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<!doctype html>
<html>
<head>
<meta charset="utf-8">
<meta name="viewport" content="width=device-width, initial-scale=1.0, maximum-scale=1.0, user-scalable=no">
<title>Analysis of a Porous Surface</title>
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<div class="reveal">
<div class="slides">
<div style="" class="footer">
<p class="footer-img pull-left">
<img src="img/URLogo.png" height="40px"/>
</p>
<p class="pull-right footer-text"> Rainier Barrett and Eric Holmgren </p>
</div>
<section class="center" data-background="#000f0">
<h4 class="attn">Analysis of a Porous Surface</h4>
<h5> Surface Analysis </h5>
<p><i><small>Rainier Barrett and Eric Holmgren</small></i></p>
<p>
<small> April 27, 2017 </small>
</p>
</section>
<section>
<section class="center">
<h3 class="red"> The Surface </h3>
<img src="img/test_pores.png">
<!-- -->
</section>
<section class="center" data-background-color="#FFF">
<h4> Goals</h4>
<div class="frag-container center">
<ol>
<li class="fragment fade-in center">Determine average pore size.</li>
<li class="fragment fade-in center">Image the profile of the pore walls.</li>
<li class="fragment fade-in center">Determine chemical composition of the pore walls.</li>
</ol>
</div>
</section>
</section>
<section>
<section class="center">
<h3 class="red"> Pore Size Analysis</h3>
<h4> SEM Tomography and Image Processing</h4>
</section>
<section class="center" data-background-color="#FFF">
<h4> SEM: Working Principles</h4>
<ul>
<li>Fire a focused beam of electrons at surface, observe what comes back. </li>
<li>Different observations for different modes: backscattered electrons, secondary electrons, and light. </li>
<li>Each mode has a different interaction volume, which determines resolution. </li>
</ul>
<img src="img/interaction_volume.png" height="330px" style="position:relative; top:-50px; right:-50px" >
</section>
<section class="center" data-background-color="#FFF">
<h4> Procedure</h4>
<ol>
<li> Scan large area of surface with secondary electron mode. </li>
<li> Perform image processing on resultant images to get a distribution of pore sizes. </li>
<li> Analyze pore size statistics, specifically mean diameter. </li>
</ol>
<aside class="notes"> By scanning a large area of the surface, with the help of image processing we can quickly measure many pore diameters. From the resulting data we can easily obtain the mean pore diameter, and any other population statistics. A major advantage of this approach is the speed and repeatability of these techniques, once implemented as a program.
</aside>
</section>
<section class="center" data-background-color="#FFF">
<h4> Why SEM? </h4>
<ul>
<li>SEM can take a scan of a large area of the sample. </li>
<li>Image or series of images can be analyzed quickly with image processing software. </li>
<li>Through the use of secondary electron mode, we can specifically image the surface, making image processing even easier. </li>
<li>Overall, these features allow for a high-throughput, easily repeatable analysis method that generalizes to any porous surface.</li>
</ul>
</section>
<section class="center" data-background-color="#FFF">
<h4> Possible Alternatives </h4>
<ul>
<li>AFM: if pores are extremely small and surface is otherwise relatively flat, AFM in tapping mode could be used, but not optimal. </li>
<li>Confocal microscopy: it is possible to observe nm-scale images with confocal microscopy, but if the pores are of a smaller scale than this, it won't have the resolution we desire. </li>
</ul>
</section>
</section>
<section>
<section class="center">
<h3 class="red"> Pore Wall Profile Imaging</h3>
<h4> Angle Resolved SEM and Photogrammetry</h4>
</section>
<section class="center" data-background-color="#FFF">
<h4>Angle Resolved SEM</h4>
<ul>
<li>Use SEM to find large target pore</li>
<li>Angle electron beam to see inside of pore</li>
<li>Set angle that will maximize projected area of pore wall surface</li>
<li>Scan pore wall with electron beam</li>
<li>Collect secondary electrons to obtain topographical information</li>
</ul>
</section>
<section class="center" data-background-color="#FFF">
<h4>Angle Resolved SEM</h4>
<ul>
<li>This technique does not require a physical tip</li>
<li>High resolution</li>
<li>Angled beam can scan surface inside of exposed pore</li>
</ul>
</section>
<section class="center" data-background-color="#FFF">
<h4> Photogrammetry </h4>
<ul>
<li>Images taken at slightly different angles</li>
<li>Software uses feature recognition and relative displacement between images</li>
<li>Three dimensional model is formed</li>
</ul>
</section>
<section class="center" data-background-color="#FFF">
<h4> Photogrammetry </h4>
<img src="img/photogrammetry.jpg" height="330px" >
<img src="img/photogrammetry_gif.gif" height="330px" >
</section>
<section class="center" data-background-color="#FFF">
<h4> Etching </h4>
<ul>
<li>Use ion etching to remove a section of the porous surface</li>
<li>Allows better angle for SEM imaging of exposed pore wall</li>
</ul>
</section>
<section class="center" data-background-color="#FFF">
<h4> Etching: Possible Problems</h4>
<ul>
<li>Debris on newly exposed surface</li>
<li>Damage to surface structure</li>
</ul>
</section>
</section>
<section>
<section class="center">
<h3 class="red">Pore Wall Chemical Composition</h3>
<h4> Angle-Resolved AES and Ion-Sputtering MS </h4>
</section>
<section class="center" data-background-color="#FFF">
<h4> AES: Working Principles </h4>
<ul>
<li>Auger Electron Spectroscopy (AES): similar principle to SEM, but measures Auger electron kinetic energies. </li>
<li>Incoming electrons displace inner-shell electrons of sample, which are replaced by nearby ones, sometimes resulting in ejection of a valence-shell electron. </li>
<li>Auger electrons have a kinetic energy characteristic to the chemical species of the nucleus.</li>
</ul>
<img src="img/auger_process.png" height="330px" style="position:relative; top:-30px; right:-120px" >
</section>
<section class="center" data-background-color="#FFF">
<h4> Ion-Sputtering MS: Working Principles </h4>
<ul>
<li>Mass Spectroscopy needs ions to analyze mass/charge ratios to help determine chemical identities. </li>
<li>Ion-Sputtering: ion beam is fired at the surface, causing a release of secondary ions which are then accelerated and analyzed. </li>
</ul>
<img src="img/sputtering.jpg" height="250px" style="position:relative; top:-5px; " >
</section>
<section class="center" data-background-color="#FFF">
<h4> Procedure</h4>
<ol>
<li> Perform AES on unaltered surface at several angles. </li>
<li> Use ion-sputtering MS to analyze the surface and etch a hole deep enough to perform further AES on pore walls. </li>
<li> Perform AES on the pore walls and compare with results from step 1. </li>
</ol>
<aside class="notes"> By scanning a large area of the surface, with the help of image processing we can quickly measure many pore diameters. From the resulting data we can easily obtain the mean pore diameter, and any other population statistics. A major advantage of this approach is the speed and repeatability of these techniques, once implemented as a program.
</aside>
</section>
<section class="center" data-background-color="#FFF">
<h4> Why AR-AES and Ion-Sputtering MS? </h4>
<ul>
<li>By using AR-AES, we can directly compare the chemical compositions of the surface (low angle of incidence) with the pore walls. </li>
<li>Combined with Ion-Sputtering, we can cross-validate chemical identities. </li>
<li>Ion sputtering allows etching of the surface, allowing angle-resolved access to a cross-section of the pore walls. </li>
<li>These techniques can be done in tandem in a single machine run, given the equipment.</li>
</ul>
</section>
</section>
<section>
<section class="center" hide-footer="yes" data-background-video="mov/md_fade.mp4" data-background-video-loop data-background="#000000">
<div class="text-background">
<h3>Any Questions?</h3>
</div>
</section>
</section>
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