Al-X（Si，Zr，Ca）-P合金中磷化物的研究
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摘要
本文利用高倍视频显微镜(HSVM)、电子探针显微分析仪(EPMA)、X射线衍射仪(XRD)、差示扫描量热仪(DSC)、透射电子显微镜(TEM)及场发射扫描电子显微镜(FESEM)等测试手段对Al-Si-P、Al-Zr-P、Al-Si-Ca-P合金中磷化物进行了研究。分析了Al-Si-P熔体中AlP团簇结构,并提出了AlP孪晶凹角生长机制；发明了一种高效稳定型Al-Zr-P中间合金,揭示了ZrP与AlP之间的演变行为；明确了Al-Si-Ca-P合金中Ca对AlP的抑制作用机制；研究了Al-Si-P、Al-Zr-P中间合金对过共晶Al-Si合金的细化行为。
本文的主要研究工作如下：
(1) Al-Si-P熔体中的AlP团簇结构及其生长机制研究
采用第一性原理分子动力学模拟对Al80Si15P5熔体中AlP团簇结构进行了研究,进一步解释了AlP在Al-Si熔体中的演变行为。研究发现,P原子周围存在强烈的化学短程序,在1100℃时熔体中存在以P原子为核心的Al6P结构单元,将熔体温度升至2600℃时该结构转变为(6Al+Si)P。
试验研究发现,Al-Si-P系合金由三种物相组成,即α-Al,Si及AlP。热力学分析表明,AlP晶体{111}晶面的生长方式为小平面生长,而{100}、{110}晶面则属于非小平面生长。对Al-Si-P合金的断口进行分析,观察到AlP具有孪晶棱边和凹槽。在此基础上提出了AlP孪晶凹角生长机制,从而解释了AlP在Al-Si熔体中的生长过程,即AlP从元素浓度较高的孪晶凹槽处开始生长,随着晶体继续生长,一些高指数晶面消失,最终AlP晶体被密排{111}面包围。
(2) Al-Zr-P合金中ZrP演变及其生长机制研究
通过第一性原理分子动力学模拟发现,在Al90Zr5P5合金体系中,Zr-P原子之间的相互作用力要远远大于其它各原子间的作用力,即Zr原子倾向于在第一近邻处与更多的P原子相键合。在800℃温度下,Al90Zr5P5合金熔体中存在(6Al+Zr)P结构单元。而在1600℃温度下,Al90Zr5P5合金熔体中存在(7Al+Zr)P结构单元。试验研究发现,在一定的熔炼条件下向Al-P合金熔体中引入Zr,可使其中的AlP转变为ZrP,从而可制备出不含AlP的Al-Zr-P合金,由α-Al、ZrAl3和ZrP相组成。进一步研究表明,向Al-Zr-P合金中添加Si时,ZrP又演变为AlP。
在该合金体系中,ZrP为复式面心立方结构,经过萃取处理后发现该物相呈现立方体结构。另外,在ZrP晶体生长过程中,各晶面之间生长速率的差异将会导致形成不同的形貌。同时,由于熔体扩散的影响,Zr、P原子更易于在已析出ZrP颗粒的边角处富集,从而促进了该晶体(111)方向的突出生长,而{100}晶面面心部分则易于形成Al富集。基于此,ZrP相呈现出立方体形貌,同时其{100}晶面呈漏斗状,而这种结构也为ZrAl3相的形核、生长提供了现成的台阶。
(3) Al-Si-Ca-P合金中Ca对AlP相的抑制作用研究
元素Ca作为Al-Si合金中常见杂质元素,严重影响了磷对初晶Si的细化效果。通过分析发现,在Al-4Ca-2P合金体系中,元素Ca以Al4Ca和Ca3P2相的形式存在。其中,Ca3P2相呈现条絮状且表面比较粗糙,存在多个晶面凸起。而在Al-xSi-2Ca-1P合金体系中,即Si含量依次为6.0%、12.0%、18.0%时,元素Ca主要以Al2Si2Ca和Ca3P2相的形式存在。通过Al-12Si-0.4Ca-0.2P合金断面组织分析发现,这两种富钙相均呈现粗大板片状。
对含Ca量约为400ppm的Al-12Si合金中添加200ppmP进行处理,合金中并未呈现磷变质效果。其原因在于,Ca与P之间生成了稳定的Ca3P2化合物,从而使得熔体中没有可作为初晶Si异质核心的AlP相。多余的元素Ca促使合金表现出Na变质效果的同时,还可与Al、Si反应生成粗大板片状Al2Si2Ca相。
(4) Al-Si-P和Al-Zr-P中间合金在过共晶Al-Si合金中的应用
基于对Al-Si-P合金中AlP团簇结构及其溶解与析出行为的分析,在细化过程中AlP在Al-Si熔体中的行为如下：大尺寸颗粒→溶解→Al6P结构单元形成的团簇→AlP微晶。对于不同的含磷中间合金而言,其细化机制均为AlP异质形核初晶Si,同时AlP在熔体中均需经历上述过程,方可呈现出良好的细化效果。
试验发现,Al-17Si-2.5P中间合金的微观组织对其细化行为有一定的影响。比如,经快速凝固处理的Al-17Si-2.5P中间合金内AlP相尺寸细小、分布均匀,这促进了细化过程中AlP的溶解,从而进一步地增加了P吸收率,最终提高了细化效率。
采用正交试验优化了Al-17Si-2.5P中间合金对A390合金的细化工艺,即磷添加量375ppm,熔体处理温度800℃,保温时间30min。在优化方案下,初晶Si的平均尺寸可以由116.3μm细化至14.0gm,其形貌呈现近球状,分布也变得更加均匀。同时,布氏硬度、室温抗拉强度分别提高了14.1%、27.8%。
Al-6Zr-2P中间合金对A390合金具有良好的细化效果。其细化机理为,在异类原子对Si-Zr之间较强作用力及化学动力学因素双重作用下ZrP转变为AlP相,从而发挥其对初晶Si相的细化作用。该中间合金中ZrP在Al-Si熔体中的演变过程可用下式表示：ZrP颗粒→溶解→局域结构重组→Al6P结构单元形成的团簇→AlP微晶。
The phosphides in Al-Si-P, Al-Zr-P and Al-Si-Ca-P alloys were systematically studied using high scope video microscope (HSVM), electron probe micro-analyzer (EPMA), X-ray diffraction (XRD), differential scanning calorimeter (DSC), transmission electron microscope (TEM) and field-emission scanning electron microscope (FESEM), etc. The AlP cluster structures in Al-Si-P melt were analyzed. Furthermore, it was discovered that AlP grows with the twin plane reentrant edge (TPRE). A novel Al-Zr-P master alloy with ZrP particles was successfully synthesized and the phase transformation between ZrP and AlP was discussed. Meanwhile, the inhibitory effect of Ca on the phosphorus modification treatment was studied in Al-Si-Ca-P alloy. In addition, the extensive applications of Al-Si-P and Al-Zr-P alloy in the refinement of hypereutectic Al-Si alloys were also researched.
The major research efforts of the present study are as follows:
(1) The cluster structure and growth mechanism of AlP in Al-Si-P melt
The structure of liquid Al80Si15P5 alloy was investigated by ab initio molecular dynamics simulation. It was found that the overwhelming chemical short-range order around P atoms is the characteristic structure of liquid Al18Si15P5 alloy. The P-centered Al6P structural units exist at 1100℃, however, the structure units are slightly distorted into (6Al+Si)P at 2600℃.
The typical microstructure of Al-Si-P master alloy is composed of a-Al, Si phases and AlP particles. Based on the thermodynamic data derived, an AlP crystal is typically faceted on the close-packed {111} faces and non-faceted on {100} and {110} faces. In the fracture plane of Al-Si-P alloy, AlP hexagonal platelets with twin reentrant and ridges are observed. Meanwhile, the twin-related growth model is applied to explain the growth process of AlP crystals. Nucleation events are allowed to take place at the reentrant corners. As the AlP crystals continue to grow, some high-index planes would disappear, AlP crystals would be surrounded by close-packed {111} planes.
(2) The phase transformation and growth mechanism of phosphide in Al-Zr-P alloy
The structure of liquid Al90Zr5P5 alloy was investigated by ab initio molecular dynamics simulation. It was found that the affinity between Zr and P atoms is much stronger than that between other atoms. That is to say the Zr atoms will be found most frequently at the first shell rather than other coordination shell of P atoms. The (6Al+Zr)P structural units exist at 800℃. However, the structural units are distorted into (7Al+Zr)P at 1600℃. With the addition of Zr into Al-P alloy under certain conditions, the transformation from AlP to ZrP can occur and a novel Al-Zr-P alloy without AlP is successfully synthesized, which is composed of a-Al, ZrAl3 and ZrP. With further studies, it is found that Si in the melt can promote the transformation from ZrP to AlP.
Under the present conditions in fabrication process, the extracted ZrP particles with a NaCl structure present the cubic three-dimensional morphologies clearly. In the crystal growth process, the difference of the growth rate between each plane will lead to crystals precipitated with different morphologies. Furthermore, due to the atoms diffusion in the melt, Zr and P atoms are enriched more easily on the corners or edges of ZrP particles, and the growth rate along <111> crystal orientation is promoted. Meanwhile, Al atoms are enriched at the center of {100} crystal planes, which leads to the {100} planes as hopper structure, and consequently this structure could supply necessary growth steps for ZrAl3 phase.
(3) The inhibition effect of Ca on AlP modification in Al-Si-Ca-P alloy
As a common impurity, Ca has serious influence on the phosphorus modification of Al-Si alloys. It is found that Ca takes the form of Al4Ca and Ca3P2 phases. Furthermore, Ca3P2 compounds exhibit flocculent morphology with rough surface. In addition, in Al-xSi-2Ca-1P alloys in which the concentrations of Si are 6.0%,12.0% and 18% respectively, all of calcium compounds take the form of Al2Si2Ca and Ca3P2 phases. It is found that these two compounds exhibit thick plate-like shape in the fracture plane of Al-12Si-0.4Ca-0.2P alloy.
The phosphorus modification effect on Al-12Si alloy can not be obtained with the addition of 400 ppm Ca and 200 ppm P. Due to the formation of Ca3P2 compounds, there is no AlP in the melt which can act as the heterogeneous nucleation sites for primary Si. Meanwhile, the residual Ca can make the microstructure of Al-12Si alloy as that modified by Na. Furthermore, it can react with Al and Si atoms to form the coarse plate-like Al2Si2Ca phase.
(4) Application of Al-Si-P and Al-Zr-P master alloys on the refinement of primary Si in hypereutectic Al-Si alloys
Based on the cluster structure, dissolution and precipitation characteristic of AlP in the melt, the behavior of AlP in Al-Si melt can be deduced as follows:larger crystal→dissolution→clustering of A6P unit→AlP microcrystal. According to different phosphorus modifier, the refinement mechanism is the same, which is the heterogeneous nucleation mechanism of AlP for the primary Si. Meanwhile, the transformation of AlP listed above is necessary for the modifier to display excellent refinement performance.
Firstly, it was found that the microstructure of Al-17Si-2.5P master alloys has a certain influence on the refinement performance. For example, the fine nodular-like AlP particles with uniform distribution can be obtained with rapid solidification processing. After addition of the master alloy into Al-Si melt, these AlP particles are easier to dissolve into the melt due to the higher energy and dislocation defect, which improves the P recovery and nucleation rate and thus leads to an improved refining performance.
Secondly, an orthogonal test was designed to investigate the integrated effects of refining factors and subsequently to optimize the processing parameters. It is found that under the optimized conditions, i.e., phosphorus addition of 375 ppm, melting temperature of 800℃, and holding time of 30 min, the average sizes of primary Si can be most remarkably decreased from 116.3μm to 14.0μm with sphere-like morphology. Meanwhile, the Brinell hardness and tensile strength can be significantly increased by 14.1% and 27.8%, respectively.
Al-6Zr-2P master alloy has excellent refinement effect on the primary Si in hypereutectic A390 alloys. The refinement mechanism is that the stronger affinity between Zr and Si atoms and the chemical kinetic factors promote the transformation from ZrP to AlP and subsequently AlP particles act as the heterogeneous nucleation sites of primary Si. The transformation behavior of ZrP in the Al-Si melt can be expressed as follows:ZrP crystal→dissolution→local structural reorganization→clustering of A6P unit→AlP microcrystal.
本文的主要研究工作如下：
(1) Al-Si-P熔体中的AlP团簇结构及其生长机制研究
采用第一性原理分子动力学模拟对Al80Si15P5熔体中AlP团簇结构进行了研究,进一步解释了AlP在Al-Si熔体中的演变行为。研究发现,P原子周围存在强烈的化学短程序,在1100℃时熔体中存在以P原子为核心的Al6P结构单元,将熔体温度升至2600℃时该结构转变为(6Al+Si)P。
试验研究发现,Al-Si-P系合金由三种物相组成,即α-Al,Si及AlP。热力学分析表明,AlP晶体{111}晶面的生长方式为小平面生长,而{100}、{110}晶面则属于非小平面生长。对Al-Si-P合金的断口进行分析,观察到AlP具有孪晶棱边和凹槽。在此基础上提出了AlP孪晶凹角生长机制,从而解释了AlP在Al-Si熔体中的生长过程,即AlP从元素浓度较高的孪晶凹槽处开始生长,随着晶体继续生长,一些高指数晶面消失,最终AlP晶体被密排{111}面包围。
(2) Al-Zr-P合金中ZrP演变及其生长机制研究
通过第一性原理分子动力学模拟发现,在Al90Zr5P5合金体系中,Zr-P原子之间的相互作用力要远远大于其它各原子间的作用力,即Zr原子倾向于在第一近邻处与更多的P原子相键合。在800℃温度下,Al90Zr5P5合金熔体中存在(6Al+Zr)P结构单元。而在1600℃温度下,Al90Zr5P5合金熔体中存在(7Al+Zr)P结构单元。试验研究发现,在一定的熔炼条件下向Al-P合金熔体中引入Zr,可使其中的AlP转变为ZrP,从而可制备出不含AlP的Al-Zr-P合金,由α-Al、ZrAl3和ZrP相组成。进一步研究表明,向Al-Zr-P合金中添加Si时,ZrP又演变为AlP。
在该合金体系中,ZrP为复式面心立方结构,经过萃取处理后发现该物相呈现立方体结构。另外,在ZrP晶体生长过程中,各晶面之间生长速率的差异将会导致形成不同的形貌。同时,由于熔体扩散的影响,Zr、P原子更易于在已析出ZrP颗粒的边角处富集,从而促进了该晶体(111)方向的突出生长,而{100}晶面面心部分则易于形成Al富集。基于此,ZrP相呈现出立方体形貌,同时其{100}晶面呈漏斗状,而这种结构也为ZrAl3相的形核、生长提供了现成的台阶。
(3) Al-Si-Ca-P合金中Ca对AlP相的抑制作用研究
元素Ca作为Al-Si合金中常见杂质元素,严重影响了磷对初晶Si的细化效果。通过分析发现,在Al-4Ca-2P合金体系中,元素Ca以Al4Ca和Ca3P2相的形式存在。其中,Ca3P2相呈现条絮状且表面比较粗糙,存在多个晶面凸起。而在Al-xSi-2Ca-1P合金体系中,即Si含量依次为6.0%、12.0%、18.0%时,元素Ca主要以Al2Si2Ca和Ca3P2相的形式存在。通过Al-12Si-0.4Ca-0.2P合金断面组织分析发现,这两种富钙相均呈现粗大板片状。
对含Ca量约为400ppm的Al-12Si合金中添加200ppmP进行处理,合金中并未呈现磷变质效果。其原因在于,Ca与P之间生成了稳定的Ca3P2化合物,从而使得熔体中没有可作为初晶Si异质核心的AlP相。多余的元素Ca促使合金表现出Na变质效果的同时,还可与Al、Si反应生成粗大板片状Al2Si2Ca相。
(4) Al-Si-P和Al-Zr-P中间合金在过共晶Al-Si合金中的应用
基于对Al-Si-P合金中AlP团簇结构及其溶解与析出行为的分析,在细化过程中AlP在Al-Si熔体中的行为如下：大尺寸颗粒→溶解→Al6P结构单元形成的团簇→AlP微晶。对于不同的含磷中间合金而言,其细化机制均为AlP异质形核初晶Si,同时AlP在熔体中均需经历上述过程,方可呈现出良好的细化效果。
试验发现,Al-17Si-2.5P中间合金的微观组织对其细化行为有一定的影响。比如,经快速凝固处理的Al-17Si-2.5P中间合金内AlP相尺寸细小、分布均匀,这促进了细化过程中AlP的溶解,从而进一步地增加了P吸收率,最终提高了细化效率。
采用正交试验优化了Al-17Si-2.5P中间合金对A390合金的细化工艺,即磷添加量375ppm,熔体处理温度800℃,保温时间30min。在优化方案下,初晶Si的平均尺寸可以由116.3μm细化至14.0gm,其形貌呈现近球状,分布也变得更加均匀。同时,布氏硬度、室温抗拉强度分别提高了14.1%、27.8%。
Al-6Zr-2P中间合金对A390合金具有良好的细化效果。其细化机理为,在异类原子对Si-Zr之间较强作用力及化学动力学因素双重作用下ZrP转变为AlP相,从而发挥其对初晶Si相的细化作用。该中间合金中ZrP在Al-Si熔体中的演变过程可用下式表示：ZrP颗粒→溶解→局域结构重组→Al6P结构单元形成的团簇→AlP微晶。
The phosphides in Al-Si-P, Al-Zr-P and Al-Si-Ca-P alloys were systematically studied using high scope video microscope (HSVM), electron probe micro-analyzer (EPMA), X-ray diffraction (XRD), differential scanning calorimeter (DSC), transmission electron microscope (TEM) and field-emission scanning electron microscope (FESEM), etc. The AlP cluster structures in Al-Si-P melt were analyzed. Furthermore, it was discovered that AlP grows with the twin plane reentrant edge (TPRE). A novel Al-Zr-P master alloy with ZrP particles was successfully synthesized and the phase transformation between ZrP and AlP was discussed. Meanwhile, the inhibitory effect of Ca on the phosphorus modification treatment was studied in Al-Si-Ca-P alloy. In addition, the extensive applications of Al-Si-P and Al-Zr-P alloy in the refinement of hypereutectic Al-Si alloys were also researched.
The major research efforts of the present study are as follows:
(1) The cluster structure and growth mechanism of AlP in Al-Si-P melt
The structure of liquid Al80Si15P5 alloy was investigated by ab initio molecular dynamics simulation. It was found that the overwhelming chemical short-range order around P atoms is the characteristic structure of liquid Al18Si15P5 alloy. The P-centered Al6P structural units exist at 1100℃, however, the structure units are slightly distorted into (6Al+Si)P at 2600℃.
The typical microstructure of Al-Si-P master alloy is composed of a-Al, Si phases and AlP particles. Based on the thermodynamic data derived, an AlP crystal is typically faceted on the close-packed {111} faces and non-faceted on {100} and {110} faces. In the fracture plane of Al-Si-P alloy, AlP hexagonal platelets with twin reentrant and ridges are observed. Meanwhile, the twin-related growth model is applied to explain the growth process of AlP crystals. Nucleation events are allowed to take place at the reentrant corners. As the AlP crystals continue to grow, some high-index planes would disappear, AlP crystals would be surrounded by close-packed {111} planes.
(2) The phase transformation and growth mechanism of phosphide in Al-Zr-P alloy
The structure of liquid Al90Zr5P5 alloy was investigated by ab initio molecular dynamics simulation. It was found that the affinity between Zr and P atoms is much stronger than that between other atoms. That is to say the Zr atoms will be found most frequently at the first shell rather than other coordination shell of P atoms. The (6Al+Zr)P structural units exist at 800℃. However, the structural units are distorted into (7Al+Zr)P at 1600℃. With the addition of Zr into Al-P alloy under certain conditions, the transformation from AlP to ZrP can occur and a novel Al-Zr-P alloy without AlP is successfully synthesized, which is composed of a-Al, ZrAl3 and ZrP. With further studies, it is found that Si in the melt can promote the transformation from ZrP to AlP.
Under the present conditions in fabrication process, the extracted ZrP particles with a NaCl structure present the cubic three-dimensional morphologies clearly. In the crystal growth process, the difference of the growth rate between each plane will lead to crystals precipitated with different morphologies. Furthermore, due to the atoms diffusion in the melt, Zr and P atoms are enriched more easily on the corners or edges of ZrP particles, and the growth rate along <111> crystal orientation is promoted. Meanwhile, Al atoms are enriched at the center of {100} crystal planes, which leads to the {100} planes as hopper structure, and consequently this structure could supply necessary growth steps for ZrAl3 phase.
(3) The inhibition effect of Ca on AlP modification in Al-Si-Ca-P alloy
As a common impurity, Ca has serious influence on the phosphorus modification of Al-Si alloys. It is found that Ca takes the form of Al4Ca and Ca3P2 phases. Furthermore, Ca3P2 compounds exhibit flocculent morphology with rough surface. In addition, in Al-xSi-2Ca-1P alloys in which the concentrations of Si are 6.0%,12.0% and 18% respectively, all of calcium compounds take the form of Al2Si2Ca and Ca3P2 phases. It is found that these two compounds exhibit thick plate-like shape in the fracture plane of Al-12Si-0.4Ca-0.2P alloy.
The phosphorus modification effect on Al-12Si alloy can not be obtained with the addition of 400 ppm Ca and 200 ppm P. Due to the formation of Ca3P2 compounds, there is no AlP in the melt which can act as the heterogeneous nucleation sites for primary Si. Meanwhile, the residual Ca can make the microstructure of Al-12Si alloy as that modified by Na. Furthermore, it can react with Al and Si atoms to form the coarse plate-like Al2Si2Ca phase.
(4) Application of Al-Si-P and Al-Zr-P master alloys on the refinement of primary Si in hypereutectic Al-Si alloys
Based on the cluster structure, dissolution and precipitation characteristic of AlP in the melt, the behavior of AlP in Al-Si melt can be deduced as follows:larger crystal→dissolution→clustering of A6P unit→AlP microcrystal. According to different phosphorus modifier, the refinement mechanism is the same, which is the heterogeneous nucleation mechanism of AlP for the primary Si. Meanwhile, the transformation of AlP listed above is necessary for the modifier to display excellent refinement performance.
Firstly, it was found that the microstructure of Al-17Si-2.5P master alloys has a certain influence on the refinement performance. For example, the fine nodular-like AlP particles with uniform distribution can be obtained with rapid solidification processing. After addition of the master alloy into Al-Si melt, these AlP particles are easier to dissolve into the melt due to the higher energy and dislocation defect, which improves the P recovery and nucleation rate and thus leads to an improved refining performance.
Secondly, an orthogonal test was designed to investigate the integrated effects of refining factors and subsequently to optimize the processing parameters. It is found that under the optimized conditions, i.e., phosphorus addition of 375 ppm, melting temperature of 800℃, and holding time of 30 min, the average sizes of primary Si can be most remarkably decreased from 116.3μm to 14.0μm with sphere-like morphology. Meanwhile, the Brinell hardness and tensile strength can be significantly increased by 14.1% and 27.8%, respectively.
Al-6Zr-2P master alloy has excellent refinement effect on the primary Si in hypereutectic A390 alloys. The refinement mechanism is that the stronger affinity between Zr and Si atoms and the chemical kinetic factors promote the transformation from ZrP to AlP and subsequently AlP particles act as the heterogeneous nucleation sites of primary Si. The transformation behavior of ZrP in the Al-Si melt can be expressed as follows:ZrP crystal→dissolution→local structural reorganization→clustering of A6P unit→AlP microcrystal.
引文
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