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Acta materialia 253, 118961 (2023). doi:10.1016/j.actamat.2023.118961, In order to obtain a fundamental understanding of the phenomena accompanying thermomechanical fatigue of Cu metallization used in power electronics, as well as the resulting deterioration of electric properties, there is a need to assess intragranular microstructure and strain evolution within individual Cu grains and near grain boundaries. Here, synchrotron dark field X-ray microscopy (DFXM) is used to characterize as-deposited and 5 × 104 times thermally-cycled 20 µm thick Cu films. The cycling was performed using a dedicated test chip in the range of 100–400 °C applying a heating rate of 106 K/s. The thermomechanical treatment results in severe shear deformation of Cu grains, film surface roughening, gradual grain microstructural refinement, the emergence of microscopic voids preferably at high angle grain boundaries (HAGBs) and finally in the voids' percolation, as revealed by in-situ and ex-situ scanning electron microscopy. DFXM provides experimental evidence that mosaicity of Cu grains, residual tensile and compressive elastic strain concentrations and full width at half maximum of Cu 111 reflections increase simultaneously in the vicinity of the HAGBs. The latter is interpreted as resulting from vacancy condensation in front of the HAGBs, after dislocations have moved across cycled grains and partly annihilated. Moreover, the observed HAGB decohesion and gradual void formation are correlated with the supposed hardening of regions near HAGBs, which thus lose their ductility during cyclic elasto-plastic deformation. The results are complemented with the ex-situ X-ray nanotomography data, which document the voids' percolation across the film's thickness with a “crack” width of up to ∼2 µm. In general, the study identifies the inhomogeneous intragranular microstructural refinement and a gradual condensation of structural defects near HAGBs as driving forces for void formation in thick Cu metallizations during fast thermo-mechanical fatigue., Published by Elsevier Science, Amsterdam [u.a.]

Focused Ion Beam (FIB) systems can be used to generate controlled micro- and nano-features on a solid surface. Prediction of surfaces fabricated in this way requires knowledge of the rate of removal of the target material in order to simulate the evolution of the surface. In this paper we present a continuous-time model of this process that allows us to predict the shape of trenches and freeform surfaces under the action of FIB. This type of model is appropriate when the points that describe the discrete trajectory of the beam (the line connecting consecutive dwell points) are close enough that the craters generated on the surface overlap. In the case of a straight beam path with constant dwell time, a trench of uniform depth is generated under these conditions. This simplified approach considerably reduces the computing time needed to simulate the process, without significantly reducing the accuracy of the predicted surface. Calibration of the model for a particular FIB setup and workpiece involves only a small number of experimental trials. The predictions of the model have been tested on a single crystalline Boron p-doped Si target material for several different beam paths. The depth and shape of the cross section of single and overlapping trenches with constant dwell time are predicted with high accuracy. The model was also used to predict three freeform surfaces, where the dwell time varies along each line of the beam path. Atomic force microscopy topography measurements show that the average relative error between the measured and simulated profiles is 2–10% depending on the complexity of the machined surface.

In this work, focused ion beam (FIB) milling of different structures is studied and compared for two different electronic materials, i.e., silicon (Si) and silicon carbide (SiC). Results show that the same processing parameters yield different trench cross sections for Si and SiC, even when the different material removal rates (MRR) are taken into account. In order to investigate more complex structures, nanocone arrays were fabricated in Si and SiC. The difference in the shape of the trench cross section and complex structures can be mainly explained by the significant difference in the angle dependent MRR for both materials. Other effects which occur during FIB irradiation by the non-ideal beam shape such as swelling and damage outside of the purposely processed region are emulated and sensitively studied by scanning probe microscopy techniques such as atomic force microscopy (in-line and off-line) and scanning spreading resistance microscopy, respectively, for SiC and the results are compared with those for Si.

Scanning probe microscopy techniques and, in particular, scanning spreading resistance microscopy (SSRM) were used for a detailed characterization of focused ion beam (FIB) induced damage in the surrounding of purposely irradiated areas on silicon. It is shown that the damaged area detected using these techniques extends up to several micrometers around the irradiated structures. The influence of the key FIB processing parameters on the FIB induced damage was examined. Parameters which were taken into account are the ion dose (from 1012 to 1018 cm−2), the milled structure size (circle diameters from 0.25 to 10 µm), the beam energy (from 10 to 30 keV), and the beam current (from 1.5 to 280 pA). Moreover, the influence of the SSRM settings on the measurement results was investigate d. Settings which were considered are the bias voltage and the force applied to the tip during the SSRM analysis. High resolution transmission electron microscopy and secondary ion mass spectroscopy analyses were performed to validate the SSRM results. Scattering between Ga ions and residual gas particles in the vacuum chamber of the FIB tool is identified as the main reason for the observed damaged area.

Imprint specific process parameters like the residual layer thickness and the etch resistance of the UV polymers for the substrate etch process have to be optimized to introduce UV nanoimprint lithography (UV NIL) as a high-resolution, low-cost patterning technique for research and industry into electron device manufacturing. Additionally, UV NIL processes have to be compatible with conventional silicon (Si) semiconductor processing. Within this work, the minimization of the residual layer thickness by using a multi-drop ink-jet system, which was integrated into the imprint stepper NPS300 from S-E-T-(formerly SUSS MicroTec), in combination with a low viscous UV polymer from Asahi Glass Company is shown. The etch resistance of different UV polymers against the poly-Si etch process was increased by 50% with an appropriate post-exposure bake. A poly-Si dry etch process was used to pattern the gates of short channel MOSFETs. After optimizing the poly-Si etch, properly working short channel MOSFETs with a minimum gate length of about 90nm were fabricated demonstrating successfully the compatibility of UV NIL with conventional Si semiconductor processing on nanosized scale.

Scanning spreading resistance microscopy (SSRM) and scanning capacitance microscopy (SCM) were used to analyze focused ion beam (FIB) induced lateral damage around milled structures on silicon. For this purpose, circular shaped structures were realized, and the influence of the implanted Ga dose (ranging from 10^1^5 to 10^1^7cm^-^2) and of the patterned area dimension (diameters ranging from 1 to [email protected]) on the damage were examined. It is shown that the extension of the lateral damage around FIB milled structures is much larger than the area of the purposely irradiated regions (up to a factor of 5) and increases with both, Ga dose and pattern diameter. Besides, the unique capability of SCM and SSRM techniques for the detection of FIB induced damage is demonstrated. In particular, it is shown that their high sensitivity to low densities of defects allows detecting larger damaged areas compared to Atomic Force Microscopy (AFM) topography maps.

Aim: The aim of this study was to compare the clinical and microbiological healing outcomes following non-surgical periodontal therapy using the new Vector™ ultrasonic system versus scaling and root planing (S/RP) with Gracey curettes. Material and Methods: The study comprised 20 chronic periodontitis patients. Using a split-mouth design, both treatment modalities were randomly applied to one quadrant of the upper and the lower jaws each. Clinical and microbiological parameters were assessed at baseline, 4 weeks, and 6 months after treatment. Furthermore, post-operative hypersensitivity was assessed. The Wilcoxon signed rank test (α=0.05) was used for statistical analysis. Results: Both therapies provided statistically significant clinical and microbiological improvements of periodontal conditions after 4 weeks and 6 months. Hypersensitive teeth were found only 4 weeks after S/RP. Besides a significantly better bleeding on probing reduction in deep S/RP sites, no other clinical and microbiological parameters revealed significant differences between the sites treated with the Vector™ system or S/RP. Conclusion: Both the Vector™ system and S/RP provided favourable periodontal healing results, although in deep pockets S/RP appeared to achieve a better resolution of inflammation.

Recent improvements in the fabrication of integrated field emitters with a control electrode into scanning probe microscopy sensors are presented and discussed. Compared to earlier work the precursor material for the electron beam induced deposition of the emitter was changed from a Pt precursor ((CH3C5H4)Pt(CH3)3) to a C precursor (C14H10) which leads to a higher process yield and an improved process stability. The change of the material for the control electrode from Pt to Cr results in better compatibility to standard semiconductor processing. The field emitter devices were fabricated by focused charged particle beam processing revealing emission currents of 0.8µA/tip for gate voltages of about 65V. Possible reasons for the high turn-on voltages Vto were investigated by high resolution transmission electron microscopy combined with EDX analyses and approaches for reducing Vto are presented.

In this work, methods for an accurate extraction of parameters for the simulation of nanoscaled structuring by focused ion beams will be discussed. For this purpose the quantitative understanding of the underlying effects (i.e. redeposition of sputtered atoms, the dependence of sputter yield on the angle of incidence, and the influence of scattered ions) is obligatory. Parameter values obtained from experiment and simulation will be compared and successfully be applied for the simulation of sputtered 2D structures.

Scanning spreading resistance microscopy (SSRM) has been applied to study focused ion beam (FIB) induced damage in silicon in dependence on ion irradiation doses from 1012 cm-2 to 2·1016 cm-2. Starting from the lowest dose, SSRM detects increasing spreading resistance (SR) with increasing dose. For doses from 2·1013 cm-2 to 4·1014 cm-2, a slight decrease of SR is measured whereas for higher doses SR again slightly increases. The results are explained by physical effects like decreased carrier mobility due to increased scattering, amorphisation of silicon and precipitation of implanted Ga ions. The results clearly prove that SSRM is well suited for the fast detection of ion beam induced damage with high lateral resolution.