几种合金熔体的不均匀性及其特征研究
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摘要
大量的研究发现,液态金属在不同的条件下表现出不同的结构、状态和性质,而作为初始状态的液相又与金属的最终凝固组织存在着密切的联系。这使得原本属于凝聚态物理领域的液态金属研究逐步被铸造和冶金工作者所重视。
研究表明,很多合金熔体中存在着不均匀现象,而且表现为多种形式,例如,存在于升温过程中的亚稳不均匀现象；难混溶合金的液相分离现象；某些熔体中稳定存在着原子间化学作用强烈的原子团簇,使得熔体处于微观不均匀状态。在实际过程当中,这些不均匀现象对合金的熔炼和制备具有不可忽视的影响,因此进一步揭示熔体的各种不均匀现象及其特点具有重要的理论和实际意义。本文通过熔体的物理性质测试,对几种合金熔体的不均匀现象展开了以下研究：
1.合金熔体在升温过程中的亚稳不均匀现象
采用熔体电阻率测试装置,测量了Bi-Ga偏晶体系熔体在升降温过程中的电阻率。结果显示,熔体的电阻率在升温过程中出现异常变化,而在降温过程中与温度呈线性关系。分析表明,不混溶区间外成分的Bi-Ga合金熔体在升温过程中存在着亚稳微观不均匀现象,固态组织中一些富Bi或富Ga的微区由于分解的滞后被遗传到了熔体中。这种现象归因于该类合金熔体中同类原子间的结合力高于异类原子间的结合力,以及两组元元素间存在较大的密度差。微区的成分取决于合金熔体的成分。进一步升温导致微区的分解,使得熔体从微观不均匀状态向均匀状态过渡,在降温过程中表现为不可逆。
难混溶Bi33.3Ga66.7合金熔体在升温至液相分离温度以上依然存在着明显的不均匀现象。通过等温电阻率测试,研究了该合金熔体的等温均匀化过程,基于熔体电阻率在等温过程中的变化特点,推导了描述熔体等温均匀化过程的半经验关系式,也即熔体中第二相液滴体积与等温时间的关系：
通过该关系式分析发现,不均匀熔体中第二相Ga液滴在573 K以下具有较大的尺寸,尺寸越大,其受到由密度差引起的浮力越大,浮力明显阻碍了扩散过程,使得熔体均匀化需要较长的时间。而升温至673 K以上时,第二相液滴尺寸突然减小,浮力对扩散的阻碍作用明显降低,随着等温温度的继续提高,熔体均匀化所需的等温时间近线性缩短。
研究了Sn对Bi33.3Ga66.7合金熔体中亚稳不均匀现象的影响。发现Sn的添加减小了熔体中第二相液滴的尺寸,降低了液滴与基体熔体间的界面张力,从而降低了不均匀现象的稳定性和缩短了等温均匀化所需时间。Sn的作用在573 K的较低温度下更为明显。
2.难混溶合金的液相分离现象研究
通过电阻率测试研究了Bi33.3Ga66.7合金熔体的液相分离现象,并着重研究了Sn、In对难混溶Bi33.3Ga66.7合金熔体液相分离的影响。结果显示,Sn能够降低Bi33.3Ga66.7合金熔体的液相分离温度、偏晶反应温度、不混溶区间的宽度,从而减弱合金熔体的液相分离趋势；In的添加提高了Bi33.3Ga66.7合金熔体的液相分离温度,降低了偏晶反应温度,增宽了不混溶区间的宽度,也即In加剧了合金熔体的液相分离趋势。
通过热力学计算,分析了添加元素与难混溶合金各组元的混合行为。根据计算结果分析不同添加元素对液相分离的影响机理发现,当添加元素与难混溶合金的各组元均呈现自配位倾向时,该添加元素能够提高难混溶合金各组元间的互溶度,从而减弱合金的液相分离趋势；当添加元素与难混溶合金的一组元呈现自配位倾向而与另一组元呈现异配位倾向时,该添加元素降低了难混溶合金各组元间的互溶度,从而增强了合金的液相分离趋势。
3.合金熔体中的原子团簇结构
测量了有化合物形成倾向的In-Bi体系合金熔体的电阻率,发现熔体的电阻率在升降温过程中具有较好的一致性,说明该类熔体在升温过程中不存在类似于Bi-Ga偏晶体系熔体中的亚稳不均匀现象。但是,基于Nordheim定律的电阻率分析进一步证实了In-Bi熔体中稳定存在着化学结合较强的InBi类型原子团簇,说明In-Bi熔体不是理想的均匀熔体,熔体处于热力学稳定的微观不均匀状态。通过电阻率数据,估算了熔体中InBi类型原子团簇在不同温度下的含量,发现InBi原子团簇的摩尔分数×lnBi与温度T呈现如下经验关系：
在降温至熔点以上不太高的温度处,In50Bi50熔体中的InBi原子团簇含量达到较高值,表现出明显的浓度起伏,导致熔体的电阻率正偏离于高温下的线性关系。
根据熔体的电阻率特点,推断In-Bi体系熔体的结构特点为：在0-50 at.％In的成分区间内,熔体表现为InBi类型的原子团簇分布在近Bi性质的基体中；在50 at.％-100 at.％In的成分区间内,熔体的结构特点为InBi类型的原子团簇分布在近In性质的基体中。
初步探讨了合金熔体电阻率与热力学性质间的关系发现,熔体的剩余电阻率Δρ与｜ΔHmΔSm｜存在着一定联系。对于673 K下的In-Bi体系熔体,通过计算分析获得Δρ与｜ΔHmΔSm｜的关系如下：
采用高温熔体黏度仪测量了Al-12 wt.％Sn-4 wt.％Si合金熔体在降温过程中的黏度,发现熔体的黏度在1103 K和968 K处出现异常增大,计算表明熔体的流团尺寸和黏流激活能也伴随着突然增大。分析认为,在降温至1103 K-1138 K温度间隙时,熔体中Si-Si和Sn-Sn原子团簇迅速长大；在降温至968 K-998 K温度间隙处,熔体中的Si-Si原子团簇可能出现较大幅度的增长。依据熔体中原子团簇的变化特点,对合金熔体进行激冷处理,结果显示,熔体激冷处理工艺能够将高温熔体中较小的原子团簇保留到浇注温度,从而产生较深的过冷,进而细化了合金凝固组织。
A great number of investigations indicate that the structure, state and nature of liquid metal vary with the condition and correlate tightly to its as-cast structure. So, the studies on liquid metal are becoming popular for foundrymen and metallurgists which have ever been topics only in field of condensed matter physics. A popular result is that many alloy melts are in heterogeneous state in various manners. Such as, the metastable heterogeneity in heating process, the liquid phase separation of immiscible alloy, stable atom clusters formed in melt which make the melt in microheterogenous state. It should be stressed that the influence of heterogeneity in melts on the fabrication of alloy can not be neglected. So it is of great significance to further disclose the characteristic of heterogeneity in alloy melt. The works in present dissertation are carried out as follows:
1. Metastable heterogeneity in alloy melts during heating
The electrical resistivity of Bi-Ga melt during heating and cooling process was measured by resistivity measurement apparatus. The results show that the resistivity of miscible Bi-Ga alloy melt behaves anomalously with temperatue in heating process but linearly in cooling process, which indicates the existence of metastable microheterogeneity in melt during heating. Micro-domains enriched in Bi or Ga in solid state are retained to liquid state due to the relaxation of dissolution. This phenomenon is attributed to the more intensive bond between Bi-Bi and Ga-Ga than Bi-Ga, as well as the large density difference between Bi and Ga. The composition of micro-domains is found to depend on melt's composition. Further heating leads to the dissolution of micro-domains and the irreversible transition of melt from microheterogenous state to real homogeneous state.
It is found that immiscible Bi33.3Ga66.7 melt is still in serious heterogeneous state even is heated up to far above phase separation temperature. Isothermal measurements of resistivity were carried out to study the homogenization process of immiscible alloy melt. Based on the characteristic of resistivity in isothermal process a semi-empirical formulation is established for the description of isothermal homogenization process of melt, i.e. the volume of second phase droplets in melt is written as a fuction of isothermal time:
Discussions based on the formulation indicate that the second phase Ga droplets have large size in heterogeneous melt below 573 K, and the buoyancy greatly impedes the diffusion process, so the droplets present high stability. As the temperature goes up to 673 K, the size of droplets decrease sharply, then the influence of buoyancy on diffusion is feeble, so, with the increase of isothermal temperature the time need for homogenization decreaes nearly linearly.
Through isothermal experiment, the influence of tin addition on the metastable heterogeneity in Bi33.3Ga66.7 melt was studied. It is found that tin addition decreases the size of second phase droplets, as well as the interface tension between droplets and matrix melt, as a result the stability of heterogeneity and the time need for homogenization is decreased. The effect of tin is more powerful at lower temperature 573 K.
1. Study on phase separation of immiscible alloy melt
The phase separation process of immiscible Bi33.3Ga66.7 alloy was studied through resistivity. Especially, the influence of tin and indium on phase separation of Bi33.3Ga66.7 alloy was investigated. The results indicate that tin addition weakens the phase separation tendency of melt through decreaing the phase separation temperature, monotectic reaction temperature and the width of immiscible gap. Contrarily, indium enhances the phase separation tendency by increasing the phase separation temperature and width of immiscible gap, as well as decreasing the monotectic reaction temperature.
Based on thermodynamic calculation, the mixing behaviours of addition element with the components of immiscible monotectic alloy were discussed. Comparative analysis between the mixing behaviours of addition element with the components of immiscible alloy and its effect on phase separation shows that:the addition element which presents hetero-coordination tendency with one of the constituent of immiscible alloy but self-coordination tendency with the other could enhance the phase separation of immiscible alloy; The addition element which shows self-coordination tendency with both of the constituents of immiscible alloy could weaken the phase separation.
The electrical resistivity of liquid In-Bi system was measured. The measured resistivity is well coincident in heating and cooling process, indicating that this liquid system does not contain metastable heterogeneity like that in liquid Bi-Ga system during heating. But, the analysis of resistivity of In-Bi melt based on Nordheim rule manifests the stable existence of InBi type atom clusters which make the melt in thermodynamically stable microheterogeneous state. The calculated mole fraction of InBi atom clusters at different temperature follows a good empirical relationship:
As the temperature decreases to the vicinity of melting point, the content of InBi atom clusters in In50Bi50 melt attains to a large value leading to an apparent concentration fluctuation and discrepancy of resistivity of melt.
The structural characteristics of liquid In-Bi system are deduced based on the characteristic of resistivity: in the composition interval 0-50 at.% In, the melt can be seen as InBi type atom clusters distributed in Bi-like melt; in the composition interval 50 at.%-100 at.% In, the melt can be seen as InBi type atom clusters distributed in In-like melt.
Preliminary study on the correlation between resistivity and thermodynamic parameters was carried out. For liquid In-Bi system, a good relationship between△ρand |△Hm△Sm| is calculated as:
The viscosity of A1-12 wt.% Sn-4 wt.% Si melt was measured by high-temperature viscometer. It is found that the viscosity increases anomalously at 1103 K and 968 K accompanied by the abrupt changes of size of fluid units and viscous activation energy. It is speculated that Si-Si and Sn-Sn atom clusters grow abruptly in the temperature interval 1103 K-1138 K, and Si-Si atom clusters may increase greatly between 968 K and 998 K. Melt chilling was carried out according to the above-mentioned characteristic of melt structure, and it is found that smaller atom clusters at high temperature can be retained to pouring temperature by chilling, which leads to deep undercooling of melt and hence refinement of solidification structure.
研究表明,很多合金熔体中存在着不均匀现象,而且表现为多种形式,例如,存在于升温过程中的亚稳不均匀现象；难混溶合金的液相分离现象；某些熔体中稳定存在着原子间化学作用强烈的原子团簇,使得熔体处于微观不均匀状态。在实际过程当中,这些不均匀现象对合金的熔炼和制备具有不可忽视的影响,因此进一步揭示熔体的各种不均匀现象及其特点具有重要的理论和实际意义。本文通过熔体的物理性质测试,对几种合金熔体的不均匀现象展开了以下研究：
1.合金熔体在升温过程中的亚稳不均匀现象
采用熔体电阻率测试装置,测量了Bi-Ga偏晶体系熔体在升降温过程中的电阻率。结果显示,熔体的电阻率在升温过程中出现异常变化,而在降温过程中与温度呈线性关系。分析表明,不混溶区间外成分的Bi-Ga合金熔体在升温过程中存在着亚稳微观不均匀现象,固态组织中一些富Bi或富Ga的微区由于分解的滞后被遗传到了熔体中。这种现象归因于该类合金熔体中同类原子间的结合力高于异类原子间的结合力,以及两组元元素间存在较大的密度差。微区的成分取决于合金熔体的成分。进一步升温导致微区的分解,使得熔体从微观不均匀状态向均匀状态过渡,在降温过程中表现为不可逆。
难混溶Bi33.3Ga66.7合金熔体在升温至液相分离温度以上依然存在着明显的不均匀现象。通过等温电阻率测试,研究了该合金熔体的等温均匀化过程,基于熔体电阻率在等温过程中的变化特点,推导了描述熔体等温均匀化过程的半经验关系式,也即熔体中第二相液滴体积与等温时间的关系：
通过该关系式分析发现,不均匀熔体中第二相Ga液滴在573 K以下具有较大的尺寸,尺寸越大,其受到由密度差引起的浮力越大,浮力明显阻碍了扩散过程,使得熔体均匀化需要较长的时间。而升温至673 K以上时,第二相液滴尺寸突然减小,浮力对扩散的阻碍作用明显降低,随着等温温度的继续提高,熔体均匀化所需的等温时间近线性缩短。
研究了Sn对Bi33.3Ga66.7合金熔体中亚稳不均匀现象的影响。发现Sn的添加减小了熔体中第二相液滴的尺寸,降低了液滴与基体熔体间的界面张力,从而降低了不均匀现象的稳定性和缩短了等温均匀化所需时间。Sn的作用在573 K的较低温度下更为明显。
2.难混溶合金的液相分离现象研究
通过电阻率测试研究了Bi33.3Ga66.7合金熔体的液相分离现象,并着重研究了Sn、In对难混溶Bi33.3Ga66.7合金熔体液相分离的影响。结果显示,Sn能够降低Bi33.3Ga66.7合金熔体的液相分离温度、偏晶反应温度、不混溶区间的宽度,从而减弱合金熔体的液相分离趋势；In的添加提高了Bi33.3Ga66.7合金熔体的液相分离温度,降低了偏晶反应温度,增宽了不混溶区间的宽度,也即In加剧了合金熔体的液相分离趋势。
通过热力学计算,分析了添加元素与难混溶合金各组元的混合行为。根据计算结果分析不同添加元素对液相分离的影响机理发现,当添加元素与难混溶合金的各组元均呈现自配位倾向时,该添加元素能够提高难混溶合金各组元间的互溶度,从而减弱合金的液相分离趋势；当添加元素与难混溶合金的一组元呈现自配位倾向而与另一组元呈现异配位倾向时,该添加元素降低了难混溶合金各组元间的互溶度,从而增强了合金的液相分离趋势。
3.合金熔体中的原子团簇结构
测量了有化合物形成倾向的In-Bi体系合金熔体的电阻率,发现熔体的电阻率在升降温过程中具有较好的一致性,说明该类熔体在升温过程中不存在类似于Bi-Ga偏晶体系熔体中的亚稳不均匀现象。但是,基于Nordheim定律的电阻率分析进一步证实了In-Bi熔体中稳定存在着化学结合较强的InBi类型原子团簇,说明In-Bi熔体不是理想的均匀熔体,熔体处于热力学稳定的微观不均匀状态。通过电阻率数据,估算了熔体中InBi类型原子团簇在不同温度下的含量,发现InBi原子团簇的摩尔分数×lnBi与温度T呈现如下经验关系：
在降温至熔点以上不太高的温度处,In50Bi50熔体中的InBi原子团簇含量达到较高值,表现出明显的浓度起伏,导致熔体的电阻率正偏离于高温下的线性关系。
根据熔体的电阻率特点,推断In-Bi体系熔体的结构特点为：在0-50 at.％In的成分区间内,熔体表现为InBi类型的原子团簇分布在近Bi性质的基体中；在50 at.％-100 at.％In的成分区间内,熔体的结构特点为InBi类型的原子团簇分布在近In性质的基体中。
初步探讨了合金熔体电阻率与热力学性质间的关系发现,熔体的剩余电阻率Δρ与｜ΔHmΔSm｜存在着一定联系。对于673 K下的In-Bi体系熔体,通过计算分析获得Δρ与｜ΔHmΔSm｜的关系如下：
采用高温熔体黏度仪测量了Al-12 wt.％Sn-4 wt.％Si合金熔体在降温过程中的黏度,发现熔体的黏度在1103 K和968 K处出现异常增大,计算表明熔体的流团尺寸和黏流激活能也伴随着突然增大。分析认为,在降温至1103 K-1138 K温度间隙时,熔体中Si-Si和Sn-Sn原子团簇迅速长大；在降温至968 K-998 K温度间隙处,熔体中的Si-Si原子团簇可能出现较大幅度的增长。依据熔体中原子团簇的变化特点,对合金熔体进行激冷处理,结果显示,熔体激冷处理工艺能够将高温熔体中较小的原子团簇保留到浇注温度,从而产生较深的过冷,进而细化了合金凝固组织。
A great number of investigations indicate that the structure, state and nature of liquid metal vary with the condition and correlate tightly to its as-cast structure. So, the studies on liquid metal are becoming popular for foundrymen and metallurgists which have ever been topics only in field of condensed matter physics. A popular result is that many alloy melts are in heterogeneous state in various manners. Such as, the metastable heterogeneity in heating process, the liquid phase separation of immiscible alloy, stable atom clusters formed in melt which make the melt in microheterogenous state. It should be stressed that the influence of heterogeneity in melts on the fabrication of alloy can not be neglected. So it is of great significance to further disclose the characteristic of heterogeneity in alloy melt. The works in present dissertation are carried out as follows:
1. Metastable heterogeneity in alloy melts during heating
The electrical resistivity of Bi-Ga melt during heating and cooling process was measured by resistivity measurement apparatus. The results show that the resistivity of miscible Bi-Ga alloy melt behaves anomalously with temperatue in heating process but linearly in cooling process, which indicates the existence of metastable microheterogeneity in melt during heating. Micro-domains enriched in Bi or Ga in solid state are retained to liquid state due to the relaxation of dissolution. This phenomenon is attributed to the more intensive bond between Bi-Bi and Ga-Ga than Bi-Ga, as well as the large density difference between Bi and Ga. The composition of micro-domains is found to depend on melt's composition. Further heating leads to the dissolution of micro-domains and the irreversible transition of melt from microheterogenous state to real homogeneous state.
It is found that immiscible Bi33.3Ga66.7 melt is still in serious heterogeneous state even is heated up to far above phase separation temperature. Isothermal measurements of resistivity were carried out to study the homogenization process of immiscible alloy melt. Based on the characteristic of resistivity in isothermal process a semi-empirical formulation is established for the description of isothermal homogenization process of melt, i.e. the volume of second phase droplets in melt is written as a fuction of isothermal time:
Discussions based on the formulation indicate that the second phase Ga droplets have large size in heterogeneous melt below 573 K, and the buoyancy greatly impedes the diffusion process, so the droplets present high stability. As the temperature goes up to 673 K, the size of droplets decrease sharply, then the influence of buoyancy on diffusion is feeble, so, with the increase of isothermal temperature the time need for homogenization decreaes nearly linearly.
Through isothermal experiment, the influence of tin addition on the metastable heterogeneity in Bi33.3Ga66.7 melt was studied. It is found that tin addition decreases the size of second phase droplets, as well as the interface tension between droplets and matrix melt, as a result the stability of heterogeneity and the time need for homogenization is decreased. The effect of tin is more powerful at lower temperature 573 K.
1. Study on phase separation of immiscible alloy melt
The phase separation process of immiscible Bi33.3Ga66.7 alloy was studied through resistivity. Especially, the influence of tin and indium on phase separation of Bi33.3Ga66.7 alloy was investigated. The results indicate that tin addition weakens the phase separation tendency of melt through decreaing the phase separation temperature, monotectic reaction temperature and the width of immiscible gap. Contrarily, indium enhances the phase separation tendency by increasing the phase separation temperature and width of immiscible gap, as well as decreasing the monotectic reaction temperature.
Based on thermodynamic calculation, the mixing behaviours of addition element with the components of immiscible monotectic alloy were discussed. Comparative analysis between the mixing behaviours of addition element with the components of immiscible alloy and its effect on phase separation shows that:the addition element which presents hetero-coordination tendency with one of the constituent of immiscible alloy but self-coordination tendency with the other could enhance the phase separation of immiscible alloy; The addition element which shows self-coordination tendency with both of the constituents of immiscible alloy could weaken the phase separation.
The electrical resistivity of liquid In-Bi system was measured. The measured resistivity is well coincident in heating and cooling process, indicating that this liquid system does not contain metastable heterogeneity like that in liquid Bi-Ga system during heating. But, the analysis of resistivity of In-Bi melt based on Nordheim rule manifests the stable existence of InBi type atom clusters which make the melt in thermodynamically stable microheterogeneous state. The calculated mole fraction of InBi atom clusters at different temperature follows a good empirical relationship:
As the temperature decreases to the vicinity of melting point, the content of InBi atom clusters in In50Bi50 melt attains to a large value leading to an apparent concentration fluctuation and discrepancy of resistivity of melt.
The structural characteristics of liquid In-Bi system are deduced based on the characteristic of resistivity: in the composition interval 0-50 at.% In, the melt can be seen as InBi type atom clusters distributed in Bi-like melt; in the composition interval 50 at.%-100 at.% In, the melt can be seen as InBi type atom clusters distributed in In-like melt.
Preliminary study on the correlation between resistivity and thermodynamic parameters was carried out. For liquid In-Bi system, a good relationship between△ρand |△Hm△Sm| is calculated as:
The viscosity of A1-12 wt.% Sn-4 wt.% Si melt was measured by high-temperature viscometer. It is found that the viscosity increases anomalously at 1103 K and 968 K accompanied by the abrupt changes of size of fluid units and viscous activation energy. It is speculated that Si-Si and Sn-Sn atom clusters grow abruptly in the temperature interval 1103 K-1138 K, and Si-Si atom clusters may increase greatly between 968 K and 998 K. Melt chilling was carried out according to the above-mentioned characteristic of melt structure, and it is found that smaller atom clusters at high temperature can be retained to pouring temperature by chilling, which leads to deep undercooling of melt and hence refinement of solidification structure.
引文
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