Variable-temperature independently driven four-tip scanning tunneling microscope

The authors have developed an ultrahigh vacuum (UHV) variable-temperature four-tip scanning tunneling microscope (STM), operating from room temperature down to 7 K, combined with a scanning electron microscope (SEM). Four STM tips are mechanically and electrically independent and capable of positioning in arbitrary configurations in nanometer precision. An integrated controller system for both of the multitip STM and SEM with a single computer has also been developed, which enables the four tips to operate either for STM imaging independently and for four-point probe (4PP) conductivity measurements cooperatively. Atomic-resolution STM images of graphite were obtained simultaneously by the four tips. Conductivity measurements by 4PP method were also performed at various temperatures with the four tips in square arrangement with direct contact to the sample surface.     

An ultrahigh vacuum fast-scanning and variable temperature scanning tunneling microscope for large scale imaging

We describe the design and performance of a fast-scanning, variable temperature scanning tunneling microscope (STM) operating from 80 to 700 K in ultrahigh vacuum (UHV), which routinely achieves large scale atomically resolved imaging of compact metallic surfaces. An efficient in-vacuum vibration isolation and cryogenic system allows for no external vibration isolation of the UHV chamber. The design of the sample holder and STM head permits imaging of the same nanometer-size area of the sample before and after sample preparation outside the STM base. Refractory metal samples are frequently annealed up to 2000 K and their cooldown time from room temperature to 80 K is 15 min. The vertical resolution of the instrument was found to be about 2 pm at room temperature. The coarse motor design allows both translation and rotation of the scanner tube. The total scanning area is about 8 x 8 microm(2). The sample temperature can be adjusted by a few tens of degrees while scanning over the same sample area.     

Invited review article: A 10 mK scanning probe microscopy facility

We describe the design, development and performance of a scanning probe microscopy (SPM) facility operating at a base temperature of 10 mK in magnetic fields up to 15 T. The microscope is cooled by a custom designed, fully ultra-high vacuum (UHV) compatible dilution refrigerator (DR) and is capable of in situ tip and sample exchange. Subpicometer stability at the tip-sample junction is achieved through three independent vibration isolation stages and careful design of the dilution refrigerator. The system can be connected to, or disconnected from, a network of interconnected auxiliary UHV chambers, which include growth chambers for metal and semiconductor samples, a field-ion microscope for tip characterization, and a fully independent additional quick access low temperature scanning tunneling microscope (STM) and atomic force microscope (AFM) system. To characterize the system, we present the cooling performance of the DR, vibrational, tunneling current, and tip-sample displacement noise measurements. In addition, we show the spectral resolution capabilities with tunneling spectroscopy results obtained on an epitaxial graphene sample resolving the quantum Landau levels in a magnetic field, including the sublevels corresponding to the lifting of the electron spin and valley degeneracies.     

MEMS-based fast scanning probe microscopes

Scanning probe microscopy is a frequently used nanometer-scale surface investigation technique. Unfortunately, its applicability is limited by the relatively low image acquisition speed, typically seconds to minutes per image. Higher imaging speeds are desirable for rapid inspection of samples and for the study of a range of dynamic surface processes, such as catalysis and crystal growth. We have designed a new high-speed scanning probe microscope (SPM) based on micro-electro mechanical systems (MEMS). MEMS are small, typically micrometer size devices that can be designed to perform the scanning motion required in an SPM system. These devices can be optimized to have high resonance frequencies (up to the MHz range) and have very low mass (10⁻¹¹ kg). Therefore, MEMS can perform fast scanning motion without exciting resonances in the mechanical loop of the SPM, and hence scan the surface without causing the image distortion from which conventional piezo scanners suffer. We have designed a MEMS z-scanner which we have integrated in commercial AFM (atomic force microscope) and STM (scanning tunneling microscope) setups. We show the first successful AFM experiments.     

A cryogenic Quadraprobe scanning tunneling microscope system with fabrication capability for nanotransport research

We describe the development and the capabilities of an advanced system for nanoscale electrical transport studies. This system consists of a low temperature four-probe scanning tunneling microscope (STM) and a high-resolution scanning electron microscope coupled to a molecular-beam epitaxy sample preparation chamber. The four STM probes can be manipulated independently with subnanometer precision, enabling atomic resolution STM imaging and four-point electrical transport study of surface electronic systems and nanostructured materials at temperatures down to 10 K. Additionally, an integrated energy analyzer allows for scanning Auger microscopy to probe chemical species of nanostructures. Some testing results are presented.     

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.     

A nanopositioner for scanning probe microscopy: the KoalaDrive

We present a new type of piezoelectric nanopositioner called KoalaDrive which can have a diameter less than 2.5 mm and a length smaller than 10 mm. The new operating principle provides a smooth travel sequence and avoids shaking which is intrinsic to nanopositioners based on inertial motion with sawtooth driving signals. In scanning probe microscopy, the KoalaDrive can be used for the coarse approach of the tip or sensor towards the sample. Inserting the KoalaDrive in a piezo tube for xyz-scanning integrates a complete scanning tunneling microscope (STM) inside a 4 mm outer diameter piezo tube of <10 mm length. The use of the KoalaDrive makes the scanning probe microscopy design ultracompact and accordingly leads to a high mechanical stability. The drive is UHV, low temperature, and magnetic field compatible. The compactness of the KoalaDrive allows building a multi-tip STM as small as a single tip STM.     

Scanning probe microscopy of biological samples and other surfaces

Scanning probe microscopes derived from the scanning tunnelling microscope (STM) offer new ways to examine surfaces of biological samples and technologically important materials. The surfaces of conductive and semiconductive samples can readily be imaged with the STM. Unfortunately, most surfaces are not conductive. Three alternative approaches were used in our laboratory to image such surfaces. 1. Crystals of an amino acid were imaged with the atomic force microscope (AFM) to molecular resolution with a force of order 10^?8 N. However, it appears that for most biological systems to be imaged, the atomic force microscope should be able to operate at forces at least one and perhaps several orders of magnitude smaller. The substitution of optical detection of the cantilever bending for the measurement by electron tunnelling improved the reliability of the instrument considerably. 2. Conductive replicas of non-conductive surfaces enabled the imaging of biological surfaces with an STM with a lateral resolution comparable to that of the transmission electron microscope. Unlike the transmission electron microscope, the STM also measures the heights of the features. 3. The scanning ion conductance microscope scans a micropipette with an opening diameter of 0·04-0·1 μm at constant ionic conductance over a surface covered with a conducting solution (e.g., the surface of plant leaves in saline solution).     

A low-temperature scanning tunneling microscopy investigation of single electron effects

The design and the performance of a low-temperature scanning tunneling microscope (STM) operating in ultrahigh vacuum (UHV) is described. The sample and the STM are cooled by means of a helium bath cryostate. The STM consists of a “beetle”-type microscope, which is mounted on a spring suspension stage that can be operated between room temperature and 30 K. We present the results of tunneling spectroscopy on ligand-stabilized Au₅₅-clusters on a thiol-covered gold substrate. I(V)-curves taken at 100 K clearly show coulomb staircase structures, which agree well with theoretical predictions for these structures.     

Light emission induced by tunneling electrons from surface nanostructures observed by novel conductive and transparent probes

We have developed an ultrahigh-vacuum low-temperature scanning tunneling microscope (STM) equipped with a near-field optical detection system using novel conductive and optically transparent probes. Tunneling-electron induced photons generated in a nanometer-scale area just under the STM probe can be collected directly into the core of the optical fiber probe within the optical near-field region. Firstly, optical fiber probes coated with indium-tin-oxide thin film are applied to quantitative analysis of p-type GaAs(110) surface, where a decrease of light emission in photon mapping clearly extracts the existence of Zn accepter atoms located at the sub-surface layers. Secondly, in order to enhance the efficiency for inelastic tunneling excitation of a tip-induced plasmon mode, a STM probe coated with an Ag/ITO dual-layer film has been developed and applied to an Ag(111) surface, where photon mapping with a step resolution has been achieved by near-field detection.     

The Frictional Response of VC(100) Surfaces: Influence of 1-Octanol and 2,2,2-Trifluoroethanol Adsorption

In this report, we present ultrahigh vacuum (UHV) atomic-scale measurements of the frictional response of the VC(100) surface and the influence on friction through the adsorption of 1-octanol (CH₃(CH₂)₇OH) and 2,2,2-trifluoroethanol (CF₃CH₂OH). Atomic force microscopy (AFM) has been used to determine the changes in interfacial friction and adhesion, while scanning tunneling microscopy (STM) has revealed changes in surface morphology upon adsorption. X-ray photoelectron spectroscopy (XPS) has been utilized to determine the composition of the surface formed through the reaction of these adsorbates with VC. Adsorption of 1-octanol on the VC(100) surface at room temperature causes a 15% reduction in the friction measured between a clean VC surface and a silicon nitride AFM tip. STM images, combined with XPS results, reveal that 1-octanol does not completely cover the surface and that saturation occurs approximately at a 500L exposure. Adsorption of 2,2,2-trifluoroethanol on the VC(100) surface at room temperature produces a significant increase in friction while at the same time producing a decrease in adhesion. These contrasting results are interpreted in terms of differences in interfacial shear strength, chemical composition, and the molecular details of the adsorbed layer.     

An entirely enclosed scanning tunnelling microscope capable of being fully immersed in liquid helium

We present an ultrahigh‐vacuum (UHV)‐sealed high‐stability scanning tunnelling microscope (STM) that can be entirely immersed in liquid helium and readily used in a commercial Dewar or superconducting magnet. The STM head features a horizontal microscanner that can become standalone and ultrastable when the coarse approach inertial motor retracts. Low voltage is enough to operate the STM even at low temperature owing to the powerful motor. It is housed in a tubular chamber of 49 mm outer diameter, which can be pumped via a detachable valve (DV), UHV‐sealed and remain sealed after the DV is removed. The entire so‐sealed chamber can then be inserted into liquid helium, where in situ sample cleavage is done via vacuum bellow. This allows sample cleavage and STM measurements to take place in better UHV with higher cooling power. Quality atomic resolution images of graphite and charge density wave on 1T‐TiSe₂ taken in ambient and 14 K conditions, respectively, are presented.     

Antenna-based ultrahigh vacuum microwave frequency scanning tunneling microscopy system

The instrumental synthesis of high resolution scanning tunneling microscopy (STM) with the ability to measure differential capacitance with atomic scale resolution is highly desirable for fundamental metrology and for the study of novel physical characteristics. Microwave frequency radiation directed at the tip-sample junction in an STM system allows for such high-resolution differential capacitance information. This ability is particularly critical in ultrahigh vacuum environments, where the additional parameter space afforded by including a capacitance measurement would prove powerful. Here we describe the modifications made to a commercial scanning tunneling microscope to allow for broad microwave frequency alternating current scanning tunneling microscopy (ACSTM) in ultrahigh vacuum conditions using a relatively simple loop antenna and microwave difference frequency detection. The advantages of our system are twofold. First, the use of a removable antenna on a commercial STM prevents interference with other UHV processes while providing a simple method to retrofit any commercial UHV-STM with UHV-ACSTM capability. Second, mounting the microwave antenna on a translator allows for specific tuning of the system to replicate experimental conditions between samples, which is particularly critical in sensitive systems like organic thin films or single molecules where small changes in incident power can affect the results. Our innovation therefore provides a valuable approach to give nearly any commercial STM, be it an ambient or UHV system, the capability to measure atomic-scale microwave studies such as differential capacitance or even single molecule microwave response, and it ensures that experimental ACSTM conditions can be held constant between different samples.     

Cleaning AFM colloidal probes by mechanically scrubbing with supersharp “brushes”

Contamination control of atomic force microscope (AFM) tips (including standard but supersharp imaging tips and particle/colloidal probes) is very important for reliable AFM imaging and surface/interface force measurements. Traditional cleaning methods such as plasma, UV–ozone and solvent treatments have their shortcomings. Here, we demonstrate that calibration gratings with supersharp spikes can be employed to scrub away contaminants accumulated on a colloidal sphere probe by scanning the probe against the spikes at high load at constant-force mode. The present method is superior to traditional cleaning methods in several aspects. First, accumulated lump-like organic/inorganic material can be removed; second, removal is non-destructive and highly efficient based on a “targeted removal” strategy; third, removal and probe shape/morphology study can be completed in a single step (we report, to our best knowledge, the first evidence of the wear of the colloidal sphere during force measurements); and fourth, both colloidal/particle probes and standard but supersharp AFM imaging tips can be treated.     

开放式多功能扫描探针显微镜系统

开放式多功能扫描探针显微镜、集成扫描隧道显微镜、原子力显微镜、横向力显微镜和静电力显微镜．具有接触、半接触和非接触工作模式，可进行作用力、电流、电位、光能量等参数的高度局域综合测量,具有极高的开放性和可扩展性，支持用户进行二次开发。     

Atom probe,AFM, and STM studies on vacuum-fired stainless steels

The surface morphology of grades 304L and 316LN stainless steels, after low-temperature bake-out process and vacuum annealing, has been studied by atomic force microscopy (AFM) and scanning tunnelling microscopy (STM). The local elemental composition on the surface before and after thermal treatment has been investigated by atom probe (AP) depth profiling measurements. After vacuum annealing, AFM and STM show significant changes in the surface structure and topology. Recrystallization and surface reconstruction is less pronounced on the 316LN stainless steel. AP depth profiling analyses result in noticeable nickel enrichment on the surface of grade 304L samples. Since hydrogen recombination is almost controlled by surface structure and composition, a strong influence on the outgassing behaviour by the particular surface microstructure can be deduced.     

A scanning near-field optical microscope having scanning electron tunnelling microscope capability using a single metallic probe tip

A new microscope system that has the combined capabilities of a scanning near-field optical microscope (SNOM) and a scanning tunnelling microscope (STM) is described. This is achieved with the use of a single metallic probe tip. The distance between the probe tip and the sample surface is regulated by keeping the tunnelling current constant. In this mode of operation, information about the optical properties of the sample, such as its refractive index distribution and absorption characteristics, can be disassociated from the information describing its surface structure. Details of the surface structure can be studied at resolutions smaller than the illumination wavelength. The performance of the microscope is evaluated by analysing a grating sample that was made by coating a glass substrate with gold. The results are then compared with the corresponding SNOM and STM images of the grating.     

Development of an ion beam alignment system for real-time scanning tunneling microscope observation of dopant-ion irradiation

An ion beam alignment system has been developed in order to realize real-time scanning tunneling microscope (STM) observation of "dopant-ion" irradiation that has been difficult due to the low emission intensity of the liquid-metal-ion-source (LMIS) containing dopant atoms. The alignment system is installed in our original ion gun and STM combined system (IG/STM) which is used for in situ STM observation during ion irradiation. By using an absorbed electron image unit and a dummy sample, ion beam alignment operation is drastically simplified and accurized. We demonstrate that sequential STM images during phosphorus-ion irradiation are successfully obtained for sample surfaces of Si(111)-7x7 at room temperature and a high temperature of 500 degrees C. The LMIS-IG/STM equipped with the developed ion beam alignment system would be a powerful tool for microscopic investigation of the dynamic processes of ion irradiation.     

Room temperature scanning Hall probe microscopy using GaAs/AlGaAs and Bi micro-hall probes

A room temperature scanning Hall probe microscope system utilizing GaAs/AlGaAs and bismuth micro-Hall probes was used for magnetic imaging of ferromagnetic domain structures on the surfaces of crystalline thin film garnets and permanent magnets. The Bi micro-Hall probes had dimensions ranging between 0.25 and 2.8 microm2 and were fabricated using a combination of optical lithography and focused ion beam milling. The use of bismuth was found to overcome surface depletion effects associated with semiconducting micro-Hall probes. Our experiments demonstrated that Bi is a practical choice of material for fabricating sub-micron sized Hall sensors.     

Simulation-aided design and fabrication of nanoprobes for scanning probe microscopy

We proposed and demonstrated a flexible and effective method to design and fabricate scanning probes for atomic force microscopy applications. Computer simulations were adopted to evaluate design specifications and desired performance of atomic force microscope (AFM) probes; the fabrication processes were guided by feedback from simulation results. Through design-simulation-fabrication iterations, tipless cantilevers and tapping mode probes were successfully made with errors as low as 2% in designed resonant frequencies. For tapping mode probes, the probe tip apex achieved a 10 nm radius of curvature without additional sharpening steps; tilt-compensated probes were also fabricated for better scanning performance. This method provides AFM users improved probe quality and practical guidelines for customized probes, which can support the development of novel scanning probe microscopy (SPM) applications.