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T. Volkov-Husovic, R.Jancic, K.Raic
Faculty of Technology and Metallurgy, Dept. Metall. Eng. Karnegijeva 4, 11000 Belgrade,
Serbia and Montenegro,

Abstract: Thermal stability of the refractory material with the content of 60 % A12O3 was investigated. Water
quench test (JUS.B.D8.319.) was applied as experimental method for thermal stability testing. Damage of porous
materials is commonly related to a modification of mechanical strength that is mostly a reduction. This is linked
with* characteristics related to pore space. Mechanical characteristics are considered such as compressive
strength, dynamic modulus of elasticity and resistance parameters resulting from resonance frequency
measurements, as well as ultrasonic velocity.
Key words: alumina based refractories, dynamic Young modulus, fracture resistance parameters, thermal

Thermal shock stability dictates refractory performance in many applications. In many instances, a
two -fold approach, i.e. 1) material properties [1-8] or/and 2) heat transfer conditions [8-13] is taken to
characterize thermal shock behavior of the refractories. As an alternative, information on the thermal
shock behavior of refractories can be obtained by experimental means. One test for this purpose,
which is highly popular because of its simplicity, consists of quenching appropriate specimens from an
oven temperature into a medium such as water, liquid metal, oil, or fused salts maintained at a lower
Damage of porous materials is commonly related to a modification of mechanical strength that is
mostly a reduction. This is above all linked with characteristics related to pore space. One has to
realize what type of test procedures and also criteria are all available and come into consideration for
any corresponding correlation. On one hand, structure-related characteristics such as pore volume and
pore size distribution can be cited here as well as some discrete values deduced therefrom, but also
water absorpcion, saturation coefficient and diffusivity. Whereas on the other hand, mechanical data
are considered such as compressive strength, dynamic modulus of elasticity resulting from resonance
frequency measurmets, as well as ultrasonic velocity.
Thermal quenching of the refractories leads to the crack nucleation and/or propagation resulting in loss
of strength. Since the formation of the cracks has profound influence on the ultrasonic velocity and the
Young modulus of the material, measuring either of these properties can directly monitor the
development of the thermal shock damage level.

The ultrasonic technique can be used to characterize selected properties of refractories because sonic
pulses travel trought a medium at a rate that is directly affected by the material properties, and internal
structure. Comparing similar materials sonic pulses will travel faster trought the densier samples,
although the interpretation of the results can also be affected by the presence of internal flaws, voids or
cracks. The measurment of ultrasonic velocity was done using the equipment OYO model 5210
according to the standard testing ( JUS.D.B8.121.). The transducers were rigidly placed on the two
parallel faces of the cylindrical specimen using vaseline grease as the coupling medium. The ultrasonic

Proceedings of 3rd BMC-2003-Ohnd, R. Macedonia

2 and assumed not to change with the development of thermal shock damage. R. a p (MPa) 54 Young modulus. Macedonia 321 . By determining the bulk density.Poasson ratio and p .1. and 2. Thermal and Mechanical Properties of the Samples Studied Parameter value A12O3.17] and previous work [18-26] that will not be grate restriction.06 Thermal expansion coefficient. Table I. RESULTS AND DISCUSSION The effect of the thermal quenching on the ultrasonic velocities is given on the figures 1. Proceedings of 3rd BMC-2003-Ohnd. p (g/cm3) 3.density (kN/m3).8 Compressive strength. MATERIAL The refractory samples used in the present study were obtained directly from commercial producer.62 Specific heat. velosity was then calculated from the spasing of the transducers and the waveform time delay on the osciloscope. and ultrasonic velosity it is possible to calculate the dynamic Young modulus using the equation: (1) where:Vp .ultrasonic velocity of longitudinal waves (m/s).Vs . k (W/mK) 1. a (%) 0. These results suggests that changes in ultrasonic velocities colud be used as nondestructive monitoring the thermal shock damage in material caused by thermal shock. N) 18 3.70 Thermal stability (number of quench experiments. According to the literarture [14. This type of refractory was used in several previous studies in which a number of physical properties related to their thermal shock behavior were measured [17-26]. The value μ was given at 0. E ( GPa) 16. From the figures. 2. as well as from the regression analysis very good correlation was obtained between degradation of the ultrasonic velocity caused by the thermal shock. c (kJ/kgK) 1.05 Thermal conductivity. (%) 60 Density. .RELATIONSHIP BETWEEN MECHANICAL CHARACTERISTICS AND.ultrasonic velosity of transverzal waves (m/s)^ .

described as: (2.RELATIONSHIP BETWEEN MECHANICAL CHARACTERISTICS AND.The results from literature [16] indicates thet the percent difference between experimental and calculated values can range between ±5% to ±10%. MPa) degradation as function of number of cycles of the quench experiment (N) As the very good results were obtained monitoring changes in ultrasonic velocites. 1400 3500 • t 3000^ 1000 2500l Q . UIstrasonic velocity (Vp) of longitudinal vawes versus number of cycles of teh quench experiment (N) Figure 2. 20 16 14 i 6 64 2 0 • • 5 10 15 20 N Figure 3. 2000 >" (A > 1500 800 600 400 1000 200 500- 0 o• c 5 10 IS 0 20 5 10 15 20 N N Figure 1.) 322 Proceedings of 3rd BMC-2003-Ohrid. Compressive strength (o. Unfortunatly. With the simplicity of the method it should be always be possible to generate a usable modulus of elasticity value for a refractory product. The good agreement between decrising the Young modulus and number of cycles suggests that thermal shock damage could also be quantitatively evaluated nondestructively by measuring the dynamic Young modulus. UIstrasonic velocity (Vs) of transverzal vawes versus number of cycles of quench experiment (N) The effect of the thermal shock fatique on the Young modulus is shown on the figure 3. R. Dynamic Young modulus as function of number of cycles of the quench experiment (N) Figure 4.. but there are certain ocasions where experimental E measuments are not feasible. although it must be remembered that there may be a significant error in the values obtained. Expression for the strength degradation was used [14]. coefficient of correlation is in this case lower than it was in comparison the ultrasonic velocity with the number of cycles (Table II). The calculated values of dynamic Young modulus must be considered as an aproximation. that was used for the correlation of strength degradation caused by thermal shock. and a calculated value at least yelds a usable number . Macedonia .

ref. excellent correlation between fracture resistance parameters degradation with the number of cycles of the quench experiment was oserved (Table II).material constant ( n = 0.first fracture resistance parameter.v) / E a and R = k R) as well as for the damage resistance parameters (R'" = E/a^(l-v) and R"" = y R'").).RELATIONSHIP BETWEEN MECHANICAL CHARACTERISTICS AND.second damage resistance parameter. where o~0 . R.second fracture resistance parameter. Damage resistance parameters versus nuber of cycles show the opposite corretaltion. C . Proceedings of 3 rd BMC-2003-Ohrid. and usual equations were used for fracture resistance parameters (R = a ( 1 . A .5. Higher values of damage resistance parameters are expected for the lower values of number of quench compressive strength of the material before exposure material to the theraml shock testing and n . D . 25 20 15 CE 10 5 0 ) 5 10 15 20 N Fig.first damage resistance parameter. were also presented in figure 5. Higher values of fracture resistance parameters are expected for the higer value of number of cycles of the water quench test. Resistance parameters behavior as function of number of cycles of the quench experiment (N). High values of coefficient of correlation suggests that degradation in strength during thermal stability testing is in strong correlation with the water quench test experiment results. From the figure 5. Thermal shock stability of the refractories could be presented using resistance parameters [1-4] Fracture and damage resistance parameters were calculated from thermal and mechanic properties listed in Table I. 14.. . B . Degradation of resistance parameters due to the degradation of strength.488. Macedonia 323 .

Monitoring of thermal shock damage development in refractories by nondestructive method is of much industrial significance in relation to productivity as well as safety.670 3.Vol. the damage level in material could be predicted with very good accourance.7 666-669 (1965) 324 Proceedings of 3rd BMC-2003-Ohrid. and as they are related to damage. Vol 48. No 11. bulk density.014 5.898 0.H.Ceram. Table II: Regression statistics for the observed correlations Regression Statistics Multiple R R Square Adjusted R Square Standard Error Vp-N Vs-N Edyn-N a-N R-N R'-N R'"-N R""-N 0. Monitoring the damage level could be obtained using the decrising of the ultrasonic velosity. J.948 0.851 0.H.Am. Am. 52 .948 0.872 0.865 0. Hasselman.RELATIONSHIP BETWEEN MECHANICAL CHARACTERISTICS AND.987 0. include modulus of elasticity .963 333.680 0.Am.986 0. " Experimental Evidence for Thermal Shock Damage Resistance ".88 3. M.922 0. 45 .895 0. J. No. J.898 0. Prediction of strength degradation could be very useful parameter to know for life time prediction of material.970 0. " Direct Measurments of Fracture Energies of Brittle Heterogenius Materials ". 600 -604 (1969) [2] D.06 0.587 ( 1965) [4] J.P.Ceram. Also.9 42. Results of the method could be obtain very fast.973 0.P. CONCLUSION .Ceram Soc. Soc.Am.987 0. Results presented in this study suggests that the resuts of the sonic measurments could be used for prediction of damage level in specimen due to the thermal shock. several examples are presented in this paper.Cer. No.18 1. and growth of the parameters caused by quench experiments was observed. as the results in the Chapter 4. Literature [1] D. Vol 46. " Unified Theory of Thermal Shock Fracture Initation and Crack Propagation in Brittle Ceramics ". 583 .Soc. Sonic measurment is very usefull tool to solve this problem since the advantages are: Type of instrument is small.. . " Elastic Energy at Fracture and Surface Energy as Design Criteria for Thermal Shock ". limited only by imagination of the user. Amer. Physival properties that are commonly correlated with ultrasonic measurments are apparent porosity.865 0.860 0.Ishizuka.973 0.946 0. modulus of rupture and cold crusging strength.964 0. No 11.l.801 0. with very strong correlation with the number of cycles of the quench experiment (N). portable and operates on either line or self-contained battery power.959 0. permeability.Soc.Soc. 535-540 ( 1963) [3] J. The non-destructive evaluation of refractory products by sonic measurments has proven to be a very useful characterization tool. The lower values of the coefficient of correlation with the water quench results in that case suggests more acurate analysis. Vol.16 3.Nakayama. such as resistance parameters were also cosidered for analysis. Thereby it is posible to generate qualitative and/or quantitative results.Nakayama J. suggests the decrining of the Young modulus could be also used for the same purpose. Calculable material properties based on ultrasonic velocity data.760 0. Strength degradation in material due to thermal schoking also could be evaluated.966 0. possibly combined with other correlation to get more accurate prediction. Fracture resistance parameters degradation caused by quench experiments was also observed with excellent correlation with the number of cycles of water quench test. Hasselman.Ceram.Bull. Damage resistance parameters showed the opposite bahavior. R Macedonia . There is a great diversity of more potencial applications.

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