Introduction to TG/DTA/DSC. Thermal Processing Technology Center Illinois Institute of Technology
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1 Introduction to TG/DTA/DSC Thermal Processing Technology Center Illinois Institute of Technology
2 Outline Introduction Theory of TG/DTA/DSC Application of TG/DTA/DSC TG/DTA/DSC in Metallurgy application Experiment difficulty
3 Application of Thermal Analysis in Material Research The almost universal applicability of thermal analysis technique has led to their use in nearly every field of science, with a strong emphasis on solving problems in materials technology and engineering, as well as "pure" scientific investigations. The change in physical properties of a substance subjected to a controlled temperature program as a function of temperature is measured. Techniques Include TG, DTA, DSC, DMA, TMA
4 Introduction to TG Thermogravimetry is a technique measuring the variation in mass of a sample when it undergoes temperature scanning in a controlled atmosphere. This variation in mass can be either a loss of mass (vapour emission) or a gain of mass (gas fixation).
5 Introduction to DTA Differential thermal analysis is a technique measuring the difference in temperature between a sample and a reference (a thermally inert material) as a function of the time or the temperature, when they undergo temperature scanning in a controlled atmosphere. The DTA method enables any transformation to be detected for all the categories of materials.
6 Introduction to DSC Differential scanning calorimetry is a technique determining the variation in the heat flow given out or taken in by a sample when it undergoes temperature scanning in a controlled atmosphere. With heating or cooling any transformation taking place in a material is accompanied by a exchange of heat ; DSC enables the temperature of this transformation to be determined and the heat from it to be quantified.
7 Theory of TG (Thermogravimetry) Measure the mass of sample as a function of temperature Determine sample purity, decomposition behavior, chemical kinetics
8 Theory of DTA (Differential Thermal Analysis) The temperature difference between reference and sample is monitored as a function of temperature
9 Theory of DSC (Differential Scanning Calorimetry) The difference in heat flow to or from a sample and to or from a reference is monitored as a function of temperature or time, while the sample is subjected to a controlled temperature program Power compensated DSC
10 Theory of DSC (Differential Scanning Calorimetry) Temperatures are measured in thin plates in contact with those, thereby measuring the difference in heat flow from crucible. This gives a signal proportional to the difference in heat capacities between the sample and reference and thus the instrument will work as DSC. Heat flux DSC
11 Different principles of DSC signal detection
12 Different principles of DSC signal detection
13 The difference between DTA and DSC DTA Temperature difference is measured, amplified and recorded. The peak area can be converted to heat only if a suitable reference is used DSC The temperature difference is controlling the electrical power to the sample and reference in order to keep them at the same temperature. The peak area directly corresponds to the heat consumed or produced by the sample Modern DTA (also called heat flow DSC) Temperatures are measured in thin plates in contact with those, thereby measuring the difference in heat flow from crucible. This gives a signal proportional to the difference in heat capacities between the sample and reference and thus the instrument will work as DSC.
14 Application of TG Study thermal degradation Chemical reaction resulting in changes of mass such as absorption, adsorption, desorption Sample purity
15 Application of DTA Primarily used for detection of transition temperature Sample purity
16 Application of DSC Determination important transition temperatures Determine heat of fusion of a crystal phase and the degree of crystallization Study crystal kinetic Determine heat capacity Determine heat of formation Sample purity
17 Summary TG DTA DSC Theory Measure the mass of sample Measure temperature difference between reference and sample Measure heat flow difference between reference and sample Application TG DTA DSC Mass change Yes No No Qualitative analysis of Heat change No Yes Yes Quantitative analysis of heat change No No Yes
18 Program experiment temperature
19 DSC curve
20 TG-DTA curve of CuSO 4-5H 2 O
21 Cp determination Instruments calibrated by a standard Heat flow ( µ V) Ab Ac As C p = Cpc m c (As A b) m s (Ac A b) T time
22 Heat Flow/ -10 Exo Metallurgy Application Phase transformation and melting of Iron C C C C C C : Point de curie 2 : Transition alpha --> Gamma 3 : Transition Gamma --> Delta 4 : Fusion 2 Results Different events may be observed during the heating : at 769 C : curie point at 924 C : α γtransition at C γ δtransition at C : melting of iron C Temperature/
23 Metallurgy application Oxydation of a steel in the scanning mode TG./ % DTG/ %/min TG DTG Results Above 700 C a mass gain is observed : the DTG shows two steps in the oxidation. Below 700 C a mass loss is observed Temperature/
24 Metallurgy application Reduction of a steel at 1200 C TG/ % Temperature/ Results T At 1000 C a small mass gain is observed due to traces of O 2 and H 2 O. But when the temperature of 1200 C is reached a strong mass decrease corresponding to the steel reduction is observed TG Time/ h
25 Metallurgy application Isothermal transformation of a high speed steel Heat Flow/ mw Temperature/ 9 Exo 8 Temperature 600 Results 7 6 Second heating First heating When the temperature is stable at 560 C a low exotherm can be observed, the DSC curve decreases slowly After the isotherm of 3 hours the same sample is cooled then heated a second time in the same conditions The difference between the two successive traces correspond to the sample transformation at 560 C Time/ h
26 Metallurgy application Melting of a Cu-Ti intermetallic compound Heat Flow (µv) Exo 50 Results C A double peak of melting is monitored. The onset peak of the first fraction is 925 C Onset point 1 : 925,2 C Onset point 2 : C Enthalpy / J/g : (Endothermic effect) ( ) The top of the second fraction is 978 C. The total heat of melting is J.g C Temperature ( C)
27 Metallurgy aplication Melting of Pb-Sn alloy HEAT FLOW/mW Exo Ent h : J/ g T. Onset : C Ent h1 : J/ g Ent h2 : J/ g Top of peak1 : C Top of peak2 : C Sn/ Pb : 86/ Results The melting curve presents two peaks. In fact only pure substances melt presenting a unique peak : generally alloys present a more complex melting curve. In this case Pb an Sn present an eutectic at C. The end of melting corresponds to the liquids curve. M 119 presents the phase diagram of Pb-Sn system. -30 TEMPERATURE/ C
28 Metallurgy application Phase diagram of Pb-Sn system Pb TEMPERATURE / C Sn Results The onset temperature of the melting curve generally corresponds to the eutectic temperature of the system. The temperature of liquids is given by the top of the peak of melting.
29 Experiment difficulty Explanation of experiment result Some curves might not be smooth and sharp System error The error of commercialized instrument is about 5% The measured thermodynamic property can be applied to modeling only if the error is less than 1% Crucible selection Crucible should not react with sample Crucible material Pt Al2O3 W Condition Nonmetallic sample Metallic sample Reacting gas BN Temperature setting The higher temperature, the more problems - high sample vapor pressure - high sample diffusivity - short life time Metallic sample
30 Setaram calorimeter Setsys1750: TG TG/DTA TG/DSC
31 Thermal analytical techniques, abbreviation and properties investigated Technique Abbreviation Physical Properties thermodilatometry - length Thermogravimetry TG(TGA) mass Derivative thermogravimetry DTG mass Differential Thermal Analysis DTA temperature Differential Scanning Calorimetry DSC enthalpy Thermomechanical Analysis TMA dimension Dynamic Mechanical Analysis DMA stiffness & damping Thermally Stimulated Current TSC dipole alignment/relaxation Dielectric Analysis DEA dielectric permittivity/loss factor Evolved Gas Analysis EGA gaseous decomposition products Thermo-optical Analysis TOA optical properties
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