Applications Laboratory

Thermophysical Properties Section

Thermophysical properties
of one Metal-Alloy 709M40 (EN19)

1209-U-10 part 4

by

A. Lindemann, D. Rapp, A. Rahner and S. Gezgin

February 16, 2018

NETZSCH-Gerätebau GmbH, Wittelsbacherstr. 42, 95100 Selb/Bavaria, Germany

Phone +49 9287 881 183, e-mail: at@netzsch.com

1209-U-10 NETZSCH Applications Laboratories 1/7

 Introduction

The Thermophysical Properties Section of the NETZSCH Applications Laboratory

received one metal alloy designated as 709M40 (EN19) from Access e.V., Aachen
for measurement of the specific heat, thermal diffusivity, thermal expansion and
room-temperature bulk density. This data was used to compute the thermal
conductivity by the following equation:

(T) = (T)  cp(T)  a(T)

with  - Thermal Conductivity
 - Bulk Density
cp - Specific Heat
a - Thermal Diffusivity
T - Temperature.

The chemical analysis of the sample was measured by Ascometal, Dunkerque,

France: [Wt %] C 0.406, Mn 0.751, Si 0.225, Cr 1.035, Ni 0.179, Mo 0.267, Cu
0.163, P 0.011, S 0.025, Al 0.020.

The thermal diffusivity was measured using a NETZSCH model

427 laser flash diffusivity apparatus. The unit used in this work
was equipped with a high-temperature, water-cooled furnace
capable of operation from 25 to 2000°C. The sample chamber is
isolated from the graphite heating element by a protective tube
allowing samples to be tested under vacuum or in an oxidizing,
NETZSCH LFA 427

reducing or inert atmosphere. The temperature rise on the back

face of the sample is measured using an In-Sb detector. Data acquisition and
evaluation are accomplished using a comprehensive PC software package. The data
evaluation software allows 2- and 3-layer calculations as well as the evaluation of the
contact resistance. The data can also be corrected for finite pulse and heat loss
effects using any number of models. The instrument can be operated in the fully-
automatic or manual mode. The LFA 427 operates in accordance with national and
international standards such as ASTM E-1461, DIN 30905 und DIN EN 821.

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The specific heat measurements were conducted using a
NETZSCH model DSC 404 F1 Pegasus differential
scanning calorimeter capable of operation from 25 to
1600°C. The system is vacuum-tight, and therefore
samples can be tested under pure inert, reducing or
oxidizing atmospheres, as well as under vacuum. The
specific heat is determined by running a baseline and
standard over the temperature range of interest. The sample is then run and the
specific heat is calculated by the standard ratio method. Instrument control and data
acquisition are accomplished via a new 32-Bit MS®-WindowsTM Thermal Analysis
software package. Data evaluation is carried out by a comprehensive PC software
package allowing computation of peak and onset temperatures, inflection points,
partial area integration, specific heat, transformation energetics, etc. The DSC 404
operates in accordance with national and international standards such as ASTM -C
351, -D 3417, -D 3418, -D 3895, -D 4565, -E 793, -E 794 and DIN 51004, -51007, -
53765, -65467, DIN EN 728 and ISO 10837, -11357, -11409.

The thermal expansion was measured using a

NETZSCH model 402 CD pushrod dilatometer. This
dilatometer was equipped with a SiC furnace capable of
operation between room temperature and 1600°C. The
system is vacuum tight, allowing measurements to be carried out in pure inert or
oxidizing atmospheres, as well as under vacuum. A set of primary standards,
including fused silica, sapphire, platinum, tungsten, etc., is available for the length
calibration. The expected expansion of the specimen and the temperature range of
the measurement, of course, dictate which standard should be used. Data
acquisition and evaluation, as well as instrument control, are accomplished with a
MS®-WindowsTM Thermal Analysis software package. The software includes semi-
automatic routines for correction of the sample holder expansion, as well as,
computation of the expansion coefficients, onset and peak temperatures, inflection
points, rate of expansion, etc. The dilatometer DIL 402 C is based on national and

1209-U-10 NETZSCH Applications Laboratories 3/7

international standards like ASTM - D 696, - E 228, - E 831, - E 1363, - E 1545, - E
1824 as well as DIN 53752.

Experimental

The dilatometer measurements were carried out using the following parameters:

Table 1: Measurement parameters

DIL 402 CD

Sample holder Al2O3

Sample thermocouple Type S (Pt/Pt10%Rh)

Pushrod force 25 cN

Atmosphere Ar at 50 ml/min

Calibration standard Al2O3*

Temperature program RT to 1400°C at 5 K/min

Sample length 12.10 mm

Density at RT** 7.823 g/cm3

* The system influence was corrected using the calibration correction. Same conditions for calibration
and sample run.
** The density at room temperature was measured by using of the buoyancy flotation method

The thermal diffusivity measurements were conducted in a dynamic argon

atmosphere at a flow rate of 100 ml/min between room temperature and 1350°C.
Standard sample holders for samples with a diameter of 12.7 mm were used. The
samples were coated with graphite on the front and back surfaces in order to
increase absorption of flash light on the samples’ front surface and to increase the
emissivity on the samples’ back surface. The presented thermal diffusivity results are
the average values of five individual tests. The density of the sample at room
temperature was measured by using the buoyancy-flotation method.

The sample tested with the DSC 404 F1 and had a mass of 149.93 mg. The
measurement was carried out in a high purity dynamic argon atmosphere (gas flow
rate: 50 ml/min). The system was equipped with a temperature-calibrated DSC-cp
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type S sensor. Platinum crucible with pierced lids and alumina liners were employed
for the test. The sample was heated between room temperature and 1400°C at a
heating rate of 20 K/min.
Results and Discussion

1. DIL Measurements
The thermal expansion, the coefficient of thermal expansion (Tref. = 50°C), the
physical alpha curve and the density of sample 709M40(EN 19) are shown in
figure 1.1. In the beginning the sample expanded continuously. A step was observed
in the thermal expansion between 762°C (maximum) and 794°C (minimum) which
might be ascribed to a phase transition. Further on the sample expanded
continuously till the end of the measurement. The values for the thermal expansion,
the coefficient of thermal expansion (T ref. = 50°C), the physical alpha and the density
are summarized in table 1.1.

T. Alpha *10-6 /K-1

dL/Lo /% Density /(g/cm^3) Alpha *10-6 /K-1

45
7.800
2.00
800
40
7.700
1209-U-10
1.50 709M40 (EN19) 35
7.600 600
black: thermal expansion 30
1.00 red: coefficient of thermal expansion
blue: physical alpha curve 7.500
green: density 25
Peak: 762 °C 400
0.50 Peak: 794 °C
7.400
20

7.300 200
15
0.00
Tref.: 50 °C 7.200 10
-0.50 0
7.100 5

-1.00 7.000 0
200 400 600 800 1000 1200 1400
Temperature /°C

Figure 1.1: Thermal expansion, coefficient of thermal expansion, physical alpha and
density of sample 709M40 (EN19)
Created with NETZSCH Proteus software

1209-U-10 NETZSCH Applications Laboratories 5/7

2. DSC Measurements
Figure 2.1 depicts the apparent specific heat capacity of the sample 709M40(EN19).
The specific heat capacity increases as expected from Debye theory from
0.46 J/(g·K) at 50°C up to 0.70 J/(g·K) at 1400°C. An endothermic effect was
detected at 783°C (peak temperature). Its assumed superimposed effects which
could indicate the curie transition (change in the magnetic properties) and phase
transition (e.g. α→γ). As an example the cp-values at 50°C, 400°C, 900°C and
1300°C are given.
In the range of the energetic effects interpolated cp-values will be used for calculation
of thermal conductivity (real cp).

Cp /(J/(g*K))

3.0
Sample 709M40(EN19)
real cp (extrapol.)
2.5 Peak: 783.3 °C

2.0

1.5

1.0
1300.0 °C, 0.632 J/(g*K)
50.0 °C, 0.457 J/(g*K) 400.0 °C, 0.611 J/(g*K) 900.0 °C, 0.573 J/(g*K)

0.5

0.0

200 400 600 800 1000 1200 1400

Temperature /°C

Figure 2.1: Apparent specific heat of sample 709M40 (EN19). Created with NETZSCH Proteus software

3. LFA Measurements

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Figure 3.1 depicts the thermophysical properties of sample 709M40 (EN19C). The
thermal diffusivity decreases with increasing temperature up to 1000°C. Above
500°C a step can be seen in thermal diffusivity and thermal conductivity. This might
be due to the  phase transition and the change of lattice conduction. The
measurement was stopped below 1400°C to prevent the start of melting (a few 10K
overheating can be expected during the heating to an isothermal segment (LFA).
Table 3.1 contains the values for thermophysical properties. The real cp values
(DSC) and thermal expansion / density data (DIL) were used for calculation of
thermal conductivity.
14 100 0.9

0.8
12
80
0.7

10

Thermal Conductivity /(W/(m*K))

Thermal Diffusivity /(mm^2/s)

0.6

Spec. Heat /(J/g/K)

60
8
0.5

0.4
6
40

0.3
4

0.2
20
2
0.1

0 0 0.0
0 200 400 600 800 1000 1200
Temperature /°C
Identity : x Material : 709M40 Coating : gr33 Operator : x
Date/Time : 2014-04-29 08:45:14 Thickness/Diameter : 1,3900 mm / 11,000 mm Atmosphere : Ar Customer : x
Sample : 709M40 (EN19C) Density (20,0 °C) : 7,823 g/cm^3 Laboratory : x Approximation : None
Instrument : LFA 427 Remark : --- Calc. code : C+p/mx/1-1-1
Created with NETZSCH Proteus software

Figure 3.1: Thermophysical properties of sample 709M40 (EN19C).

NETZSCH-Gerätebau GmbH
Applications Laboratory

16.02.2018 12:31

____________________________
Dr.-Ing. André Lindemann

1209-U-10 NETZSCH Applications Laboratories 7/7