Effect of heat treatment duration on microstructure evolution and electrochemical degradation behavior of electrodeposited Fe-4.8Zn alloy
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摘要: 以脉冲电沉积制备的 Fe-4.8Zn 合金为研究对象,在 450 ℃下进行不同保温时间热处理,系统研究了热处理时间对其显微组织、物相组成、元素分布、显微硬度及电化学降解行为的影响。结果表明,热处理促进了合金表面及截面组织的回复、重排与均匀化;XRD 结果显示,各样品均以 α-Fe 固溶体为主,热处理后衍射峰向高角度方向轻微偏移。合金中Fe与Zn分布均匀,未发生明显的元素再分布。随着保温时间延长,合金显微硬度逐渐升高,腐蚀电位逐步正移,腐蚀电流密度和腐蚀速率持续降低,电荷转移电阻逐渐增大。表明热处理时间对 Fe-4.8Zn 合金的组织结构、力学性能及电化学降解行为具有显著影响,可为 Fe-Zn 可降解血管支架材料的热处理调控提供试验依据。Abstract: Fe-4.8Zn alloy prepared by pulse electrodeposition was heat-treated at 450 ℃ for different holding times. The effects of heat treatment duration on the microstructure, phase composition, elemental distribution, microhardness, and electrochemical degradation behavior of the alloy were systematically studied. The results showed that heat treatment improved the recovery, rearrangement and homogenization of the microstructure on the surface and cross-section of the alloy. XRD analysis indicated that all samples were mainly composed of the α-Fe solid solution, and the diffraction peaks shifted slightly toward higher angles after heat treatment. The distributions of Fe and Zn were uniform, and no obvious elemental redistribution was observed. With increasing holding time, the microhardness of the alloy gradually increased, the corrosion potential shifted positively, the corrosion current density and corrosion rate decreased continuously, and the charge transfer resistance increased progressively. These results indicate that heat treatment duration has a significant effect on the microstructure, mechanical properties, and electrochemical degradation behavior of Fe-4.8Zn alloy, which provides an experimental support for the heat-treatment optimization of Fe-Zn alloys for biodegradable vascular stent applications.
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表 1 电沉积Fe-Zn合金溶液组成
Table 1. Bath compositions of electrodeposition for Fe-Zn alloys
Chemicals Concentration/(g·L-1) Purity/% FeCl2·4H2O 253.00 99.0 ZnCl2 30.50 98.0 NaCl 45.00 AR MnCl2·4H2O 19.50 99.0 C6H8O6 5.00 AR C6H5Na3O7·2H2O 0.88 99.0 C6H4SO2NNaCO·2H2O 1.90 AR CH3(CH2)11OSO3Na 0.10 AR H3BO3 30.00 99.5 C3H4O4 5.00 98.0 表 2 电沉积Fe-4.8Zn合金的工艺参数
Table 2. Process parameters for the electrodeposition of Fe-4.8Zn alloy
Parameters ton+/ms toff+/ms ton−/ms toff−/ms Ip+/(A·dm-2) Ip−/(A·dm-2) N+ N− F/Hz setpoint 0.2 1.8 0.2 1.8 10 8 20 5 500 表 3 配制
1000 mL SBF所需的试剂及用量Table 3. Reagents and dosages for preparing 1000 mL SBF
Reagents Amount/g Purity/% NaCl 8.036 AR NaHCO3 0.352 AR KCl 0.225 AR K2HPO4·3H2O 0.230 AR MgCl2·6H2O 0.311 AR HCl* 40* CaCl2 0.293 AR Na2SO4 0.072 AR TRIS 6.063 99.8 注:*指浓度为1.0 mol/mL的HCl溶液,用量为40 mL。 表 4 从动电位极化曲线获得的电化学参数
Table 4. Electrochemical parameters obtained from potentiodynamic polarization curves
Times/min Ecorr /V Icorr /(μA·cm-2) CR/(mm·a-1) Untreated −0.769 17.431 0.205 20 −0.757 14.699 0.173 40 −0.737 13.310 0.157 60 −0.706 11.804 0.139 表 5 电化学阻抗谱拟合结果
Table 5. Fitting results of EIS
Times/min Rs/(Ω·cm−2) WR/(Ω·cm2) CPEdl×104/(F·cm2·s1-n) ndl Rct/(Ω·cm-2) Untreated 24.31 1257 6.99 0.72 922 20 29.14 1246 3.66 0.77 1128 40 30.51 1295 2.04 0.81 1578 60 35.40 1326 2.18 0.77 1749 -
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