微合金化对Cu基块体非晶合金形成和性能的影响
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摘要
本论文利用X射线衍射分析仪(XRD)、光学显微系统(OM)、示差扫描量热仪(DSC)、差热分析仪(DTA)、X射线光电子能谱仪(XPS)、动电位极化、失重分析法、交流阻抗谱(EIS)、扫描电子显微镜(SEM)及能谱分析仪(EDX)、电液伺服万能材料试验机(MTS)和电阻测试系统等手段系统的研究了微合金化对Cu47Zr11Ti34Ni8大块非晶合金的形成、腐蚀行为、电解水析氢活性、压缩力学性能及热电阻的影响。
采用电弧熔炼/水冷铜模吸铸法制备了Ф3mm和Ф4mm的(Cu47Zr11Ti34Ni8)100-xMx (M=Cr,Mo,W; x=0~5 at%)合金。XRD和OM分析表明,含有少量M的合金基本为单相非晶,而较高M含量的合金则为非晶合金基复合材料。由于添加元素的不同则玻璃形成能力和复合材料中析出相的形态也有差异。
DSC和DTA分析表明,相对于基体合金(x=0)而言,Cr、Mo和W的微量添加均显著提高其玻璃转变温度Tg和晶化开始温度Tx1,明显降低其熔化开始温度Tm和液态温度Tl,从而增大了约化玻璃转变温度Trg (=Tg/Tm或Tg/Tl)和参数γ(=Tx1/(Tg+Tl))。其中,含Mo合金具有最低的Tm和Tl以及最大的Trg和γ。对不同Mo含量的非晶合金的研究表明,随Mo含量的增加,Tg和Tx1显著增加而Tm和Tl明显降低,从而Trg和γ值随Mo含量的增加而增大,且熔化特征从两步变为单步。这些现象证实,微合金化既可提高基体合金玻璃态的热稳定性又可增强其玻璃形成能力,尤其是Mo的掺杂。
在室温下,采用动电位极化和静态失重法研究了微量Cr、Mo和W对基体合金在含氧的酸和碱性介质中的腐蚀行为。结果表明,这些元素的添加明显提高了基体合金的耐蚀性能。在所有的非晶态合金中,含Mo合金具有最低的腐蚀速率、钝化电流密度、钝化开始电位和最高的钝化膜破裂电位,因而其具有最好的耐蚀性能。不同Mo含量对基体合金耐蚀性能的影响不同,当Mo≤2 at%时,合金的耐蚀性随着Mo含量增加而增加,当Mo>2 at%时,合金的耐蚀性反而降低了。XPS分析表明,相对于无Mo合金而言,Mo的添加促使合金表面形成富Zr、Ti氧化物而贫Cu、Ni氧化物的钝化膜,进而提高了合金的抗腐蚀性能。恒电流阶跃分析表明,Mo的添加增加了表面钝化膜的形成速度和致密度。EIS分析表明,Mo的掺杂增加了基体合金中的“氧空位”和表面活性,抑制了阴离子空位在金属/表面膜(M/F)界面上形成,促使Zr、Ti元素在M/F界面上快速形成相应的氧化物,并增加了钝化膜中氧化层的厚度和稳定性。另外,根据该体系在电解质中的电化学反应,基于点缺陷模型(PDM)分析了微合金化提高Cu基块体非晶合金耐蚀性能的动力学机制。
水的电解实验结果表明,随着Mo含量的增加,电极过电位逐渐降低,活性逐渐增强。借用Arrhenius方程得到,Mo的掺杂降低了合金的表观激活能,有利于电解析氢反应的进行。SEM和EDX分析表明,Mo的掺杂加快金属Cu在电解过程中的析出,导致电极表面粗糙度及Ti、Zr含量增大,这不仅有利于Volmer反应发生,还有利于Heyrovsky反应或Tafel反应发生,从而提高了电极的电解活性。
力学性能测试表明,适量Mo的添加能显著改善基体合金的准静态压缩力学性能。其中,含2 at%Mo铜基块体非晶合金具有较大的塑性应变量和较高的强度,两者的值分别达到2.31 %和2. 21GPa;而3 at%Mo铜基块体非晶合金基复合材料则具有最高的强度和塑性应变量,两者的值分别为2.24 GPa和3.82%。分析认为,2 at%Mo“塑性”块体非晶合金与3 at%Mo块体非晶合金复合材料可能以不同的方式影响剪切带的行为进而提高材料的整体塑性。而5 at%Mo复合材料的第二相体积分数较高且尺寸较大,在宏观上呈脆性断裂。
利用自制的电阻测量系统,研究了(Cu47Zr11Ti34Ni8)100-xMox(x=0,2)块体非晶合金电阻率随温度变化的特征。结果表明:1)无Mo块体非晶合金具有负的电阻温度系数(TCR= -1.64×10-4)而含Mo合金具有正的TCR(=1.86×10-4),这可借助于修正的Ziman-Faber理论给以合理的解释;2)在含Mo合金的晶化前存在电阻率极大化,这是源于Mo的添加引起了合金中相分离区不同所致;3)两合金的电阻均有四个突变点,每次突变分别对应着合金微结构的调整和相的形成与长大。
In this dissertation, the effect of micro-addition of foreign elements on glass-formation, corrosion behavior, electrocatalytic behavior for hydrogen evolution reaction, compressive mechanical property, and electrical resistance at high temperature of the as-cast Cu47Zr11Ti34Ni8 bulk metallic glass was investigated profoundly using X-ray diffraction (XRD), optical microscopy (OM), differential scanning calorimetry (DSC), and differential thermal analysis (DTA), potentiodynamic polarization, weight-loss method, X-ray photoelectron spectroscopy (XPS), electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) coupled with energy dispersive X-ray detector (EDX), mechanical testing system(MTS) and resistance measurement system.
The alloying ingots with compositions of (Cu47Zr11Ti34Ni8)100-xMx (M=Cr,Mo,W; x=0~5 at%) were prepared by arc-melting the mixture of Cu, Zr, Ti, Ni, and M metals. Sample rods with a diameter of 3 mm or 4 mm were fabricated by casting the master ingots into copper mold. XRD patterns and OM observations demonstrate that a small amount of foreign element does not change the monolithic amorphous structure of the obtained alloys. Bulk metallic glass matrix composites containing crystalline precipitates will be obtained when the content of foreign element is beyond limited range. The glass-forming ability of the alloys obtained and morphologies of the precipitates in the amorphous matrix varies with the content of foreign elements.
DSC and DTA thermal analysis show that the onset temperature for glass transition (Tg) and the first crystallization (Tx) were enhanced while the melting temperature (Tm) and liquidus temperature (Tl) were decreased with a micro-addition of foreign element in (Cu47Zr11Ti34Ni8)100-xMx (M=Cr,Mo,W; x=0~5 at%) alloys, leading to the glass transition temperature (Trg=Tg/Tl or Tg/Tm) reduced and parameter (γ= Tx/(Tg+Tl)) increased. Mo-bearing alloy has the lowest Tm and Tl and the largest Trg andγ. For (Cu47Zr11Ti34Ni8)100-xMox (x=0~5 at%) bulk metallic glasses (BMGs).both Tg and Tx1 were increased while both Tm and Tl were decreased with increasing of Mo contents for the single amorphous BMGs, resulting in the enhancement of both Trg andγ. In addition, the addition of appropriate amount of Mo changes the melting process of the base BMG (i.e. Cu47Zr11Ti34Ni8 BMG) from two-step melting process to single one. The results of thermal analyses present that the thermal stability and glass-formation ability were increased with the micro-addition of foreign element, especially with the addition of Mo.
The effect of the addition of Cr, Mo or W on corrosion resistance of the base BMG was investigated by means of electrochemical polarization and weight-loss measurements. Electrochemical measurements on various Cu-based BMGs were conducted in 1 mol/L H2SO4 and 1 mol/L NaOH aqueous solutions, respectively, open to air at room temperature. It revealed that the BMGs with a small amount of Cr, Mo or W exhibited a superior corrosion resistance in the two electrolytes as compared with the base alloy (i.e. Cu47Zr11Ti34Ni8 BMG). Mo-bearing BMG exhibited the greatest corrosion resistance, as indicated by the lowest passive current density and corrosion rate, the highest pitting potential and the lowest passive potential among these BMGs. Moreover, it is found that the corrosion resistance of Cu-based BMGs was increased with increasing Mo content for (Cu47Zr11Ti34Ni8)100-xMox (x=0-3 at%) BMGs when x=0-2. However, the corrosion resistance of the sample with 3 at% Mo or higher, which is a composite containing a few of crystallites in amorphous matrix, seemed not very satisfactory, as indicated by relatively high passive current densities and corrosion rate in both electrolytes. XPS results revealed that the improvement of corrosion resistance of Cu-based BMG containing appropriate amount of Mo originated from the enrichment of ZrO2 and TiO2, but depletion in Cu- or Ni- oxides in the passive films formed during electrochemical polarization. Secondly, the galvanostatic-step measurement was performed to investigate the kinetics of the formation of passive films on the BMG surfaces. It is demonstrated that the addition of an appropriate amount of Mo can effectively improve the stability and uniformity of the passive film. Finally, EIS results implied that the micro-addition of Mo increased the surface activity and promoted the generation of positive defects (i.e., oxygen vacancies), but suppressed the formation of negative defects at the interfaces between metal/passive film (M/F). As a result, the addition of Mo could speed up the formation of the passive film of Zr-, and Ti-oxides, and stabilize simultaneously the oxides film. Base on point defect model (PDM), a qualitatively kinetic model is established to explain tentatively the effect of micro-addition of Mo on the improvement of the corrosion resistance of the Cu-based bulk metallic glasses.
The results of the catalytic studies indicates that the hydrogen over-potential for single amorphous alloys decreased gradually with the increase of Mo content and the electrocatalytic activity for hydrogen evolution reaction (HER) is improved by means of a microadulteration of Mo. According to the Arrhenius plots of the HER of the electrodes, the apparent energy of activation is then calculated from the temperature dependence of the exchange current densities. It can be seen that the apparent energy of activation decreased for the adulteration of Mo in comparison with the base alloy. SEM and EDX results imply that an increase of the electrocatalytic activity of the alloy with addition of Mo is due to the copper peeling off the surface which leading to Zr and Ti enrichment and increase of porosity on the surface of compared with the base alloy. Therefore, Tafel reaction route or Heyrovsky reaction step was promoted.
In addition, quasi-static compression test reveals that both plasticity and strength of the base alloy are remarkably enhanced by the addition of appropriate amount of Mo. The Cu-based BMG containing 2 at% Mo exhibits the large plastic strain of 2.31 and higher fracture strength of about 2.21 GPa. The Cu-based BMG matrix composite containing 3 at% Mo exhibits the highest fracture strength of 2.24 GPa and largest plastic strain of about 3.82. It is believed that the ductile BMG (for example, (Cu47Zr11Ti34Ni8)98Mo2) may follow a different deformation mechanism from the (Cu47Zr11Ti34Ni8)97Mo3 BMG composite as far as the improvement in general plasticity is concerned. However, (Cu47Zr11Ti34Ni8)95Mo5 BMG composite exhibits brittle fracture behavior due to the existence of high volume fraction of large quenched-in crystalline particles.
The electric resistance (ER) of the (Cu47Zr11Ti34Ni8)100-xMox (x=0, 2 at %) BMGs obtained were studied via the testing-system self-produce under Ar atmosphere. It was found that the temperature coefficient of resistance (TCR) is negative (-1.64×10-4) for Mo-free Cu-based BMG while the TCR is positive (1.86×10-4) for Mo-bearing. The phenomenon is interpreted based on the modified Ziman-Faber theory. Moreover, there is the maximization of ER for Mo-bearing BMG but not for the Mo-free BMG, which is originated from the different phase separatation due to the microalloying of Mo. In addition, it was found that the plots of resistivity vs. temperature exhibited four distinctive reduction-stages for two BMGs. The drops of ER are related to the change of the microstructure or the formation of crystalline phases in amorphous microstructure with temperature increasing for two BMGs.
采用电弧熔炼/水冷铜模吸铸法制备了Ф3mm和Ф4mm的(Cu47Zr11Ti34Ni8)100-xMx (M=Cr,Mo,W; x=0~5 at%)合金。XRD和OM分析表明,含有少量M的合金基本为单相非晶,而较高M含量的合金则为非晶合金基复合材料。由于添加元素的不同则玻璃形成能力和复合材料中析出相的形态也有差异。
DSC和DTA分析表明,相对于基体合金(x=0)而言,Cr、Mo和W的微量添加均显著提高其玻璃转变温度Tg和晶化开始温度Tx1,明显降低其熔化开始温度Tm和液态温度Tl,从而增大了约化玻璃转变温度Trg (=Tg/Tm或Tg/Tl)和参数γ(=Tx1/(Tg+Tl))。其中,含Mo合金具有最低的Tm和Tl以及最大的Trg和γ。对不同Mo含量的非晶合金的研究表明,随Mo含量的增加,Tg和Tx1显著增加而Tm和Tl明显降低,从而Trg和γ值随Mo含量的增加而增大,且熔化特征从两步变为单步。这些现象证实,微合金化既可提高基体合金玻璃态的热稳定性又可增强其玻璃形成能力,尤其是Mo的掺杂。
在室温下,采用动电位极化和静态失重法研究了微量Cr、Mo和W对基体合金在含氧的酸和碱性介质中的腐蚀行为。结果表明,这些元素的添加明显提高了基体合金的耐蚀性能。在所有的非晶态合金中,含Mo合金具有最低的腐蚀速率、钝化电流密度、钝化开始电位和最高的钝化膜破裂电位,因而其具有最好的耐蚀性能。不同Mo含量对基体合金耐蚀性能的影响不同,当Mo≤2 at%时,合金的耐蚀性随着Mo含量增加而增加,当Mo>2 at%时,合金的耐蚀性反而降低了。XPS分析表明,相对于无Mo合金而言,Mo的添加促使合金表面形成富Zr、Ti氧化物而贫Cu、Ni氧化物的钝化膜,进而提高了合金的抗腐蚀性能。恒电流阶跃分析表明,Mo的添加增加了表面钝化膜的形成速度和致密度。EIS分析表明,Mo的掺杂增加了基体合金中的“氧空位”和表面活性,抑制了阴离子空位在金属/表面膜(M/F)界面上形成,促使Zr、Ti元素在M/F界面上快速形成相应的氧化物,并增加了钝化膜中氧化层的厚度和稳定性。另外,根据该体系在电解质中的电化学反应,基于点缺陷模型(PDM)分析了微合金化提高Cu基块体非晶合金耐蚀性能的动力学机制。
水的电解实验结果表明,随着Mo含量的增加,电极过电位逐渐降低,活性逐渐增强。借用Arrhenius方程得到,Mo的掺杂降低了合金的表观激活能,有利于电解析氢反应的进行。SEM和EDX分析表明,Mo的掺杂加快金属Cu在电解过程中的析出,导致电极表面粗糙度及Ti、Zr含量增大,这不仅有利于Volmer反应发生,还有利于Heyrovsky反应或Tafel反应发生,从而提高了电极的电解活性。
力学性能测试表明,适量Mo的添加能显著改善基体合金的准静态压缩力学性能。其中,含2 at%Mo铜基块体非晶合金具有较大的塑性应变量和较高的强度,两者的值分别达到2.31 %和2. 21GPa;而3 at%Mo铜基块体非晶合金基复合材料则具有最高的强度和塑性应变量,两者的值分别为2.24 GPa和3.82%。分析认为,2 at%Mo“塑性”块体非晶合金与3 at%Mo块体非晶合金复合材料可能以不同的方式影响剪切带的行为进而提高材料的整体塑性。而5 at%Mo复合材料的第二相体积分数较高且尺寸较大,在宏观上呈脆性断裂。
利用自制的电阻测量系统,研究了(Cu47Zr11Ti34Ni8)100-xMox(x=0,2)块体非晶合金电阻率随温度变化的特征。结果表明:1)无Mo块体非晶合金具有负的电阻温度系数(TCR= -1.64×10-4)而含Mo合金具有正的TCR(=1.86×10-4),这可借助于修正的Ziman-Faber理论给以合理的解释;2)在含Mo合金的晶化前存在电阻率极大化,这是源于Mo的添加引起了合金中相分离区不同所致;3)两合金的电阻均有四个突变点,每次突变分别对应着合金微结构的调整和相的形成与长大。
In this dissertation, the effect of micro-addition of foreign elements on glass-formation, corrosion behavior, electrocatalytic behavior for hydrogen evolution reaction, compressive mechanical property, and electrical resistance at high temperature of the as-cast Cu47Zr11Ti34Ni8 bulk metallic glass was investigated profoundly using X-ray diffraction (XRD), optical microscopy (OM), differential scanning calorimetry (DSC), and differential thermal analysis (DTA), potentiodynamic polarization, weight-loss method, X-ray photoelectron spectroscopy (XPS), electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) coupled with energy dispersive X-ray detector (EDX), mechanical testing system(MTS) and resistance measurement system.
The alloying ingots with compositions of (Cu47Zr11Ti34Ni8)100-xMx (M=Cr,Mo,W; x=0~5 at%) were prepared by arc-melting the mixture of Cu, Zr, Ti, Ni, and M metals. Sample rods with a diameter of 3 mm or 4 mm were fabricated by casting the master ingots into copper mold. XRD patterns and OM observations demonstrate that a small amount of foreign element does not change the monolithic amorphous structure of the obtained alloys. Bulk metallic glass matrix composites containing crystalline precipitates will be obtained when the content of foreign element is beyond limited range. The glass-forming ability of the alloys obtained and morphologies of the precipitates in the amorphous matrix varies with the content of foreign elements.
DSC and DTA thermal analysis show that the onset temperature for glass transition (Tg) and the first crystallization (Tx) were enhanced while the melting temperature (Tm) and liquidus temperature (Tl) were decreased with a micro-addition of foreign element in (Cu47Zr11Ti34Ni8)100-xMx (M=Cr,Mo,W; x=0~5 at%) alloys, leading to the glass transition temperature (Trg=Tg/Tl or Tg/Tm) reduced and parameter (γ= Tx/(Tg+Tl)) increased. Mo-bearing alloy has the lowest Tm and Tl and the largest Trg andγ. For (Cu47Zr11Ti34Ni8)100-xMox (x=0~5 at%) bulk metallic glasses (BMGs).both Tg and Tx1 were increased while both Tm and Tl were decreased with increasing of Mo contents for the single amorphous BMGs, resulting in the enhancement of both Trg andγ. In addition, the addition of appropriate amount of Mo changes the melting process of the base BMG (i.e. Cu47Zr11Ti34Ni8 BMG) from two-step melting process to single one. The results of thermal analyses present that the thermal stability and glass-formation ability were increased with the micro-addition of foreign element, especially with the addition of Mo.
The effect of the addition of Cr, Mo or W on corrosion resistance of the base BMG was investigated by means of electrochemical polarization and weight-loss measurements. Electrochemical measurements on various Cu-based BMGs were conducted in 1 mol/L H2SO4 and 1 mol/L NaOH aqueous solutions, respectively, open to air at room temperature. It revealed that the BMGs with a small amount of Cr, Mo or W exhibited a superior corrosion resistance in the two electrolytes as compared with the base alloy (i.e. Cu47Zr11Ti34Ni8 BMG). Mo-bearing BMG exhibited the greatest corrosion resistance, as indicated by the lowest passive current density and corrosion rate, the highest pitting potential and the lowest passive potential among these BMGs. Moreover, it is found that the corrosion resistance of Cu-based BMGs was increased with increasing Mo content for (Cu47Zr11Ti34Ni8)100-xMox (x=0-3 at%) BMGs when x=0-2. However, the corrosion resistance of the sample with 3 at% Mo or higher, which is a composite containing a few of crystallites in amorphous matrix, seemed not very satisfactory, as indicated by relatively high passive current densities and corrosion rate in both electrolytes. XPS results revealed that the improvement of corrosion resistance of Cu-based BMG containing appropriate amount of Mo originated from the enrichment of ZrO2 and TiO2, but depletion in Cu- or Ni- oxides in the passive films formed during electrochemical polarization. Secondly, the galvanostatic-step measurement was performed to investigate the kinetics of the formation of passive films on the BMG surfaces. It is demonstrated that the addition of an appropriate amount of Mo can effectively improve the stability and uniformity of the passive film. Finally, EIS results implied that the micro-addition of Mo increased the surface activity and promoted the generation of positive defects (i.e., oxygen vacancies), but suppressed the formation of negative defects at the interfaces between metal/passive film (M/F). As a result, the addition of Mo could speed up the formation of the passive film of Zr-, and Ti-oxides, and stabilize simultaneously the oxides film. Base on point defect model (PDM), a qualitatively kinetic model is established to explain tentatively the effect of micro-addition of Mo on the improvement of the corrosion resistance of the Cu-based bulk metallic glasses.
The results of the catalytic studies indicates that the hydrogen over-potential for single amorphous alloys decreased gradually with the increase of Mo content and the electrocatalytic activity for hydrogen evolution reaction (HER) is improved by means of a microadulteration of Mo. According to the Arrhenius plots of the HER of the electrodes, the apparent energy of activation is then calculated from the temperature dependence of the exchange current densities. It can be seen that the apparent energy of activation decreased for the adulteration of Mo in comparison with the base alloy. SEM and EDX results imply that an increase of the electrocatalytic activity of the alloy with addition of Mo is due to the copper peeling off the surface which leading to Zr and Ti enrichment and increase of porosity on the surface of compared with the base alloy. Therefore, Tafel reaction route or Heyrovsky reaction step was promoted.
In addition, quasi-static compression test reveals that both plasticity and strength of the base alloy are remarkably enhanced by the addition of appropriate amount of Mo. The Cu-based BMG containing 2 at% Mo exhibits the large plastic strain of 2.31 and higher fracture strength of about 2.21 GPa. The Cu-based BMG matrix composite containing 3 at% Mo exhibits the highest fracture strength of 2.24 GPa and largest plastic strain of about 3.82. It is believed that the ductile BMG (for example, (Cu47Zr11Ti34Ni8)98Mo2) may follow a different deformation mechanism from the (Cu47Zr11Ti34Ni8)97Mo3 BMG composite as far as the improvement in general plasticity is concerned. However, (Cu47Zr11Ti34Ni8)95Mo5 BMG composite exhibits brittle fracture behavior due to the existence of high volume fraction of large quenched-in crystalline particles.
The electric resistance (ER) of the (Cu47Zr11Ti34Ni8)100-xMox (x=0, 2 at %) BMGs obtained were studied via the testing-system self-produce under Ar atmosphere. It was found that the temperature coefficient of resistance (TCR) is negative (-1.64×10-4) for Mo-free Cu-based BMG while the TCR is positive (1.86×10-4) for Mo-bearing. The phenomenon is interpreted based on the modified Ziman-Faber theory. Moreover, there is the maximization of ER for Mo-bearing BMG but not for the Mo-free BMG, which is originated from the different phase separatation due to the microalloying of Mo. In addition, it was found that the plots of resistivity vs. temperature exhibited four distinctive reduction-stages for two BMGs. The drops of ER are related to the change of the microstructure or the formation of crystalline phases in amorphous microstructure with temperature increasing for two BMGs.
引文
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