Mg-Al合金熔体在三种常用增强体陶瓷基板上的润湿
摘要
陶瓷增强镁基和铝基复合材料因具有低密度、高比强度和比模量等诸多优点近年来受到了人们的广泛关注。众所周知,采用铸造或熔体浸渗等液相法制备金属基复合材料时,陶瓷增强体与金属基体的润湿性好坏很大程度上决定了复合材料制备的难易程度以及其界面结合质量和最终性能的优劣。另一方面,液态金属尤其是蒸气压高的金属(如Mg)高温时普遍存在蒸发现象,而且Mg-Al合金熔体与大部分陶瓷都能发生反应。对于这种高温下润湿、蒸发和反应相互耦合的材料体系,如何评价其真实润湿性及润湿动力学是一个重要的基础科学问题。
尽管如此,由于Mg易挥发、Mg-Al熔体易氧化且与陶瓷反应等特征增加了润湿实验的难度,目前人们对Mg-Al合金熔体与陶瓷的润湿性及界面结合特征了解甚少,这在一定程度上阻碍了镁铝基复合材料的开发。因此,本文采用一种改良座滴法对全成分范围内的Mg-Al合金熔体与三种常用增强体陶瓷(Al2O3. SiC和Si02)的润湿性进行了系统地测定,利用XRD和SEM-EDS等手段对冷却试样的界面微结构及其演变行为进行了细致地考察,并结合热力学计算对体系界面反应进行了深入分析,获得的主要研究结果如下：
(1)提出了蒸发和反应共存下润湿行为的科学评价方法。体系真实润湿性建议用改良座滴法测得的初始平衡接触角进行表征。体系润湿动力学表征必须综合考虑接触角θ和接触直径D(或半径R)随时间的变化情况：(i) dD/dt>0, dθ/dt/dt=O, dθ/dt<0,表明三相线被滞留；蒸发引起接触角降低,此时接触角为后退接触角,润湿性并未真正得到改善。(iii) dD/dt<0,表明三相线发生回撤；接触角的变化(增大、减小或不变)取决于三相线回撤与蒸发之间的竞争。
(2)揭示了Mg-Al/(Al2O3、SiC和Si02)三个体系中Mg对润湿性影响的共性机制。Mg既能降低A1滴表面张力(σlv)又能降低固-液界面张力(σsl)。如果液滴表面洁净(无氧化膜)且原始体系不润湿(0>90°),则Mg的加入不一定能够改善体系的润湿性,表观上观察到的润湿性改善往往是由于Mg通过蒸发破除了Al滴表面的氧化膜所致。反之,如果原始体系润湿(θ<90°),那么Mg能够显著改善体系的润湿性。
(3)揭示了高温下三相线运动的内在控制机制。三相线运动趋势(铺展或回撤)主要取决于体系瞬时表观接触角[θa(t)]和瞬时理想平衡接触角[θe(t)]之间的大小关系。若θa(t)>θe(t),液滴倾向于铺展；若θa(t)>θe(t),则液滴倾向于回撤。三相线能否运动主要受控于三相线铺展(或回撤)驱动力[Fd(t)]与滞留作用力[Fp(t)]之间的竞争。若Fd(t)>Ep(t),则三相线发生运动；否则,三相线被滞留。Fd(t)可表述为Fd (t)=σlv(t)[cosθe (t)-cosθa (t)], σlv(t)为瞬时液体表面张力；Fp(t)主要源于固体表面上的物理缺陷(如粗糙度)和化学缺陷(如化学不均匀性)。
(4)建立了润湿、蒸发、界面反应及Mg-Al合金浓度之间的内在联系。蒸发不仅能够减小液滴体积和瞬时表观接触角[θa(t)],而且会显著改变合金浓度,从而影响体系的润湿性。界面反应能够改变界面性质及合金浓度进而影响润湿性。合金浓度的变化不但本身会影响体系的润湿性和液滴的蒸发速度,而且会影响界面反应尤其是反应产物的生成从而进一步影响润湿性。此外,通过热力学计算确定了界面反应与Mg-Al合金浓度之间的定量关系。
(5)揭示了Mg-Al/Al2O3体系液滴三相线回撤的内在机理。三相线回撤分为两种情况：第一种发生在液滴体积不断减小的阶段,主要归因于Mg蒸发引起合金中A1含量的升高[增大θe(t)]和液滴体积的减小[降θa(t)]；第二种发生在液滴体积几乎不变的阶段,主要归因于界面处MgAl2O4的形成[增大θe(t)]和液滴中少量残留Mg的蒸发[增大σlv(t)]。
(6)揭示了Mg-Al/SiC体系三相线铺展的内在机理。润湿前期液滴三相线铺展主要受控于SiC基板表面的去氧化过程。1173K时低Mg含量Mg-Al合金(如8、20和43mol.%Mg-Al)在α-SiC基板上的铺展出现由慢变快的现象主要归因于Mg向固-液界面的偏聚以及其对SiC表面去氧化速度大于Al的特征。
(7)揭示了Mg-Al/SiO2体系三相线铺展的内在机理与界面组织结构的形成机制。液滴三相线铺展主要归因于界面上尤其是三相线处Mg2Si的形成。增加Mg含量会显著提高液滴的铺展速度。体系界面反应产物区域呈现出典型的层状结构特征。它们的形成在热力学上主要受蒸发和反应导致瞬时合金浓度变化的影响；在动力学上主要受控于Mg、Al和Si的渗透与扩散。
上述研究结果可望为镁铝基复合材料的制备和开发提供一定的理论指导,并进一步丰富人们对金属-陶瓷高温润湿性及其界面化学特征的科学认识。
Ceramic reinforced magnesium-and aluminum-matrix composites have received great attention because of outstanding properties such as low density, high specific strength and stiffness. As we know, when a liquid casting or infiltration route is employed in the fabrication of metal matrix composites, the wettability between metallic matrix and ceramic reinforcement largely determines the ease of the process, the bonding quality and the final properties of the composites. On the other hand, the evaporation is ubiquitous for liquid metals especially the volatile substances such as Mg at high temperature, and most of ceramics can react with molten Mg-Al alloys. For a material system under the circumstance of the coupling of wetting, evaporation and reaction at high temperature, how to evaluate the intrinsic wettability and wetting kinetics is an important basic scientific topic.
However, Mg is highly volatile, and Mg-Al alloy is easily oxidized and also easy to react with ceramics, which would lead to difficulty in the wetting experient. As a result, up to date, the understanding of the wettability and interfacial bonding characteristics between molten Mg-Al alloy and ceramic is very poor, which could hinder the development of magnesium-aluminum matrix composites. Therefore, in this paper, we investigated systematically the wetting of three ceramic substrates normally used as reinforcements (Al2O3, SiC and SiO2) by molten Mg-Al alloys over a full composition range using an improved sessile drop method, and examined thoroughly the interfacial microstructures of some cooled samples as well as their behavior of evolution by using XRD, SEM-EDS and other means. Furthermore, the interfacial reaction was analyzed deeply by combining thermodynamic calculations and experimental results. The main studies obtained are as follows:
(1) A scientific criterion for evaluation of the wetting behavior under the circumstance of the coupling of evaporation and reaction was proposed. The initial contact angles measured by improved sessile drop method were suggested to be used to characterize the intrinsic wettability of the original systems. The characterization of wetting kinetics should simultaneously concern the variation in contact angle θ and contact diameter D (or radius R) with time:(i) dD/dt>0, d0/dt<0, suggesting that the interfacial reaction promotes the spreading of the triple line; the contact angles are advancing angles and the wetting is really improved.(ii) dD/dt=0, dθ/dt<0, suggesting that the triple line is pinned; the contact angle decreases due to the evaporation; the contact angles are receding angles and the wetting is not actually improved,(iii) dD/dt<0, suggesting that the triple line recedes; the change (increase, decrease or unchange) in contact angle depends on the competition between the recession of the triple line and the evaporation.
(2) The common mechanism for the effects of Mg on the wettability in the Mg-Al/(Al2O3, SiC and SiO2) systems was revealed. Mg can decrease not only the surface tension of the A1drop (σ/ν) but also the solid-liquid interfacial tension (σsl). Provided that the drop surface is clean (non-oxidation), if the oiginal system is non-wetting (θ>90°), the addition of Mg does not always improve the wettability; the improvement of the wetting observed is usually attributed to the disruption of the oxide film on the Al drop surface caused by the Mg evaporation. Conversely, if the original system is wetting (θ<90°), Mg can significantly improve the wettability of the system.
(3) The controlling mechanism for the movement of the triple line at high temperature was revealed. The trend of the triple line movement (spreading or receding) mainly depends on the difference in the instantaneous apparent contact angle [θa(t)] and the instantaneous assumed equilibrium contact angle [θe(t)]-If θα(t)>θe(t), the drop tends to spread; if θa(t)<θe(t), the drop tends to recede. The movement of the triple line was cotrolled by the competition between the driving force for the spreading or recession [Fd(t)] and the pinning force [Fp(t)]. If Fd(t)>Fp(t), the triple line moves. Conversely, the triple line is pinned. Fd(t) could be written as Fd(t)=σlv,(t)[cosθe(t)-cosθa(t)],σlv(t) is the instantaneous liquid surface tension; Fp(t) arises mainly from the physical (such as roughness) and chemical (such as chemical heterogeneities) defects of the solid surface.
(4) The underlying relationships between wetting, evaporation, interfacial reaction and Mg-Al alloy concentration were established. The evaporation can not only reduce the drop volume and instantaneous apparent contact angle [θa(t)], but also change significantly the alloy concentration, thereby affecting the wetting. The interfacial reaction can influence the interfacial condition, the alloy concentration, and thus the wetting. The variation in alloy concentration could affect the wetting and the evaporation rate of the drop; in addition, it would influence the interfacial reaction, especially the formation of reaction products, and further make an effect on the wetting. Furthermore, the relationship between the interfacial reaction and the Mg-Al alloy concentration was established quantificationally based on thermodynamic considerations.
(5) The underlying mechanism for the recession of the triple line in the Mg-Al/Al2O3 system was revealed. The recession of the triple line could be roughly classified into two cases. The first occurred in the stage with a decreasing drop volume and was mainly attributed to the increasing Al concentration in the alloy, which increased [θe(t)], and the diminishing drop volume, which decreased [θa(t)], resulting from the Mg evaporation; while the second in the stage with a constant drop volume and to the formation of MgAl2O4at the interface, which increased [θe(t)], and the evaporation of small amount of residual Mg in the drop, which increased [σlv(t)].
(6) The underlying mechanism for the drop spreading in the Mg-Al/SiC system was revealed. The initial spreading was mainly controlled by the deoxidation of SiC substrate surface. At1173K, for the Mg-Al alloys with lower Mg concentrations such as8,20and43mol.%on the a-SiC substrate surface, the spreading showed a transition from slow to fast, which was primarily attributed to the segregation of Mg at the solid-liquid interface and the larger deoxidation rate of SiC substrate surface for Mg than Al.
(7) The underlying mechanism for the spreading of the drop and the formation mechanism of the interfacial structures in the Mg-Al/SiO2system were revealed. The spreading was mainly attributed to the formation of Mg2Si at the interface, especially at the triple junction. The spreading rate increased with increasing the Mg concentration. Interfacial reaction product zones exhibited characteristic layered structures. The formation of these complex structures was controlled by the variation in instantaneous alloy concentration due to the evaporation and reaction from the viewpoint of thermodynamics and by the penetration and diffusion of Mg, Al and Si from the viewpoint of kinetics.
The above results are expected to not only provide helpful guidance for the preparation and development of the magnesium-aluminum matrix composites, but also further enrich the scientific understanding of the wetting and interfacial chemistry in the metal-ceramic systems at high temperatures.
尽管如此,由于Mg易挥发、Mg-Al熔体易氧化且与陶瓷反应等特征增加了润湿实验的难度,目前人们对Mg-Al合金熔体与陶瓷的润湿性及界面结合特征了解甚少,这在一定程度上阻碍了镁铝基复合材料的开发。因此,本文采用一种改良座滴法对全成分范围内的Mg-Al合金熔体与三种常用增强体陶瓷(Al2O3. SiC和Si02)的润湿性进行了系统地测定,利用XRD和SEM-EDS等手段对冷却试样的界面微结构及其演变行为进行了细致地考察,并结合热力学计算对体系界面反应进行了深入分析,获得的主要研究结果如下：
(1)提出了蒸发和反应共存下润湿行为的科学评价方法。体系真实润湿性建议用改良座滴法测得的初始平衡接触角进行表征。体系润湿动力学表征必须综合考虑接触角θ和接触直径D(或半径R)随时间的变化情况：(i) dD/dt>0, dθ/dt
(2)揭示了Mg-Al/(Al2O3、SiC和Si02)三个体系中Mg对润湿性影响的共性机制。Mg既能降低A1滴表面张力(σlv)又能降低固-液界面张力(σsl)。如果液滴表面洁净(无氧化膜)且原始体系不润湿(0>90°),则Mg的加入不一定能够改善体系的润湿性,表观上观察到的润湿性改善往往是由于Mg通过蒸发破除了Al滴表面的氧化膜所致。反之,如果原始体系润湿(θ<90°),那么Mg能够显著改善体系的润湿性。
(3)揭示了高温下三相线运动的内在控制机制。三相线运动趋势(铺展或回撤)主要取决于体系瞬时表观接触角[θa(t)]和瞬时理想平衡接触角[θe(t)]之间的大小关系。若θa(t)>θe(t),液滴倾向于铺展；若θa(t)>θe(t),则液滴倾向于回撤。三相线能否运动主要受控于三相线铺展(或回撤)驱动力[Fd(t)]与滞留作用力[Fp(t)]之间的竞争。若Fd(t)>Ep(t),则三相线发生运动；否则,三相线被滞留。Fd(t)可表述为Fd (t)=σlv(t)[cosθe (t)-cosθa (t)], σlv(t)为瞬时液体表面张力；Fp(t)主要源于固体表面上的物理缺陷(如粗糙度)和化学缺陷(如化学不均匀性)。
(4)建立了润湿、蒸发、界面反应及Mg-Al合金浓度之间的内在联系。蒸发不仅能够减小液滴体积和瞬时表观接触角[θa(t)],而且会显著改变合金浓度,从而影响体系的润湿性。界面反应能够改变界面性质及合金浓度进而影响润湿性。合金浓度的变化不但本身会影响体系的润湿性和液滴的蒸发速度,而且会影响界面反应尤其是反应产物的生成从而进一步影响润湿性。此外,通过热力学计算确定了界面反应与Mg-Al合金浓度之间的定量关系。
(5)揭示了Mg-Al/Al2O3体系液滴三相线回撤的内在机理。三相线回撤分为两种情况：第一种发生在液滴体积不断减小的阶段,主要归因于Mg蒸发引起合金中A1含量的升高[增大θe(t)]和液滴体积的减小[降θa(t)]；第二种发生在液滴体积几乎不变的阶段,主要归因于界面处MgAl2O4的形成[增大θe(t)]和液滴中少量残留Mg的蒸发[增大σlv(t)]。
(6)揭示了Mg-Al/SiC体系三相线铺展的内在机理。润湿前期液滴三相线铺展主要受控于SiC基板表面的去氧化过程。1173K时低Mg含量Mg-Al合金(如8、20和43mol.%Mg-Al)在α-SiC基板上的铺展出现由慢变快的现象主要归因于Mg向固-液界面的偏聚以及其对SiC表面去氧化速度大于Al的特征。
(7)揭示了Mg-Al/SiO2体系三相线铺展的内在机理与界面组织结构的形成机制。液滴三相线铺展主要归因于界面上尤其是三相线处Mg2Si的形成。增加Mg含量会显著提高液滴的铺展速度。体系界面反应产物区域呈现出典型的层状结构特征。它们的形成在热力学上主要受蒸发和反应导致瞬时合金浓度变化的影响；在动力学上主要受控于Mg、Al和Si的渗透与扩散。
上述研究结果可望为镁铝基复合材料的制备和开发提供一定的理论指导,并进一步丰富人们对金属-陶瓷高温润湿性及其界面化学特征的科学认识。
Ceramic reinforced magnesium-and aluminum-matrix composites have received great attention because of outstanding properties such as low density, high specific strength and stiffness. As we know, when a liquid casting or infiltration route is employed in the fabrication of metal matrix composites, the wettability between metallic matrix and ceramic reinforcement largely determines the ease of the process, the bonding quality and the final properties of the composites. On the other hand, the evaporation is ubiquitous for liquid metals especially the volatile substances such as Mg at high temperature, and most of ceramics can react with molten Mg-Al alloys. For a material system under the circumstance of the coupling of wetting, evaporation and reaction at high temperature, how to evaluate the intrinsic wettability and wetting kinetics is an important basic scientific topic.
However, Mg is highly volatile, and Mg-Al alloy is easily oxidized and also easy to react with ceramics, which would lead to difficulty in the wetting experient. As a result, up to date, the understanding of the wettability and interfacial bonding characteristics between molten Mg-Al alloy and ceramic is very poor, which could hinder the development of magnesium-aluminum matrix composites. Therefore, in this paper, we investigated systematically the wetting of three ceramic substrates normally used as reinforcements (Al2O3, SiC and SiO2) by molten Mg-Al alloys over a full composition range using an improved sessile drop method, and examined thoroughly the interfacial microstructures of some cooled samples as well as their behavior of evolution by using XRD, SEM-EDS and other means. Furthermore, the interfacial reaction was analyzed deeply by combining thermodynamic calculations and experimental results. The main studies obtained are as follows:
(1) A scientific criterion for evaluation of the wetting behavior under the circumstance of the coupling of evaporation and reaction was proposed. The initial contact angles measured by improved sessile drop method were suggested to be used to characterize the intrinsic wettability of the original systems. The characterization of wetting kinetics should simultaneously concern the variation in contact angle θ and contact diameter D (or radius R) with time:(i) dD/dt>0, d0/dt<0, suggesting that the interfacial reaction promotes the spreading of the triple line; the contact angles are advancing angles and the wetting is really improved.(ii) dD/dt=0, dθ/dt<0, suggesting that the triple line is pinned; the contact angle decreases due to the evaporation; the contact angles are receding angles and the wetting is not actually improved,(iii) dD/dt<0, suggesting that the triple line recedes; the change (increase, decrease or unchange) in contact angle depends on the competition between the recession of the triple line and the evaporation.
(2) The common mechanism for the effects of Mg on the wettability in the Mg-Al/(Al2O3, SiC and SiO2) systems was revealed. Mg can decrease not only the surface tension of the A1drop (σ/ν) but also the solid-liquid interfacial tension (σsl). Provided that the drop surface is clean (non-oxidation), if the oiginal system is non-wetting (θ>90°), the addition of Mg does not always improve the wettability; the improvement of the wetting observed is usually attributed to the disruption of the oxide film on the Al drop surface caused by the Mg evaporation. Conversely, if the original system is wetting (θ<90°), Mg can significantly improve the wettability of the system.
(3) The controlling mechanism for the movement of the triple line at high temperature was revealed. The trend of the triple line movement (spreading or receding) mainly depends on the difference in the instantaneous apparent contact angle [θa(t)] and the instantaneous assumed equilibrium contact angle [θe(t)]-If θα(t)>θe(t), the drop tends to spread; if θa(t)<θe(t), the drop tends to recede. The movement of the triple line was cotrolled by the competition between the driving force for the spreading or recession [Fd(t)] and the pinning force [Fp(t)]. If Fd(t)>Fp(t), the triple line moves. Conversely, the triple line is pinned. Fd(t) could be written as Fd(t)=σlv,(t)[cosθe(t)-cosθa(t)],σlv(t) is the instantaneous liquid surface tension; Fp(t) arises mainly from the physical (such as roughness) and chemical (such as chemical heterogeneities) defects of the solid surface.
(4) The underlying relationships between wetting, evaporation, interfacial reaction and Mg-Al alloy concentration were established. The evaporation can not only reduce the drop volume and instantaneous apparent contact angle [θa(t)], but also change significantly the alloy concentration, thereby affecting the wetting. The interfacial reaction can influence the interfacial condition, the alloy concentration, and thus the wetting. The variation in alloy concentration could affect the wetting and the evaporation rate of the drop; in addition, it would influence the interfacial reaction, especially the formation of reaction products, and further make an effect on the wetting. Furthermore, the relationship between the interfacial reaction and the Mg-Al alloy concentration was established quantificationally based on thermodynamic considerations.
(5) The underlying mechanism for the recession of the triple line in the Mg-Al/Al2O3 system was revealed. The recession of the triple line could be roughly classified into two cases. The first occurred in the stage with a decreasing drop volume and was mainly attributed to the increasing Al concentration in the alloy, which increased [θe(t)], and the diminishing drop volume, which decreased [θa(t)], resulting from the Mg evaporation; while the second in the stage with a constant drop volume and to the formation of MgAl2O4at the interface, which increased [θe(t)], and the evaporation of small amount of residual Mg in the drop, which increased [σlv(t)].
(6) The underlying mechanism for the drop spreading in the Mg-Al/SiC system was revealed. The initial spreading was mainly controlled by the deoxidation of SiC substrate surface. At1173K, for the Mg-Al alloys with lower Mg concentrations such as8,20and43mol.%on the a-SiC substrate surface, the spreading showed a transition from slow to fast, which was primarily attributed to the segregation of Mg at the solid-liquid interface and the larger deoxidation rate of SiC substrate surface for Mg than Al.
(7) The underlying mechanism for the spreading of the drop and the formation mechanism of the interfacial structures in the Mg-Al/SiO2system were revealed. The spreading was mainly attributed to the formation of Mg2Si at the interface, especially at the triple junction. The spreading rate increased with increasing the Mg concentration. Interfacial reaction product zones exhibited characteristic layered structures. The formation of these complex structures was controlled by the variation in instantaneous alloy concentration due to the evaporation and reaction from the viewpoint of thermodynamics and by the penetration and diffusion of Mg, Al and Si from the viewpoint of kinetics.
The above results are expected to not only provide helpful guidance for the preparation and development of the magnesium-aluminum matrix composites, but also further enrich the scientific understanding of the wetting and interfacial chemistry in the metal-ceramic systems at high temperatures.
引文
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