Atomic Force Microscope Platform Research Articles

Characterizing and controlling infrared phonon anomaly of bilayer graphene in optical-electrical force nanoscopy

We, for the first time, report the nanoscopic imaging study of anomalous infrared (IR) phonon enhancement of bilayer graphene, originated from the charge imbalance between the top and bottom layers, resulting in the enhancement of E1u mode of bilayer graphene near 0.2 eV. We modified the multifrequency atomic force microscope platform to combine photo-induced force microscope with electrostatic/Kelvin probe force microscope constituting a novel hybrid nanoscale optical-electrical force imaging system. This enables to observe a correlation between the IR response, doping level, and topographic information of the graphene layers. Through the nanoscale spectroscopic image measurements, we demonstrate that the charge imbalance at the graphene interface can be controlled by chemical (doping effect via Redox mechanism) and mechanical (triboelectric effect by the doped cantilever) approaches. Moreover, we can also diagnosis the subsurface cracks on the stacked few-layer graphene at nanoscale, by monitoring the strain-induced IR phonon shift. Our approach provides new insights into the development of graphene-based electronic and photonic devices and their potential applications.

In Situ Detection of Local Structure Transformation of 2D SnSe Nanosheets through Nanothermomechanical Behavior

2D tin selenide (SnSe) is a promising semiconductive material and its thermal stability is one of the most significant evaluating indicators. However, few works are involved in the temperature‐dependent structure stability of 2D SnSe nanosheets. Herein, local structure transformation of a 2D SnSe nanosheet into SnSe2 under high temperature is characterized by a novel atomic force microscope (AFM)‐based nanoscale thermomechanical method. Based on an AFM platform, the temperature‐dependent nanomechanical properties are investigated. A softness process is found to occur upon the surface of 2D SnSe, accompanying the structure transformation under high temperature. It means that the generation of SnSe2 is due to the structure collapse of SnSe, stemming from the evaporation of Sn atoms under about 90 °C. The transformation mechanism is further verified by a real‐time nanothermomechanical method. A deeper understanding of the thermal stability and thermal decomposition mechanism of 2D SnSe is promoted. The improved in situ nanomechanical method offers a highly sensitive method to probing the nanomechanical properties of 2D materials.

Photoinduced Thermal Desorption on an Atomic Force Microscope Platform Coupled with Mass Spectrometry for Multimodal Imaging

Photoinduced Thermal Desorption on an Atomic Force Microscope Platform Coupled with Mass Spectrometry for Multimodal Imaging

Feedback control of local hotspot temperature using resistive on-substrate nanoheater/thermometer.

This article reports the active control of a local hotspot temperature for accurate nanoscale thermal transport measurement. To this end, we have fabricated resistive on-substrate nanoheater/thermometer (NH/T) devices that have a sensing area of ∼350 nm × 300 nm. Feedback-controlled temporal heating and cooling experiments of the NH/T device confirm that the feedback integral gain plays a dominant role in device's response time for various setpoint temperatures. To further verify the integration of the feedback controller with the NH/T devices, a local tip-induced cooling experiment is performed by scanning a silicon tip over the hotspot area in an atomic force microscope platform. By carefully optimizing the feedback gain and the tip scan speed, we can control the hotspot temperature with the accuracy of ∼±1 K for a broad range of setpoints from 325 K to 355 K. The obtained tip-substrate thermal conductance, including the effects of solid-solid conduction, water meniscus, air conduction, and near-field thermal radiation, is found to be a slightly increasing function of temperature in the range of 127 ± 25 to 179 ± 16 nW/K. Our work demonstrates the reliable controllability of a local hotspot temperature, which will allow the further improvement of various nanoscale thermal metrologies including scanning thermal microscopy and nanoscale thermometry.

Development of in-situ high-voltage and high-temperature stressing capability on atomic force microscopy platform

Reliability has become an increasingly important issue as photovoltaic technologies mature. However, researching reliability at the nanometer scale is in its infancy; in particular, in-situ studies have not been reported to date. Here, to investigate potential-induced degradation (PID) of solar cell modules, we have developed an in-situ stressing capability with applied high voltage (HV) and high temperature (HT) on an atomic force microscopy (AFM) platform. We designed a sample holder to simultaneously accommodate 1000-V HV and 200°C HT stressing. Three technical challenges have been overcome along with the development: thermal drift at HT, HV interference with measurement, and arc discharge caused by HV. We demonstrated no observable measurement artifact under the stress conditions. Based on our in-situ stressing AFM, Kelvin probe force microscopy potential imaging revealed the evolution of electrical potential across the junction along with the PID stressing time, which provides vital information to further study the PID mechanism.

G-mode magnetic force microscopy: Separating magnetic and electrostatic interactions using big data analytics

In this work, we develop a full information capture approach for Magnetic Force Microscopy (MFM), referred to as generalized mode (G-Mode) MFM. G-Mode MFM acquires and stores the full data stream from the photodetector, captured at sampling rates approaching the intrinsic photodiode limit. The data can be subsequently compressed, denoised, and analyzed, without information loss. Here, G-Mode MFM is implemented and compared to the traditional heterodyne-based MFM on model systems, including domain structures in ferromagnetic Yttrium Iron Garnet and the electronically and magnetically inhomogeneous high entropy alloy, CoFeMnNiSn. We investigate the use of information theory to mine the G-Mode MFM data and demonstrate its usefulness for extracting information which may be hidden in traditional MFM modes, including signatures of nonlinearities and mode-coupling phenomena. Finally, we demonstrate detection and separation of magnetic and electrostatic tip-sample interactions from a single G-Mode image, by analyzing the entire frequency response of the cantilever. G-Mode MFM is immediately implementable on any atomic force microscopy platform and as such is expected to be a useful technique for probing spatiotemporal cantilever dynamics and mapping material properties, as well as their mutual interactions.

Focus on materials, semiconductors, vacuum, and cryogenics

Focus on materials, semiconductors, vacuum, and cryogenics

Multifrequency spectrum analysis using fully digital G Mode-Kelvin probe force microscopy

Since its inception over two decades ago, Kelvin probe force microscopy (KPFM) has become the standard technique for characterizing electrostatic, electrochemical and electronic properties at the nanoscale. In this work, we present a purely digital, software-based approach to KPFM utilizing big data acquisition and analysis methods. General mode (G-Mode) KPFM works by capturing the entire photodetector data stream, typically at the sampling rate limit, followed by subsequent de-noising, analysis and compression of the cantilever response. We demonstrate that the G-Mode approach allows simultaneous multi-harmonic detection, combined with on-the-fly transfer function correction—required for quantitative CPD mapping. The KPFM approach outlined in this work significantly simplifies the technique by avoiding cumbersome instrumentation optimization steps (i.e. lock in parameters, feedback gains etc), while also retaining the flexibility to be implemented on any atomic force microscopy platform. We demonstrate the added advantages of G-Mode KPFM by allowing simultaneous mapping of CPD and capacitance gradient (C′) channels as well as increased flexibility in data exploration across frequency, time, space, and noise domains. G-Mode KPFM is particularly suitable for characterizing voltage sensitive materials or for operation in conductive electrolytes, and will be useful for probing electrodynamics in photovoltaics, liquids and ionic conductors.

Simultaneous differential spinning disk fluorescence optical sectioning microscopy and nanomechanical mapping atomic force microscopy.

Combined microscopy techniques offer the life science research community a powerful tool to investigate complex biological systems and their interactions. Here, we present a new combined microscopy platform based on fluorescence optical sectioning microscopy through aperture correlation microscopy with a Differential Spinning Disk (DSD) and nanomechanical mapping with an Atomic Force Microscope (AFM). The illumination scheme of the DSD microscope unit, contrary to standard single or multi-point confocal microscopes, provides a time-independent illumination of the AFM cantilever. This enables a distortion-free simultaneous operation of fluorescence optical sectioning microscopy and atomic force microscopy with standard probes. In this context, we discuss sample heating due to AFM cantilever illumination with fluorescence excitation light. Integration of a DSD fluorescence optical sectioning unit with an AFM platform requires mitigation of mechanical noise transfer of the spinning disk. We identify and present two solutions to almost annul this noise in the AFM measurement process. The new combined microscopy platform is applied to the characterization of a DOPC/DOPS (4:1) lipid structures labelled with a lipophilic cationic indocarbocyanine dye deposited on a mica substrate.

In situ probing the interior of single bacterial cells at nanometer scale

We report a novel approach to probe the interior of single bacterial cells at nanometre resolution by combining focused ion beam (FIB) and atomic force microscopy (AFM). After removing layers of pre-defined thickness in the order of 100 nm on the target bacterial cells with FIB milling, AFM of different modes can be employed to probe the cellular interior under both ambient and aqueous environments. Our initial investigations focused on the surface topology induced by FIB milling and the hydration effects on AFM measurements, followed by assessment of the sample protocols. With fine-tuning of the process parameters, in situ AFM probing beneath the bacterial cell wall was achieved for the first time. We further demonstrate the proposed method by performing a spatial mapping of intracellular elasticity and chemistry of the multi-drug resistant strain Klebsiella pneumoniae cells prior to and after it was exposed to the ‘last-line’ antibiotic polymyxin B. Our results revealed increased stiffness occurring in both surface and interior regions of the treated cells, suggesting loss of integrity of the outer membrane from polymyxin treatments. In addition, the hydrophobicity measurement using a functionalized AFM tip was able to highlight the evident hydrophobic portion of the cell such as the regions containing cell membrane. We expect that the proposed FIB–AFM platform will help in gaining deeper insights of bacteria–drug interactions to develop potential strategies for combating multi-drug resistance.

Automated Manipulation of Carbon Nanotubes Using Atomic Force Microscopy

The manipulation of carbon nanotubes is an important and essential step for carbon-based nanodevice or nanocircuit assembly. However, the conventional push-and-image approach of manipulating carbon nanotubes using atomic force microscopy has low efficiency on account of the reduplicated scanning process during manipulation. In this article, an automated manipulation system is designed and tested. This automated manipulation system, which includes an atomic force microscope platform and a self-developed computer program for one-dimensional manipulation, is capable of automatically moving any assigned individual carbon nanotube to a defined target location without any intermediate scanning procedure. To demonstrate the high-efficiency of this automated manipulation system and its potential applications in nanoassembly, two experiments were conducted. The first experiment used this system to manipulate a carbon nanotube to a defined target location. In the second experiment, this system was used to automatically manipulate several carbon nanotubes for generating and translating a defined pattern of nanotubes.

Deep and Alignment Free Patterned Etching of GaN Surface Using an Atomic Force Microscope

Successful deep and alignment-free patterned etching on GaN using atomic force microscope (AFM) local oxidation followed by in-situ chemical etching is demonstrated. Oxide ridges are grown on GaN on an AFM by applying positive sample bias at 80% humidity, with the oxidation reaction expedited by UV light. The oxide ridges are then etched by HCl solution, leaving troughs in the GaN surface. A dripping strategy for the in-situ chemical etching is recommended that allows deep, alignment-free multiple AFM oxidation/etching works on the GaN surface without any need of substrate removal from the AFM platform. Repeated etching followed by AFM oxidation on a spot on a GaN surface resulting in a hole as deep as 800 nm was also demonstrated. Further, a preliminary evaluation of the porosity of the AFM-grown oxide indicates that the oxide ridges grown on GaN at an AFM cantilever moving speed of 300 nm/s are porous in structure, with an estimated porosity of 86%, which porosity could be reduced if longer resident time of the AFM cantilever on the target oxidation region was used.

Design, characterization and evaluation of high performance 2.8 μm pitch zero space microlens

Utilization of the zero space microlens technology can significantly improve the image quality of CMOS sensors. In this study, we present systematical data of design, simulation, characterization and silicon level testing during the initial stage of development of the zero space microlens based CMOS imaging technology. The optimal structure of zero space microlens was obtained based on the simulation results. Sample CMOS image sensors with a 2.8 μm pitch zero space microlens above each pixel have been successfully fabricated based on 0.18 μm CMOS technology. Using AFM (atomic force microscopy) and sensor test platform, the structural and optical properties of both space microlens and zero space microlens have been characterized, and their performances have been evaluated respectively. Both AFM results and silicon tests have demonstrated that the 2.8 μm pitch zero space microlens can remarkably improve the pixel sensitivity and pixel array non-uniformity, and reduce the optical crosstalk. Compared to the space 2.8 μm square microlens, the zero space microlens shows 78.83% (68.42% and 75.93%) enhancement of photosensitivity and increment of pixel non-uniformity up to 20% (45.6% and 30.77%) for R (G and B), and reduction of the optical crosstalk up to 44.49%, under 45 lux light and 30 ms exposure time. In addition, the zero space microlens has also shown a great potential in further reducing pixel size down to less than 2.8 μm and meanwhile improving imaging performance of CMOS image sensors.

Imaging Electron Transport across Grain Boundaries in an Integrated Electron and Atomic Force Microscopy Platform: Application to Polycrystalline Silicon Solar Cells

AbstractWe have investigated the local electron transport in polycrystalline silicon (pc-Si) thin-films by atomic force microscopy (AFM)-based measurements of the electron-beam-induced current (EBIC). EVA solar cells are produced at UNSW by <i>EVAporation</i> of a-Si and subsequent <i>solid-phase crystallization</i>–a potentially cost-effective approach to the production of pc-Si photovoltaics. A fundamental understanding of the electron transport in these pc-Si thin films is of prime importance to address the factors limiting the efficiency of EVA solar cells. EBIC measurements performed in combination with an AFM integrated inside an electron microscope can resolve the electron transport across individual grain boundaries. AFM-EBIC reveals that most grain boundaries present a high energy barrier to the transport of electrons for both p-type and n-type EVA thin-films. Furthermore, for p-type EVA pc-Si, in contrast with n-type, charged grain boundaries are seen. Recombination at grain boundaries seems to be the dominant factor limiting the efficiency of these pc-Si solar cells.

Iterative control approach to high-speed force-distance curve measurement using AFM: Time-dependent response of PDMS example

Force–distance curve measurements using atomic force microscope (AFM) has been widely used in a broad range of areas. However, currently force-curve measurements are hampered the its low speed of AFM. In this article, a novel inversion-based iterative control technique is proposed to dramatically increase the speed of force-curve measurements. Experimental results are presented to show that by using the proposed control technique, the speed of force-curve measurements can be increased by over 80 times—with no loss of spatial resolution—on a commercial AFM platform and with a standard cantilever. High-speed force curve measurements using this control technique are utilized to quantitatively study the time-dependent elastic modulus of poly(dimethylsiloxane) (PDMS). The force-curves employ a broad spectrum of push-in (load) rates, spanning two-order differences. The elastic modulus measured at low-speed compares well with the value obtained from dynamic mechanical analysis (DMA) test, and the value of the elastic modulus increases as the push-in rate increases, signifying that a faster external deformation rate transitions the viscoelastic response of PDMS from that of a rubbery material toward a glassy one.

Piezoresistive cantilever array for life sciences applications

Atomic Force Microscopy (AFM) techniques are used with one- or two-dimensional arrays of piezoresistive probes for parallel imaging. We present a newly designed AFM platform to drive these passivated piezoresistive cantilever arrays in air and liquid environments. Large area imaging in liquid as well as qualitative and quantitative analysis of biological cells are demonstrated by the means of piezoresistive cantilever for the first time to our knowledge. Noise limitations in topography and force resolutions of these piezolevers are quantified.

Direct nanoscale dehydration of hydrogen bonds

The removal of surrounding water strengthens and stabilizes pre-formed intramolecular hydrogen bonds in soluble proteins. This dehydration contributes to determining the cooperative nature of protein folding because the formation of hydrogen-bond microenvironments involves additional residues besides those paired by the hydrogen bond itself. Here we report on a molecular force probe used to assess the dehydration propensity of a pre-formed hydrogen bond, describing an experiment geared at probing the force exerted on a nonpolar group by a solvent-exposed hydrogen bond. Thus, an atomic-force microscopy platform is adapted to translate the dehydration propensity into a measurable force orthogonal to the coulombic field. This force results from the local decrease in water polarization around the hydrogen bond caused by the approach of a nonpolar group.

Tip-induced oxidative nano-machining of conducting diamond-like carbon (DLC)

Electrically conducting diamond-like carbon films have been nano-machined by local deposition of thermal energy at the tip-to-film point of contact; the process is implemented on an atomic force microscope platform. Features with linewidth resolution down to 20 nm have been demonstrated; lateral irregularities along edges were less than 5 nm, while the radius of curvature at the edges was less than 10 nm; and the slope of features was limited by the aspect ratio of the tip. The mechanism arises from prompt thermal oxidation by intermittent transfer of heat from an ohmically heated tip, where Fowler–Nordheim tunnelling is likely to play a role in completing an electrical circuit when the physical continuity of the thermal circuit is interrupted. When heat transfer is insufficient to ensure prompt oxidation, then formation of a metastable low-density carbon phase is found to take place. That phase will then, at room temperature and in the presence of oxygen, relax back to a ‘normal’ higher density phase over a period of one hour. The many desirable physico-chemical properties of diamond-like carbon, in combination with the good spatial resolution of local probe methodology, suggest that the outcomes could have significant implications for next-generation nano-machine and nano-templating technologies.

Combined force and photonic probe microscope with single molecule sensitivity

Direct integration of atomic force microscopy (AFM) imaging with single molecule optical detection promises to combine the resolving power of AFM with the chemical identification capabilities of optical techniques. We present a straightforward experimental approach to achieving such integration. Our design allows simultaneous acquisition of topographical images and optical images with single molecule sensitivity at any region of the optical spectrum. We describe an instrument that combines atomic force microscopy and scanning confocal optical microscopy in a single multifunctional setup that maximizes the use of commercially available parts. To build this instrument we replaced the built-in piezoscanner of a commercial optical microscope–AFM platform with an external scanner that translates the sample. We also added a simple circuit to the setup that modulates the AFM head laser and synchronizes collection of the AFM and optical data in interleave scanning mode. Finally, we demonstrate the technique’s identification capabilities using a model system of dye-labeled beads.

Versatile scanning near-field optical microscope for material science applications

We describe an aperture emission mode scanning near-field optical microscope (SNOM), optimized for material surface science applications. This instrument can be operated in both transmission and reflection configurations, in order to investigate transparent as well as opaque samples. It employs optical shear-force detection for tip/sample distance control, designed to minimize interference with the probe light. The SNOM head has been fully integrated on a homemade atomic force microscope platform and is placed in a controlled atmosphere chamber for reduction of surface contaminants. Within the compactness and the versatility obtained in our instrument, we have been able to optically discriminate different materials with a λ/20 lateral resolution, and to distinguish polymeric aggregates, without damaging the surface, in spite of their rather poor optical contrast.