NSF Grant for Chemical Engineering

The technique of initiated Chemical Vapor deposition (iCVD) of polymers was developed by Dr. Karen Gleason at the Massachusetts Institute of Technology. The technique involves introducing monomer and initiator vapors into a vacuum chamber, where polymerization and deposition occur on the surface of the substrate. It offers the following advantages over conventional liquid-phase polymer deposition:

• Solvent-less process
• Decouples initiation and polymerization temperatures
• Adaptable to different monomer initiator chemistries
• Generates conformal coatings on complex substrates
• Excellent control of film composition and thickness
• Versatile fabrication tool suitable for various applications

As a faculty member in the chemical engineering department at the University of Connecticut (UConn) from 2011 to 2015, Dr. Aravind Suresh carried out research projects using iCVD[1-3] and taught it to undergraduate students as part of the senior laboratory course. Based on his knowledge and experience, he identified and listed five important modifications to the iCVD process in the NSF-MRI proposal to develop an instrument with enhanced capabilities for materials research:

• In situ infrared spectroscopy using ATR crystal embedded in the chamber stage
• Photo initiated chemical vapor deposition using lamp suspended inside the chamber
• Consistent delivery and polymerization of very low vapor pressure monomers inside the chamber
• Polymerization and deposition of high vapor pressure monomers
• Using the chamber for photocatalytic studies by coupling the instrument with a gas chromatograph

The assembled and operational instrument is expected to enhance the research capabilities of the faculty at Manhattan University and enable the conception and execution of interdisciplinary research projects. It is expected to foster collaboration between different departments at Manhattan University as well as between the institution and other academic and industrial entities. The instrument is also expected to function as a teaching tool for undergraduate and graduate students at Manhattan University and as an outreach tool for school students in the Bronx and other regions of New York.

As part of the grant, the engineering team at Manhattan University was charged with developing the instrument. They achieved this goal by following these steps:

1. A plan for the design was submitted as part of the grant proposal and was modified along the way as needed.
2. Components and parts were procured from a variety of specialized as well as general vendors and assembled to form the final instrument.
3. Two graduate assistants from the chemical engineering department at Manhattan University – Mr. Jason Risolo (B.S. 2020, M.S. 2022) and Mr. Connor Smith (B.S. 2022, M.S. 2024) provided valuable assistance in both the design and assembly aspects of the process.
4. The technicians at the machine shop at UConn fabricated components and parts that needed to be customized based on the desired capabilities of the instrument. The control system for the instrument was purchased from GVD corporation based in Massachusetts.
5. The assembly of the instrument was completed in the summer of 2024. The instrument is located in LEO 429, a laboratory in the chemical engineering department at Manhattan University.

The most challenging aspect of the development process involved the customized components that required coordination between the team in Bronx, NY and the machine shop in Storrs, CT.  A particularly time-consuming part was putting together the circuit for in situ spectrophotometry. A system had to be designed for the crystal in the Attenuated Total Reflectance (ATR) accessory to mate with the slit in the chamber (for measurement) and then detach (for cleaning) and then reattach in the same position so that the optical connection between the spectrophotometer and the accessory could be reestablished. Before that, a flexible base had to be built for the spectrophotometer so that the optical connection could be set up in the first place. The PI would be happy to arrange a campus visit for those interested to show them the instrument and provide more specific details about the instrument development process.