A new beam-assisted process for removing silicon from a surface in the nanometer scale in a conventional scanning electron microscope is presented. This approach is based on focused electron beam induced etching with pure chlorine gas being used as the precursor. In contrast to the established etching process using a focused ion beam (with or without the addition of a precursor), no amorphization and gallium implanting of the substrate takes place. The observed low etch rates facilitate removal with sub-nanometer precision. No spontaneous etching of silicon as in the case of xenon difluoride was observed. Etch rates of up to 4 nm min( - 1) could be achieved as well as a minimum feature size of below 80 nm. The effect of etching parameters like electron beam energy, electron beam accelerating voltage or pixel spacing were systematically examined. Finally, the underlying etching mechanism in terms of secondary electron interactions and precursor replenishment is discussed.
In any scanning electron microscope (SEM) organic contamination of the vacuum chamber leads to undesired material deposition resulting in artifacts in imaging or compromises focused electron beam induced processes like etching (FEBIE) [S. Matsui and K. Mori, Appl. Phys. Lett 51, 1498 (1987)] or deposition (FEBID) [S. Matsui and K. Mori, J. Vac. Sci. Technol. B 4, 299 (1986); W. F. van Dorp and C. W. Hagen, J. Appl. Phys. 4, 081301 (2008)]. This effect can also be used on purpose as a method to evaluate the contamination level of a SEM. With a standardized process for controlled deposition from residual gas, a method to evaluate the contamination level of an electron microscope quantitatively and reproductively was developed. Additionally, this method not only allows monitoring the contamination level of a SEM over its lifetime. Also the impact of various deposition parameters on the extent of contamination deposition has been investigated systematically. This method also allows comparing the status of different tools. A comparison of three different SEM tools of different vendors and with different fields of application is demonstrated.
Recently focused-electron-beam-induced etching of silicon using molecular chlorine (Cl(2)-FEBIE) has been developed as a reliable and reproducible process capable of damage-free, maskless and resistless removal of silicon. As any electron-beam-induced processing is considered non-destructive and implantation-free due to the absence of ion bombardment this approach is also a potential method for removing focused-ion-beam (FIB)-inflicted crystal damage and ion implantation. We show that Cl(2)-FEBIE is capable of removing FIB-induced amorphization and gallium ion implantation after processing of surfaces with a focused ion beam. TEM analysis proves that the method Cl(2)-FEBIE is non-destructive and therefore retains crystallinity. It is shown that Cl(2)-FEBIE of amorphous silicon when compared to crystalline silicon can be up to 25 times faster, depending on the degree of amorphization. Also, using this method it has become possible for the first time to directly investigate damage caused by FIB exposure in a top-down view utilizing a localized chemical reaction, i.e. without the need for TEM sample preparation. We show that gallium fluences above 4 × 10(15) cm(-2) result in altered material resulting from FIB-induced processes down to a depth of ∼ 250 nm. With increasing gallium fluences, due to a significant gallium concentration close beneath the surface, removal of the topmost layer by Cl(2)-FEBIE becomes difficult, indicating that gallium serves as an etch stop for Cl(2)-FEBIE.
A new approach using focused electron beam induced deposition (FEBID) to deposit catalyst particles is reported for the synthesis of single crystalline silicon nanowires (SiNWs) grown by low pressure chemical vapor deposition (LPCVD). The FEBID deposited gold dot arrays fabricated from an acac-Au(III)-Me(2) precursor were investigated by AFM and EDX. The depositions were found to form a sharp tip and a surrounding halo and consist of only 10 at.% Au. However, SiNWs could be synthesized on the deposited catalyst using the vapor-liquid-solid (VLS) method with a mixture of 2% SiH(4) in He at 520 °C. NW diameters from 30 nm up to 150 nm were fabricated and the dependency of the NW diameter on the FEBID deposition time was observed. TEM analysis of the SiNWs revealed a [110] growth direction independent of the NW diameter. This new method provides a maskless and resistless approach for generating catalyst templates for SiNW synthesis on arbitrary surfaces.
A novel method for cleaning a high vacuum chamber is presented. This method is based on concurrent in situ high-energetic UV light activation of contaminants located in the residual gas and at the vacuum chamber surfaces as well as the in situ generation of highly reactive ozone. Ozone oxidizes the contaminants to volatile species. Investigations by energy-dispersive x-ray analysis of residual gas depositions and mass-spectroscopy measurements of the residual gas in the vacuum chamber identify the contaminant species as hydrocarbons. After a cleaning period of 8 h, a decrease in measured chamber contamination by about 90% could be achieved according to atomic force microscope analysis. Mass spectroscopy measurements using a residual gas analyzer indicate the creation of volatile, carbonaceous species during the cleaning process.
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