nasys nstruments - center for hierarchical manufacturing |...
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Craig Prater, CTO
Research Challenges for Nanomanufacturing Systems
Februay 11-12th, 2008
Nanoscale Thermal Analysis
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Motivations
• Nanomanufacturing needs characterization for research, product development & process control.
– “You can’t manage what you can’t measure”
Rear Admiral Grace Hopper:– “One accurate measurement is worth one thousand
expert opinions”
• Successful nanomanufacturing needs robust, easy-to-use instruments– Instruments operated by technicians and
manufacturing floor personnel
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Some driving questions…• What the &%*# is that?• Where did component X go?• What phase is my material?• Throughput...
AFM images courtesy of Veeco Instruments
High Impact Engineering Plastic
Syndiotacticpolystyrene
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AFM Introduction
Z driveGain
Setpoint Error
Cantilever motion
LaserXY scan
Atomic Force Microscope
(AFM) Image
Z
XY
Photodetector
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ThermoMechanical Analysis (TMA)• Thermomechanical analysis measures sample displacement as a function of temperature, time and applied force
• Identify thermal transitions (e.g. glass transitions)
•Transitions signatures of material composition
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Microfabricated Thermal Probes*
IR pulse
• R = V/I ~ Tip Temperature (T)• ΔT direct measure of absorbed heat• Also heat locally to measure thermal expansion
* Developed in collaboration with Prof. W. King, UIUC
VI
I
ΔT
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•AFM probe with an integrated heater to measure thermal properties of samples
• Ramp tip temperature and monitor the lever to see observe thermal transitions (Tg, Tm)
Nano Thermal Analysis (NanoTA)
Infrared Microscopy
200 μm200 μm
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Correlation to Bulk Thermal Analysis
Three crystalline samples and three amorphous samples were measured by TMA (left) and DSC (right) and compared against nano-TA measurements.
y = 1.0088x - 3.8173R2 = 0.9811
y = 1.0027x + 0.2778R2 = 0.9701
y = 1.0047x + 2.9657R2 = 0.95810
50
100
150
200
250
300
0.0 100.0 200.0 300.0
TMA onset
Nano
Ta O
nset
0.1°C/s1°C/s10°C/s
Slopes: 1.003 - 1.009Offsets: -4 to +3ºC
y = 0.996x + 7.0995R2 = 0.9888
y = 1.0018x + 1.6592R2 = 0.9978
y = 0.9949x + 4.5541R2 = 0.9943
0
50
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200
250
300
0.0 100.0 200.0 300.0
DSC onset
Nan
oTA
Der
iv O
nset
0.1°C/s1°C/s10°C/s
Slopes: 0.995- 1.002Offsets: +2 to +7ºC
Data courtesy of G. Meyers and A. Pasztor, DOW
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Example Applications• Thermal analysis can enable localized identification of
components in blends, composites, multilayers
• Detection of material changes caused by wear, defects, UV exposure, etc.
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Advantages over bulk thermal analysis
• Conventional AFM images with sub-30nm spatial resolution
• Thermal analysis on heterogeneous samples with sub-100 nm resolution
• Local heating to over 500 C at heating rates up to 600,000˚ C/min– Eliminates thermal drift issues that plague bulk sample heating
approaches– Provides much faster sample throughput
• Map the temperatures across the sample with a resolution of <0.1 ºC
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Sample: Toner particles embedded in epoxy and microtomedShown below is a 15 x 7.5 µm topographic scan of toner particles embedded in epoxy and microtomed. To the left are the corresponding nano-TA scans.
Toner ParticleCenter RegionMiddle layer Outer layerEpoxy
74.3 ºC
70.4 ºC
60.4 ºC
Toner Particles
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Data averaged from 3 lenses
The AFM images reveal different microstructures
and the nano-TMA results show very different behavior through the glass
transition
Lens ALens BLens C
Contact Lens
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instrumentsanasysData courtesy of M. Reading, D Craig and L. Harding, UEA
The existence of different solid-state forms such as polymorphs, solvates, hydrates, and amorphous form in pharmaceutical drug substances and excipients have downstream consequences in drug products and biological systems
Nanoscale Drug Analysis
Crystalline only Crystalline and amorphousIndomethacin
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•AFM image with simultaneous nanoscale temperature metrology
Scanning Thermal Microscopy
Magnetic recordinghead
Epoxy composite
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Brightfield Optical Microscope
XY Stage
Laser Detection System
Thermal Probe
Sample
Point & Click Nanothermal Analysis
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An optical image and nano-TA measurement on the four layers in a multilayer film composed of Nylon, PET and two forms of low density polyethylene.
94˚ C
88˚ C
180˚ C 218˚ C++ +
+
Multilayer Film
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• Nano-TA extends the capabilities of the AFM by adding localized thermal analysis for localized identification of components and material forms in nanoscale polymers, pharmaceuticals and devices
• Scanning Thermal Microscopy can map thermal conductivity and temperature distributions
• New instruments allow rapid, automated, easy to use localized thermal analysis in environments ranging from R&D to process quality control
Summary
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Backup
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NanoTA AFM accessory
New DSP based control electronics and software have been designed to more accurately control the nano-TA probes with faster ramping and improved signal to noise. This controller is an accessory that operates on most commercial SPMs.