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Today, selection of the proper refractory material is more crucial than The testing of refractories – clearly
ever when it comes to improving the cost-effectiveness of a process and an essential process – includes the
∙∙
prolonging the life cycle. Appropriate selection of the refractory furnace following applications:
lining can only be made with accurate knowledge of the properties of Selection of material
the refractory materials and the stresses on the materials during service. Characterization of new
∙∙
materials
Thermomechanical properties are determined using high-temperature Prediction of service conditions
test methods with external forces causing stresses on the tested material. Quality control of the process
∙∙
The stress-strain behavior of refractories at high temperatures includes and the product
reversible elastic strain as well as non-reversible time-dependent defor- Failure analysis
mations. Therefore, the thermomechanical behavior of refractories must Mathematical modeling for
be considered as an interaction of stress, strain, temperature and time. product improvements
3
RUL/CIC 421
Refractoriness Under Load and
Method
Refractoriness under load (RUL) is
a measure of the resistance of a
refractory product to subsidence when
subjected to the combined effects of
load, rising temperature at a pre-
defined heating rate. The range in
which softening occurs is not identical
with the melting range of pure raw
materials, but it is influenced by the
content and the degree of distribution
of low melting point fluxing agents.
RUL
The RUL test method is described in
ISO 1893, Refractoriness under load
(RUL, differential – with rising temper-
ature). A cylindrical test piece (50 mm
in Ø and height with coaxial bore of
12.5 mm) is subjected to a specified
constant compressive load and heated
at a specified rate until a prescribed
deformation or subsidence occurs.
The deformation of the test piece is
recorded as the temperature increases,
and the temperatures corresponding
to specified proportional degrees of
deformation are determined.
CIC
RUL/CIC 421
4
Creep in Compression
Variable load
Gas outlet
Loading column
Protective tube Heating element
Inner thermocouple Sample
Outer thermocouple Control
thermocouple
Sample with
coaxial bore
Outer tube
and inner tube
Hood type Inner tube
furnace
Supporting Bellows
column
Vacuum-tight seal
Variable
Gastight contact force
casing
Evacuating
Inductive
system
transducer
Gas inlet
5
RUL/CIC 421
Test Atmosphere Test Piece Dimension
Measurements can be carried out Generally, identical test piece
in static air (basic version) or using dimensions of 50 mm in diameter
n for an optional device for inert gas and 50 mm in height are used for
t i g h t versio
Gas- oxyge
n- purge within the test piece area. both the RUL and the CIC test. For
testing pecimens the high-precision differential
ve s
sensiti
measuring system used in deter-
mining expansion and defor-
Testing Carbon-Containing mation, the cylindrical test piece
Materials has a coaxial bore of 12.5 mm.
The ground faces should be plane,
For testing carbon-containing parallel and perpendicular to the
materials (e.g., magnesia-carbon axis of the cylinder (ISO/DIN).
graphite bricks), a non-oxidizing Other test piece dimensions are
test atmosphere can be realized also possible (e.g., 36 mm, GOST
with a gas-tight test chamber 4070-20000). .
(optional; see figure on previous
page). This chamber can be
evacuated and then purged with Sample Preparation
protective gas. Measurements can
be carried out up to 1600°C.
Machines
NETZSCH offers the following
machines for the appropriate
Variable Loading Device preparation of optimum
test pieces:
Optionally, the loading device can ∙∙
Drilling machine 421/11
∙
be equipped for load variation. Grinding machine 421/12
The preload can be up to 300 N Sawing machine 421/13
and the verifying load can be
applied in the range from 0 N to
700 N at a rate between 0.3 N/s
and 3 N/s.
6
Peak:
Peak: 1387.0
1387.0 °C
Evaluation Routines 0.8 °C
0.8 Peak: 1387.0 °C
0.8
/%
L0/%
measurement (differential) on a
/%
0.2
0.2
//L0
0.2
test piece of a fireclay brick with
/ L0
dL
dLdL
0.0
0.0
increasing temperature. At 0.0
1387°C, the test piece reaches -0.2
-0.2
its maximum expansion. Defor- -0.2
dLmax
dLmax =
= 0.724
0.724 %
%
mations of 0.5% and 1.0% -0.4
-0.4
T(dLmax)
dLmax
T(dLmax) = 1387.0%°C
= 0.724
1387.0 °C
-0.4
occurred at 1565°C (T0.5) and -0.6 TT 0.5
0.5
T(dLmax) = 1564.7 °C
= 1387.0
1564.7 °C
-0.6 1.0
TT 0.5 = 1599.8 °C
= 1564.7
1600°C (T1), respectively. -0.6
1.0
T 1.0
1599.8 °C
= 1599.8 °C
0
0 200
200 400
400 600
600 800
800 1000
1000 1200
1200 1400
1400 1600
1600
0 200 400 600 Temperature
800
Temperature // °C
°C 1000 1200 1400 1600
Temperature / °C
Refractoriness under Load; test conditions: 0.2 N/mm², 5 K/min, static air
presented.
L0/%
/%
//L0
0.6
0.6
/ L0
0.6
dL
dLdL
0.2
0.2
0.2
0.0
0.0
0.0 200
200 400
400 600
600 800
800 1000
1000 1200
1200
200 400 600 800
Temperature
Temperature // °C
°C 1000 1200
Temperature / °C
Creep in Compression; heating segment at a heating rate of 5 K/min
cr (0.00,
cr (0.00, 1.00)
1.00) == 0.063
0.063 %/h
%/h
cr (0.00,
cr (0.00, 1.00)
10.00) =
10.00) = 0.063
0.019 %/h
0.019 %/h
0.70
0.70 15.00) = 0.015 %/h
cr
cr (0.00,
(0.00, 10.00)
15.00) = 0.019
0.015 %/h dLmax =
dLmax = 0.729
0.729 %
%
0.70 cr 20.00) =
= 0.013
0.013 %/h
cr (0.00,
(0.00, 15.00)
20.00) 0.015 %/h T(dL max)
dLmax
T(dL max) = 1283.0%°C
= 0.729
1283.0 °C
cr
cr (0.00, 25.00) =
(0.00, 20.00)
25.00) = 0.011
0.011 %/h
0.013 %/h T(2.5max)
T(dL
T(2.5 h) =
h) 1280.4 °C
= 1283.0
1280.4 °C
0.65
0.65 cr (0.25) 25.00) =
cr (0.00,
(0.25) = 0.011
0.011 %/h
%/h ISO h) = 1280.4 °C
T(2.5
ISO
0.65
cr (0.25) = 0.011 %/h Z 0.00
0.00 =
ISO
Z = 0.000
0.000 %
%
0.60 Z 5.00 =
Z 0.00
5.00 = 0.136
0.136 %
0.000 %
/%
0.60
L0/%
0.60 Z 10.00 =
Z 5.00
10.00 0.191 %
= 0.136
0.191 %
/%
//L0
Z 15.00 =
Z 10.00
15.00 0.228 %
= 0.191
0.228 %
/ L0
0.55 Z 20.00 =
Z 15.00 0.258 %
= 0.228
dL
0.55 Z 25.00
20.00 = 0.282
0.258
Z 25.00 = 0.282 %%
Z(5.25)
Z 25.00 = 0.146
0.282
Z(5.25) = 0.146 %
0.50
0.50 Z(5.25) = 0.146
0.50
0.45
0.45
0.45
0
0 5
5 10
10 15
15 20
20 25
25
0 5 10 Time // h
Time h 15 20 25
Time / h
7
RUL/CIC 421
Applications
Refractoriness under Load 0.8
from the RUL tests where 0.5%, 1% -0.6 1510 1670 >1700 >1700
0.7
0.6
Expansion / %
0.5
0.4
0.3
1.5
1.0
Expansion / %
0.5
0.0
8
-0.5
Expansi
0.6
0
0.4
-0.2
Firing at T0.5 T1 T2
(°C) (°C) (°C) (°C)
0.2 1430 1625 1675 >1700
Expansion / %
-0.4
1470 1650 1695 >1700
0
-0.6 1510 1670 >1700 >1700
-0.2
-0.8
Firing at T0.5 T1 T2
0 200 400 600 (°C) 800 (°C) 1000 (°C) 1200 1400 1600 1800
(°C)
Temperature / °C
-0.4 1430 1625 1675 >1700
1470 1650 1695 >1700
-0.6 1510 1670 >1700 >1700
-0.8
0.7 0
Creep in Compression (CIC)
200 400 600 800 1000 1200 1400 1600 1800
Temperature / °C
0.2
0.5 Firing at (°C)
1430
tests, where the load is applied
from the very beginning of the
0.1
0.4 1470
1510
measurement. This plot only
0
shows the time-scaled creep at
0.3
0 5 10 15 20 25 constant temperature (the heating
Time at 1425°C / h segment is not depicted).
0.2 Firing at (°C)
1430
0.1 CIC behavior
1470of andalusite bricks (approx. 65% Al2O3) fired at three different
temperatures; test conditions: 0.2 N/mm2, 5 K/min, static air, 25 h at 1425°C
1510
1.5
0
0 5 10 15 20 25
Time at 1425°C / h
1.0
Expansion / %
0.5
0.0
1.5
Quality Control of Castable
-0.5
1.0 Refractories by RUL Tests
Castables are mixed with water
Expansion / %
-1.0
0.5
Lab Test
and then installed by either
Product 1; poor result
-1.5
0.0 pouring or pumping. These
Product 1; good result
measurements were carried out on
-0.5
-2.0 finished construction parts.
0 200 400 600 800 1000 1200 1400 1600 1800
Temperature / °C
Castables have to be prepared
-1.0 exactly as instructed by the product
Lab Test
manufacturer. Field tests show that
Product 1; poor result
-1.5 the product depicted here by the
Product 1; good result
red sample curve was improperly
-2.0
0 200 400 600 800 1000 1200 1400 1600 1800
handled. The divergent shrinkage
Temperature / °C behavior (as compared to the blue
and green curves) causes failures in
RUL test as quality control for a finished construction part the finished product.
9
RUL/CIC 421
Software
∙ ∙
dynamic temperature program
Correction of the measured steps) Calculation of creep rates in
∙
data by calibration curves preset time intervals
∙ ∙
Presentation of the measuring
Determination of characteristic values temperature- or time- Simultaneous analysis of up to
data according to user’s require- scaled for RUL and time-scaled 8 curves/temperature segments
ments for CIC (curve comparison)
∙
dilatation spectrum (RUL) coefficients
∙ ∙
Derivation of curves for deter-
mination of the temperature- Determination of the sample Calculation and graphic display
or time-dependent linear temperature 2.5 h after start of of the 1st and/or 2nd derivative,
expansion rates isothermal phase (CIC) peak determination
10
Technical Specifications
RUL/CIC 421
Measuring range
0.5 N/mm2
20 mm; resolution
as extrapolated onset, point of 4,000,000 steps
inflection, peak, peak end
Measuring system Differential
∙ Graphic export
∙∙
Electronics : 230 V/10 A 50 Hz
∙
610 mm x 2400 mm
Dimensions
Control unit: 562 mm x
555 mm x 1183 mm
Weights ∙∙
Measuring unit: ≈ 480 kg
Control unit: ≈ 220 kg
11
Thermal Diffusivity and
Laser/Light Flash Analysis – An
For decades, thermophysical properties (thermal diffu- simultaneous measurement of the specific heat capacity
sivity [a], specific heat capacity [cp], and thermal conduc- so that thermal conductivity can be determined, without
tivity [λ]) have been determined using sta- additional measurements, per the following formula:
tionary methods (e.g., guarded hot plate technique) or
standardized transient techniques such as the hotwire λ(T) = a(T) · ρ(T) · cp(T)
method according to ISO 8894. However, these methods
are time-consuming and limited to large samples and In addition, the rapidity of the flash methods allows
materials of low thermal conductivity. for testing on a larger number of samples (up to
25.4 mm in Ø).
Light/Laser Flash methods (LFA) are absolute,
non-contact measurement techniques and can handle Precise determination of the thermal diffusivity is
high thermal conductivity materials without any offered by the NETZSCH LFA 427, LFA 457 MicroFlash®
difficulties. Modern LFA systems often also allow for and LFA 467 HyperFlash® systems.
LFA 427
12
Specific Heat Capacity
Thermal Conductivity /
Thermal Diffusivity /
5
3
1.0 4
#1
7
tank regenerators and lime kilns. LFA 427 #3
6 Average
Elevated kiln capacity and the
Conductivity
Thermal Conductivity
(LFA/TCT) ±10%
increasing use of alternative fuels 5
present a challenge to basic
refractories for the burning zone 4
of cement rotary kilns. When
3
Thermal
13
Alumina-based bricks for high-temperature kiln
linings – With increasing Al2O3 content, thermal
stability and chemical resistance increase.
1.5 6
The thermal diffusivity of even
5 inhomogeneous samples can be
3
measured with the LFA. This
1.0 4
#1 example depicts LFA measure-
#2 3
2 ments on three brick specimens
#3 with silicon carbide content (#1,
0.5 2 #2 and #3) cut from the same
#1 1 brick. The tests were conducted in
#3
#2 1 the temperature range between
20°C and 1400°C. In addition to
0.0 0 0
0 200 400 600 800 1000 1200 1400 the measured thermal diffusivity
Temperature / °C (red curves) and specific heat
capacity (black curves), the plot
Thermal diffusivity, thermal conductivity and specific heat capacity of
also shows the calculated results
a brick containing 45% Al2O3, 29% SiO2 and 25% SiC; three specimens
cut from the same brick. for the thermal conductivity (blue
curves). Only minor deviations are
observed within one specimen.
9
K)
TCT 426
8
LFA 427 #1
W/(m·K)
LFA 427 #2
/ /W/(m
High Temperature
7
LFA 427 #3 1.0 1.4
Insulating Firebrick
6 Average
Conductivity
0.6 0.9
Thermal Conductivity
(LFA/TCT) ±10%
1.2
5
0.8
0.5
An aluminosilicate product was
Thermal Conductivity / W/(m·K)
4 1.0
measured with the NETZSCH LFA 0.7
3
427. The thermal diffusivity (red
Thermal
0.4 0.6
curve),
2
specific heat capacity (black 0.8
curve) and thermal conductivity 0.5
(blue 1curve) of this specimen are 0.3
0.6
0.4
plotted for the temperature range
RT to 01500° C. The thermal 0.2 0.3
0 200 400 600 800 1000 1200 1400 1600 0.4
conductivity is monotonously
Temperature / °C
increasing with a change in the Sample: JM 30 0.2
slope at about 1200°C, which is 0.1 Thickness: 2.570 mm 0.2
Density: 1.014 g/cm³ 0.1
most probably due to increasing
contribution of heat transfer by 0 0.0 0.0
radiation within the ceramic 0 500 1000 1500
Temperature / °C
structure.
Comprehensive characterization of a firebrick containing
69.9% Al2O3, 28.1% SiO2, 1.2% TiO2 and some minor amounts
of Fe2O3, CaO, MgO, Na2O and K2O.
14
All over the world, the name NETZSCH stands for
comprehensive support and expert, reliable service,
both before and after sale. Our qualified personnel
from the technical service and application depart-
ments are always available for consultation. In special
training programs tailored for you and your employees,
you will learn to tap the full potential of your
instrument.
Expertise in
SERVICE
15
HMOR 422
High-Temperature
Bending Strength Tester
Determination of the Hot Modulus of Rupture HMOR 422 Models
∙
characterization of refractories. Along with other thermophysical
properties, the maximum load until breakage at high temperatures HMOR 422 D/3 for continuous
plays a significant role in the quality control and development of operation up to 1500°C and a
furnace linings. maximum load of 5000 N with
optional devices for:
∙∙
Load and deformation tests
Constant deformation rate
Method
HMOR 422
16
HMOR 422 D/3
Inductive
Measurement of Load and Deformation – displacement
HMOR 422 D/3/G transducer
Loading column
In the standard version (HMOR 422 D/3), the sliding
weight stops at the sample's breakage. This force is Refrence rod
read on the scale and the bending strength is
calculated.
Test piece
Optionally, deformation of the test piece can be
recorded as a function of the increasing load. For
this set up, the inductive displacement transducer
for the bending signal and a linear potentiometer
Configuration for displacement measurement
for the load signal are required.
17
HMOR 422
18
Technical Specifications
HMOR 422 D/3 HMOR 422 E/4
Distance between
N/A 20 mm
4-point bending edges
∙ ∙
0 ... 500 ... 1250 ... 2500 ... 5000 N; 0 ... 500 ... 1250 ... 2500 ... 5000 N;
movable weight
Load rate: Load rate:
4 speeds (2, 4.2, 8, 12 N/s) 4 speeds (2, 4.2, 8, 12 N/s)
Measuring unit dimensions 2200 x 1800 x 870 mm; 540 kg 2100 x 1600 x 750 mm; 430 kg
Control unit dimensions 1120 x 565 x 452 mm; 250 kg 1120 x 565 x 452 mm; 250 kg
19
HMOR 422
Applications
Quality Control – Modulus of Rupture of a Kiln
Furnace Product
HMOR / N/mm2
30
25 30
25
20
20
15 15
10 10
5 5
0 0
1 6 11 16 21 26 31 1 2 3 4 5 6 7 8 9 10 11
sample no. sample no.
30
HMOR / N/mm2
25 25
20 20
15 15
10 10
5 5
0 0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 1100°C 1200°C 1300°C
sample no. temperature
20
TEST PIECE PREPARATION
Depending upon user needs, a variety of accessory
machines is available for the preparation of test
pieces for each instrument, as follows:
21
Pillar Drilling Machine
The NETZSCH drilling machine is used for drilling cylindrical test pieces from refrac-
tories, stone, ceramics or products similar to ceramics.
The drilling machine is a sturdy boxtype construction with a complete casing for all
rotating parts. The drilling table can be swung 360° to include the water-protective
case. In addition, it has a working table light incorporated and infinitely variable
speed control for the drilling spindle via a V-belt control system. The water-protective
case, two clamping angles to hold the workpiece and a water-flushing box with
plug MK2/B16 (without drills) are included.
Various drills are available for the outer diameter of the test piece:
∙∙ Diamond hollow drill, outer Ø 30 mm, inner Ø 25 mm, drilling depth 100 mm
∙∙
Diamond hollow drill, outer Ø 42 mm, inner Ø 36 mm, drilling depth 100 mm
Diamond hollow drill, outer Ø 56 mm, inner Ø 50 mm, drilling depth 100 mm
Diamond hollow drill, outer Ø 108.4 mm, inner Ø100 mm, drilling depth 120 mm
To fulfill DIN/ISO standards, these drills for the inner coaxial bore are also available:
∙∙ Diamond hollow drill, outer Ø 12 mm, inner Ø 7 mm, drilling depth 100 mm
Diamond hollow drill, outer Ø 12.5 mm, inner Ø 7.5 mm, drilling depth 100 mm
Grinding Machine
The surface grinding machine with swingable grinding head and precision
grinding spindle for mounting cup grinding wheels (Ø 125 mm) is available for the
preparation of test pieces used for RUL/CIC and HMOR measurements. The vertical
fine adjustment has a reading accuracy of 0.01 mm. The permanent magnet plate
(Ø 125 mm) is designed for clamping steel support devices. The wet grinding
device consists of a cooling agent vessel with a clearing tank, an electric immersion
pump, and a water-collection plate with plate slide, cock and hose line. A ceramic
cup grinding wheel (Ø 125 x 60 x Ø 20 mm) is included.
∙ Clamping device for holding test bodies, Ø 50 mm, height 50 mm, with reducing
∙
clamp rings for Ø 35.7 mm and Ø 30 mm
Cup grinding wheel made of a ceramic compound for soft to medium-hard test
∙
pieces, Ø 125 mm, height 60 mm, hole 20 mm
Diamond cup grind wheel for special hard ceramic materials, Ø 125 mm,
hole 32 mm, coating width 5 mm, coating height 2 mm, grain size Ø 100 µm for
∙
rough grinding
Diamond cup grinding wheel for special hard ceramic materials, Ø 125 mm,
hole 32 mm, coating width 5 mm, coating height 2 mm, grain size Ø 30 µm for
finish grinding
22
Sawing Machine for RUL/CIC and HMOR Systems
The NETZSCH sawing machine is used for cutting test pieces from refractories, stone,
ore, ceramics, glass and hard metals.
The circular blade cuts from bottom to top, plunging into the cooling agent tank
below the table and drawing the cooling agent into the cut over the shortest path.
The sawing machine consists of a plate (700 x 600 mm) with spindle for cutting
wheels of Ø 200 mm to 350 mm, a pole-reversible three-phase motor with motor
protection and foot switch revolutions of 3500 min-1 and 1750 min-1, and a feed
table. In addition, it comes with a clamping device, yoke support, prism support with
column, stop angle and guide pulley for automatic feed. Included are also a swing
and spindle along with hand bar and counter weight (with angle support). There is
a two-jawed vise that can be both turned and swung, and a three-jawed vise that
can be turned.
∙
cutting width 1.5 mm, max. cutting depth 45 mm, hole Ø 30 mm
Diamond cutoff wheel Ø 350) mm, with bronze-alloy bonding,
cutting width 1.8 mm, max. cutting depth 120 mm, hole Ø 30 mm
ource!
ro m one s
All f
23
The NETZSCH Group is an owner-managed, international technology
company with headquarters in Germany. The Business Units Analyzing &
Testing, Grinding & Dispersing and Pumps & Systems represent customized
solutions at the highest level. More than 3,700 employees in 36 countries and
a worldwide sales and service network ensure customer proximity and
competent service.
NGB · Refractory Materials · EN · 0420 · NWS · Technical specifications are subject to change.
NETZSCH-Gerätebau GmbH
Wittelsbacherstraße 42
95100 Selb
Germany
Tel.: +49 9287 881-0
Fax: +49 9287 881 505
at@netzsch.com