**Appendix A Appendix A**

**Appendix A** The main challenge of TSV characterization is to gain information from inside of the hole particularly the bottom part. As the TSV dimensions are almost larger than the cutting methods capability, such as FIB cross sectioning, it is hard to design a metrology in order to investigate the depth compositional profile, layer thicknesses, surface quality, conformality and overall step coverage all the way through a hole. The FIB could perform on TSV, but there are some challenges involved, such as sidewall Si redeposition, time consumption in the range of hours as well as low accuracy of a wavy cut known as curtaining e ffect. Transmission electron microscopy (TEM) with high resolution images gives the most information about deposited layers in a few nanometers range, but it takes lot of time and e ffort, not only for sample imaging, but also for sample preparation. According to the aforementioned challenges, for observing the TSV bottom sidewalls with TEM, the sample was cleaved precisely. Therefore, a series of indentations before and after the target structure were applied by a Nano Indenter tool in a way to hit the TSV. Subsequently, the cleaved sample was transferred to the FIB/SEM Strata 400, FEI tool. Figures below show the lamella preparation and lift-out procedure systematically using FIB technique. Carbon and e-Pt protection layers were applied respectively before utilizing any ion beam so as to protect the thin film on the structure (Figure A1a). The main challenge of TSV characterization is to gain information from inside of the hole particularly the bottom part. As the TSV dimensions are almost larger than the cutting methods capability, such as FIB cross sectioning, it is hard to design a metrology in order to investigate the depth compositional profile, layer thicknesses, surface quality, conformality and overall step coverage all the way through a hole. The FIB could perform on TSV, but there are some challenges involved, such as sidewall Si redeposition, time consumption in the range of hours as well as low accuracy of a wavy cut known as curtaining effect. Transmission electron microscopy (TEM) with high resolution images gives the most information about deposited layers in a few nanometers range, but it takes lot of time and effort, not only for sample imaging, but also for sample preparation. According to the aforementioned challenges, for observing the TSV bottom sidewalls with TEM, the sample was cleaved precisely. Therefore, a series of indentations before and after the target structure were applied by a Nano Indenter tool in a way to hit the TSV. Subsequently, the cleaved sample was transferred to the FIB/SEM Strata 400, FEI tool. Figures below show the lamella preparation and lift-out procedure systematically using FIB technique. Carbon and e-Pt protection layers were applied respectively before utilizing any ion beam so as to protect the thin film on the structure (Figure A1a). The main challenge of TSV characterization is to gain information from inside of the hole particularly the bottom part. As the TSV dimensions are almost larger than the cutting methods capability, such as FIB cross sectioning, it is hard to design a metrology in order to investigate the depth compositional profile, layer thicknesses, surface quality, conformality and overall step coverage all the way through a hole. The FIB could perform on TSV, but there are some challenges involved, such as sidewall Si redeposition, time consumption in the range of hours as well as low accuracy of a wavy cut known as curtaining effect. Transmission electron microscopy (TEM) with high resolution images gives the most information about deposited layers in a few nanometers range, but it takes lot of time and effort, not only for sample imaging, but also for sample preparation. According to the aforementioned challenges, for observing the TSV bottom sidewalls with TEM, the sample was cleaved precisely. Therefore, a series of indentations before and after the target structure were applied by a Nano Indenter tool in a way to hit the TSV. Subsequently, the cleaved sample was transferred to the FIB/SEM Strata 400, FEI tool. Figures below show the lamella preparation and lift-out procedure systematically using FIB technique. Carbon and e-Pt protection layers were applied respectively before utilizing any ion beam so as to protect the thin film on the structure (Figure A1a). 

**Figure A1.** SEM images of (**a**) structure layout and (**b**) SEM images of applied carbon and e-Pt protection layers to the cleaved TSV and rough thinning lamella before lift-out and after tilting. **Figure A1.** SEM images of (**a**) structure layout and (**b**) SEM images of applied carbon and e-Pt protection layers to the cleaved TSV and rough thinning lamella before lift-out and after tilting. **Figure A1.** SEM images of (**a**) structure layout and (**b**) SEM images of applied carbon and e-Pt protection layers to the cleaved TSV and rough thinning lamella before lift-out and after tilting. 

After depositing carbon, e-Pt and also i-Pt protection layers, the target layer is safe, and it is time to dig in the lamella surroundings. Then, as the lamella is still attached and stable enough, rough thinning has to be done line by line via "cleaning cross section thinning" mode before lift-out (Figure A1b). After the lamella release-cutting at the very bottom, next step is lifting out the free lamella which was welded earlier with Pt to the Omniprobe manipulator (Figure A2a) by GIS. After depositing carbon, e-Pt and also i-Pt protection layers, the target layer is safe, and it is time to dig in the lamella surroundings. Then, as the lamella is still attached and stable enough, rough thinning has to be done line by line via "cleaning cross section thinning" mode before lift-out (Figure A1b). After the lamella release-cutting at the very bottom, next step is lifting out the free lamella which was welded earlier with Pt to the Omniprobe manipulator (Figure A2a) by GIS. After depositing carbon, e-Pt and also i-Pt protection layers, the target layer is safe, and it is time to dig in the lamella surroundings. Then, as the lamella is still attached and stable enough, rough thinning has to be done line by line via "cleaning cross section thinning" mode before lift-out (Figure A1b). After the lamella release-cutting at the very bottom, next step is lifting out the free lamella which was welded earlier with Pt to the Omniprobe manipulator (Figure A2a) by GIS. 

**Figure A2.** SEM images of (**a**) lifting out the free lamella and (**b**) oblique view during finishing and post-finishing processes with i-Beam and e-Beam.

 F.;

*Nanomaterials* **2019**, *9*, 1035 **Figure A2.** SEM images of (**a**) lifting out the free lamella and (**b**) oblique view during finishing and post-finishing processes with i-Beam and e-Beam. 

Then, the lamella was welded to the TEM sample holder. The manipulator welded area was unattached and finally it was withdrawn. In this stage, finishing and post-finishing processes of the lamella with i-Beam and e-Beam were performed respectively which is shown in Figure A2b. The sample is now thin and transparent enough for TEM observation. Therefore, the welded sample to the sample holder was transferred to the TEM Tecnai F20 200 kV, FEI tool for high resolution pictures (Figure A3). Then, the lamella was welded to the TEM sample holder. The manipulator welded area was unattached and finally it was withdrawn. In this stage, finishing and post-finishing processes of the lamella with i-Beam and e-Beam were performed respectively which is shown in Figure A2b. The sample is now thin and transparent enough for TEM observation. Therefore, the welded sample to the sample holder was transferred to the TEM Tecnai F20 200 kV, FEI tool for high resolution pictures (Figure A3). 

**Figure A3.** TEM images of the entire overview of halved TSV structure. **Figure A3.** TEM images of the entire overview of halved TSV structure.
