Phase variation experiments in non-contact dynamic force microscopy using phase locked loop techniques

This work presents constant amplitude Dynamic Force Microscopy (DFM) measurements under ultra-high vacuum conditions performed with home-built digital electronics based on the principle of phase locked loop (PLL) techniques. In DFM so-called topography is often measured in constant frequency shift (Δf) mode. This study describes the influence of phase shifts on constant Δf imaging. Therefore, phase variation experiments were acquired, leading to information about the cantilever resonance behaviour close to the surface. As sample, an evaporated thin film of NaCl on a Cu(111) substrate was chosen in order to obtain a heterogeneous system with clean Cu and NaCl areas. The atomic structure of both materials was resolved, which is the first time true atomic resolution was obtained on a metal. Large apparent topography variations are observed on this heterogeneous sample when changing the phase between the excitation and oscillation of the cantilever end. Such artefacts can be explained by comparison with phase variation experiments.     

Noncontact atomic force microscopy: Bond imaging and beyond

It was a long-cherished dream for chemists to take a direct look at chemical bonding, a fundamental component of chemistry. This dream was finally accomplished by the state-of-the-art noncontact atomic force microscopy (NC-AFM) equipped with qPlus force sensors and carbon monoxide (CO) functionalized tips. The resolved interconnectivity between atoms and molecules in NC-AFM frequency shift images is interpreted as chemical bonding, providing essential knowledge of the bond length, bond angle and even bond order. The featured contrast of different chemical bonds can serve as fingerprints for further interpretation of chemical structures toward unknown species synthesized on surfaces. This breakthrough enriches characterization tools for surface science and brings our understanding of on-surface reactions to a new level. Beyond bond imaging, the application of NC-AFM has been extended to quantifying interatomic interactions, identifying three-dimensional nanostructures, manipulating molecules and reactions, as well as determining molecular electronic characteristics. Moreover, some recent efforts address the improvement of the usability and versatility of the bond-resolved NC-AFM technique, including high-resolution molecular investigation on bulk insulators, application-specific tip modification, stable bond imaging above liquid helium temperature and autonomous experimentation implemented by artificial intelligence.     

Surface morphology of InGaAs on GaAs(100) by chemical beam epitaxy using unprecracked monoethylarsine, triethylgallium and trimethylindium

Temperature-dependent evolution of surface corrugation and the interface dislocation in In_0.15Ga_0.85As epilayer on GaAs(100) substrate grown by chemical beam epitaxy using unprecracked monoethylarsine have been investigated by atomic force microscope (AFM) and transmission electron microscopy (TEM). AFM images showed that the line direction of surface ridge changes from [011] to [0 1] with increasing temperature. However, TEM micrographs showed that dislocation networks are formed along both [011] and [0 1] directions at the interface. These results indicate that growth kinetics on the terrace and at surface steps generated by the dislocations play an important role in determining the direction of surface corrugation. We suggest that the temperature-dependent change of surface corrugation is caused by an anisotropic surface diffusion on the terrace and different sticking probability of adsorbates on the surface steps which were produced by interface misfit dislocation along the two orthogonal surface directions.     

Ferroelastic domains in lead phosphate-arsenate: An afm,X-ray diffraction,tem and Raman study

Ferroelastic domain patterns in lead phosphate-type crystals depend on their chemical composition. The intersection of ferroelastic W domain walls with the (100) surface of lead phosphate-arsenate mixed crystals has been imaged using tapping mode atomic force microscopy. Dilution of the strain leads to characteristic surface deformations which deviate from those in pure lead phosphate. In highly twinned lead phosphate-arsenate X-ray diffraction was used to show renormalization effects and scattering phenomena stemming from the twin walls. Raman-active hard modes show wall-related profile changes and low-frequency tails. Symmetry mode analysis is used to describe the displacive modes characterizing the structural distortion in lead phosphate-arsenate for the sequence K m → P2₁/c.     

Nano-scale chemical and structural segregation induced in surface layer of NaNbO3 crystals with thermal treatment at oxidising conditions studied by XPS,AFM, XRD,and electric properties tests

The process of ionic segregation in the surface layer induced by the thermal treatment of the NaNbO₃ crystal was studied. The study of the as grown crystal and the crystal heated at 970 K in ambient air was carried out for comparison. The changes in the concentration of the elements within the surface layer were determined using XPS measurements. The AFM technique was applied to determine the surface morphology related to nano-scale transformation. The possibility of appearance of the Ruddlesden–Popper phases was detected by the XRD test. The change in the features of the electric permittivity, the loss tangent, and the electric conductivity was ascribed to the marked participation of the chemically modified surface layer in the measured effective electrical properties.     

Surface studies on bimetallic thiocyanate ligand based single crystals of MnHg(SCN)4, CdHg(SCN)4 and ZnCd(SCN)4

Bimetallic SCN ligand based single crystals of manganese mercury thiocyanate (MMTC), cadmium mercury thiocyanate (CMTC) and zinc cadmium thiocyanate (ZCTC) are grown by slow solvent evaporation technique. The growth mechanism and surface features are investigated by optical microscopic techniques such as scanning electron microscopy (SEM) and atomic force microscopy (AFM). The laser induced surface damage measurements were carried out using a Q-switched Nd:YAG laser at 1064 nm with laser beam of 1.0 Hz and pulse duration 25 ps. The laser damage threshold values of MMTC, CMTC and ZCTC are found to be 15.9, 22.9 and 19.7 GW/cm², respectively. The SEM analysis of MMTC reveals the formation of elongated dendrite growth pattern caused by the fluctuations of Mn and Hg metal ligands when thiocyanate (SCN) bridges them. The etching study indicates the occurrence of different types of etch pit patterns like terraced triangles, pillars, pyramids and rods. The AFM images confirm the formation of three major hillocks with cavities in MMTC. The measured roughness values for CMTC crystal are very much lower than that of MMTC.