NETZSCH DSC 404 F1 thermal analysis system with digital display and sample holders for precise material testing.
differential scanning calorimetry

DSC 404 F1 Pegasus®

High-Temperature DSC up to 2000°C

Highlights

Fascinating Flexibility in Thermal Analysis 

The DSC 404 F1 Pegasus®, High-Temperature Differential Scanning Calorimeter, is designed for the exact determination of specific heat of high-performance materials at high temperatures.

The concept of the DSC 404 F1 Pegasus® allows configuration for up to seven different furnace types, easily interchangeable by the user, for a wide temperature range within -150°C to 2000°C (please see accessories). 

We offer diverse sensors for DSC and DTA measurements, various crucible types as well as a great variety of technical accessories.

The coupling to a FT-IR or MS is possible without problems.

An important hardware extension, like the automatic sample changer (ASC) for up to 20 sample and reference crucibles, and software features, such as BeFlat® for an optimized baseline or the optional temperature modulation of the DSC signal (TM-DSC) make the DSC 404 F1 Pegasus® the most versatile DSC system for research & development, quality assurance, failure analysis and process optimization.

NETZSCH at the Max-Planck Institute

How is the Max-Planck Institute for Chemical Physics of Solids using the NETZSCH DSC 404 Pegasus®??

Method

The DSC 404 F1 Pegasus® comprises a high-capacity heat flux DSC for highly sophisticated application measurements:

The DSC 404 F1 as well as the F3 Pegasus® systems operate according to the heat flux principle. With this method, a sample and a reference are subjected to a controlled temperature program (heating, cooling or IsothermalTests at controlled and constant temperature are called isothermal.isothermal). The actual measured properties are the temperature of the sample and the temperature difference between sample and reference. From the raw data signals, the heat flow difference between sample and reference can be determined.

Diagram illustrating a thermal analysis setup with a furnace, sample, reference material, and temperature measurement.
More on the Functional Principle of a Heat-Flux DSC

A DSC measuring cell consists of a furnace and an integrated heat-flux sensor with designated positions for the sample and reference pans.

The sensor areas are connected to thermocouples or may even be part of the thermocouple. This allows for recording both the temperature difference between the sample and reference side (DSC signal) and the absolute temperature of the sample or reference side.

Due to the heat capacity (cp) of the sample, the reference side (usually an empty pan) generally heats faster than the sample side during heating of the DSC measuring cell; i.e., the reference temperature (TR, green) increases a bit faster than the sample temperature (TP, red). The two curves exhibit parallel behavior during heating at a constant heating rate – until a sample reaction occurs. In the case shown here, the sample starts to melt at t1. The temperature of the sample does not change during melting; the temperature of the reference side, however, remains unaffected and continues exhibiting a linear increase. When melting is completed, the sample temperature also begins to increase again and, beginning with the point in time t2, again exhibits a linear increase.

The differential signal (ΔT) of the two temperature curves is presented in the lower part of the image. In the middle section of the curve, calculation of the differences generates a peak (blue) representing the EndothermicA sample transition or a reaction is endothermic if heat is needed for the conversion.endothermic melting process. Depending on whether the reference temperature was subtracted from the sample temperature or vice versa during this calculation, the generated peak may point upward or downward in the graphs. The peak area is correlated with the heat content of the transition (enthalpy in J/g).

Graph illustrating signal generation in heat flux differential scanning calorimetry, highlighting transition temperature and enthalpy.
Figure: Signal generation in a heat flux DSC

Specifications

Technical Data

A graphite furnace with W/Re sensors
For DTA-measurements up to 2000°C is available
Extension
with unique OTS® system is available
Optional available is the TM-DSC software feature
For temperature modulation of the DSC signal
NETZSCH DSC 404 F1, a differential scanning calorimeter, displays testing parameters on a digital screen for precise material analysis.

The DSC Specific Heat Capacity (cp)Heat capacity is a material-specific physical quantity, determined by the amount of heat supplied to specimen, divided by the resulting temperature increase. The specific heat capacity is related to a unit mass of the specimen.cp sensors enable extremely accurate determination of the specific heat:   

RT to 1400°C: ± 2.5%

RT to 1500°C: ± 3.5%

An automatic sample changer (ASC) for up to 20 samples and references is available (option).

TypeTemperature rangeCooling system
Silver furnace-120°C to 675°Cliquid nitrogen
Copper furnace-150°C to 500°Cliquid nitrogen
Steel furnace -150°C to 1000°Cliquid nitrogen
Platinum furnaceRT to 1500°Cforced air
Silicon carbide furnaceRT to 1600°Cforced air
Rhodium furnaceRT to 1650°Cforced air
Graphite furnaceRT to 2000°Ctap or chilled water
Technical diagram of a gas analysis system, featuring components like a heating element, thermocouple, and evacuating system.

A variety of sample crucibles (pans) made of alumina, platinum, aluminum, graphite, fused silica etc. is available in different sizes.

The concept allows for equipping the measuring instrument with a double-furnace hoisting device for two furnaces. Instead of a second furnace, an automatic sample changer (ASC) can optionally be used. Modular flexibility and particularly the combinability with the ASC saves a great amount of time and thus directly results in an increased sample throughput.

Optionally available, the OTS® system allows for reducing effectively the oxygen partial pressure at the sample vicinity.

The automatic sample changer (ASC) is designed for routine measurements. It works day and night, giving you time for other tasks, and provides for optimal use of the DSC 404 F1 Pegasus® (e.g. calibrations on the weekend).

A carousel is available for up to 20 sample and reference crucibles (pans) which can be automatically run in any order. The controlled generation of the required gas atmosphere in the sample chamber and cooling are automatic.

Of course, each sample can be assigned an individual measurement and evaluation macro. Easy-to-understand input masks lead you through the programming of the measurement series. And it is always possible to insert unplanned analyses into a preprogrammed series of measurements that is already in progress.

Three different styles of medical electrodes with connectors, featuring metallic and plastic components for patient monitoring.
NETZSCH Differential Scanning Calorimeter featuring a digital display, designed for thermal analysis and material characterization.

PulseTA®

With the PulseTA® technique an exactly defined quantity of gas is injected to the purge gas of the thermobalance (TGA) or the simultaneous thermal analysis instrument (STA).

This clearly increases the measuring possibilities:

  • Defined/incremental chemical reactions or adsorption of the injection gas with the sample
  • Quantification of gases evolved from the sample.
Diagram illustrating a gas analysis system with components like injected gas, pulse device, and MS/FT-IR for testing.

Crucibles (Pans) for the DSC 404 F1 /F3 Pegasus®

Material
(Purity)
Temperature
Range
Consisting ofDimension/
Volume
RemarksOrder Number
PtRh/Al2O3Max. 1700°CCrucible + liner + lidFor metal melts and other reactive materials 6.225.6-93.2.00
Al2O3 (99.7%)Max. 1700°CCrucible∅6.8mm/85µl GB399972
Al2O3 (99.7%)Max. 1700°CLid For GB399972GB399973
Pt/Rh (80/20)Max. 1700°CCrucible∅6.8mm/85µl GB399205
Pt/Rh (80/20)Max. 1700°CCrucible∅6.8mm/0.19mlHeight 6mmNGB801556
Al (99.5)Max. 600°CCrucible∅6.7mm/85µlSet of 100 piecesNGB810405
Al (99.5)Max. 600°CLid For NGB810405NGB810406
Gold (99.9)Max. 900°CCrucible + lid∅6.7mm/85µl  6.225.6-93.3.00
ZrO2Max. 2000°CCrucible85µlCaO-stabilizedGB397053
ZrO2Max. 2000°CLid For GB397053GB397052

* Please note: One and the same sealing press is capable of sealing all the Al crucibles (pan + lid), order no. 6.240.10-80.0.00A

Software

Proteus®: Excellent Thermal Analysis Software

The DSC 404 F1 Pegasus® runs under Proteus® Software on Windows®. The Proteus® Software includes everything you need to carry out a measurement and evaluate the resulting data. Through the combination of easy-to-understand menus and automated routines, a tool has been created that is extremely user-friendly and, at the same time, allows sophisticated analysis. The Proteus® Software is licensed with the instrument and can of course be installed on other computer systems.

DSC features:

Further Advanced Software Options

The Proteus® modules and expert software solutions offer further advanced processing of the thermoanalytical data for more sophisticated analyses. 

TM-DSC module software extension for temperature-modulated DSC tests:

Temperature-modulated DSC (TM-DSC) is a DSC technique whereby a sample is subjected to a superposition of a linear and a periodic temperature program. Temperature-modulated DSC enables the separation of overlapped DSC effects by calculating the reversing and non-reversing signals. Glass Transition TemperatureThe glass transition is one of the most important properties of amorphous and semi-crystalline materials, e.g., inorganic glasses, amorphous metals, polymers, pharmaceuticals and food ingredients, etc., and describes the temperature region where the mechanical properties of the materials change from hard and brittle to more soft, deformable or rubbery.Glass transitions can therefore be well separated from, for example, ExothermicA sample transition or a reaction is exothermic if heat is generated.exothermal Curing (Crosslinking Reactions)Literally translated, the term “crosslinking“ means “cross networking”. In the chemical context, it is used for reactions in which molecules are linked together by introducing covalent bonds and forming three-dimensional networks.curing, Decomposition reactionA decomposition reaction is a thermally induced reaction of a chemical compound forming solid and/or gaseous products. decomposition, evaporation, RelaxationWhen a constant strain is applied to a rubber compound, the force necessary to maintain that strain is not constant but decreases with time; this behavior is known as stress relaxation. The process responsible for stress relaxation can be physical or chemical, and under normal conditions, both will occur at the same time. relaxation or cold-CrystallizationCrystallization is the physical process of hardening during the formation and growth of crystals. During this process, heat of crystallization is released.crystallization processes in a single TM-DSC test. The DSC 404 F1 Pegasus® is the only DSC which allows for TM-DSC tests up to 1650°C. Nearly all available furnaces in combination with different DSC sensors are suited for such tests. It is totally based on a software solution. The NETZSCH TM-DSC solution improves separation of time-dependent events from the total heat flow.

Peak Separation permits accurate separation and evaluation of overlapping transitions. 

PeakSeparation allows for the presentation of experimental data in the form of the additive overlap­ping of peaks. This program offers different curve types such as Pearson, Gauß, Cauchy, pseudoVoigt, Fraser-Suzuki, modified Laplace and Pearson. With it, the experimental data is fitted as an additive superposition of peaks. 

Purity Determination is a program for determining the purity of a material through analysis of the DSC melting peak.

Prediction of Material Behavior and Reaction Processes:

Materials with accurately defined properties can be transformed into other substances with other properties by chemical reactions. The reactions can take place within a fraction of a second – like in the case of explosions – or take hundreds of thousands of years, as is the case in the formation of minerals. This is because processes like decomposition, curing, crystallization and sintering of materials are dependent on time and temperature. Knowledge about the speed of these processes is therefore important in order to simulate material behavior or optimize a process.

Kinetics, also called reaction kinetics or chemical kinetics, studies the rate of chemical processes and allows for determination of reaction rates. It also takes the factors, which control these reactions, into account.

NETZSCH Kinetics Neo software is used to analyze chemical processes. The software allows for the analysis of temperature-dependent processes. The result of such analysis is a kinetics model or method correctly describing experimental data under different temperature conditions. Use of the model allows for predictions of a chemical system’s behavior under user-defined temperature conditions. Alternatively, such models can be used for process optimization.

The software can analyze different types of thermal curves that depict the changes in a given material property measured during a process. Potential data sources include studies using Differential Scanning Calorimetry (DSC), Thermogravimetry (TGA), Dilatometry (DIL), Dielectric Analysis (DEA), Accelerating Rate Calorimetry (ARC)The method describing isothermal and adiabatic test procedures used to detect thermally exothermic decomposition reactions.Accelerating Rate Calorimetry (Accelerating Rate Calorimetry (ARC)The method describing isothermal and adiabatic test procedures used to detect thermally exothermic decomposition reactions.ARC®), Rheology and Viscosity (Torque).

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