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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