.3762/bjnano.12.86

• influence the rate of precursor molecule fragmentation. The chosen value of the deposited energy can be verified by comparing the dependence of surface coverage of precursor elements on the electron dose with the experimental data measured by means of X-ray photoelectron spectroscopy (XPS). Electron energy

The role of convolutional neural networks in scanning probe microscopy: a review

• Ido Azuri,
• Irit Rosenhek-Goldian,
• Neta Regev-Rudzki,
• Georg Fantner and
• Sidney R. Cohen

Beilstein J. Nanotechnol. 2021, 12, 878–901, doi:10.3762/bjnano.12.66

• (STEM) images after nearest neighbor down-sampling. This enabled an increase in image resolution of up to 100-fold, decreasing scanning time and electron dose [120]. Another application of CNNs for STEM was for atomic defect classification [121]. The goal was to characterize defects related to Si

Exploring the fabrication and transfer mechanism of metallic nanostructures on carbon nanomembranes via focused electron beam induced processing

• Christian Preischl,
• Linh Hoang Le,
• Elif Bilgilisoy,
• Armin Gölzhäuser and
• Hubertus Marbach

Beilstein J. Nanotechnol. 2021, 12, 319–329, doi:10.3762/bjnano.12.26

• Figure 2b. The irradiated 2 × 2 µm2 area is not completely covered with iron (purity ca. 90 atom %), as there is no iron at the edges of the square. This process occurs because for EBISA usually a much higher electron dose is necessary to effectively activate the substrate than for EBID. Thus, the edges

• of the square, which due to the lack of proximity effects are exposed to a lower overall electron dose than the center, are not fully covered. The AG process results in the formation of presumably pure crystalline iron [10][12], as evidenced in the blowup SE image in Figure 2c and the orange spectrum

• min, for all electron doses, the irradiated square areas are apparently not fully covered by deposits. For the highest electron dose of 6.08 C/cm2 just small areas at the edges of the squares are not covered. The area of the uncovered parts increases with decreasing electron dose. At 1.01 C/cm2 the

Gold(I) N-heterocyclic carbene precursors for focused electron beam-induced deposition

• Cristiano Glessi,
• Aya Mahgoub,
• Cornelis W. Hagen and
• Mats Tilset

Beilstein J. Nanotechnol. 2021, 12, 257–269, doi:10.3762/bjnano.12.21

• pillar its total deposition time is converted to the total number of incident electrons, or electron dose, used to deposit that pillar. Figure 6 shows that the shapes of the pillar deposits from different precursors are different. Therefore, the volume was chosen to fairly compare the growth rate of the

• different precursors. The height and diameter of the pillars were measured and used to calculate the volume. Figure 7 shows the calculated deposit volumes as a function of the electron dose. Clearly different deposition rates are found ranging from 3 × 10−5 to 1 × 10−2 nm3/e−, assuming linear growth. For

• Information File 1. Deposits from all precursors show a rather linear increase in height with electron dose (Figure S20a, Supporting Information File 1), whereas the deposit diameter increases at first but saturates at higher doses (Figure S20b, Supporting Information File 1). The saturation values differ

Electron beam-induced deposition of platinum from Pt(CO)₂Cl₂ and Pt(CO)₂Br₂

• Aya Mahgoub,
• Hang Lu,
• Rachel M. Thorman,
• Konstantin Preradovic,
• Titel Jurca,
• Lisa McElwee-White,
• Howard Fairbrother and
• Cornelis W. Hagen

Beilstein J. Nanotechnol. 2020, 11, 1789–1800, doi:10.3762/bjnano.11.161

• scanning electron microscope (SEM), wherein series of pillars were successfully grown from both precursors. The growth of the pillars was studied as a function of the electron dose and compared to deposits grown from the commercially available precursor MeCpPtMe3. The composition of the deposits was

• pressure (8 × 10−6 mbar). The pillars deposited from Pt(CO)2Cl2 have a conical shape, and the height is smaller and seems to saturate much more rapidly with electron dose than for the pillars deposited from MeCpPtMe3 (Figure 5). Note that in Figure 5 the dose is plotted as the total number of incident

• slowly in height but faster in width; this makes it interesting to plot the deposited volume as a function of the electron dose and compare the growth rates with those at higher currents. Approximating the shape of the pillars either as a cone (shorter pillars) or as a cylinder with a conical top (taller

Gold-coated plant virus as computed tomography imaging contrast agent

• Alaa A. A. Aljabali,
• Mazhar S. Al Zoubi,
• Khalid M. Al-Batanyeh,
• Ali Al-Radaideh,
• Mohammad A. Obeid,
• Abeer Al Sharabi,
• Walhan Alshaer,
• Bayan AbuFares,
• Tasnim Al-Zanati,
• Murtaza M. Tambuwala,
• Naveed Akbar and
• David J. Evans

Beilstein J. Nanotechnol. 2019, 10, 1983–1993, doi:10.3762/bjnano.10.195

• nanoparticles distributed uniformly on the same position as the electron-dense particles in (A); (D) carbon from the biological matrix of the cells. The electron dose is 20e−/Å2 per frame (200 kV, probe current of 691 pA). Top and lower panels represent different magnifications of two independent experiments

Direct observation of oxygen-vacancy formation and structural changes in Bi₂WO₆ nanoflakes induced by electron irradiation

• Hong-long Shi,
• Bin Zou,
• Zi-an Li,
• Min-ting Luo and
• Wen-zhong Wang

Beilstein J. Nanotechnol. 2019, 10, 1434–1442, doi:10.3762/bjnano.10.141

• complex (inset of Figure 3b) consisting of two large nanoflakes each of ca. 140 nm in size, and the specimen was tilted along the [010] zone axis. In order to capture the transition state, the electron beam was spread out to match the large screen of the TEM to reduce the electron dose, and the exposure

Fabrication of phase masks from amorphous carbon thin films for electron-beam shaping

• Lukas Grünewald,
• Dagmar Gerthsen and
• Simon Hettler

Beilstein J. Nanotechnol. 2019, 10, 1290–1302, doi:10.3762/bjnano.10.128

• objective lens are known problems. These effects are expected to only marginally affect the PM performance because of the almost parallel illumination of the PMs leading to a substantially reduced areal electron dose [17][21]. We have developed two different procedures to fabricate aC PMs in this work. The

Charged particle single nanometre manufacturing

• Philip D. Prewett,
• Cornelis W. Hagen,
• Claudia Lenk,
• Steve Lenk,
• Marcus Kaestner,
• Tzvetan Ivanov,
• Ahmad Ahmad,
• Ivo W. Rangelow,
• Xiaoqing Shi,
• Stuart A. Boden,
• Alex P. G. Robinson,
• Dongxu Yang,
• Sangeetha Hari,
• Marijke Scotuzzi and
• Ejaz Huq

Beilstein J. Nanotechnol. 2018, 9, 2855–2882, doi:10.3762/bjnano.9.266

Pattern generation for direct-write three-dimensional nanoscale structures via focused electron beam induced deposition

• Lukas Keller and
• Michael Huth

Beilstein J. Nanotechnol. 2018, 9, 2581–2598, doi:10.3762/bjnano.9.240

Electron interactions with the heteronuclear carbonyl precursor H₂FeRu₃(CO)₁₃ and comparison with HFeCo₃(CO)₁₂: from fundamental gas phase and surface science studies to focused electron beam induced deposition

• Ragesh Kumar T P,
• Paul Weirich,
• Lukas Hrachowina,
• Marc Hanefeld,
• Ragnar Bjornsson,
• Helgi Rafn Hrodmarsson,
• Sven Barth,
• D. Howard Fairbrother,
• Michael Huth and
• Oddur Ingólfsson

Beilstein J. Nanotechnol. 2018, 9, 555–579, doi:10.3762/bjnano.9.53

• monitored in situ by X-ray photoelectron spectroscopy (XPS) and mass spectrometry. Figure 9 shows the evolution of the O 1s, Fe 2p and Ru 3d/C 1s XPS regions of a nanometer-thick film of H2FeRu3(CO)13 adsorbed onto a gold substrate at 213 K, plotted as a function of increasing electron dose. Area analysis

• changes as electron irradiation, but at a much slower rate. Based on the variation in the O 1s area we estimate that the time taken to acquire one XPS scan of the O 1s, Fe 2p and C 1s/Ru 3d regions corresponds to an electron dose of ≈6.3 × 1014 e−/cm2. Consequently, the effect of X-ray irradiation during

• follow a similar dependence on the electron dose; specifically, they both decrease significantly for comparatively low electron doses (<≈6 × 1016 e−/cm2), but remain constant thereafter. In the case of the Ru 3d5/2 peak the binding energy decreases systematically from 282.2 eV initially to 280.6 eV

Gas-assisted silver deposition with a focused electron beam

• Luisa Berger,
• Katarzyna Madajska,
• Iwona B. Szymanska,
• Katja Höflich,
• Mikhail N. Polyakov,
• Jakub Jurczyk,
• Carlos Guerra-Nuñez and
• Ivo Utke

Beilstein J. Nanotechnol. 2018, 9, 224–232, doi:10.3762/bjnano.9.24

• , silver crystal growth presents a strong dependency on electron dose and precursor refreshment. Keywords: focused electron beam induced deposition; low volatility precursor; silver; Introduction The fabrication of defined patterns in the nanometer regime demands techniques with high lateral resolution

• irradiates it again, thus the FEBID can continue with fresh adsorbates and less co-deposition of carbon. For further studies, box deposits were written with the same electron dose of 7.44 nC/µm2 but different dwell and refreshment times. On first sight it is visible that for short refreshment times as in

• evidence that the crystals seen in the scanning electron micrographs (Figure 1) are made of silver. Figure 3a depicts a line written on a carbon membrane of a TEM grid in our SEM with 25 kV and 0.5 nA and an electron dose of 0.79 pC/µm. Figure 3b displays a bright field scanning transmission electron

Localized growth of carbon nanotubes via lithographic fabrication of metallic deposits

• Fan Tu,
• Martin Drost,
• Imre Szenti,
• Janos Kiss,
• Zoltan Kónya and
• Hubertus Marbach

Beilstein J. Nanotechnol. 2017, 8, 2592–2605, doi:10.3762/bjnano.8.260

• contain high amounts of carbon as contamination. For example, Sharma et al. [20] presented the possibility to control the deposited particle size by varying the EBID parameters (i.e., electron dose and beam current) but no further CNTs were shown to grow on these as-deposited Fe-containing nanoparticles

• catalysts to synthesize well-defined CNTs with controllable morphology via CVD. The influence of the chemical composition and, in particular, of the fabrication parameters (i.e., electron dose and AG time) of Fe deposits were investigated with respect to their suitability and properties as seeds for

• subsequent AG (≈60 min autocatalytic growth time) in our UHV instrument. Here, the EBID process was performed as a point irradiation, that is, the electron beam rests at a fixed position for a certain amount of time and thus provides a controlled local electron dose. The enlargement of the deposits with

Amplified cross-linking efficiency of self-assembled monolayers through targeted dissociative electron attachment for the production of carbon nanomembranes

• Sascha Koch,
• Christopher D. Kaiser,
• Paul Penner,
• Michael Barclay,
• Lena Frommeyer,
• Daniel Emmrich,
• Patrick Stohmann,
• Tarek Abu-Husein,
• Andreas Terfort,
• D. Howard Fairbrother,
• Oddur Ingólfsson and
• Armin Gölzhäuser

Beilstein J. Nanotechnol. 2017, 8, 2562–2571, doi:10.3762/bjnano.8.256

• spectroscopy (XPS), to determine whether the high relative DEA cross section for iodide loss from 2-I-BPT as compared to 2-Br-BP and 2-Cl-BP is reflected in the cross-linking efficiency of SAMs made from these materials. Such sensitization could reduce the electron dose needed for the cross-linking process and

• ) verified the existence of a mechanically stable CNM created from 2-I-BPT after exposure to an electron dose as low as 1.8 mC/cm2. In contrast, SAMs made from BPT, 2-Cl-BPT and 2-Br-BPT did not form stable CNMs after a significantly higher electron dose of 9 mC/cm2. Keywords: 2D materials; carbon

• , covering the interval from 0 to 120 min. The electron dose per minute during these experiments was 0.6 mC/cm2. The chlorine 2p doublet for 2-Cl-BPT is seen at 200 eV with an energy separation of 1.6 eV [33] and the bromine 3p doublet for 2-Br-BPT at 183.6 eV with an energy separation of 6.5 eV [34]. The

Direct writing of gold nanostructures with an electron beam: On the way to pure nanostructures by combining optimized deposition with oxygen-plasma treatment

• Domagoj Belić,
• Mostafa M. Shawrav,
• Emmerich Bertagnolli and
• Heinz D. Wanzenboeck

Beilstein J. Nanotechnol. 2017, 8, 2530–2543, doi:10.3762/bjnano.8.253

• samples were produced using the same HT and I values, the electron dose that the material sustained during deposition was approximately two times higher in the case of planar structure (2.3 × 10−7 C·μm−2 vs ≈1 × 10-7 C·μm−2). It was the first clear evidence that a change of electron beam parameters could

• , the full experimental parameter space of a typical FEBID system is multidimensional – it encompasses electron beam parameters (such as acceleration voltage, i.e., high tension, electron beam current, electron dose, i.e., deposition time), precursor parameters (such as precursor type, flux, and

• and DT values had to be chosen wisely in order to keep the whole study experimentally feasible. The overall strategy was to firstly produce a planar structure by setting PPS to 3 nm and DT to 0.2048 ms, which represents the smallest electron dose per unit area. In the second step, keeping PPS at 3 nm

Comparing postdeposition reactions of electrons and radicals with Pt nanostructures created by focused electron beam induced deposition

• Julie A. Spencer,
• Michael Barclay,
• Miranda J. Gallagher,
• Robert Winkler,
• Ilyas Unlu,
• Yung-Chien Wu,
• Harald Plank,
• Lisa McElwee-White and
• D. Howard Fairbrother

Beilstein J. Nanotechnol. 2017, 8, 2410–2424, doi:10.3762/bjnano.8.240

• ) and was invariant to further increases in electron dose. In related studies, EDS of PtCl2 deposits exposed to 20 h of electron irradiation in the AES revealed only a small decrease (≈5%) in the Cl EDS signal (see Figure 1d). Similarly, electron beam irradiation of PtCl2 deposits in the SEM for 2 h at

• , under precursor limited deposition conditions. In such a scenario, each PtCl2 moiety deposited at the surface of the growing nanostructure could be exposed to a sufficiently large electron dose to effect Cl loss. Atomic hydrogen (AH) As shown in Figures 2–5, exposure of PtCl2 deposits to AH using the

Involvement of two uptake mechanisms of gold and iron oxide nanoparticles in a co-exposure scenario using mouse macrophages

• Dimitri Vanhecke,
• Dagmar A. Kuhn,
• Dorleta Jimenez de Aberasturi,
• Sandor Balog,
• Ana Milosevic,
• Dominic Urban,
• Diana Peckys,
• Niels de Jonge,
• Wolfgang J. Parak,
• Alke Petri-Fink and
• Barbara Rothen-Rutishauser

Beilstein J. Nanotechnol. 2017, 8, 2396–2409, doi:10.3762/bjnano.8.239

• pixel-dwell times between 30 and 100 μs were used. The image sizes were 2048 × 1768 or 1024 × 884 pixels. The electron dose for an image ranged between 81 and 376 e−/Å2, and was below the limit of radiation damage [49]. Transmission electron microscopy Fixation was carried out with 2.5% glutaraldehyde

The role of low-energy electrons in focused electron beam induced deposition: four case studies of representative precursors

• Rachel M. Thorman,
• Ragesh Kumar T. P.,
• D. Howard Fairbrother and
• Oddur Ingólfsson

Beilstein J. Nanotechnol. 2015, 6, 1904–1926, doi:10.3762/bjnano.6.194

• . Hence, through electron irradiation, a chemical change clearly converted the physisorbed MeCpPtMe3 to a chemically bound deposit containing platinum and carbon. In addition to the mass spectra recorded to monitor desorbing fragments, the evolution of the surface composition with increasing electron dose

• in Figure 10. This ratio was found to remain the same for initial film thicknesses of 1–3 nm and for incident electron irradiation with 500 and 200 eV electron energy. Furthermore, the RAIRS data showed a systematic loss of absorbance in the ν(C–H) stretching region with increasing electron dose. The

• the chemical composition of the remaining film was probed by XPS, HREELS was used to study the change in vibrational modes of the adsorbed molecules. Figure 15 shows a time-resolved mass spectrum monitoring the PF3 desorption during electron exposure after an initial electron dose of 0, 1.5 × 1014

Possibilities and limitations of advanced transmission electron microscopy for carbon-based nanomaterials

• Xiaoxing Ke,
• Carla Bittencourt and
• Gustaaf Van Tendeloo

Beilstein J. Nanotechnol. 2015, 6, 1541–1557, doi:10.3762/bjnano.6.158

• , which reduces the intensity of the beam [10][11][12]. This again is of benefit for imaging soft matter materials because a lower electron dose means less damage to the material. More importantly, it improves the energy resolution for spectroscopic studies, which is another major step in the increase of