Recent advances in atomic-scale spin-polarized scanning tunneling microscopy

The Mn3N2 (010) surface has been studied using spin-polarized scanning tunneling microscopy at the atomic scale. The principle objective of this work is to elucidate the properties and potential of this technique to measure atomic-scale magnetic structures. The experimental approach involves the use of a combined molecular beam epitaxy/scanning tunneling microscopy system that allows the study of atomically clean magnetic surfaces. Several key findings have been obtained. First, both magnetic and non-magnetic atomic-scale information has been obtained in a single spin-polarized image. Magnetic modulation of the height profile having an antiferromagnetic super-period of c = 12.14 A (6 atomic rows) together with a non-magnetic superstructure having a period of c/2 = 6.07 A (3 atomic rows) was observed. Methods of separation of magnetic and non-magnetic profiles are presented. Second, bias voltage-dependent spin-polarized images show a reversal of the magnetic modulation at a particular voltage. This reversal is clearly due to a change in the sign of the magnetic term in the tunnel current. Since this term depends on both the tip's as well as the sample's magnetic local density of states, the reversal can be caused by either the sample or the tip. Third, the shape of the line profile was found to vary with the bias voltage, which is related to the energy-dependent spin contribution from the 2 chemically inequivalent Mn sites on the surface. Overall, the results shown here expand the application of the method of spin-polarized scanning tunneling microscopy to measure atomic-scale magnetic structures.     

Data scattering in scanning tunneling spectroscopy

We investigated the scattering of current-voltage data obtained with scanning tunneling spectroscopy (STS) at room temperature at a solid-liquid interface on highly oriented pyrolytic graphite (HOPG) and in ultrahigh vacuum on HOPG and Au(111). For both experimental conditions, the data scattering can be described by a lognormal function for a moderate number of subsequent measurements. The lognormal distribution of the current can be explained by a normal distribution of the tip-surface distance. We give a simple empirical rule for STS data sorting.     

Imaging the switching behavior of superparamagnetic nanoislands by spin-polarized scanning tunneling microscopy

In the past, spin-polarized scanning tunneling microscopy (SP-STM) was mainly applied to static domain configurations that do not vary in time. Here, we show that SP-STM may also be used to image the thermal switching behavior of superparamagnetic nanoislands. Special experimental care has to be taken in order to allow the unambiguous interpretation of the obtained data. Most important, the imaging of superparamagnetic particles requires the use of antiferromagnetic probe tips as the stray field of ferromagnetic tips may modify the sample's intrinsic switching behavior. Our results show that Fe monolayer islands on Mo(110) switch thermally when their area is smaller than 40 nm2. Dipolar coupling between adjacent islands is observed at small inter-particle distance. A pronounced shape dependence is found that confirms existing but yet unverified analytical predictions. The first experiments performed on Fe double-layer islands on W(001) also show thermal switching events, but no clear-cut size dependence is found.     

Scanning tunneling spectroscopy under large current flow through the sample

We describe a method to make scanning tunneling microscopy/spectroscopy imaging at very low temperatures while driving a constant electric current up to some tens of mA through the sample. It gives a new local probe, which we term current driven scanning tunneling microscopy/spectroscopy. We show spectroscopic and topographic measurements under the application of a current in superconducting Al and NbSe(2) at 100 mK. Perspective of applications of this local imaging method includes local vortex motion experiments, and Doppler shift local density of states studies.     

Self-navigation of a scanning tunneling microscope tip toward a micron-sized graphene sample

We demonstrate a simple capacitance-based method to quickly and efficiently locate micron-sized conductive samples, such as graphene flakes, on insulating substrates in a scanning tunneling microscope (STM). By using edge recognition, the method is designed to locate and to identify small features when the STM tip is far above the surface, allowing for crash-free search and navigation. The method can be implemented in any STM environment, even at low temperatures and in strong magnetic field, with minimal or no hardware modifications.     

A modular designed ultra-high-vacuum spin-polarized scanning tunneling microscope with controllable magnetic fields for investigating epitaxial thin films

A room-temperature ultra-high-vacuum scanning tunneling microscope for in situ scanning freshly grown epitaxial films has been developed. The core unit of the microscope, which consists of critical components including scanner and approach motors, is modular designed. This enables easy adaptation of the same microscope units to new growth systems with different sample-transfer geometries. Furthermore the core unit is designed to be fully compatible with cryogenic temperatures and high magnetic field operations. A double-stage spring suspension system with eddy current damping has been implemented to achieve ≤5 pm z stability in a noisy environment and in the presence of an interconnected growth chamber. Both tips and samples can be quickly exchanged in situ; also a tunable external magnetic field can be introduced using a transferable permanent magnet shuttle. This allows spin-polarized tunneling with magnetically coated tips. The performance of this microscope is demonstrated by atomic-resolution imaging of surface reconstructions on wide band-gap GaN surfaces and spin-resolved experiments on antiferromagnetic Mn(3)N(2)(010) surfaces.     

A low temperature scanning tunneling microscope for electronic and force spectroscopy

In this article, we describe and test a novel way to extend a low temperature scanning tunneling microscope with the capability to measure forces. The tuning fork that we use for this is optimized to have a high quality factor and frequency resolution. Moreover, as this technique is fully compatible with the use of bulk tips, it is possible to combine the force measurements with the use of superconductive or magnetic tips, advantageous for electronic spectroscopy. It also allows us to calibrate both the amplitude and the spring constant of the tuning fork easily, in situ and with high precision.     

Tip-enhanced near-field Raman spectroscopy with a scanning tunneling microscope and side-illumination optics

Conventional Raman spectroscopy (RS) suffers from low spatial resolution and low detection sensitivity due to the optical diffraction limit and small interaction cross sections. It has been reported that a highly localized and significantly enhanced electromagnetic field could be generated in the proximity of a metallic tip illuminated by a laser beam. In this study, a tip-enhanced RS system was developed to both improve the resolution and enhance the detection sensitivity using the tip-enhanced near-field effects. This instrument, by combining RS with a scanning tunneling microscope and side-illumination optics, demonstrated significant enhancement on both optical sensitivity and spatial resolution using either silver (Ag)-coated tungsten (W) tips or gold (Au) tips. The sensitivity improvement was verified by observing the enhancement effects on silicon (Si) substrates. Lateral resolution was verified to be below 100 nm by mapping Ag nanostructures. By deploying the depolarization technique, an apparent enhancement of 175% on Si substrates was achieved. Furthermore, the developed instrument features fast and reliable optical alignment, versatile sample adaptability, and effective suppression of far-field signals.     

Modification of the sample holder for a variable temperature scanning tunneling microscope (Omicron)

The design of a sample holder for a variable temperature scanning tunneling microscope (VT STM (Omicron)) with a variable sample temperature is described. This design considerably extends the range of investigated materials whose surface structure is sensitive to low concentrations of contaminations. The device is manufactured on the basis of the components of a standard holder with the possibility of heat-treating samples in a temperature range of 100–1500 K. The working capacity of the modified sample holder was demonstrated for an example of obtaining a Si(100)?2 × 1 surface with an ultimately low concentration of structural defects.     

Background removal in scanning tunneling spectroscopy of single atoms and molecules on metal surfaces

Scanning tunneling spectroscopy has developed into a powerful spectroscopic technique that has found wide application in the atomic scale characterization of the electronic properties of clean surfaces as well as adsorbates and defects at surfaces. However, it still lacks the standard methods for data treatment and removal of artifacts in spectra as they are, e.g., common in photoemission spectroscopy. The properties of the atomic scale tip apex--the probe of the instrument--tend to introduce spurious background signals into tunneling spectra. We present and discuss two methods which permit to extract tip-independent information from low temperature tunneling spectra acquired on single atoms and molecules on single crystal surfaces by background subtraction. The methods rely on a characterization of the tip on the clean metal surface. The performance of both methods is demonstrated and compared for simulated and experimental tunneling spectra.     

Combined low-temperature scanning tunneling/atomic force microscope for atomic resolution imaging and site-specific force spectroscopy

We present the design and first results of a low-temperature, ultrahigh vacuum scanning probe microscope enabling atomic resolution imaging in both scanning tunneling microscopy (STM) and noncontact atomic force microscopy (NC-AFM) modes. A tuning-fork-based sensor provides flexibility in selecting probe tip materials, which can be either metallic or nonmetallic. When choosing a conducting tip and sample, simultaneous STM/NC-AFM data acquisition is possible. Noticeable characteristics that distinguish this setup from similar systems providing simultaneous STM/NC-AFM capabilities are its combination of relative compactness (on-top bath cryostat needs no pit), in situ exchange of tip and sample at low temperatures, short turnaround times, modest helium consumption, and unrestricted access from dedicated flanges. The latter permits not only the optical surveillance of the tip during approach but also the direct deposition of molecules or atoms on either tip or sample while they remain cold. Atomic corrugations as low as 1 pm could successfully be resolved. In addition, lateral drifts rates of below 15 pm/h allow long-term data acquisition series and the recording of site-specific spectroscopy maps. Results obtained on Cu(111) and graphite illustrate the microscope's performance.     

Scanning tunneling microscope spectroscopy of polymers

This paper presents theoretical results on the relationship between density of states (DOS) and scanning tunneling microscope current-voltage curves in polymers. We considered samples of linear hydrocarbons electrically grounded at one of their extremes. The other extreme is electrically connected to the microscope tip via electron tunneling through vacuum. When a voltage, V, is applied to the tip, electric current, I, flows in the tip-sample circuit. This current varies as the voltage varies and depends on the DOS to the extent that no current would flow if no electron states exist at a certain energy (or voltage). The detailed relationship between DOS and the current-voltage (I-V) curve is not known a priori. We solve the corresponding quantum problem in the context of tight binding and find that I-V reproduces accurately the resonant energy peaks of the DOS. We apply the results to 100 atom-long alkane and alkene chains and found that there is a significant voltage shift in the corresponding curves as to discriminate one structure from the other.     

扫描隧道显微镜系统的优化研究

对扫描隧道显微镜(STM)系统进行了优化研究,实现了对环境振动的隔绝和电噪声的屏蔽,并在此基础上,设计并完成CCD显微监测系统,实现了对样品—探针逼近过程的实时临控。对整个系统进行了联合调试,成功获得高定向热解石墨和金表面的结构图像。     

Imaging of metal-coated biological samples by scanning tunneling microscopy

A method for imaging biological samples by scanning tunneling microscopy (STM) is presented. There are two main difficulties in imaging biological samples by STM: (1) the low conductivity of biological material and (2) finding a method of reliably depositing the sample on a flat conducting surface. The first of these difficulties was solved by coating the samples with a thin film of platinum-carbon. The deposition problem was solved by a method similar to a procedure used to deposit biological molecules onto field ion microscope (FIM) tips. STM images of bacteriophage T7 and filamentous phage fd are shown. The substrate on which the samples were absorbed was atomically flat gold. The images do not show molecular detail due to the metal coating, but the gross dimensions and morphology are correct for each type of virus. Also, the surface density of virus particles increases and decreases in the way expected when the conditions of deposition are changed. These methods allow reliable and reproducible STM imaging of biological samples.     

Construction of a versatile ultralow temperature scanning tunneling microscope

We constructed a dilution-refrigerator (DR)-based ultralow temperature scanning tunneling microscope (ULT-STM) which works at temperatures down to 30 mK, in magnetic fields up to 6 T and in ultrahigh vacuum (UHV). Besides these extreme operation conditions, this STM has several unique features not available in other DR-based ULT-STMs. One can load STM tips as well as samples with clean surfaces prepared in an UHV environment to a STM head keeping low temperature and UHV conditions. After then, the system can be cooled back to near the base temperature within 3 h. Due to these capabilities, it has a variety of applications not only for cleavable materials but also for almost all conducting materials. The present ULT-STM has also an exceptionally high stability in the presence of magnetic field and even during field sweep. We describe details of its design, performance, and applications for low temperature physics.     

Nanomanipulation and nanofabrication with multi-probe scanning tunneling microscope: from individual atoms to nanowires

The wide variety of nanoscale structures and devices demands novel tools for handling, assembly, and fabrication at nanoscopic positioning precision. The manipulation tools should allow for in situ characterization and testing of fundamental building blocks, such as nanotubes and nanowires, as they are built into functional devices. In this paper, a bottom-up technique for nanomanipulation and nanofabrication is reported by using a 4-probe scanning tunneling microscope (STM) combined with a scanning electron microscope (SEM). The applications of this technique are demonstrated in a variety of nanosystems, from manipulating individual atoms to bending, cutting, breaking carbon nanofibers, and constructing nanodevices for electrical characterizations. The combination of the wide field of view of SEM, the atomic position resolution of STM, and the flexibility of multiple scanning probes is expected to be a valuable tool for rapid prototyping in the nanoscience and nanotechnology.     

A new method of scanning tunneling spectroscopy for study of the energy structure of semiconductors and free electron gas in metals

In this study, anew method for the scanning tunneling spectroscopy (STS) of direct and indirect gap semiconductors and free electron gas in metals is proposed. Band structures of Si, porous Si, and Ge were studied. The tunneling current-voltage characteristics of Si and porous Si surfaces were measured over different voltage intervals from tens of mV to 20 V under incident light from an Xe lamp and those of a Ge surface in the dark. The correlation between the shapes of the I-V curves and band structure of the materials was calculated. It was found that the curves are linear if measured in the voltage range V₀ E_g/(2e) and nonlinear when V₀ α E_g/(2e) (in the measurements the applied voltage was changed from -V₀ to V₀). The method was used for the observation of a new effect of tunneling of free electron gas having thermal energies from a metal tip to a band gap state of the semiconductor. The energy spectrum of free electron gas was measured.     

Combining scanning tunneling microscopy and synchrotron radiation for high-resolution imaging and spectroscopy with chemical, electronic, and magnetic contrast

The combination of high-brilliance synchrotron radiation with scanning tunneling microscopy opens the path to high-resolution imaging with chemical, electronic, and magnetic contrast. Here, the design and experimental results of an in-situ synchrotron enhanced x-ray scanning tunneling microscope (SXSTM) system are presented. The system is designed to allow monochromatic synchrotron radiation to enter the chamber, illuminating the sample with x-ray radiation, while an insulator-coated tip (metallic tip apex open for tunneling, electron collection) is scanned over the surface. A unique feature of the SXSTM is the STM mount assembly, designed with a two free-flex pivot, providing an angular degree of freedom for the alignment of the tip and sample with respect to the incoming x-ray beam. The system designed successfully demonstrates the ability to resolve atomic-scale corrugations. In addition, experiments with synchrotron x-ray radiation validate the SXSTM system as an accurate analysis technique for the study of local magnetic and chemical properties on sample surfaces. The SXSTM system's capabilities have the potential to broaden and deepen the general understanding of surface phenomena by adding elemental contrast to the high-resolution of STM.     

High-resolution photon scanning tunneling microscopic investigations of NaCl crystal surfaces

Cleaved NaCl crystal surfaces were investigated with a photon scanning tunneling microscope. Steps 4 nm high and 3 nm wide could be resolved. The lateral resolution is coupled to the step height by the steepest measured slopes of about 50°. The measured stepwidth at shallow steps is noise-and slope-limited to 3 nm. The mapping of the decay coefficient of the evanescent field shows spatial inhomogeneities often coupled to the crystalline structure.