Damped Cantilever Microprobes for High-Speed Contact Metrology with 3D Surface Topography.

We addressed the coating 5 mm-long cantilever microprobes with a viscoelastic material, which was intended to considerably extend the range of the traverse speed during the measurements of the 3D surface topography by damping contact-induced oscillations. The damping material was composed of epoxy glue, isopropyl alcohol, and glycerol, and its deposition onto the cantilever is described, as well as the tests of the completed cantilevers under free-oscillating conditions and in contact during scanning on a rough surface. The amplitude and phase of the cantilever's fundamental out-of-plane oscillation mode was investigated vs. the damping layer thickness, which was set via repeated coating steps. The resonance frequency and quality factor decreased with the increasing thickness of the damping layer for both the free-oscillating and in-contact scanning operation mode, as expected from viscoelastic theory. A very low storage modulus of E'≈100kPa, a loss modulus of E″≈434kPa, and a density of ρ≈1.2gcm-3 were yielded for the damping composite. Almost critical damping was observed with an approximately 130 µm-thick damping layer in the free-oscillating case, which was effective at suppressing the ringing behavior during the high-speed in-contact probing of the rough surface topography.

Performance of an Electrothermal MEMS Cantilever Resonator with Fano-Resonance Annoyance under Cigarette Smoke Exposure.

An electrothermal piezoresistive cantilever (EPC) sensor is a low-cost MEMS resonance sensor that provides self-actuating and self-sensing capabilities. In the platform, which is of MEMS-cantilever shape, the EPC sensor offers several advantages in terms of physical, chemical, and biological sensing, e.g., high sensitivity, low cost, simple procedure, and quick response. However, a crosstalk effect is generated by the coupling of parasitic elements from the actuation part to the sensing part. This study presents a parasitic feedthrough subtraction (PFS) method to mitigate a crosstalk effect in an electrothermal piezoresistive cantilever (EPC) resonance sensor. The PFS method is employed to identify a resonance phase that is, furthermore, deployed to a phase-locked loop (PLL)-based system to track and lock the resonance frequency of the EPC sensor under cigarette smoke exposure. The performance of the EPC sensor is further evaluated and compared to an AFM-microcantilever sensor and a commercial particle counter (DC1100-PRO). The particle mass-concentration measurement result generated from cigarette-smoke puffs shows a good agreement between these three detectors.

Atomic Force Microscopy Imaging in Turbid Liquids: A Promising Tool in Nanomedicine.

Tracking of biological and physiological processes on the nanoscale is a central part of the growing field of nanomedicine. Although atomic force microscopy (AFM) is one of the most appropriate techniques in this area, investigations in non-transparent fluids such as human blood are not possible with conventional AFMs due to limitations caused by the optical readout. Here, we show a promising approach based on self-sensing cantilevers (SSC) as a replacement for optical readout in biological AFM imaging. Piezo-resistors, in the form of a Wheatstone bridge, are embedded into the cantilever, whereas two of them are placed at the bending edge. This enables the deflection of the cantilever to be precisely recorded by measuring the changes in resistance. Furthermore, the conventional acoustic or magnetic vibration excitation in intermittent contact mode can be replaced by a thermal excitation using a heating loop. We show further developments of existing approaches enabling stable measurements in turbid liquids. Different readout and excitation methods are compared under various environmental conditions, ranging from dry state to human blood. To demonstrate the applicability of our laser-free bio-AFM for nanomedical research, we have selected the hemostatic process of blood coagulation as well as ultra-flat red blood cells in different turbid fluids. Furthermore, the effects on noise and scanning speed of different media are compared. The technical realization is shown (1) on a conventional optical beam deflection (OBD)-based AFM, where we replaced the optical part by a new SSC nose cone, and (2) on an all-electric AFM, which we adapted for measurements in turbid liquids.

In-Plane and Out-of-Plane MEMS Piezoresistive Cantilever Sensors for Nanoparticle Mass Detection.

In this study, we investigate the performance of two piezoresistive micro-electro-mechanical system (MEMS)-based silicon cantilever sensors for measuring target analytes (i.e., ultrafine particulate matters). We use two different types of cantilevers with geometric dimensions of 1000 × 170 × 19.5 µm3 and 300 × 100 × 4 µm3, which refer to the 1st and 2nd types of cantilevers, respectively. For the first case, the cantilever is configured to detect the fundamental in-plane bending mode and is actuated using a resistive heater. Similarly, the second type of cantilever sensor is actuated using a meandering resistive heater (bimorph) and is designed for out-of-plane operation. We have successfully employed these two cantilevers to measure and monitor the changes of mass concentration of carbon nanoparticles in air, provided by atomizing suspensions of these nanoparticles into a sealed chamber, ranging from 0 to several tens of µg/m3 and oversize distributions from ~10 nm to ~350 nm. Here, we deploy both types of cantilever sensors and operate them simultaneously with a standard laboratory system (Fast Mobility Particle Sizer, FMPS, TSI 3091) as a reference.

3D Nanoprinting of All-Metal Nanoprobes for Electric AFM Modes.

3D nanoprinting via focused electron beam induced deposition (FEBID) is applied for fabrication of all-metal nanoprobes for atomic force microscopy (AFM)-based electrical operation modes. The 3D tip concept is based on a hollow-cone (HC) design, with all-metal material properties and apex radii in the sub-10 nm regime to allow for high-resolution imaging during morphological imaging, conductive AFM (CAFM) and electrostatic force microscopy (EFM). The study starts with design aspects to motivate the proposed HC architecture, followed by detailed fabrication characterization to identify and optimize FEBID process parameters. To arrive at desired material properties, e-beam assisted purification in low-pressure water atmospheres was applied at room temperature, which enabled the removal of carbon impurities from as-deposited structures. The microstructure of final HCs was analyzed via scanning transmission electron microscopy-high-angle annular dark field (STEM-HAADF), whereas electrical and mechanical properties were investigated in situ using micromanipulators. Finally, AFM/EFM/CAFM measurements were performed in comparison to non-functional, high-resolution tips and commercially available electric probes. In essence, we demonstrate that the proposed all-metal HCs provide the resolution capabilities of the former, with the electric conductivity of the latter onboard, combining both assets in one design.

Universal conductance correction in a tunable strongly coupled nanogranular metal.

We present temperature-dependent conductivity data obtained on a sample set of nanogranular Pt-C with finely tuned intergrain tunnel coupling strength g. For samples in the strong-coupling regime g > g(C), characterized by a finite conductivity for T→0, we find a logarithmic behavior at elevated temperatures and a crossover to a √T behavior at low temperatures over a wide range of coupling strengths g(C) ≈ 0.25 < g ≤ 3. The experimental observation for g > 1 is in very good agreement with recent theoretical findings on ordered granular metals in three spatial dimensions. The results indicate a validity of the predicted universal conductivity behavior that goes beyond the immediate range of the approach used in the theoretical derivation.

Structural evolution of perfluoro-pentacene films on Ag(111): transition from 2D to 3D growth.

The structural evolution and thermal stability of perfluoro-pentacene (PF-PEN) thin films on Ag(111) have been studied by means of low-temperature scanning tunnelling microscopy (STM), low-energy electron diffraction (LEED), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and thermal desorption spectroscopy (TDS). Well-defined monolayer films can be prepared by utilizing the different adsorption energy of mono- and multilayer films and selectively desorbing multilayers upon careful heating at 380 K, whereas at temperatures above 400 K, a dissociation occurs. In the first monolayer, the molecules adopt a planar adsorption geometry and form a well-ordered commensurate (6 × 3) superstructure where molecules are uniformly oriented with their long axis along the <110> azimuth. This molecular orientation is also maintained in the second layer, where molecules exhibit a staggered packing motif, whereas further deposition leads to the formation of isolated, tall islands. Moreover, on smooth silver surfaces with extended terraces, growth of PF-PEN onto beforehand prepared long-range ordered monolayer films at elevated temperature leads to needle-like islands that are uniformly aligned at substrate steps along <110> azimuth directions.

Granular Hall Sensors for Scanning Probe Microscopy.

Scanning Hall probe microscopy is attractive for minimally invasive characterization of magnetic thin films and nanostructures by measurement of the emanating magnetic stray field. Established sensor probes operating at room temperature employ highly miniaturized spin-valve elements or semimetals, such as Bi. As the sensor layer structures are fabricated by patterning of planar thin films, their adaption to custom-made sensor probe geometries is highly challenging or impossible. Here we show how nanogranular ferromagnetic Hall devices fabricated by the direct-write method of focused electron beam induced deposition (FEBID) can be tailor-made for any given probe geometry. Furthermore, we demonstrate how the magnetic stray field sensitivity can be optimized in situ directly after direct-write nanofabrication of the sensor element. First proof-of-principle results on the use of this novel scanning Hall sensor are shown.

A tunable strain sensor using nanogranular metals.

This paper introduces a new methodology for the fabrication of strain-sensor elements for MEMS and NEMS applications based on the tunneling effect in nano-granular metals. The strain-sensor elements are prepared by the maskless lithography technique of focused electron-beam-induced deposition (FEBID) employing the precursor trimethylmethylcyclopentadienyl platinum [MeCpPt(Me)(3)]. We use a cantilever-based deflection technique to determine the sensitivity (gauge factor) of the sensor element. We find that its sensitivity depends on the electrical conductivity and can be continuously tuned, either by the thickness of the deposit or by electron-beam irradiation leading to a distinct maximum in the sensitivity. This maximum finds a theoretical rationale in recent advances in the understanding of electronic charge transport in nano-granular metals.

Electronic structure at the perylene-tetracarboxylic acid dianhydride/Ag(111) interface studied with two-photon photoelectron spectroscopy.

The electronic structure of the prototype metal/organic contact 3,4,9,10-perylene-tetracarboxylic acid dianhydride (PTCDA) on a Ag(111)-surface has been investigated using time- and angle-resolved two-photon photoelectron spectroscopy (2PPE). Our analysis addresses particularly the nature of the interface state (IS) emerging at the interface due to the substrate-adsorbate interaction [C. H. Schwalb, S. Sachs, M. Marks et al., Phys. Rev. Lett. 101, 146801 (2008)]. Its free-electron-like dispersion and a possible backfolding at the surface Brillouin zone boundaries are discussed. Time-resolved pump-probe experiments reveal the inelastic electron lifetime along the dispersion parabola and show its decrease for increasing parallel momentum. The temperature dependence of the peak linewidth indicates a coupling of the IS to molecular vibrations. Moreover, additional aspects are addressed, such as the determination of the electron attenuation length of photoelectrons for low kinetic energy originating from the IS and the work function change of the sample upon PTCDA adsorption with very high energy resolution.

Three-Dimensional Nanothermistors for Thermal Probing.

Accessing the thermal properties of materials or even full devices is a highly relevant topic in research and development. Along with the ongoing trend toward smaller feature sizes, the demands on appropriate instrumentation to access surface temperatures with high thermal and lateral resolution also increase. Scanning thermal microscopy is one of the most powerful technologies to fulfill this task down to the sub-100 nm regime, which, however, strongly depends on the nanoprobe design. In this study, we introduce a three-dimensional (3D) nanoprobe concept, which acts as a nanothermistor to access surface temperatures. Fabrication of nanobridges is done via 3D nanoprinting using focused electron beams, which allows direct-write fabrication on prestructured, self-sensing cantilever. As individual branch dimensions are in the sub-100 nm regime, mechanical stability is first studied by a combined approach of finite-element simulation and scanning electron microscopy-assisted in situ atomic force microscopy (AFM) measurements. After deriving the design rules for mechanically stable 3D nanobridges with vertical stiffness up to 50 N m-1, a material tuning approach is introduced to increase mechanical wear resistance at the tip apex for high-quality AFM imaging at high scan speeds. Finally, we demonstrate the electrical response in dependence of temperature and find a negative temperature coefficient of -(0.75 ± 0.2) 10-3 K-1 and sensing rates of 30 ± 1 ms K-1 at noise levels of ±0.5 K, which underlines the potential of our concept.

Focused Electron Beam-Based 3D Nanoprinting for Scanning Probe Microscopy: A Review.

Scanning probe microscopy (SPM) has become an essential surface characterization technique in research and development. By concept, SPM performance crucially depends on the quality of the nano-probe element, in particular, the apex radius. Now, with the development of advanced SPM modes beyond morphology mapping, new challenges have emerged regarding the design, morphology, function, and reliability of nano-probes. To tackle these challenges, versatile fabrication methods for precise nano-fabrication are needed. Aside from well-established technologies for SPM nano-probe fabrication, focused electron beam-induced deposition (FEBID) has become increasingly relevant in recent years, with the demonstration of controlled 3D nanoscale deposition and tailored deposit chemistry. Moreover, FEBID is compatible with practically any given surface morphology. In this review article, we introduce the technology, with a focus on the most relevant demands (shapes, feature size, materials and functionalities, substrate demands, and scalability), discuss the opportunities and challenges, and rationalize how those can be useful for advanced SPM applications. As will be shown, FEBID is an ideal tool for fabrication / modification and rapid prototyping of SPM-tipswith the potential to scale up industrially relevant manufacturing.

Direct-write nanoscale printing of nanogranular tunnelling strain sensors for sub-micrometre cantilevers.

The sensitivity and detection speed of cantilever-based mechanical sensors increases drastically through size reduction. The need for such increased performance for high-speed nanocharacterization and bio-sensing, drives their sub-micrometre miniaturization in a variety of research fields. However, existing detection methods of the cantilever motion do not scale down easily, prohibiting further increase in the sensitivity and detection speed. Here we report a nanomechanical sensor readout based on electron co-tunnelling through a nanogranular metal. The sensors can be deposited with lateral dimensions down to tens of nm, allowing the readout of nanoscale cantilevers without constraints on their size, geometry or material. By modifying the inter-granular tunnel-coupling strength, the sensors' conductivity can be tuned by up to four orders of magnitude, to optimize their performance. We show that the nanoscale printed sensors are functional on 500 nm wide cantilevers and that their sensitivity is suited even for demanding applications such as atomic force microscopy.

In situ growth optimization in focused electron-beam induced deposition.

We present the application of an evolutionary genetic algorithm for the in situ optimization of nanostructures that are prepared by focused electron-beam-induced deposition (FEBID). It allows us to tune the properties of the deposits towards the highest conductivity by using the time gradient of the measured in situ rate of change of conductance as the fitness parameter for the algorithm. The effectiveness of the procedure is presented for the precursor W(CO)6 as well as for post-treatment of Pt-C deposits, which were obtained by the dissociation of MeCpPt(Me)3. For W(CO)6-based structures an increase of conductivity by one order of magnitude can be achieved, whereas the effect for MeCpPt(Me)3 is largely suppressed. The presented technique can be applied to all beam-induced deposition processes and has great potential for a further optimization or tuning of parameters for nanostructures that are prepared by FEBID or related techniques.

Focused electron beam induced deposition: A perspective.

BACKGROUND: Focused electron beam induced deposition (FEBID) is a direct-writing technique with nanometer resolution, which has received strongly increasing attention within the last decade. In FEBID a precursor previously adsorbed on a substrate surface is dissociated in the focus of an electron beam. After 20 years of continuous development FEBID has reached a stage at which this technique is now particularly attractive for several areas in both, basic and applied research. The present topical review addresses selected examples that highlight this development in the areas of charge-transport regimes in nanogranular metals close to an insulator-to-metal transition, the use of these materials for strain- and magnetic-field sensing, and the prospect of extending FEBID to multicomponent systems, such as binary alloys and intermetallic compounds with cooperative ground states. RESULTS: After a brief introduction to the technique, recent work concerning FEBID of Pt-Si alloys and (hard-magnetic) Co-Pt intermetallic compounds on the nanometer scale is reviewed. The growth process in the presence of two precursors, whose flux is independently controlled, is analyzed within a continuum model of FEBID that employs rate equations. Predictions are made for the tunability of the composition of the Co-Pt system by simply changing the dwell time of the electron beam during the writing process. The charge-transport regimes of nanogranular metals are reviewed next with a focus on recent theoretical advancements in the field. As a case study the transport properties of Pt-C nanogranular FEBID structures are discussed. It is shown that by means of a post-growth electron-irradiation treatment the electronic intergrain-coupling strength can be continuously tuned over a wide range. This provides unique access to the transport properties of this material close to the insulator-to-metal transition. In the last part of the review, recent developments in mechanical strain-sensing and the detection of small, inhomogeneous magnetic fields by employing nanogranular FEBID structures are highlighted. CONCLUSION: FEBID has now reached a state of maturity that allows a shift of the focus towards the development of new application fields, be it in basic research or applied. This is shown for selected examples in the present review. At the same time, when seen from a broader perspective, FEBID still has to live up to the original idea of providing a tool for electron-controlled chemistry on the nanometer scale. This has to be understood in the sense that, by providing a suitable environment during the FEBID process, the outcome of the electron-induced reactions can be steered in a controlled way towards yielding the desired composition of the products. The development of a FEBID-specialized surface chemistry is mostly still in its infancy. Next to application development, it is this aspect that will likely be a guiding light for the future development of the field of focused electron beam induced deposition.

Binary Pt-Si nanostructures prepared by focused electron-beam-induced deposition.

Binary systems of Pt-Si are prepared by electron-beam-induced deposition using the two precursors, trimethyl(methylcyclopentadienyl)platinum(IV) (MeCpPt(Me)(3)) and neopentasilane (Si(SiH(3))(4)), simultaneously. By varying the relative flux of the two precursors during deposition, we are able to study composites containing platinum and silicon in different ratios by means of energy-dispersive X-ray spectroscopy, atomic force microscopy, electrical transport measurements, and transmission electron microscopy. The results show strong evidence for the formation of a binary, metastable Pt(2)Si(3) phase, leading to a maximum in the conductivity for a Si/Pt ratio of 3:2.