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Review Article
DOI: 10.1016/j.jmrt.2019.07.042
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Available online 11 September 2019
Structural analysis of Al–Ce compound phase in AZ-Ce cast magnesium alloy
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Su Juan, Guo Feng
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, Cai Huisheng, Liu Liang
School of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010051, Inner Mongolia, China
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Received 23 April 2019. Accepted 19 July 2019
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Table 1. The equilibrium electrode potentials of samples under given conditions of this test.
Table 2. Test bar number and main element content and diameter of the test bar.
Table 3. Gibbs free energy calculation results of Al–Ce compound formation reaction (J/mol).
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Abstract

The AlvCe intermetallic compound is an important component of the as-cast AZ-Ce magnesium alloy. Accurately determining the type of the Al–Ce compound is a necessary prerequisite for analyzing the alloying mechanism of Ce in the AZ magnesium alloy. In this study, the compound in the as-cast AZ-Ce magnesium alloy was extracted and enriched by electrochemical phase separation. The Al–Ce intermetallic compound was calibrated by X-ray diffraction and transmission electron diffraction. The thermodynamic parameters of the formation of Al4Ce and Al11Ce3 compounds were calculated. The results show that for die casting samples with Ce content of 0.3–1.2wt%, Al content of 3–9wt% and diameter of Φ6–Φ24mm, the Al–Ce compound in the as-cast microstructure is always Al4Ce, instead of other Al–Ce compound. The Gibbs free energy change of Al11Ce3 compound formation reaction in alloy melt is negative compared with Al4Ce, that is, Al11Ce3 compound has stronger forming ability than Al4Ce. The reason why Al4Ce is formed may be that the kinetic conditions are more likely to satisfy the nucleation and growth requirements of the Al4Ce compound for Ce, Al element concentration and atomic ratio.

Keywords:
AZ-Ce magnesium alloy
Al–Ce compound
Electrochemical phase separation
Phase analysis
Thermodynamic calculation
Full Text

AZ and AM alloys are magnesium alloys in which Al is the main alloying element. Ce is added to these magnesium alloys to form Al–Ce intermetallic compounds. These metal compounds can strengthen the alloy by pinning dislocations and strengthening grain boundaries [1–3]. At present, for the magnesium alloys such as AZ and AM containing Ce, the Al–Ce intermetallic compounds given in different references have different structures, including Al4Ce, Al11Ce3, and Al2Ce. Correspondingly, the researchers believe that the Al–Ce compounds of different structures have different roles in the alloy [4–8]. Xiong et al. [9–11] analyzed the lattice matching relationship between the Al–Ce intermetallic compound and the α-Mg matrix, and found that the Al4Ce compound has a small mismatched corresponding crystal face with the α-Mg phase. But there is no corresponding crystal face with small mismatch between A111Ce3 and α-Mg phase, so it is considered that Al4Ce can be used as a good heterogeneous crystal nucleus in the α-Mg phase, while A111Ce3 cannot. Wang et al. [2,12–15] study on the high temperature properties of Ce-containing magnesium alloys shows that the high melting point Al4Ce or Al11Ce3 dispersed in the grain boundaries and in the crystal can effectively hinder the movement of grain boundaries and dislocations at high temperatures. So Al–Ce intermetallic compound can improve the high temperature creep properties of the alloy, but the Al11Ce3 intermetallic compound can only stabilize below 200°C. Above this temperature, the strength of the alloy is lowered due to the conversion of the compound. The above results indicate that Ce is an important additive element in magnesium alloys such as AZ and AM, and some of its action behavior in the alloy depends on the structure of the formed Al–Ce intermetallic compound. That is to say, understanding the structure of the Al–Ce intermetallic compound is a necessary prerequisite for analyzing the mechanism of action of Ce in the alloy. Therefore, for certain Ce-containing magnesium alloys, it is extremely necessary to accurately determine the structure of the Al–Ce intermetallic compound in the alloy system.

X-ray diffraction analysis is one of the most direct and reliable methods for phase identification. However, for alloys such as AZ and AM with lower Ce content, the number of characteristic peaks of Al–Ce phase is small and insignificant due to the small amount of Al–Ce compounds in the structure, so it is difficult to accurately calibrate the phase by X-ray diffraction analysis. In addition, some diffraction peaks of Al4Ce and Al11Ce3, Al11Ce3 and Mg17Al12 have similar positions, which hinders the accurate determination of the phase. Therefore, if the Al–Ce phase is accurately identified by X-ray diffraction analysis, it should be separated from the alloy to be enriched. Electrochemical phase separation is an effective method for phase separation of metallic materials. It has been applied to steel, nickel, aluminum and zirconium alloys [16–19]. However, the potential of the magnesium alloy is relatively negative, and the magnesium alloy is highly susceptible to corrosion in the electrolyte. At the same time, the solid solution in the alloy is similar to the electrochemical behavior of some compound phases, so electrochemical phase separation is less used in magnesium alloys. After repeated exploration, in this work, a method of low-temperature and constant-potential phase separation in organic solvent electrolyte was established, which achieved effective separation of the compound phase and solid solution phase and enrichment of Al–Ce phase in AZ-Ce magnesium alloy. On this basis, the structure of the separated Al–Ce phase was analyzed by X-ray diffraction and electron diffraction. Furthermore, by adjusting the Ce and Al contents of the alloy and the cross-sectional dimensions of the sample, the effects of alloy composition and alloy solidification rate on the structure of the Al–Ce intermetallic compound were investigated.

1Experimental methods and materials

According to the references, the composition phase of the Ce-containing AZ alloy mainly includes α-Mg solid solution, β-Mg17Al12 eutectic compound, and Al–Ce intermetallic compound Al4Ce or Al11Ce3. Mg17Al12, Al4Ce, Al11Ce3 and α-Mg solid solution sample with Al content of 1% are smelted separately according to the atomic ratio using a non-consumption arc furnace. In an electrolyte containing acetic acid, abietic acid, ammonium benzoate, and ethanol, the equilibrium electrode potential of each sample was determined by Zahner three-electrode electrochemical system (platinum as auxiliary electrode and saturated calomel electrode as reference electrode). Fig. 1 shows the X-ray diffraction spectrum and the standard spectrum of each sample. However, the atomic ratio of Al to Ce is 4:1 or 11:3, and the phases synthesized by smelting are all Al11Ce3. Table 1 shows the equilibrium electrode potentials of each sample and pure magnesium measured. It can be seen that the equilibrium electrode potential of pure magnesium and α-Mg solid solution with Al content of 1% is not much different, indicating that the amount of solid solution of Al has little effect on the equilibrium electrode potential of α-Mg. Therefore, −1140mV can be used as the equilibrium electrode potential of α-Mg solid solution with different Al content. The equilibrium electrode potential difference between β-Mg17Al12 and α-Mg phase is about 390mV, which meets the requirement that the two-phase safety extraction potential difference should be greater than 100mV [20]. Therefore, this experiment selects −900mV as the electrolysis potential to decompose the α-Mg phase and retain the compound phase.

Fig. 1.

The measured XRD patterns of samples and standard patterns of relevant phases.

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Table 1.

The equilibrium electrode potentials of samples under given conditions of this test.

Sample  Pure magnesium  1% Al α-Mg  Mg17Al12  Al11Ce3 
Decomposition potential  −1148mV  −1140mV  −750mV  −132mV 

The AZ91, AZ61, AZ31 and Mg–30%Ce intermediate alloys were used as raw materials, and the experimental alloys with different Ce and Al contents were melted in an electric resistance furnace under the argon protection. The cylindrical test bars with diameters of Φ6, Φ12, Φ18 and Φ24 were die-cast with a cold chamber die casting machine, and the solidification cooling rate of the alloy was changed by the change of the diameter of the test bar. The actual composition of the alloy was determined using an OPTIMA 2X/5000 inductively coupled plasma optical emission spectrometer (ICP). The test bar number and measured Al and Ce content and diameter of the test bar are shown in Table 2.

Table 2.

Test bar number and main element content and diameter of the test bar.

Numbering  Al content (mass%)  Ce content (mass%)  Test rod diameter (mm) 
Mg–9Al–1.2Ce-Φ18  8.78  1.17  18 
Mg–9Al–0.6Ce-Φ18  8.76  0.63  18 
Mg–9Al–0.3Ce-Φ18  8.81  0.29  18 
Mg–6Al–0.6Ce-Φ18  6.07  0.59  18 
Mg–3Al–0.6Ce-Φ18  3.02  0.61  18 
Mg–9Al–0.6Ce-Φ24  8.76  0.63  24 
Mg–9Al–0.6Ce-Φ12  8.76  0.63  12 
Mg–9Al–0.6Ce-Φ6  8.76  0.63 

The metallographic sample was taken from the die-casting test bar, and the as-cast microstructure of the alloy was observed by scanning electron microscope. The die-casting test bar is processed into an electrolytic sample with a diameter of 100mm and a diameter of 5mm. A three-electrode electrolysis system is formed by using the MCP-1 constant potentiometer as an electrolytic power source. The electrolyzer is placed in a BLJI-07 cold trap that can accurately control the temperature, and the electrolyte temperature is kept at −15°C to −10°C for 12h. The electrolysis product attached to the surface of the sample is brushed into the electrolyte with a soft brush, and the electrolysis product is separated by filtration using a microporous membrane negative pressure filtration device. The powder on the filter membrane is washed with absolute ethanol and collected for X-ray diffraction analysis and scanning electron microscope and transmission electron microscope analysis. The X-ray diffractometer model is D/Max 2500/PC and the transmission electron microscope model is JEM-2100.

2Experimental results2.1Basic structure and phase composition of AZ-Ce as-cast alloy

Figs. 2 and 3 are scanning electron micrographs and corresponding X-ray diffraction spectra of typical samples of AZ-Ce magnesium alloys with different Ce content, different Al content and different solidification cooling rates, respectively. The results show that the above alloys are composed of α-Mg phase, network-like β-Mg17Al12 phase and acicular Al–Ce phase, among which α-Mg phase and β-Mg17Al12 phase has obvious X-ray diffraction peaks, while the Al–Ce phase has weaker diffraction peaks.

Fig. 2.

The variation of microstructures with different compositions and solidification rates.

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Fig. 3.

The XRD patterns of experimental alloys.

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Fig. 4 is a scanning electron micrograph of a compound electrolytically separated from an alloy. It can be seen from the morphology and gradation that there are mainly two kinds of compounds. According to the results of the energy spectrum analysis shown in Fig. 5 and the analysis of the basic structure shown in Figs. 2 and 3, it can be concluded that the gray block compound is β-Mg17Al12 phase, while the white and bright acicular compound should be Al–Ce phase.

Fig. 4.

The SEM morphology of compounds separated from alloys.

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Fig. 5.

The EDS analysis of metallic compounds.

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2.2Structure of Al–Ce compounds in AZ-Ce as-cast alloys

Fig. 6 shows the X-ray diffraction spectra of compounds isolated by electrolysis from the Mg–9Al–1.2Ce, Mg–9Al–0.6Ce and Mg–9Al–0.3Ce die-casting test rods with a diameter of Φ18. Because of the enrichment of the compound after electrolysis separation, the diffraction peak of α-Mg phase in the diffraction spectrum basically disappeared, while the diffraction peak of Mg17Al12 and Al–Ce phase was obvious. Comparing the standard diffraction spectra of Al4Ce (No: 03-065-2678) and Al11Ce3 (No: 00-019-0006), it is not difficult to see that the diffraction peaks corresponding to the 2θ angles of 22.08, 33.52 and 33.92 in the diffraction spectrum are completely corresponding to the peak position and peak intensity order of the Al4Ce standard diffraction spectrum. However, it does not correspond to the standard diffraction peaks of Al11Ce3. That is, in the range of Ce content of the experiment, the Al–Ce compound in the alloy should be Al4Ce, not Al11Ce3 or other compounds, and the structure does not change with the change of Ce content in the alloy. Fig. 7 is an electron diffraction pattern of the Al–Ce compound in the Mg–9Al–1.2Ce-Φ18 sample and its calibration result. The calculated interplanar spacing of the (110) crystal plane is 0.3093nm, the (004) crystal plane is 0.2533nm, and the (114) crystal plane is 0.1806nm, which is basically the same as that of Al4Ce (110) (004) (114) crystal plane ((110) 0.3087nm, (004) 0.2525nm, (114) 0.1954nm, respectively). This result further confirms that the Al–Ce phase in the alloy is indeed Al4Ce.

Fig. 6.

The XRD patterns of compounds separated from alloys with different Ce.

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Fig. 7.

The TEM morphology and electronic diffraction patterns of Al–Ce compound.

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Fig. 8 shows the X-ray diffraction spectra of compounds isolated by electrolysis from the Mg–9Al–0.6Ce, Mg–6Al–0.6Ce, and Mg–3Al–0.6Ce die-cast test bar having a diameter of the same as Φ18. From the results of phase calibration, it is found that for alloys with different Al content, the separated compounds are also Mg17Al12 and Al4Ce, that is, in the range of experimental Al content, the structure of Al–Ce compounds in the alloy does not change with the change of Al content.

Fig. 8.

The XRD patterns of compounds separated from alloys with different Al.

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Fig. 9 shows the X-ray diffraction spectrum of the compounds separated by electrolysis from die-casting samples of Mg–9Al–0.6Ce alloys with diameters 24mm, 18mm, 12mm and 6mm, respectively. The peak positions of diffraction peaks of each sample are the same. The results of phase calibration show that the Al–Ce compound in the separation is still Al4Ce for the alloy specimens with different solidification rates, and there is no Al11Ce3. That is to say, the change of solidification cooling rate (test rod diameter) does not change the structure type of Al–Ce compound in the alloy (Fig. 10).

Fig. 9.

The XRD patterns of compounds separated from samples of different diameters.

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Fig. 10.

The standard Gibbs free energy of Al–Ce formation reaction in Mg–Al–Ce ternary alloy melt.

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2.3Discussion of results

The experimental results show that for the AZ-Ce as-cast magnesium alloy, the Al–Ce intermetallic compound in the as-cast microstructure is Al4Ce phase in the range of Ce, Al content and solidification cooling rate in this experiment. There is no Al–Ce compound phase of Al11Ce3 or other structural types.

However, if the experimental AZ-Ce alloy is approximated as Mg–Al–Ce ternary alloy, the reaction equation is constructed with an equimolar amount of Ce. Then, according to the Van’t Hoff equation and the thermodynamic parameters of Al and Ce in the Al4Ce and Al11Ce3 compounds involved in the reaction, the Gibbs free energy change of the Al4Ce and Al11Ce3 compounds in the Mg–Al–Ce ternary alloy melt can be calculated. Table 3 lists the relationship between ΔG and temperature of the reaction of the two compounds in the experimental alloy and the ΔG value at the alloy melting temperature Ts (973K) and the solidification end temperature Te (743K). It can be seen that in the temperature range of alloy cooling and solidification, although the ΔG of the reaction of the two compounds is negative (the Mg–3Al–0.6Ce alloy is lower than 902K), the ΔG of the Al11Ce3 compound formation reaction is negative compared with Al4Ce, that is, from a thermodynamic point of view, Al11Ce3 is easier to form than Al4Ce in the alloy melt. In addition, according to the definition of Gibbs free energy G=HTS, the constant term and the temperature coefficient term in the ΔG expression are regarded as the reaction enthalpy change ΔH and the reaction entropy change ΔS, respectively, and ΔH and ΔS are both negative values, indicating that the formation of the compound is an exothermic process, at the same time, the reaction elements change from disordered to ordered. The numerical values of ΔH and ΔS for the formation of the two compounds mean that the thermal effect of the eqmolar Ce reaction to form the Al11Ce3 compound is greater than that of the Al4Ce. The order of the Al11Ce3 compound is also higher than that of Al4Ce. For the formation reaction of any compound, |ΔH| is greater than |TΔS| of a specific temperature range, indicating that the dominant factor affecting the formation ability of the two compounds is the enthalpy change ΔH. According to the above phase analysis and thermodynamic calculation results, whether Ce and Al elements in the melt actually form Al4Ce or Al11Ce3, obviously depends not only on the formation ability of the two compounds in equilibrium. According to the crystallization theory, the nucleation of the Al–Ce phase requires a certain degree of concentration fluctuation of Ce and Al elements, and the growth of the core of the Al–Ce phase also requires a certain flux diffusion of Ce and Al elements. The alloy is non-equilibrium solidified, and the Al–Ce phase is mainly formed before the α-Mg solid solution begins to crystallize, so the diffusion time of the Ce and Al elements is limited. Therefore, the local concentration fluctuation of Ce and Al elements and the diffusion migration rate are bound to become important dynamic factors that restrict the formation of compounds. For the two compounds, the molecular composition of Al11Ce3 and Al4Ce is different. Since the number of Ce and Al atoms of Al11Ce3 molecule is much larger than that of Al4Ce, the formation of Al11Ce3 requires higher Ce, Al element fluctuation and faster diffusion rate than formation of Al4Ce. Thermodynamic calculations also show that the order degree of Al11Ce3 compound is higher than that of Al4Ce, that is, the formation of Al11Ce3 compound needs to meet higher Ce and Al atomic ratio requirements. Therefore, the formation of Al11Ce3 is more dependent on the kinetic conditions than Al4Ce, which means the formation of Al11Ce3 is more difficult than Al4Ce in a specific alloy. From this, it can be explained that for the AZ-Ce magnesium alloy having a low Ce content and a high solidification cooling rate, an Al4Ce compound is preferentially formed in the structure.

Table 3.

Gibbs free energy calculation results of Al–Ce compound formation reaction (J/mol).

Alloy  11/3 [Al]+[Ce]=1/3Al11Ce34 [Al]+[Ce]=Al4Ce
  ΔGT  ΔG (Ts)  ΔG (Te)  ΔGT  ΔG (Ts)  ΔG (Te) 
Mg–9Al–1.2Ce  −156,229+117.11T  −42,281  −69,216  −122,507+93.03T  −31,989  −53,386 
Mg–9Al–0.6Ce  −156,229+123.07T  −36,482  −64,788  −122,507+99.00T  −26,180  −48,950 
Mg–9Al–0.3Ce  −156,229+128.93T  −30,780  −60,434  −122,507+104.86T  −20,478  −44,596 
Mg–6Al–0.6Ce  −156,229+135.55T  −24,339  −55,515  −122,507+112.61T  −12,937  −38,838 
Mg–3Al–0.6Ce  −156,229+156.79T  −3672  −39,734  −122,507+135.78T  9607  −21,622 

In this study, the Al–Ce binary alloy was melted in a non-self-consuming arc furnace according to the atomic ratio of the Al4Ce compound. The resulting compound was Al11Ce3 instead of Al4Ce. This should be the higher concentration of Ce and Al atoms, the formation of Al–Ce phases does not require the long-range diffusion of elements, and the atomic ratio is close to 11:3. That is to say, no matter which Al–Ce compound is formed at this time, the kinetic conditions will be satisfied, and the thermodynamic conditions become the main factor determining the structure of the Al–Ce compound, so that the Al11Ce3 compound is formed. This demonstrates the rationality of the preferential formation of Al4Ce compounds in the experimental alloys from another aspect.

3Conclusions

The solid solution and the compound can be separated from the AZ-Ce alloy in a low-temperature organic solvent electrolyte by a potentiostatic electrochemical phase separation method, and the compound phase can be extracted and enriched, thereby, the X-ray diffraction of the extracted phase can be accurately calibrated. For die casting samples with Ce content of 0.3–1.2wt%, Al content of 3 to 9wt% and diameter of Φ6–Φ24mm, the Al–Ce compounds in the microstructure are always Al4Ce, rather than other Al–Ce compounds. The reason why Al4Ce compound in AZ–Ce magnesium alloy is easier to form than that in Al11Ce3 compound is that the alloy composition and solidification cooling rate conditions are easier to meet the requirements of Al4Ce phase nucleation and growth on the concentration and atomic ratio of Ce and Al elements.

Conflicts of interest

The authors declare no conflicts of interest.

Acknowledgments

This work was financially supported by Natural Science Foundation of Inner Mongolia (2018MS05050) and National Natural Science Foundation of China (51661025).

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