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    Measurement of The Thermal Conductivity of Solid Substances by DSC

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    Sai Li
    The document describes a method for measuring the thermal conductivity of solid substances using differential scanning calorimetry (DSC). A pure metal like indium or gallium is placed on top of a cylindrical sample pellet in the DSC cell. As the metal melts, the temperature at the top of the pellet remains constant, allowing the thermal conductivity to be calculated from the temperature difference recorded by the DSC sensor. Thermal conductivity values measured for various materials using this method, such as polymers, ceramics and porous substances, are reported and agree with literature values.

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    Measurement of The Thermal Conductivity of Solid Substances by DSC

    Uploaded by

    Sai Li
    204 views4 pages
    The document describes a method for measuring the thermal conductivity of solid substances using differential scanning calorimetry (DSC). A pure metal like indium or gallium is placed on top of a cylindrical sample pellet in the DSC cell. As the metal melts, the temperature at the top of the pellet remains constant, allowing the thermal conductivity to be calculated from the temperature difference recorded by the DSC sensor. Thermal conductivity values measured for various materials using this method, such as polymers, ceramics and porous substances, are reported and agree with literature values.

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    Measurement of the Thermal Conductivity of Solid Substances by DSC

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    The document describes a method for measuring the thermal conductivity of solid substances using differential scanning calorimetry (DSC). A pure metal like indium or gallium is placed on top of a cylindrical sample pellet in the DSC cell. As the metal melts, the temperature at the top of the pellet remains constant, allowing the thermal conductivity to be calculated from the temperature difference recorded by the DSC sensor. Thermal conductivity values measured for various materials using this method, such as polymers, ceramics and porous substances, are reported and agree with literature values.

    Copyright:

    Attribution Non-Commercial (BY-NC)
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    204 views4 pages

    Measurement of The Thermal Conductivity of Solid Substances by DSC

    Uploaded by

    Sai Li
    The document describes a method for measuring the thermal conductivity of solid substances using differential scanning calorimetry (DSC). A pure metal like indium or gallium is placed on top of a cylindrical sample pellet in the DSC cell. As the metal melts, the temperature at the top of the pellet remains constant, allowing the thermal conductivity to be calculated from the temperature difference recorded by the DSC sensor. Thermal conductivity values measured for various materials using this method, such as polymers, ceramics and porous substances, are reported and agree with literature values.

    Copyright:

    Attribution Non-Commercial (BY-NC)
    Download as PDF, TXT or read online from Scribd
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    The paper describes a method to measure the thermal conductivity of solid samples using differential scanning calorimetry (DSC) by melting a pure metal on top of the sample pellet. Key factors like sample dimensions, thermal contact, and calibration are discussed.

    A pure metal like indium or gallium is placed on top of the sample pellet in the DSC cell. During constant rate heating, the melting point of the metal is used to determine the temperature profile and calculate thermal conductivity from the heat flow signal.

    Samples with high thermal conductivity require improved thermal contact between the sensor and sample for accurate measurements. Porous materials can be well measured without contact paste if the contact faces are flat. The thermal conductivity of porous materials depends on the gas phase.

    Thermochimica Acta,93 (1965) 317-320 Elsevier Science Publishers B.V.

    ,Amsterdam

    MEASUREMENT OF THE THERMAL CONDUCTIVITY OF SOLID SUBSTANCES BY DSC. G. HakvoortX and L.L. van Reijen Delft University of Technology, Chemistry Department, Netherlands A.J. Aartsen, Du Pont de Nemours(Nederland) B.V., Is-Hertogenbosch

    ABSTRACT The" thermal conductivity of solid samples can be measured with DSC by melting experiments with a pure metal (indium or gallium) on top of cylindrical pellets. Particularly samples with a low thermal conductivity, like plastics or porous substances, can be determined INTRODUCTION At our laboratory the catalytic activity of Ni/A1205 pellets, used for the highly exothermic methanatlon reaction, is investigated. One aspect concerns the temperature profile inside the pellet, which strongly depends on the thermal conductivity h (ref.1). Measurement of X has to be performed by measuring the heat flow through one side of a sample as function of a known temperature difference between that side and the opposite parallel side. In a DSC cell of the Boersma type, both temperature and heat flow are measured at the contact area between sample and sensor. The temperature at the dbposite side of the sample cannot be measured directly, but by applying a pure metal, placed on the sample, the temperature of that opposite side is known during the melting of the metal. EXPERIMENTAL A DuPont 910 DSC apparatus was used (see ref.1). Two kinds of experiments are to be made: First the calibration factor (C.F.) is determined by melting indium or gallium, directly placed on the sensor, without using a cup, and measuring the DSC signal A (mV). In that case it is assumed that practically all heat of melting Q, flows to the sensor and not to the gas phase, resulting in a calibration constant (C-F.), expressed in W/mV, according to: Qm = * QJensor dt = (C.F.)/ Adt, giving: Qlensor = (C.F.)A The value of (C.F.) depends on the gas phase and varies a little with temperature. For gallium (melting temperature Tm = 30.0 "C)
    Proceedingsof ICTA 85, Bratislava

    - 318 -

    measured values of (C.F.) are (0.245 and 0.174) 10q3 W/mV in hydrogen en nitrogen respectlvily. For indium (Tm = 156.6 'C) these values are (0.261 and 0.188) 10s3 W/mV. Secondly two identical flat cylindrical pellets are directly placed on sample and reference side of the DSC cell. In some cases, when the thermal conductivity of the pellet is high, the thermal contact between sensor and sample has to be improved by applying a silicone paste. A flat piece of pure metal (indium or gallium) is placed on the top of the sample pellet (see fig 1A). The best results are obtained when the metal totally covers the sample pellet, having the same cylindrical diameter, and when the pellet dimensions are not too small: height l-3 mm, diameter 2-4 mm. The weight of the piece of metal varies from 10 to 40 mg. Starting at low temperature, when the metal is solid, sample and reference are heated with a constant rate (2-10 OC/mln). The sensor temperature Ts and the DSC signal A are recorded against time. During the melting the top of the pellet remains at constant temperature Tm, while the temperature of the lower side of the sample still increases with a constant rate. The resulting DSC plot is shown in fig. 1B.

    T
    h Fig. 1. Melting experiment with indium on top of a pellet. A: sample geometry, B: DSC plot, a: Ts against time -tdTs/dt, b: A against time + dA/dt, (dTs/dt)/(dA/dt) = dTs/dA = BP

    - 319 -

    RESULTS AND DISCUSSION The following direction from formulas (x=0) = A, can be derived to area the top of for the heat pellet flow in one sensor (x=h):

    Q' sensor

    = (C.F.)A

    . (-h(dT/dx)x=O)
    between sensor profile and pellet. inside the pellet: temperature

    = *d2/4 = contact As Suppose there is a linear (dT/dx) x = (Tm - Ts)/h gives

    This dA/dt dTJdA

    :
    (Ts - T,)/h (C.F.) A of zp can be determined, are values. given for so of samples can give and and (C.F.))(dTS/dt) value

    A = h A,

    = {A As/h = B ?B the

    = h (C.F.)/X

    From fig.

    X = h(C.F.)/AsBp In table compared be drawn: - Samples only sensor - Samples materials, paste sample is with is with

    can be calculated. 1 the results a number literature a thermal The following of conclusions

    conductivity thermal

    1 W/m.K or higher between paste. like that plastics of the sample

    good

    results improved

    when the

    contact

    by applying very

    a special well. flat.

    with not

    low thermal strictly are

    conductivity, provided porous on the substances of the the same. Ni/y-A1203, large giving it

    or porous a contact faces or is of

    can be measured

    Application

    needed, sufficiently

    contact like glass. is cork

    and sensor foam, for

    - The thermal polystyrene not for that are type found - The thermal Ni/a-A1203 a-A1203 very of and porosity contact

    conductivityof depends non-porous conductivity than are consists the divided, experiments is of for of about

    substances, gasphase. like This Pyrex pellets is caused with

    dependance

    catalyst This

    much greater composition fact thermal and pores the Boersma the

    though

    chemical a good

    by the

    crystals In y-A1203

    between finely

    particles.

    particles that for

    a low thermal instrument

    conductivity. measuring

    From these thermal

    can be concluded

    DSC or DTA cell conductlvlty

    a helpful

    solids.

    - 320 -

    TABLE 1. Thermal conductivity X for solid substances in H2 and N2, as determined by applying Ga and In on top of the pellets.

    gasphase

    Metal

    X (W/m.K)* measured B A lit.value (ref.2)

    Pyrex glass 11 1, quartz glass tt PMMA teflon cork 11 polystyrene foam ,t

    nitrogen I, hydrogen nitrogen ,, 11 I, II hydrogen nitrogen

    Ga In Ga Ga In Ga ,I 11 I, ,I 11 il ,I

    1.02 1.12 0.94 0.96 0.189 0.246 0.082 0.185 0.103 0.328 1.24 0.34

    1.14 1.24 1.12 1.42 1.45

    1.14 1.30 1.14 1.37 1.54 0.194 0.256

    hydrogen fr catalyst pellet CL I, 11 Y

    teflon = poly3(tetraOPMMA = poly (methyl methacrylate); fluorethylene), cork: corkplate,,density 659 kg/m ; polystyrene foam, density 79 kg/aJ. Catalyst pellet a : 6 wt % NI on u-alumina,porosity 0.60; *Y : 6 wt % Ni on y-alumlna,poroslty 0.63 (see ref. 1). A: wathout, and B : with use of a silicone compound for better thermal contact between pellet and sensor. ACKNOWLEDGEMENT The authors wish to thank Y. Tammerman for performing most of the experimental work and H. Doetsch of the KFA at Jillrchfor inspiring discussions. The research described in this paper has been supported by a NATO Research Grant for International Collaboration in Science, REFERENCES 1. G. Hakvoort, W. van der Klugt, Y. T~mmerman and L.L. van Reijen, Proc. third ESTAC, to he published in Thermochim. Acta (1985). 2. Landolt-Bornstein, Zahlenwerte und Funktionen, 6e Aufl., IV. Band, 4. Tell (Warmetechnlk), Springer-Verlag (1972).

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