金属熔体过热及过冷液态电阻率与结构的相关性研究
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摘要
本文通过电阻率测量,结合高温X射线衍射,从头算分子动力模拟(AIMD),粘度测量等手段,对Pb-Sb, Cu-Ni, Cu-Co, Cu-Sb及C079.5Sn20.5等合金的液态、过冷液态熔体局域结构的演变进行研究,在电子层次上(价电子、自由电子等)揭示金属熔体的液态及过冷液态的电阻率变化、微观结构演变以及它们的相关性,为完善金属凝固理论奠定一定的理论基础,为新型合金材料的开发提供理论支持。
首先,根据费米面实验数据修正的模型赝势,结合实验结构因子及硬球结构因子,计算不同温度下液态铅的电阻率,并对计算过程中的误差及模型赝势的适用性进行了分析。这加深了我们对电阻率与结构相关性的认识,也为二元Pb-Sb合金电阻率的计算奠定基础。通过测量Pb-Sb合金熔体的电阻率及粘度,发现Pb3oSb7o, Pb2oSb8O及Pb10Sb90熔体在降温过程中具有非线性的电阻率温度关系。Pb20Sb80与Pb30Sb70熔体的异常的粘度温度关系证实了异常结构转变的存在,这种异常转变被认为是具有Peierls畸变的大尺寸Sb团簇的形成。
再次,通过高温XRD, AIMD,电阻率测量及粘度测量对Cu-Sb合金熔体的结构演变进行了研究。Cu80Sb20熔体结构因子(S(q))主峰之前存在的预峰表明,熔体中存在中程有序(MRO)。熔体的偏双体分布函数表明,异类原子间距明显小于同类原子半径之和。负的V(?)arren-Cowley参数及负的TCR,异常大的粘流激活能也都表明熔体中CSRO的存在。通过纳米晶粒模型的计算得到的Cu3Sb衍射强度曲线上,也具有与实验得到的衍射强度曲线一致的预峰,这直接表明熔体中存在着与晶体Cu3Sb团簇相类似的团簇结构。Cu37Sb63及Cu20Sb80的结构因子曲线上具有明显的主峰劈裂现象,这被认为是熔体中存在着Cu-和Sb-类团簇的标志。Cu20Sb80的粘度温度关系上存在着转折,低温下粘流激活能增大,这表明了Sb类团簇及皮尔斯畸变的强化。在整个Cu-Sb合计的AIMD模拟研究中,我们发现,异类原子偏配位数明显高于同类原子的偏配位数,这表明了熔体中原子异类配位具有优先性。Sb-Sb原子间距在Cu75Sb25处具有明显的跌落,这意味着Sb-Sb配位的快速增加。电阻率的成分关系,也表明了熔体中的结构的不均匀性。而熔体中Warren-Cowley参数与浓度相关函数的负的最大值的位置明显不同,被认为是尺寸效应及其导致的成分不均匀性造成的。
其次,通过无电极测量方式,对Cu-Ni, Cu-Co合金的液态及过冷液态电阻率温度关系进行了研究。结果表明,Cu-Ni合金的液态及过冷液态具有线性的电阻率温度关系,而Cu-Co合金的液相线附近及以上温度具有线性电阻率温度关系,而在过冷区域发生了明显的转折,并且电阻率温度系数(TCR)变化的温度区间与亚稳相分离的温度区间相吻合。凝固组织研究也表明TCR发生改变的试样的凝固组织发生了相分离。这些结果表明,熔体进入过冷液态不会影响其电阻率温度关系,当熔体发生相变或者电子浓度明显变化时,TCR才会发生变化。
最后,通过对C079.5Sn20.5合金的液态、过冷结构的结构进行了XRD,电阻率,DSC表征,获得了熔体由液态到过冷液态的局域结构参数的变化。结果发现,进入过冷液态后,熔体的局域团簇的原子数目快速增加。通过凝固组织研究发现,随着过冷度的变化,Co79.5Sn20.5合金不同过冷度凝固的表面形貌及横截面的微观组织形貌均会发生变化。通过成分分析,发现初生Co固溶体的Sn含量高于固溶度极限值,获得α-Co相的溶质截留效应的直接证据,结合组织形貌分析,探索过冷结构对凝固过程中的枝晶生长方式的影响。
Using resistivity measurement, Pb-Sb, Cu-Ni, Cu-Co, Cu-Sb and melts are studied. Cu-Sb and Co79.5Sn20.5melts are also investigated combining high temperature XRD, AIMD, viscosity measurement. The structure evolution in superheated and undercooled liquid, and its relationship to resistivity change have been studied on electronic level (valence electrons, free electrons). These would lay a theoretical basis to perfect metal solidification theory and provide theoretical support to develop new alloys.
Firstly, using the pseudopotential corrected by data of Fermi surface, combined with experimental and hard-sphere structure factor, resistivity of liquid Pb is calculated. The validity and errors of calculation are discussed. This not only deepens our understanding of the relationship between resistivity and structure, but also is helpful to calculate the resistivity of Pb-Sb alloys. In Pb30Sb70, Pb20Sb80, and Pb10Sb90melts, temperature dependence of resistivity deviates from linear dependence during cooling. In Pb30Sb70and Pb20Sb80melts, abnormal viscosity verifies the existence of abnormal structure transition, which is attributed to the reinforcement of Peierls distortion.
Secondly, local structure of Cu-Sb alloys has been studied by X-ray diffraction, ab initio molecular dynamics simulation, viscosity and resistivity measurements. Over the whole concentration range, heterogeneous coordination numbers are larger than that of homogeneous atoms, indicating preferential Cu-Sb coordination. A drop is observed in maximum position of simulated Sb-Sb partial distribution functions around Cu75Sb25, which reveals the rapid increase of Sb-Sb coordination. Structural inhomogeneity has been discussed by resistivity measurements. Pre-peaks in relation with medium-range order are observed in structure factor of Cu-20at.%Sb. Negative Warren-Cowley parameters, abnormally large activation energy of viscous flow and negative TCR, reflect the existence of chemical order, which is interpreted as Cu3Sb clusters following nano-crystal model. Around eutectic melts, main peak splitting is observed in both structure factor and simulated total PDFs, which reveals the co-existence of Cu-Sb heterogeneous and Sb-Sb clusters. This results in the smaller first neighbor radius and higher viscosity in Cu37Sb63melts. In pair distribution functions of Cu20Sb80melts, the hump around0.44nm becomes obvious below973K, which reveals the reinforcement of Sb clusters with Peierls distortion. This is consistent with the increase in viscous-flow activation energy in Cu20Sb80melts around973K.
Thirdly, the resistivity behavior of undercooled liquid Cu-Ni and Cu-Co alloys had been studied by the electrodeless method, to probe the structure transition in undercooled melts during the cooling process. Over the entire concentration range, linear behavior of resistivity with temperature was obtained in Cu-Ni system. And similar results were obtained in Cu-Co system in the vicinity of liquidus temperature. However, a turning point was obvious in temperature coefficient of resistivity of Cu-Co alloys around the bimodal line, which was interpreted to be responsible for metastable liquid-liquid phase separation. During liquid phase separation process, resistivity decreased and the temperature coefficient of resistivity was larger than that of homogeneous melts. In combination with TEM and SEM studies on the as-solidified microstructure, this was interpreted as the formation of egg-type structure and concentration change in Cu-rich and Co-rich phases. These indicate that, when noble and transition melts enter into undercooled liquid states, temperature dependence of resistivity does not change.
Finally, with the help of XRD, resistivity, viscosity and DSC, structure evolution of Co79.5Sn20.5alloys has been studied from superheated to undercooled liquid state. In undercooled liquid state, the number of atoms in atomic clusters rapidly increased. The microstructure and surface morphology change with undercooling of Co79.5Sn20.5alloy. Combing melts structure, EDS and morphology analysis, the growth model in undercooled melts has been discussed.
首先,根据费米面实验数据修正的模型赝势,结合实验结构因子及硬球结构因子,计算不同温度下液态铅的电阻率,并对计算过程中的误差及模型赝势的适用性进行了分析。这加深了我们对电阻率与结构相关性的认识,也为二元Pb-Sb合金电阻率的计算奠定基础。通过测量Pb-Sb合金熔体的电阻率及粘度,发现Pb3oSb7o, Pb2oSb8O及Pb10Sb90熔体在降温过程中具有非线性的电阻率温度关系。Pb20Sb80与Pb30Sb70熔体的异常的粘度温度关系证实了异常结构转变的存在,这种异常转变被认为是具有Peierls畸变的大尺寸Sb团簇的形成。
再次,通过高温XRD, AIMD,电阻率测量及粘度测量对Cu-Sb合金熔体的结构演变进行了研究。Cu80Sb20熔体结构因子(S(q))主峰之前存在的预峰表明,熔体中存在中程有序(MRO)。熔体的偏双体分布函数表明,异类原子间距明显小于同类原子半径之和。负的V(?)arren-Cowley参数及负的TCR,异常大的粘流激活能也都表明熔体中CSRO的存在。通过纳米晶粒模型的计算得到的Cu3Sb衍射强度曲线上,也具有与实验得到的衍射强度曲线一致的预峰,这直接表明熔体中存在着与晶体Cu3Sb团簇相类似的团簇结构。Cu37Sb63及Cu20Sb80的结构因子曲线上具有明显的主峰劈裂现象,这被认为是熔体中存在着Cu-和Sb-类团簇的标志。Cu20Sb80的粘度温度关系上存在着转折,低温下粘流激活能增大,这表明了Sb类团簇及皮尔斯畸变的强化。在整个Cu-Sb合计的AIMD模拟研究中,我们发现,异类原子偏配位数明显高于同类原子的偏配位数,这表明了熔体中原子异类配位具有优先性。Sb-Sb原子间距在Cu75Sb25处具有明显的跌落,这意味着Sb-Sb配位的快速增加。电阻率的成分关系,也表明了熔体中的结构的不均匀性。而熔体中Warren-Cowley参数与浓度相关函数的负的最大值的位置明显不同,被认为是尺寸效应及其导致的成分不均匀性造成的。
其次,通过无电极测量方式,对Cu-Ni, Cu-Co合金的液态及过冷液态电阻率温度关系进行了研究。结果表明,Cu-Ni合金的液态及过冷液态具有线性的电阻率温度关系,而Cu-Co合金的液相线附近及以上温度具有线性电阻率温度关系,而在过冷区域发生了明显的转折,并且电阻率温度系数(TCR)变化的温度区间与亚稳相分离的温度区间相吻合。凝固组织研究也表明TCR发生改变的试样的凝固组织发生了相分离。这些结果表明,熔体进入过冷液态不会影响其电阻率温度关系,当熔体发生相变或者电子浓度明显变化时,TCR才会发生变化。
最后,通过对C079.5Sn20.5合金的液态、过冷结构的结构进行了XRD,电阻率,DSC表征,获得了熔体由液态到过冷液态的局域结构参数的变化。结果发现,进入过冷液态后,熔体的局域团簇的原子数目快速增加。通过凝固组织研究发现,随着过冷度的变化,Co79.5Sn20.5合金不同过冷度凝固的表面形貌及横截面的微观组织形貌均会发生变化。通过成分分析,发现初生Co固溶体的Sn含量高于固溶度极限值,获得α-Co相的溶质截留效应的直接证据,结合组织形貌分析,探索过冷结构对凝固过程中的枝晶生长方式的影响。
Using resistivity measurement, Pb-Sb, Cu-Ni, Cu-Co, Cu-Sb and melts are studied. Cu-Sb and Co79.5Sn20.5melts are also investigated combining high temperature XRD, AIMD, viscosity measurement. The structure evolution in superheated and undercooled liquid, and its relationship to resistivity change have been studied on electronic level (valence electrons, free electrons). These would lay a theoretical basis to perfect metal solidification theory and provide theoretical support to develop new alloys.
Firstly, using the pseudopotential corrected by data of Fermi surface, combined with experimental and hard-sphere structure factor, resistivity of liquid Pb is calculated. The validity and errors of calculation are discussed. This not only deepens our understanding of the relationship between resistivity and structure, but also is helpful to calculate the resistivity of Pb-Sb alloys. In Pb30Sb70, Pb20Sb80, and Pb10Sb90melts, temperature dependence of resistivity deviates from linear dependence during cooling. In Pb30Sb70and Pb20Sb80melts, abnormal viscosity verifies the existence of abnormal structure transition, which is attributed to the reinforcement of Peierls distortion.
Secondly, local structure of Cu-Sb alloys has been studied by X-ray diffraction, ab initio molecular dynamics simulation, viscosity and resistivity measurements. Over the whole concentration range, heterogeneous coordination numbers are larger than that of homogeneous atoms, indicating preferential Cu-Sb coordination. A drop is observed in maximum position of simulated Sb-Sb partial distribution functions around Cu75Sb25, which reveals the rapid increase of Sb-Sb coordination. Structural inhomogeneity has been discussed by resistivity measurements. Pre-peaks in relation with medium-range order are observed in structure factor of Cu-20at.%Sb. Negative Warren-Cowley parameters, abnormally large activation energy of viscous flow and negative TCR, reflect the existence of chemical order, which is interpreted as Cu3Sb clusters following nano-crystal model. Around eutectic melts, main peak splitting is observed in both structure factor and simulated total PDFs, which reveals the co-existence of Cu-Sb heterogeneous and Sb-Sb clusters. This results in the smaller first neighbor radius and higher viscosity in Cu37Sb63melts. In pair distribution functions of Cu20Sb80melts, the hump around0.44nm becomes obvious below973K, which reveals the reinforcement of Sb clusters with Peierls distortion. This is consistent with the increase in viscous-flow activation energy in Cu20Sb80melts around973K.
Thirdly, the resistivity behavior of undercooled liquid Cu-Ni and Cu-Co alloys had been studied by the electrodeless method, to probe the structure transition in undercooled melts during the cooling process. Over the entire concentration range, linear behavior of resistivity with temperature was obtained in Cu-Ni system. And similar results were obtained in Cu-Co system in the vicinity of liquidus temperature. However, a turning point was obvious in temperature coefficient of resistivity of Cu-Co alloys around the bimodal line, which was interpreted to be responsible for metastable liquid-liquid phase separation. During liquid phase separation process, resistivity decreased and the temperature coefficient of resistivity was larger than that of homogeneous melts. In combination with TEM and SEM studies on the as-solidified microstructure, this was interpreted as the formation of egg-type structure and concentration change in Cu-rich and Co-rich phases. These indicate that, when noble and transition melts enter into undercooled liquid states, temperature dependence of resistivity does not change.
Finally, with the help of XRD, resistivity, viscosity and DSC, structure evolution of Co79.5Sn20.5alloys has been studied from superheated to undercooled liquid state. In undercooled liquid state, the number of atoms in atomic clusters rapidly increased. The microstructure and surface morphology change with undercooling of Co79.5Sn20.5alloy. Combing melts structure, EDS and morphology analysis, the growth model in undercooled melts has been discussed.
引文
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