{"id":111992,"date":"2023-04-28T10:36:01","date_gmt":"2023-04-28T14:36:01","guid":{"rendered":"https:\/\/www.hajim.rochester.edu\/senior-design-day\/?p=111992"},"modified":"2024-03-01T14:59:20","modified_gmt":"2024-03-01T18:59:20","slug":"characterization-of-vapor-phase-concentrations-for-icvd","status":"publish","type":"post","link":"https:\/\/www.hajim.rochester.edu\/senior-design-day\/characterization-of-vapor-phase-concentrations-for-icvd\/","title":{"rendered":"Characterization of Vapor Phase Concentrations for iCVD"},"content":{"rendered":"\n<h2 class=\"wp-block-heading\">Team Members<\/h2>\n\n\n\n<ul class=\"wp-block-list\">\n<li>Lauren Redus<\/li>\n\n\n\n<li>Samuel Meil<\/li>\n\n\n\n<li>Autumn Kudlack<\/li>\n\n\n\n<li>Ana Cerezer<\/li>\n<\/ul>\n\n\n\n<h2 class=\"wp-block-heading\">Project Sponsor<\/h2>\n\n\n\n<p>Dr. Wyatt Tenhaeff, Chemical Engineering<\/p>\n\n\n\n<h4 class=\"wp-block-heading\">Abstract<\/h4>\n\n\n\n<p>Initiated Chemical Vapor Deposition (iCVD) is a technique utilized by Tenhaeff Labs at the University of Rochester to control the properties of polymeric thin films and coatings. A critical component of studying iCVD kinetics is dependent on the concentration of the monomer and initiator in the gas phase. This concentration measurement is nontrivial due to the low volatility of the monomers, and therefore, there is demonstrated need for the construction and implementation of a concentration measurement system.<\/p>\n\n\n\n<h4 class=\"wp-block-heading\">Background<\/h4>\n\n\n\n<p>The monomer and initiator are vaporized using a bubbler system and co-fed into the iCVD reactor. Typical iCVD monomers are large organic molecules with low vapor pressures at room temperature, and as a result, are present at very low vapor concentrations. Therefore, measurement methods must be sensitive enough to identify these small composition changes with the mixture of the monomer and carrier gas.<\/p>\n\n\n\n<h4 class=\"has-text-align-left wp-block-heading\">System Requirements <\/h4>\n\n\n\n<ul class=\"wp-block-list\">\n<li>Operating conditions of 1 atm, 25\u00b0C <\/li>\n\n\n\n<li>Continuous concentration measurement system capable of being integrated into the current iCVD system used by Tenhaeff Labs <\/li>\n\n\n\n<li>Model compound with similar properties to butyl acrylate <\/li>\n\n\n\n<li>Optimize bubbler design<\/li>\n<\/ul>\n\n\n\n<h4 class=\"wp-block-heading\">Proposed Approach<\/h4>\n\n\n\n<ul class=\"wp-block-list\">\n<li>Chosen Model Compound: ethyl acetate<\/li>\n\n\n\n<li>Infrared Radiation Cell (IR): IR LED emitter + IR receiver, chosen compound absorbs within C-H wavenumber of 3.4 \u00b5m<\/li>\n\n\n\n<li>Mass Flow Measurements (MFC\/MFM): measure difference before and after bubbler system through a small differential heat transfer<\/li>\n\n\n\n<li>Gas Chromatograph (GC): correlate obtained voltages from IR cell with known concentrations<\/li>\n<\/ul>\n\n\n\n<h4 class=\"wp-block-heading\">Results<\/h4>\n\n\n\n<h5 class=\"wp-block-heading\">Optimization Experiment<\/h5>\n\n\n\n<figure class=\"wp-block-image size-full is-resized\"><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/frits-3.png\" alt=\"\" class=\"wp-image-133952\" width=\"455\" height=\"509\" srcset=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/frits-3.png 649w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/frits-3-268x300.png 268w\" sizes=\"auto, (max-width: 455px) 100vw, 455px\" \/><figcaption class=\"wp-element-caption\">Figure 1: Frit Optimization Prototype<\/figcaption><\/figure>\n\n\n\n<figure class=\"wp-block-image size-large is-resized\"><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/labels-2-1024x338.png\" alt=\"\" class=\"wp-image-133982\" width=\"334\" height=\"110\" srcset=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/labels-2-1024x338.png 1024w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/labels-2-300x99.png 300w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/labels-2-768x253.png 768w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/labels-2-1536x506.png 1536w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/labels-2-2048x675.png 2048w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/labels-2-1200x396.png 1200w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/labels-2-1980x653.png 1980w\" sizes=\"auto, (max-width: 334px) 100vw, 334px\" \/><\/figure>\n\n\n\n<figure class=\"wp-block-table is-style-regular\"><table class=\"has-background-background-color has-background\"><thead><tr><th class=\"has-text-align-center\" data-align=\"center\">Frit Type<\/th><th class=\"has-text-align-center\" data-align=\"center\">Avg. Vaporization Rate (mL\/h)<\/th><th class=\"has-text-align-center\" data-align=\"center\">Flow Rate (SCCM)<\/th><\/tr><\/thead><tbody><tr><td class=\"has-text-align-center\" data-align=\"center\">Coarse<\/td><td class=\"has-text-align-center\" data-align=\"center\">3.0<\/td><td class=\"has-text-align-center\" data-align=\"center\">13. \u00b1 1.2<\/td><\/tr><tr><td class=\"has-text-align-center\" data-align=\"center\">Extra Fine<\/td><td class=\"has-text-align-center\" data-align=\"center\">2.8<\/td><td class=\"has-text-align-center\" data-align=\"center\">12. \u00b1 1.8<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n<h5 class=\"wp-block-heading\" style=\"text-transform:none\">Mass Flow System<\/h5>\n\n\n\n<figure class=\"wp-block-gallery has-nested-images columns-default is-cropped wp-block-gallery-1 is-layout-flex wp-block-gallery-is-layout-flex\">\n<figure class=\"wp-block-image size-large\"><img loading=\"lazy\" decoding=\"async\" width=\"432\" height=\"288\" data-id=\"133712\" src=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/MFC_Calib_Curve-1-2.png\" alt=\"\" class=\"wp-image-133712\" srcset=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/MFC_Calib_Curve-1-2.png 432w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/MFC_Calib_Curve-1-2-300x200.png 300w\" sizes=\"auto, (max-width: 432px) 100vw, 432px\" \/><figcaption class=\"wp-element-caption\">Figure 2: MFM Calibration Curve between Voltage and Flow Rate<\/figcaption><\/figure>\n\n\n\n<figure class=\"wp-block-image size-large\"><img loading=\"lazy\" decoding=\"async\" width=\"432\" height=\"288\" data-id=\"133702\" src=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/MFC_Conc_Curve-1-2.png\" alt=\"\" class=\"wp-image-133702\" srcset=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/MFC_Conc_Curve-1-2.png 432w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/MFC_Conc_Curve-1-2-300x200.png 300w\" sizes=\"auto, (max-width: 432px) 100vw, 432px\" \/><figcaption class=\"wp-element-caption\">Figure 3: Vapor Phase Mole Fraction Ethyl Acetate vs. Time<\/figcaption><\/figure>\n<\/figure>\n\n\n\n<p>In 5 hours, ~ 2 mol% ethyl acetate was measured in the vapor phase. <\/p>\n\n\n\n<p>Theoretical maximum ethyl acetate mole fraction percentage: 12 mol%  <\/p>\n\n\n\n<h5 class=\"wp-block-heading\">IR Cell<\/h5>\n\n\n<div class=\"wp-block-image\">\n<figure class=\"aligncenter size-full is-resized\"><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/Picture1-1.png\" alt=\"\" class=\"wp-image-133762\" width=\"318\" height=\"182\" srcset=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/Picture1-1.png 640w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/Picture1-1-300x172.png 300w\" sizes=\"auto, (max-width: 318px) 100vw, 318px\" \/><figcaption class=\"wp-element-caption\">Figure 4: IR Cell Schematic<\/figcaption><\/figure>\n<\/div>\n\n<div class=\"wp-block-image\">\n<figure class=\"aligncenter size-full is-resized\"><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-26.png\" alt=\"\" class=\"wp-image-133772\" width=\"394\" height=\"170\" srcset=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-26.png 871w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-26-300x130.png 300w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-26-768x332.png 768w\" sizes=\"auto, (max-width: 394px) 100vw, 394px\" \/><figcaption class=\"wp-element-caption\">Figure 5: 3D-Printed Models of IR Fittings<\/figcaption><\/figure>\n<\/div>\n\n\n<figure class=\"wp-block-image size-large is-resized\"><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/finalircell-1-1-1024x562.jpg\" alt=\"\" class=\"wp-image-133802\" width=\"610\" height=\"334\" srcset=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/finalircell-1-1-1024x562.jpg 1024w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/finalircell-1-1-300x165.jpg 300w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/finalircell-1-1-768x422.jpg 768w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/finalircell-1-1-1536x844.jpg 1536w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/finalircell-1-1-2048x1125.jpg 2048w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/finalircell-1-1-1200x659.jpg 1200w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/finalircell-1-1-1980x1088.jpg 1980w\" sizes=\"auto, (max-width: 610px) 100vw, 610px\" \/><figcaption class=\"wp-element-caption\">Figure 6: Implemented IR Cell<\/figcaption><\/figure>\n\n\n\n<p>The IR cell utilizes an IR LED emitter and an IR sensor that operate with a wavenumber of 3.4 \u00b5m, the region where C-H absorbs in ethyl acetate. The measured absorbance can be related to concentration through Beer&#8217;s Law, where A = \u025bcl. A circuit was implemented to enhance the signal from the sensor and operate with a pulsed IR light input. <\/p>\n\n\n\n<figure class=\"wp-block-image size-large is-resized\"><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-27-1024x389.png\" alt=\"\" class=\"wp-image-134092\" width=\"610\" height=\"231\" srcset=\"https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-27-1024x389.png 1024w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-27-300x114.png 300w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-27-768x292.png 768w, https:\/\/www.hajim.rochester.edu\/senior-design-day\/wp-content\/uploads\/2023\/04\/image-27.png 1072w\" sizes=\"auto, (max-width: 610px) 100vw, 610px\" \/><figcaption class=\"wp-element-caption\">Figure 7: Oscilloscope Input Reading (Left), Sensor Reading from LabJack (Right)<\/figcaption><\/figure>\n\n\n\n<h4 class=\"wp-block-heading\">Conclusion and Future Work<\/h4>\n\n\n\n<p>The differential measurements of the mass flow controllers displayed ~2 mol% ethyl acetate after 5 hours. The MFC system can be further improved with higher sensitivity and calibration of the instruments. The IR system is complete and additional testing is required to correlate the measured voltages with ethyl acetate concentration using a gas chromatograph. <\/p>\n\n\n\n<p>Both prototype measurement methods demonstrate promise to be utilized within the Tenhaeff Labs and would require minimal changes to the current configuration of the iCVD reactors. The limiting factor for implementation of the proposed measurements is instrument sensitivity. If these methods are to be pursued further, it is suggested to build or utilize instrumentation that is more specialized and easily programmable. Vacuum conditions with these measurement methods should be explored as the current iCVD system is performed under vacuum pressure.<\/p>\n\n\n\n<h4 class=\"wp-block-heading\">Acknowledgements<\/h4>\n\n\n\n<p>We would like to thank their project sponsor, Dr. Wyatt Tenhaeff, graduate students Fei Hu and Ni Huo, and their TA, Levi Sunday-Lefkowitz. Additionally, we would like to thank Dr. Doug Kelley, Clair Cunningham, Mason Garlatti, Dr. Melodie Lawton, Jeff Lefler, Professor Mark Juba, Wayne Griffin, and Paul Osborne. We are grateful for their time, support, and dedication to the project. This work was supported in part by the National Science Foundation under grant CBET-1845805.<\/p>\n","protected":false},"excerpt":{"rendered":"<p>This project aims to build and design a continuous concentration measurement system for a low-volatile monomer in the vapor phase. <\/p>\n","protected":false},"author":6242,"featured_media":134392,"comment_status":"closed","ping_status":"closed","sticky":false,"template":"","format":"standard","meta":{"_coblocks_attr":"","_coblocks_dimensions":"","_coblocks_responsive_height":"","_coblocks_accordion_ie_support":"","_monsterinsights_skip_tracking":false,"_monsterinsights_sitenote_active":false,"_monsterinsights_sitenote_note":"","_monsterinsights_sitenote_category":0,"footnotes":""},"categories":[76],"tags":[16422,16502,16512,6392],"coauthors":[8612],"class_list":["post-111992","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-che-archive","tag-chemical-engineering","tag-icvd","tag-ir-detector","tag-mass-transfer"],"acf":[],"yoast_head":"<!-- This site is optimized with the Yoast SEO plugin v27.5 - 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