Dilatometry (DIL) (Thermodilatometry)
A technique in which a dimension of a substance under negligible load is measured as a function of
temperature while the substance is subjected to a controlled temperature program." (ICTA, ASTM E 473-
85).
Temperature-dependent length change LT : Length change of a specimen from the initial length L0 at
the initial temperature T0 (usually 20 °C) to the length LT at the temperature T.
Temperature-dependent length change relative to L0 caused by the temperature change in length relative
to the initial length L0
The average (technical) expansion coefficient for the temperature interval T is mathematically defines as:
L0 – sample length measured at ambient temperature, e.g. T0=237.15K. Sometimes, T0 is the initial
measurement temperature.
The physical expansion coefficient is the slope of the relative length change curve at the respective
temperature. Thus it corresponds to the first derivative of the dL/L0 curve according to the temperature:
Examples from Daily Life
Expansion gaps in concrete buildings, Metal transitions of highway bridges, Bimetals, Sintering of ceramics,
Softening point of glasses.
Detailed example : Magdeburg Water Bridge
It connects the Elbe-Havel Canal to the Mittelland Canal, crossing over the Elbe River. It is notable for
being the longest navigable aqueduct in the world, with a total length of 918 meters. On heating up: it can
expand in summer by over 150 cm. Relevant expansion gaps are filled with enormous double-walled rubber
seals.
Fields of Application DIL :
Linear thermal expansions, Expansion coefficients (CTE), Sintering temperatures, Sintering levels, Phase
transitions, Decomposition temperatures, Glass transition temperatures, Softening points, Volume
expansion, Density changes.
Measurement Principle
The sample is placed in the homogenous temperature zone of the furnace. The furnace temperature is
controlled either by the control thermocouple (usually without STC) or the sample thermocouple (with
STC). Sample temperature is measured by the sample thermocouple.
The pushrod is connected to the inductive displacement pickup and stays always in contact with the
sample. Changes of the sample length are registered by the inductive displacement pickup (Moving of the
core in the coil of the inductive displacement pickup).
All materials expand in the hot zone of the furnace during the measurement. Therefore, the registered length
variation is the sum of the length change of the sample, the sample support and the pushrod.
Practice:
- Sample preparation:
Sample quality: solid, plastic, powdery.
Sample shape: primarily cylindrical or rectangular shaped, three or angular also possible.
Sample dimensions: rod sample holder max. diam. 8 mm, length: 0 to 25 mm tube sample holder max.
diam. 2 mm, length: 0 to 25 mm.
Dilatometer
In our case, the sample is cut from a larger piece of material. Grind the end surfaces of the sample plane
parallel and smooth. Depending on the degree of hardness, use either emery paper or a grinding machine.
Make sure that the end surfaces are even and at right angles to the longitudinal axis of the sample and free of
ridges and foreign particles.
For measurement of the sample length, use a slide caliper rule or micrometer screw. According to DIN
51045, the sample length must be determined with a precision of 0.002 L0 (L0 = initial length of the sample
at 20°C).
Measurement:
- A correction measurement is carried out usually at first and after that a sample measurement. It’s also
possible to carry out a sample measurement at first and afterwards the correction measurement.
- Switch on the computer, the measurement part and the thermostat at least 2 up to 3 hours before a
measurement start. Switch on the measurement software. Select carefully the measurement conditions
according to the sample material state and to expected effects before the measurement.
- The following parameters should be considered especially by experiment preparation: • type of sample
(possible reactions with sample holder etc.), • sample preparation • temperature program • atmosphere in
sample chamber.
- Define the sample length at room temperature.
- Loosen the retaining nut at protective tube.
- Slide the furnace to the right all the way to the stop.
- Move the push rod to the left.
- If required, place support rings in the sample holder.
- Insert the sample (or standard sample e.g. Al2O3 sample) and slide the push rod to the sample.
- Contact pressure: 15-45 cN, standard setting: 25 cN.
- Slide the push rod over the sample by “” -button.
- Watch whether the sample changes its position.
- Slide the push rod to the left and then again to the rights. Watch again. If the sample moves it should be
positioned otherwise or check the end faces of the sample and if required grind the sample sides for better
contact. Gauge the sample once again and insert the sample.
- Carefully bend the sample thermocouple as close to the center of the sample as possible. The
thermocouple must not touch the sample - danger of alloy formation or chemical corrosion.
- Slide the furnace carefully to the left. The sample holder should have no contact to the protective tube.
- Close the dilatometer with the retaining nut.
- Define the measurement conditions: start temperature 25 C, end temperature 550 C, heating rate: 10 C|
min, atmosphere air.
Report: 1. Describe all what you have seen during the lab séance, 2. Plot the dilatometric curve and the
derivative of the heating segment, 3. Describe the dilatometric results and give son interpretation of the
observed anomalies.
