Transition Temperature Microscopy Localized Thermal Analysis

Revolutionary Nano- and Micro-Scale Thermal Analysis PLUS Imaging…
At the Push of a Button
2008 Winner
Transition Temperature Microscopy
Localized Thermal Analysis
Nano Thermal Analysis
Reveal what you have been missing
The VESTA is the world’s first “point and click” instrument for localized thermal property measurement and
Transition Temperature Microscopy. This R&D100 Award winning technology uses a nanoscale thermal probe to
locally heat samples to measure and map thermal transition temperatures and other thermal properties. Transition
Temperature Microscopy gives critical information on samples from the scale of millimeters to nanometers and
provides information that is not obtainable by any other technique. Easy to learn and operate, the VESTA allows you
to move beyond bulk thermal anaysis to see the critical information you’ve been missing.
When Bulk Thermal Analysis Isn’t Enough…
Bulk thermal analysis provides widely used techniques for materials analysis. But bulk techniques like DSC, TMA, DMA and others are limited to
measuring average or aggregrate properties of the entire sample. This masks critical variations in material properties that can have a huge impact on
material performance. Materials and pharmaceutical developers increasingly need information about the spatial variation of thermal properties to
engineer materials with desired properties. Bulk thermal analysis is also difficult to apply to thin films and coatings, where the underlying substrate
may complicate or render bulk measurements impractical. …Add the easy to use VESTA to your analytical capabilities.
Localized Thermal Analysis (LTA)
The sample is heated locally with a thermal
probe and the localized thermal transition
temperature is measured via thermo mechanical
analysis (TMA). This is shown to the right in Fig 1
where the plot shown is the physical deflection
of the thermal probe versus its temperature.
Tip engages to surface
Tip heating
Measure local thermal transitions
Fig 1. Localized Thermal Analysis can provide glass and melting transition
temperatures on the sub 100 nm scale.
Point and Click Operation
VESTA is easy to use. Locate a region of interest on
the video microscope image and then click to
start a local thermal analysis. Measurement
data appears in seconds. You can even program
an array of points for automatic and unattended
operation.
Transition Temperature
Microscopy (TTM)
A TTM Image is obtained by plotting the localized
tansition temperatures at different points on the
sample. You simply select the region on your
optical microscope image on which you’d like a
TTM image and the VESTA automatically
proceeds to create the image. This powerful
new form of microscopy enables you to identify
localized thermal inhomogeneities on the
sample surface that cannot be identified by
conventional forms of microscopy and bulk
thermal analysis.
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218Û C
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60 80 100 120 140 160 180 200 220 240
Fig 2. The VESTA’s video microscope supports point and click local thermal analysis.
Video image (L) and LTA measurements (R) on multi-layer polymer film.
Automatically identify
transition temp.
Color code phase
transitions into map
pixel by pixel
TTM image shows transition
temperature variations
Fig 3. Transtion Temperature Microscopy (TTM) maps local variations in thermal
transitions.
Example Applications
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Applications of Localized Thermal Analysis / Transition Temperature Microscopy (TTM)
--The VESTA works on a wide variety of samples to provide you critical information needed to be successful.
Optical microscope image showing
a ring like artifact around microfibers
TTM Image (100um*100um)
identifies artifact
Distribution of
Transition Temperatures
Polymer blends. TTM allows
mapping of components on the basis of
their transition temperatures. The image
above is a Tg map of a blend of
polystyrene and PMMA.
Identification of Processing Artifacts: The optical microscopy image revealed a skin around
the microfibers which was an artifact that formed during the microfiber embedding process, but could not
identify the artifact. The TTM image determined that it was the use of 'aged' epoxy resin monomer and catalyst
that had hydrolyzed during storage and led to this formation.
Characterization of Multilayers from Flat
Panel Displays:
Understanding the effect of morphology and
composition on the optical properties of the
micron-sized layers present in LCD flat panel displays
is critical to understanding their performance. TTM
successfully identified the thermal properties of
individual layers, as well as the presence of gradients
within individual layers and interfaces that were not
detected by the optical image.
Pharmaceuticals. Transition
Temperature Microscopy image of a mix
of paracetamol and HPMC. TTM reveals
the drug particles (dark blue) by its
thermal transition.
Pharmaceutical applications are a special challenge for
conventional bulk analysis. Many modern pharmaceutical
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very different thermal properties. Even single drug
formulations may have a variety of different polymorphs,
solvates, hydrates, etc. Bulk thermal analysis masks these
inhomogeneities and makes it challenging to engineer the
most highly effective pharmaceutical materials. The VESTA
allows you to locally map and distinguish drug polymorphs
and other material variations to give you the information you
need to understand and control your process. VESTA also
provides temperature ramp rates thousands of times faster
than bulk thermal analysys and can prevent recrystallization
events that mask your sample’s true composition.
7
Localized nanoscale thermal analysis
6
5
Defect
111 °C
4
3
2
Matrix
92 °C
1
0
-1
50µm
Deflection V
Focus on Pharma
Optical Microscopy Image
of Polymers with gel formation
-2
-3
Phase Transition Temperature
-4
-5
50
55
60
65
70
75
80
85
90
95
100 105 110 115 120 125 130
Identifying defects such as gels: Haze or visible defects negatively impact the
optical clarity of packaging materials. In these cases, it is important to know if the haze or
defects are caused by gel particles (higher melting temperature material) or an external
contaminant. The LTA data confirms the source of the haze in this example as gel particles.
Customers Testimonials for Local Thermal Analysis
I use the LTA technique routinely and have found it to be very
useful in applications where interfacial properties are difficult
to access, such as for weathering, thin films or multilayer
systems where DSC can only provide average thermal
properties and cannot differentiate the surface or particulate
VESTA is the first tool to enable bulk thermal analysis users to
make local thermal property measurements with ease of use
through push button control.
Dr. Jiping Ye
Nissan Analytical Research
from the matrix.
Dr. L.T.Germinario
Eastman Chemical
System Specifications:
Temp. Ramp Rate:
Max. Controllable Temp. of Probe:
Thermal Probe Radius:
XY Stage Range:
Z Stage Range:
Z Piezo Range:
Spatial Resolution (optics):
Sample Size:
Up to 600,000°C /min
450°C
<30 nm
12 mm x 8 mm
8 mm
>10 µm
~1.5 µm
≤40 mm dia.
Feature
Benefit
Point and click thermal analysis
Measurements with minimal training time
Localized Thermal Analysis
Material characterization within a heterogeneous sample
Transition Temperature Microscopy (TTM)
Automatically identify/map thermal inhomogeneities
Probe heatable up to 450 °C
Covers transition temperatures of most organic materials
Temperature ramp rate of up to 600,000 °C/min
High throughput, avoid recrystallization during heat ramps
Thermal probe radius of 30nm
Local thermal analysis on sub 100-nm scale
121 Gray Avenue, Suite 100
Santa Barbara, CA 93101
www.anasysinstruments.com
Tel: 805-730-3310
Fax: 805-730-3300