The effect of particle-size distribution on flow of refractory castables Elkem 2 RefractoriesThe effect of particle-size distribution on flow of refractory castables Bjorn Myhre im Refractor Abstract Norway The effect of the particle-size distribution on cas- ling characteristics has been investigated. for several castables. Due to the simple form, the equation given by Andreassen has been used to ‘outline the criteria of a castable with good flow Tchas been found that to obtain good flow, a Introduction and background table should contain more of the fine fraction than has earlier reported for optimum packi Furthermore it has been found that the particle size distribution of the finest fraction is very important, deciding the rheological behaviour of the castable Refractory monolithies are composed of refracto- ry aggregates bonded together by cements, clays, Sometimes. of binding agents or combinations of binding agents are added. The conventional refra castables tory consist of various aggregates, from firec lay to, tabular alumina, bonded together with calcium ‘aluminate cements Castable refractories appeared on the market in 1928, and was a commercial success by 1930. However, most of these were inferior to formed refractory shapes, and did not give the type of service-life that the fired refractories did Original refractory castables comtained calc! ‘aluminate cements that had been developed for their resistance to chemical attack and fast set ting properties. These cements were mixed with various refractory aggregates, commonly disca ded material from brick production, Henee, refractory monolithies were not considered equal to brick shapes Due to the widespread use of inferior raw materi- als, monolithic refractories could not replace shi ped and fired refractories in many applications ‘This meant that their growth was seve ely prohi bited until the late 60°s when monolithics with properties equal to bricks appeared. ‘The practise in producing castable refractories up to the early 70’s was to use higher purity ore strength was needed. This increased the cold str able, but added fluxes t0 the J product. The use of more cement lowe- red the refractoriness, as well as decreased its Hence, high temperature strength. a reverse effect of what was desired was actually obtained By using more cv nt, refractory mixes became less refractory and had Tess stre hat operating \ Before 1970, strengths were mea. peratures, sured mainly as cold modulus of rupture after heating a sample to a certain temperature, Actual strength at temperature was rarely ever conside: red. This probably led to a lot of misuse of pro ducts and was part of the reason that refractory monolitics did not gain their current accept ‘until the mid 70°s,Figure 1 Continous particle-size distribution curve for ‘maximum density safier Furnas. From reference 3 Particle packing In the simplest case, a refractory castable may be wacroscopically characterised as a coarse structure consisting of larger grog particles, or saregales, bonded together by a finer, viscous bond phase (matrix) that is able to harden, usually by the hydration of ae type of refractory, the a Cf similar or vastly different chemi It is evident tha almost i ‘combinations exist when both different unerewates, bonding matrixes and particle-size distributions are taken into account, The choice of aggregate, bond phase, their proportions and particle-size distributi ‘on for a particular refractory castable is determined by the application and economic considerations ‘The relative proportions of aggregates and bond phase, as well as particle-size distributions and, 10 some extent, the chemistry and mineralogy, affect the refractory castable, both the flow properties and the properties of the final refractory, ‘The use of particle packing principles in desig. ning refractory jixes provides the basis of the development of castables with low porosity Means for achieving high compaction in mortar and coneret were reported by Furnas! an Anderegg” in the early 1930°s, Fumas developed ‘a mathematical relationship for two different types of grading. One with intermittent or gap fading based on mixing two, three or four sizes, tand one grading based on a continuous size dis- ‘Tyler Mesh Size Uibution, According to MacZura et al.’ the gap sized distribution gives poor workability while f ‘ontinuous gives improved workability, low water requirement and good compactness rest fing in low shrinkage and high suength. However, there are indications! that gap sized distributions may give higher thermal shock resistance than the continuous, To obtain a particle-size distribution close t0 Furnas’ continuous grading, it is necessary to we the system into @ number of screened ns. In Figure 1, a calculated Furnas distri- bution t obtain mum density by optimum packing of particles in the range 0.2 to 4760 micron (4 mesh) particles is shown. This distri- bution is based on the assumption that particle packing of narrow sized fra ons of component materials is constant at 50 voids, Particle pac king curves are generally on a volume basis, but garded as weight for one component or for particles with similar density Parallel with Furnas, Andreassen* worked on the same problem, but with a different approach, Obje mns have been raised to calling Andreas- "s approach to packing a theory, we it part- ly represents an empirical study of particle pac king. However, the equation is so simple that itis easily applied 325 200100 48 28 18 8 4 os 10 Om je 30 et 4 440 208 S08 1100 23804760 99.9 ii GL % Undersize ot 1 10 Equivalent particle spher 100 ical dia. - wmerrr = (a/D)-100 Where CPFT is Cu ve Percent Finer Than (volume), dis particle-size, D is the maximum: particle-size and q is an exponent, To obtain opt ‘mum packing, Andreassen found that the expo: 1 should be between 1/3 and 1/2. If the expo nent is increased, this means an increase of coarse material, if it decreases, the amount of fines will increase, If log(CPET) is plotted against log. then q is found as the slope of the curve. Therefore is it common to present the particle size distributions in log-log plots. In a series of papers recently published, Di and F made @ comprebensive treatment of packing theories. According to computer si lations, the exponent of Andreassen’s equation should be 0.37 to get optimum particle packing According to Dinger and Funk, the following conclusions may be drawn “Distribuions with an exponent greater than optimum (i.e. 0.37) pack in a scheme appro. ching « minimum non-zero porosity. In other words, regardless of the width of the distribu- tion, porosity will never approach zero. The greater the value of the exponent, the higher the limiting porosity Distributions with exponents less than 0.37, Conventional castab! approach zero porosity as the width of the dis tribution increases. As finer and finer particles are added 1 the distribution, porosity will decrease and approach zero.” Hence, according to the above conclusion, it has tno meaning using exponents greater than 0.37 if the objective is to create a maximum packing den: sity. Furthermore, for castable systems, there is also a requirement for mobility of the various par ticles in order to place the castable, Mobility may be obtained by using more water, bu as it evapo. rates, poros! is the result, hence water should be minimised, ‘The wanted fluidity could be obtained. by keeping the coarser particles apart by a suspen- sion of fine pa es. The viscosity of this suspen sion should be suitable for the intended applicati: fon, and is determined by the amount of fines and superfines, and the state of flocculation within the suspension. An important factor in making a dense packi to widen the particle-size distribution, An inerea- sed maximum particle-size may reduce the total porosity of a system, However, other factors are usually determining the maximum particle-size. The option is then to expand the particle-size dis- tribution towards smaller and smaller particles, a development that was going on in the late 60°. ‘There are two main differences between a fired brick and a hydraulically bonded castable: a), the water content during shaping, and b) the role of the binder. During manufacture of e.g. high al mina bricks, the refractory mix is usually made plastic by the addition of 0.5-3% water, possibly with « temporary binder, then shaped under high pressure in a mould, Subsequent firing creates a ceramic bond which essentially is established belore the refractory is put in service, Ina com ventional hydraulic castable, a water content of 8- 15% is needed to obtain sufficient flow for the castable to be pled, The water reaets with the cement and creates a hydraulic bond that gives good mechanical strength at room temperature. A ceramie bond is not for until the castable has been heated t0 above 800-1000°C. Compared to a fired brick, this castable has seve: ral drawbacks of which high op perhaps the most important. The open porosity of porosity is a castable dried at 110°C is generally about 9- 17%, Even though some of the porosity is caused by air bubbles, the main contrib sult ‘of the water added during mixing, A major drawback of the conventional castables is closely connected to the cement content During the first heatup, the hydraulic bond is modified. At peratures between 250-350°C, the hydrates of the hydraulie bond loose theirwater and result in caleium aluminate phases as well as reactive &-Alj03, This reconstruction of the bond ph aand_ most conventional castables have a mini- 250-700°C!, ‘The hot- strength reaches a maximum at 800-1000°C due lowers the mechanical strength, mum strength between to the formation of a ceramic bond. At higher temperatures, the strength of silica containing astables diminishes due to liquid formation, In non-silica contai ng systems e.g. tabular alumi nna systems, this liquid formation does not occu hi and very high hot-strengths have been reported! As the bulk of refractory aggregates is within the Microsilica in castables sroup of alumina-silicates, the only viable way to improve hot-strength was to reduce the cement content of the castable, The formation of a vis- ‘cous liquid is deleterious both to corrosion resis- tance and hot strength, and the amount ata given temperature for a given is mainly dependent on the impurity content of the bond phase, ie. the quality and quantity of the cement. Even with a high-purity aluminous cement with 70-80% AlyO4, it is not possible to reduce the CaO content to a level below 3-4% for conventi- onal refractory eastables. ‘The need for castables with a reduced cement con- tent led 10 a substantial effort within the R&D departments of the various refractory companies, and it was French research that led to some very important patents on reduced cement castables, called Prost (1969)!8 and Lafarge (197744 patents. The first attempts to prove the p for mance of the refractory castibles by reducing, water and cement content were relatively unsue~ cessful due to low mechanical strength for compo- sitions with less than 10% cement. However, by addition of clay minerals in combination with a deflocculant, excellent strengths were obtained with cement contents of 5-8%. These ccastables, al cast had lower open porosity than con bles, and corrosion resistance way improved. One drawback was their tendeney to explosive spalling fon rapid heating. This was mainly due to the Fact that the chemically bonded water was liberated ‘over a narrow temperature range. Further development work, led to so-called explo: sion-proof castables. These are clay-free, and are placed with only 3-74 water. They are characteri- sed by a carefully graded particle-size distributio including superfine powders. In 197 Lafarge filed ‘a patent! where the cement content could be redu- cod 10 1% ‘The superfine powders should be particles with ‘no internal porosity and should be inert to water. Although an superfine powder may in principle be used, microsilica is preferred for most appli cations. As micrositica normally are the finest particles in the system, having a specific surface area of approx. 20m?gram, surface properties, and impurities are important in determining the properti contribute with more than 50% casting and settin of a castable, The ‘of the total surface area in certain mixes. Microsilica normally has a negative surface char- of approximately 20-30 n¥ in aqueous sys- mis, the zero point of charge being around pH 3. On the other hand, cement may show a iahtly positive charge. He wee, without disper ints added, the particles of the bond system will be attracted to each other, thus demanding a high amount of water to allow the particles to move freely relative to each other. The surface active agent, normally termed deflocculant (in Portland cement based syster ss termed plast superplasticiser), is believed to create an equal normally negative charge of the particles of the bond system. As the particles then will repel each other, casting can take place at reduced water additions ‘The deflocculating mechanism may vary betwe- fen an inorganic and an organic type dispersant Commonly used are sodium hexametaphosphate (inorganic) and sodium polyacrylate (organic), Results from Elkem Refractories laboratories indicate that the phosphates might actually adhe~re to the microsilica surface, more or less “clea ning” the surface from other impurities, whereas. high molecular weight organic molecules might actually “curl up” between the particles, keeping. them apart, When applying phosphates in casta- bles, offen a black surface film on the castuble being formed during vibration. This seems to be ¢arbon-containing impurities from amongst ‘others the microsilica surface. This effect m: rot be observed when organic defloceulants are used. ‘The effect of micrositica in a castable is at least dual. Onee properly dispersed, one important pro- perty is to reduce the cement content of refractory ceastables due to the small particle-size, Accord to the patents by Prost and Lafarge, the cement content of refractory « ables may be reduced 16 approximately 1% by using carefully graded part cles all the way down to sub-micron sizes. The use of supe ne particles is based on the assumption that in a castable with a class particle-size dis- tribution, the density is limited by intengranul voids that are filled with excess water during installation, These voids m be filled by successi- vely finer particles, thus replacing the water. The remaining micropores are filled by a gel of hyd ted cement. The use of these principles has lead to refractory castables with very low water demand, and consequently high compactness. Use of mierosilica reduces the open porosity from about 20-30% to 8-164 ater firing at 1000 al strength that is exp >, and the drop in mec need in onal castables at intermediate temperatu- res is altered to a steady increase. Acting as a filler is by no means the only effect of microsilica in refractory castables. It hay been Shown! in studies of & nent pastes with micro- silica that a certain fraction of the microsilica reacts with the cement and water to form so-cal- led CASH phases in addition w the CAH and AH phases normally found in hydrated cement The CASH phases are of zeolithic nature and the amount of these hydration products is dependent ‘on the quality (purity) of the micrositica, ‘The addition of microsilica was also found to alter the pore-size distribution towards finer pores, an ‘effect that is probably more of physical than che mical nature. During heating, the CASH phases convert to CAS3 and (probably) to cristobalite or quar, It should be stressed that successful use of both low, and in particular, ultralow-cement castables, is dependent on proper use and installation, Due to their high content of fines, these eastables are often thixotropi and requites vibration for pla- ‘cement. The recommended water addition should be stietly followed as the quality of the final refractory is very dependent on proper installati- ‘on. The water should be potable, One com problem found on site is the lack of suitable n This often results in too much wate added, a practice that is detrimental to the final properties of the castable. As ano ample! a fireclay based low-cement castable with 4-54% water may develop a cold crushing strength of 110 MPa. ‘This value drops to 80 MPa with 6% water, and around 50 MPa with 7% water. In addition, the se me will be negatively influen- cced and the final product will be more porous. The beneficial effect of microsilica in castables is well established both in theory and practice With superfine powders, dense packing is achie ved, and the cement content can be drastically 12 the actual amount of superfi- duced. Rew: ne powder added to the eastables, most papers do not give any figures except what can be deduced from the chemical analysis. However. 4 t0 5% seems to be relatively common. Ulvalow-cement castables have @ lime content below approximately 1.04 CaO, while the low coment castubles have lime contents between 2.5, and 1.0%. With their content of carefully graded .gregates and superfine particles, these oo classes have much in common, The main diffe- rence is the cement content and thereby their refractoriness,Figure 2. Tabular alumina based castables. Cateulated purtcie-size distribution of castables with 2and 8% microsilica and the theoretical Furnas curve according ta MacZura et ats. Experimental results and discussion Even though the particle-size distribution is one of the most important variables affecting the eas- Ling properties, it is rarely presented in literature. In the following, the effect of mierosilica additi ‘ons {0 a tabular alumina based refractory eastable ‘composition will be discussed. The particle-size distribution was composed to fit the distribution of Furn reasonably well, however there were discrepancies for the fraction below approxima tely 100 micron, The investigation covered casta- ble compositions with cement content from 1.5% to 7.5% and microsilica addition ranging from 0 to 10% cement will be reported here, More about these For brevity, only results with 1.5% castables, both cold and hot properties, can be found in the three papers: Tabular alumina based. tory castables part 13161718 Figure 2 shows the particle-size distributions (calculated from the particle size distributions of the individual components) for the tabular alumi- nna based castables with 1.5% cement and 2 or 8% microsilica and the Furnas distribution curve as given by MacZura et al.}. The calculated cur- ves were based on particle-size distributions. obtained by laser diffraction for the sub Fraction, and sieve curves for the coarser materi- al. The composition with 2% microsilica is clo- sest to the distribution given by Furnas, while that at 89% has much more microsilica than requi- Cumulative % ot 1 10 8% microsilica Furnas red according to the packing model. However, both have a close fit above approximately 100 Figure 3 shows the effect of microsilica additions fon flow and water demand for the 1.59% cement castables as a function of microsilica content measured by filling the Ko a cone (ASTM C230) Flow testing) placed on a vibrating table. The ‘The flow-values wi freshly mixed castable cone was removed and the castable vibrated for 15 sec. at a double amplitude of 0.75mm. The flow-value represents the % increase in the dia- meter of the cone. A value above $0 is normally regarded as sufficient for placing. It is seen that the addition of microsilica has a strong effect on both flow and water demand, In fact the mix with 0% microsilie Addi castable. ctically not was pr onally, it is seen that the optin ica content to obtain good flow with a minimum above 6% for this ccastable. The need for at least 6%, and preferably water addition is somewha ‘8%, microsilica was found to be consistent for all cement contents covered by the investigation From the particle-size distributions presented in Figure 2, one may speculate why this drama difference in flow and water demand should ‘occur. It seems that the distribution of Furnas as applied in this example is not very suited for this particular kind of castable, {i | 100 1000 10000 Particle size [micron]In Figure 4, a comparison is made between the particle-size distributions of Fumas, Andreassen and the tabular alumina based castable with 8% mnicrosilica, The castable having very good flow sat moderate water addition, fits relatively nice to the Andreassen distribution, In this case the ‘exponent was 0.22, a value that i far below the value of 0.37 found for optimum packing. This may reflect the need for mobility in the ease of ibles.- the particles must be able to move around each other= not just fit in the voids. A high amount of very fine particles properly dis- persed in the liquid phase, ereates the volume to Fill the voids between the coarser aggregates and to keep them apart so that good flowability is on of the fine ‘obtained. The particle-size distribut ‘material is probably also important, being able to cause effects ike dilatan The above results prompted a program to invest: gate the effect of particle-size distribution on flow, water demand, density and cold strength of two materials with very different p: ticle Shape: fused alumina with its angular appearance and fused silica with flaky glass particles. Because the particle-size distribution of Andte- aassen is so simple and easily applied, further work concentrated on using this model. Several ceastable compos jons were prepared to match the particle-size distribution of Andreassen close Chosen exponents, q, were from 0.2 to 0.35 in steps of 0.05. In Figure 5 the resultant particle- size distribution is shown for the fused alumin castable with a q-value of 0.3, The theoretical Andreassen distribution is also shown. The le compositions contained 1.5% 120 100 z” 2 32 6 s $ z 5 «0 = 20 o 8 Water addition [%] 2 Microsili = Fonvalue 6 8 a content [%] 0 —O— Water addition Andreassen, q=0.22 8% microsilica Furnas " if . HA it 8 5 0} 3 z 5 3 1 on 1 10 100 1000 10000 Particle size [micron Figure 3 Flow vatue and water ‘addition for 1.5% ‘cement, tabular alumina used refractory cast bles as a function of ‘microsilica content Figure 4 Particle-sice distribution of tabular alumina cas table with 1.5% cement and 8% microsilica together with distribu ‘ons as given hy Andrews sen and MacZura etal) (Furnas).Figure 5 Partiele-sice distribution Jora fused alumina based castable with a q- value of 0.3. The theore= tical distribution aceor dng to Andreassen Is ‘also shown, Figure 6. low-value as a fanction of distribution coefic- ent for refractory casta bles based on fused ale mina and fused silica 0 cement with fused alumina and 6% cement for the fused silica compositions, One must be aware that all distributions are based on volume, mea- ning that for fused alumina with large difference in demsity of the aggregate and the microsilica, all components must be transformed to volume the de ‘making it less important to use volume percent in percent. For fused sili ties are close, composing the mixture. The difference in densi ties and particle-size distribution of the compo~ nents, resulted in large differences in microsilica content for a given particle-size distribution, Ata ‘q-value of 0.2, a fused alumina castable contains approxima ly 10% microsiliea, while fused siti- cea contains approximately 23% microsilica In Figure 6 the flow-valucs are shown as a fune~ tion of the distribution coefficient, 4. The water Andreassen, q-0.3 100 = 0 q 5 81 04 o1 1 10 8 3 —O— Fused siica $ “A Fused alumina s & iva 025 Distribution coeficient [q-value] audition was 4% by weight for the fused alumina, % for the fused silica castable Due to the difference in density, the volume per cent of water added is similar, 14-15% by volu- ime. The best flowability is obtained with q-valu- sof 0.2 to 0.25, while the castable with a q- value of 0135 was not castable at the fixed water addition level. Another interesting aspect is that the particle shape has. seemingly only minor influence on flow. A possible interpretation may ‘be that the fine fraction of the composition, per- haps the material below 50 micron, is decisive {or the flow properties. In Figure 7 the cold crushing strength after dry. ing at 110°C and 12 hours firing at 600 or 1000°C is shown for the different particle-size distributions of fused alumina, The cold erushing, 400 1000 10000 0.30 035strength is very dependent on the distribution being highest for the lower g-values, This is in accordance with earlier experiences that has indi- more fines. At higher q-values, the strength decreases signif cantly. Still, for the particle-size distribution with 4 q-value of 0.35, the low strength isnot only caused by the distribution alone but also. by the absence of flow when prepa e castables, Fig fused silica compositions, ure 8 Shows the cold crushing strength of the ain it is apparent that the strength is dependent on the particle-size distribution with a relationship that is. almost ‘demtical to that obtained by the use of fused alu- The strongest samples are those with the highest amount of microsilica except after 1000°C where a distribution coefficient of 0.25 ives highest value. A q-value of 0.25 equals to approximately 8% and 159% microsilica for the fused alumina and fused silica castable respecti vely Iis commonly believed that the density of a cas table increases if more coarse material is used This is true if the maximum particle-size is inere ased. However, in the case of a fixed maximum value, this may not be so. In Figure 9, the bulk density of the fused silica and the fused alumi ceastables are shown after firing at 1000°C as function of the distribution coefficient, In the cease of the used silica eastable, the bulk density is directly related to the pucking efficiency. For the fused alumina sample, the picture is not cl ar-cut, Because of the large difference in density for microsilica and alumina (approximate 2.3 to 3.9), the theoretical density is a function of the microsilica content, i. the -value. To compli cate matters further, also the water addition in terms of volume is a function of the same, since 200 Cold crushing strength [MPa] 110 609 1000 Temperature [°C] 200 200 Cold crushing strength [MPa] 600 1000 Temperature [°C] Figure bles. Cold crushing strenguh of different par sice distributions as Figure 8 Fused silica cast Cold crushing sirength distributions as a funct 1"Figure 9, Bulk density of sed silica and fused alunina eastables as a function of particle-size distrib fuon, Samples fired 12h at 100°C Figure 10, Tabular alumina cast bles with 1.3% cement ‘and micrositica contents hereon O and IOs Calculate particle-size distributions forthe dif ferent microsilica con 2 water was added at a constant perventage by weight. Hence, the results from the fused silica compositions are more reliable in terms of jud- xing the packing efficiency as a funetion of parti cle-size distribution, Figure 9 shows that the den- sity of the fused silica castable decreases with increasing q-value. ‘This implies that with more coarse material in the castable, the amount of trapped air increases. If the results of the fused alumina is corrected for the variation q-value of 0.25 gives the best packing, closely followed by that of 0.2. A q-value of 0.3 gives Jower packing efficiency, and that with 0.35 much lower. However, the results are not really comparable, since also the volume of water added is dependent on the composition in this, case and will influence the results Reverting to the tabular alumina castables that gave the flow values presented in Figure 3, whe- re the addition of the finest fraction, i.e. microsi- fica, greatly improved the casting properties. Addition of microsilica effectively reduced the amount of water needed to obtain a specitic low Higher addition levels ie. 8 or 10wt% seemingly did not influence neither water requirement nor the Now significantly In Figure 10 the particle-size distribution curves of these tabular alumina castables are given. All , The values are transformed {© volum est curve represents the LOWw1% microsilica, the next highest the 8w1% microsilica, and so on. The lowest curve is the Ow% microsilica castable All the compositions had the same amount (weight %) of particles below 125 micron as microsilica substituted alumina fines. Because of the difference in density between alumina and ¢ g = on 2 a i g 2 Boos 8 2 2 5 ¢ § 3 = a0 5 os a & Cumulative % Ra 0 = a \ Particle si 10% microsilica go. microsilica 8 2 § @ 3 Lis § g é 1.90, 3 2 i 3 2 5 3 ww om ve Distribution coefficient [q-value] 100 1000 [micron] 10000microsifica, the curves do not join at 125 micron fas they would in the case of equal densities. In spite of the difference in casting characteristics there is seemingly little difference in the distribu- tions down to about 20 micron, Furthermore, the particle-size distribution is nearly gap-sized, with different slopes for the coarse and the fine fracti fon, and only about 10% material is between 20 ‘and 150 micron, Hence, the reason for the diffe rence in casting characteristics must be the parti cle-size distribution of the finest material, ie. the fraction below 125 micron, It is tempting to conclude that the particle-size distribution of the finest fraction is determining the flow characte- istics in this particular ease A. gap-sized distribution may be considered a combination of wo or more continues distributi- fons, Here, we have two main fractions, one abo ve 125 micron and one below approximately 30 micron, Figure 6 showed that thy particle-size distribution should have a q-value below appro ximate 0.3 t0 get good flow. This is probably most relevant for the “coarse” material, that builds ‘skeleton” of the castable and determi- the amount of fines. Ifthe distribution coef cient becomes too large, e.g. 0.35, there will be insufficient fines tand the coarse particles will interfere with cach other such that flow is obstructed. Therefore, is it important that the dis tribution coetfic ent for the coarse fr jon is not too high. In this particular case, the distribution \Lof the coarse material is approximate yo. (see Figure 4), a value that should provi- de enough fines for good flow. However, we know from Figure 3 that good flow is not obtai- ned unless a minimum of 6wt% microsilica is used. If the fine fraction does not have the right particle-size distribution, it may not pack opti ‘mum, thus requiring increased water addition. By increasing the microsiliea content of the tabular alumina castables shown in Figure 10, the distri- bution coefficient (slope of the logarithmic plot) of the fine fraction is lowered. At some point the distribution coefficient moves below a value that zzives good packing and good flow. If the results from flow-measurements (Figure 3) is compared to those of the particle-size distributions (Figure 10), itis seen that microsiliea enables a lowering the flow. The in water addition while maintaining feplaces the water, ie. the packing is improved. At microsilica levels above 6w1% 1 re is no significant effect on the flow. The distri- use of 6% microsilica may therefore represent the optimum q-value for these castables, A q-value of 0.37 has earlier been found to be the highest q-value giving zero porosity for an infin Funk"®), A distribu distribution (Dinger and on coefficient of 0.37 could therefore be regarded the maximum optimum packing. In Figure 10 a distribution coefficient of 0.37 is indicated for the fine fracti ‘on, It is seen that this approximately represents the slope of the castable with 6-8% microsiliea From the above discussion it is concluded that castable should have a particle-size distribution for the coarse “skeleton” according to a distribu tion coefficient of 0.3 or lower. With respect to the fine fraction, the distribution coe! jent can be somewhat higher, exemplified by a slope (q- value) of 0.37 in the logarithmie plotFigure 11 Particte-sice distribution ofa high cement vbracable com position Figure 12 Particle-size distribution of aself flowing, cement castable “ Examples The follow present some examples of parti cle-size distributions of different types of casta bles. Special emphasis is put on the effect of the particle-size distribution on casting characteris In Figure 11, the particle-size distribution of high-cement castable suited for vibration plac ment is shown, This eastable is characterised by very high strength and good flow when subjected to vibration. However, itis relatively vulnerable to incorrect water addition, as too much may result in s aration, This particular composition has a q-value f about 0.29. As higher g-values implies tower fines content, the coarser particles fof such castables will be closer packed. The coarse particles could interfere with each other, and obstruct the flow, unless energy is introduced. Cumulative % oa 1 10 during casting. Adding more water, will separate the aggregates and thus improve flow, but due to limited amount of fines, this may result in sepa ration/segregation, If, on the other hand, a casta- ble is composed using a lower q-value, more fines and superfines will be present, resulting in increased distance between the coarser aggreza- tes. Higher amounts of fines also makes the cas- table less susceptible to separation at higher water saldtion. However, all these effects are deper dent on a well dispersed system, In Figure 12 a high-cement castable with self-flo- swing characteristics is shown, It is based on the same raw materials as that presented in Fi 11, The eastable may Well be vibrated, but will at slightly higher water additions become self-flo- wing. Compared to the castable presented in 100 1000 Particle size [micron] 100 Cumulative % \ 90.23 on 1 10 100 41000 Particle size [micron]Figure 11, this one will be self-flowing at the same water addition as the other need vibration ‘casting (approximately 5.5% water), The next example, Figure 13, is a self-flowing tltralow-cement castable. This particular casta- ble is characterised by very good flow without vibration at low water additions 4% water) refracto resulting in very high ness (To, approx. 180°C) and very high strength at high temperature ( ho-M.OR, of 30 MPa at 1400°C). ed being hetween 60 and approximate- The distribution of this castable, is. gap: with the ly 15 micron. The coarse end of the distribution is according to a q-value of 0.21, whereas the fine end has @ steeper distribution, Due to the tow q-value of the aggregates, the amount of fines is, very high, this to provide minimum interference between the coarser particles, In Figure 13, also the distribution coeffi « Cumulative % E o4 1 10 value) of the finest fraction is indicated. ‘This seems to be around 0.37, indicated as optimum cearlier. This particular castable has a fine fraction that is composed of two powders; one essentially sub-micron (microsiliea) and one with a particle- size of 5-10 micron (calcined alumina), According 0 the previous discussion, it seemed likely that only slight variations in the amounts, of fines could change the rheological behaviour significantly. Particularly for changes resulting in higher q-values of the fines, To check this assumption, a small fraction of the ictosilica was replaced by reactive alumina, The castable became dilatant and jammed the mixer complete~ ly at the same water addition us the original com= position, although the low of these castables In Figure 14 is the particle-size distributions of the two self-fowing castable compositions and 100 1000 10000 Particle size [micron] Cumulative % « dilatant 0-1 _ i 100 1000 Particle size [micron] 10000 Figure 13, Particte-size distribution of a selPflowing, gap siced ultralow-cement ‘astable. The distribu ‘on coefficient is indica ted both forthe fine and the coarse fraction, Figure 14 Particle-size distribut ‘ons ofthe nso self fo wing compositions, The dilatant isthe lowest of the two curves 8g-values of the fine fraction shown, The particle size distributions are similar with q-values of 0.37 and 0.43, The lower curve is the ditatant ceastable havin, a. qevalue of 043. It is likely that the distribution-coefficient of the finest fraction determines whether the castable becomes dil tant, and that the total amount of fines is impor tant whether the castable becomes pote ally self flowing. It is possible to make a vibratable from a self-flowing composition by adding less water, however is it generally impossible make a self-flowing castuble from a typical vibratable. This is due to the higher content of fines in the self-flowing composition making it less susceptible to separation, Control of the dis: tribution of the finest particles is of vital impor- tance as has be scen in the above example. To avoid dil ney, i is impor a distribution coefficient of approximately 0.37 in the finest fraction. To reduce the q-value of a composition, more ofthe finest fraction has to be used. As this usually is microsili flow and pac King can be improved by increased additions. However, an upper limit for micrositica addition exist. At a level of 15-20 vol% the castables often become sticky, However, using defloccu- Tunis, good flow has been obtained with mierosi- lica contents in excess of 20 vol% A successful use of these high amounts of mi Conclusion silica is dependent on the micrositica quality Some microsil perform much better than fothers. ‘This is, at least partly, connected 10 the purity of the microsilica. The cement quality is another important factor when composing these densely packed castables, Sometimes it is easier to make ultralow-cement castables than high- cement castables, This is due to early stiffening that often occur at high cement contents. For such mixes is it imperative to use retarders, In hand, ultralow-cement castables on the oth Under any ay be a probl wees, the set time as 10 be adjusted (0 avoid premature stiffening and delayed Finally, it should be mentioned that there are other reasons for addi ‘0 alumina ceastables, in particular to ultralow-cement casta bles. Mierosilica serves as a source of silica for the formation of mullite at high temperature. ‘This reaction is very important for the develop- ‘ment of hot-strength, and a minimum amount of microsilica has to be added 10 obtain high hot strength 718.9, ‘The particle-size distribution of a castable deter mines the flow-properties. There has to be enough fine material pre "at so that placing is possible, The particle-size distribution of the finest fraction is also of vital importance Incorrect particle size distribution in this region may cause dilataney, or the castable may need. excess water to be placeable, If the packing model of Andreassen is applied to the system, results have shown that the coarse fraction of the castable should have a distribution coe ent not much higher than approximately 0.30. The finest fraction may have a distribution-coefficient ‘of up to 0.37. The present results have indicated that the distribution coefficient of the coarse fraction determines whether the castable beco- mes. potentially self-flowing. The distribution coefficient of the finest fraction, on the other hhand, determines whether the castable becomes diatantReferences TC. Furnas: "Grading Ageregares: FInd. Eng, Chem, 28,1052-58 (1931) FO. Anderese: "Grading Aggregates I, Ind. Eng. Chem, 23, 1058-64 (1931) 3G. MacZura, V. Gnauck and PT. Rothenbuchter in "Propoint of The First ternational Conference on Refractories” Now. 15-18, 1983 Tokyo, tapan, The Techn, Ass. Ref. Japan 1988 p.s500575 4 L-Homens, RC. Bradt in “Advances in Ceramies vol. 13, New Developments in Monolithic Refractories” ed by Robert E, Fisher, The Au. Ceram, Soe, ine. Columbus, Oto 1985 p. 110-130 5 AMM. Andreassen and J. Andersen, Kolloid Z, 30 (1930) 217-228 6 D.R. Dinger and LE, Funk, Inerceram 41 (1992) [10-14 D.R, Dinger and JE, Funk, Interceramm 41 (1992) (2198.97 8 DLR Dinge (31 176-179 9 DR. Dingerand J.8. Funk, Inerceram 41 (1992) 15) 332-334 10... Dinger and LE. Funk, nerceram 42 (1993) 131 150-152 1B, Clasaud, J.P. Kiehl and RD. Schon Whitley in “Preprint of The First nernational Conference fom Refractories" Nov. 15-18, 1983 Tokyo, Japan ‘The Techn. As. Refr. Japan 1983 p.589-6006 12 G. MacZura, HE. Kopanda and FJ, Rob in“ Advances in Ceramics vol 13, New Developments fn Monolithic Refractories” ed. by Robert E. 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