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At least 919 records · Page 51

Atomic resolution scanning tunneling microscopy in a cryogen free dilution refrigerator at 15 mK

Pulse tube refrigerators are becoming more common, because they are cost efficient and demand less handling than conventional (wet) refrigerators. However, a downside of a pulse tube system is the vibration level at the cold-head, which is in most designs several micrometers. We implemented vibration isolation techniques which significantly reduced vibration levels at the experiment. These optimizations were necessary for the vibration sensitive magnetic resonance force microscopy experiments at milli-kelvin temperatures for which the cryostat is intended. With these modifications we show atomic resolution scanning tunneling microscopy on graphite. This is promising for scanning probe microscopy applications at very low temperatures.

42 ENGINEERING↗

Imaging of buried phosphorus nanostructures in silicon using scanning tunneling microscopy

We demonstrate the locating and imaging of single phosphorus atoms and phosphorus dopant nanostructures, buried beneath the Si(001) surface using scanning tunneling microscopy. The buried dopant nanostructures have been fabricated in a bottom-up approach using scanning tunneling microscope lithography on Si(001). We find that current imaging tunneling spectroscopy is suited to locate and image buried nanostructures at room temperature and with residual surface roughness present. From these studies, we can place an upper limit on the lateral diffusion during encapsulation with low-temperature Si molecular beam epitaxy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Plasma etching of superconducting Niobium tips for scanning tunneling microscopy

We have developed a reproducible technique for the fabrication of sharp superconducting Nb tips for scanning tunneling microscopy (STM) and scanning tunneling spectroscopy. Sections of Nb wire with 250 μm diameter are dry etched in an SF₆ plasma in a Reactive Ion Etcher. The gas pressure, etching time, and applied power are chosen to control the ratio of isotropic to anisotropic etch rates and produce the desired tip shape. The resulting tips are atomically sharp, with radii of less than 100 nm, mechanically stable, and superconducting. They generate good STM images and spectroscopy on single crystal samples of Au(111), Au(100), and Nb(100), as well as a doped topological insulator Bi₂Se₃ at temperatures ranging from 30 mK to 9 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Phase modulation mode of scanning ion conductance microscopy

This Letter reports a phase modulation (PM) mode of scanning ion conductance microscopy. In this mode, an AC current is directly generated by an AC voltage between the electrodes. The portion of the AC current in phase with the AC voltage, which is the current through the resistance path, is modulated by the tip-sample distance. It can be used as the input of feedback control to drive the scanner in Z direction. The PM mode, taking the advantages of both DC mode and traditional AC mode, is less prone to electronic noise and DC drift but maintains high scanning speed. The effectiveness of the PM mode has been proven by experiments.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

High-stability cryogenic scanning tunneling microscope based on a closed-cycle cryostat

We report on the design and operation of a cryogenic ultra-high vacuum (UHV) scanning tunneling microscope (STM) coupled to a closed-cycle cryostat (CCC). The STM is thermally linked to the CCC through helium exchange gas confined inside a volume enclosed by highly flexible rubber bellows. The STM is thus mechanically decoupled from the CCC, which results in a significant reduction of the mechanical noise transferred from the CCC to the STM. Noise analysis of the tunneling current shows current fluctuations up to 4% of the total current, which translates into tip-sample distance variations of up to 1.5 picometers. This noise level is sufficiently low for atomic-resolution imaging of a wide variety of surfaces. To demonstrate this, atomic-resolution images of Au(111) and NaCl(100)/Au(111) surfaces, as well as of carbon nanotubes deposited on Au(111), were obtained. Thermal drift analysis showed that under optimized conditions, the lateral stability of the STM scanner can be as low as 0.18 Å/h. Scanning Tunneling Spectroscopy measurements based on the lock-in technique were also carried out, and showed no detectable presence of noise from the closed-cycle cryostat. Using this cooling approach, temperatures as low as 16 K at the STM scanner have been achieved, with the complete cool-down of the system typically taking up to 12 h. These results demonstrate that the constructed CCC-coupled STM is a highly stable instrument capable of highly detailed spectroscopic investigations of materials and surfaces at the atomic scale.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Novel scanning electron microscope bulge test technique integrated with loading function

Membranes and film-on-substrate structures are critical elements for some devices in electronics industry and for Micro Electro Mechanical Systems devices. These structures are normally at the scale of micrometer or even nanometer. Thus, the measurement for the mechanical property of these membranes poses a challenge over the conventional measurements at macro-scales. In this study, a novel bulge test method is presented for the evaluation of mechanical property of micro thin membranes. Three aspects are discussed in the study: (a) A novel bulge test with a Scanning Electron Microscope system realizing the function of loading and measuring simultaneously; (b) a simplified Digital Image Correlation method for a height measurement; and (c) an imaging distortion correction by the introduction of a scanning Moiré method. Combined with the above techniques, biaxial modulus as well as Young's modulus of the polyimide film can be determined. Besides, a standard tensile test is conducted as an auxiliary experiment to validate the feasibility of the proposed method.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Investigation of surface defect states in CeO{sub 2-y} nanocrystals by Scanning−tunneling microscopy/spectroscopy and ellipsometry

Synthesis process strongly influences the nanocrystalline CeO{sub 2-y} defective structure. The presence of surface defects, in the form of oxygen vacancies in different charge states (F centers), can change the electronic properties of ceria nanocrystals. Nanocrystalline CeO{sub 2-y} samples were synthesized using three different methods (precipitation, self-propagating room temperature, and hydrothermal synthesis). Raman spectroscopy was used to identify the presence of oxygen vacancies which presumably were formed at the nanoparticle surface. The defect concentration depended on the crystallite size of differently prepared CeO{sub 2-y} samples. Scanning tunneling microscopy/spectroscopy and ellipsometry were employed to investigate the electronic band structure of defective CeO{sub 2-y} nanocrystals. Scanning tunneling spectroscopy measurements demonstrated that inside the band gap of CeO{sub 2-y} nanocrystals, besides the filled 4 f states, appeared additional states which were related to occupied and empty F center defect states. From the ellipsometric measurements, using the critical points model, the energy positions of different F centers states and the values of the reduced band gap energies were determined. The analysis of obtained data pointed out that depending on the synthesis method, different types of F centers (F{sup +} and F{sup 0}) can be formed in the CeO{sub 2-y} nanocrystals. The formation of different F center defect states inside the ceria gap have a strong impact on the electrical, optical, and magnetic properties of ceria nanocrystals.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Three axis vector magnet set-up for cryogenic scanning probe microscopy

We describe a three axis vector magnet system for cryogenic scanning probe microscopy measurements. We discuss the magnet support system and the power supply, consisting of a compact three way 100 A current source. We obtain tilted magnetic fields in all directions with maximum value of 5T along z-axis and of 1.2T for XY-plane magnetic fields. We describe a scanning tunneling microscopy-spectroscopy (STM-STS) set-up, operating in a dilution refrigerator, which includes a new high voltage ultralow noise piezodrive electronics and discuss the noise level due to vibrations. STM images and STS maps show atomic resolution and the tilted vortex lattice at 150 mK in the superconductor β-Bi{sub 2}Pd. We observe a strongly elongated hexagonal lattice, which corresponds to the projection of the tilted hexagonal vortex lattice on the surface. We also discuss Magnetic Force Microscopy images in a variable temperature insert.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Atomic-scale electrochemistry on the surface of a manganite

The doped manganese oxides (manganites) have been widely studied for their colossal magnetoresistive effects, for potential applications in oxide spintronics, electroforming in resistive switching devices, and are materials of choice as cathodes in modern solid oxide fuel cells. However, little experimental knowledge of the dynamics of the surfaces of perovskite manganites at the atomic scale exists. Here, through in-situ scanning tunnelling microscopy (STM), we demonstrate atomic resolution on samples of La 0.625 Ca 0.375 MnO 3 grown on (001) SrTiO 3 by pulsed laser deposition (PLD). Furthermore, by applying triangular DC waveforms of increasing amplitude to the STM tip, and measuring the tunnelling current, we demonstrate the ability to both perform and monitor surface electrochemical processes at the atomic level, including, for the first time in a manganite, formation of single and multiple oxygen vacancies, disruption of the overlying manganite layers, and removal and deposition of individual atomic units or clusters. Our work paves the way for better understanding of surface oxygen reactions in these systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Influence of mechanical noise inside a scanning electron microscope

The scanning electron microscope is becoming a popular tool to perform tasks that require positioning, manipulation, characterization, and assembly of micro-components. However, some of these applications require a higher level of performance with respect to dynamics and precision of positioning. One limiting factor is the presence of unidentified noises and disturbances. This work aims to study the influence of mechanical disturbances generated by the environment and by the microscope, identifying how these can affect elements in the vacuum chamber. To achieve this objective, a dedicated setup, including a high-resolution vibrometer, was built inside the microscope. This work led to the identification and quantification of main disturbances and noise sources acting on a scanning electron microscope. Furthermore, the effects of external acoustic excitations were analysed. Potential applications of these results include noise compensation and real-time control for high accuracy tasks.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Surface characterization of InP trenches embedded in oxide using scanning probe microscopy

Metrology for structural and electrical analyses at device level has been identified as one of the major challenges to be resolved for the sub-14 nm technology nodes. In these advanced nodes, new high mobility semiconductors, such as III–V compounds, are grown in narrow trenches on a Si substrate. Probing the nature of the defects, the defect density, and the role of processing steps on the surface of such structures are prime metrology requirements. In order to enable defect analysis on a (III–V) surface, a proper sample preparation for oxide removal is of primary importance. In this work, the effectiveness of different chemical cleanings and thermal annealing procedures is investigated on both blanket InP and oxide embedded InP trenches by means of scanning probe microscopy techniques. It is found that the most effective approach is a combination of an HCl-based chemical cleaning combined with a low-temperature thermal annealing leading to an oxide free surface with atomically flat areas. Scanning tunneling microscopy (STM) has been the preferred method for such investigations on blanket films due to its intrinsic sub-nm spatial resolution. However, its application on oxide embedded structures is non-trivial. To perform STM on the trenches of interest (generally <20 nm wide), we propose a combination of non-contact atomic force microscopy and STM using the same conductive atomic force microscopy tip Our results prove that with these procedures, it is possible to perform STM in narrow InP trenches showing stacking faults and surface reconstruction. Significant differences in terms of roughness and terrace formation are also observed between the blanket and the oxide embedded InP.

36 MATERIALS SCIENCE↗

Spin-polarized scanning tunneling microscopy experiments on the rough surface of a polycrystalline NiFe film with a fine magnetic tip sensitive to a well-defined magnetization component

We developed a micrometer-sized magnetic tip integrated onto the write head of a hard disk drive for spin-polarized scanning tunneling microscopy (SP-STM) in the modulated tip magnetization mode. Using SP-STM, we measured a well-defined in-plane spin-component of the tunneling current of the rough surface of a polycrystalline NiFe film. The spin asymmetry of the NiFe film was about 1.3% within the bias voltage range of -3 to 1 V. We obtained the local spin component image of the sample surface, switching the magnetic field of the sample to reverse the sample magnetization during scanning. We also obtained a spin image of the rough surface of a polycrystalline NiFe film evaporated on the recording medium of a hard disk drive.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Note: Electron energy spectroscopy mapping of surface with scanning tunneling microscope

We report a novel scanning probe electron energy spectrometer (SPEES) which combines a double toroidal analyzer with a scanning tunneling microscope to achieve both topography imaging and electron energy spectroscopy mapping of surface in situ. The spatial resolution of spectroscopy mapping is determined to be better than 0.7 ± 0.2 μm at a tip sample distance of 7 μm. Meanwhile, the size of the field emission electron beam spot on the surface is also measured, and is about 3.6 ± 0.8 μm in diameter. This unambiguously demonstrates that the spatial resolution of SPEES technique can be much better than the size of the incident electron beam.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A robust high sensitivity scanning thermal probe for simultaneous microscale thermal and thermoelectric property mapping

Scanning Thermal Microscopy (SThM) provides efficient thermal property measurement with micro- or nanoscale spatial resolution. However, the sensitivity and accuracy of state-of-the-art thermal probes have been limited by excessive thermal contact resistance between the probe and sample. Introduced herein is a robust thermal microprobe that can increase the probe-sample contact force by more than two orders of magnitude, thereby reducing the probe-sample thermal contact resistance by as much as 96% and increasing measurement sensitivity by more than 240% compared to a commercial thermal probe with the same dimensions and measurement principle. The relationship between the probe-sample thermal contact resistance, thermal exchange radius, and sample thermal conductivity is determined experimentally. Simultaneous measurement of thermal conductivity and Seebeck coefficient with unprecedented sensitivity is demonstrated using the enhanced scanning thermal microprobe on samples of an extended range of thermal conductivity up to 18 W/m K, increasing the range of samples applicable to SThM when compared to the conventional commercial probe with diminished measurement sensitivity above ~10 W/m K. The probe is further demonstrated by simultaneously mapping thermal conductivity and Seebeck coefficient as a function of depth from the irradiated surface of an ion-irradiated bulk nanostructured thermoelectric material. In addition to enabling microscale thermal conductivity and Seebeck coefficient measurement of materials previously not applicable to SThM, the probe can also facilitate high-throughput characterization of combinatorial materials to aid the rapid discovery of compositions and processing conditions that yield highly desired thermal and thermoelectric properties.

36 MATERIALS SCIENCE↗

Deep-learning-aided extraction of optical constants in scanning near-field optical microscopy

Scanning near-field optical microscopy is one of the most effective techniques for spectroscopy of nanoscale systems. However, inferring optical constants from the measured near-field signal can be challenging because of a complicated and highly nonlinear interaction between the scanned probe and the sample. Conventional fitting methods applied to this problem often suffer from the lack of convergence or require human intervention. Here, we develop an alternative approach where the optical parameter extraction is automated by a deep learning network. The network provides an initial estimate that is subsequently refined by a traditional fitting algorithm. In conclusion, we show that this method demonstrates superior accuracy, stability against noise, and computational speed when applied to simulated near-field spectra.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A scanning resonator for probing quantum coherent devices

Superconducting resonators with high quality factors are extremely sensitive detectors of the complex impedance of materials and devices coupled to them. This capability has been used to measure losses in multiple different materials and, in the case of circuit quantum electrodynamics (circuit QED), has been used to measure the coherent evolution of multiple different types of qubits. Here, we report on the implementation of a scanning resonator for probing quantum coherent devices. Our scanning setup enables tunable coherent coupling to systems of interest without the need for fabricating on-chip superconducting resonators. We measure the internal quality factor of our resonator sensor in the single-photon regime to be >104 and demonstrate capacitive imaging using our sensor with zeptoFarad sensitivity and micron spatial resolution at milliKelvin temperatures. We then use our setup to characterize the energy spectrum and coherence times of multiple transmon qubits with no on-chip readout circuitry. Our experiments introduce a new tool for using circuit QED to measure existing and proposed qubit platforms.

47 OTHER INSTRUMENTATION↗

Design and fabrication of a differential scanning nanocalorimeter

This paper describes the design, fabrication, and characterization of a differential scanning nanocalorimeter that significantly reduces the sample volume to microliters and can potentially improve the temperature sensitivity to 10 µK. The nanocalorimeter consists of a polymeric freestanding membrane, four high-sensitive low-noise thermistors based on silicon carbide (SiC), and a platinum heater and temperature sensor. With the integrated heater and sensors, temperature scanning and power compensation can be achieved for calorimetric measurement. Temperature sensing SiC film was prepared by using sintered SiC target and DC magnetron sputtering under different gas pressures and sputtering power. The SiC sensing material is characterized through the measurement of current–voltage curves and noise levels. The thermal performance of a fabricated nanocalorimeter is studied in simulation and experiment. The experiment results show the device has excellent thermal isolation to hold thermal energy. As a result, the noise test together with the simulation show the device is promising for micro 10 µK temperature sensitivity and nanowatt resolution which will lead to low-volume ultra-sensitive nanocalorimetry for biological processes, such as protein folding and ligand binding.

42 ENGINEERING↗

Nanoscale imaging of quantum dot dimers using time-resolved super-resolution microscopy combined with scanning electron microscopy

Abstract Time-resolved super-resolution microscopy was used in conjunction with scanning electron microscopy to image individual colloidal CdSe/CdS semiconductor quantum dots (QD) and QD dimers. The photoluminescence (PL) lifetimes, intensities, and structural parameters were acquired with nanometer scale spatial resolution and sub-nanosecond time resolution. The combination of these two techniques was more powerful than either alone, enabling us to resolve the PL properties of individual QDs within QD dimers as they blinked on and off, measure interparticle distances, and identify QDs that may be participating in energy transfer. The localization precision of our optical imaging technique was ∼3 nm, low enough that the emission from individual QDs within the dimers could be spatially resolved. While the majority of QDs within dimers acted as independent emitters, at least one pair of QDs in our study exhibited lifetime and intensity behaviors consistent with resonance energy transfer from a shorter lifetime and lower intensity donor QD to a longer lifetime and higher intensity acceptor QD. For this case, we demonstrate how the combined super-resolution optical imaging and scanning electron microscopy data can be used to characterize the energy transfer rate.

36 MATERIALS SCIENCE↗