Labor Nanoanalytik und Halbleiterchemie (Nanochem)
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- Silicon (4)
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The high surface to volume ratio of nanoparticles allows a detailed experimental study of the surface phenomena associated with solid bridging. Besides bulk analyses, the local view on the structure and composition via HRTEM is particularly essential. 50 nm core shell particles consisting of a silicon (Si) core and a SiO2 shell were used as model system to understand surface phenomena appearing for Si-based nanostructures. Evaporative drying from de-ionized water shows the most significant bridging effect based on SiO2. There is only a localized deposition of oxides between the particles during the drying process and no overall oxidation. For the deposition material, silicates are the most likely candidates.
Online trace analysis based on UV/Vis spectroscopy requires long detection paths. Therefore an isotropic wet etch process in silicon is developed to fabricate a 300 µm deep channel with low channel wall roughness for desired light guidance application. Four etchant compositions were compared in terms of etching rate, surface roughness and selectivity in a beaker process. The best fitting mixture was selected. To further increase the surface quality (bubble issue) a spin etcher tool is used for producing the channels. The dependence of homogeneity and defect density on media flux, and rotation velocity was investigated. Results show that high rotation velocity and high media flux lead to great defects in the channel wall. Through rotation of the wafer during etching, the etching rate of silicon rises compared to the beaker process due to the rapid removal of etch products and simultaneous supply of fresh etchant. After 38 min of etching, 300 µm deep semi-circular channels with high optical quality (Rq=10 nm±2 nm) over 3 m were produced.
In high-tech processing even smallest concentrations of metal ions in process media are of the utmost significance because they cause expensive production failures. Currently, cost-intensive equipment, special trained staff and time consuming analyses are necessary to detect these contaminations in order to avoid failures. The Centers of Excellence Nanochem and Sensorics at the University of Applied Sciences Regensburg (owner of patent PCT/EP2010/064833) and their industrial partner Micro-Epsilon GmbH are developing a new miniaturized measurement device which allows cost-effective real-time analysis of fluidic media for the first time. The system is fully automated and can be directly connected to wet-etch benches. Hence it allows continuous real-time surveillance of metal contaminations in the ppb-range through absorption spectroscopy in process media. For this purpose a very small sample amount of the process medium and a specific complexing agent are mixed together. This leads to an increase in the molar extinction coefficients and though even smallest contaminations become visible. The main parts of our development are the simulation of the different system components, their production and chemical analyses with the evaluation model.
The mechanical stability of nanostructures depends on the surrounding medium. Their stability was probed by lateral force microscopy in liquid media. Previously reported data on water and isopropanol showed an increase in the fracture strength for the latter. Further tests with other alcohols (ethanol, 1-butanol) also showed an increasing strength. The interface between the liquid and the surface is the decisive factor for the influence of the media. When altering the interface with a cationic surfactant or a self-assembled monolayer, an increase of the fracture force by 100 % compared to de-ionized water could be measured.
Enhanced particle removal processes in wet cleaning as well as drying processes of semiconductor wafers can cause significant lateral forces on surface structures. These forces, however, must not exceed the mechanical stability of structures on the wafer. Thus, a mechanical fracture test was used to assess the lateral mechanical stability of polysilicon line structures in relevant process liquids. The mechanical test was based on nanomanipulation with an atomic force microscope. Compared to fracture tests in air, data acquired in liquid isopropanol revealed a stabilizing effect. The differences in fracture forces can be attributed to a stress corrosion process on the surface. The size of the generated damage was influenced by the viscosity of the surrounding media.
As demonstrated with SPA-LEED and STM uniform height islands of preferred thickness form during the growth of Pb on Si(111). The islands form at temperatures T<250K and for fluxes F 1/60ML/sec which requires fast kinetics and balance between several atomic processes: diffusion towards the islands , diffusion to higher layers and preference for the atoms to remain on top of the preferred height islands. We have carried out SPA-LEED experiments to measure the barriers of the processes: we prepare an initial predominantly 5-step island height distribution and we deposit an additional 0.5ML Pb at different growth temperatures Tg to determine the transition to the next preferred height of 7-step islands (i.e. 2-step islands on top of the 5-step islands) with Spot Profile Analysis(SPA-LEED). We observe that 7-step island formation is possible above a minimum temperature Tg*=175K which indicates that the transfer of atoms from the surrounding region to the top of the islands is the main controlling process.
While surface kinetics measurements for single atom diffusion have proliferated, little work exists attempting to measure surface dynamics under equilibrium conditions. We will present our recent work on developing Temporal LEED Spectroscopy (TLS) as a dynamic probe of surfaces capable of kinetics measurements at both high temperatures and surface coverages. By tuning the diffraction to specific structural entities such as steps, islands, etc., and monitoring the diffracted signal as a function of time, dynamics information about these structures can be obtained. As an example we will present TLS results for the dynamics of step fluctuations on Si(001) [1]. We have measured activation energies and identified step-edge diffusion as the rate limiting process for 950K < T < 1130K. Although this result is in apparent disagreement with earlier work, a careful analysis, considering crossover temperatures between different microscopic processes, can reconcile the differences. 1. M. Kammler, et al., Phys. Rev. B (in press).
We present the first demonstration of Temporal LEED Spectroscopy’s ability to measure surface dynamics as shown by a study of step dynamics on vicinal Si(001). While we measure activation energies consistent with other work, the observed microscopic mechanism driving the fluctuations is inconsistent with previous claims. We exclude evaporation/condensation of atoms from the steps as the rate limiting kinetics in the temperature range of this experiment. Possible reasons for these differences are discussed.
Ultrafast X-ray diffraction
(2004)
Many fundamental processes in solids, such as heat transport and phase transitions involve atomic movement on ultrafast time-scales, but cannot be directly measured with visible light. Using ultrafast x-ray diffraction, atomic motion can be measured on its natural time-scale. Photo-excitation of bulk and layered semiconductors was achieved with 800-nm wavelength femtosecond laser pulses. Optical excitation triggers a chain of relaxation processes, causing rapid lattice heating, generation and propagation of stress/strain waves into the bulk and eventual anharmonic decay of coherent acoustic phonons into the thermal bath of the solid. While the first steps of carrier relaxation, excitation and decay of Raman-active optical phonons have been in the past characterized optically at surfaces, the bulk acoustic dynamics at longer times has not. We measure length scales of lattice excitation, thereby detecting ultrafast heat diffusion via fast electrons, coherent acoustic pulse propagation into the bulk or across buried interfaces and anharmonic damping of non-equilibrium acoustic phonons. The measurement is performed with sensitivity on lattice spacing of 10 femtometers (i.e., 3 nuclear diameters).