Outline Chemical Microsystems Applications Microfluidic Component Examples Chemical Microsystems for Analysis Chemical Microsystems for Synthesis Fundamentals of Micromachining Dr. Bruce Gale With Special Thanks to Dr. Ron Besser Microchannels, Fluidic Vias KOH Etch vs. DRIE KOH Etched (100 µm channels) DRIE Etched (5 µm channels)
Microchannels Microchannel Reaction Zone 100 µm Channels 5 µm Channels First generation PDMS Microreactors Reactor Cross Section PDMS MicroReactor 5 cm 7.5 cm 10 cm Urea Ammonia Product 150 µm Scale = 1 mm Inside Channel Scale = 100 µm
Features Flow depicted by contrasting dark lines/light green areas Fluid mixing to bring soluble reactant into contact with catalyst surface Flow characteristics of transverse mixing features Scale Comparison Nanoreactor or Micelle Macroscale, Industrial Scale
C.M. for Analysis Lab-On-Chip Definition Lab-on-chip Example: micro gas-analysis device Example: Caliper oligonucleotide separation Example: Nanogen biochips Micro-Gas-Analyzer Micro-Gas Analyzer Result
Applications of Microreactors 1. Distributed Processing 2. Toxic or Hazardous Chemicals 3. Chemical Prototyping 4. High-Value, Low-Volume Chemicals 5. Bulk Production of Commodity Chemicals 6. Special Environments 7. Laboratory Systems 8. Combinatorial Chemistry C.M. for Synthesis Definition Conversion Selectivity Example: IfM Microreactor IfM Microreactor for Synthesis Device Design Inlet Via Outlet Via Inlet Channel Pyrex Cover Manifold Silicon Chip Microchannels 5µm or 100 µm Catalyst
Device Fabrication Temperature Effect starting wafer topside via mask layer inlet/outlet 100 mm Si wafer, 18 reactors 1.0 0.9 0.8 0.7 0.6 0.5 1 2 3 4 5 6 7 8 9 10 100 µm channels Temperature holds 0.4 0.3 0.2 hydrogenation dehydrogenation 0.1 bottom via channels anodic bond [KOH or DRIE Etching] Final 1 x 3 cm 2 device 0.0 0 50 100 150 200 Temperature (ºC) Conversion near 100% Activity at T room Degradation of Conversion Selectivity Reversal at T>150 C Both products at T room 1.0 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0.0 0 50 100 150 200 250 Temperature ( C) Cyclohexane Benzene Benzene Space Time Yield- Effect of Composition Microreactor 2 Design STYA (g/cm^2/min) Benzene Space Time Yield (200ºC) 3.5E-03 3.0E-03 2.5E-03 2.0E-03 1.5E-03 1.0E-03 5.0E-04 0.0E+00 0 100 200 300 400 500 600 PH2 (torr) 0.3 sccm Ar (E) 0.6 sccm Ar (E) 1.0 sccm Ar (E) 0.3 sccm Ar (F) 0.6 sccm Ar (F) 1.0 sccm Ar (F) STYA (g/cm^2/min) Space Time Yield = yield X flow rate / catalyst area 3.5E-03 3.0E-03 2.5E-03 2.0E-03 1.5E-03 1.0E-03 5.0E-04 Benzene Space Time Yield (200ºC) Features 6 channels 50 channel length transverse mixing features in each straight section Increasing H 2 suppresses dehydrogenation Increasing C 6 H 10 favors dehydrogenation 0.0E+00 0 20 40 60 80 100 PC6H10 (torr) 0.3 sccm Ar (E) 0.6 sccm Ar (E) 1.0 sccm Ar (E) 0.3 sccm Ar (H) 0.6 sccm Ar (H) 1.0 sccm Ar (H) 0.3 sccm H2 (D)
Observations 4-6 samples averaged for each data point critical influence of residence time evident Urea Conversion (X) Continous Microreactor Results 50 cm channel with transverse features Averaged data Packaged Microreactor Systems microreactor operated 48 hours with no substantial loss in enzyme activity Flow rate (ml/min-channel) Distributed Processing Distributed Processing: the Cell Nature s Model Example: Oil Processing An Analogy of Distributed vs. Centralized Processing Mitochondrion: chemical factory in every cell
Distributed Processing: Petroleum Petroleum Processing centralized distributed Analogy: Centralized vs. Distributed Toxic or Hazardous Chemicals Toxic = Hazardous = Motivation: Operation in explosive regime Motivation: transport, storage, monitoring Example: ion-implantation of As + 1965 2000
Explosive Regime Example MIT Microreactor Fabrication H 2 + ½ O 2 H 2 O 500 C, water produced without explosion Mass Transfer Characteristics: MIT Example: Ion-Implantation Source Doped n-type region 0.1 to 1 µm Silicon wafer [As + ] 1e18 cm -3
Ion-Implanter Schematic Scale-Up Benchtop AsH3 tank Pilot Plant Iteration 1 Plant Iteration 2 Microreactor Prototype Plant Scale-Up Example High-Value, Low-Volume Chemicals Examples Pharmaceuticals NO Motivation Short shelf lives Toxicity New therapies Implantation
Bulk Production of Commodity Chemicals Definitions: No distinction by brand Oil Polymers Motivation Higher yields Less pollution Modularity (repairs) Likely impact Slow adoption Special Environments: Space Combinatorial Screening for Discovery of New Materials Systematic Variation of Component Compositions Applications Pharmaceuticals Luminescent Materials Superconductors Magnetic Materials Heterogeneous Catalysts Method Batch Processing Systematic Variation of Composition or Substitutional Groups High Sample Count Rapid Evaluation Substrate Pure B Pure A Pure C
Pure A Rapid Evaluation Rapidly Probe Each Unit Sample for Desired Activity UCLA System Array Microreactor System: A: Feed gas preheater; B: Catalyst pellets; C: Reactant gas inlet; D: Flow distribution baffles; E: Bottom aluminum heating block; F: Reactor channels; G: Signal detection microelectrodes; Pure B Pure C Activity Amount of A Amount of B Combinatorial Array for Screening Catalysts 75 Microreactor Array Systematic variation of catalyst by sputter deposition Evaluation of conversion and selectivity by Mass Spectrometry