Zr基块体金属玻璃变形行为研究
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摘要
金属玻璃因为其优异的性能可以作为结构材料、功能材料在众多尖端领域有着极其重要的应用前景。然而,由于其有限的玻璃形成能力和室温塑性,金属玻璃的实际应用受到严重地制约。本文以Zr基金属玻璃为对象,研究了添加合金元素对其玻璃形成能力以及变形能力的影响,并设计了一系列实验研究了块体金属玻璃的变形行为。
研究了Al、Fe和Ag的添加对Zr_35Ti_(30)Cu_(7.5)Be_(27.5)合金玻璃形成能力的影响。结果显示,当添加Al和Ag的含量为1at.%以及Fe的含量为2at.%、3at.%、5at.%和7at.%时,Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al、Fe和Ag)玻璃形成体系的临界尺寸均由15 mm大幅度提高到20 mm以上。同时,热力学判据(ΔT_x或γ或T_(rg))可以有效地表征Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al、Fe和Ag)玻璃形成体系的非晶形成能力。
研究了Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al、Fe和Ag)块体金属玻璃的室温单轴压缩性能,结果表明,Al含量为1.5at.%时,块体金属玻璃(直径为3 mm)的不可恢复应变达到了15.3%,而且具有非常优异的变形能力。通过SEM对块体金属玻璃的断裂形貌进行了观察,发现Fe含量为10at.%以及Ag含量为7at.%和10at.%的样品断口类似于准解理断裂。利用TEM手段对Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al、Fe和Ag)块体金属玻璃进行了微观结构表征,Al含量为1.5at.%和2at.%、Fe含量为1at.%和2at.%以及所有添加Ag的块体金属玻璃均发生了液相分离现象。
研究了纳米尺度下退火温度对Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5)块体金属玻璃变形行为的影响,结果表明553 K弛豫态玻璃试样的变形能力要好于铸态和693 K晶化态试样的塑性变形能力。
剪切带的形成和扩展是金属玻璃进行室温变形的主要途径。利用在块体金属玻璃压缩试样上做标记的方法,通过FESEM手段测量了压缩过程中剪切带的滑移位移。结果表明,无论是变形能力较差的Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5)还是变形能力优异的Zr_(64.13)Cu_(15.75)Ni_(10.12)Al_(10)块体金属玻璃,单轴压缩条件下剪切带沿着加载方向上的位移之和分别达到了各自不可回复应变总量的95.32%和93.89%。
最后,为了进一步理解剪切带在金属玻璃变形过程中的作用,本文设计了新颖的压缩-拉伸混合实验,对比研究了剪切带对块体金属玻璃和304不锈钢拉伸强度的影响。结果表明,压缩过程中产生的剪切带极大地降低了块体金属玻璃的抗拉强度,相反,304不锈钢的屈服强度和拉伸强度则几乎没有变化。同时结合TEM和SEM结果,讨论了块体金属玻璃中剪切带的演变规律。
Metallic glasses can be used as structural and advanced functional materials in many fields and have extremely important applications due to their excellent properties. However, the practical applications of metallic glasses are severely constrained because of their limited glass forming ability (GFA) and plasticity. In the dissertation, we studied the effects of minor addition on the GFA and deformability of a Zr-based bulk metallic glass (BMG). Additionally, a series of experiments were designed to study the deformation behavior of BMGs.
The effects of alloying elements Al, Fe and Ag on the GFA of Zr_35Ti_(30)Cu_(7.5)Be_(27.5) alloy were discusssed. It was found that 1at.% Al (or Ag) or 2, 3 , 5 and 7at.% Fe addition can greatly improve the GFA of Zr_35Ti_(30)Cu_(7.5)Be_(27.5) alloy and the critical size were increased from 15 mm to larger than 20 mm. Meanwhile, the thermodynamic criterion (ΔT_x orγor T_(rg)) were effective in evaluating the GFA of Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al, Fe and Ag) glass forming systems.
The uniaxial compression performance of Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x (M=Al, Fe and Ag) BMGs were studied. The results indicated that BMG (3 mm in diameter) containing 1.5at.% Al showed a irreversible strain of 15.3% and excellent deformability.
The morphologies of the fractured samples were examined by scanning electron microscopy (SEM). Different from conventional vein-like pattern, the fracture morphology of BMGs containing 10at.% Fe, 7 and 10at.% Ag was similar to that of quasi-cleavage fracture. The microstructures of Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x (M=Al, Fe and Ag) BMGs were investigated by using transmission electron microscopy (TEM). It was found that TEM bright field images of BMGs of Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)Al_x (x=1.5 and 2), Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)Fe_x (x=1 and 2) and Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)Ag_x (x=1, 2, 3, 5 and 7) were composed of phases with brighter and darker contrasts, indicating phase separation occurred during sodification.
Nanoindentation experiments were carried out to study the influence of annealing temperatures on deformation behavior of Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5) BMG. The results showed that the deformability of the sample annealed at 553 K was significantly better than that of the as-cast samples and the ones annealed at 693 K.
The deformation of metallic glasses was mainly caused by the formation and propagation of shear bands. In the current work, the sliding displacements of shear bands under compression were measured precisely by field emission scanning electron microscopy (FESEM). From the FESEM observations, the sliding displacements of shear bands accounts for 95.32% and 93.89% of the total irreversible strain for Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5) BMG and Zr_(64.13)Cu_(15.75)Ni_(10.12)Al_(10) BMG, respectively.
For further understanding the role of shear bands played during deformation in BMGs, innovative and reliable compression-tension experiment was designed. We comparatively studied the influence of the shear bands formed during compression on the tensile strength of Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5) BMG and the 304 stainless steeel. It was found that while the tensile strength of Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5) BMG decreased remarkably after precompression, the yielding and tensile strength of the 304 stainless steel remain nearly the same as that without pre-compression. The evolution of shear bands in BMGs was also discussed.
研究了Al、Fe和Ag的添加对Zr_35Ti_(30)Cu_(7.5)Be_(27.5)合金玻璃形成能力的影响。结果显示,当添加Al和Ag的含量为1at.%以及Fe的含量为2at.%、3at.%、5at.%和7at.%时,Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al、Fe和Ag)玻璃形成体系的临界尺寸均由15 mm大幅度提高到20 mm以上。同时,热力学判据(ΔT_x或γ或T_(rg))可以有效地表征Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al、Fe和Ag)玻璃形成体系的非晶形成能力。
研究了Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al、Fe和Ag)块体金属玻璃的室温单轴压缩性能,结果表明,Al含量为1.5at.%时,块体金属玻璃(直径为3 mm)的不可恢复应变达到了15.3%,而且具有非常优异的变形能力。通过SEM对块体金属玻璃的断裂形貌进行了观察,发现Fe含量为10at.%以及Ag含量为7at.%和10at.%的样品断口类似于准解理断裂。利用TEM手段对Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al、Fe和Ag)块体金属玻璃进行了微观结构表征,Al含量为1.5at.%和2at.%、Fe含量为1at.%和2at.%以及所有添加Ag的块体金属玻璃均发生了液相分离现象。
研究了纳米尺度下退火温度对Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5)块体金属玻璃变形行为的影响,结果表明553 K弛豫态玻璃试样的变形能力要好于铸态和693 K晶化态试样的塑性变形能力。
剪切带的形成和扩展是金属玻璃进行室温变形的主要途径。利用在块体金属玻璃压缩试样上做标记的方法,通过FESEM手段测量了压缩过程中剪切带的滑移位移。结果表明,无论是变形能力较差的Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5)还是变形能力优异的Zr_(64.13)Cu_(15.75)Ni_(10.12)Al_(10)块体金属玻璃,单轴压缩条件下剪切带沿着加载方向上的位移之和分别达到了各自不可回复应变总量的95.32%和93.89%。
最后,为了进一步理解剪切带在金属玻璃变形过程中的作用,本文设计了新颖的压缩-拉伸混合实验,对比研究了剪切带对块体金属玻璃和304不锈钢拉伸强度的影响。结果表明,压缩过程中产生的剪切带极大地降低了块体金属玻璃的抗拉强度,相反,304不锈钢的屈服强度和拉伸强度则几乎没有变化。同时结合TEM和SEM结果,讨论了块体金属玻璃中剪切带的演变规律。
Metallic glasses can be used as structural and advanced functional materials in many fields and have extremely important applications due to their excellent properties. However, the practical applications of metallic glasses are severely constrained because of their limited glass forming ability (GFA) and plasticity. In the dissertation, we studied the effects of minor addition on the GFA and deformability of a Zr-based bulk metallic glass (BMG). Additionally, a series of experiments were designed to study the deformation behavior of BMGs.
The effects of alloying elements Al, Fe and Ag on the GFA of Zr_35Ti_(30)Cu_(7.5)Be_(27.5) alloy were discusssed. It was found that 1at.% Al (or Ag) or 2, 3 , 5 and 7at.% Fe addition can greatly improve the GFA of Zr_35Ti_(30)Cu_(7.5)Be_(27.5) alloy and the critical size were increased from 15 mm to larger than 20 mm. Meanwhile, the thermodynamic criterion (ΔT_x orγor T_(rg)) were effective in evaluating the GFA of Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x(M=Al, Fe and Ag) glass forming systems.
The uniaxial compression performance of Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x (M=Al, Fe and Ag) BMGs were studied. The results indicated that BMG (3 mm in diameter) containing 1.5at.% Al showed a irreversible strain of 15.3% and excellent deformability.
The morphologies of the fractured samples were examined by scanning electron microscopy (SEM). Different from conventional vein-like pattern, the fracture morphology of BMGs containing 10at.% Fe, 7 and 10at.% Ag was similar to that of quasi-cleavage fracture. The microstructures of Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)M_x (M=Al, Fe and Ag) BMGs were investigated by using transmission electron microscopy (TEM). It was found that TEM bright field images of BMGs of Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)Al_x (x=1.5 and 2), Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)Fe_x (x=1 and 2) and Zr_(35-x)Ti_(30)Cu_(7.5)Be_(27.5)Ag_x (x=1, 2, 3, 5 and 7) were composed of phases with brighter and darker contrasts, indicating phase separation occurred during sodification.
Nanoindentation experiments were carried out to study the influence of annealing temperatures on deformation behavior of Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5) BMG. The results showed that the deformability of the sample annealed at 553 K was significantly better than that of the as-cast samples and the ones annealed at 693 K.
The deformation of metallic glasses was mainly caused by the formation and propagation of shear bands. In the current work, the sliding displacements of shear bands under compression were measured precisely by field emission scanning electron microscopy (FESEM). From the FESEM observations, the sliding displacements of shear bands accounts for 95.32% and 93.89% of the total irreversible strain for Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5) BMG and Zr_(64.13)Cu_(15.75)Ni_(10.12)Al_(10) BMG, respectively.
For further understanding the role of shear bands played during deformation in BMGs, innovative and reliable compression-tension experiment was designed. We comparatively studied the influence of the shear bands formed during compression on the tensile strength of Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5) BMG and the 304 stainless steeel. It was found that while the tensile strength of Zr_(41.2)Ti_(13.8)Cu_(12.5)Ni_(10)Be_(22.5) BMG decreased remarkably after precompression, the yielding and tensile strength of the 304 stainless steel remain nearly the same as that without pre-compression. The evolution of shear bands in BMGs was also discussed.
引文
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