ISSN 00360295, Russian Metallurgy (Metally), Vol. 2013, No. 8, pp. 600–606. © Pleiades Publishing, Ltd., 2013. Original Russian Text © L.T. Denisova, V.M. Denisov, S.A. Istomin, E.A. Pastukhov, N.V. Korchemkina, 2013, published in Rasplavy, 2013, No. 3, pp. 74–82.

Oxidation of Liquid Ternary BismuthBased Alloys L. T. Denisova*, V. M. Denisov, S. A. Istomin, E. A. Pastukhov, and N. V. Korchemkina Institute of Nonferrous Metals and Materials Science, Siberian Federal University, Svobodnyi pr. 79, Krasnoyarsk, 660041 Russia Institute of Metallurgy, Ural Branch, Russian Academy of Sciences, ul. Amundsena 101, Yekaterinburg, 620016 Russia *email: [email protected] Received February 19, 2013

Abstract—The oxidation of liquid alloys Bi–Ag–Cu, Bi–Ag–Ge, Bi–Ag–Sn, Bi–Ag–Pb, Bi–Cu–Sn, Bi⎯Sn–Pb, and Bi–In–Pb in air is studied as a function of the alloy composition by hightemperature gravimetry. The compositions of the oxide layers that form on these alloys are determined. DOI: 10.1134/S003602951308003X

INTRODUCTION Although oxidizing refining is often used to pro duce various metals and alloys [1–4], many problems of the interaction of liquid metals with oxygen have not yet been resolved [5]. This is especially true of alloys, since some information for pure metals is avail able [5–8]. The oxidation of binary bismuthbased alloys was analyzed in [9]. Therefore, the purpose of this work is to study the air oxidation of ternary alloys Bi–Ag–Cu, Bi–Ag–Ge, Bi–Ag–Sn, Bi–Ag–Pb, Bi–Cu–Sn, Bi–Sn–Pb, and Bi–In–Pb as a function of the alloy composition.

is observed in a certain region of ternary alloy compo sitions in this system. This phenomenon was earlier detected during the oxidation of solid metals in the presence of V2O5, WO3, Bi2O3, and PbO [6, 15]. Dur ing this oxidation, a porous spongy film characterized by bad adhesion to a metallic alloy formed on its sur face. It was noted that the presence of at least a small amount of a liquid phase in the reaction products plays an important role in CO [6, 15, 17]. The authors of [15] explained CO by the appearance of cracks in a forming scale (e.g., due to the formation of a volatile oxide). According to [18], the sensitivity of alloys to CO manifests itself in the concentration range corre

Ag RESULTS AND DISCUSSION 100 0 The oxidation of bismuthbased liquid alloys was studied by hightemperature gravimetry, as in [10, 11]. The oxidation of the boundary binary alloys for the 20 80 ternary Bi–Ag–Cu system was investigated earlier: Bi–Cu in [12], Bi–Ag [13], and Ag–Cu [14]. It was 1 found that an increase in the silver content in the 40 60 binary alloys did not result in a monotonic decrease in 2 9 the melt oxidation rate. These results support the data 3 in [15], where the authors noted that the existing opin 40 60 ion that a metal should be alloyed with a precious 4 metal to increase its corrosion resistance against oxi 5 dation is not always true in practice. 6 2 80 20 It was found that almost all ternary Bi–Ag–Cu alloys oxidize according to a linear law. According to 7 8 5 [15, 16], this fact indicates that the oxidation rate is 100 0 controlled by a process or reaction on a surface or an 20 Cu 0 40 100 Bi 80 60 interface. Figure 1 shows oxidation isochrones for liquid Fig. 1. Oxidation isochrones for liquid Bi–Ag–Cu (at %) Bi⎯Ag–Cu alloys. The alloys with a low Ag content in alloys at 1123 K and υ (×104 kg/(m2 s)) = (1) 7, (2) 8, (3) 9, the range 55–70 at % Bi have the maximum oxidation (4) 10, (5) 11, (6) 12, (7) 12.5, and (8) 13. (9) is the cata rate. Moreover, socalled catastrophic oxidation (CO) strophic oxidation region. 600

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sponding to the formation of electronic compounds during solidification. The CO of metals can proceed according to both an electrochemical mechanism (ion diffusion along intergranular channels) and a fluxing mechanism (dis solution of a protective layer) [17]. The operation of these mechanisms depends on the ratio of the liquid phase mass to the metal mass and the Gibbs energies of a solid product and a liquid phase.

601

Ag 0 100

20

40

80

60

Bismuthbased compounds with selenite 40 60 (Bi12GeO20, Bi12SiO20, etc.) and eulytine (Bi4Ge3O12, Bi4Si3O12, etc.) structures are widely used in practice 1 3 [19, 20]. The problem of growing single crystals of 2 45 6 these compounds is caused by the fact that Bi2O3 80 20 based melts are very aggressive liquids, which cause 7 8 corrosion of platinum crucibles [21–23]. An alterna 10 9 100 tive method for the synthesis of such compounds is 0 likely to be the oxidation of liquid Bi–Ge alloys. The Bi 0 20 40 80 60 100 Sn experiments performed in [24] showed that the scale formed during the oxidation of Bi–Ge melts con Fig. 2. Oxidation isochrones for Bi–Ag–Sn (at %) melts at 1123 K and υ (×104 kg/(m2 s)) = (1) 10, (2) 9, (3) 8, (4) 7, tained bismuth only when an initial alloy contained (5) 6, (6) 5, (7) 4, (8) 3, (9) 2, and (10) 1. ≥80 at % Bi. This phenomenon was attributed to the reaction 3Ge + 2Bi2O3 = 3GeO2 + 4Bi. Allowing for the data that silver can substantially affect the oxida The introduction of silver leads to a decrease in the tion of liquid alloys, we [24] studied the effect of silver oxidation rate of Bi–Ge melts. An increase in the sec on the oxidation of liquid binary Bi–Ge alloys and on ondcomponent content to 30 at % in the Bi–Ag sys the composition of the formed scale. It was found that tem decreases the oxidation rate insignificantly, and the scale composition is almost the same during the the further increase in the Ag concentration deceler oxidation of Bi–Ge and (Bi–Ge) + 20 at % Ag melts ates the oxidation process [13, 28]. Irrespective of the (oxide layer contains Bi2GeO5 at Bi ≥ 80 at % and only silver content, an increase in the Ge concentration GeO2 in all other cases). During the oxidation of all decreases the oxidation rate of these alloys. This is an other alloys, the scale has no complex oxide com unexpected result, since germanium oxidizes at a high pounds (only GeO2). Moreover, the oxidation rates of rate [25]. Bi–Ge and (Bi–Ge) + Ag melts are rather close to each other at low values of τ, i.e., when the forming The oxidation of liquid Bi–Ag–Sn alloys was stud scale has a small thickness (initial stage of oxidation) ied in the content range 0–100 at % of each compo and insignificantly affects the oxidation kinetics of the nent at a step of 10 at % at temperatures of 1123 and melts. 1273 K (in the first case, the Ag concentration was changed from 0 to 80 at %). The oxidation of the According to [25], pure Bi and Ge oxidize accord boundary binary systems of this ternary system was ing to a linear law at a temperature of 1273 K, whereas investigated in the following works: Bi–Ag [13], Bi–Ge melts oxidize in most cases according to a lin Bi⎯Sn [29], and Ag–Sn [10, 18]. According to our ear law to τ = 1200 s and, then, according to a para data, CO in the Ag–Sn system at a temperature of bolic law. 1273 K occurs at a silver content of 60–75 at % and is The following two sequential linear oxidation laws are accompanied by the formation of a brittle mixture of operative during the oxidation of (Bi–Ge) + 20% Ag and highly dispersed crystals consisting of SnO2 and silver (Bi–Ge) + 40% Ag. As the bismuth content increases, microparticles, which were uniformly distributed over the time of the inflection point in the curve Δm/s = the surface of larger oxide crystals and were present as f(τ), where Δm/s is the sample mass change per area, isolated particles. increases [26]. This is related to a change in the scale Figure 2 shows the oxidation rates of Bi–Ag–Sn composition and porosity. melts at 1123 K that were obtained in our work [30]. It was found that silver is almost absent in the oxide υ is minimal for alloys with high Sn and Ag contents. layer that forms during the oxidation of Bi–Ag–Ge The established laws of oxidation of these molten melts. However, the Bi2O3–Ag phase diagram demon alloys were related to the properties of the formed strates that certain silver dissolution is possible at the scale. For example, porous agglomerates of metallic experiment temperature in air in the Bi2O3 region [27]. silver globules form in the continuous oxide layer of RUSSIAN METALLURGY (METALLY)

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12 2 10

3

8 6 4 2

0

10

20

30

50

40

60

70

80

90 100 Sn, at %

Fig. 3. Oxidation of Bi–Ag–Sn melts: (1) Bi–(Sn–Ag), (2) Bi–(Sn–3Ag), and (3) Bi–(3Sn–Ag).

SnO2 and Bi2O3 that forms on the alloys containing 30–60–10, 20–70–10, and 10–80–10 at % Bi, Ag, and Sn, respectively. Such behavior was also detected for solid alloys based on precious metals that were oxi dized under the conditions where the formation of their oxides is impossible according to thermody namic reasons. It is interesting that silver globules do not form on other Bi–Ag–Sn alloys. The scale formed on ternary alloys containing 5–70 at % Sn consists of several layers having different colors. The lower layer is enriched in tin and has an insignificant silver content, and the second layer has a higher silver content and a lower tin content. According to Xray diffraction analy sis, the composition of the scale on ternary Bi–Ag–Sn alloys includes Ag, SnO2, and Bi2Sn2O7. The compo nent content in the scale depends on the initial melt composition. The Bi content in the scale increases as the bismuth concentration in the initial melt increases at a constant silver content. At a constant Bi content in Properties of the scales forming on Bi–Ag–Sn melts Initial composition, at % (Bi, Ag, Sn) Bi

Scale αBi2O3

60–30–10

γBi2O3, Bi2Sn2O7

40–30–30

Bi2Sn2O7, Ag2O, SnO2

10–30–60

Bi2Sn2O7, SnO2, Ag

Sn

SnO2

an initial alloy, the Ag concentration in the scale increases as the silver content in the alloy increases. When studying the oxidation of Bi–Ag–Sn melts at 1273 K, the authors of [31] found that different oxida tion laws take place as a scale layer grows in most cases (except for the Bi–Ag system). Therefore we analyzed the effect of the compositions of Bi–Ag–Sn melts using ray sections at τ = 900 s. For the ray sections Sn–(Ag : Bi = 1 : 1, 1 : 3, 3 : 1), the oxidation rate decreases with increasing Sn con tent and passes through a maximum at CSn ≈ 15 at %. For the ray sections Ag–(Sn : Bi = 1 : 1, 3 : 1), the υ = f(CAg) curves are similar: the oxidation rate increases with the silver content in the alloys. For the Ag–(Sn : Bi = 1 : 3) section, the oxidation rate behaves in a complex manner depending on the alloy compo sition: it first increases as the Ag concentration increases to 40 at % and then decreases with increasing silver content. Except for a few cases, similar dependences are observed for the oxidation rate of Bi–(Sn : Ag = 1 : 1, 3 : 1) melts as a function of the bismuth content (Fig. 3). It should be noted that the oxidation rate has a complex dependence on the alloy composition for these ray sections and for the Ag–(Sn : Bi = 1 : 3) section. These laws of oxidation of liquid Bi–Ag–Sn alloys are related to the scale composition. As an example, we present some data on the scale composition in the table. Figure 4 shows the isochrones of oxidation of Bi– Ag–Sn alloys at 1273 K. These data were obtained for τ = 900 s, since the scale layer thickness increases with time and, hence, the oxidation conditions change.

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Sn 1 2 20

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10

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80

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4 65 8 7

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9 87 6 5 43 21

40

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Bi

Fig. 4. Oxidation isochrones for Bi–Ag–Sn (at %) melts at 1273 K and υ (×103 kg/(m2 s)) = (1) 1, (2) 2, (3) 3, (4) 4, (5) 5 (6) 6, (7) 7, (8) 8, (9) 9, (10) 10, (11) 11, (12) 12, (13) 13, (14) 14, and (15) 15.

It follows from a comparison of the data on the oxi dation kinetics of Bi–Ag–Sn melts at 1123 (Fig. 2) and 1273 K (Fig. 4) that a change in the temperature causes significant changes in υ and the law of oxida tion. The following is of particular interest. The boundary binary Ag–Sn system is characterized by CO, whereas any ternary Bi–Ag–Sn alloy does not undergo CO. Our experiments show that CO takes place in the case where the thirdcomponent concen tration is less than 1%. The study of the oxidation kinetics of ternary Bi⎯Ag–Pb alloys at 1123 K demonstrates that most melts are characterized by a parabolic oxidation law. In this case, the oxidation rate is determined by the diffusion rate in the forming scale. As follows from Fig. 5, υ is maximal in bismuth rich alloys. The conditions of oxide formation are determined by the composition of a metallic alloy and the partial oxygen pressure in an oxidizing atmosphere, which is higher than the dissociation pressure of each oxide [16]. As a result, several types of cations, the behavior of which with respect to oxygen ions determines the subsequent development and morphology of a film, form in the immediate vicinity of the metal–oxide interface. Therefore, one has to know the composition RUSSIAN METALLURGY (METALLY)

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of the scale forming on a certain alloy to analyze data on the oxidation kinetics of liquid Bi–Ag–Pb alloys. Xray diffraction analysis of the scale formed on alloys with a high lead and bismuth content showed the presence of the Pb2Bi6O11 and PbBi12O19 com pounds, which were detected earlier in the scale formed on a Bi–Pb melt [32]. An analysis of the element contents in the scale that forms during the oxidation of ternary Bi–Ag–Pb alloys demonstrates that the silver and bismuth con tents increase and the lead content decreases in the scale as the Ag concentration in an initial alloy increases at CBi = const. For CAg = const, the bismuth content in the scale increases and the silver and lead concentrations decrease as the bismuth content in an initial alloy increases. When studying the oxidation of ternary Bi–Cu–Sn alloys at 1273 K, the authors of [33] found that differ ent oxide layer growth laws are operative depending on the composition of a liquid alloy. A linear–parabolic law was most often observed. In this case, the oxida tion rate is described by the complete parabolic equa tion [16]

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80 1

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Fig. 5. Oxidation isochrones for Bi–Ag–Pb (at %) melts at 1123 K and υ (×104 kg/(m2 s)) = (1) 0.5, (2) 1, (3) 3, (4) 3, (5) 4, (6) 5, (7) 6, (8) 7, (9) 8, (10) 9, and (11) 10.

Sn 100

0

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Fig. 6. Oxidation isochrones for Bi–Cu–Sn (at %) melts at 1273 K and υ (×103 kg/(m2 s)) = (1) 0.3, (2) 0.5, (3) 0.7, (4) 0.9, (5) 1.1, and (6) 1.2.

where a, b, and c are constants; δ is the oxide layer thickness; and τ is the time. Figure 6 shows oxidation isochrones for ternary Bi–Cu–Sn alloys. Note that υ increases in the ray sec tion Sn : Bi = 1 : 1 when the copper concentration increases at low copper concentrations. In contrast, the oxidation rate of ternary liquid Bi–Cu–Sn alloys

decreases as the copper concentration increases at high copper concentrations. Similar behavior is observed for the Bi : Cu = 1 : 1 and Sn : Cu = 1 : 1 ray sections: the addition of Sn and Bi first increases the oxidation rate and then decreases it. The established laws of oxidation of Bi–Cu–Sn melts are assumed to be caused by the presence of

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compounds (such as the compounds CuO, Cu2O, Bi2CuO4, Bi2Sn2O7, Bi2O3 formed on the correspond ing binary alloys) in an oxide layer and by the disorder ing reactions [34] ••

''' + 3V O , 0 ↔ 2V Bi

(2)

•• 2CuO ↔ 2Cu 'Bi + V O + 2O 0 ,

(3)

•• 3 Bi 2 O 3 ↔ 2Bi 'Sn + V O +  O 2 , 2

(4)

•

3SnO 2 ↔ 3Sn Bi + V ''' Bi + 4O 0 + O 2 .

(5)

It follows from Eqs. (4) and (5) that oxygen vacancy •• concentration V O increases in the first case and cation vacancy concentration V ''' Bi increases in the second case, which naturally affects the disordering of the corre sponding oxide and, hence, its transport properties. When studying the behavior of Bi–Sn–Pb melts in air at 973 K, the authors of [35] found that alloys with a high tin content have the minimum oxidation rate. This finding was related to the formation of the chem ical compounds PbBi12O19, Pb2Bi6O11, Bi2Sn2O7, and Pb3Sn2O7 in a scale. Note that the diffusion coefficient of oxygen in liquid lead is higher than in liquid bis muth [36]. A linear oxidation law is characteristic of all ternary Bi–In–Pb alloys at the initial stage (up to τ = 600 s) [37]. Then, as a scale layer grows, these alloys oxidize according to a parabolic law. It was found that, at a temperature of 1123 K, alloys with a high indium con tent have the lowest oxidation rate and alloys with a high Bi content have the highest oxidation rate. CONCLUSIONS The oxidation of ternary bismuthbased melts in air was studied. The composition and morphology of the forming scale layer were found to play a key role in the oxidation of these melts. REFERENCES 1. M. P. Smirnov, Refining of Lead and Processing of Semi products (Metallurgiya, Moscow, 1977). 2. V. M. Malyshev and D. V. Rumyantsev, Silver (Metal lurgiya, Moscow, 1976). 3. A. I. Okunev and M. D. Galimov, Oxidation of Iron and Sulfur in Oxide–Sulfide Systems (Nauka, Moscow, 1983). 4. S. S. Korovin, V. I. Bukin, P. I. Fedorov, et al., Rare and Scattered Elements. Chemistry and Technology (MISiS, Moscow, 2003), Vol. 3. 5. N. V. Belousova, V. M. Denisov, S. A. Istomin, et al., Interaction of Liquid Metals and Alloys with Oxygen (UrO RAN, Yekaterinburg, 2004). 6. P. Kofstad, HighTemperature Oxidation of Metals (Mir, Moscow, 1969). RUSSIAN METALLURGY (METALLY)

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Translated by K. Shakhlevich

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