MgCu_2型Laves相Mg（Cu_（1-X）Al_X）_2的制备与表征
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摘要
AB_2型Laves相因其特殊的物理及化学性能使其成为潜在的功能材料和结构材料,引起了国内外研究学者的极大兴趣。常见的三种晶体结构为:六方C14(MgZn_2结构)、立方C15(MgCu_2结构)、复六方C36(MgNi_2结构)。这三种结构的稳定性受A原子与B原子的原子尺寸比以及Laves相的价电子浓度所控制;另外,成分、温度、第三组成元素也影响晶体结构。用轻质的、抗氧化性能高的Al、Si元素替代AB_2中的B组元,可以改变其本身的价电子浓度,以致引起晶体结构的变化。也就是说,这三种晶体结构中的任一种都可以通过适当控制Al、Si的含量使之稳定化,已成为进一步改善AB_2型Laves相性能的一条有效途径。
本文深入研究AB_2型Laves相Mg(Cu_(1-x)Al_x)_2(0≤X≤0.35)的制备工艺及成分优化,重点探讨Al替代MgCu_2中Cu对其结构稳定性及性能的影响,主要得到如下结论:
(1)3Cu-2Mg-Al粉末球磨过程中,随球磨时间的延长,粉末的颗粒尺寸减小,显微应变和有效温度系数增加;晶粒尺寸与有效温度系数和显微应变呈逆变关系,显微应变随有效温度系数增加而增大;球磨30 h后,Mg衍射峰完全消失,球磨至60 h,Al衍射峰也完全消失,Cu衍射峰进一步宽化,此时,Cu衍射峰位置向小角度偏移,形成了Mg和Al在Cu中的过饱和固溶体;球磨90 h后,有新相Mg_(32)Al_(47)Cu_7生成。
(2)采用机械活化+热爆法制备了低放热体系AB_2型Laves相Mg(Cu_(1-x)Al_x)_2(0≤x≤0.35)合金,并对热爆产物进行XRD、EPMA、SEM和DSC分析。结果表明:MgCu_2中的部分Cu被Al替代,晶体结构并不发生改变,主相是MgCu_2型λ_1相。随Al替代量的增加λ_1相的晶格常数逐渐增大,整个XRD衍射峰向低角偏移增大,致密度逐渐提高,晶粒尺寸减小,晶格畸变增大。随Al替代量的增加λ_1相的熔点先升后降,当化学计量比为Mg_2Cu_3Al(x=0.25)时,其熔点达最高,约为910℃,比MgCu_2的熔点(约797℃)高113℃,说明用轻质、抗氧化性能高的Al元素进行合金化,能够使C15结构的AB_2型Laves相的热稳定性提高,其中Mg_2Cu_3Al是更具开发潜力的化合物。
(3)采用机械活化+热压法合成Laves相Mg(Cu_(1-x)Al_x)_2(X=0,0.25),研究组织和性能。结果表明:C15结构的Laves相Mg_2Cu_3Al与MgCu_2相比,具有高的致密性、硬度和杨氏模量,其断口显示两者均为脆性断裂。最后采用基于密度函数理论(DFT)的缀加平面波加局域轨道方法和广义梯度近似对立方C15结构的MgCu_2 Laves相金属间化合物的生成焓,弹性性质,进行理论计算。计算结果与实验结构相似。
There is an increasing interest in Laves phase as their excellent physical and chemical properties make them available for potential functional as well as structural applications. Laves phase are classified into the three fundamental structures C14, C15 and C36 which are typified by MgZn_2, MgCu_2 and MgNi_2,respectively. Although they are well known since long, there are still unsolved problems concerning the stability of the respective crystal structures. Some geometric and electronic factors such as the atomic size ratio of the A and B atoms and their valence electron numbers are well known to affect the occurrence of a Laves phase and there exist various simple models based on these factors that aim at a prediction of the stable Laves phase. In addition, deviations from the stoichiometric composition were reported to result in a change of the stable polytype in various systems. The B atoms in the AB_2 were substituted by Al ,Si partially, could improve Structure and stability of Laves phases.
In this paper, The majour work of this study is the Cu atoms in the MgCu_2 were substituted by Al partially. the microstructure and property of the test materials were measured. The new opinions as follows were obtained:
(1) The mechanochemical effects of 3Cu-2Mg-Al in mechanical milling process are studied with XRD, SEM, and pulverisette5 miller. The result showed that, the crystallite size decreases, the micro strain and effective temperature factor increases, respectively, with the increasing of milling time. The effective temperature factor and micro strain increased with the decreasing of crystallite size, and micro strain increase with the increasing of effective temperature factor. After being milled for 30 hours, the diffraction peak of Mg is vanished completely. when the milling time get 60 hours, the diffraction peak of Al is vanished, also, and the diffraction peak of Cu further broaden, at the same time, its' diffraction angular shift to lower angles. The supersaturated solid solution of Mg and Al in the Cu formed, at this time. 90 hours later, the new phase of Mg_(32)Al_(47)Cu_7 can be found.
(2) The AB_2 type Laves Mg(Cu_(1-x)Al_x)_2(0≤x≤0.35) were prepared by the method of mechanical activation combining with thermal explosion and the products of thermal explosion were analyzed by XRD,EPMA ,SEM and DSC. The result showed that, although the Cu atoms in the MgCu_2 were substituted by Al partially, the structure of the intermetallcs was not changed. And the main phase wasλ_1 phase with a MgCu_2 type structure. At the same time, by the increasing of Al content, the lattice constant and angular shift to lower angles of the total diffraction peaks increased, the compactness improved, the grain size decreases, crystal lattice aberration increased a little. By the increasing of Al content, the melting point ofλ_1 phase present increasing firstly the decreasing later, the melting point of stoichiometric Mg_2Cu_3Al(X=0.25) was about 910℃which was 113℃higher than the counterpart of MgCu_2(about 797℃). This showed that choosing Al of the light and high oxidation resistance as alloying element could make the Laves phase of C15 structure more stable, and could improve various properties of the intermetallics.
(3) The Laves Mg(Cu_(1-x)Al_x)2(x=0, 0. 25) were prepared by the method of mechanical activation combining with hot pressing. Its microstructure and properties were investigated. The result showed that, compared with MgCu_2, compactness improved, hardness and Young's modules increases greatly of C15 Laves phase Mg_2Cu_3Al. Ab initio calculations were performed to calculate the elastic moduli of C15 Laves phase MgCu_2.The calculation was conducted using the method of augmented plane wave plus local orbitals (APW+lo) with the generalized gradient approximation (GGA). The enthalpy of formation for MgCu_2 was obtained by calculating the total energy. The results show that the calculated elastic properties are close to the experimental results.
本文深入研究AB_2型Laves相Mg(Cu_(1-x)Al_x)_2(0≤X≤0.35)的制备工艺及成分优化,重点探讨Al替代MgCu_2中Cu对其结构稳定性及性能的影响,主要得到如下结论:
(1)3Cu-2Mg-Al粉末球磨过程中,随球磨时间的延长,粉末的颗粒尺寸减小,显微应变和有效温度系数增加;晶粒尺寸与有效温度系数和显微应变呈逆变关系,显微应变随有效温度系数增加而增大;球磨30 h后,Mg衍射峰完全消失,球磨至60 h,Al衍射峰也完全消失,Cu衍射峰进一步宽化,此时,Cu衍射峰位置向小角度偏移,形成了Mg和Al在Cu中的过饱和固溶体;球磨90 h后,有新相Mg_(32)Al_(47)Cu_7生成。
(2)采用机械活化+热爆法制备了低放热体系AB_2型Laves相Mg(Cu_(1-x)Al_x)_2(0≤x≤0.35)合金,并对热爆产物进行XRD、EPMA、SEM和DSC分析。结果表明:MgCu_2中的部分Cu被Al替代,晶体结构并不发生改变,主相是MgCu_2型λ_1相。随Al替代量的增加λ_1相的晶格常数逐渐增大,整个XRD衍射峰向低角偏移增大,致密度逐渐提高,晶粒尺寸减小,晶格畸变增大。随Al替代量的增加λ_1相的熔点先升后降,当化学计量比为Mg_2Cu_3Al(x=0.25)时,其熔点达最高,约为910℃,比MgCu_2的熔点(约797℃)高113℃,说明用轻质、抗氧化性能高的Al元素进行合金化,能够使C15结构的AB_2型Laves相的热稳定性提高,其中Mg_2Cu_3Al是更具开发潜力的化合物。
(3)采用机械活化+热压法合成Laves相Mg(Cu_(1-x)Al_x)_2(X=0,0.25),研究组织和性能。结果表明:C15结构的Laves相Mg_2Cu_3Al与MgCu_2相比,具有高的致密性、硬度和杨氏模量,其断口显示两者均为脆性断裂。最后采用基于密度函数理论(DFT)的缀加平面波加局域轨道方法和广义梯度近似对立方C15结构的MgCu_2 Laves相金属间化合物的生成焓,弹性性质,进行理论计算。计算结果与实验结构相似。
There is an increasing interest in Laves phase as their excellent physical and chemical properties make them available for potential functional as well as structural applications. Laves phase are classified into the three fundamental structures C14, C15 and C36 which are typified by MgZn_2, MgCu_2 and MgNi_2,respectively. Although they are well known since long, there are still unsolved problems concerning the stability of the respective crystal structures. Some geometric and electronic factors such as the atomic size ratio of the A and B atoms and their valence electron numbers are well known to affect the occurrence of a Laves phase and there exist various simple models based on these factors that aim at a prediction of the stable Laves phase. In addition, deviations from the stoichiometric composition were reported to result in a change of the stable polytype in various systems. The B atoms in the AB_2 were substituted by Al ,Si partially, could improve Structure and stability of Laves phases.
In this paper, The majour work of this study is the Cu atoms in the MgCu_2 were substituted by Al partially. the microstructure and property of the test materials were measured. The new opinions as follows were obtained:
(1) The mechanochemical effects of 3Cu-2Mg-Al in mechanical milling process are studied with XRD, SEM, and pulverisette5 miller. The result showed that, the crystallite size decreases, the micro strain and effective temperature factor increases, respectively, with the increasing of milling time. The effective temperature factor and micro strain increased with the decreasing of crystallite size, and micro strain increase with the increasing of effective temperature factor. After being milled for 30 hours, the diffraction peak of Mg is vanished completely. when the milling time get 60 hours, the diffraction peak of Al is vanished, also, and the diffraction peak of Cu further broaden, at the same time, its' diffraction angular shift to lower angles. The supersaturated solid solution of Mg and Al in the Cu formed, at this time. 90 hours later, the new phase of Mg_(32)Al_(47)Cu_7 can be found.
(2) The AB_2 type Laves Mg(Cu_(1-x)Al_x)_2(0≤x≤0.35) were prepared by the method of mechanical activation combining with thermal explosion and the products of thermal explosion were analyzed by XRD,EPMA ,SEM and DSC. The result showed that, although the Cu atoms in the MgCu_2 were substituted by Al partially, the structure of the intermetallcs was not changed. And the main phase wasλ_1 phase with a MgCu_2 type structure. At the same time, by the increasing of Al content, the lattice constant and angular shift to lower angles of the total diffraction peaks increased, the compactness improved, the grain size decreases, crystal lattice aberration increased a little. By the increasing of Al content, the melting point ofλ_1 phase present increasing firstly the decreasing later, the melting point of stoichiometric Mg_2Cu_3Al(X=0.25) was about 910℃which was 113℃higher than the counterpart of MgCu_2(about 797℃). This showed that choosing Al of the light and high oxidation resistance as alloying element could make the Laves phase of C15 structure more stable, and could improve various properties of the intermetallics.
(3) The Laves Mg(Cu_(1-x)Al_x)2(x=0, 0. 25) were prepared by the method of mechanical activation combining with hot pressing. Its microstructure and properties were investigated. The result showed that, compared with MgCu_2, compactness improved, hardness and Young's modules increases greatly of C15 Laves phase Mg_2Cu_3Al. Ab initio calculations were performed to calculate the elastic moduli of C15 Laves phase MgCu_2.The calculation was conducted using the method of augmented plane wave plus local orbitals (APW+lo) with the generalized gradient approximation (GGA). The enthalpy of formation for MgCu_2 was obtained by calculating the total energy. The results show that the calculated elastic properties are close to the experimental results.
引文
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