We present a combined scanning force and tunneling microscope working in a dilution refrigerator that is optimized for the study of individual electronic nano-devices. This apparatus is equipped with commercial piezo-electric positioners enabling the displacement of a sample below the probe over several hundred microns at very low temperature, without excessive heating. Atomic force microscopy based on a tuning fork resonator probe is used for cryogenic precise alignment of the tip with an individual device. We demonstrate the local tunneling spectroscopy of a hybrid Josephson junction as a function of its current bias.
In this work, we report the integration of an atomic force microscope (AFM) into a helium ion microscope (HIM). The HIM is a powerful instrument, capable of sub-nanometer resolution imaging and machining of nanoscale structures, while the AFM is a well-established versatile tool for multiparametric nanoscale characterization. Combining the two techniques opens the way for unprecedented, in situ, correlative analysis at the nanoscale. Nanomachining and analysis can be performed without contamination of the sample and environmental changes between processing steps. The practicality of the result…
The Scanning Tunneling Microscope is a powerful tool for studying the electronic properties at the atomic level, however it's relatively small scanning range and the fact that it can only operate on conducting samples prevents its application to study heterogeneous samples consisting on conducting and insulating regions. Here we present a long-range scanning tunneling microscope capable of detecting conducting micro and nanostructures on insulating substrates using a technique based on the capacitance between the tip and the sample and performing STM studies.
A scheme of the scanning rotational microscope is designed. This scheme is based on using carbon nanotubes simultaneously as a probe tip and as a bolt/nut pair which converts translational displacements of two piezo actuators into pure rotation of the probe tip. First-principles calculations of the interaction energy between movable and rotational parts of the microscope confirms the capability for its operation. The scanning rotational microscope with a chemically functionalized nanotube-based tip can be used to study how the interaction between individual molecules or a molecule and a surfac…
An atomic force microscope is used to structure a film of multilayer graphene. The resistance of the sample was measured in-situ during nanomachining a narrow trench. We found a reversible behavior in the electrical resistance which we attribute to the movement of dislocations. After several attempts also permanent changes are observed. Two theoretical approaches are presented to approximate the measured resistance.
We report on the fabrication of nanocontacts by indentation of an ultrathin insulating photoresist layer deposited on various types of conductive structures. A modified atomic force microscope (AFM) designed for local resistance measurements is used as a nanoindenter. The nanoindentation is performed while measuring continuously the resistance between the conductive tip of the AFM and the conductive layer, which is used as the trigger parameter to stop the indentation. This allows an extremely accurate control of the indentation process. The indented hole is subsequently filled by a metal to c…
We summarize our new scanning magnetic 3-D imaging system. This scanning system uses optically detected magnetic resonance in a single nitrogen vacancy center in a diamond nanocrystal. The theoretical analysis and the first experimental demonstrations have proved that this method has single spin sensitivity and a sub-nanoscale spatial resolution at room temperature.
We present a fabrication method of superconducting quantum interference devices (SQUIDs) based on direct write lithography with an Atomic Force Microscope (AFM). This technique involves maskless local anodization of Nb or NbN ultrathin films using the voltage biased tip of the AFM. The SQUIDs are of weak-link type, for which two geometries have been tested: Dayem and variable thickness nanobridges. The magnetic field dependence of the maximum supercurrent Ic(flux) in resulting SQUIDs is thoroughly measured for different weak link geometries and for both tested materials. It is found that the m…
We report low-temperature transport spectroscopy of a graphene quantum dot fabricated by atomic force microscope nanolithography. The excellent spatial resolution of the atomic force microscope allows us to reliably fabricate quantum dots with short constrictions of less than 15 nm in length. Transport measurements demonstrate that the device is dominated by a single quantum dot over a wide gate range. The electron spin system of the quantum dot is investigated by applying an in-plane magnetic field. The results are consistent with a Lande g-factor of 2 but no regular spin filling sequence is …
We use an Atomic Force Microscope (AFM) tip to locally probe the electronic properties of semiconducting carbon nanotube transistors. A gold-coated AFM tip serves as a voltage or current probe in three-probe measurement setup. Using the tip as a movable current probe, we investigate the scaling of the device properties with channel length. Using the tip as a voltage probe, we study the properties of the contacts. We find that Au makes an excellent contact in the p-region, with no Schottky barrier. In the n-region large contact resistances were found which dominate the transport properties.
Nanoscale lithography on SrRuO3 (SRO) thin film surfaces has been performed by scanning tunneling microscopy under ambient conditions. The depth of etched lines increases with increasing bias voltage but it does not change significantly by increasing the tunneling current. The dependence of line width on bias voltage from experimental data is in agreement with theoretical calculation based on field-induced evaporation. Moreover, a three-square nanostructure was successfully created, showing the capability of fabricating nanodevices in SRO thin films.
We use an atomic force microscope (AFM) to manipulate graphene films on a nanoscopic length scale. By means of local anodic oxidation with an AFM we are able to structure isolating trenches into single-layer and few-layer graphene flakes, opening the possibility of tabletop graphene based device fabrication. Trench sizes of less than 30 nm in width are attainable with this technique. Besides oxidation we also show the influence of mechanical peeling and scratching with an AFM of few layer graphene sheets placed on different substrates.
We investigate atomic force microscope nanolithography of single and bilayer graphene. In situ tip current measurements show that cutting of graphene is not current driven. Using a combination of transport measurements and scanning electron microscopy we show that, while indentations accompanied by tip current appear in the graphene lattice for a range of tip voltages, real cuts are characterized by a strong reduction of the tip current above a threshold voltage. The reliability and flexibility of the technique is demonstrated by the fabrication, measurement, modification and re-measurement of…
We conducted local anodic oxidation (LAO) lithography in single-layer, bilayer, and multilayer graphene using tapping-mode atomic force microscope. The width of insulating oxidized area depends systematically on the number of graphene layers. An 800-nm-wide bar-shaped device fabricated in single-layer graphene exhibits the half-integer quantum Hall effect. We also fabricated a 55-nm-wide graphene nanoribbon (GNR). The conductance of the GNR at the charge neutrality point was suppressed at low temperature, which suggests the opening of an energy gap due to lateral confinement of charge carriers…
The quantitative characterization of the degree of randomness and aggregation of surface micro and nanostructures is critical to evaluate their effects on targeted functionalities. To this end, the methods of Point Pattern Analysis (PPA), largely used in ecology and medical imaging, seem to provide a powerful toolset. However, the application of these techniques requires the extraction of the point pattern of nanostructures from their microscope images. In this work, we address the issue of the impact that Scanning Electron Microscope (SEM) image processing may have on the fundamental metric o…
A method is described intended for distributed calibration of a probe microscope scanner consisting in a search for a net of local calibration coefficients (LCCs) in the process of automatic measurement of a standard surface, whereby each point of the movement space of the scanner can be defined by a unique set of scale factors. Feature-oriented scanning (FOS) methodology is used to implement the distributed calibration, which permits to exclude in situ the negative influence of thermal drift, creep and hysteresis on the obtained results. The sensitivity of LCCs to errors in determination of p…
Most methods for optical visualization beyond the diffraction limit rely on fluorescence emission by molecular tags. Here, we report a method for visualization of nanostructures down to a few nanometers using a conventional bright-field microscope without requiring additional molecular tags such as fluorophores. The technique, Bright-field Nanoscopy, is based on the strong thickness dependent color of ultra-thin germanium on an optically thick gold film. We demonstrate the visualization of grain boundaries in chemical vapour deposited single layer graphene and the detection of single 40 nm Ag …
Quantum sensors based on solid-state spins provide tremendous opportunities in a wide range of fields from basic physics and chemistry to biomedical imaging. However, integrating them into a scanning probe microscope to enable practical, nanoscale quantum imaging is a highly challenging task. Recently, the use of single spins in diamond in conjunction with atomic force microscopy techniques has allowed significant progress towards this goal, but generalisation of this approach has so far been impeded by long acquisition times or by the absence of simultaneous topographic information. Here we r…
We report on the experimental demonstration of single photon state generation and characterization in an electron microscope. In this aim we have used low intensity relativistic (energy between 60kV and 100 keV) electrons beams focused in a ca 1 nm probe to excite diamond nanoparticles. This triggered individual neutral Nitrogen-vacancies (NV0) centers to emit photon which could be gathered and sent to a Hanbury Brown Twiss intensity interferometer. The detection of a dip in the correlation function at small time delays clearly demonstrates antibunching and thus the creation of non-classical l…
We describe a scanning device where a single spin is used as an ultrasensitive, nanoscale magnetic field sensor. As this "probe spin" we consider a single nitrogen-vacancy defect center in a diamond nanocrystal, attached to the tip of the scanning device. Changes in the local field seen by the probe spin are detected by optically monitoring its electron paramagnetic resonance transition. The room-temperature scanning device may be useful for performing nanoscale magnetic resonance imaging and spectroscopy, and for the characterization of magnetic nanostructures down to the single atom level.
A method is described intended for distributed calibration of a probe microscope scanner consisting in a search for a net of local calibration coefficients (LCCs) in the process of automatic measurement of a standard surface, whereby each point of the movement space of the scanner can be defined by a unique set of scale factors. Feature-oriented scanning (FOS) methodology is used to implement the distributed calibration, which permits to exclude in situ the negative influence of thermal drift, creep and hysteresis on the obtained results. The sensitivity of LCCs to errors in determination of p…
Multi-tip scanning tunneling microscopy (STM) is a powerful method to perform charge transport measurements at the nanoscale. With four STM tips positioned on the surface of a sample, four-point resistance measurements can be performed in dedicated geometric configurations. Here, we present an alternative to the most often used scanning electron microscope (SEM) imaging to infer the corresponding tip positions. After initial coarse positioning monitored by an optical microscope, STM scanning itself is used to determine the inter-tip distances. A large STM overview scan serves as a reference ma…
We define superconducting constrictions by ploughing a deposited Aluminum film with a scanning probe microscope. The microscope tip is modified by electron beam deposition to form a nano-plough of diamond-like hardness, what allows the definition of highly transparent Josephson junctions. Additionally a dc-SQUID is fabricated to verify appropriate functioning of the junctions. The devices are easily integrated in mesoscopic devices as local radiation sources and can be used as tunable on-chip millimeter wave sources.
Atomic force microscopy (AFM) is an essential nanoinstrument technique for several applications such as cell biology and nanoelectronics metrology and inspection. The need for statistically significant sample sizes means that data collection can be an extremely lengthy process in AFM. The use of a single AFM instrument is known for its very low speed and not being suitable for scanning large areas, resulting in very-low-throughput measurement. We address this challenge by parallelizing AFM instruments. The parallelization is achieved by miniaturizing the AFM instrument and operating many of th…
A method of distributed calibration of a probe microscope scanner is suggested which main idea consists in a search for a net of local calibration coefficients (LCCs) in the process of automatic measurement of a standard surface, whereby each point of the movement space of the scanner can be characterized by a unique set of scale factors. Feature-oriented scanning (FOS) methodology is used as a basis for implementation of the distributed calibration permitting to exclude in situ the negative influence of thermal drift, creep and hysteresis on the obtained results. Possessing the calibration da…
ANTARES beamline (BL), a new soft X-ray scanning photoemission microscope located at the SOLEIL synchrotron storage ring has been recently designed, built and commissioned. The implemented interferometer control allows the accurate measurement of the transverse position of the Fresnel zone plate (FZP) relative to the sample. An effective sample position feedback has been achieved during experiments in static mode, with a fixed FZP position required to perform nano Angle-Resolved Photoelectron Spectroscopy (Nano-ARPES) measurements. Likewise, long-term stability has been attained for the FZP po…
We report electronic measurements on high-quality graphene nanoconstrictions (GNCs) fabricated in a transmission electron microscope (TEM), and the first measurements on GNC conductance with an accurate measurement of constriction width down to 1 nm. To create the GNCs, freely-suspended graphene ribbons were fabricated using few-layer graphene grown by chemical vapor deposition. The ribbons were loaded into the TEM, and a current-annealing procedure was used to clean the material and improve its electronic characteristics. The TEM beam was then used to sculpt GNCs to a series of desired widths…
Imaging of the optical properties of individual nanosystems beyond fluorescence can provide a wealth of information. However, the minute signals for absorption and dispersion are challenging to observe, and only specialized techniques requiring sophisticated noise rejection are available. Here we use signal enhancement in a scanning optical microcavity to demonstrate ultra-sensitive imaging. Harnessing multiple interactions of probe light with a sample within an optical resonator, we achieve a 1700-fold signal enhancement compared to diffraction-limited microscopy. We demonstrate quantitative …
Nitrogen-vacancy (NV) center in diamond is a promising quantum sensor with remarkably versatile sensing capabilities. While scanning NV magnetometry is well-established, NV electrometry has been so far limited to bulk diamonds. Here we demonstrate imaging external alternating (AC) and direct (DC) electric fields with a single NV at the apex of a diamond scanning tip under ambient conditions. A strong electric field screening effect is observed at low frequencies due to charge noise on the surface. We quantitatively measure its frequency dependence, and overcome this screening by mechanically o…
We have combined direct nanofabrication by local anodic oxidation with conventional electron-beam lithography to produce a parallel double quantum dot based on a GaAs/AlGaAs heterostructure. The combination of both nanolithography methods allows to fabricate robust in-plane gates and Cr/Au top gate electrodes on the same device for optimal controllability. This is illustrated by the tunability of the interdot coupling in our device. We describe our fabrication and alignment scheme in detail and demonstrate the tunability in low-temperature transport measurements.
We demonstrate a simple method to significantly improve the sharpness of standard silicon probes for an atomic force microscope, or to repair a damaged probe. The method is based on creating and maintaining a strong, spatially localized electric field in the air gap between the probe tip and the surface of conductive sample. Under these conditions, nanostructure growth takes place on both the sample and the tip. The most likely mechanism is the decomposition of atmospheric adsorbate with subsequent deposition of carbon structures. This makes it possible to grow a spike of a few hundred nanomet…
We describe a new type of scanning probe microscope based on a superconducting quantum interference device (SQUID) that resides on the apex of a sharp tip. The SQUID-on-tip is glued to a quartz tuning fork which allows scanning at a tip-sample separation of a few nm. The magnetic flux sensitivity of the SQUID is 1.8 μ_0/Hz^{1/2} and the spatial resolution is about 200 nm, which can be further improved. This combination of high sensitivity, spatial resolution, bandwidth, and the very close proximity to the sample provides a powerful tool for study of dynamic magnetic phenomena on the nanoscale.…
We demonstrate a scanning force microscope, based upon a quartz tuning fork, that operates below 100 mK and in magnetic fields up to 6 T. The microscope has a conducting tip for electrical probing of nanostructures of interest, and it incorporates a low noise cryogenic amplifier to measure both the vibrations of the tuning fork and the electrical signals from the nanostructures. At millikelvin temperatures the imaging resolution is below 1 um in a 22 um x 22 um range, and a coarse motion provides translations of a few mm. This scanned probe is useful for high bandwidth measurement of many high…
Two-probe electronic transport measurements on a Molybdenum Disulphide (MoS_2) surface were performed at low temperature (30K) under ultra-high vacuum conditions. Two scanning tunneling microscope tips were precisely positioned in tunneling contact to measure the surface current-voltage characteristics. The separation between the tips is controllably varied and measured using a high resolution scanning electron microscope. The MoS_2 surface shows a surface electronic gap (E_S) of 1.4eV measured at a probe separation of 50nm. Furthermore, the two- probe resistance measured outside the electroni…
An atomic force microscope is used to structure a film of multilayer graphene. The resistance of the sample was measured in-situ during nanomachining narrow trenches. We found a reversible behavior in the electrical resistance which we attribute to the movement of dislocations. After several attempts also permanent changes are observed.
A low-temperature ultra-high-vacuum scanning probe microscope with in situ electronic transport capabilities: from macro to nano in 10 minutes
Universidad Autónoma de Madrid（马德里自治大学）；Condensed Matter Physics Center (IFIMAC), Universidad Autónoma de Madrid（马德里自治大学凝聚态物理中心（IFIMAC））；Instituto Nicolás Cabrera (INC), Universidad Autónoma de Madrid（马德里自治大学尼科拉斯·卡布雷拉研究所（INC））；National Institute for Materials Science (NIMS)（国立材料研究所）
Patterning graphene into various mesoscopic devices such as nanoribbons, quantum dots, etc. by lithographic techniques has enabled the guiding and manipulation of graphene's Dirac-type charge carriers. Graphene, with well-defined strain patterns, holds promise of similarly rich physics while avoiding the problems created by the hard to control edge configuration of lithographically prepared devices. To engineer the properties of graphene via mechanical deformation, versatile new techniques are needed to pattern strain profiles in a controlled manner. Here we present a process by which strain c…
The junction of a scanning tunneling microscope (STM) operating in the tunneling regime was irradiated with femtosecond laser pulses. A photo-excited hot electron in the STM tip resonantly tunnels into an excited state of a single molecule on the surface, converting it from the neutral to the anion. The electron transfer rate depends quadratically on the incident laser power, suggesting a two-photon excitation process. This nonlinear optical process is further confirmed by the polarization measurement. Spatial dependence of the electron transfer rate exhibits atomic-scale variations. A two-pul…
Magnetic microscopy that combines nanoscale spatial resolution with picosecond scale temporal resolution uniquely enables direct observation of the spatiotemporal magnetic phenomena that are relevant to future high-speed, high-density magnetic storage and logic technologies. Magnetic microscopes that combine these metrics has been limited to facility-level instruments. To address this gap in lab-accessible spatiotemporal imaging, we develop a time-resolved near-field magnetic microscope based on magneto-thermal interactions. We demonstrate both magnetization and current density imaging modalit…
The electroluminescence of molecules confined inside a nanocavity in the scanning tunneling microscopy possesses many intriguing but unexplained features. We present here a general theoretical approach based on the density matrix formalism to describe the electroluminescence from molecules near a metal surface induced by both electron tunneling and local surface plasmon excitations simultaneously. It reveals the underlying physical mechanism for the external bias dependent electroluminescence. The important role played by the local surface plasmon on the electroluminescence is highlighted. Cal…
