多元共电沉积制备Mg-Li-X（X=Gd，Sb，Bi）合金及机理研究
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摘要
本文以等质量的LiCl–KCl为熔盐电解质，采用循环伏安法、方波伏安法、计时电流法、计时电位和开路计时电位法研究了Gd(III)、Sb(III)和Bi(III)离子的电化学行为，探讨了在含有上述离子的LiCl–KCl–MgCl_2熔盐中多元共电沉积制备Mg–Li–Gd(Sb, Bi)合金的机理。应用XRD、SEM、EDS、OM、ICP-AES等技术对所得样品的结构和组成进行了分析。
直接以Gd_2O_3为稀土Gd原料，在LiCl–KCl–MgCl_2–Gd_2O_3熔盐中共电沉积制备了Mg–Li–Gd合金。采用理论计算和实验相结合的方法证明了在LiCl–KCl熔盐中MgCl_2对Gd_2O_3有氯化作用，少量的Gd_2O_3与MgCl_2反应生成GdCl_3。循环伏安可知，Gd(III)离子在熔盐中的还原峰电位为-2.28V(vs Ag/AgCl)。在3.0wt%Gd_2O_3–2.0wt%MgCl_2–LiCl–KCl熔盐体系中考察了Gd(III)、Mg(II)和Li(I)离子的共电沉积机理。当阴极电流密度达到–0.776A/cm~2或阴极电位比–2.30V(vs Ag/AgCl)更负时，Gd(III)、Mg(II)和Li(I)离子共电沉积。研究了共电沉积条件对Mg–Li–Gd合金的影响。采用恒电流电解的方法共电沉积制备了Mg–Li–Gd合金，实验结果表明，在合金中存在Mg_3Gd和Mg2Gd相，分布在Mg–Li合金的晶界处。Mg–Li合金中添加金属Gd，细化了Mg–Li合金的晶粒，增强了合金的抗腐蚀性能。
在673K，Mo电极上，研究了Sb(III))和Bi(III)离子在LiCl-KCl熔盐中的电化学性质。结果表明，Sb(III)和Bi(III)离子在熔盐中还原峰电位分别是-1.67和-2.03V(vsAg/AgCl)，而且计算了Sb(III)和Bi(III)离子在熔盐中的扩散系数。循环伏安研究发现，金属Sb或Bi的沉积和氧化不是完全可逆的反应。计时电流法研究表明Sb(III)在Mo电极上被还原为金属Sb的成核过程是连续成核过程。
在LiCl–KCl–MgCl_2–SbCl_3(BiCl_3)熔盐中考察了Sb(III)或Bi(III)、Mg(II)和Li(I)离子的共电沉积机理。在LiCl–KCl–MgCl_2(3.29×10~(–4)mol cm~(–3))–SbCl_3(2.53×10~(–4)mol cm~(–3))熔盐中，当阴极电流密度达到–0.466A/cm~2或阴极电位比–2.35V(vsAg/AgCl)更负时，Sb(III)、Mg(II)和Li(I)离子共电沉积。采用恒电流或恒电压电解的方法制备了Mg–Li–Sb、Mg–Li–Bi合金。XRD分析表明，在Mg–Li–Sb合金中存在Mg_3Sb_2和Li_3Sb相。在Mg–Li–Bi合金中存在Mg_3Bi_2和Li_3Bi相，Sb、Bi元素的面扫描和EDS分析可知，上述金属间化合物分布在Mg–Li合金的晶界处。
在Al电极上研究了Sb(III)离子在LiCl–KCl熔盐中的电化学行为。与Mo电极相比，Sb(III)离子在Al电极上发生欠电位沉积的现象，这主要是由于Sb和Al能生成AlSb金属间化合物。应用开路计时电位方法，计算了生成AlSb合金化合物的热力学函数，并且电化学沉积制备了AlSb金属间化合物。
The electrochemical behaviour of Gd(III), Sb(III) and Bi(III) ions was investigated in theLiCl–KCl(50:50wt%) molten salt at673K. The reaction mechanism and transportparameters of electroactive species were determined by transient electrochemical techniques(such as cyclic voltammetry, square wave voltammetry, chronopotentiometry,chronoamperometry and open-circuit chronopotentiometry) at a molybdenum or analumimum electrodes, the mechanism of electrochamical co-deposition of ternaryMg–Li–X(X=Gd, SB, Bi) alloys were studied in LiCl–KCl–MgCl_2melts containing theGd(III), Sb(III) or Bi(III) ions. X–ray diffraction(XRD), scan electron micrograph (SEM),energy dispersive spectrometry (EDS), optical microscope(OM) and inductively coupledplasma atomic emission spectrometer(ICP-AES) were employed to characterize the alloys.
Mg–Li–Gd alloys were directly obtained by electrochemical codeposition method inLiCl–KCl–MgCl_2–Gd_2O_3molten salt on molybdenum electrode at1073K. The resultssuggested that a little of Gd_2O_3could dissolve in LiCl–KCl–MgCl_2molten salt while it couldnot in LiCl–KCl melt. The codeposition of Mg, Li and Gd occurred when applied potentialswere more negative than–2.30V (vs. Ag/AgCl) or current densities were higher than–0.776A/cm~2in3.0wt%Gd_2O_3–2.0wt%MgCl_2–LiCl–KCl melt. Electrolysis temperature exerted agreat influence on current efficiency,78.87%current efficiency was obtained whenelectrolysis temperature was873K. Li content in Mg–Li–Gd alloys increased with the highcurrent densities. XRD results showed that Mg_3Gd and Mg2Gd intermetallic compoundsformed in Mg–Li–Gd alloys. Grain size of Mg-Li alloy became smaller as the Gd metalcontent increased in the alloy. The analysis of SEM and EDS demonstrated that the Mg_3Gdand Mg2Gd intermetallic compounds were mainly distributed at grain boundaries. Thecorrosion resistance of Mg-Li alloys was enhanced with addition of Gd metal.
The electrochemical behavior of Sb(III) or Bi(III) ions was investigated inLiCl–KCl(50:50wt%) molten salt on molybdenum at673K. The results showed thatelectrochemical reduction of Sb(III) or Bi(III) ions in LiCl–KCl melts occurred at-1.67V and-2.03V vs. Ag/AgCl respectively. A voltammogram with a different scan rate in LiCl–KClcontaining SbCl_3(BiCl_3) showed that the deposition/dissolution reaction of Sb or Bi were notcompletely reversible. The diffusion coefficient of Sb(III) or Bi(III) ions in LiCl–KCl molten salt was calculated at673K. Chronoamperometric studies indicated progressive nucleation ofantimony whatever the applied overpotential.
Mg–Li–Sb(Bi) alloys were obtained by galvanostatic electrolysis or potentiostaticelectrolysis at673K. The electrochemical codeposition of Mg, Li and Sb was investigated ona molybdenum electrode in LiCl–KCl–MgCl_2(3.29×10~(–4)mol cm~(–3))–SbCl_3(2.53×10~(–4)molcm–3) melts at673K by cyclic voltammetry, chronopotentiometry and chronoamperometry.Cyclic voltammograms, chronopotentiometry and chronoamperometry measurementsindicated that the electrochemical codeposition of Mg, Li and Sb metal occurred at currentdensities lower than–0.466A cm-2or at an applied potential more negative than–2.35V vs.Ag/AgCl. XRD results suggested that Mg_3Sb_2and Li3Sb were formed in Mg–Li–Sb alloys,Mg_3Bi_2and Li_3Bi were formed in Mg–Li–Bi alloys. The analysis of SEM and EDS indicatedthat the Sb(Bi) intermetallic compounds showed a distribution in grain boundaries of Mg-Lialloy.
The electroreduction of Sb(III) ions at an Al electrode was also studied by cyclicvoltammetry and open circuit chronopotentiometry in the temperature range of668–742K.The redox potential of Sb(III)/Sb at an Al electrode was observed at the more positivepotentials values than those at an inert electrode. This potential shift due to the formation ofAlSb intermetallic compound with Al electrode. AlSb intermetallic compound was preparedin LiCl–KCl–SbCl_3melts at742K by potentiostatic electrolysis at an Al electeode. Thethermodynamic properties of AlSb formation were also calculated by open-circuitchronopotentiometry method.
直接以Gd_2O_3为稀土Gd原料，在LiCl–KCl–MgCl_2–Gd_2O_3熔盐中共电沉积制备了Mg–Li–Gd合金。采用理论计算和实验相结合的方法证明了在LiCl–KCl熔盐中MgCl_2对Gd_2O_3有氯化作用，少量的Gd_2O_3与MgCl_2反应生成GdCl_3。循环伏安可知，Gd(III)离子在熔盐中的还原峰电位为-2.28V(vs Ag/AgCl)。在3.0wt%Gd_2O_3–2.0wt%MgCl_2–LiCl–KCl熔盐体系中考察了Gd(III)、Mg(II)和Li(I)离子的共电沉积机理。当阴极电流密度达到–0.776A/cm~2或阴极电位比–2.30V(vs Ag/AgCl)更负时，Gd(III)、Mg(II)和Li(I)离子共电沉积。研究了共电沉积条件对Mg–Li–Gd合金的影响。采用恒电流电解的方法共电沉积制备了Mg–Li–Gd合金，实验结果表明，在合金中存在Mg_3Gd和Mg2Gd相，分布在Mg–Li合金的晶界处。Mg–Li合金中添加金属Gd，细化了Mg–Li合金的晶粒，增强了合金的抗腐蚀性能。
在673K，Mo电极上，研究了Sb(III))和Bi(III)离子在LiCl-KCl熔盐中的电化学性质。结果表明，Sb(III)和Bi(III)离子在熔盐中还原峰电位分别是-1.67和-2.03V(vsAg/AgCl)，而且计算了Sb(III)和Bi(III)离子在熔盐中的扩散系数。循环伏安研究发现，金属Sb或Bi的沉积和氧化不是完全可逆的反应。计时电流法研究表明Sb(III)在Mo电极上被还原为金属Sb的成核过程是连续成核过程。
在LiCl–KCl–MgCl_2–SbCl_3(BiCl_3)熔盐中考察了Sb(III)或Bi(III)、Mg(II)和Li(I)离子的共电沉积机理。在LiCl–KCl–MgCl_2(3.29×10~(–4)mol cm~(–3))–SbCl_3(2.53×10~(–4)mol cm~(–3))熔盐中，当阴极电流密度达到–0.466A/cm~2或阴极电位比–2.35V(vsAg/AgCl)更负时，Sb(III)、Mg(II)和Li(I)离子共电沉积。采用恒电流或恒电压电解的方法制备了Mg–Li–Sb、Mg–Li–Bi合金。XRD分析表明，在Mg–Li–Sb合金中存在Mg_3Sb_2和Li_3Sb相。在Mg–Li–Bi合金中存在Mg_3Bi_2和Li_3Bi相，Sb、Bi元素的面扫描和EDS分析可知，上述金属间化合物分布在Mg–Li合金的晶界处。
在Al电极上研究了Sb(III)离子在LiCl–KCl熔盐中的电化学行为。与Mo电极相比，Sb(III)离子在Al电极上发生欠电位沉积的现象，这主要是由于Sb和Al能生成AlSb金属间化合物。应用开路计时电位方法，计算了生成AlSb合金化合物的热力学函数，并且电化学沉积制备了AlSb金属间化合物。
The electrochemical behaviour of Gd(III), Sb(III) and Bi(III) ions was investigated in theLiCl–KCl(50:50wt%) molten salt at673K. The reaction mechanism and transportparameters of electroactive species were determined by transient electrochemical techniques(such as cyclic voltammetry, square wave voltammetry, chronopotentiometry,chronoamperometry and open-circuit chronopotentiometry) at a molybdenum or analumimum electrodes, the mechanism of electrochamical co-deposition of ternaryMg–Li–X(X=Gd, SB, Bi) alloys were studied in LiCl–KCl–MgCl_2melts containing theGd(III), Sb(III) or Bi(III) ions. X–ray diffraction(XRD), scan electron micrograph (SEM),energy dispersive spectrometry (EDS), optical microscope(OM) and inductively coupledplasma atomic emission spectrometer(ICP-AES) were employed to characterize the alloys.
Mg–Li–Gd alloys were directly obtained by electrochemical codeposition method inLiCl–KCl–MgCl_2–Gd_2O_3molten salt on molybdenum electrode at1073K. The resultssuggested that a little of Gd_2O_3could dissolve in LiCl–KCl–MgCl_2molten salt while it couldnot in LiCl–KCl melt. The codeposition of Mg, Li and Gd occurred when applied potentialswere more negative than–2.30V (vs. Ag/AgCl) or current densities were higher than–0.776A/cm~2in3.0wt%Gd_2O_3–2.0wt%MgCl_2–LiCl–KCl melt. Electrolysis temperature exerted agreat influence on current efficiency,78.87%current efficiency was obtained whenelectrolysis temperature was873K. Li content in Mg–Li–Gd alloys increased with the highcurrent densities. XRD results showed that Mg_3Gd and Mg2Gd intermetallic compoundsformed in Mg–Li–Gd alloys. Grain size of Mg-Li alloy became smaller as the Gd metalcontent increased in the alloy. The analysis of SEM and EDS demonstrated that the Mg_3Gdand Mg2Gd intermetallic compounds were mainly distributed at grain boundaries. Thecorrosion resistance of Mg-Li alloys was enhanced with addition of Gd metal.
The electrochemical behavior of Sb(III) or Bi(III) ions was investigated inLiCl–KCl(50:50wt%) molten salt on molybdenum at673K. The results showed thatelectrochemical reduction of Sb(III) or Bi(III) ions in LiCl–KCl melts occurred at-1.67V and-2.03V vs. Ag/AgCl respectively. A voltammogram with a different scan rate in LiCl–KClcontaining SbCl_3(BiCl_3) showed that the deposition/dissolution reaction of Sb or Bi were notcompletely reversible. The diffusion coefficient of Sb(III) or Bi(III) ions in LiCl–KCl molten salt was calculated at673K. Chronoamperometric studies indicated progressive nucleation ofantimony whatever the applied overpotential.
Mg–Li–Sb(Bi) alloys were obtained by galvanostatic electrolysis or potentiostaticelectrolysis at673K. The electrochemical codeposition of Mg, Li and Sb was investigated ona molybdenum electrode in LiCl–KCl–MgCl_2(3.29×10~(–4)mol cm~(–3))–SbCl_3(2.53×10~(–4)molcm–3) melts at673K by cyclic voltammetry, chronopotentiometry and chronoamperometry.Cyclic voltammograms, chronopotentiometry and chronoamperometry measurementsindicated that the electrochemical codeposition of Mg, Li and Sb metal occurred at currentdensities lower than–0.466A cm-2or at an applied potential more negative than–2.35V vs.Ag/AgCl. XRD results suggested that Mg_3Sb_2and Li3Sb were formed in Mg–Li–Sb alloys,Mg_3Bi_2and Li_3Bi were formed in Mg–Li–Bi alloys. The analysis of SEM and EDS indicatedthat the Sb(Bi) intermetallic compounds showed a distribution in grain boundaries of Mg-Lialloy.
The electroreduction of Sb(III) ions at an Al electrode was also studied by cyclicvoltammetry and open circuit chronopotentiometry in the temperature range of668–742K.The redox potential of Sb(III)/Sb at an Al electrode was observed at the more positivepotentials values than those at an inert electrode. This potential shift due to the formation ofAlSb intermetallic compound with Al electrode. AlSb intermetallic compound was preparedin LiCl–KCl–SbCl_3melts at742K by potentiostatic electrolysis at an Al electeode. Thethermodynamic properties of AlSb formation were also calculated by open-circuitchronopotentiometry method.
引文
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