Effects of Calcium Addition on Properties of Mg Alloys: A Review

Effects of Calcium Addition on Properties of Mg Alloys: A Review

1. S.Gunabalan, 2. Dr. R. Elansezhian 1. Ph.D. (Research Scholar), 2. Associate Professor, Dept. of Mechanical Engineering, Pondicherry Engineering College, Puducherry.

Abstractthe Magnesium alloys attract the automobile, aerospace and electronic equipments manufacturing industries with its superior specific strength, processability and electromagnetic shielding. Aluminium alloys and polymer matrix composites are the strong contenders for magnesium alloys. Alloying is the way to improve the properties of the magnesium to defend its position as a structural material. Calcium one of the low cost alloying elements which improves the mechanical properties, provides thermal stability and enhances the formation of a thin and uniform oxide layer and thus improves the oxidation resistance and also increases the ignition temperature with a decrease in elongation and loss of fluidity. This article summarizes the effects of Calcium addition on the properties of magnesium alloys. Index TermsMg-Ca alloys, creep resistance, strengthening mechanism, corrosion.

I. INTRODUCTION A wide spectrum of materials is presently available for the innovative product designer. Although the versatility of the various engineering plastics especially fiber reinforced plastics has made a strong impact on material utilization, the metals have defended their strong position as materials for high performance, loaded structures [1]. Magnesium, a density of 2/3 that of aluminium, and little higher than fiber reinforced plastics, combined with excellent mechanical and physical properties as well as processability and recyclability, make magnesium alloys an obvious choice when designing for light weight. Magnesium and its alloys are becoming widely recognized in automotive, aircraft, and also in electronic consumer products with its good electromagnetic shielding characteristics [1],[2]. Commercial cast magnesium alloys for automotive applications are AZ and AM series alloys (AZ91D, AM50A, and AM60B). These alloys offer an excellent combination of

mechanical properties, corrosion resistance, machinability and die-castability. But, they have poor creep resistance above 125 , which makes them inadequate for major powertrain applications. A new improved high performance magnesium alloys, could well be used in the automatic transmission cases, which can operate up to 175 , engine blocks where up to 200 , and engine pistons where even higher than 300 . Creep resistance is a major requirement for use of magnesium in automotive powertrain components that are currently made up of aluminium or cast iron [2]. Present consumption of aluminium and magnesium in passenger cars is 120-140 kg and approximately 5 kg per vehicle respectively [3]. Magnesium in pure form is soft and can only be hardened by deformation. For structural applications a variety of magnesium alloys have been developed. The alloying elements are added both to secure adequate processability of the metal, and to obtain the performance required by the applications [1]. Magnesium is classified as an alkaline earth metal. It is found in Group three of the periodic table. It possesses a similar electronic structure to Beryllium (Be), Calcium (Ca), Strontium (Sr), Barium (Ba) and Radium (Ra) [4]. The alloy elements used for enhancing thermal stability of magnesium alloy mainly consists of rare-earth elements, the alkali soil elements (Ca, Sr, Ba) and the IV,V Race elements such as silicon (Si), tin (Sn), antimony (Sb), bismuth (Bi). These elements can form high melting point compounds with Mg, Al and other alloying element (for example, Zn, Mn, Zr) to realize good thermal stability by dispersion strengthening of alloys [5]. Alloying with Ca in the range from 0.01 to 3% is becoming more common in the development of cheap creep resistant magnesium alloys essentially to replace -Mg17Al12 phase in Mg-Al alloys [4]. Fig.1. shows the direction of new magnesium alloys development based on the required properties for different performance range. This grouping clearly shows that the Ca containing magnesium alloys 88

ISBN: 978-1-4673-4948-2 2013 IEEE

IEEE - International Conference on Research and Development Prospects on Engineering and Technology (ICRDPET 2013) March 29,30 - 2013 Vol.1

participate in many groups such as creep resistance, diecastability and wrought Magnesium alloys [6]. This is the indication of importance of calcium in development of new magnesium alloys.

The ultimate tensile strength and elongation of ZA104 + 0.3Ca alloy are superior to those of ZA104 + 0.6Ca alloy. Tensile properties of ZA104 + 0.3Ca die-casting alloy are comparable to those of AZ91D alloy. Ultimate tensile strength and fracture strain of the two ZA experimental alloys decrease while calcium content increases [8]. III. CREEP PROPERTIES The creep properties of magnesium alloys are mainly related to the structure stability at high temperatures. The creep properties of the Ca-containing Mg-5Zn-5Sn alloys are possibly related to the formation of eutectic and/or primary CaMgSn phase with high thermal stability. With the Ca amount increasing from 0.5% to 1.5%, the amount and size of the CaMgSn phase increase gradually. Ca addition to the Mg5Zn-5Sn alloy does not significantly change the fracture mode of the alloy. The tensile rupture of the experimental alloys occurs along inter-granular boundary, but the cracks seem to extend easily along the interfaces between the coarse primary CaMgSn particle and -Mg matrix which possibly results in the relatively poor mechanical properties of the Mg-5Zn-5Sn1.0Ca and Mg-5Zn-5Sn-1.5Ca alloys [7]. Mg-3Sn-2Ca alloy has more potential as elevated temperature magnesium alloy due to its higher creep properties as compared to Mg-3Sn-1Ca alloy [9]. The microstructure of the Mg-Ca alloys is characterized by the discontinuously distributed primary magnesium phase and Mg2Ca phases. Increase in calcium content decreases the volume fraction of the primary magnesium phase. Mg2Ca is the reason for the creep resistance [10]. In Mg-Al based alloys Mg17Al12 phase is the reason for the poor creep property. Ca suppresses Mg17Al12 phase in AC515 alloy due to the suppression of its generation caused by a strong combination with Ca and Al atoms [11]. The Ca added to AZ91D + 3% Ca alloys forms insoluble Al 2Ca which decreases the amount of Mg17Al12 phase in the matrix. In AZ91D + 5% Ca, Mg17Al12 is not detected, but Al2Ca detected. In AZ91D + 1% CaO alloy Mg17Al12 is detected as the minor phase. In the case of the AZ91D + 10% CaO alloy only -Mg and Al2Ca are detected as the matrix phases [12]. IV. STRENGTHENING MECHANISM Grain refinement is the most desirable strengthening mechanism. The strengthening mechanism of Ca-containing Mg-5Sn-5Zn alloy is mainly attributed to the microstructure refinement and/or the formation of the CaMgSn phase [7]. With the combined addition of 0.5% Ca and 1.0% Y to AZ91 alloy, the grain size in microstructure decreases. Further increasing Ca content can cause the change of microstructure 89

Fig.1. Direction of Mg alloy development to improve the performance [6]

II. MICRO STRUCTURE AND MECHANICAL PROPERTIES The mechanical properties of the pure magnesium can be improved by the addition of alloying elements. Ca addition from 0.5% to 1.5% (mass fraction) in Mg-5Zn-5Sn system increases the yield strength and creep properties of the Cacontaining Mg-5Zn-5Sn alloys. As-cast Mg-5Zn-5Sn alloys are mainly composed of -Mg, CaMgSn, MgZn and Mg2Sn phases. The CaMgSn intermetallics is more easily formed due to the higher electronegative difference value between Ca and Sn elements, while the Mg2Ca intermetallics is less easily formed due to the lower electronegative difference value between Mg and Ca elements. The CaMgSn compound which has a high thermal stability can possibly restrict the growth of -Mg primary phase and secondary solidification phases during solidification. Consequently, the Ca-containing Mg5Zn-5Sn alloys obtain finer microstructures than the Mg-5Zn5Sn alloy. This improves the tensile properties both at room temperature and at 150 , which is beneficial to the creep properties. Among the Ca-containing Mg-5Zn-5Sn alloys, the alloy added 1.5% Ca exhibits the optimum yield strength and creep properties, however, the maximum ultimate tensile strength of 174.7MPa and elongation of 4.79% at room temperature and ultimate tensile strength of 147.9MPa and elongation of 14.21 % at 150 are achieved in the alloy added with 0.5% Ca [7]. Mg-3Sn-1Ca alloy shows higher ultimate tensile strength and elongation at room temperature (138MPa) and at 150 (120MPa) than Mg-3Sn-2Ca alloy with 127MPa at room temperature and 116MPa at 150 . However, the yield strength of the Mg-3Sn-1Ca alloy is 101MPa at room temperature and 82MPa at 150 , which is lower than that of Mg-3Sn-2Ca alloy having yield strength of 112MPa and 104MPa respectively [9].

ISBN: 978-1-4673-4948-2 2013 IEEE

Effects of Calcium Addition on Properties of Mg Alloys: A Review

from dentritic to equiaxed. When 1.5% Ca and 1.0% Y are added to AZ91 alloy, the grains are remarkably refined, and the average grain size is 2030 m. the grain refinement may be the result of the formation of new particles that can act as potent nucleation sites for magnesium [13]. Micro-hardness of Mg-Zn-Ca system increases with the increase in Ca content and age hardening occurs after aging at 200 in the flakes probably due to the precipitation strengthening of the fine precipitates Mg2Ca and Ca2Mg6Zn3[14]. The combined addition of Y and Ca can refine the as-diecast microstructure, result in the formation of Al2Ca phase and Al2Y phase, and inhibit the precipitation of Mg17Al12 phase. The combined addition of Y and small amount of Ca has little influence on the ambient temperature tensile properties, but increasing the content of Ca can improve significantly the tensile strength at both ambient and elevated temperatures. In AZ91-1Y alloy, formation of coarse block and rod-like Al2Y phase are seen. The increase of ambient ultimate tensile strength of AZ91-1Y-1.5Ca alloy is due to microstructure improvement, refinement of Al2Y phases and dispersion strengthening with Al2Ca phases and Al2Y phases. Unfortunately, the combined addition of Y and Ca can decrease the elongation at 150 [13]. V. CORROSION In spite of the great advantages of magnesium alloys, their application as engineering material is still restricted by their high susceptibility to corrosion [15]. Magnesium is highly resistant to alkalies, chromic and hydrofluoric acids. But it is less resistant to other acidic or salt-laden environments. Magnesium is anodic to any other structural metal and will be preferentially attacked in the presence of an electrolyte [16]. Adding Ca to AZ91 magnesium can refine the microstructure, improve the elevated temperature properties and the corrosion resistance of magnesium alloys [17]. AsCast AZ91 magnesium alloy containing 0.14 wt.% Ca consists of -Mg17Al12, Mg17Al8Ca0.5 and Mg2Ca. When the alloys are exposed to 3.5% NaCl solution no corrosion attack is observed in Mg17Al8Ca0.5 and Mg2Ca phases [18]. On other hand addition of calcium to the Mg6% Zn1% Mn5% Si alloy decreases the corrosion resistance [19]. VI. DAMPING PROPERTIES The structural materials required to withstand the intended load and also required to absorb shock load occasionally. Pure magnesium has the better damping properties among various metallic materials. As-cast Mg1 wt%Ca binary alloy exhibits good damping capacities. The damping curve of Mg1 wt%Ca

alloy is close to high damping pure magnesium, while it is much higher than AZ91D alloy, which indicates that Mg1 wt%Ca alloy exhibits good damping capacity. Mg1 wt%Ca alloy could be considered as a potential candidate for high damping magnesium alloy. But further increase in Ca content in MgCa binary alloy exhibits the lower damping capacities [20]. VII. CAST ABILITY

Magnesium alloys, especially those with aluminium as a major alloying element show a very good castability [6]. In magnesium alloy casting, the viscosity of the molten metal is increases clearly with increasing the amount of Ca addition and firmer surface oxide film is formed by Ca addition. The flow length is shortened by Ca addition on the effect of the above factors [11]. Ca can be introduced in magnesium alloy casting as Mg-Ca master alloy. Mg-Ca master alloys are commercially available in 15, 20 and 30% Ca. Recommended addition temperatures for these master alloys depend on the Ca content and range from 680 720C. Dissolution or mixing time of 1530 minutes after the addition is recommended. Recoveries are quite high around 8090% under fluxless alloying conditions. As mentioned above, standard magnesium fluxes react with calcium so flux free melt protection is the preferred method for Ca addition [4]. Ca addition to the Mg-5Zn-5Sn alloy can result in the micro structural refinement of the alloy. It is well known that the Ca atom has a larger atomic radius than the Zn and Sn atoms (Ca: 0.197 nm; Zn: 0.131 nm; Sn: 0.141 nm), with the Ca addition to the Mg-5Zn-5Sn alloy, the Ca element is mainly rich in the solid-liquid interface during solidification [7]. More than about 1% Ca addition to AM50 alloy significantly improves creep resistance. It is accompanied by a tendency to hot cracking. By the addition of approximately 0.2%Sr, such casting cracks are significantly suppressed, and besides the enhancement in creep resistance and mechanical properties. The improvement of creep resistance by Sr addition seems to be attributed to the suppression of grain boundary sliding due to the creation of thermally stable Al-Sr compound along the grain boundary and the suppression of discontinuous precipitation of Mg17Al12 phase [4],[11].
VIII. OXIDATION AND IGNITION RESISTANCE A. Oxidation The interaction of oxygen with base metal forms the oxide layer. PillingBedworth principle of oxidation is the condition of oxidation film on the surface of the oxidizing metal. The PillingBedworth ratio () is the ratio of the oxide volume to 90

ISBN: 978-1-4673-4948-2 2013 IEEE

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the volume of the original metal which is consumed to form the oxide. When > 1, oxide can expand to bring compressive stress, under the action of which the oxidation film becomes tightly coherent. The value of magnesium is 0.81, so the MgO film is loose and there are a lot of small holes on oxidation film which allows oxygen infiltrating into the molten alloy [21],[22],[23]. The surface changes, of pure magnesium during casting and solidification under ambient atmosphere without any protective gas, are seen such as severe oxidation begins and tarnished surface appears in 10 seconds just after being poured. Severe burning starts in 10 seconds and continues even with white flame to the point when all melts [5]. Ca strongly improves oxidation performance. As little as 1% of Ca is enough to reduce the oxidation rate to extremely low values, even for longer oxidation times. Rare earths (added in the form of mischmetal) are not as effective as Ca, and slightly higher contents are necessary to achieve similar performance [15]. Elements with high affinity to oxygen such as Ca, Sr or Zr enhance the formation of a thin and uniform oxide layer and prevent growth of thick nodular oxide features [24]. B. Ignition The lowest temperature associated with the observation of a flame is called Ignition temperature. Ignition also defined as the temperature at which an exothermic oxidation reaction becomes self-sustaining at a rate which causes a significant temperature increase. The ignition temperature measurement is critical when the heat accumulates in the specimen [25], [26]. In the case of magnesium machining, most of the energy put into cutting processes is converted into heat, this leads to a risk of fire due to chip ignition [4]. Surface changes, of Mg alloy with 0.3wt% CaO during casting and solidification under ambient atmosphere without any protective gas, see no burning appears and shiny surfaces are maintained even after the solidification is completely stopped. The similar phenomena occurs in AZ310.27wt%CaO, AM50-0.27wt%CaO, AM60-0.3wt%CaO, and AZ91-0.27wt%CaO magnesium alloys [5]. The ignition point of AZ91 alloy increases linearly with the increase of Ca content. The data of ignition points of Cabearing AZ91 alloys can be fit as a linear equation: (1) Where is the ignition point in and x is the analyzed content of Ca (mass fraction, %) in AZ91 alloy. Ca-bearing AZ91 alloys are in agreement with linear equation when the

content of Ca is lower than 1.3% (analyzed content). When the content is higher than 1.3%, the ignition temperature is unstable. The minimum ignition temperature is higher than 770 and some of the alloys do not burn up to 900 . The testing results of ignition points of Ca-bearing AZ91 alloys imply that the proper addition of Ca is effective to improve the ignition point of AZ91 alloy up to 770 , but at a higher temperature the ignition of AZ91 cannot entirely be inhibited by addition of Ca [27]. The ignition point of Mg-5Ca alloy is about 1,030 .The average ignition point of Mg-5Ca powder in the size range of 150-250 m, is 685 , this average ignition temperature increases with the increasing particle size [11]. IX. DEVELOPMENT OF ECO MAGNESIUM ALLOY As environmental benefits provided by lightweight, being unlimited, and recyclable, magnesium alloys have the potential to grow significantly in the future by Eco-Mg (Environment Conscious Magnesium) approach. The simple and plain approach of Eco-Mg alloy is to introduce CaO particles in the range of 0.3wt% to 0.7wt% as an ingredient into conventional cast and wrought magnesium alloys for (1) nonSF6 process, (2) Be elimination, (3) improved melt cleanliness, (4) ensured original process adjustability for casting, forming, joining as well as surface treatment, (5) improved mechanical property by grain refinement and internal soundness, (6) ensured safety during manufacturing and application by raising oxidation and ignition resistances of machined chips and products, and (7) improved recyclability. CaO of over 0.5~0.7wt% can be introduced for special purposes to develop creep-resistant, fire-retardant or fire-proof magnesium alloys [5]. It is confirmed that CaO is reduced to Ca through phase analysis. Mg2Ca phase is formed even in 0.07% CaO added pure magnesium by reduction, while Mg2Ca phase is formed over 1.35% in Ca added magnesium. With respect to CaO content, the hardness of CaO added pure magnesium increased by grain refinement [28]. X. RECYCLABILITY Ca content in magnesium alloys disappears during recycling due to the reaction of Ca with the fluxes so flex free melt protection is recommended for Ca addition[4]. In a fluxed magnesium melting process, a suitable flux also can minimize the reduction of Ca content during recycling for Ca added magnesium alloys. KCl and NaCl are the suitable fluxes for magnesium alloys with Mg2Ca or Al2Ca phases without Ca content loss [5]. XI. SUMMARY AND CONCLUSIONS The research in the area of Ca addition on Properties of 91

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Effects of Calcium Addition on Properties of Mg Alloys: A Review

magnesium alloy is summarized as follows: 1) In Mg-Al based alloys Mg17Al12 phase is the reason for the poor creep property. Ca suppresses Mg17Al12 phase in AC515 and AZ91D + 3% Ca alloys forms insoluble Al2Ca which decreases the amount of Al12Mg17 phase in the matrix. 2) Ca addition from 0.5% to 1.5% (mass fraction) increases the yield strength and creep properties of the Cacontaining Mg-5Zn-5Sn alloys. The maximum ultimate tensile strength of 174.7MPa and elongation of 4.79% at room temperature and ultimate tensile strength of 147.9MPa and elongation of 14.21% at 150 are achieved in the alloy added with 0.5% Ca. 3) Increasing Ca content in magnesium alloys enhances the grain refinement and also change of microstructure from dentritic to equiaxed. When 1.5% Ca and 1.0% Y are added to AZ91 alloy, the grains are remarkably refined, and the average grain size is 2030 m. 4) Ca addition of more than about 1% to AM50 alloy significantly improves creep resistance but increases the cast cracking tendency. By the addition of approximately 0.2%Sr, casting cracks are significantly suppressed, and besides increasing the creep resistance and mechanical properties. 5) The fluidity of the molten metal decreases with increasing the amount of Ca addition. 0.07% CaO added pure magnesium is reduced to Ca forming Mg2Ca phase, while Mg2Ca phase is formed over 1.35% in Ca added magnesium. So Ca can be effectively added to magnesium alloys in the form of CaO. REFERENCES
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