Reflection imaging with a helium zone plate microscope.

Neutral helium atom microscopy is a novel microscopy technique which offers strictly surface-sensitive, non-destructive imaging. Several experiments have been published in recent years where images are obtained by scanning a helium beam spot across a surface and recording the variation in scattered intensity at a fixed total scattering angle θSD and fixed incident angle θi relative to the overall surface normal. These experiments used a spot obtained by collimating the beam (referred to as helium pinhole microscopy). Alternatively, a beam spot can be created by focusing the beam with an atom optical element. However up till now imaging with a focused helium beam has only been demonstrated in transmission (using a zone plate). Here we present the first reflection images obtained with a focused helium beam (also using a zone plate). Images are obtained with a spot size (FWHM) down to 4.7µm±0.5µm, and we demonstrate focusing down to a spot size of about 1µm. Furthermore, we present experiments measuring the scattering distribution from a focused helium beam spot. The experiments are done by varying the incoming beam angle θi while keeping the beam-detector angle θSD and the point where the beam spot hits the surface fixed - in essence, a microscopy scale realization of a standard helium atom scattering experiment. Our experiments are done using an electron bombardment detector with adjustable signal accumulation, developed particularly for helium microscopy.

Neutral helium atom microscopy.

Neutral helium atom microscopy, also referred to as scanning helium microscopy and commonly abbreviated SHeM or NAM (neutral atom microscopy), is a novel imaging technique that uses a beam of neutral helium atoms as an imaging probe. The technique offers a number of advantages such as the very low energy of the incident probing atoms (less than 0.1 eV), unsurpassed surface sensitivity (no penetration into the sample bulk), a charge neutral, inert probe and a high depth of field. This opens up for a range of interesting applications such as: imaging of fragile and/or non-conducting samples without damage, inspection of 2D materials and nano-coatings, with the possibility to test properties such as grain boundaries or roughness on the Å ngström scale (the wavelength of the incident helium atoms) and imaging of samples with high aspect ratios, with the potential to obtain true to scale height information of 3D surface topography with nanometer resolution: nano stereo microscopy. However, for a full exploitation of the technique, a range of experimental and theoretical issues still needs to be resolved. In this paper we review the research in the field. We do this by following the trajectory of the helium atoms step by step through the microscope: from the initial acceleration in the supersonic expansion used to generate the probing beam over the atom optical elements used to shape the beam (resolution limits), followed by interaction of the helium atoms with the sample (contrast properties) to the final detection and post-processing. We also review recent advances in scanning helium microscope design including a discussion of imaging with other atoms and molecules than helium.

Adsorption of glutamic acid on clean and hydroxylated rutile TiO2(110): an XPS and NEXAFS investigation.

Due to its biocompatibility, TiO2is a relevant material for the study of bio-interfaces. Its electronic and chemical properties are influenced by defects, which mainly consist of oxygen vacancies or adsorbed OH groups and which affect, consequently, also the interaction with biological molecules. Here we report on an x-ray photoemission spectroscopy and near edge adsorption fine structure study of glutamic acid (Glu) adsorption on the rutile TiO2(110) surface, either clean or partially hydroxylated. We show that Glu anchors to the surface through a carboxylate group and that the final adsorption state is influenced by the presence of hydroxyl groups on the surface prior to Glu deposition. Indeed, molecules adsorb both in the anionic and in the zwitterionic form, the former species being favored on the hydroxylated substrate.

Material properties particularly suited to be measured with helium scattering: selected examples from 2D materials, van der Waals heterostructures, glassy materials, catalytic substrates, topological insulators and superconducting radio frequency materials.

Helium Atom Scattering (HAS) and Helium Spin-Echo scattering (HeSE), together helium scattering, are well established, but non-commercial surface science techniques. They are characterised by the beam inertness and very low beam energy (<0.1 eV) which allows essentially all materials and adsorbates, including fragile and/or insulating materials and light adsorbates such as hydrogen to be investigated on the atomic scale. At present there only exist an estimated less than 15 helium and helium spin-echo scattering instruments in total, spread across the world. This means that up till now the techniques have not been readily available for a broad scientific community. Efforts are ongoing to change this by establishing a central helium scattering facility, possibly in connection with a neutron or synchrotron facility. In this context it is important to clarify what information can be obtained from helium scattering that cannot be obtained with other surface science techniques. Here we present a non-exclusive overview of a range of material properties particularly suited to be measured with helium scattering: (i) high precision, direct measurements of bending rigidity and substrate coupling strength of a range of 2D materials and van der Waals heterostructures as a function of temperature, (ii) direct measurements of the electron-phonon coupling constant λ exclusively in the low energy range (<0.1 eV, tuneable) for 2D materials and van der Waals heterostructures (iii) direct measurements of the surface boson peak in glassy materials, (iv) aspects of polymer chain surface dynamics under nano-confinement (v) certain aspects of nanoscale surface topography, (vi) central properties of surface dynamics and surface diffusion of adsorbates (HeSE) and (vii) two specific science case examples - topological insulators and superconducting radio frequency materials, illustrating how combined HAS and HeSE are necessary to understand the properties of quantum materials. The paper finishes with (viii) examples of molecular surface scattering experiments and other atom surface scattering experiments which can be performed using HAS and HeSE instruments.

Spectroscopic ellipsometry meets AFM nanolithography: about hydration of bio-inert oligo(ethylene glycol)-terminated self assembled monolayers on gold.

For the first time, to our knowledge, spectroscopic ellipsometry (SE) has been combined with state-of-the-art AFM differential height measurements conducted after shaving nano-lithography of ultrathin, soft-matter films for thickness determination. We investigated self-assembled monolayers of SH-(CH2)11-EGn-OH molecules on gold, where EG is ethylene glycol units and n = 3 and 6, a prototypical non-fouling system. We performed SE measurements (245-1200 nm) focusing on the changes induced by the formation of the film (difference spectra). SE measurements, analysed by simple models, confirm the formation of the S-Au interface, transparency of the SAMs and provide a sharp picture of the ability of the EG functionality to protect the surface from unspecific adsorption of proteins. A quantitative assessment of the film thickness by SE was carried out ex situ, thanks to the optical contrast between the film and the ambient, and by AFM in liquid. The cross-check between SE and AFM height measurements combined with the comparison between in-liquid and ex situ SE measurements allowed obtaining non-perturbative information about the vertical density profile of the SAM. The in-liquid SE measurements indicate a refractive index matching between the aqueous medium and the outer part of the SAM, consistent with a disordered configuration of OEG and/or the penetration of water amid the OEG strands. A critical discussion provides a detailed insight into the subtle issues and pitfalls related to the thickness determination of soft-matter films to the monolayer limit.

Investigation of the deposition and thermal behavior of striped phases of unsymmetric disulfide self-assembled monolayers on Au(111): the case of 11-hydroxyundecyl decyl disulfide.

Self-assembled monolayers (SAMs) of unsymmetric disulfides on Au(111) are used to form mixed SAMs that can be utilized in many applications. Here, we have studied 11-hydroxyundecyl decyl disulfide (CH3-(CH2)9-S-S-(CH2)11-OH, HDD) SAMs produced by supersonic molecular beam deposition and characterized by He diffraction. The film growth was monitored at different temperatures up to a coverage which corresponds to a full lying down phase and the diffraction analysis shows that below 250 K the phase is different from the phase measured above 300 K. During the annealing of the film, two phase transitions were observed, at 250 K and 350 K. The overall data suggest that the former is related to an irreversible phase separation of HDD above 250 K to decanethiolate (-S-(CH2)9-CH3, DTT) and hydroxyundecylthiolate (-S-(CH2)11-OH, MUDT), while the latter to a reversible melting of the film. Above 450 K, the specular intensity shows an increase related to film desorption and different chemisorbed states were observed with energies in the same range as observed for decanethiol (H-S-(CH2)9-CH3, DT) and mercaptoundecanol (H-S-(CH2)11-OH, MUD) SAMs.

Note: Design and test of a compact flexure z-stage for atomic force microscopy.

We describe the design and test of a flexure z-stage with 12.5 mm height and 4 microm travel to be coupled with a commercial xy stage. The geometrical model was simulated by means of finite element calculations which have provided an accurate description of the stage dynamics also taking into account the effect of a load to get a resonance frequency of 8 kHz with a 10 g load. The tests of the complete xyz stage were performed in intermittent-contact mode on a sample having periodic features (1.6 microm period, 100 nm height) and with additional loads to increase the mass up to 20 g. The results show that for a 10 g load the surface profiles are well reproduced up to 60 microm/s while with a 20 g sample the speed is reduced to 40 microm/s.

Direct images of the virtual source in a supersonic expansion.

Direct images of the virtual source in a supersonic expansion of helium are presented. The images were obtained using a Fresnel zone plate with free-standing zones, 540 microm in diameter and with an outermost zone width of 50 nm. The general method can be extended to other beams, including seeded beams. Measurements were carried out at absolute source pressures ranging from 11 to 171 bar using a 10 microm nozzle with a source temperature of 320 K. The size of the virtual source was found to be strongly dependent on pressure, changing from a diameter of 67+/-6 microm at an absolute nozzle pressure of 11 bar to 180+/-9 microm at 171 bar. The virtual-source brightness displays a maximum at an absolute nozzle pressure of around 30 bar. This phenomenon occurs because of two competing effects: As the pressure increases, the total flux also increases, but at the same time the virtual source broadens. We modeled the expansion process by calculating the velocity distribution with solutions from the Boltzmann equation to estimate the location of the quitting surface where the frequency of interatomic collisions is assumed negligible. Realistic potentials have been used to calculate the cross section for atomic collisions and, for the velocity distribution perpendicular to the center streamline, a proper scaling with distance derived from the continuum expansion model has been introduced. A good agreement between experiments and model has been found and we discuss its approximation limits. For instance, backscattering effects are not included in the calculations and at present we cannot exclude that they also contribute to a broadening of the virtual-source size for the highest pressure regime. The results presented here are important for improving the understanding of the supersonic expansion process. The experimental method might eventually be used as a new way to test molecular and atomic interaction potentials.