Paper ID #8018

A New Interdisciplinary Engineering Course on Nanoscale Transport Phe-nomena

Prof. Zhiyong Gu, University of Massachusetts, LowellProf. Bridgette Maria Budhlall, University of Massachusetts

I received my B.Sc. degree with Honors in Natural Sciences, double-majoring in Analytical Chemistryand Biochemistry, from the University of the West-Indies, St. Augustine, Trinidad in 1992. I spenttwo years working as an R&D Chemist developing vinyl-acrylic latex for pressure sensitive adhesiveapplications and styrene-acrylic emulsions for architectural coatings.

My doctoral work was conducted at Lehigh University, Bethlehem, PA. with Professor Mohammed El-Aasser in the Emulsion Polymers Institute in the Department of Chemical Engineering as part of the Poly-mer Science and Engineering program. I received my Ph.D in 2000 for a dissertation entitled: ”GraftingReactions in the Emulsion Polymerization of Vinyl Acetate using Poly(vinyl alcohol) as Emulsifier”.

Upon graduation, I was hired into the Ph.D Career Development Program at Air Products & Chemicals,Inc., PA. where I conducted three one-year rotations in each of the three divisions: Polymer ChemicalsTechnology, Corporate R&D Science & Technology Center (CSTC) and Gases and Electronics AdvancedTechnology. I gained experience developing photoresist polymers for nanolithography and supportedthe development of a high-throughput, integrated monolith catalyst reactor system, the Monolith LoopReactor. I spent the next three years in CSTC as the Project Leader for the High Refractive Index Fluidsfor 193nm Lithography Program where I was responsible for invention, implementation, and support ofadvanced immersion fluids for 193nm Immersion Lithography. I also lead and coordinated the Stage Gateof this program, including the development and feasibility efforts between Electronics R&D, CorporateR&D and Electronics Business Development team members.

In 2006, I was awarded an International Network of Emerging Science & Technology (INEST) Fellowshipfrom Phillip Morris USA to spend the year working with Professor Orlin D. Velev in the departmentof Chemical and Bimolecular Engineering at North Carolina State University, Raleigh, NC. There, Isynthesized novel polymer microcapsules with core-shell morphology comprising of Au@Polymer thatare microwave-, photo- and thermo-responsive.

I began the 2007 academic year as an Assistant Professor in the Department of Plastics Engineering at theUniversity of Massachusetts Lowell. I am a member of the Nanomanufacturing Center at UML, wheremy Polymer Colloids group studies the chemistry and physics of nanocolloidal systems. These colloidalentities are assembled and fabricated into more complex supracolloidal structures. I am interested inthe synthesis of nanostructured materials with controlled morphologies specifically designed to triggerand control motility and assembly, the development of methods for self-assembly of colloidal matter, theunderstanding of the molecular interactions involved between molecular and colloidal building blocksand potential macroscopic substrates. I find it important that my technology be scaled-up and is of usein a variety of industrial applications ranging from biosensors, chemical sensors and nanofluidic devices,smart coatings, electronic inks and adhesives, drug delivery systems, polymers for cellular transport andanalysis and for biomedical devices.

Dr. Hongwei Sun, University of Massachusetts, Lowell

Hongwei Sun is an associate professor in the Department of Mechanical Engineering at University ofMassachusetts Lowell (UML). He graduated with a Ph. D. from Institute of Engineering Thermophysicsat Chinese Academy of Science in 1998. Prior to joining UML in 2005, he worked as a postdoctoralresearcher at University of Rhode Island (URI) and later a research scientist at Massachusetts Instituteof Technology (MIT). His research interests are in the areas of Power Microelectromechanical systems(Power MEMS), MEMS acoustic sensors, and microscale cooling systems. His other interests are inmicro/nano fabrication technology, fundamental understanding of micro/nanoscale fluidics and their ap-plications in biological analysis and energy areas.

c©American Society for Engineering Education, 2013

Page 23.80.1

Paper ID #8018

Dr. Carol Forance Barry, University of Massachusetts Lowell

Carol Barry is a Professor of Plastics Engineering at the University of Massachusetts Lowell and an As-sociate Director of the NSF NSEC - the Center for High-rate Nanomanufacturing. Her research interestsinclude extrusion, injection molding, novel processing techniques and analysis, and nano plastics pro-cessing. She received her doctor of engineering degree in plastics engineering from the University ofMassachusetts Lowell and her bachelor of science in chemistry from Boston College.

Prof. Alfred A. Donatelli, University of Massachusetts, LowellJill Hendrickson Lohmeier, University of Massachusetts Lowell

Dr. Lohmeier is an assistant professor in the Graduate School of Education at The University of Mas-sachusetts Lowell. She specializes in educational program evaluation.

c©American Society for Engineering Education, 2013

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A New Interdisciplinary Engineering Course on Nanoscale Transport Phenomena

Abstract A new interdisciplinary engineering course, “Nanoscale Transport Phenomena for Manufacturing Nanodevices”, was recently developed. The course focuses on the principles of nanoscale transport phenomena needed for manufacturing nanodevices and aims to close a large gap between nanoscience and commercial production of nanotechnology products. The course also helps to integrate the interdisciplinary knowledge required for designing and manufacturing nanodevices into undergraduate curricula. To meet these unique needs and challenges, five instructors from three engineering departments (Chemical, Mechanical, and Plastics Engineering) have created this interdisciplinary course. The course was offered for the first time as an elective to seniors during the 2011 fall semester and again in the 2012 fall semester. The course for students in the three engineering departments included lectures, hands-on laboratory exercises, demonstration experiments, and a final design project. In this paper, we discuss the lecture topics and eight hands-on laboratory experiments that were developed into modules to complement lectures in fluid mechanics, heat transfer, mixing, reaction engineering, electroosmosis, electophoresis, and manufacturing methods for micro and nanoscale devices. We also show the final project designs for the nanodevices or nanosystems that were proposed by student teams at the end of the course. Finally, we present the assessment results from the pre-post student surveys as well as faculty interviews. This new interdisciplinary course will better prepare undergraduates for employment focused on designing and manufacturing nano/microfluidic systems, lab-on-a-chip devices, electronic devices, medical devices, and other micro and nano scale emerging technologies. The impact of this senior-level course will significantly enhance the “Nanomaterials Engineering Option” in the Chemical Engineering Department undergraduate curriculum as well as the medical device industry focus in the Plastics Engineering Department. It also can be used in the popular accelerated BS-MS program in the College of Engineering. The course will be available to the chemical, mechanical, and plastics engineering seniors each year. The lab modules can be exported to freshman introductory engineering courses in the College of Engineering. In addition, the microscale fluid mechanics and heat transfer experiments may be incorporated into the undergraduate chemical engineering Unit Operations Laboratory courses.   1. Introduction Transport phenomena, including fluid mechanics, heat transfer and mass transfer, are important fundamental subjects in fields, such as Chemical and Mechanical Engineering. This type of knowledge also is important in Electrical Engineering (electronics cooling), Civil and Environmental Engineering (fluid flow), and Materials Engineering. These subjects are often taught at the junior or senior levels, and most courses are focused on macroscale behavior. Few courses have been developed for the micro and scale region1, which are important for microelectronic and microfluidic devices, and micro-reactor design.

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In the last two decades, with the emerging and significant developments in nanotechnology, there is a need to develop courses that focus on nanoscale transport phenomena. The final commercialization of many nanotechnology-based products will require the incorporation of nanoscience discoveries into macro, micro, and nanoscale designs and manufacturing methods. From an educational point of view, interdisciplinary courses such as ours can help educate and train students in the fundamental areas of nanoscience which will be useful for the commercial production of nanotechnology products. Even though there have been many courses related to nanoscience, there has been little development in nanomanufacturing education. Currently, the integration of the interdisciplinary knowledge required for designing and manufacturing nanodevices into undergraduate curricula still remains a big challenge. To address this educational challenge and generate practical ways of introducing nanotechnology into undergraduate education with a focus on manufacturing nanodevices, five faculty from three engineering departments (Chemical, Mechanical and Plastics Engineering) have created an interdisciplinary course, “Nanoscale Transport Phenomena for Manufacturing Nanodevices,” covering the principles of nanoscale transport phenomena needed for the manufacturing of nanodevices (Figure 1).The purpose of this course is to design and fabricate microfluidic devices for nanomanufacturing education, which can provide undergraduate students in the College of Engineering a better understanding of the transport phenomena at the micro- and nanoscale. Lecture and laboratory modules have been developed for students in the three departments in the College of Engineering. The modules focused on the design and fabrication of micro and nanofluidic devices as well as the transport phenomena on the micro and nanoscale. 

Figure 1. Interdisciplinary approach for the new interdisciplinary course in nanoscale transport phenomena.

Interdisciplinary courseNanoscale Transport

Phenomena for manufacturing nanodevices

Focus: fluids, reactorsFocus: solid mechanics, machining

Focus: polymers, design

Chemical Eng.•Fluids Mechanics•Heat Transfer•Reaction Engineering

Mechanical Eng.•Conduction & Radiation

Heat Transfer • Fluids Mechanics•Thermo-Fluid Processes

Plastics Eng.•Fluids Flow•Heat Transfer

Nano/Micro Fluidic Systems

Lab-on-a-chip DevicesNano-sensors

Bio SensorsNanoelectronic

Devices

Biomedical Devices

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2. Course Content For the course “Nanoscale Transport Phenomena for Manufacturing Nanodevices”, the five instructors selected topics that were useful to students in all three engineering disciplines. As shown in Table 1, these topics were (1) a review of macroscale fluid mechanics and heat transfer as well as an introduction to microscale fluid mechanics and heat transfer; (2) micro and nanoscale heat transfer; (3) electrically-driven micro flows; (4) microscale reactions and mixing; and (5) manufacturing methods for micro and nanoscale devices. Each of these topics was addressed in four 50-minute-long lectures and two laboratory experiments (modules). The sixth “module” was a team project which utilized the content of the five lectures to design and propose a manufacturing method for a micro or nanodevice.

Table 1.Lecture Topics and Laboratory Modules for “Nanoscale Transport Phenomena for Manufacturing Nanodevices”

Module Lecture Topics Laboratory Modules

1-1 Review of Fluids Mechanics I: Flow in Microchannels

1-2 Review of Heat Transfer II: Enhanced Heat Transfer with Microchannel Cooling 2 Enhanced Heat Transfer

III: Nanofluids: a New Coolant

3 Electrodynamics, Electroosmosis,

Electrophoresis, and Dielectrophoresis

IV: Effect of Ionic Strength on Electro-osmotic Flow

V: Dielectrophoresis of Polystyrene Particles

4 Microscale Reaction Engineering and Microscale

Mixing

VI: Reactions in Microchannels – Nanoparticle Synthesis

VII: Microfluidic Mixing

5 Manufacturing of Micro and Nanodevices

VIII: Comparison of Manufacturing Methods for Microfluidic Devices

IX: Laminated Microfluidic Devices X: Bonding of Microfluidic Devices

“6” Team Project --- Module 1-1: Review of Fluid Mechanics The lecture portion of the fluid mechanics module reviewed selected concepts in macroscale fluid mechanics and briefly introduced differences that occur in microscale fluids mechanics. Concepts reviewed were the solution of the continuity and Navier-Stokes equations for laminar flow in conduits; and the use of the steady-state mechanical energy balance for performing hydraulic circuit analyses for series and parallel conduit arrangements. For microscale fluid mechanics, the lecture focused on four factors:

• Microscale flows are typically laminar due to the small length scales,

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Page 23.80.6

Students were asked to use the experimental data to: • Evaluate of the hydrodynamic entrance length to determine if it is significant, • Evaluate the hydraulic resistance of the microchannel, • Use the hydraulic resistance method to predict the flow rates for the various pressure

drops and compare these data with the experimental results, • Use the mechanical energy balance and the Fanning friction factor for the appropriate

aspect ratio to predict the pressure drop at the various flow rates, and then, compare with experimental results.

• Use the Fanning friction factor equation and the experimental pressure drop and flow rate data to determine f, and

• Compare the experimental value of fReDh with the theoretical value. Non-rigid (PDMS) microchannels were used to add another degree of complexity to the analysis. Typical results for the Fanning friction factor in the microchannel as presented in Figure 2b. Module 1-2: Review of Heat Transfer The lecture portion of the heat transfer module reviewed selected concepts in heat transfer and compared macro and micro heat transfer. As with the fluid mechanics module, this lecture was designed to provide a common background for students from the three engineering disciplines as well as support new materials introduced in other modules. The topics reviewed were forced convection in conduits for constant surface temperature and constant surface energy flux cases, and forced convection heat transfer with finned surfaces. The new concepts introduced for micro heat transfer were:

• Macroscale results should be used with caution for liquids when the hydraulic diameter, Dh, ≤ 10 µm,

• Macroscale results are not expected to apply for gases when Dh/λmfp ≤ 100 µm, and • As Dh → 0.1 µm = 100 nm, molecular interactions must be accounted for in the fluid and

in the solid wall. Laboratory Module II: Enhanced Heat Transfer with Microchannel Cooling was an examination of the heat transfer characteristics of water flowing through a microchannel device. The students investigated the cooling of a device with several hundred microchannels (which simulated the heat transfer process for cooling an electronics device) and compared the experimental results with predictions from the macro theory equations. The microchannel cooling device used for this work consisted of a silicon chamber with a microchannel array which was fabricated on a silicon substrate using lithography and microfabrication techniques. The microchannel array contained 300 rectangular channels which were 50 μm wide, 150 μm deep, and about 25 mm long. The chamber was heated by a copper block heater to provide a constant heat flux boundary condition; (i.e., an electrical heating strip was attached to one surface of the device and the other surfaces were assumed to be well insulated).The surface temperature of the device on the heater side was measured by a thermocouple. Deionized water was used as the working fluid. The temperatures of the water at the inlet and outlets of the microchannel cooling chamber were measured by thermocouples, and the water feed flow rate was determined by a flow transmitter. The experimental set up is shown in Figure 3a.

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Each laboratory group investigated the heat transfer performance of the device over a range of flow rates (typically, 20 to 60 ml/min.) at a specified heating rate. i.e., a different power input from the electrical strip heater (e.g., 20-100 W). The product of the mass flow rate, specific heat capacity, and temperature difference (between inlet and exit) were used to determine the heat transfer rate over the bottom of the microchannel chip Students performed a fin-based analytical analysis for determining the heat transfer coefficient for microchannel; then the correlations among Re, Nu and characteristic diameter of channel were developed. The students were asked to report an:

• Evaluation of the hydraulic and thermal entrance lengths to determine if they are significant and whether a fully developed flow assumption valid;

• Evaluation of adiabatic operation - i.e., determining the actual heat transfer rate to the water at the various flow rates and comparing it to the heating rate from the strip heater;

• Evaluation of the average convection heat transfer coefficient at each flow rate; • Development of a Nusselt number expression for the heat transfer process - i.e., whether

the Nusselt number was a constant and, if not, whether a Nusselt number equation of the form Nu = CReaPrb (with b = 1/3) was more appropriate; and

• Evaluation of the significance of any assumptions and uncertainty in the experimental technique and measurements and the impact on the results.

A compilation of results for heat transfer through the microchannel cooling device is presented in Figure 3b.

(a) (b)

Figure 3. (a) Experimental setup for enhanced heat transfer in electronic cooling and (b) results for heat transfer in the microchannel cooling device. Module 2: Enhanced Heat Transfer This lecture portion of this module focused on heat transfer improved enabled by micro and nanotechnologies. They built on Module 1's introduction of fluid mechanics and heat transfer. The lectures highlighted two topics: (1) micro/nanotechnologies in engineering system cooling

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Page 23.80.8

and (2) nanofluids. The first lecture provided an overview of micro/nanotechnologies in engineering system cooling applications as well as presenting:

• Pressure drops and heat transfer coefficients for single phase flow in microchannels; • The effects of surface roughness on the friction factor and heat transfer coefficient; and • Analyses of micro/nano pin fin coolers/heat exchangers

The topics for the “Nanofluids” lecture included an introduction; fabrication of nanofluids; mechanisms of thermal conductivity enhancement in nanofluids; thermal conductivity measurement techniques for nanofluids; and future research directions for nanofluids. Laboratory Module II: Enhanced Heat Transfer with Microchannel Cooling provided a bridge between Modules 1 and 2 by illustrating enhancement of convection and conduction heat transfer in microchannels as well as with micro pin fin coolers. Laboratory Module III: Nanofluids - a New Coolant introduced nanofluids which are colloidal suspensions of nanoparticles in low viscosity fluids. They exhibit great potential for significantly improving thermal transport of liquids, especially coolant whose poor thermal conductivity has led to bulky and less efficient heat transport systems2-5. In this experiment, the students investigated the thermal conductivity of nanofluids. The nanofluid created for this experiment was aluminum oxide (Al2O3) nanoparticles with a nominal diameter of 40 nm dispersed in deionized water; nanoparticle concentrations were 1%, 2%, 3%, and 5%. As shown in Figure 4a, these nanoparticles existed as primary particles, rather than large aggregates and agglomerates. The thermal conductivity of these nanofluids was measured using a transient hotwire system which included a Wheatstone bridge, test cell with a platinum wire, and data acquisition system3 (Figure 4b). Students measured the thermal conductivity of Al2O3 nanofluids as well as the neat deionized water baseline. After students plotted the measured thermal conductivity enhancement as a function of the nanoparticle concentration, they performed an analysis to evaluate the mechanism of thermal conductivity enhancement.

(a) (b)

Figure 4. (a) TEM images of Al2O3nanoparticles and (b) schematic of the transient hot wire system used for measuring the thermal conductivity of the nanofluids.

Page 23.80.9

Module 3: Electrodynamics, Electroosmosis, Electrophoresis, and Dielectrophoresis This module consisted of four lectures which introduced new concepts to the students. The first lecture, “Basics of Electrostatics”, provided a foundation for subsequent lectures. It focused on the origin of electrostatic forces, surface charge, and repulsive forces; counter ion density on the surface and the midplane between two parallel plates; electrostatic forces in the presence of electrolytes; the Grahme equation; and the importance of, expressions, and examples of the Debye length. The topic of the second lecture, “Electrophoresis and Electroosmosis”, was “why do charged particles move in an electric field?”. Concepts introduced were particle mobility; the zeta potential; the streaming potential; liquid mobility in a capillary; solution of the electroosmosis is equation; the Hemoltz-Schmulowski, Henry, and Huckel equations; decoupling electrophoretic mobility and hydrodynamic fluxes; and the principle of electroosmotic microfluidic pumping. “Lecture 3: Dielectrophoresis” expanded this focus with particle assembly and crystallization under AC electric fields, the advantages of AC over DC electric fields, the Clausius-Mossotti equation for dielectrophoretic force, and particle chaining force. Finally, the fourth lecture, “Electrokinetics in Microfluidics”, provided a comparison of electroosmotic microfluidic pumping with pumping and valving by MEMS and pumping by passive valves. It also included on-chip function of electrophoretic separations in microchannels. Laboratory Module IV: Effect of Ionic Strength on Electroosmotic Flow was a simple exploration electroosmosis. The goal of this experiment was to "relate the electroosmotic mobility of a solid-liquid interface to the electrical potential at the wall" i.e., the surface potential.6 This approach assumes that the double layer is a boundary layer and is thin compared the dimensions of the flow channels. Electroosmotic flow (EOF) or electroosmosis is the flow a flow due to an applied electrical field. Type of flow can occur in capillary tubes, microfluidic channels, and porous materials. The electroosmotic velocity, however, does not depend on channel size when the the double layer is much smaller than the critical channel dimensions. In this experiment, the students measured the electro-osmotic flow rate in microchannels filled with two solutions of different ionic strengths. The rectangular microchannels were 1000 μm wide, 80 μm deep, and 10.2 mm long; they were manufactured from polydimethylsiloxane (PDMS). An indicator dye (red or blue food dye) was used to demonstrate the visible phenomenon. Students graphically obtained the flow rates in the microchannel and corresponding voltages; evaluated the effect of the voltage on EOF; discussed causes of failures in this processes; and reported possible applications for electroosmosis. A typical result is illustrated in Figure 5a.

Page 23.80.10

Figure 5. Cartoon of electrical double layer and electroosmotic flow. A negatively-charged wall in this figure coincides with a thin, positively charged electrical double layer. Coulomb forces in the electrical double layer induce a fluid flow that is approximately uniform outside the electrical double layer. The (typically nanoscale) thickness of the electrical double layer is exaggerated for the purposes of the figure. The difference between the local electrical potential and that of the bulk fluid is denoted by φ—this value is zero far from the wall but is finite near the wall.

Although this approach provided no information about the size of the electrical double layer, its physical underpinnings, or its structure, these experiments did require that the assumption that the double layer is a boundary layer, i.e., it is relatively thin as compared to the flow field dimensions. Despite these omissions, however, the 1D analysis leads to several important conclusions about purely electroosmotically driven flows: (1) the velocity field near the wall is proportional to the voltage difference between that point and the wall; (2) the velocity at the edge of the boundary layer is proportional to the local electric field and the voltage difference between the bulk fluid and the wall; and (3) if the fluid conductivity and electroosmotic mobility are uniform, the velocity at any point far from the wall is proportional to the local electric field, and thus the velocity field far from the wall is irrotational. Electro-osmotic flow (EOF) synonymous with electro osmosis is the motion of liquid induced by an applied potential across a porous material, capillary tube micro channel, or any other fluid conduit. Because electro-osmotic velocities are independent of conduit size as long as the double layer is much smaller than the characteristic length scale of the scale of the channel, electro-osmosis is most significant in microchannels. In this experiment, the students measured the electro-osmotic flow rate in microchannels filled with two solutions of different ionic strengths. The rectangular microchannels were 1000 μm wide, 80 μm deep, and 10.2 mm long; they were manufactured from polydimethylsiloxane (PDMS). An indicator dye (red or blue food dye) was used to demonstrate the visible phenomenon. Students graphically obtained the flow rates in the microchannel and corresponding voltages; evaluated the effect of the voltage on EOF; discussed causes of failures in this processes; and reported possible applications for electroosmosis. A typical result is illustrated in Figure 6a.

Page 23.80.11

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• Determine the electrophoretic mobility of the particles in the two different solutions; • Fit the data to a plot comparing mobility in water to 0.1M NaCl; • Calculate the Debye length; • Discuss common defects - e.g., corrosion and delimitation; and • Provide applications for electrophoresis

Module 4: Microscale Reaction Engineering and Microscale Mixing Module 4 covered two topics: (1) microscale reaction engineering and (2) microscale mixing. The first topic focused on microreactors and their advantages; microreactor fabrication and design; flow and reaction control; chemical reactions in microreactors; catalytic reaction in microreactors; nanoparticle synthesis in microfluidic devices; and from microfluidic applications to nanofluidic phenomena. Concepts taught in the second part of the lecture included diffusion and mass transfer along with Fick’s laws of diffusion and diffusion coefficients; reactors and mixing; plug flow reactors (PFR); microreactors; passive and active micro-mixers; applications of micro-mixers; and fabrication and design of micro-mixers. Laboratory Module VI: Reactions in Microchannels – Nanoparticle Synthesis employed microchannels for the synthesis of gold nanoparticles. Using microfluidic device to synthesize nanoparticles is a promising technique to prepare nanomaterials.7 Therefore, this experiment introduced the students to an emerging technique. Gold nanoparticles, which are nontoxic and biocompatible, have received much attention in a variety of applications due to their novel optical and catalytic properties.8 The gold nanoparticles were prepared from hydrogen tetrachloroaureate (III) hydrate (HAuCl4·3H2O) in an aqueous solution9. In this single-step synthesis, poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (PEO-PPO-PEO) block copolymers was used to reduce and stabilize the gold nanoparticles9. The nanoparticle synthesis was inexpensive because it required only water and commercially-available polymers (e.g., Pluronics or Poloxamers). The reaction also was relatively rapid and the gold nanoparticle dispersions are stable for a long time, i.e., up to several years. In this experiment, the students prepared aqueous solutions of 10 mM/L HAuCl4 and10 mM/L PEO-PPO-PEO block copolymer (Pluronic P105: MW = 6500, 50% PEO). As shown in Figure 7, the solutions were used for reactions at five different flow rate settings. Reactions were carried out in a PDMS microreactor (Figure 7). Using a microscope, the students observed the mixing of the two solutions in this microfluidic channel. A color change of the reacting solution in the microchannel indicated gold nanoparticle formation; the stabilized gold nanoparticles appear pink when it is formed. With different flow rates, the students observed the color change at different positions in the channel. Using the microscope’s camera, they collected images of these color changes; they also analyzed the images to determine how the microchannel influenced the reaction progress. The reacted product was collected from the microreactor’s outlet and the product (gold nanoparticles) was analyzed under the microscope. It was found that microscale mixing is critical in facilitating the synthesis of nanoparticles in the microchannels.

Page 23.80.13

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Module 5: Manufacturing of Micro and Nanodevices The four lectures of the manufacturing methods module provided an overview of methods used to fabricate microfluidic and nanofluidic devices as well as an introduction to methods employed in assembling these devices. Table 2presents an outline of the lecture topics. These lectures were designed to familiarize the students with manufacturing processes to which they had not previously been exposed. The modules also included three manufacturing experiments.

Table 2. Outline of Manufacturing Methods Lectures

Lecture Focus Topics 1 Forming Technologies Issues with manufacturing micro and nanodevices

Casting Hot embossing Nanoimprint lithography Injection molding and injection compression molding

2 Machining Technologies CNC machining (baseline) Micromachining Micro wire EDM Excimer laser machining Laser machining Focus ion beam (FIB) machining

3 Lithographic Processes Overview of CMOS process Photoresists Lithographic techniques Etching Examples

4 Other Mfg Approaches Assembly of Devices

Lamination processes Stereolithography processes Thermal processes Solvent welding Adhesive bonding Surface treatment bonding

Laboratory Module VIII: Comparison of Manufacturing Methods for Microfluidic Devices exposed the students to four manufacturing methods. In fall 2012, these processes were

• Casting of polydimethylsiloxane (PDMS) • Nanoimprint lithography • Injection molding • Lithography

The processes were selected on the basis of equipment availability. In 2011, these processes had been nanoimprint lithography, injection molding, lithography, focused ion beam machining, and dip pen nanolithography (DPN). For each manufacturing process, the students examined the equipment and materials needed for fabricating a microfluidic or nanofluidic device; manufactured one or more devices; record critical processing conditions and the cycle time (i.e.,

Page 23.80.15

time to make one complete device); and noted any defects visible in the device. After the laboratory session, the students measured the replication of the micro/nanoscale features with a profilometer and scanning electron microscope (SEM). Figure 9shows devices fabricated during the experiment. The students were then asked to (1) compare the processes for manufacturing microfluidic devices, and (2) evaluate and compare the replication quality of selected manufacturing processes.

(a) (b)

Figure 9.Students fabricated (a) a micro-reactor using lithography and (b) 110-μm wide channels using injection molding.

Laboratory Module IX: Laminated Microfluidic Devices was introduced in fall 2012. The objectives were to (1) design and create a “microfluidic device” using a lamination process and to evaluate the layer bonding and design of the device using a leak test. The students designed the 10 or more layers of the device on graph paper. The device was then fabricated from layers of polymeric sheet with a pressure sensitive adhesive; the students cut this material with scissors and exacto knives. After tubing was connected to the devices, leak testing was performed with colored water. Laboratory Module X: Bonding of Microfluidic Devices explored bonding of microfluidic devices (which are often fabricated as two planar sheets with micro or nanochannels in the surface of one sheet. The objectives of this experiment were to (1) bond one or more microfluidic devices and (2) evaluate the bonding of the device using a leak test. Methods used included thermal and adhesive bonding of polymethylmethacrylate (PMMA), polycarbonate (PC), and PDMS devices. The PDMS was bonded to glass. Leak testing was performed with colored water. Module 6: Team Projects During the course, students formed small groups (up to three students per group) to design a micro or nanodevice. Each group was required to incorporate two or more of the topics learned during the course into the design project. Some example projects included “A Microfluidic-based Sensor for Heavy Metal Detection” and “Enhanced Heat Transfer with Nanofluids for Electronics Cooling.”

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3. Implementation of the Course “Nanoscale Transport Phenomena for Manufacturing Nanodevices” was an interdisciplinary course involving faculty and students from three departments: Chemical Engineering, Mechanical Engineering, and Plastics Engineering (a unique program at our institution). This situation produced issues with scheduling, recruiting of students, course structure, team projects, teaching assistants, and faculty workload. Scheduling of the Course. The course was offered as senior elective in fall 2011 and fall 2012. The prerequisites were the fluid mechanics and heat transfer courses required of students in the three target departments. Chemical Engineering majors were expected to be taking the Chemical Reaction Engineering course simultaneously, whereas the Mechanical Engineering and Plastics Engineering majors would have completed lower level design courses (specifically, course teaching basic design and solid modeling). The course was scheduled into time slots not already occupied by required senior courses in three departments. This scheduling was facilitated by Instructor 2 who is the Chair of the Chemical Engineering Department. This scheduling system produced two 50-minute lectures and one 270-minute laboratory each week. Recruiting of Students: The target class size was 15-20 students with the actual 2011 and 2012 enrollments averaging 15 students per year. The course fit well as elective for Chemical Engineering majors in the Nanotechnology option. As a result, most of the students were from this track. Recruiting efforts directed toward Mechanical and Plastics Engineering majors were less successful. The course fits as design elective in both disciplines, but seemed to conflict with capstone design courses and industrial cooperative learning opportunities. Course Structure. The five instructors agreed that the course would include lectures, hands-on laboratory experiments, and a final design project. As shown in Table 3, the course modules were delivered in two-week blocks with the lecture and laboratory modules scheduled in the same periods. Instructor 1 provided an introduction to the course during the class and tracked the students during the team design projects. Grading for course was based primarily on the laboratory reports and team project; a few instructors did assign homework, which was included in the grading. Attendance was taken for all lectures and laboratories.

Table 3. Basic Course Structure for First Offering (Fall 2011)

Week Instructor Lecture Module Laboratory

1 1 Course introduction, design concept, laboratory group formation

Overview

2 2 1-1: Fluids Mechanics I

3 1-2: Heat Transfer II

4 3 2: Enhanced Heat Transfer

5 III

6 4 3: Electrodynamics, Electroosmosis, etc. IV

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7 V

8 1 4-1: Microscale Reaction Engineering VI

9 4-2: Microscale-Mixing VII

10-11 5 5: Manufacturing of Devices VIII (two weeks)

12-15 1 + Team Project --- Laboratory modules I to VII were offered to all students during a given week. Some changes in group scheduling were accommodated issues with equipment and time needed for an experiment. For example, with the nanoparticle synthesis, the students did not collect data for all five flow rates, but data traded between laboratory groups enabled the students to analyze data for all five flow rates. With the manufacturing laboratory module (VIII), the teams were rotated between fabrication processes over a two-week period. This system has long been used by the Plastics Engineering Department to produce better learning and provide good safety around manufacturing equipment. Table 4 presented the course structure for the second course offering in fall 2012. The major changes were moving the manufacturing module to the beginning of the course; the addition of new manufacturing laboratory modules (IX and X); and a new structure for the team project (discussed later). Moving the manufacturing module to the beginning of the course was a result of feedback from fall 2011 evaluations. Since the students were introduced to the manufacturing processes while they were beginning to think about possible projects, they had a better idea about the limitations or possibilities of the device fabrication. The new experiments also enhanced their knowledge of the manufacturing processes.

Table 4. Basic Course Structure for Second Offering (Fall 2012)

Week Instructor Lecture Module Laboratory

1 1 Course introduction, design concept, laboratory group formation

Overview

2 5 5: Manufacturing of Devices VIII and IX

3 X

4 2 1-1: Fluids Mechanics I

5 1-2: Heat Transfer II

6 3 2: Enhanced Heat Transfer

7 III

8 4 3: Electrodynamics, Electroosmosis, etc. IV

9 V

10 1 4-1: Microscale Reaction Engineering VI

11 4-2: Microscale-Mixing VII

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12-15 1 + Team Project --- Team Projects. Table 5 presents the team project schedules for fall 2011 and fall 2012. Changes in the schedule were due to feedback from the fall 2011 offering.

Table 5. Schedules for Team Projects

Fall 2011 Fall 2012

November 29 Group Clean Up October 1 Group Formation

November 28 Project Abstract and Introduction

October 22 Project Abstract

December 5 Project Update I November 19 Project Update I

December 12 Project Update II December 3 Project Update II

December 20 Final Presentation December 18 Final Presentation In fall 2012, group formation (i.e., providing the names of the team members and a possible topic) was much earlier. This change provided more time for team thinking and prevented the one-member teams from fall 2011. The project abstract, which was a one page outline of the project along with an illustrative concept, was also moved to an earlier date. All instructors provided feedback on these abstracts in both years, but the schedule was less compressed in fall 2012. The project updates were 8-10 minute presentations with a written progress report. Students were encouraged to include CAD drawings of their devices; (this requirement was stressed because the Chemical Engineering majors had limited formal CAD training). Again, the schedule for the progress reports was less compressed in fall 2012. The final project presentation was a 15-minute group presentation which required a final report, and in fall 2012, a prototype device for display or demonstration. Teaching Assistants. The course had three assigned teaching assistants who were responsible for specific laboratory modules. Laboratory Modules VIII and IX required additional teaching assistants (who were Instructor 5’s research assistants). In fall 2011 and fall 2012, the teaching assistants were funded through the National Science Foundation’s NUE program (Award #: 1042119). This award also supported graduate students to improve laboratory modules in spring and summer 2012. The instructors are currently negotiating with the Administration for teaching assistants to support the fall 2013 offering of the course. The fall 2011 teaching assistants included two senior doctoral students and one master student. The former were very effective, but the latter was not (due to overall skill levels). The fall 2012 teaching assistants included one of the previous doctoral students, a new doctoral student, and a master student who took the course in fall 2011. Faculty Workload. The five instructors for this course were two Professors - one of whom is a Department Chair, one Associate Professor, and two Assistant Professors. Both Assistant Professors have been tenured during 2011-2013. As shown in Table 6, the overall workload for these faculty varied depending on their other activities. The course had three course numbers

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and three instructors (1, 3 and 4) - i.e., one for each Department. Only Instructor 1, however, received credit for this course. At the University, the workload credit for multi-instructor courses varies significantly. For example, Instructor 4 receives full credit for her one-third of a polymer synthesis laboratory, but no real credit for teaching “Nanoscale Transport Phenomena for Manufacturing Nanodevices”. This issue of uniform workload credit for multi-instructor courses is currently being discussed by the faculty union.

Table 6. Faculty Workload

Instructor Rank Courses Taught in Fall 2011 2011-2012 Fall 2012 2012-2013

1 Assistant Professor

1 + course 4 1 + course 4

2 Professor 1* 2* 1* 2* 3 Associate

Professor 2* 5* 1* 1*

(sabbatical) 4 Assistant

Professor 1.3* 3.3* 1.3* 3.3*

5 Professor 2* 3* 2* 3*

* Does not include “Nanoscale Transport Phenomena for Manufacturing Nanodevices” 4. Assessment of the Course Pre-post student surveys, faculty/instructor interviews, and feedback from Student Advisory Boards (in Chemical Engineering) were used to assess the effectiveness of the course. The program evaluation was completed based on an objectives based evaluation model10 as well as the first two levels of Kirkpatrick’s11 Four Level Model of training evaluation. The student surveys and faculty interviews were conducted by a faculty member in the Graduate School of Education. Her primary research interests lie in the area of evaluation and research of educational programs, particularly (1) how collaboration changes during and contributes to the effectiveness of educational programs and (2) utilizing our understanding of cognitive processing in problem solving and decision making within the evaluation process. The fall 2011 pre- and post-surveys contained 11 statements (Q1-Q11).

1. I know the difference between macroscale fluid flow behavior and microscale fluid flow behavior

2. I know the difference between macroscopic forced convection heat transfer and microscale forced convection heat transfer

3. I know the concept of micro pin fin cooler for enhanced heat transfer 4. I know the concept of “nanofluids” and how they can enhance heat transfer 5. I know what the electrodynamics and electroosmosis are and their difference 6. I know what electrophoresis and dielectrophoresis are and their difference 7. I know microscale reaction engineering and their advantage over macroscale reaction

engineering 8. I can differentiate between hot embossing, micromolding, and nanoimprint lithography 9. I understand how lithographic processes are used to create nano and microfluidic devices.

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10. I know how nanotechnology is used in multiple engineering fields. 11. I understand how I might use nanotechnology in a future job.

The students ranked their understanding of 11 questions on a scale of 1 to 4, where the rankings were 1: Not at all; 2: Not very well; 3: Somewhat; and 4: Very well. The survey results for the first offering (fall 2011) are shown in Figure 10.

Figure 10. Results of pre-test and post-test surveys for the first offering (fall 2011).

When starting the course, the students had some understanding of flow and heat transfer (Q1-Q3) as well as the impact of nanotechnology on their possible futures (Q10-Q11); less understanding of nanofluids (Q4) and reaction engineering (Q7); and little understanding of electric-based operations (Q5-Q6) and manufacturing (Q8-Q9). The course provided significant increases in their understanding of all concepts, but they still exhibited limited understanding of the electric-based operations (Q5-Q6) and manufacturing (Q8-Q9). The fall 2012 pre- and post-surveys contained 21 statements (Q1-Q21).

1. I know the difference between macroscale fluid flow behavior and microscale fluid flow behavior.

2. I know the difference between macroscopic forced convection heat transfer and microscale forced convection heat transfer.

3. I know the concept of micro pin fin cooler for enhanced heat transfer. 4. I know what the concept of “nanofluids” is. 5. I know how nanofluids can enhance heat transfer. 6. I know what electrodynamics are. 7. I know what electroosmosis is. 8. I know what the difference between electrodynamics and electroosmosis is. 9. I know how electrolysis works. 10. I know what electrophoresis is. 11. I know what dielectrophoresis is.

0

1

2

3

4

Q1 Q2 Q3 Q4 Q5 Q6 Q7 Q8 Q9 Q10 Q11

Ran

king

Pre-test 1 Post-test 1

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12. I know what the difference between electrophoresis and dielectrophoresis is. 13. I understand microscale reaction engineering. 14. I understand the advantages of microscale reaction engineering over macroscale

reaction engineering. 15. I understand the differences between major forming methods -(casting, hot

embossing, micromolding, and nanoimprint lithograph) used to create devices. 16. I understand how lithographic processes are used to create nano devices. 17. I understand how lithographic processes are used to create microfluidic devices. 18. I understand new machining techniques used to create devices. 19. I understand the assembly process for micro and nanodevices 20. I know how nanotechnology is used in multiple engineering fields. 21. I understand how I might use nanotechnology in a future job.

As with the previous surveys, the students ranked their understanding of the 21 questions on a scale of 1 to 4, where the rankings were 1: Not at all; 2: Not very well; 3: Somewhat; and 4: Very well. Figure 11 presents the survey results for the second offering (fall 2012). The addition of details questions in problem areas provided a better understanding of what the students did and did not know at the start of the course. This break down was particularly helpful for the electric-based operations (Q6-Q12). The resultant focus on problem topics and concepts - as well as improved lectures and laboratory modules - produced a significant improvement in learning compared to fall 2011. For almost all questions, the rankings were 3 or greater, indicating that the students had acquired some knowledge to a solid understanding of all concepts presented in the course.

Figure 11. Partial results of pre-test and post-test surveys for the second offering (fall 2012).

Some key findings from the first year faculty interviews were:

0

1

2

3

4

Ran

king

Pre-test 2 Post-test 2

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• Faculty reported learning both content and teaching methods from their colleagues. • All faculty reported being happy with the split of teaching responsibilities. • The primary faculty concerns included the need for more laboratory set-ups, increased

communication among faculty about the course, better teaching assistant training, faculty credit for the course, and the need to plan earlier. Several of these concerns were also noted by the students.

Course Improvements (from fall 2011 to fall 2012). For fall 2012, the selection and training of teaching assistants was improved. More experimental set-ups were produced (using $10,000 of University funds). Moreover, the laboratory modules were overhauled during spring and summer 2012. These changes produced significant improvements in the fall 2012 laboratories. General feedback from the students and faculty showed that the Chemical Engineering students had little background in manufacturing; (this was not as clear in the fall 2011 pre-surveys). So, the manufacturing lectures were revised to accommodate this issue. In addition, the revised laboratory experiments in this area focused on (1) comparing the casting, nanoimprint lithography, injection molding, and lithography processes with respect to replication of features, i.e., compared to tooling or mask dimensions; (2) ‘designing’ and fabricating a device using an additive manufacturing method; and (3) joining polymer devices. (There was less focus on processing conditions than in fall 2011.) As was discussed earlier, the manufacturing module was moved to the beginning of the course. The faculty believed that this change would help the student better understand the methods and techniques that are used for making microfluidic devices and the nanofeatures that are used in the laboratory modules. Formal evaluation of this change is not completed, but the students worked very hard on 'designing' and fabricating a device using the additive manufacturing method. The student design projects were started earlier when the course was offered for the second time. Last year, the student design projects were initiated midway through the course, while this year the design projects were begun at the beginning of the course. This earlier start helped the students initiate the project and spend more time on their projects. Many student groups also had the time to synthesize, design, and revise their micro or nanodevice. 5. Conclusions A new undergraduate course on nanoscale transport phenomena has been developed and taught by five faculty members in three different engineering departments. Ten laboratory modules have been developed to accompany the lectures on microscale fluid mechanics, heat transfer, electrically-driven flows, reactions, and mixing as well as the manufacturing of microdevices. Evaluation of the course and laboratory modules showed increased learning in the course topics. The course is currently being transitioned from grant funding to the regular University teaching system. It may be extended to be a senior and graduate course. Moreover, the modules are being used elsewhere. For example, in spring 2012, the “Microscale Mixing” laboratory module was used in the freshmen-level “Introduction to Engineering II” course for the Chemical

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Engineering program. This lab module provided a good illustration of chemical engineering principles, while exciting the freshman students with emerging technologies like nanotechnology and microfluidic devices. Bibliography 1. Z. M. Zhang (2007), Nano/Microscale Heat Transfer (McGraw-Hill Nanoscience and Technology), McGraw

Hill Professional. 2. S. K. Das, S. U. Choi, W. Yu and T. Pradeep (2007), Nanofluids: Science and Technology, Wiley-Interscience. 3. R. Gowda, H. Sun, P. Wang, M. Charmchi, F. Gao, Z. Gu, B. Budhlall, “Effects of Particle Surface Charge,

Species, Concentration, and Dispersion Methods on the Thermal Conductivity of Nanofluids”, Advances in Mechanical Engineering, 2010, ID: 807610.

4. X. Wang, X. Xu, S. Choi, “Thermal Conductivity of Nanoparticle-Fluid Mixture”, J. Thermophys. & Heat Transfer 1999, 13, 474-480.

5. S. Lee, S. Choi, S. Li, J. Eastman, “Measuring Thermal Conductivity of Fluids Containing Oxide Nanoparticles”, J. Heat Transfer 1999, 121, 280-289.

6. H. A. Pohl (1978), Dielectrophoresis: The Behavior of Neutral Matter in Nonuniform Electric Fields, Cambridge University Press.

7. Challa S. S. R. Kumar (2010), Microfluidic Devices in Nanotechnology: Applications, Wiley. 8. P. Alexandridis. “Gold Nanoparticle Synthesis, Morphology Control, and Stabilization Facilitated by

Functional Polymers”, Chem. Eng. Technol. 2011, 34, 15–28. 9. T. Sakai, P. Alexandridis, “Single-step Synthesis and Stabilization of Metal Nanoparticles in Aqueous Pluronic

Block Copolymer Solutions at Ambient Temperature”, Langmuir 2004, 20, 8426-8430. 10. D. L. Stufflebeam (2001). Evaluation Models: New Directions for Evaluation, no. 89. San Francisco, CA:

Jossey-Bass. 11. D. Kirkpatrick (1994). Evaluating Training Programs: The Four Levels. San Francisco: Berrett-Koehler.

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