PCE (Pyrometric Cone Equivalent) value

It is the measure of refractory's ability to sustain high temperature without fusion or deformation. This is
measured by heating a standard size cone made of the material to be tested in a furnace along with another
standard cone having refractoriness very close to the test material (determined by a pre-test), and noting
the furnace temperature at bending (9' or 3' o'clock positions viewed upside down) of the cone inclined at
one end due to its own weight.
Significance
This is the most important value for selection of any refractory material for a given application in the furnace.
The maximum working temperature.
PCE Value (Steps)
Step 1. Sample preparation:
• Pre-formed bricks: Several bricks are taken to have good representation of the refractory, and broken into
smaller size (5-10 mm). Out of the total mass, nearly 1 kg sample is taken, and ground to have - 200 μm
particles for making cone.
•Dry monolithic form: The ramming mass, refractory cement, etc. may be already in powder form and
further grinding may not be required. This powder may be sieved to have -200 μm, particles for making cone.
• Step 2. Cone molding: The powder mixed with binder (dextrine or glue) and water is cast into a cone shape
using a metal mold. The cone dimensions must be in accordance with standard followed. The cone is
tetrahedron in shape with some inclination to one side. The Indian standard (IS) 1528: 2010 prescribes 82°
for cone with 8 mm base and 25 mm high.
• Step 3. Cone heat hardening: The green molded cone is dried and heat hardened at 1000 °C to make cone
strong enough for handling.
• Step 4. Mounting cone for test: The prepared cone for testing and a standard cone are mounted on a
refractory plate with the help of a refractory paste which will not affect the fusion behavior of the test cone.
• Step 5. Heating cones in high temperature furnace: The high temperature furnace used for the purpose
must be capable of reaching the expected temperature. The test cone mounted plate is inserted in the
furnace and heating is initiated keeping oxidizing atmosphere. In case of gas fired furnace, the flames must
not have any impact on cones. In case of electrical heating, the plate must be in central zone with constant
temperature. The furnace is initially heated slowly to reach 200 °C in approximately two hours, and then it
is heated at the rate of 2.5 °C per minute.
• Step 6. Softening point temperature and PCE value: The furnace temperature is allowed to attain the
expected temperature to begin observing the sagging of cone through peep hole using suitable dark glass
filter to avoid radiation. The temperature must be noted at which the test cone tip sags to 9' or 3' o'clock
position depending on cone mounting angle.
| 2. RUL (Refractoriness Under Load) value
•RUL is the capability of a brick to sustain itself without breaking at high temperature under pressure of
overlying load. This working load could be due to burden, liquid metal or its own structural weight.
• In simple words, RUL is the crushing strength of a brick at elevated temperature.
• This RUL value is more important for brick which is heated from different sides as in case of coke oven
heating chamber, checker brick work, etc.
• It is a guiding parameter to use the brick at high temperature with safety against brick failure due to
pressure and high temperature.
RUL TEST PROCEDURE
• A cylindrical test sample (50 mm diameter and height) with a coaxial bore (12.5 mm) is prepared by cutting
and drilling.
• Step 1: A defect free test sample is placed on the ram slab and the loading column is lowered. The furnace
is brought in a position to keep the test specimen in constant temperature zone.
• Step 2: The load is applied on the test piece. This load would give 0.2 N/mm2 stress to a dense sample.
The porous samples may be given a load to give 0.05 N/mm2 stress.
• Step 3: The furnace temperature is raised at the rate of 15 °C/minute to reach 1000 °C and then further
heated at the rate of 8 °C/min.
• Step 4: The change in sample height with temperature is noted and plotted as percent height change with
temperature.
• Step 5: The temperatures for 0.5% (0.5), 1% (T1) and 2% (T2) negative change in sample height are
reported. The temperature Tos indicates initiation of failure under load and T2 gives failure of the refractory
under load.
3. High Temperature Modulus of Rupture (HMOR)
• It is the maximum stress that a rectangular test piece of defined size can withstand when it is bent in a
three point bending device. It is expressed as N/mm2 or MPa.
•HMOR (E) is expressed as the ratio of bending moment at the point of failure (Max) to the moment of
resistance W (the section modulus) at working temperature. It is expressed as Hooke's law for elastic
materials as follows:
Mmax 3
OF = W
FmaxxLs bxh2
High Temperature Modulus of Rupture (HMOR)
Sample size: A refractory slab of size 150 mm x 25 mm x 25 mm is used for testing.
Test unit: The testing unit has two basic components-furnace and loading device.
• The test sample is heated in the furnace to a desired temperature and then it is internally moved on
alumina rollers to a point where loading device is located.
• The unit can pre-heat a fixed number of samples to test in sequence.
•The loading device can have arrangements for measurement of load and deformation together with device
for loading with constant deformation rate.
• The maximum load is noted and MOR is calculated as per Hooks law and expressed as N/mm2 or Pa. The
result must be given with test conditions, e.g. average value for number of test, test piece size and loading
details (N/mm2/second), test temperature, heating rate, soaking time, etc.
4. Thermal Shock Resistance
Thermal shock resistance is a measure of refractory property when it is exposed to alternate heating and
cooling. This thermal shock leads to breaking of refractory particles which is termed as 'spalling' and loss of
strength due to micro-cracks.
Significance
• It is an important property for a refractory material. Many refractory components in high-temperature
processes undergo heating and cooling. The refractory grains and the grain bonding material expand while
being heated, and contract during cooling. The different expansion and contraction behavior of grains and
the bond material lead to breaking away and development of micro cracks.
• The nature and magnitude of the cracks would decide the thermal shock resistance of the material. The
refractory materials with high thermal expansion are generally prone to failure due to thermal shock and
refractories with lower thermal expansion behavior are considered safe.
Thermal Shock Resistance (Water Quench)
Testing method: The thermal shock resistance is tested in two ways: • Spalling test
• and loss in modulus of Rupture (MOR) strength.
Spalling test: This test is conducted by water quenching or air cooling.
• Water quenching test: The test is conducted with cylindrical refractory sample (50 mm diameter and 50
mm height) free from apparent defect. The sample is dried at 110 °C till constant weight to expel any
moisture present. The dried sample is heated in furnace at 950° ± 5°C for 15 minutes and then quenched in
water (10-30 °C) for 3 minutes.
• The sample is withdrawn and put in moisture oven (110 °C) for 30 minutes to make it dry. This heating,
quenching and drying constitute one cycle of operation. This heating, quenching and drying cycle is repeated
till the sample breaks into pieces. This test is terminated after 30 cycles if the refractory fails to break.
Thermal Shock Resistance (Air Cooling)
Air cooling test:
• Three test pieces of prism shaped (75 mm high and 50 mm square base) are taken for this test. The samples
are dried at 110 °C before test.
• The samples are heated at 1000° ± 5 °C for 30 minutes and withdrawn to place on a brick floor for 10
minutes cooling having no air draught.
• The heating and cooling constitute one cycle. This heating and air cooling cycle is repeated till the sample
break.
• The number of cycle required to cause breaking is reported as spalling number.
Thermal Shock Resistance (Loss in MOR)
Loss in MOR strength:
• This test requires a pair of sample (80 mm x 30 mm x 30 mm).
• One sample is given five cycles of heating and cooling.
•Then both the samples (unheated and heated) are tested for MOR.
• The percent loss of MOR value is taken as index for spalling.
•The lower MOR loss percent represents better resistance to thermal shock.
•More pairs are tested for better result.
5. Thermal Expansion
The increase in volume of the material due to heating is called thermal expansion. This expansion process is
reversible in nature, and material regains its size on cooling, hence, it is also called reversible thermal
expansion.
• It is the inherent property of all the materials. This property is measured as linear expansion with heating
due to practical reasons.
• The test can be done by using two methods:
• Dial Gauge method and
• Telescopic/video method.
Dial gauge method:
• This method uses mechanical dial gauge to monitor expansion in test sample mounted in vertical.
• The test apparatus consists of a one end closed silica tube enclosed in a removable furnace. The silica tube
is rigidly mounted while a refractory rod transmits the expansion to the dial gauge for observing the change
in length.
•The test sample (50 mm long and 10 mm diameter) is mounted in the set-up after making initial
measurements.
• The furnace is heated at 3-4 °C per minute to 1000 °C and the change in length is noted with a fixed interval
of temperature rise.
•The plot of linear expansion with time indicates the nature of expansion.
Dial gauge method (Limitations):
• This method has a limitation that dial indication for expansion depends on the sensitivity of mechanical
system, and is prone to error.
•The weight of the refractory rod connecting the dial gauge counters the expansion force to some extent.
Telescopic/Video method:
• This method overcomes the demerits of dial gauge method. The expansion is measured in sample without
subjecting any kind of pressure due to contactless technique. The sample (10 mm long and 10 diameter) is
placed on a flat platform in a horizontally placed silica tube in a tube furnace.
•The two ends of the silica tube is kept open and a telescope fitted with travelling microscale is placed at
one end focusing the top edge of the sample on the cross-wire. The other end of the tube is provided with
a light source to help in viewing the sample when tube is dark at low temperatures.
•The increase in linear height of the sample with temperature can be noted by telescope micro-scale.
• The light source would not be needed after the thermal glow at ~ 400-500 °C.
• This can be automated by replacing telescope with video camera and computing system network to record
thermal expansion with rising temperature with time automatically.
• The change in sample height could be computed by image analysis.
6. Permanent Linear Change (PLC)
The permanent linear/volume change refers to non-reversible expansion in the refractory materials due to
heating process. This permanent linear/volume changes could be due to the following reasons:
1. Phase changes in the refractory due to allotropic forms having different specific gravity.
2. Chemical reactions causing formation of new compound having different specific gravity. This could be
due to chemical attack by gas or slag.
3. Sintering of the material causing densification and shrinkage.
4. Melting of some phase causing densification and shrinkage or expansion.
Significance of PLC
• The permanent change in refractory could alter the furnace structure and may cause its failure. • This
phenomenon of permanent volume change is significant in case of silica brick manufacture. •The silica
undergoes phase changes, and it is desirable to allow completion of the changes at manufacturing stage
such that their use is made without trouble and is more assured during use. • However, this is not practical
due to long time required for phase change.
Sample for test: Two test samples (60 mm x 50 mm × 50 mm) are cut from the refractory block. The square
faces are ground to make them parallel and smooth.
Apparatus: An electrical furnace giving uniform 1500 °C temperature is needed for heating.
Test procedure: The test is conducted as per the following steps:
• Step 1: The dimensions between two parallel surfaces are measured at many points to consider the
average value accurately (reading up to 0.05 mm).
• Step 2: The two test pieces are placed in the constant temperature zone area of the furnace vertically
horizontally 25 mm apart for free flow of air.
• Step 3: The furnace temperature is raised to 500 °C and then heated with 5-6 °C/min to the desired
temperature and soaked for one hour.
Permanent Linear Change (PLC)
• Step 4: The furnace is then cooled to 200 °C in 30 minutes and allowed to cool in air overnight.
• Step 5: The cooled test samples are withdrawn and the dimensions are measured again to note the
difference expressed as %PLC. The test sample's physical appearance is also noted and reported as
unchanged, wrapped or bloated.