Thermal Analysis Excellence

Flash DSC1
STARe System
Innovative Technology
Versatile Modularity
Swiss Quality

Flash Differential Scanning Calorimetry

for Research and Development

Flash DSC Excellence

A Quantum Leap in Innovation

Opens up New Frontiers
Differential Scanning Calorimetry, DSC, is the most important method in thermal analysis.
It measures the heat flow to or from a sample as a function of temperature or time and
thereby allows physical transitions and chemical reactions to be quantitatively measured.
The Flash DSC1 revolutionizes rapid-scanning DSC. The instrument can analyze reorganization processes that
were previously impossible to measure. The Flash DSC1 is the ideal complement to conventional DSC. Heating
rates now cover a range of more than 7 decades.
Features and benefits of the Flash DSC1:
n Ultra-high cooling rates allow materials with defined structural properties to be prepared
n Ultra-high heating rates reduce measurement times and suppress reorganization processes
n Fast response sensor enables the kinetics of extremely fast reactions or crystallization processes to be studied
n High sensitivity low heating rates can also be used; scan rates overlap with those of conventional DSC
n Wide temperature range measurements can be performed in the range -95 to 450 C
n User-friendly ergonomics and functionality sample preparation is quick and easy

The Flash DSC1 allows you to prepare samples with

defined structures such as occur during rapid cooling
in injection molding processes. The application of different cooling rates influences the crystallization behavior and structure of the sample.
The use of high heating rates enables materials to be
analyzed without interference from reorganization processes there is no time for such processes to occur.
The Flash DSC1 is also the ideal tool for studying
crystallization kinetics.

The heart of the Flash DSC1 is

the chip sensor based on MEMS
technology.
MEMS: Micro-Electro-Mechanical Systems
2

MEMS-Based DSC Sensor Technology

Unsurpassed Heating and Cooling Rates
In conventional DSC instruments, the sample is measured in a crucible in order to protect the sensor. The heat capacity and thermal conductivity of the crucible however have
a significant influence on the measurement. In the Flash DSC1, the sample is placed directly onto the MultiSTAR chip sensor. The patented dynamic power compensation control
circuit allows measurements to be performed with minimum noise level at high heating
and cooling rates.
MultiSTAR UFS1 Sensor
The Full Range UFS1 sensor has 16 thermocouples and exhibits high sensitivity and excellent
temperature resolution. The MEMS chip sensor is mounted on a stable ceramic substrate with
electrical connections.
Sensitivity
The high sensitivity results from the use of 16 thermocouples, 8 each on the sample and reference sides. The thermocouples are arranged symmetrically around the sample measurement area in the form of a star so that temperatures are measured with great accuracy. The
outstanding sensitivity means that measurements can also be performed at low heating and
cooling rates.
Temperature resolution
The temperature resolution is determined by the time constant of the sensor. The smaller the
time constant, the better close-lying thermal effects can be separated. The time constant of
the Flash DSC1 is about 1 millisecond or about 1000 times less than that of a conventional
DSC instrument.
Baseline
The revolutionary multiple temperature measurement around the sample guarantees excellent
accuracy. The high degree of symmetry of the differential sensor results in flat and extremely
reproducible baselines.

Reusable chip sensors

Samples are positioned directly on
the sensor. Used sensors can be
stored in the chip sensor box supplied so that further measurements
can be performed later on if
needed.
It takes less than a minute to
change a sensor.

Swiss Quality

Flash DSC1 from METTLER TOLEDO

the Fastest Commercial DSC

Sensor environment
The sensor support is heatable. In
the low-temperature operation, the
sensor support can be brought to
room temperature before the sensor
is inserted. This prevents the gold
contact pins from icing over.

Terminal
The large easy-to-read color touchscreen terminal at
the front of the Flash DSC1 indicates the status of the
instrument. If the instrument is not next to your PC,
you can enter individual sequences and queries directly via the terminal.

Complete thermal analysis system

A complete thermal analysis system comprises four different measurement techniques. Each characterizes the
sample in a different way. The combination of all the results simplifies interpretation. Besides heat flow measurements using DSC or Flash DSC, the other instruments measure weight loss (TGA), change in length (TMA) or the
mechanical modulus (DMA). All these quantities change as a function of temperature.

DSC

Flash DSC

TGA

TMA

DMA

Ergonomic Perfection
Is What Customers Value
Perfect ergonomics
The preparation and insertion of a
sample is performed sitting comfortably in front of the instrument.
The sample is first cut to size on a
small glass microscope slide
placed over the sensor. A suitable
sample specimen is then transferred directly to the sensor and positioned using a hair.

AGC Thermal
Book 20%
Cyan
Analysis

Sample preparation
Sample preparation is carried out
using a microscope. The microscope is also used to accurately
position the very small sample
specimen on the sensor.

Application
Handbook

Thermal Analysis in Practice

Collected Applications

Important support services

METTLER TOLEDO prides itself in supplying outstanding instruments together with the support needed for you
to be successful in your field of work. Our well-trained engineers are ready to help you in any way possible:
Service and maintenance
Calibration and adjustment
Training and application advice
Equipment qualification
METTLER TOLEDO also provides comprehensive literature on thermal analysis applications.

Innovation

Unbelievable Performance
Leads to New Results
Measurement principle
High heating or cooling rates are
only possible when the sample is
sufficiently small and is in good
thermal contact with the sensor.
In the first heating run, the sample
melts. Thermal contact with the
sensor is thereby greatly improved.
Defined sample structures can then
be produced by varying the cooling
rate over a wide range.

Temperature

Sample
preparation

Formation of sample
structure

Analysis

Melting of the
sample optimizes thermal
contact.

Different cooling rates allow defined sample structures to be formed.

High heating rates

suppress the reorganization of the sample. It
can therefore be measured as received.

Time

In the second heating run, the

sample has no time to reorganize
because of the very high heating
rates. The enormous range of cooling and heating rates allow many
different sample structures to be
measured in one experiment.

Chip sensor principle

The sample and reference sides of
the sensor each have two thermal
resistance heaters which together
generate the desired temperature
program. The smaller heater is for
compensation control (dynamic
compensation control). The heat
flow is measured using the two
sets of 8 thermocouples arranged
symmetrically around the measurement area on the sample and reference sides of the sensor.

1. Ceramic plate
2. Silicon frame
3. Connecting wire

4 Resistance heater
5. Aluminum plate (sample area)
6. Thermocouple

Homogeneous temperature distribution
The sample measurement area of the chip sensor is made of silicon
nitride and silicon dioxide coated with a thin layer of aluminum. This
provides in an extremely homogeneous temperature distribution across
the sensor. The small active measurement area is approximately
2.1 m thick so that the time constant is mainly determined by the
sample.

Optimized Evaluation Software

Brings Efficiency into the Laboratory
Software support
In a typical Flash DSC experiment,
the measurement results are analyzed as a function of the heating
or cooling rate or the isothermal
time. The experiment is usually
performed very quickly. Sample
preparation needs somewhat more
time. Evaluation and interpretation
takes longest but is at the same
time the most interesting part of
the work.

The STARe software has been expanded to include new requirements. For example, complex measurement programs are set up
within a few minutes and large
numbers of curves can be efficiently evaluated.

n Selection of curve segments On opening the measurement,

you choose only the curve segments of interest.
n Multicurve evaluation Select the curves, click the evaluation
and the individual results are immediately available.
n Rapid set up of function table with fit functions Activate the
result line: One click copies all the selected results into a table.
Now choose the fit function and the evaluation is completed.

Reorganization of polyethylene terephthalate (PET)

Many polymers exhibit reorganization effects in the DSC measurement curve when they are heated. The curve
does not therefore show the melting of the crystallites originally present in the sample. This is demonstrated using a sample of PET that had been allowed to crystallize at 170 C for 5 min before cooling to room temperature.
The measurement curves at heating rates between 0.2 K/s and 1000 K/s show two peaks. The peak at lower
temperatures shifts to higher temperatures with increasing heating rate (blue arrow). This peak occurs when the
original crystallites melt. The high-temperature peak shifts to lower temperatures (red arrow). This peak is due to
the melting of crystallites produced through reorganization during the measurement. Only one peak is observed
at 1000 K/s. Practically no reorganization occurs from this heating rate onward.

Modularity and Expansion

Many Options
Microscope options
You can adapt the microscope attachment according
to your needs. There are two options:
1. Not modular, but excellent value
2. Modular, with adjustable viewing angle, different illumination possibilities, and cameras.

ErgoModule

Camera kit

Binocular ErgoTube

ErgoTube 45

Binocular tube 45

ErgoWedge

Camera kit

M50 (Step)

ErgoWedge

Video module

Filter slide housing

Video/photo tube

M60 (Zoom)

Video/photo tube

Light housing

M80 (Zoom)

Temperature range and cooling options

The IntraCooler is an electrical cooling device with a closed-loop cooling system. The vaporized coolant
is liquefied by means of compressors and heat exchangers.
Three temperature ranges are available:
Air cooling:

RT 450 C

IntraCooler (1 stage)

-35 450 C

IntraCooler (2 stage)

-95 420 C

Efficiency
Thanks to Practical Accessories
Chip sensor box
Since the chip sensors can only be
used for one sample, it is a good
idea to store them safely just in
case you want to make more measurements afterward with the same
sample. This avoids having to use
a new sensor. Up to ten chip sensors with adhering sample material
can be stored in the sensor box for
experiments later on.

Standard accessories
The following tools needed to
prepare thin layers are supplied
with the instrument as standard
equipment:
knife with spare blades
lancet-shaped needle
tweezers
leather cloth
grinding stone
brush
hair holder
glass support and
indium for calibration

Microtome (optional accessory)

The microtome can be used to cut 10 to 30 m thick layers of a material, for example from small pieces of a
polymer granule. The layers are then cut to small sample specimens for analysis using the knife supplied.

Application Power

New Materials for the Future

Flash DSC Has the Answers
The Flash DSC1 is the ideal addition for characterizing modern materials and optimizing
production processes by thermal analysis.

Polymers, polymorphic substances, and many composites and

blends have metastable structures
that depend on the cooling conditions used in their production. On
heating, reorganization processes
such as the melting and recrystallization of unstable crystallites or the
separation of phases may occur.
The influence of reorganization on
the heating curve can be analyzed
by varying the heating rate.

Fast measurements save time in

the analysis and development of
materials. The quality of products
can be improved through knowledge of structure formation at actual process cooling rates.
The data can be used for simulation calculations and to optimize
production conditions.

Flash DSC can simulate technical

processes in which rapid cooling
occurs. This yields information
about the effect of additives (e.g. nucleating agents) under near-process
conditions. Isothermal measurements provide information on the kinetics of transitions and reactions
that take place in a few seconds.

Application Possibilities of Flash DSC

Detailed analysis of processes involving the formation of structure in materials
Direct measurement of rapid crystallization processes
Determination of the reaction kinetics of fast reactions
Investigation of the mechanism of action of additives under near-production conditions
Comprehensive thermal analysis of materials in very short time
Analysis of very small sample amounts
Determination of data for simulation calculations

10

Melting of indium at
different heating rates
The melting of indium (1 g) was measured at different heating rates between
0.05 K/s and 10000 K/s. As in conventional DSC, the conduction of heat between the
sensor and the sample (thermal lag) influences the measured onset temperature, Ton.
Without correction, Ton increases linearly
with the heating rate. The same is true for
the Flash DSC1.
To accommodate the large heating rate
range, the abscissa is displayed logarithmically in the diagram. For this reason, the
linear function appears as a curve (blue).

Crystallization of isotactic
polypropylene (iPP) on cooling
In technical processes such as injection
molding, the molding materials are cooled
at several hundred K/s. To optimize their
properties, it is important to have information about the crystallization behavior at
these high rates. This information can be
obtained from Flash DSC cooling experiments as shown in the upper diagram.
The lower diagram displays the crystallization peak temperature of isotactic polypropylene (iPP) as a function of the cooling
rate. The peak temperature shifts to lower
temperatures at higher cooling rates.
A conventional DSC1 (red points) was used
for cooling rates between 0.1 K/min and
60 K/min (0.0017 K/s and 1 K/s) and the
Flash DSC1 for rates between 0.5 K/s and
1000 K/s. The peak temperatures agree
with one another in the region where the
cooling rates of the instruments overlap.
Above 50 K/s, the formation of the mesophase is observed at about 30 C in a second crystallization process (blue points).
At cooling rates above 1000 K/s, no crystallization occurs. The material remains
amorphous with a glass transition at
about -10 C.
The complete crystallization behavior is
measured by the Flash DSC1 in less
than 30 min.

11

Reorganization of amorphous iPP

Amorphous isotactic polypropylene (iPP) is
produced by cooling from the melt at
4000 K/s. The material obtained was measured at heating rates between 5 K/s and
30000 K/s. The glass transition occurs just
below 0 C followed by an exothermic peak
due to cold crystallization. The crystallites
melt above 100 C.
At higher heating rates, the cold crystallization peak is shifted to higher temperatures
and melting peak to lower temperatures.
From 1000 K/s onward, the peak areas become significantly smaller until at 30000
K/s reorganization no longer occurs in the
sample.

Isothermal crystallization of iPP

To measure the isothermal crystallization
behavior of isotactic polypropylene (iPP),
the melt was first cooled to different crystallization temperatures between 110 C and
-20 C at 2000 K/s. No formation of structure occurs under these conditions.
Afterward, the crystallization process was
measured isothermally. The exothermic
crystallization peaks have their peak maximum at times between 0.05 s and 10 s.
The reciprocal peak time is a measure of
the crystallization rate and is displayed as a
function of the crystallization temperature.
The resulting curve exhibits a maximum at
about 20 C. At these low temperatures,
crystallization takes place very rapidly. The
crystallization process involves homogeneous nucleation.
The measurement curves also show the
change of crystallization kinetics with temperature.

12

Nanofillers in PA
The properties of polyamide 11 (PA 11) can
be optimized through the addition of
nanoparticles and the use of suitable processing conditions (e.g. for the injection
molding of gearwheels). The effect of the
fillers at the actual cooling rates influences
the size of the crystallites and hence the
mechanical properties.
Three PA 11 samples with nanofiller contents of 0%, 2.5% and 5% were measured
at different cooling rates in the Flash DSC1
and in a conventional DSC1. The enthalpy
of crystallization at low cooling rates is
constant up to 50 K/s, but becomes smaller
at higher cooling rates. At 200 K/min, the
sample no longer crystallizes.
The influence of the cooling rate on the effect of the filler become clear when the peak
temperatures are displayed as a function of
the cooling rate. At cooling rates below
0.3 K/s (20 K/min), the unfilled PA 11 crystallizes first. At the technologically important
high cooling rates, this changes and the
nanoparticles accelerate crystallization.

Melting and decomposition

of organic substances
The determination of the melting behavior
of organic substances is difficult if decomposition occurs in the melting range.
At high heating rates, the decomposition reaction shifts to higher temperatures and
separation of the two effects becomes possible. This is shown using saccharin as an
example.
At heating rates between 50 K/s and
100 K/s, melting and decomposition overlap. At higher heating rates, the two effects
are separated.

13

Flash DSC1 Specifications

Temperature data
Temperature range

Air cooling

(Room temperature + 5 K) 500C

IntraCooler (1-stage)

-35C 450C

IntraCooler (2-stage)

-95C 420C

Cooling rates (typical)

-6 K/min. (-0.1 K/s) -240000K/min (-4000 K/s)

Heating rates (typical)

30 K/min. (0.5 K/s) 2400000K/min (40000 K/s)

Sensor data
Sensor material

Ceramic

Thermocouples

16

Signal time constant, nitrogen

0.001s

Sample size

10 ng 1 g

DSC Sensor
Sensor type

Ultra-fast-sensor 1st generation

Pmax heat flow signal

20 mW

Noise heat flow signal

rms < 0.5 W (typical)

Isothermal drift heat flow signal

< 5 W/h (typical)

Baseline drift heat flow signal (empty sensor)

< 100 W/h (typical)

Terminal
Touch control

Color TFT, VGA 640 x 480 pixel

Signal generation
Resolution

0.005 K (0C 250C)

0.01 K (-100C 400C)

Signal detection
Sampling rate

Max. 10 kHz (10000 points per second)

Resolution of temperature signal

2.5mK

Noise temperature signal

rms < 0.01K (typical)

Communication
With personal computer (PC)

Ethernet

Dimensions
Instrument dimensions (width x depth x height)

45 cm x 60 cm x 50 cm

Approvals
IEC/EN61010-1:2001, IEC/EN61010-2-010:2003
CAN/CSA C22.2 No. 61010-1-04
UL Std No. 61010A-1
EN61326-1:2006 (class B)
EN61326-1:2006 (industrial environments)
FCC, Part 15, class A
AS/NZS CISPR 22, AS/NZS 61000.4.3
Conformity mark: CE

www.mt.com
For more information

Mettler-Toledo AG, Analytical

CH-8603 Schwerzenbach, Switzerland
Tel. +41 44 806 77 11
Fax +41 44 806 73 60

Subject to technical changes

09/2010 Mettler-Toledo AG
51725315, Printed in Switzerland
Marketing MatChar / MarCom Analytical

Quality certificate. Development, production

and testing according to ISO 9001.

Environmental management system

according to ISO 14001.
European conformity. The CE conformity
mark provides you with the assurance that
our products comply with the EU directives.