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NSF Nanoscale Science and Engineering Center for High-rate Nanomanufacturing Thrust 3: Testbeds Nick McGruer Director: Ahmed Busnaina, NEU Deputy Director: Joey Mead, UML, Associate Directors: Carol Barry, UML; Nick McGruer, NEU; Glen Miller, UNH; Jacqueline Isaacs, NEU, Group Leader: David Tomanek, MSU Collaboration and Outreach: Museum of Science-Boston, City College of New York, Hampton Univ., Rice Univ., Hanyang Univ., Korean Center for Nanoscale Mechatronics and Manufacturing (CNMM), University of Hyogo, Japan NEU; UML; UNH Thrust 2: High-rate Assembly and Transfer NEU; UML; UNH Thrust 1: Manufacture Nanotemplates and Nanotubes NEU; UNH Education & Outreach NEU; UML; UNH Thrust 3: Testbeds Memory Device and Biosensor Thrust 4: Societal Implications NEU; UML CHN Path to Nanomanufacturing Nanotube Devices Testbed Biosensors Testbed Alignment Processes Reliability and Defect Control Developing Testbeds and Applications NSF Center for High-rate Nanomanufacturing Application Road Map Thrust 3: Testbeds, Memory Device and Biosensor PIs: Ahmed Busnaina, Nick McGruer, George Adams, NEU Post Docs: Siva Somu, Nam Goo Cha, NEU. Students: Taehoon Kim, Anup Sing, Suchit Shah, NEU. Nanotube Devices Testbed Biosensors Testbeds Alignment Processes Reliability and Defect Control Developing Testbeds and Applications PIs: Joey Mead, Carol Barry, Susan Braunhut, Ken Marx, Sandy McDonald, UML, Ahmed Busnaina, NEU. Post Docs:, Lisa Clarizia, UML. Students: Vikram Shankar, UML. PIs: Ahmed Busnaina, Nick McGruer, NEU, Jim Whitten, UML, Howard Mayne, UNH. Students: Jose Medina, Jagdeep Singh, UML. PIs: Ahmed Busnaina, Nick McGruer, George Adams, NEU. Students: Juan Aceros, Peter Ryan, NEU. PIs: Sanjeev Mukerjee, Nick McGruer, Ahmed Busnaina, Mehmet Dokmeci, Jung Joon Jung, NEU, Glen Miller, UNH, Joey Mead, Carol Barry, UML What are the Critical Barriers to Nanomanufacturing? Barrier 2. How can we scale up assembly processes in a continuous or high rate manner? Demonstration of assembly processes; scale-up; technology transfer. Barrier 3. How can we test for reliability in nanoelemnts and connections? How can we efficiently detect and remove defects? MEMS Testbed for accelerated test of nanoelements. Collaboration with the Center for Microcontamination Control on removal of nanoscale defects. Barrier 4. Do nanoproducts and processes require new economic, environmental, and ethical/regulatory assessment and new sociallyaccepted values? Testbed process can be case studies for environmental, economic, and regulatory needs. Two Established Proof of Concept Testbeds Chosen to verify CHN- Developed manufacturing processes. Easy to measure to validate functionality. Strong industry partnership for product realization. Nanotube Memory Device Biosensor Partner: Nantero first to make memory devices using nanotubes Properties: nonvolatile, high Partner: Triton Systems developed antibody attachment for medical applications speed programming at <3ns, lifetime goal >1015 cycles, resistant to heat, cold, magnetism, vibration, and radiation. Properties: increased sensitivity, smaller sample size, detection of multiple antigens with one device, small/low cost. Four Examples of Carbon Nanotube Switches MWNT Mechanical Switch Jang et al., Appl. Phys. Lett. (2005) 87, 163114. Self-assembled switches based on electroactuated multiwalled nanotubes E. Dujardin,a V. Derycke,b M. F. Goffman, R. Lefèvre, and J. P. Bourgoin Applied Physics Letters 87, 193107 2005 Carbon Nanotube Non-Volatile Memory Device, Ward, J.W.; Meinhold, M.; Segal, B.M.; Berg, J.; Sen, R.; Sivarajan, R.; Brock, D.K.; Rueckes, T. IEEE, 2004, 34-38. High Density Memory Chip Testbed Current Nantero process Uses conventional optical lithography to pattern carbon nanotube films Switches are made from belts of nanotubes ON state OFF state CHN Nanomanufacturing Processes: Electrodes (~100nm with 300 nm period) • Nanotemplates will enable aligned CNT. •Near Term, smaller linewidth, better process control. •Ultimately, single CNT switches. (Nantero, 2004) Template Transfer Technology Validation in Memory Device Testbed Testbeds: Testbeds: Memory Devices Memory Devices and Biosensor CNTs on trenches form memory elements. Assemble and Transfer Nanoelements Carbon nanotubes assembled from solution Manufacture Nanotemplates and Nanotubes Type II CHN Nanotube Switch for Non-Volatile Memory • Type II Switch has two symmetric non-volatile states. • Simple process. • CNTs assembled directly on chip using dielectrophoresis or using template transfer. • Measurements in progress. • CNT/Surface interaction critical, measurements in progress. Schematic of state I and II. Directed Assembly of a Single SWCNT by Dielectrophoresis SWNT Memory Testbed Status and Plan • Why Important? – We need new manufacturing methods to scale beyond CMOS (to approach terabytes/cm2 in memory density for example). – CHN templates will reduce current line width by 10X (10 nm line width) in the initial phase. – Developing manufacturing processes for manipulating nanotubes/nanoelements. Can be applied to FETs, molecular switches. • Current Status – Developing templated and template-less SWNT assembly techniques. – Preparing silicon-based and polymer-based templates to develop transfer processes. – Fabricating Nantero-style switches and switches with a symmetrical two-state design. • Transition Plan – In 2009 will have large scale directed assembly of SWNT over 4” wafers – Technology transfer anticipated by 2012 ELISA (Enzyme-Linked ImmunoSorbent Assay), Background Antigen binding sites Adsorb primary antibody onto a solid substrate Elisa analysis of a serum sample with breast cancer. Source: Richard Zangar, Nature Bind antigen (biomarker for specific disease) to antibody Add labeled detection antibody Detection of fluorescence or color change of substrate Biosensor; State of the Art Elisa analysis of a serum sample with breast cancer. Source: Richard Zangar, Nature • Commercial ELISA systems • Cantilevers for detection – M. Calleja et al, IMM-Centro Nacional de Microelectronias, Tres Cantos, Spain – V. Dauksaite et al, University of Aarhus, Aarhus, Denmark • Nanowire sensors – Antibodies are not patterned (immobilized), so maximum sensitivity is not attained F. Patolsky and C.M. Lieber, "Nanowire nanosensors," Materials Today, 8, 20-28 (2005) Cantilevers are coated with antibodies to PSA, When PSA binds to the antibodies, the cantilever is deflected, Mujumdar, UC BERKELEY Increase Performance of Antibody-Based Sensors Opportunity: • Random orientation and spacing of antibodies. • Want to control: Spacing too wide for maximum sensitivity •Orientation of antibodies (Functional antibodies estimated to be : 10-20%) •Spacing of antibodies. Spacing too close for antigen detection Controlled orientation: Can increase sensitivity by 5-10x. Templates not required. Method 1: Chemical attachment May disrupt antibody activity. Must evaluate for a specific antibody. Method 2: Protein G based attachment. Controlled spacing: Can increase sensitivity by 5-10x? Less non-specific binding. Use templates to pattern polymer blends. High-rate, high-volume process. Wide choice of polymers. Orientation Fab to Fc Response Ratios •Ratio of Oriented FAB 8 6 RATIO (Fab) to disOriented (Fc) response was much higher for the CHN system. 4 FC 2 0 UHB HB MB POLYMER PMMA CHN Keck Nano Bio Chip Biosensor Goals – – – – – Simultaneous measurement of multiple biomarkers with one device Very small size (can be as small as 100 µm x 100 µm) Can be made of all biocompatible material Low cost Future development will lead to a device where drugs are released based on the detected antigen. – In-vivo measurement – No issues with sample collection and storage BioSensor Status, Plan and Goals • Why Important? – CHN templates will improve sensitivity by 10-100X and provide selectivity not available now by improving both antibody orientation and spacing. – Potential for physically smaller, less expensive arrays with more sensitivity and functionality. (Detect multiple antibodies/diseases in one test, for example.) • Current Status – Developed oriented attachment approaches for antibodies on candidate components of polymer blends. – Assembly of polymer blends using templates. • Biosensor Goals – Demonstrate high-rate assembly of antibody selective polymer blends. – Demonstrate selective antibody attachment to one component of a template-assembled polymer blend. – Demonstrate control of antibody spacing with appropriate assembled polymer blend pattern. Reliability, Accelerated Test, Properties • Monitor reliability of materials, MEMS Devices for Accelerated Test interfaces, and systems to ensure manufacturing readiness. Nanowire Contacts N an ow ire SiO2 Si Contacts – Changes in material or contact properties with environmental exposure, stress, temperature … Si (2um) • Accelerated testing for reduced manufacturing risk. – – Rapid mechanical, electrical, and thermal cycling with measurement capability. Example: MEMS devices to rapidly cycle strain or temperature while measuring resistance and imaging in SEM or STM. UHV compatible. • Nanoscale material, contact, and interface property monitoring. – – Example: Measure adherance force and friction between functionalized nanoelements and functionalized substrates. Example: Measure Young’s modulus and yield strength of nanoelements. SiO2 (2um) Si Substrate Interaction of AFM Cantilever with Suspended Nanotube MEMS Nanoscale Characterization and Reliability Testbed, Introduction Nanowire Contacts SiO2 Si Contacts N an ow ire •Considerable work on MEMS resonators – properties of the resonator itself: •C. L. Muhlstein, S. B. Brown, R. O. Ritchie, High-Cycle fatigue of Single –Crystal Silicon Thin Films, J. MEMS, 10, 4 (2001) pp. 593-600. Si (2um) SiO2 (2um) Si Substrate •Work on MEMS material properties, much less quantative work on properties/reliability of nanoscale structures or interfaces. •M. A. Haque, M. T. A. Saif, “Mechanical Behavior of 3050 nm thick Aluminum Films Under Uniaxial Tension”, Scripta Mat. pp 863, Vol 47 (2002). •T. Yi, C. J. Kim, "Measurement of Mechanical Properties for MEMS Materials", Meas. Sci. Technol., pp. 706-716, Vol 10, (1999). •M. T. A. Saif, N. C. MacDonald, “Measurement of Forces and Spring Constants of Microinstruments”, Rev. Scien. Inst. pp 1410, Vol 69, 3 (1998). •M. Yu, B. S. Files, S. Arepalli, R. S. Ruoff, “Tensile Loading of Ropes of Single Wall Carbon Nanotubes and their Mechanical Properties”, Phys. Rev. Lett. pp 5552, Vol 84, 24 (2000). •A. V. Desai, M. A. Haque, “Test Bed for Mechanical Characterization of Nanowires”, JNN Proc. IMechE. Part N. pp 57-65, Vol 219, N2 (2006). MEMS Testbed for Accelerated Test and Properties Measurement Test Devices Angular Resonator Tensile Test Bend Test Horizontal Resonator MicroHotPlate Innovative MEMS devices characterize nanowires (also nanotubes, nanorods and nanofibers) and conduct accelerated lifetime testing allowing rapid mechanical, electrical, and thermal cycling which can be combined with AFM/SEM/UHV SPM observation. Suitable for remote testing: Space or radiation environments. Small, lightweight, low-power. MEMS Nanoscale Characterization and Reliability Testbed, Nano Pull Test Currently characterizing electrospun fibers from UML. MEMS Nanoscale Characterization and Reliability Testbed, Hot Plate with Nanowire Au, Ru, and RuO2 nanowires tested, currently testing CNT bundles. AFM Measurement of CNT-Surface Interaction (in support of assembly, transfer and CNT switches). • What: Development of techniques for measurement of interactions between functionalized nanotubes and functionalized surfaces. • Purpose: Process control for single nanotube switch process. F/d On Suspended CNT F/d On neighboring Substrate RMS and A-B Data Plotted for a 100 nm Z-Piezo Displacement Below the Substrate Summary and Goal • Generally Applicable Tools Available Now for: 1. Measurements of Reliability of Nanoelements, Contacts, and Systems. 2. Accelerated Test of Nanoelements, Contacts, and Systems. 3. Measurements of Properties of Nanoscale Elements and Interactions between Elements. • These tools will help to ensure manufacturing readiness and will help to reduce the time for technology transition to manufacturing. Low Cost, High Power and Energy Density Secondary Storage Batteries •Sanjeev Mukerjee, Professor, Dept. of Chemistry and Chemical Biology Director, Energy Research Center, Northeastern University •Collaborate with CHN to develop unique micro-arrays for 2-D and 3-D batteries based on Li-ion chemistry. 3-D designs will have up to 350 times higher energy and power density as compared to the conventional designs. High rate 2D templates for Microbatteries SiO2 Si P-type SWNT Assembly N-type SWNT Assembly P type N type P type N type SWNTs Assembled within polymer 260 nm trenches over 100m long in 60 Sec. 3D templates for Microbatteries Si/SiO2 Substrate Co Seed Catalyst Patterning Grown SWNT pillars Jung, NEU SWNT CVD Growth SWNT network grown between SiO2 nano pillars. Jung, NEU Lightweight Structural Materials with Integrated Wiring, Thermal Management, and EMI Shielding assembly transfer • Controlled orientation of CNTs • Patterned conducting elements (thermal and electrical) • Embed in polymeric matrix Reduced time to implement since process has been developed Lightweight Structural Materials Process can be advanced to produce large sheets • Widths: 3-6 feet • Rates: 60 48,000 feet per hour Polymer film Patterned surface Template roller with nano or micro patterns Carbon nanotubes CNT supply Lightweight structural materials Lightweight Structural Materials Nanocomposites (e.g. carbon nanotubes, nanowhiskers, etc.) • Compared to conventional reinforcements 40X greater strength to weight ratio • Lighter weight and lower cost Material Modulus, GPa Strength, GPa Density, g/cm3 SWNT 1054 150 1.40 MWNT 1200 150 2.60 Glass fiber 87 4.6 2.50 Carbon fiber 228 3.8 1.80 Kevlar 186 3.6 --- Steel 208 1.0 7.80 Thermal Management Nanoparticles and carbon nanotubes • Greater thermal conductivity than polymers Material Thermal Conductivity, W/m-K CNT 2000 Density, g/cm3 1.4 Silver 418 10.5 Copper 386 8.95 Gold 143 2.8 Silica Kapton (PI) 1.40 0.37 2.2 1.5 Summary, Lightweight Multifunctional Materials • CHN provides manufacturing ready processes for lightweight, flexible materials with – High strength • 40X greater strength-to-weight ratio – Tailored thermal management • Thermal conductivity at < 10% particle loading • Placement of thermal management layers or wires where required – Multiple functionalities • Strength and thermal management • Also, internal wires, EMI shielding, and stealth capabilities