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Eur. Phys. J. Special Topics 220, 101110 (2013) EDP Sciences, Springer-Verlag 2013 DOI: 10.

1140/epjst/e2013-01800-9

THE EUROPEAN PHYSICAL JOURNAL


SPECIAL TOPICS

Regular Article

Viscosity of liquid metal suspensions experimental approaches and open issues


Dmitry Borina and Stefan Odenbach
Technische Universit at Dresden, Institute of Fluid Mechanics, 01062 Dresden, Germany Received 17 December 2012 / Received in nal form 5 February 2013 Published online 26 March 2013 Abstract. Knowing the viscosity of metal melts with suspended particles is necessary to interpret experimental results and to simulate uid ow in such materials. At present, reliable viscosity data is only available for pure metals and alloys. In order to study the viscosity behavior of metal melts with suspended solid particles in detail, samples with dened particle amounts are needed. Various methods of incorporating particles into the metallic melts were evaluated, and viscosity was experimentally determined using an oscillating cup technique. It was shown that solid particles in suspension change the melts viscosities dramatically, far beyond the eects expected from normal colloidal rheology.

1 Introduction
Liquid metal suspensions are essential to numerous applications, such as the production of metal foams and particle-reinforced metal composites [13]. Furthermore, metal in a mushy or semi-solid state includes both solid and liquid components and therefore is identied as a suspension as well [4]. Thus, the thermophysical properties, and particularly the viscosity, of metal melt suspensions is relevant to both basic research and industrial metallurgical tasks [57]. Realistic data are needed to interpret experimental results and to simulate uid ow in such materials. Previous fundamental assumptions about the rheology of the liquid metal systems suggests that they should be considered as Newtonian uids, i.e. the viscosity of the liquid metal is independent of shear deformation [8]. However, data presented in the literature show a variation in the evaluated viscosity of metals up to several hundred percent [6, 812]. The Newtonian behavior is still not veried, and there is a lack of understanding of the liquid metals rheology [13]. Moreover, theoretical studies using non-equilibrium molecular dynamics simulations predict shear thinning behavior of the molten metal [14, 15]. Despite some discrepancies, investigations of the viscous behavior of pure melts are quite comprehensive. However, information about melts containing solid particles is rare. In the majority of cases, investigations are limited to the consideration of metal alloys in the semi-solid state [1619] and signicant deviation from the Newtonian has been observed in their ow behavior. According to well-established colloidal rheology,
a

e-mail: dmitry.borin@tu-dresden.de

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Fig. 1. Schematic representation of the methods to incorporate the solid particles into metal melts: a) mechanical stirring; b) electromagnetic stirring; c) laser injection.

the presence of solid particles in a liquid matrix leads to an increase in viscosity. Furthermore, even small changes in the particle concentration can dramatically inuence the rheology of the liquid [20]. Therefore, only suspensions with an accurately dened amount of solid should be used in rheological analysis. Incorporation of the powder material in the molten metal has been a technological problem for many years, and numerous patents [2126] and publications [13, 2729] are devoted to this topic. Nevertheless, there are still no satisfactory methods of incorporating an exact amount of solid particles into metal melts [30]. In this study, methods of particle incorporation into the liquid metal, including mechanical and electromagnetic stirring, laser injection and metallurgical sintering have been considered and evaluated. Moreover, the viscosity of metal suspensions was determined experimentally using an oscillating cup technique. Experimental approaches, problems and results are discussed below.

2 Incorporation of the solid particles into metal melts


High melting points of liquid metals, as well as their chemical reactivity, restrict experimental methods and make it dicult to incorporate a known concentration of solid particles. For the incorporation experiments, various combinations of metals and solid particles were used. In addition to the problem of successful dispersion, the metal suspension should be suciently stable. Therefore, particles with approximately the same density as the matrix metal should be used, and so the choice of material for the particles is limited. Pure metals including Sn, Ga and Pb, as well as low-melting alloys such as Woods metal (eutectic alloy of Bi, Pb, Sn and Cd) and the eutectic of Ga, In and Sn were used for the liquid phase. Both metallic and ceramic particles were used for the solid phase, inter alia oxides of the metals used for the liquid phase as well as Cu, ZrB and ZrO particles. We also considered dierent laboratory techniques for introducing solid particles into metal melts. 2.1 Methods 2.1.1 Mechanical stirring Mechanical dispersion of particles in the melt can be achieved by a conventional overhead stirrer (Fig. 1(a)). According to the DIN 28131, a propeller mixer and diagonal at blade agitator in axial arrangement are applicable. However, two crucial diculties come with this procedure. First, mechanical stirring cannot be performed in

Electromagnetic Flow Control in Metallurgy, Crystal Growth and Electrochemistry 103

Fig. 2. Microscopic pictures of Woods metal with PbO (a) and Cu (b) particles as a result of the mechanical stirring with an inorganic protection layer.

an oxygen-containing atmosphere, due to the strong oxidizing tendency of the metal melt. Second, the stirrer is in direct contact with liquid metal, which has a high reactivity. Therefore, reaction of the melt with the stirrer should be prevented by a proper choice of stirrer material or with a suitable coating of its surface. A solution to prevent oxidation is to use a vacuum oven lled with an inert gas. This is an appropriate technique for industrial applications. Otherwise, the free surface of the melt can be covered with a protective layer, a technique well-known in welding. In our experiments, dierent ux melting agents including rosin, an organic and an inorganic agents were used to protect the melt from oxidation during stirring. The ux covers the surface of the metal before it has been melted to prevent the appearance of a thick oxidation lm. Particles are incorporated after the metal is in the liquid state. The microstructure of solidied samples was studied using optical and scanning electron microscopy after the particles were incorporated into the melt. Samples made of a material with a low melting point were frozen in liquid nitrogen and fractured. Samples with a melting point higher than 200 C were sawed and polished by conventional metallographic procedure prior to microscopy. With one of these two methods, samples with various combinations of particles and metals were analyzed. Results showed that an inorganic layer can successfully be used to avoid oxidation of the liquid metal surface during the incorporation of the solid particles through intensive mechanical stirring (Fig. 2). However, the migration or alloying of copper particles into the liquid matrix was observed, which makes further rheological study of this composite meaningless.

2.1.2 Electromagnetic stirring The electromagnetic stirring of liquid metals has the advantage of being a contactless process [31, 32]. The melt is placed in a non-magnetic vessel under the inuence of a moving magnetic eld, which induces an electric current in the metal. The current and the applied eld generate a Lorentz force, which initiates ow in the liquid metal. In our experiments, a combination of a rotating and traveling magnetic eld was used to produce an intense contact between the liquid melt and the solid particles (Fig. 1(b)). The microstructure of the solidied samples showed that all attempts to disperse particles in the melts were unsuccessful. Flow induced by the Lorentz force in the metal is not strong enough to incorporate the particles.

2.1.3 Laser Melt Injection Another possible method to disperse particles in the melt utilizes thermal Marangoni convection [34]. In this process, the surface of the solid metal is locally melted by a laser beam and solid particles are injected into the melt pool through a special nozzle (Fig. 1(c)). Results of the laser melt injection are presented in Figure 3. Due to the

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Fig. 3. SEM pictures of Ga with suspended ZrB2 (a) and ZrO2 (b) particles as a result of the laser melt injection.

Fig. 4. Particles of SnO2 incorporated into the Sn as a result of metallurgical sintering.

high energy used in this method, it is necessary to use particles above a certain size. Particles may be divided or even destroyed by the laser if their size is underestimated. Furthermore, particles were dispersed in the metal inhomogeneously, and it was not possible to suciently control the amount of solid that was incorporated.

2.1.4 Metallurgical sintering Pressure-induced deformation and sintering processes should force the particle to connect with the metal [35]. In this procedure, metal and oxide powders in the desired fractions are shear-mixed and pressed uniaxially. To avoid the appearance of the dross in the melt, an additional extrusion should be done after the sample has been pressed. With a technique described in [36, 37] the sample is pressed through an angular die so that the deformation is purely shear. This leads to the destruction of the oxide lm on the surface of the powders particles. As a result, the molten metal will be almost free of dross. Whatever of it is left in the melt after extrusion should be removed by the rst melting. Additional improvement could be achieved if the powder processing is done in an inert atmosphere. The successful result of sintering the Sn02 particles in the Sn-matrix is shown in Figure 4. This method produces a concentrated composite which can be further diluted. The pure metal is mixed with a previously prepared composite in the solid state and melted afterwards. High intensity ultrasonic pulses are used in the next step to mix the suspension by cavitation and the acoustic streaming eect [33]. Metallographic studies of the samples prepared in this way have shown its eciency. However, the optically observed concentration of the solid particles is mostly inconsistent with the intended value.

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2.2 Discussion Productive incorporation of particles into liquid metal depends mainly on three mutually correlated factors. The rst of these is the tendency of the melt to wet the particles surfaces. In particular, liquid metals do not wet ceramic particles well [26, 30, 39]. In addition, the relatively high surface tension of the liquid metals opposes the incorporation of the particles [8, 40]. Furthermore, the size of the particles has an impact on the dispersion. According to [26], the smaller the size of the particles, the greater the signicance of surface eects compared to volume eects, hindering the incorporation process. Successful particle incorporation has been observed in the case of mechanical stirring with an inorganic protection layer and through the laser melt injection process. An important disadvantage of the mechanical stirring procedure is the high toxicity and corrosive action of inorganic agents. Moreover, these agents contain halides, which can inuence the rheology of the liquid metals [4143]. In contrast to mechanical stirring, only an undened amount of solid particles can be introduced through laser melt injection. Furthermore, particles injected by the laser are distributed in the volume inhomogeneously. It may be presumed that electromagnetic stirring should result in increased homogeneity of the particles distribution. However, whether the Lorentz force can provide enough energy for the dispersion process is still an open question. The most appropriate method for controlled particle incorporation is metallurgical sintering, combined with ultrasonic stirring for further dilution of the composite in the liquid state. However, the results of this method are also not certain.

3 Viscosity of liquid metals with suspended particles


The experimental determination of thermophysical properties like the viscosity of melts has been a research focus for many years. Due to the low viscosity of liquid metals, their chemical reactivity, and high melting point, only a few experimental methods have been proven suitable [6,8, 44]. The most commonly used method is the oscillating cup technique [9, 4548]. In this method, the viscosity is determined from the decrement and time period of the motion of a vessel lled with the liquid which is put into oscillation around the vertical axis of the vessel. The shear rate applied to the uid during the oscillating cup measurement is not constant with time and diers for each oscillation. The maximal estimated magnitude of the shear rate in the oscillating crucible is usually 1 s1 [49]. The applicability of the rotational technique for this range of slow deformations in liquid metals has not been proven [13, 44]. However, to calculate the zero-shear viscosity of suspensions, measurements of the minimal shear deformation are necessary [20]. We performed experiments with an oscillating cup viscometer, built according to [8], and results for dierent metal suspensions are presented below.

3.1 Theoretical predictions The presence of solid incorporations will change the velocity distribution in a owing liquid and will lead to the increase in viscosity due to the extra energy dissipation. The zero-shear viscosity of diluted colloidal suspensions can be estimated with the classical theoretical predictions given by Einstein [50, 51] and by Batchelor [52].

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Einstein has calculated the shear viscosity of a suspension with a volume concentration in a carrier liquid with a viscosity 0 as follows: () = 0 (1 + 2.5). (1)

Einsteins formula is obtained from the viscous dissipation produced by the ow around a single hard sphere and is valid for very dilute systems ( <3 vol.%) without any interaction between neighboring particles. Moreover, such assumptions as incompressibility of the uid, creeping ow, neutral density, no slip between the particle and the uid, no particle migration as well as locality of the velocity perturbation due to a particle were used in the analysis. The numerical factor 2.5 in the equation (1) is valid for spheres and represents the intrinsic viscosity, which is the dilute limit of the viscosity increment per unit volume fraction, divided by the carrier liquid viscosity. In Batchelors prediction, which is one of the extensions of Einsteins results, the inuence of thermodynamic forces on particles is considered. Batchelor solved numerically the dierential equation representing the eects of the bulk deforming motion and the Brownian motion on the probability density of the separation vector of particle pairs in a dilute suspension. As a result the eective viscosity is calculated as follows: (2) () = 0 (1 + 2.5 + 6.22 ). This prediction takes into account the eect of two-body interactions and is valid for <10 vol.%. Further predictions [20, 53] evaluate the viscosity of concentrated suspensions and are not related to the current topic. A detailed theory of viscosity of liquid metals with suspended particles is actually missing and the experiments discussed below may serve as a rst step towards an understanding of viscosity of liquid metal suspensions. 3.2 Experimental results 3.2.1 Water-based colloid To prove that the oscillating cup technique can provide realistic viscosity measurements for classical colloids, a suspension of hollow glass spheres in an iron(III)-chloride aqueous solution was characterized. The concentration of the solid phase was varied within the range of 0 and 3 vol.%. The dependence of the viscosity on the concentration of the solid is shown in Figure 5. During the oscillating cup experiment, the temperature was not controlled and varied between 22.7 and 23.2 C. The results were compared to the theoretical predictions considered above. The decrease in the suspensions shear viscosity due to the temperature increase during measurement and the tolerance determined by statistical error calculations do not invalidate classical colloid rheology as a framework for analyzing the results. Thus, the oscillating cup method is applicable for measurements of the colloids shear viscosities. 3.2.2 Metal suspensions The viscosity of suspensions of ZrB2 and ZrO2 particles in liquid Ga was measured at the temperature of 45 C. The solid particles were introduced by the laser melt injection method, and their exact amount is undened. Nevertheless, the concentration of particles did not exceed 3 vol.%. Measured viscosity values are given in Table 1. The presence of particles does not inuence the viscosity of the liquid Ga. The experimental values cannot be compared to theoretical predictions because the concentration of the powder is unknown. Calculation of the viscosity according to

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experiment model by Einstein model by Batchelor

14

Viscosity, mPa*s

12

10

6 -0.5 0 0.5 1 1.5 2 2.5 3

Concentration, vol. %

Fig. 5. Viscosity of the water-based suspension as a function of the concentration of the solid fraction measured with the oscillating cup technique. Solid lines show the theoretical prediction for the viscosity based on the models by Einstein and Batchelor. Table 1. The viscosity of gallium-based suspensions at 45 C. Ga 2.59 0.15 mPa s
3.5 experiment prediction by Einstein 3

Ga+ZrB2 < 3 vol.% 2.58 0.16 mPa s

Ga+ZrO2 < 3 vol.% 2.69 0.10 mPa s

Viscosity, mPa*s

2.5

1.5 0 0.5 1 1.5 2 2.5

Concentration of SnO2, vol. %

Fig. 6. Measured viscosity of liquid Sn as a function of the concentration of suspended SnO2 particles at the temperature of 350 C. The solid line shows the theoretical prediction based on the model of Einstein (Eq. (1)).

Equation (1) for = 3 vol.% gives a value of = 2.78 mPas, which is higher than the experimentally obtained results. Probably, the amount of eectively suspended particles is not sucient for a pronounced eect. Using a material with a higher melting point, the solid was incorporated into the metal through a sintering procedure performed in our own facilities. Solid particles of Sn02 were introduced into the Sn-matrix with a concentration of 3 vol.%. The sintered composite was diluted by the addition of pure Sn with further ultrasonic stirring for homogenization. The dependence of the viscosity on the concentration of solid particles for the tin-based suspension at T = 350 C is shown in the Figure 6.

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Viscosity, mPa*s

pure Pb (experiment) pure Pb (literature) Pb with 0.9 vol. % of Pb203 Pb with 6.6 vol. % of Pb203 prediction by Einstein prediction by Batchelor

2 600 620 640 660 680 700

T,K

Fig. 7. Measured viscosity of liquid Pb with dierent concentrations of suspended Pb2 O3 particles [54, 55]. Literature values have been taken from [8]. The dashed and solid lines show the theoretical prediction for the viscosity based on the models by Einstein (for 0.9 vol.%, solid line) and Batchelor (for 6.6 vol.%, dashed line) respectively.

In contrast to the gallium-based suspension, the viscosity of the liquid tin signicantly increases if solid particles are introduced. Einsteins prediction (Eq. (1)) fails even for the smallest concentration (0.7 vol.%), even considering the tolerance in the amount of particles. Thus, colloidal rheology cannot be applied to such metal suspensions. The inuence of the solid particles on the viscosity of liquid lead were studied in [54, 55]. The solid particles have been incorporated into the metal through a sintering procedure. Figure 7 shows a dramatic increase in the viscosity of the melt with increasing concentration of solid particles. The relative change in the melts viscosity for a volume concentration of 0.9 vol.% of Pb2 O3 particles is about 35%, and, for a concentration of 6.6 vol.%, the increase is more than 100%. Moreover, the dependence of viscosity on temperature is considerably weaker for the higher volume fraction. These results cannot be explained by the classical theoretical predictions for the viscosity of colloidal suspensions (Eqs. (1) and (2)). The reason for the tremendous changes is unclear at this point. The inuence of the dross, which may be present in the volume of the melted lead, on the data cannot be disregarded.

4 Conclusion
With oscillating cup viscosimetry, it could be shown that solid particles suspended in a liquid metal can change the melts viscosity far beyond the eects expected from normal colloidal rheology, and the eect of the solid particles is dependent on the composition of the suspension. Particles of Sn and Pb oxides, when suspended in liquid Sn and Pb, dramatically change the viscosity of the melts, while the eect has not been conrmed for liquid gallium with incorporated solid particles. The variation in the behavior of these systems can be attributed to material-dependent properties. We have evaluated several methods of incorporating solids into the metallic melts, but none of them were found to give consistent results. In most cases, the amount of the incorporated particles could not be controlled. Metallurgical sintering is the most suitable technique investigated. It can be combined with a stirring method for further homogenization, as it was done for the dilution of the Sn-based suspension. However, it should be examined whether the sintering process itself can has an inuence on the purity and viscosity of the metal suspension through the presence of the dross.

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Furthermore, experiments on diverse metal-particle systems should be done to clarify the basis of the inuence of solid particles on the rheology of metallic melts and to provide realistic data for metallurgical applications and theoretical research. Moreover, possible inuence of the shear deformation, known from the rheology of colloids, such as shear thinning or thickening, should be addressed in further studies. Therefore, the implementation of the rotational rheometry is the next challenge in the rheology of the metal suspensions.
Financial support by the Deutsche Forschungsgemeinschaft through the Collaborated Research Center Electromagnetic ow control in metallurgy, crystal growth and electrochemistry (SFB-609, project A11) is gratefully acknowledged. We acknowledge the support of project A2 during the measurements with electromagnetic stirring, as well as contributions to this study made by Christoph Jakobitz, Lisa Sprenger, Martin Queck and Thomas Richter.

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