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    7-Thermal Analysis

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    Maaz Zafar
    Thermal analysis techniques such as thermogravimetric analysis (TGA), differential thermal analysis (DTA), and differential scanning calorimetry (DSC) can be used to monitor changes in materials' structural and chemical composition when heated. TGA measures weight change, DTA measures temperature differences between a sample and reference, and DSC directly measures heat flow differences. These techniques provide information about thermal events like melting, crystallization, and decomposition. DSC in particular can determine heat capacities and enthalpy changes by measuring the heat required to increase a sample's temperature versus a reference.

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    7-Thermal Analysis

    Uploaded by

    Maaz Zafar
    62 views27 pages
    Thermal analysis techniques such as thermogravimetric analysis (TGA), differential thermal analysis (DTA), and differential scanning calorimetry (DSC) can be used to monitor changes in materials' structural and chemical composition when heated. TGA measures weight change, DTA measures temperature differences between a sample and reference, and DSC directly measures heat flow differences. These techniques provide information about thermal events like melting, crystallization, and decomposition. DSC in particular can determine heat capacities and enthalpy changes by measuring the heat required to increase a sample's temperature versus a reference.

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    slide package for Thermal analysis.

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    Thermal analysis techniques such as thermogravimetric analysis (TGA), differential thermal analysis (DTA), and differential scanning calorimetry (DSC) can be used to monitor changes in materials' structural and chemical composition when heated. TGA measures weight change, DTA measures temperature differences between a sample and reference, and DSC directly measures heat flow differences. These techniques provide information about thermal events like melting, crystallization, and decomposition. DSC in particular can determine heat capacities and enthalpy changes by measuring the heat required to increase a sample's temperature versus a reference.

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    © All Rights Reserved
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    Download as ppt, pdf, or txt
    62 views27 pages

    7-Thermal Analysis

    Uploaded by

    Maaz Zafar
    Thermal analysis techniques such as thermogravimetric analysis (TGA), differential thermal analysis (DTA), and differential scanning calorimetry (DSC) can be used to monitor changes in materials' structural and chemical composition when heated. TGA measures weight change, DTA measures temperature differences between a sample and reference, and DSC directly measures heat flow differences. These techniques provide information about thermal events like melting, crystallization, and decomposition. DSC in particular can determine heat capacities and enthalpy changes by measuring the heat required to increase a sample's temperature versus a reference.

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    © All Rights Reserved
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    Download as ppt, pdf, or txt
    of 27

    Thermal Analysis

    • When a material is heated its structural and


    chemical composition can undergo changes such as
    fusion, melting, crystallization, oxidation,
    decomposition, transition, expansion and sintering.

    • Using Thermal Analysis such changes can be


    monitored in every atmosphere of interest.
    Thermal Analysis
    Thermal Analysis Techniques

    Thermal Gravimetric Analysis (TGA)


    – Measure change in weight during heating or cooling

    Differential Thermal analysis (DTA)


    - Measure temperature difference between the sample and reference.

    Differential Scanning Calorimetry (DSC)


    – Measure heat absorbed or liberated during heating or cooling
    Thermogravimetric analysis (TGA)

    Monitor change in mass of a sample


    Sample: Gas atmosphere:
    can be both solid &liquid; CaCO3 →CaO + CO2
    2-100 mg In vacuum, decompose at ~500ºC
    In air, decompose at ~700ºC
    In CO2, ~900ºC
    Differential Thermal analysis (DTA)

    » Measure sample temperature relative to a reference, for the


    same heat transferred

    Thermal events: Exothermic event and endothermic event


    Reaction/decomposition, Melting, Crystallization, Change in crystal structure
    Glass transition
    Apparatus

    • The key features of a differential thermal analysis


    kit are as follows

    1. Sample holder comprising thermocouples,


    sample containers and a ceramic or metallic
    block.
    2. Furnace.
    3. Temperature programmer.
    4. Recording system.
    Working of DTA

    • In DTA both test sample & an inert reference material (alumina) –


    controlled heating or cooling programming

    • If zero temperature difference b/w sample & reference material –


    sample does not undergo any chemical or physical change.

    • If any reaction takes place temperature difference (∆T) will occur b/w
    sample & reference material
    DTA Curves
    DTA Combined with TGA

    * The area under a DTA peak is


    the enthalpy change

    Lowering heating rate;


    Reducing sample weight

    sharper peaks with improved


    resolution
    DTA + TG
    Differential scanning calorimetric (DSC)
    Differential scanning calorimetry or DSC is a thermoanalytical
    technique in which the difference in the amount of heat required to increase
    the temperature of a sample and reference are measured as a function of
    temperature.
    DTA DSC
    Working of DSC

    • Heat flux DSC measures the temperature


    difference directly and then converts it to heat flow
    difference accomplished by an algorithm in
    computer

    • The power-compensated DSC directly measures


    the enthalpy change of a sample during a thermal
    event
    DSC
    DSC
    • Constant Heating Rate
    – Initial Temp
    – Final Temp
    – Heating Rate (°C/min)
    • Data
    – Heat flow to sample minus
    Heat flow to reference vs
    Time (Temp.)
    • Measures heat of
    crystallization

    Polymer without weight change in this temperature range


    Chapter 2: Optimization of Thermoelectric Properties of Ca3Co4O9 through
    ionic doping at Ca-site
    Synthesis of Ca3Co4O9 via sol-gel method
    i. Raw materials: reagent-graded Ca(NO3)2.4H2O, Co(NO3)2.6H2O and citric acid
    monohydrate (molar ratio: citric acid/metallic cations ≈ 1.5) as a chelating agent
    ii. Stirring at 80oC for 3h in distilled water
    iii. Solution was dried at 130 oC in an oven for 12 h and the obtained dried gel was crushed
    iv. Calcination: heated at various temperatures from 400 0C to 850 0C for 4 h in air
    Applications of DSC
    Determination of Heat Capacity
    (1) The heat capacity of materials under
    constant pressure is the following.

    (2) The displacement between the baseline and sample line


    (h) should be proportional to sample heat capacity

    (3) The proportional factors are determined by the heating


    rate (β) and by the calibration factor (B).

    (4) We can eliminate these factors if a DSC curve of a


    standard sample (Saphire) is recorded under exactly same
    experimental conditions

    Heat capacity of the standard (CPs), Ms and M are the


    mass of standard and sample, respectively

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