Non-conventional solutions to physical and engineering problems facing microfluidics

Microfluidics is a vital tool for scientific research utilising micrometre scale features to provide unparalleled control of micro-, nano- and pico-litres of fluid. Planar lithographic design and fabrication techniques have become more versatile and refined over time. However, stagnation of novel designs, fabrication methodologies and experimental conditions is increasing due to the current limitations. 3D printing is approaching the resolution required in microfluidics, whilst also providing greater freedom of design, materials, and fabrication techniques. This thesis seeks to overcome the traditional limitations using 3D printing to innovate design and production, enabling rapid prototyping methodologies and truly 3D structures, which are typically expensive and labour intensive. The first system discussed within this work generates cells-laden gelatin microdroplets and featured heating and cooling water channels, with a performance comparative to commercial devices. Secondly, a flow cell for the screening of extracellular lectins via glycomimetic liposomes was produced. Additionally, stereolithographic printing was used to produce a bioinspired monolithic droplet generator which featured intertwined channels. Finally, a Van de Graaff generator-based electrophoresis system was developed in order to generate record breaking separation resolutions whilst extended capillary lifespan compared to other experimental systems.Die Mikrofluidik ist ein wichtiges Werkzeug für die wissenschaftliche Forschung, das Merkmale im Mikrometerbereich nutzt, um eine beispiellose Kontrolle von Mikro-, Nano- und Pikolitern von Flüssigkeiten zu ermöglichen. Planare lithografische Konstruktions- und Herstellungstechniken sind im Laufe der Zeit vielseitiger und verfeinert worden. Aufgrund der derzeitigen Einschränkungen nimmt jedoch die Stagnation neuartiger Designs, Herstellungsmethoden und experimenteller Bedingungen zu. Der 3D-Druck nähert sich der in der Mikrofluidik erforderlichen Auflösung und bietet gleichzeitig eine größere Freiheit bei Design, Materialien und Herstellungstechniken. Diese Dissertation versucht, die traditionellen Einschränkungen bei der Verwendung von 3D-Druck zu überwinden, um Design und Produktion zu erneuern und schnelle Prototyping-Methoden und echte 3D-Strukturen zu ermöglichen, die normalerweise teuer und arbeitsintensiv sind. Das erste in dieser Arbeit diskutierte System erzeugt mit Zellen beladene Gelatine-Mikrotröpfchen und verfügt über Heiz- und Kühlwasserkanäle mit einer Leistung, die mit kommerziellen Geräten vergleichbar ist. Zweitens wurde eine Durchflusszelle für das Screening von extrazellulären Lektinen über glykomimetische Liposomen hergestellt. Darüber hinaus wurde stereolithografischer Druck verwendet, um einen bioinspirierten monolithischen Tröpfchengenerator herzustellen, der ineinander verschlungene Kanäle aufweist. Schließlich wurde ein auf einem Van-de-Graaff-Generator basierendes Elektrophoresesystem entwickelt, um rekordverdächtige Trennauflösungen zu erzeugen und gleichzeitig die Kapillarlebensdauer im Vergleich zu anderen experimentellen Systemen zu verlängern

Bucky gel actuator for morphing applications

Since the demonstration of Bucky Gel Actuator (BGA) in 2005, a great deal of effort has been exerted to develop novel applications for electro-active morphing materials. Three-layered bimorph nanocomposite has become an excellent candidate for morphing applications since it can be easily fabricated, operated in air, and driven with few volts. There has been limited published study on the mechanical properties of BGA. In this study, the effect of three parameters: layer thickness, carbon nanotube type, and weight fraction of components, on the mechanical properties was investigated. Samples were characterized via nano-indentation and DMA. It was found that BGA composed of 22 wt% single-walled carbon nanotubes and 45 wt% ionic liquid exhibited the highest hardness, adhesion, elastic and storage moduli. Most of BGA potential applications would require control over one BGA output: displacement. In this study, various sets of experiments were designed to investigate the effect of several parameters on the maximum lateral displacement of BGA. Two input parameters: voltage and frequency, and three material/design parameters: carbon nanotube type, thickness, and weight fraction of constituents, were selected. A new thickness ratio term was also introduced to study the role of individual layers on BGA displacement. In addition, an important factor in the design of BGA-based devices, lifetime, was investigated. Finally, possible degradation of BGA was studied by repeating displacement measurements after several weeks of being stored. Based on displacement studies, a new model was established utilizing nonlinear regression to predict BGA maximum displacement based on the effect of these parameters. This model was verified by comparing its predictions with other reported results in the literature. The model displayed a very good fit with various reported cases of BGA samples made with different types of CNT and ionic liquid. Microfluidics is a promising field of application for BGA. A brief literature review on the electroactive mechanisms used in microfluidics is presented. Preliminary force studies proved that BGA has the capability to be employed as a microvalve. A flow regulator utilizing a BGA microvalve was designed and fabricated. Flow rate measurements showed the capability of BGA-valve in manipulating the flow rate in different ranges

Micro/Nano-Chip Electrokinetics

Micro/nanofluidic chips have found increasing applications in the analysis of chemical and biological samples over the past two decades. Electrokinetics has become the method of choice in these micro/nano-chips for transporting, manipulating and sensing ions, (bio)molecules, fluids and (bio)particles, etc., due to the high maneuverability, scalability, sensitivity, and integrability. The involved phenomena, which cover electroosmosis, electrophoresis, dielectrophoresis, electrohydrodynamics, electrothermal flow, diffusioosmosis, diffusiophoresis, streaming potential, current, etc., arise from either the inherent or the induced surface charge on the solid-liquid interface under DC and/or AC electric fields. To review the state-of-the-art of micro/nanochip electrokinetics, we welcome, in this Special Issue of Micromachines, all original research or review articles on the fundamentals and applications of the variety of electrokinetic phenomena in both microfluidic and nanofluidic devices

Characterization Of Commercially Available Conductive Filament And Their Application In Sensors And Actuators

The primary aim of this study is to contribute to the field of additives that would enable the fabrication of electrical sensors and actuators completely via Material Extrusion based Additive Manufacturing (MEAM). The second aim of the study is to provide the necessary characterization to facilitate the development of applications that predicts electrical part performance. The electrical characterization of two conductive poly-lactic acid (PLA) filaments, namely, c-PLA with carbon black and graphene PLA was performed to study the temperature coefficient of the resistance. Resistivity of carbon black filament was compared to a printed single layer and with that of a cube. The raw and printed c-PLA showed a positive temperature coefficient of resistance (α) ranging from ~0.03-0.01 ℃-1 while its counterpart in the study, graphene PLA, did not exhibit significant (α). Parts from graphene PLA with multilayer MEAM exhibited a negative α to a certain temperature before exhibiting positive α. The resistivity of the printed parts was 300 times higher for c-PLA and 1500 times for graphene PLA. However, no microstructural or chemical compositional changes were observed between the raw filaments and the printed parts. Due to the high α of the c-PLA, it was deemed as the better material for constructing electro thermal sensors and actuators using MEAM. First, c-PLA was used to fabricate and package a completely 3D printed flow meter that operates on the principle of Joule heating and hotwire anemometry. When the designed flowmeter was simulated using a finite element package, a flow sensitivity of -2.33 Ω sccm-1 and a relative change in resistivity of 0.036 sccm-1 was expected. For an operating voltage of 12-15 V, the experimental results showed a flow sensitivity within the range of 0.014-0.032 sccm-1 and the relative change in resistivity ranged from 0.039 – 0.065 sccm-1. Thus, a completely 3D printed flowmeter was demonstrated. Second, using the same principle of Joule heating, an actuator inspired from MEMS chevron grippers was designed, simulated, and fabricated. Simulation showed the feasibility of the structure and further predicted a displacement of a few hundred microns with a potential as low as 3 V with a cooling time as little less than 120 seconds. Experimentally, a displacement of 120.04, 97.05, and 88.96 μm were achieved in 15, 10, and 5 seconds with actuation potentials of 12.7, 13.8, and 17.9 V, respectively. As predicted by the simulation results, it took longer for the gripper to cool (close to 180 seconds) when compared to actuation times. During the above studies, we discovered the printing parameters altered the part resistance. Our final study examined how extrusion temperature and printing speed affects the impedance of the MEAM printed parts. Further, anisotropy in the impedance was observed and the influence of the interface to it was examined. From the experimental results, the anisotropy was quantified with a Z/F ratio and was found to be nearly constant, ~2.15±0.23. Impedance scaling with the number of interfaces was measured and showed conclusively that the interlayer bonding was the sole source for the observed Z/F ratio. Scanning electron microscope images shows the absence of air gaps at the interface, and energy dispersion spectroscopy shows the absence of oxidation at the interface. By investigating the role of print parameters and scaling of impedance with interfaces, a framework to model and predict electrical behavior of electro thermal sensors and actuators made via MEAM can be realized

Hydrogel-based logic circuits for planar microfluidics and lab-on-a-chip automation

The transport of vital nutrient supply in fluids as well as the exchange of specific chemical signals from cell to cell has been optimized over billion years of natural evolution. This model from nature is a driving factor in the field of microfluidics, which investigates the manipulation of the smallest amounts of fluid with the aim of applying these effects in fluidic microsystems for technical solutions. Currently, microfluidic systems are receiving attention, especially in diagnostics, \textit{e.g.} as SARS-CoV-2 antigen tests, or in the field of high-throughput analysis, \textit{e.g.} for cancer research. Either simple-to-use or large-scale integrated microfluidic systems that perform biological and chemical laboratory investigations on a so called Lab-on-a-Chip (LoC) provide fast analysis, high functionality, outstanding reproducibility at low cost per sample, and small demand of reagents due to system miniaturization. Despite the great progress of different LoC technology platforms in the last 30 years, there is still a lack of standardized microfluidic components, as well as a high-performance, fully integrated on-chip automation. Quite promising for the microfluidic system design is the similarity of the Kirchhoff's laws from electronics to predict pressure and flow rate in microchannel structures. One specific LoC platform technology approach controls fluids by active polymers which respond to specific physical and chemical signals in the fluid. Analogue to (micro-)electronics, these active polymer materials can be realized by various photolithographic and micro patterning methods to generate functional elements at high scalability. The so called chemofluidic circuits have a high-functional potential and provide “real” on-chip automation, but are complex in system design. In this work, an advanced circuit concept for the planar microfluidic chip architecture, originating from the early era of the semiconductor-based resistor-transistor-logic (RTL) will be presented. Beginning with the state of the art of microfluidic technologies, materials, and methods of this work will be further described. Then the preferred fabrication technology is evaluated and various microfluidic components are discussed in function and design. The most important component to be characterized is the hydrogel-based chemical volume phase transition transistor (CVPT) which is the key to approach microfluidic logic gate operations. This circuit concept (CVPT-RTL) is robust and simple in design, feasible with common materials and manufacturing techniques. Finally, application scenarios for the CVPT-RTL concept are presented and further development recommendations are proposed.:1 The transistor: invention of the 20th century 2 Introduction to fluidic microsystems and the theoretical basics 2.1 Fluidic systems at the microscale 2.2 Overview of microfluidic chip fabrication 2.2.1 Common substrate materials for fluidic microsystems 2.2.2 Structuring polymer substrates for microfluidics 2.2.3 Polymer chip bonding technologies 2.3 Fundamentals and microfluidic transport processes 2.3.1 Fluid dynamics in miniaturized systems 2.3.2 Hagen-Poiseuille law: the fluidic resistance 2.3.3 Electronic and microfluidic circuit model analogy 2.3.4 Limits of the electro-fluidic analogy 2.4 Active components for microfluidic control 2.4.1 Fluid transport by integrated micropumps 2.4.2 Controlling fluids by on-chip microvalves 2.4.3 Hydrogel-based microvalve archetypes 2.5 LoC technologies: lost in translation? 2.6 Microfluidic platforms providing logic operations 2.6.1 Hybrids: MEMS-based logic concepts 2.6.2 Intrinsic logic operators for microfluidic circuits 2.7 Research objective: microfluidic hydrogel-based logic circuits 3 Stimuli-responsive polymers for microfluidics 3.1 Introduction to hydrogels 3.1.1 Application variety of hydrogels 3.1.2 Hydrogel microstructuring methods 3.2 Theory: stimuli-responsive hydrogels 3.3 PNIPAAm: a multi-responsive hydrogel 4 Design, production and characterization methods of hydrogel-based microfluidic systems 4.1 The semi-automated computer aided design approach for microfluidic systems 4.2 The applied design process 4.3 Fabrication of microfluidic chips 4.3.1 Photoresist master fabrication 4.3.2 Soft lithography for PDMS chip production 4.3.3 Assembling PDMS chips by plasma bonding 4.4 Integration of functional hydrogels in microfluidic chips 4.4.1 Preparation of a monomer solution for hydrogel synthesis 4.4.2 Integration methods 4.5 Effects on hydrogel photopolymerization and the role of integration method 4.5.1 Photopolymerization from monomer solutions: managing the diffusion of free radicals 4.5.2 Hydrogel adhesion and UV light intensity distribution in the polymerization chamber 4.5.3 Hydrogel shrinkage behavior of different adhesion types 4.6 Comparison of the integration methods 4.7 Characterization setups for hydrogel actuators and microfluidic measurements . 71 4.7.1 Optical characterization method to describe swelling behavior 4.7.2 Setup of a microfluidic test stand 4.8 Conclusion: design, production and characterization methods 5 VLSI technology for hydrogel-based microfluidics 5.1 Overview of photolithography methods 5.2 Standard UV photolithography system for microfluidic structures 5.3 Self-made UV lithography system suitable for the mVLSI 5.3.1 Lithography setup for the DFR and SU-8 master exposure 5.3.2 Comparison of mask-based UV induced crosslinking for DFR and SU-8 5.4 Mask-based UV photopolymerization for mVLSI hydrogel patterning 5.4.1 Lithography setup for the photopolymerization of hydrogels 5.4.2 Hydrogel photopolymerization: experiments and results 5.4.3 Troubleshooting: photopolymerization of hydrogels 5.5 Conclusion: mVLSI technologies for hydrogel-based LoCs 6 Components for chemofluidic circuit design 6.1 Passive components in microfluidics 6.1.1 Microfluidic resistor 6.1.2 Planar-passive microfluidic signal mixer 6.1.3 Phase separation: laminar flow signal splitter 6.1.4 Hydrogel-based microfluidic one-directional valves 6.2 Hydrogel-based active components 6.2.1 Reversible hydrogel-based valves 6.2.2 Hydrogel-based variable resistors 6.2.3 CVPT: the microfluidic transistor 6.3 Conclusion: components for chemofluidic circuits 7 Hydrogel-based logic circuits in planar microfluidics 7.1 Development of a planar CVPT logic concept 7.1.1 Challenges of planar microfluidics 7.1.2 Preparatory work and conceptional basis 7.2 The microfluidic CVPT-RTL concept 7.3 The CVPT-RTL NAND gate 7.3.1 Circuit optimization stabilizing the NAND operating mode 7.3.2 Role of laminar flow for the CVPT-RTL concept 7.3.3 Hydrogel-based components for improved switching reliability 7.4 One design fits all: the NOR, AND and OR gate 7.5 Control measures for cascaded systems 7.6 Application scenarios for the CVPT-RTL concept 7.6.1 Use case: automated cell growth system 7.6.2 Use case: chemofluidic converter 7.7 Conclusion: Hydrogel-based logic circuits 8 Summary and outlook 8.1 Scientific achievements 8.2 Summarized recommendations from this work Supplementary information SI.1 Swelling degree of BIS-pNIPAAm gels SI.2 Simulated ray tracing of UV lithography setup by WinLens® SI.3 Determination of the resolution using the intercept theorem SI.4 Microfluidic master mold test structures SI.4.1 Polymer and glass mask comparison SI.4.2 Resolution Siemens star in DFR SI.4.3 Resolution Siemens star in SU-8 SI.4.4 Integration test array 300 μm for DFR and SU-8 SI.4.5 Integration test array 100 μm for SU-8 SI.4.6 Microfluidic structure for different technology parameters SI.5 Microfluidic test setups SI.6 Supplementary information: microfluidic components SI.6.1 Compensation methods for flow stabilization in microfluidic chips SI.6.2 Planar-passive microfluidic signal mixer SI.6.3 Laminar flow signal splitter SI.6.4 Variable fluidic resistors: flow rate characteristics SI.6.5 CVPT flow rate characteristics for high Rout Standard operation proceduresDer Transport von lebenswichtigen Nährstoffen in Flüssigkeiten sowie der Austausch spezifischer chemischer Signale von Zelle zu Zelle wurde in Milliarden Jahren natürlicher Evolution optimiert. Dieses Vorbild aus der Natur ist ein treibender Faktor im Fachgebiet der Mikrofluidik, welches die Manipulation kleinster Flüssigkeitsmengen erforscht um diese Effekte in fluidischen Mikrosystemen für technische Lösungen zu nutzen. Derzeit finden mikrofluidische Systeme vor allem in der Diagnostik, z.B. wie SARS-CoV-2-Antigentests, oder im Bereich der Hochdurchsatzanalyse, z.B. in der Krebsforschung, besondere Beachtung. Entweder einfach zu bedienende oder hochintegrierte mikrofluidische Systeme, die biologische und chemische Laboruntersuchungen auf einem sogenannten Lab-on-a-Chip (LoC) durchführen, bieten schnelle Analysen, hohe Funktionalität, hervorragende Reproduzierbarkeit bei niedrigen Kosten pro Probe und einen geringen Bedarf an Reagenzien durch die Miniaturisierung des Systems. Trotz des großen Fortschritts verschiedener LoC-Technologieplattformen in den letzten 30 Jahren mangelt es noch an standardisierten mikrofluidischen Komponenten sowie an einer leistungsstarken, vollintegrierten On-Chip-Automatisierung. Vielversprechend für das Design mikrofluidischer Systeme ist die Ähnlichkeit der Kirchhoff'schen Gesetze aus der Elektronik zur Vorhersage von Druck und Flussrate in Mikrokanalstrukturen. Ein spezifischer Ansatz der LoC-Plattformtechnologie steuert Flüssigkeiten durch aktive Polymere, die auf spezifische physikalische und chemische Signale in der Flüssigkeit reagieren. Analog zur (Mikro-)Elektronik können diese aktiven Polymermaterialien durch verschiedene fotolithografische und mikrostrukturelle Methoden realisiert werden, um funktionelle Elemente mit hoher Skalierbarkeit zu erzeugen.\\ Die sogenannten chemofluidischen Schaltungen haben ein hohes funktionales Potenzial und ermöglichen eine 'wirkliche' on-chip Automatisierung, sind jedoch komplex im Systemdesign. In dieser Arbeit wird ein fortgeschrittenes Schaltungskonzept für eine planare mikrofluidische Chiparchitektur vorgestellt, das aus der frühen Ära der halbleiterbasierten Resistor-Transistor-Logik (RTL) hervorgeht. Beginnend mit dem Stand der Technik der mikrofluidischen Technologien, werden Materialien und Methoden dieser Arbeit näher beschrieben. Daraufhin wird die bevorzugte Herstellungstechnologie bewertet und verschiedene mikrofluidische Komponenten werden in Funktion und Design diskutiert. Die wichtigste Komponente, die es zu charakterisieren gilt, ist der auf Hydrogel basierende chemische Volumen-Phasenübergangstransistor (CVPT), der den Schlüssel zur Realisierung mikrofluidische Logikgatteroperationen darstellt. Dieses Schaltungskonzept (CVPT-RTL) ist robust und einfach im Design und kann mit gängigen Materialien und Fertigungstechniken realisiert werden. Zuletzt werden Anwendungsszenarien für das CVPT-RTL-Konzept vorgestellt und Empfehlungen für die fortlaufende Entwicklung angestellt.:1 The transistor: invention of the 20th century 2 Introduction to fluidic microsystems and the theoretical basics 2.1 Fluidic systems at the microscale 2.2 Overview of microfluidic chip fabrication 2.2.1 Common substrate materials for fluidic microsystems 2.2.2 Structuring polymer substrates for microfluidics 2.2.3 Polymer chip bonding technologies 2.3 Fundamentals and microfluidic transport processes 2.3.1 Fluid dynamics in miniaturized systems 2.3.2 Hagen-Poiseuille law: the fluidic resistance 2.3.3 Electronic and microfluidic circuit model analogy 2.3.4 Limits of the electro-fluidic analogy 2.4 Active components for microfluidic control 2.4.1 Fluid transport by integrated micropumps 2.4.2 Controlling fluids by on-chip microvalves 2.4.3 Hydrogel-based microvalve archetypes 2.5 LoC technologies: lost in translation? 2.6 Microfluidic platforms providing logic operations 2.6.1 Hybrids: MEMS-based logic concepts 2.6.2 Intrinsic logic operators for microfluidic circuits 2.7 Research objective: microfluidic hydrogel-based logic circuits 3 Stimuli-responsive polymers for microfluidics 3.1 Introduction to hydrogels 3.1.1 Application variety of hydrogels 3.1.2 Hydrogel microstructuring methods 3.2 Theory: stimuli-responsive hydrogels 3.3 PNIPAAm: a multi-responsive hydrogel 4 Design, production and characterization methods of hydrogel-based microfluidic systems 4.1 The semi-automated computer aided design approach for microfluidic systems 4.2 The applied design process 4.3 Fabrication of microfluidic chips 4.3.1 Photoresist master fabrication 4.3.2 Soft lithography for PDMS chip production 4.3.3 Assembling PDMS chips by plasma bonding 4.4 Integration of functional hydrogels in microfluidic chips 4.4.1 Preparation of a monomer solution for hydrogel synthesis 4.4.2 Integration methods 4.5 Effects on hydrogel photopolymerization and the role of integration method 4.5.1 Photopolymerization from monomer solutions: managing the diffusion of free radicals 4.5.2 Hydrogel adhesion and UV light intensity distribution in the polymerization chamber 4.5.3 Hydrogel shrinkage behavior of different adhesion types 4.6 Comparison of the integration methods 4.7 Characterization setups for hydrogel actuators and microfluidic measurements . 71 4.7.1 Optical characterization method to describe swelling behavior 4.7.2 Setup of a microfluidic test stand 4.8 Conclusion: design, production and characterization methods 5 VLSI technology for hydrogel-based microfluidics 5.1 Overview of photolithography methods 5.2 Standard UV photolithography system for microfluidic structures 5.3 Self-made UV lithography system suitable for the mVLSI 5.3.1 Lithography setup for the DFR and SU-8 master exposure 5.3.2 Comparison of mask-based UV induced crosslinking for DFR and SU-8 5.4 Mask-based UV photopolymerization for mVLSI hydrogel patterning 5.4.1 Lithography setup for the photopolymerization of hydrogels 5.4.2 Hydrogel photopolymerization: experiments and results 5.4.3 Troubleshooting: photopolymerization of hydrogels 5.5 Conclusion: mVLSI technologies for hydrogel-based LoCs 6 Components for chemofluidic circuit design 6.1 Passive components in microfluidics 6.1.1 Microfluidic resistor 6.1.2 Planar-passive microfluidic signal mixer 6.1.3 Phase separation: laminar flow signal splitter 6.1.4 Hydrogel-based microfluidic one-directional valves 6.2 Hydrogel-based active components 6.2.1 Reversible hydrogel-based valves 6.2.2 Hydrogel-based variable resistors 6.2.3 CVPT: the microfluidic transistor 6.3 Conclusion: components for chemofluidic circuits 7 Hydrogel-based logic circuits in planar microfluidics 7.1 Development of a planar CVPT logic concept 7.1.1 Challenges of planar microfluidics 7.1.2 Preparatory work and conceptional basis 7.2 The microfluidic CVPT-RTL concept 7.3 The CVPT-RTL NAND gate 7.3.1 Circuit optimization stabilizing the NAND operating mode 7.3.2 Role of laminar flow for the CVPT-RTL concept 7.3.3 Hydrogel-based components for improved switching reliability 7.4 One design fits all: the NOR, AND and OR gate 7.5 Control measures for cascaded systems 7.6 Application scenarios for the CVPT-RTL concept 7.6.1 Use case: automated cell growth system 7.6.2 Use case: chemofluidic converter 7.7 Conclusion: Hydrogel-based logic circuits 8 Summary and outlook 8.1 Scientific achievements 8.2 Summarized recommendations from this work Supplementary information SI.1 Swelling degree of BIS-pNIPAAm gels SI.2 Simulated ray tracing of UV lithography setup by WinLens® SI.3 Determination of the resolution using the intercept theorem SI.4 Microfluidic master mold test structures SI.4.1 Polymer and glass mask comparison SI.4.2 Resolution Siemens star in DFR SI.4.3 Resolution Siemens star in SU-8 SI.4.4 Integration test array 300 μm for DFR and SU-8 SI.4.5 Integration test array 100 μm for SU-8 SI.4.6 Microfluidic structure for different technology parameters SI.5 Microfluidic test setups SI.6 Supplementary information: microfluidic components SI.6.1 Compensation methods for flow stabilization in microfluidic chips SI.6.2 Planar-passive microfluidic signal mixer SI.6.3 Laminar flow signal splitter SI.6.4 Variable fluidic resistors: flow rate characteristics SI.6.5 CVPT flow rate characteristics for high Rout Standard operation procedure

Phase-Change Meta-Devices for Tuneable Bandpass Filtering in the Infrared

Tuneable light filters, especially those which are compact and fast to tune, are essential in a wide range of technologies, especially for multispectral imaging applications. However, state-of-the-art approaches to create such filters all possess drawbacks, with many wavelength regions poorly served. This thesis attempts to address this problem by combining metasurfaces which support extraordinary optical transmission (ultra-thin band-pass filters) with chalcogenide phase-change materials (adding dynamic tuneability). The optical properties of phase-change materials are very different in their amorphous and crystalline states and switching between such states can be rapidly controlled via thermal excitations. In this work nine different phase-change materials, including alloys of GeTe, GeSbTe, GeSbSeTe and GaLaS, were optically and elementally characterised and assessed for their application-specific suitability. The resulting materials data was used to computationally design and evaluate a range of tuneable infrared filter device designs both optically and thermally. These filters exhibit high transmission (≈80% at best) with large spectral tuning ranges of approximately +50% relative to their shortest wavelength; this range is sufficient to cover entire atmospheric transmission windows. This is the first such combination of phase-change materials and extraordinary optical transmission for application from the visible through to long-wave infrared (14 μm) regions of the spectrum. A rigorous computational study was conducted to produce comprehensive design guidelines for such filters, and confirm the viability of in-situ electrical switching. Several filter devices were experimentally fabricated, and the viability for a number of applications, including tuneable filtering, chemical sensing and infrared displays, was investigated and confirmed computationally.Engineering and Physical Sciences Research Council (EPSRC

Doctor of Philosophy

dissertationMetamaterials have gained significant attention over the last decade because they can exhibit electromagnetic properties that are not readily available in naturally occurring materials. This dissertation describes our work on design, fabrication and characterization of liquid metal-based metamaterials with focus on their applications in the terahertz (THz) frequency range. In contrast to the more conventional approaches to fabricating these structures, which rely on vacuum deposited solid metal films, we used metals that are liquid at room temperature. This family of materials is especially attractive for such applications, since it enables large-scale reconfigurability in the overall geometry of the device. We demonstrate a number of unique plasmonic and metamaterial devices. Within the topic of plasmonics, we demonstrate a device that allows for mechanical stretching that is reversibly deformable. In an analogous structure, we can change the geometry dramatically by injecting or withdrawing liquid metals from specific area of the pattern. We also developed a liquid metal-based reconfigurable THz metamaterial device that is not only pressure driven, but also exhibits pressure memory. As an alternate approach to demonstrate reconfigurability, we developed a technique for creating dramatic configuration changes in a device via selective erasure and refilling of metamaterial unit cells that utilizes hydrochloric acid. While the approach is successful in changing the geometry, it does not allow for fine spatial control of the pattern. Thus, we have refined the approach by developing an electrolytic process to change the geometry of a liquid metal-based structured device in a more localized and controlled manner. Since liquid metals can be solidified under certain conditions, we have demonstrated a novel technique for fabrication of free-standing two-dimensional and three-dimensional terahertz metamaterial devices using injection molding of gallium. Finally, we developed a technique of printing three-dimensional solid metal structures by pulling liquid gallium out of a reservoir via solid/liquid interface. Based on these results, we are currently extending our work towards development of metamaterials that can be used in real-world applications. Based on the significant progress made the THz field over the last two decades, the likelihood of THz systems level applications is much brighter

Copper to copper bonding by nano interfaces for fine pitch interconnections and thermal applications

Ever growing demands for portability and functionality have always governed the electronic technology innovations. IC downscaling with Moore s law at IC level and system miniaturization with System-On-Package (SOP) paradigm at system level, have resulted and will continue to result in ultraminiaturized systems with unprecedented functionality at reduced cost. However, system miniaturization poses several electrical and thermal challenges that demand innovative solutions including advanced materials, bonding and assembly techniques. Heterogeneous material and device integration for thermal structures and IC assembly are limited by the bonding technology and the electrical and thermal impedance of the bonding interfaces. Solder - based bonding technology that is prevalent today is a major limitation to future systems. The trend towards miniaturized systems is expected to drive downscaling of IC I/O pad pitches from 40µm to 1- 5µm in future. Solder technology imposes several pitch, processability and cost restrictions at such fine pitches. Furthermore, according to International Technology Roadmap for Semiconductors (ITRS-2006), the supply current in high performance microprocessors is expected to increase to 220 A by 2012. At such supply current, the current density will exceed the maximum allowable current density of solders. The intrinsic delay and electromigration in solders are other daunting issues that become critical at nanometer sized technology nodes. In addition, formation of intermetallics is also a bottleneck that poses significant mechanical issues. Similarly, thermal power dissipation is growing to unprecedented high with a projected power of 198 W by 2008 (ITRS 2006). Present thermal interfaces are not adequate for such high heat dissipation. Recently, copper based thin film bonding has become a promising approach to address the abovementioned challenges. However, copper-copper direct bonding without using solders has not been studied thoroughly. Typically, bonding is carried out at 400oC for 30 min followed by annealing for 30 min. High thermal budget in such process makes it less attractive for integrated systems because of the associated process incompatibilities. Hence, there is a need to develop a novel low temperature copper to copper bonding process. In the present study, nanomaterials - based copper-to-copper bonding is explored and developed as an alternative to solder-based bonding. To demonstrate fine pitch bonding, the patterning of these nanoparticles is crucial. Therefore, two novel self-patterning techniques based on: 1.) Selective wetting and 2.) Selective nanoparticle deposition, are developed to address this challenge. Nanoparticle active layer facilitates diffusion and, thus, a reliable bond can be achieved using less thermal budget. Quantitative characterization of the bonding revealed good metallurgical bonding with very high bond strength. This has been confirmed by several morphological and structural characterizations. A 30-micron pitch IC assembly test vehicle is used to demonstrate fine pitch patternability and bonding. In conclusion, novel nanoparticle synthesis and patterning techniques were developed and demonstrated for low-impedance and low-cost electrical and thermal interfaces.M.S.Committee Chair: Rao R. Tummala; Committee Member: C. P. Wong; Committee Member: P. M. Ra