Cu-Sn/Sb及Pb-Bi/Sb合金熔体结构转变的可逆性及其对凝固的影响
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摘要
凝固现象及规律的研究,既涉及基础学科的发展又关系到材料研发和加工工艺的革新。人们认识到液态物质结构及基本性质对固体材料最终组织与性能具有重要影响,即液-固相关性,这一领域的研究引起了越来越多的关注,并被认为是凝固理论及技术发展的新突破口之一。过去人们多集中于采用熔体热处理工艺改变熔体热历史,籍以改变材料的组织和性能。但由于对其本质和规律的认知不足,其效果及人们对其认识往往大相径庭。
近年,液态物质多型性得到了科学界普遍关注,很多物质的液态结构被发现随温度或压力而发生异常变化。随着温度诱导液-液结构转变在越来越多的纯金属和合金中被发现,使得人们对熔体结构变化的规律和机理有了进一步的认识,同时也为液-固相关性的研究提供了一个新的切入点。本文从探索温度诱导液-液结构转变的可逆性入手,运用多种实验及分析手段研究了不同类型(不可逆型与可逆型)的液-液结构转变对Cu-Sn/Sb、Pb-Bi/Sb等系统不同成分合金的凝固行为和组织的影响,期望能够进一步深化对液-固相关性的本质、规律及作用机制的认识,从而为采用不同熔体处理方法来操控熔体状态,进而为更有效地控制材料凝固行为及最终组织与性能提供科学与技术依据。本文取得的创新性工作进展及主要结论如下:
(1)选取InSn49.1(wt.%)共晶合金熔体作为研究对象,通过高温XRD实验证实了采用电阻率、热电势和内耗这些间接方法来探索温度诱导液-液结构转变是非常有效的。此外,应用近自由电子模型(NFE)和液体内耗、粘度相关理论,本文初步探讨了熔体内部的结构参数如何影响电阻率、热电势、内耗和粘度等物性参数发生变化。结果表明,在熔体发生液-液结构转变期间,电子密度n_e和导电电子平均自由程L_0的突变导致了电阻率和热电势发生了异常变化,而内耗和粘度的突变则可能与近邻原子间距等结构参数的异常变化有关。
(2)利用直流四电极电阻法和热电势法研究了Cu-Sn/Sb、Pb-Bi/Sb等合金的液态电阻率、热电势随温度的变化关系,并与DSC/DTA和内耗实验结果作对比,发现这些熔体的物性参数在一些特定温度区间内发生了不连续变化,这揭示了这几种熔体在相应的温度范围内发生了温度诱导的液-液结构转变。此外,不同的合金系或同一合金系不同成分的合金熔体的结构转变具有自身的特点,表现为转变模式、类型和发生温度区间不同。
对于CuSn30、PbBi56.1、PbBi80和PbSb5.8熔体来说,它们的电阻率在升温过程中发生了突变,而在降温过程中则呈线性变化,这揭示了熔体在升温过程中发生了不可逆的液-液结构转变。分析认为,这种不可逆液-液结构转变主要是由低温时残留于熔体中的类固型原子团簇在高温时被打破引起的。
CuSn80和CuSb70合金熔体的多轮升降温电阻实验结果表明,两种合金熔体在首轮升温过程中都发生了不可逆的液-液结构转变,并且经过首轮升温过程中的不可逆结构转变之后,熔体由原先的结构状态变为另一种新的结构状态,新的熔体所发生的温度诱导结构转变具有自身的可逆性。通过对比各轮ρ-T曲线的变化模式和参考凝固实验结果可知:CuSn80熔体在首轮升温过程中发生的两次不可逆结构转变可能与对应于固体中的η相(Cu_6Sn_5)及ε相(Cu_3Sn)的熔体异类原子团簇被破坏有关,可逆结构转变则可能与新形成的Cu_(33)Sn_(67)或者Sn原子团簇具有可逆性有关;CuSb70熔体的结构转变可逆性与Cu_2Sb化学短程序具有可逆性有关。
(3)由于熔体结构转变类型不同,其对合金的凝固过程影响不同。实验结果表明,不可逆型液-液结构转变对亚包晶成分合金CuSn30、共晶合金PbBi56.1和过共晶合金PbBi80的凝固组织和凝固行为产生了明显影响,例如会导致形核过冷度增大、凝固体积分数增长速率的峰值增大、枝晶搭接阶段提前、晶粒尺寸细化和凝固组织形态等参数的变化。
对于可逆结构转变来说,则需分两种情况来讨论。若可逆原子团簇能够在降温过程中重新建立,则可逆型液-液结构转变对合金的凝固行为和凝固组织没有明显的影响。如果可逆原子团簇不能够在该冷却速度下重新建立,那么可能会对合金的凝固行为和组织产生明显的影响。
这两方面的结果揭示了“固体结构和性能与其母相液体热历史相关”的物理本质,同时也表明,工艺上要达到有效地运用熔体处理方法来操控材料的凝固行为和组织,需要预先掌握熔体结构是否、如何发生变化。否则,存在一定的盲目性,也可能达不到预期目的。
(4)考察了不可逆型液-液结构转变对PbSb5.8(wt.%)合金定向凝固的影响,发现结构转变对溶质再分配和枝晶生长过程有显著影响。研究结果表明:液-液结构转变会导致溶质分配系数k减小,进而引起界面前沿的溶质富集程度和成分过冷加剧,一次枝晶芯部溶质含量降低(除后期液淬区外),并在不同抽拉速度下对成分偏析产生不同程度影响;此外,液-液结构转变还导致液淬区二次枝晶间距明显减小。在不同抽拉速度条件下,液-液结构转变对试样的一次枝晶间距λ_1有着不同的影响,但呈现出一定的规律性。
Researches on the phenomena and regularities of solidifications are not only realted to the development of basic subjects, by also to the inovations of development and processing technolgies of materials. It has been recognized that melt structures have great effects on solidified microstructures and properties of solids, namely "the correlations between liquid to solid". This field attracts more and more attentions and become a new breaktrough of solidification theories and techniques. In the past, people changed the melt thermal history by melt overheating treatments, and further improved the solidified microstructures and properties of materials. However, due to the exact mechanism of the melt overheating is still not fully understood, the actual effects of melt overheating treatments are tend to not as good as the expectations.
Recently, more and more attentions have been paid to liquid polyamorphism, and the liquid structure transitions are observed and verified to occur with temeperature or pressure. With the fact that temperature-induced liquid-liquid structure transitions (TI-LLSTs) have been found in more and more liquid metals and alloys, the regularity and mechanism of liquid structure changes have been understood more and more clearly. At the same time, the above mentioned facts provide a new viewpoint to investigate the liquid-solid correlation. In the present paper, the reversibility of TI-LLSTs of Cu-Sn, Pb-Bi and Pb-Sb alloys was explored, and the influences of TI-LLSTs with different characteristics (reversible and irreversible) on the solidified behaviors and solidified microstructures of those alloys were investigated. The present work aimed at deepening the understand of the essence and mechanism of the liquid-solid correlationship, and furthermore, providing a scientific and technical basis for controlling the solidified beaviors, solified microstructures and properties of as-cast by manipulating the liquid structural states. The innovative points and mian results of this paper are listed below.
(1) The high temperature XRD results of InSn49.1(wt.%) melt proved that the methods of exploration the liquid structure by measuring their resistivity, thermal power, and internal friction are effective. In addition, in present paper, a theoretical discussion on the correlation between structure and physical properties of InSn49.1 melt was also given. It is believed that, during the TI-LLST, the sudden changes of electron density n_e and mean free path of conduction electrons L_0 lead to the abnormal change of resistivity and thermal power, and anomalous changes of internal friction and viscosity might related to the discontious variation of pair distribution functions and mean nearest neighbor distance.
(2)The temperature dependences of resistivity(p-T) and thermal power(S-T) of Cu-Sn/Sb and Pb-Bi/Sb melts were investigated with the DC four probes method, and compared with the results of DSC/DTA and internal friction(Q~(-1)). The p-T, S-T, DSC/DTA and Q~(-1)-T curves of those melts also changed within certain temperatures, which suggested the TI-LLSTs occurred in those melts. In addition, the structure changes of different alloys have different features, which reflected on the occurring temperature ranges, pattern and types of those TI-LLSTs were different.
Theρ-T curves of CuSn30, PbBi56.1, PbBi80 and PbSb5.8 melts changed unlinearly in the heating procedure, but changed linearly in the cooling process, which suggested the irreversible TI-LLSTs occurred in the heating procedure of those melts. It is believed that the TI-LLSTs were resulted from the destruction of solid-like clusters in the certain high temperature ranges.
The results of resisitivity experiments show that the reversible TI-LLSTs were occurred in the heating process of CuSn80 and CuSb70 melts. After the melts experienced irreversible TI-LLSTs, the structures of them changed into new ones, and the TI-LLSTs occurred in new melt are reversible. By analysis the pattern ofρ-T curves and the results of solidification experiments, it is believed that the irreversible TI-LLSTs is related to the destruction of the solid-like clusters corresponding to Cu_6Sn_5 and Cu_3Sn, but the reversible TI-LLST may be related to Cu_(33)Sn_(67) or Sn clusters. The reversible TI-LLST occurred in CuSb70 melt may be related to the rebuliting/destruction of Cu_2Sb clusters.
(3) Different types of TI-LLSTs have different influences on the solidification of alloy. The results of solidification experiments show that, the irreversible TI-LLSTs have great effects on solidification of CuSn30, PbBi56.1 and PbBi80 melts, such as the enlarged undercooling, increased nucleation rate, advanced dendrite coherency point, refined microstructures, and modified morphologies.
However, to the melt which experienced reversible TI-LLST, we should discuss it from two aspects. If the reversible clusters return to the state of beforehand, then the reversible TI-LLST has no obvious effects on solidification behaviors and microstructures. If we can prevent the reversible clusters not return to the state of beforehand, the solidification behaviors and microstructures would be apparently changed.
These results revealed the physical nature of "correlation between solidified microstructures and the melt thermal history", and also suggested that, to control the solidification behaviors and solidified microstructures more effectively by manipulating the melt thermal history, whether and how the melt structures change should be kwown in advance. Or else, due to the blindness, the melt thermal treatments may not be effective for controlling solidification.
(4) We also investigated the influences of TI-LLST on the directional solidification microstructures and the composition segregation patterns of the alloy PbSb5.8. It was found that the TI-LLST affected greatly on the solute redistribution and the dendrite growth. Firstly, the TI-LLST would lead to the reduction of solute redistribution coefficient. Secondly, it results in the aggravation of solute enrichment and composition undercooling in front of the liquid-solid interface. Furthermore, TI-LLST gives rise to an obvious reduction of the secondary dendrtic spacing and composition decrease along the dendrite core. The effects of TI-LLST on the primary dendrtic spacing revealed some regularities, although the TI-LLST has different effects on the primary dendrtic spacing under different drawing velocitys.
近年,液态物质多型性得到了科学界普遍关注,很多物质的液态结构被发现随温度或压力而发生异常变化。随着温度诱导液-液结构转变在越来越多的纯金属和合金中被发现,使得人们对熔体结构变化的规律和机理有了进一步的认识,同时也为液-固相关性的研究提供了一个新的切入点。本文从探索温度诱导液-液结构转变的可逆性入手,运用多种实验及分析手段研究了不同类型(不可逆型与可逆型)的液-液结构转变对Cu-Sn/Sb、Pb-Bi/Sb等系统不同成分合金的凝固行为和组织的影响,期望能够进一步深化对液-固相关性的本质、规律及作用机制的认识,从而为采用不同熔体处理方法来操控熔体状态,进而为更有效地控制材料凝固行为及最终组织与性能提供科学与技术依据。本文取得的创新性工作进展及主要结论如下:
(1)选取InSn49.1(wt.%)共晶合金熔体作为研究对象,通过高温XRD实验证实了采用电阻率、热电势和内耗这些间接方法来探索温度诱导液-液结构转变是非常有效的。此外,应用近自由电子模型(NFE)和液体内耗、粘度相关理论,本文初步探讨了熔体内部的结构参数如何影响电阻率、热电势、内耗和粘度等物性参数发生变化。结果表明,在熔体发生液-液结构转变期间,电子密度n_e和导电电子平均自由程L_0的突变导致了电阻率和热电势发生了异常变化,而内耗和粘度的突变则可能与近邻原子间距等结构参数的异常变化有关。
(2)利用直流四电极电阻法和热电势法研究了Cu-Sn/Sb、Pb-Bi/Sb等合金的液态电阻率、热电势随温度的变化关系,并与DSC/DTA和内耗实验结果作对比,发现这些熔体的物性参数在一些特定温度区间内发生了不连续变化,这揭示了这几种熔体在相应的温度范围内发生了温度诱导的液-液结构转变。此外,不同的合金系或同一合金系不同成分的合金熔体的结构转变具有自身的特点,表现为转变模式、类型和发生温度区间不同。
对于CuSn30、PbBi56.1、PbBi80和PbSb5.8熔体来说,它们的电阻率在升温过程中发生了突变,而在降温过程中则呈线性变化,这揭示了熔体在升温过程中发生了不可逆的液-液结构转变。分析认为,这种不可逆液-液结构转变主要是由低温时残留于熔体中的类固型原子团簇在高温时被打破引起的。
CuSn80和CuSb70合金熔体的多轮升降温电阻实验结果表明,两种合金熔体在首轮升温过程中都发生了不可逆的液-液结构转变,并且经过首轮升温过程中的不可逆结构转变之后,熔体由原先的结构状态变为另一种新的结构状态,新的熔体所发生的温度诱导结构转变具有自身的可逆性。通过对比各轮ρ-T曲线的变化模式和参考凝固实验结果可知:CuSn80熔体在首轮升温过程中发生的两次不可逆结构转变可能与对应于固体中的η相(Cu_6Sn_5)及ε相(Cu_3Sn)的熔体异类原子团簇被破坏有关,可逆结构转变则可能与新形成的Cu_(33)Sn_(67)或者Sn原子团簇具有可逆性有关;CuSb70熔体的结构转变可逆性与Cu_2Sb化学短程序具有可逆性有关。
(3)由于熔体结构转变类型不同,其对合金的凝固过程影响不同。实验结果表明,不可逆型液-液结构转变对亚包晶成分合金CuSn30、共晶合金PbBi56.1和过共晶合金PbBi80的凝固组织和凝固行为产生了明显影响,例如会导致形核过冷度增大、凝固体积分数增长速率的峰值增大、枝晶搭接阶段提前、晶粒尺寸细化和凝固组织形态等参数的变化。
对于可逆结构转变来说,则需分两种情况来讨论。若可逆原子团簇能够在降温过程中重新建立,则可逆型液-液结构转变对合金的凝固行为和凝固组织没有明显的影响。如果可逆原子团簇不能够在该冷却速度下重新建立,那么可能会对合金的凝固行为和组织产生明显的影响。
这两方面的结果揭示了“固体结构和性能与其母相液体热历史相关”的物理本质,同时也表明,工艺上要达到有效地运用熔体处理方法来操控材料的凝固行为和组织,需要预先掌握熔体结构是否、如何发生变化。否则,存在一定的盲目性,也可能达不到预期目的。
(4)考察了不可逆型液-液结构转变对PbSb5.8(wt.%)合金定向凝固的影响,发现结构转变对溶质再分配和枝晶生长过程有显著影响。研究结果表明:液-液结构转变会导致溶质分配系数k减小,进而引起界面前沿的溶质富集程度和成分过冷加剧,一次枝晶芯部溶质含量降低(除后期液淬区外),并在不同抽拉速度下对成分偏析产生不同程度影响;此外,液-液结构转变还导致液淬区二次枝晶间距明显减小。在不同抽拉速度条件下,液-液结构转变对试样的一次枝晶间距λ_1有着不同的影响,但呈现出一定的规律性。
Researches on the phenomena and regularities of solidifications are not only realted to the development of basic subjects, by also to the inovations of development and processing technolgies of materials. It has been recognized that melt structures have great effects on solidified microstructures and properties of solids, namely "the correlations between liquid to solid". This field attracts more and more attentions and become a new breaktrough of solidification theories and techniques. In the past, people changed the melt thermal history by melt overheating treatments, and further improved the solidified microstructures and properties of materials. However, due to the exact mechanism of the melt overheating is still not fully understood, the actual effects of melt overheating treatments are tend to not as good as the expectations.
Recently, more and more attentions have been paid to liquid polyamorphism, and the liquid structure transitions are observed and verified to occur with temeperature or pressure. With the fact that temperature-induced liquid-liquid structure transitions (TI-LLSTs) have been found in more and more liquid metals and alloys, the regularity and mechanism of liquid structure changes have been understood more and more clearly. At the same time, the above mentioned facts provide a new viewpoint to investigate the liquid-solid correlation. In the present paper, the reversibility of TI-LLSTs of Cu-Sn, Pb-Bi and Pb-Sb alloys was explored, and the influences of TI-LLSTs with different characteristics (reversible and irreversible) on the solidified behaviors and solidified microstructures of those alloys were investigated. The present work aimed at deepening the understand of the essence and mechanism of the liquid-solid correlationship, and furthermore, providing a scientific and technical basis for controlling the solidified beaviors, solified microstructures and properties of as-cast by manipulating the liquid structural states. The innovative points and mian results of this paper are listed below.
(1) The high temperature XRD results of InSn49.1(wt.%) melt proved that the methods of exploration the liquid structure by measuring their resistivity, thermal power, and internal friction are effective. In addition, in present paper, a theoretical discussion on the correlation between structure and physical properties of InSn49.1 melt was also given. It is believed that, during the TI-LLST, the sudden changes of electron density n_e and mean free path of conduction electrons L_0 lead to the abnormal change of resistivity and thermal power, and anomalous changes of internal friction and viscosity might related to the discontious variation of pair distribution functions and mean nearest neighbor distance.
(2)The temperature dependences of resistivity(p-T) and thermal power(S-T) of Cu-Sn/Sb and Pb-Bi/Sb melts were investigated with the DC four probes method, and compared with the results of DSC/DTA and internal friction(Q~(-1)). The p-T, S-T, DSC/DTA and Q~(-1)-T curves of those melts also changed within certain temperatures, which suggested the TI-LLSTs occurred in those melts. In addition, the structure changes of different alloys have different features, which reflected on the occurring temperature ranges, pattern and types of those TI-LLSTs were different.
Theρ-T curves of CuSn30, PbBi56.1, PbBi80 and PbSb5.8 melts changed unlinearly in the heating procedure, but changed linearly in the cooling process, which suggested the irreversible TI-LLSTs occurred in the heating procedure of those melts. It is believed that the TI-LLSTs were resulted from the destruction of solid-like clusters in the certain high temperature ranges.
The results of resisitivity experiments show that the reversible TI-LLSTs were occurred in the heating process of CuSn80 and CuSb70 melts. After the melts experienced irreversible TI-LLSTs, the structures of them changed into new ones, and the TI-LLSTs occurred in new melt are reversible. By analysis the pattern ofρ-T curves and the results of solidification experiments, it is believed that the irreversible TI-LLSTs is related to the destruction of the solid-like clusters corresponding to Cu_6Sn_5 and Cu_3Sn, but the reversible TI-LLST may be related to Cu_(33)Sn_(67) or Sn clusters. The reversible TI-LLST occurred in CuSb70 melt may be related to the rebuliting/destruction of Cu_2Sb clusters.
(3) Different types of TI-LLSTs have different influences on the solidification of alloy. The results of solidification experiments show that, the irreversible TI-LLSTs have great effects on solidification of CuSn30, PbBi56.1 and PbBi80 melts, such as the enlarged undercooling, increased nucleation rate, advanced dendrite coherency point, refined microstructures, and modified morphologies.
However, to the melt which experienced reversible TI-LLST, we should discuss it from two aspects. If the reversible clusters return to the state of beforehand, then the reversible TI-LLST has no obvious effects on solidification behaviors and microstructures. If we can prevent the reversible clusters not return to the state of beforehand, the solidification behaviors and microstructures would be apparently changed.
These results revealed the physical nature of "correlation between solidified microstructures and the melt thermal history", and also suggested that, to control the solidification behaviors and solidified microstructures more effectively by manipulating the melt thermal history, whether and how the melt structures change should be kwown in advance. Or else, due to the blindness, the melt thermal treatments may not be effective for controlling solidification.
(4) We also investigated the influences of TI-LLST on the directional solidification microstructures and the composition segregation patterns of the alloy PbSb5.8. It was found that the TI-LLST affected greatly on the solute redistribution and the dendrite growth. Firstly, the TI-LLST would lead to the reduction of solute redistribution coefficient. Secondly, it results in the aggravation of solute enrichment and composition undercooling in front of the liquid-solid interface. Furthermore, TI-LLST gives rise to an obvious reduction of the secondary dendrtic spacing and composition decrease along the dendrite core. The effects of TI-LLST on the primary dendrtic spacing revealed some regularities, although the TI-LLST has different effects on the primary dendrtic spacing under different drawing velocitys.
引文
[1]傅恒志,魏炳波,郭景杰.凝固科学技术与材料.中国工程科学,2003,5(8):1-15.
[2]W.Kurz,D.J.Fisher.Fundamentals of Solidification.Switzerland:Trans Tech Pub Ltd,1998.
[3]M.C.Fleming,Solidification Processing.NewYork:McGraw-Hill Book Co,1974.
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