Lehrstuhl für Werkstoffanwendungen im Maschinenbau

Univ.- Prof. Dr.-Ing. C. Broeckmann

Report No. 13054 Rev.1

Determination of Thermo-Physical Properties of

KALPUR

Customer: Access e.V. - Materials + Processes

Dr.rer.nat. F.Hediger
Intzestraße 5
52072 Aachen

Order No.: AU 13058

Authors: Sabine Fröhlich

Dr. Beate Balzer

Date: 20.06.13

Responsible: Dr. Beate Balzer Operator: S. Fröhlich

Institute for Materials Applications in Mechanical Engineering

RWTH Aachen University
Nizzaallee 32
D-52072 Aachen

IWM report 13054 rev. 1 1

Contents

1 Objectives .....................................................................................................................3
2 Samples.........................................................................................................................3
3 Measurements ..............................................................................................................4
3.1 Density .............................................................................................................. 4
3.2 Thermal Diffusivity............................................................................................. 5
3.3 Specific Heat Capacity ...................................................................................... 5
3.4 Determination of Thermal Conductivity .............................................................. 6
4 Methods of investigation..............................................................................................7
4.1 Mercury Intrusion Porosimetry (MIP) ................................................................. 7
4.2 Laser Flash Analysis (LFA) ............................................................................... 7
4.3 Differential Scanning Calorimetry (DSC) ........................................................... 8

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1 Objectives
The goal of the analysis is the determination of thermo-physical properties of KALPUR up to 1000°C. It
includes the measurement of the thermal diffusivity ‘a’ by laser flash analysis (LFA) and of specific heat
capacity ‘cp’ by differential scanning calorimetry (DSC) as function of temperature and density ‘’ at room
temperature by mercury intrusion porosimetry (MIP). From the measured values the values of thermal
conductivity ‘’ at RT, 200, 400, 600, 800, 900 and 1000°C were calculated according to the equation  =
a · cp ·.

2 Samples
One sample of KALPUR was delivered by Access in June 2013. Samples for each analysis were
prepared by dry diamond cutting and grinding. The sample was about 91.5 mm in height and about 80.5
mm in mean diameter.

Figure 1: Bottom of Filterspeiser KALPUR Figure 2: Top of Filterspeiser KALPUR

Figure 3: Side of Filterspeiser KALPUR Figure 4: Inside view of Filterspeiser KALPUR

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Samples for subsequent analysis were prepared as follows:

LFA: A cylinder of Ø= 12.7 mm is turned out. Plane parallel disks of approx. 2 mm

thickness are cut. Subsequently a fine coating of graphite is sprayed on.
DSC: A cylinder of Ø= 5 mm is turned out. Plane disks of approx. 1 mm thickness were
cut.
MIP: Several pieces of undefined geometry were cut.

3 Measurements

3.1 Density
Density was measured using mercury intrusion porosimetry (see annex). Samples get infiltrated with
mercury on different pressure steps at room temperature.

Table 1: Test overview MIP

Sample Run Date Weight [g]

KALPUR MIP13055 20.06.2013 0.1858

Table 2: Density and porosimetry

Name of sample KALPUR

Density [g/ccm] 0.451
Porosity (open) [%] 77.27

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3.2 Thermal Diffusivity
Thermal diffusivity was determined by the Laser Pulse Method (see annex).
Samples were heated to measuring temperature and kept there until thermal equilibrium. Then 8 laser
shots were evaluated with average and standard deviation. Thermal diffusivity was only measured up to
1000°C to protect the sample carrier, because the DSC pan was seriously damaged above 1000°C.

Table 3: Test overview a

Sample Run Date Thickness
[mm]
KALPUR 13250 11.06.2013 1,8730

Figure 5: Thermal diffusivity measured of KALPUR as f(T) under argon (± 5 %)

3.3 Specific Heat Capacity

Determination of specific heat capacity was carried out in the DSC-equipment (Netzsch, DSC 404
Pegasus F/SO) by the relation method with calibration on sapphire under argon. Specific heat capacity
surges from 1000°C to 1400°C (see fig. 2). The sample interacted with the pan material. The pan was
seriously damaged.

Table 4: Test overview cp

Sample Run Date Mass
[mg]
KALPUR p21-13 5.06.2013 10.4

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Figure 6: Specific heat of KALPUR measured as f(T) under argon

3.4 Determination of Thermal Conductivity

Thermal conductivity λ was calculated from data measured for thermal diffusivity a, specific heat capacity
cp and density ρ in the relation λ = a . cp . ρ.
The change in density with increasing temperature was neglected as well as the increasing sample
thickness during laser flash measurement. The resulting failure depends on the coefficient of thermal
expansion and is about 1% at 1000°C for a cte=10-10K-1. With an additional measurement of the thermal
expansion (by dilatometry) this failure would be wiped out.

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Figure 7: Thermal conductivity λ of KALPUR as f(T)

4 Methods of investigation

4.1 Mercury Intrusion Porosimetry (MIP)

Density ρ [g/cm³] at room temperature was measured by mercury intrusion porosimetry.

Equipment Analytical balance for mass determination

AutoPore IV 9500 (Micromeritics)
Instrument read-out Mass u(M) 0.0001 g
Sample weight 0.1858 g
Penetrometer 13-0342
Used Stem. Volume 78%
Pressure table 20/Dekade

4.2 Laser Flash Analysis (LFA)

Thermal diffusivity a [mm2/s] as a function of temperature was measured by the Laser Flash method.

Specification EN 821/2

Equipment LFA 427 (NETSCH Gerätebau GmbH, Selb)

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 Nd:YAG-Laser of variable output (< 60 J/pulse) and
pulse length (0.2 – 1.2 ms), wavelength: 1.046 nm
In-Sb infrared detector (N2-cooled)
Temperature range: 20°C… 1600°C (thermocouple Type S)
Measurement range: 0.001… 10 cm 2/s
Software with separate data evaluation models including finite pulse and
heat loss correction
Atmosphere: Argon 4.8 / vacuum ( 3*10-4 mbar )
Pulse width: 0.6 ms
Voltage: 300 V
Uncertainty of measurement: Thermal diffusivity < 5%
Sample carrier material: Al2O3 + SSiC cap
Coating of samples: Carbon spray (graphit 33, Kontakt Chemie, Iffezheim)
Analysis software: LFA Proteus Analysis
Correction: „Best Model“ for each shot

4.3 Differential Scanning Calorimetry (DSC)

Specific heat capacity as function of temperature cp [J/gK]

Specification DIN EN 821/3

Equipment DSC Pegasus404/So (NETSCH Gerätebau GmbH, Selb)

Atmosphere:
Sample dimensions:
Error of measurement:
Uncertainty of measurement:
Sample crucible material:
Heating rate:
Temperature range: 100°C… 1450°C (thermocouple Type S)
Argon 4.8
d  5 mm (accurate dimensions were not recorded since not relevant to
analysis)
Temperature u(T) < 10 K
Specific heat capacity u(cp) < 5%
Pt/Rh + Al2O3 Inlay
15 K/min (analysis of heating curve)

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Figure Index
Figure 1: Bottom of Filterspeiser KALPUR.................................................................................. 3
Figure 2: Top of Filterspeiser KALPUR ....................................................................................... 3
Figure 3: Side of Filterspeiser KALPUR ...................................................................................... 3
Figure 4: Inside view of Filterspeiser KALPUR ........................................................................... 3
Figure 5: Thermal diffusivity measured of KALPUR as f(T) under argon (± 5 %) ........................ 5
Figure 6: Specific heat of KALPUR measured as f(T) under argon ............................................. 6
Figure 7: Thermal conductivity λ of KALPUR as f(T) ................................................................... 7

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