TEM ANALYSIS REPORT Company: Santa Barbara Infrared

TEM ANALYSIS REPORT Company: Santa Barbara Infrared
Client: Tom Danielson Job Number: C0KBM520 EAG Technical Contact: Martin Izquierdo Date: May 9, 2019 810 Kifer Road Sunnyvale, CA 94086

Background Information from Client
EAG LABORATORIES | eag.com Job #C0KBM520

Background Information from Client
After discussing your concerns and reviewing the SEM images, we have decided to proceed with the 2um x 10um TEM cores in the following manner: Prepare the first core (sample #1) using the bottom core from the Lower Left Quadrant sample. We are aware that the core may come apart at the boundary between the intermetal and Indium. If it does come apart, that already tells us something important about our intermetal-Indium boundary. 2) If the first sample does not fall apart, please use the original indicated site for sample #2 (RIIC-side core of the Lower Left Quadrant). If the first sample falls apart, proceed to select sample #2 using either one of the three green boxes I’ve drawn, *or* if you can find a better candidate for a core (thin enough intermetal to capture both the RIIC and the intermetal-Indium boundary and good boundary continuity) outside the region of this SEM image, please use that instead. For sample #3 (RIIC side core of Upper Right Quadrant) please use the originally indicated site for the Upper Right Quadrant—I do see a continuity between the intermetal and Indium there. 4) Hold off on sample #4 (bottom core of Upper Right Quadrant) for now – it is of lower importance. EAG LABORATORIES | eag.com Job #C0KBM520

EAG LABORATORIES | eag.com Job #C0KBM520
Analysis Overview Analysis Scope: S/TEM analysis of layered interfaces. Sample Identification: Lo left #1 Lo left #2 Upper Right #3 Summary: Preferential thinning was observed. Client feedback is requested. EAG LABORATORIES | eag.com Job #C0KBM520

Lo Left #1 EAG LABORATORIES | eag.com Job #C0KBM520

Top down SEM AOI EAG LABORATORIES | eag.com Job #C0KBM520

FIB thinning progression Preferential thinning EAG LABORATORIES | eag.com Job #C0KBM520

Pt (EAG) Thick region BF STEM HAADF STEM EAG LABORATORIES | eag.com Job #C0KBM520

BF STEM HAADF STEM EAG LABORATORIES | eag.com Job #C0KBM520

EDS Maps Lo Left#1 EAG LABORATORIES | eag.com Job #C0KBM520

Lo Left #2 EAG LABORATORIES | eag.com Job #C0KBM520

FIB thinning progression Preferential thinning EAG LABORATORIES | eag.com Job #C0KBM520

Pt (EAG) Thick region BF STEM HAADF STEM EAG LABORATORIES | eag.com Job #C0KBM520

EDS Maps Lo Left#2 (1/2) EAG LABORATORIES | eag.com Job #C0KBM520

EDS Maps Lo Left#2 (2/2) EAG LABORATORIES | eag.com Job #C0KBM520

Upper Right #3 EAG LABORATORIES | eag.com Job #C0KBM520

Pt (EAG) Grid Post Thick region BF STEM HAADF STEM EAG LABORATORIES | eag.com Job #C0KBM520

EDS Maps Upper Right #3 (1/2) EAG LABORATORIES | eag.com Job #C0KBM520

EDS Maps Upper Right #3 (2/2) EAG LABORATORIES | eag.com Job #C0KBM520

Technical Notes The TEM-ready samples were prepared using the in situ FIB lift out technique on an FEI Strata 400 Dual Beam FIB/SEM. The samples were capped with sputtered Ir and e-C/e-Pt/I-Pt prior to milling. The TEM lamella thickness was ~100nm. The samples were imaged with a FEI Tecnai TF-20 FEG/TEM operated at 200kV in bright-field (BF) STEM mode and high-angle annular dark-field (HAADF) STEM mode. The STEM probe size was 1-2nm nominal diameter. EDS spectra were acquired in STEM mode using FEI Osiris 4SDD system. The images in this report were compressed to allow for easy file sharing. Full resolution *.TIFF images are available upon request. EAG has an image viewing and measurement software called EMview that can be used to open these images and make additional measurements after calibrating the image from the scale marker. It can be downloaded from: EAG LABORATORIES | eag.com Job #C0KBM520

C0JR456 Appendix Data are provided in several possible forms: There are four types of contrast in Transmission Electron Microscopy Mass Thickness Contrast is the easiest to understand and arises when the sample is locally thicker and or contains material with a high atomic number or both. These regions of larger mass thickness reduce the number of electrons which get to the detector and the image is locally darker. Voids have bright contrast, tungsten particles look dark. Amorphous materials always show only mass thickness contrast. Diffraction Contrast is very strong in bright field TEM or STEM images and is always seen in polycrystalline materials. These images are labeled as either “BF-TEM” or “TE images”. Very small changes in crystal orientation have a dramatic effect on the local transmission properties of crystalline materials. Diffraction contrast is very commonly seen across grain boundaries where there is slight tilt from one grain to another. Strongly transmitting grains are bright; diffracting grains are dark, even though each grain has the same chemistry. Strain contrast is a variant of diffraction contrast and is seen as a result of large local strain fields like those generated by dislocations and precipitates. Dark field TEM images are another form of diffraction contrast (not to be confused with High Angle Annular Dark Field STEM images). These images are labeled as DF-TEM. These images highlight specific crystallographic orientations of specific compounds. These images are much less commonly shown than HAADF images. Phase Contrast is found in HR-TEM images and requires very thin samples. The TEM image is interference pattern resulting from the combination of the transmitted and diffracted beams. The fringe pattern that results has the atomic spacing distance of the diffracted beams that have combined with the transmitted beam. HRTEM images show lattice points (not atoms). Z-Contrast STEM is a special form of Mass Thickness contrast performed in a Scanning-Transmission Electron Microscope. EAG has six such instruments. These images are labeled as “ZC” images. Z-contrast STEM is a form of Rutherford Scattering in which electrons are scattered to very large angles and are collected with a special detector. The scattering goes as Z2 and the resulting image can be directly interpreted as qualitative chemical map. The image contrast is due to differences in the average atomic mass; with heavier atomic masses appearing brighter than lighter average atomic masses. There is typically very little diffraction contrast in these images. These images are sometimes referred to as High Angle Annular Dark Field images (HAADF). “Z Contrast” can show atomic columns in the highest resolution images. EAG LABORATORIES | eag.com Job #C0KBM520

C0JR456 Appendix Diffraction patterns These patterns show the symmetry of the crystallographic structure being investigated. Interpretation of these patterns can be complex: intensities, peak sharpness, overlapping patterns and other characteristics can be the due to a multitude of causes. TEM EDS (Energy Dispersive Spectroscopy analysis of x-rays) allows for qualitative elemental chemical analysis on the 1nm scale and can be in the form of point spectra, line scans, or 2D maps. Analysis is possible across the Periodic Table (B-Pb) with a detection limit of about 1 atomic percent. Higher concentrations ~10% are required for the very light elements (Li, Be, and B). Please note that the typical “standard less quantification” has an unknown accuracy. For well behaved samples, accuracy can be quite good (5% relative, compared to standard values); other samples are more problematic. Not all problematic samples can be identified - therefore the error in the quantification of TEM EDS is often unknown. EAG has taken special care to eliminate artifactual EDS peaks (C, Ga, Cu) which can come from specimen preparation. EELS (Electron Energy Loss Spectroscopy). Typically used as a compliment to EDS. It can have some advantages vs EDS it can have slightly better resolution It has better sensitivity to lower mass elements (Boron to Oxygen) EELS can provide additional information on the chemical state of some elements Aberration Corrected STEM images (AC-STEM) This is an advanced tool set that provides substantially higher resolution images than either traditional HR-TEM or STEM images. These images typically required modified preparation techniques and can provide sub 1nm EDS resolution. Unless specifically stated otherwise elsewhere in this report the uncertainty of dimensional TEM measurements is about ±3% (providing an estimated level of confidence of 95% using a coverage factor k = 2 for well defined features >3nm). Uncertainty estimates are calculated in accordance with the ISO “Guide to the Expression of Uncertainty in Measurement. Sharp, well-defined interfaces yield better measurements. EAG LABORATORIES | eag.com Job #C0KBM520

Feedback Thank you for using EAG Laboratories. Please take a moment and let us know how well we met your expectations. You can click on this link or copy it into your internet browser: This is the end of the Report. This report should not be reproduced except in full without the written approval of EAG. EAG LABORATORIES | eag.com Job #C0KBM520

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