brochure flash

7/26/2019 Brochure Flash

1/14

ThermalAnalysisExcellence

Flash DSC 1

STAReSystem

Innovative Technology

Versatile Modularity

Swiss Quality

Flash Differential Scanning Calorimetry

for Research and Development


2/142

Fla

shDSCExcellence 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.

Features and benefits of the Flash DSC 1:

nUltra-high cooling rates allow materials with defined structural properties to be prepared

nUltra-high heating rates reduce measurement times and suppress reorganization processes

nFast response sensor enables the kinetics of extremely fast reactions or crystallization processes to be studied

nHigh sensitivity low heating rates can also be used; scan rates overlap with those of conventional DSC

nWide temperature range measurements can be performed in the range -95 to 450 C

nUser-friendly ergonomics and functionality sample preparation is quick and easy

The Flash DSC 1 allows you to prepare samples with

defined structures such as occur during rapid cooling

in injection molding processes. The application of dif-

ferent cooling rates influences the crystallization be-

havior and structure of the sample.

The use of high heating rates enables materials to be

analyzed without interference from reorganization pro-

cesses there is no time for such processes to occur.

The Flash DSC 1 is also the ideal tool for studying

crystallization kinetics.

The heart of the Flash DSC 1 is

the chip sensor based on MEMStechnology.

MEMS: Micro-Electro-Mechanical Systems

The Flash DSC 1 revolutionizes rapid-scanning DSC. The instrument can analyze reorganization processes that

were previously impossible to measure. The Flash DSC 1 is the ideal complement to conventional DSC. Heating

rates now cover a range of more than 7 decades.


3/143

MEMS-Based DSC Sensor Technology

Unsurpassed Heating and Cooling Rates

Reusable chip sensors

Samples are positioned directly onthe sensor. Used sensors can be

stored in the chip sensor box sup-

plied so that further measurements

can be performed later on if

needed.

It takes less than a minute to

change a sensor.

In conventional DSC instruments, the sample is measured in a crucible in order to pro-tect the sensor. The heat capacity and thermal conductivity of the crucible however have

a significant influence on the measurement. In the Flash DSC 1, the sample is placed di-

rectly 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 UFS 1 Sensor

The Full Range UFS 1 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 ref-

erence sides. The thermocouples are arranged symmetrically around the sample measure-

ment 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 DSC 1 is about 1 millisecond or about 1 000 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.


4/144

TGADSC Flash DSC TMA DMA

Flash DSC 1 from METTLER TOLEDO

the Fastest Commercial DSC

SwissQua

lity

Complete thermal analysis system

A complete thermal analysis system comprises four different measurement techniques. Each characterizes thesample in a different way. The combination of all the results simplifies interpretation. Besides heat flow measure-

ments 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.

Terminal

The large easy-to-read color touchscreen terminal at

the front of the Flash DSC 1 indicates the status of the

instrument. If the instrument is not next to your PC,

you can enter individual sequences and queries direct-

ly via the terminal.

Sensor environment

The sensor support is heatable. Inthe 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.


5/145

AGCBook20%C

yan

Thermal Analysis in Practice

Collected Applications

ThermalAnalysis

Application

Handbook

Perfect ergonomics

The preparation and insertion of a

sample is performed sitting com-

fortably 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 trans-

ferred directly to the sensor and po-

sitioned using a hair.

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.

Ergonomic Perfection

Is What Customers Value

Sample preparation

Sample preparation is carried out

using a microscope. The micro-

scope is also used to accurately

position the very small samplespecimen on the sensor.


6/146

Innovation

Unbelievable Performance

Leads to New Results

Measurement principleHigh 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.

In the second heating run, the

sample has no time to reorganize

because of the very high heating

rates. The enormous range of cool-

ing 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 measure-ment area on the sample and refer-

ence sides of the sensor.

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 thesample.

Melting of the

sample opti-

mizes thermal

contact.

Different cooling rates al-

low defined sample struc-

tures to be formed.

High heating rates

suppress the reorgani-

zation of the sample. It

can therefore be mea-sured as received.

Temperature

Sample

preparation

Formation of sample

structure

Analysis

Time

1. Ceramic plate

2. Silicon frame3. Connecting wire

4 Resistance heater

5. Aluminum plate (sample area)6. Thermocouple


7/147

nSelection of curve segments On opening the measurement,

you choose only the curve segments of interest.

nMulticurve evaluation Select the curves, click the evaluation

and the individual results are immediately available.

nRapid 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.

Optimized Evaluation Software

Brings Efficiency into the Laboratory

Software supportIn a typical Flash DSC experiment,

the measurement results are ana-

lyzed 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 STAResoftware has been ex-

panded to include new require-

ments. For example, complex mea-

surement programs are set up

within a few minutes and large

numbers of curves can be efficient-

ly evaluated.

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 us-

ing 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 1 000 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 1 000 K/s. Practically no reorganization occurs from this heating rate onward.


8/148

M80 (Zoom)M50 (Step) M60 (Zoom)

Camera kitCamera kit Video/photo tube

ErgoTube 45Binocular tube 45 Binocular ErgoTube

ErgoModule ErgoWedge ErgoWedge Filter slide housing Video/photo tube

Video module Light housing

Modularity and Expansion

Many Options

Microscope optionsYou 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 il-

lumination possibilities, and cameras.

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 CIntraCooler (1 stage) -35 450 C

IntraCooler (2 stage) -95 420 C


9/149

Efficiency

Thanks to Practical Accessories

Chip sensor boxSince 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 mea-

surements afterward with the same

sample. This avoids having to use

a new sensor. Up to ten chip sen-

sors with adhering sample material

can be stored in the sensor box for

experiments later on.

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.

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


10/1410

ApplicationPower

New Materials for the Future

Flash DSC Has the Answers

The Flash DSC 1 is the ideal addition for characterizing modern materials and optimizing

production processes by thermal analysis.

Polymers, polymorphic substanc-es, and many composites and

blends have metastable structures

that depend on the cooling condi-

tions used in their production. On

heating, reorganization processes

such as the melting and recrystalli-

zation 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.

Flash DSC can simulate technical

processes in which rapid cooling

occurs. This yields information

about the effect of additives (e.g. nu-

cleating agents) under near-process

conditions. Isothermal measure-

ments provide information on the ki-

netics of transitions and reactions

that take place in a few seconds.

Fast measurements save time inthe analysis and development of

materials. The quality of products

can be improved through knowl-

edge of structure formation at actu-

al process cooling rates.

The data can be used for simula-

tion calculations and to optimize

production conditions.

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


11/1411

Melting of indium atdifferent heating ratesThe melting of indium (1 g) was mea-

sured at different heating rates between

0.05 K/s and 10 000 K/s. As in convention-

al DSC, the conduction of heat between the

sensor and the sample (thermal lag) influ-

ences the measured onset temperature, Ton.

Without correction, Tonincreases linearly

with the heat ing rate. The same is t rue for

the Flash DSC 1.

To accommodate the large heating rate

range, the abscissa is displayed logarithmi-

cally in the diagram. For this reason, the

linear function appears as a curve (blue).

Crystallization of isotacticpolypropylene (iPP) on coolingIn 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 informa-

tion about the crystallization behavior at

these high rates. This information can be

obtained from Flash DSC cooling experi-

ments as shown in the upper diagram.

The lower diagram displays the crystalliza-tion peak temperature of isotactic polypro-

pylene (iPP) as a function of the cooling

rate. The peak temperature shifts to lower

temperatures at higher cooling rates.

A convent ional DSC 1 (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 DSC 1 for rates between 0.5 K/s and

1 000 K/s. The peak temperatures agree

with one another in the region where the

cooling rates of the inst ruments overlap.

Above 50 K/s, the formation of the meso-

phase is observed at about 30 C in a sec-

ond crystallization process (blue points).

At cooling rates above 1 000 K/s, no cr ys-

tallization occurs. The material remains

amorphous with a glass transition at

about -10 C.

The complete crystallization behavior is

measured by the Flash DSC 1 in less

than 30 min.


12/1412

Reorganization of amorphous iPPAmorphous isotactic polypropylene (iPP) is

produced by cooling from the melt at

4 000 K/s. The material obtained was mea-

sured at heating rates between 5 K/s and

30 000 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 crystalliza-

tion peak is shifted to higher temperatures

and melting peak to lower temperatures.

From 1 000 K/s onward, the peak areas be -

come significantly smaller until at 30 000

K/s reorganization no longer occurs in the

sample.

Isothermal crystallization of iPPTo measure the isothermal crystallization

behavior of isotactic polypropylene (iPP),

the melt was first cooled to different crystal-

lization temperatures between 110 C and

-20 C at 2 000 K/s. No formation of struc-

ture occurs under these conditions.

Afterward, the crystallization process was

measured isothermally. The exothermic

crystallization peaks have their peak maxi-

mum 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 homoge-

neous nucleation.

The measurement curves also show the

change of crystallization kinetics with tem-

perature.


13/1413

Nanofillers in PAThe properties of polyamide 11 (PA 11) can

be optimized through the addition of

nanoparticles and the use of suitable pro-

cessing 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 con-

tents of 0%, 2.5% and 5% were measured

at different cooling rates in the Flash DSC 1

and in a conventional DSC 1. 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 ef-

fect 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 crys-

tallizes first. At the technologically important

high cooling rates, this changes and the

nanoparticles accelerate crystallization.

Melting and decompositionof organic substancesThe determination of the melting behavior

of organic substances is difficult if decom-position occurs in the melting range.

At high heating rates, the decomposit ion re-

action shifts to higher temperatures and

separation of the two effects becomes pos-

sible. This is shown using saccharin as an

example.

At heat ing rates between 50 K/s and

100 K/s, melting and decomposition over-

lap. At higher heating rates, the two eff ects

are separated.


14/14

www.mt.com

Flash DSC 1 Specifications

Temperature data

Temperature range Air cooling (Room temperature + 5 K) 500 C

Int raCooler (1-stage) -35 C 450 C

Int raCooler (2-s tage) -95 C 420 C

Cooling rates (typical) -6 K/min. (-0.1 K/s) -240 000 K/min (-4 000 K/s)Heating rates (typical) 30 K/min. (0.5 K/s) 2 400 000 K/min (40 000 K/s)

Sensor data

Sensor material Ceramic

Thermocouples 16

Signal time constant, nitrogen 0.001 s

Sample size 10 ng 1 g

DSC Sensor

Sensor type Ultra-fast-sensor 1stgeneration

Pmaxheat 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 (0 C 250 C)

0.01 K (-100 C 400 C)

Signal detection

Sampling rate Max. 10 kHz (10 000 points per second)

Resolution of temperature signal 2.5 mK

Noise tempera ture signal rms < 0.01 K (typical)

Communication

With personal computer (PC) Ethernet

Dimensions

Ins trument d imensions (wid th 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

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.

brochure flash

Documents