液态置氢对锆基块体非晶合金形成能力和力学性能的影响
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摘要
块体非晶合金具有一系列的优异性能，如屈服强度高、弹性应变极限大以及良好的耐腐蚀性能和优异的软硬磁学性能，成为当今材料界的研究热点之一。本文采用液态置氢的方法将氢加入到锆基块体非晶合金中，所谓液态置氢，指的是在氢/氩混合气氛下熔炼合金，使氢扩散到合金熔体中的一种新的置氢方法。研究了液态置氢对非晶合金熔体的净化作用，对非晶合金玻璃形成能力和力学性能的影响规律以及作用机制。
首先研究了液态置氢对去除Zr_(55)Cu_(30)Ni_5Al_(10)合金中杂质元素氧的作用，发现液态置氢对非晶合金具有明显的脱氧作用。随着氢氩混合气氛中氢含量和熔炼时间的增加，合金中的氧含量逐渐降低。当氢氩混合气氛中氢含量为15%，熔炼时间为400s时，具有最佳的脱氧作用，随后凝固得到的合金呈完全的非晶态结构。根据吉布斯自由能的变化情况，可知在高温区时，氢与氧反应的吉布斯自由能较锆与氧反应的吉布斯自由能更低，因此氢与氧更容易发生反应，从而避免了锆与氧反应形成的氧化锆或者锆/氧团簇作为异质形核核心对非晶合金形成能力的有害作用。
对Zr_(55)Cu_(30)Ni_5Al_(10)合金进行液态置氢，发现随着氢氩混合气氛中氢含量的增加，钮扣锭中含有的晶体相CuZr_3和AlZr_2的数量逐渐减少，当氢含量达到10%时，钮扣锭中的晶体相会完全消失，结构呈现出完全的非晶态特征。采用楔形试样对比研究了液态置氢前后Zr_(55)Cu_(30)Ni_5Al_(10)合金的玻璃形成能力，发现随着氢氩混合气氛中氢含量的增加，Zr_(55)Cu_(30)Ni_5Al_(10)合金的临界尺寸逐渐增加，当氢含量增加到10%时，其临界尺寸达到最大值。
对液态置氢后的Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金的脆性参数和临界冷却速度的研究表明，置氢的Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金相对于其未置氢时具有更小的脆性参数和临界冷却速度。此外，还对比了置氢前后Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金的吉布斯自由能差的变化，发现置氢后Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金具有更低的吉布斯自由能差，从动力学与热力学的角度解释了液态置氢后Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金具有更大玻璃形成能力的原因。
根据正电子湮没寿命(PALS)研究结果，并结合硬球无规密堆模型中的Bernal孔洞结构，研究了液态置氢后Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金的结构变化。研究表明Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金中存在三种湮没寿命成分，说明合金中存在三种不同尺寸的结构缺陷，对应的非晶结构分别为密堆垛结构中的间隙位置、流动缺陷位置与亚纳米孔洞。密堆垛结构中间隙缺陷浓度的增加，说明置氢后扩大了非晶合金中有效的堆垛区域，从而形成更加有效的致密堆垛，从结构的角度解释了Zr_(55)Cu_(30)Ni_5Al_(10)合金的玻璃形成能力提高的原因。
研究了液态置氢后Zr_(55)Cu_(30)Ni_5Al_(10)与Zr_(57)Al_(10)Cu_(15.4)Ni_(12.6)Nb_5两种块体非晶合金的室温力学性能，发现室温压缩塑性不但没有降低，反而有很大程度的提高。氢致塑性的增加归因于氢在非晶合金中形成了一些应力集中区，这些区域导致了剪切带的增殖与稳定化，从而起到弱化高度局域化的剪切变形，使非晶合金具有更大的塑性应变。
Bulk metallic glasses (BMGs) have a series of superior mechanical properties,e.g., high yield strengths, large elastic strain limits, good corrosion resistance, andgood soft magnetism and hard magnetism, which is a popular research for currentmaterial world. In this dissertation, hydrogen is added to Zr-based bulk metallicglasses (BMGs) by melt hydrogenation. Melt hydrogenation is a new hydrogenationmethod. In this method, the alloys are melted in the gaseous mixture of hydrogenand argon, and the hydrogen diffuses into alloy melt. The effects of melthydrogenation on the melt purification, glass-forming ability (GFA), mechanicalproperties and mechanisms are studied.
The removal effect of melt hydrogenation on the impurities of oxygen inZr_(55)Cu_(30)Ni_5Al_(10)alloy is studied first, and it is found that this method has significantdeoxidation effect in the process of melt hydrogenation. When the hydrogenpercentage in gaseous mixture and melting time are increased, oxygen content ofthe alloys gradually decreases. A hydrogen percentage of15%and melting durationof400s are effective in deoxidizing of these alloys and gaining the completelyamorphous alloy structure. Based on the change of Gibbs free energy, the Gibbsfree energy of reaction hydrogen with oxygen is lower than oxygen with zirconium.Therefore, hydrogen and oxygen is more prone to react. It will avoid the formationof zirconium oxide or zirconium/oxygen clusters which can deteriorate the GFA ofBMGs due to heterogeneous nucleation.
The melt hydrogenation is applied to Zr_(55)Cu_(30)Ni_5Al_(10)master alloys, and it isfound that the volume fraction of crystalline phases CuZr3and AlZr_2graduallydecreases with the increase of hydrogen percentage in the gaseous mixture ofhydrogen and argon, and the crystalline phases completely disappear when thehydrogen percentage increases up to10%, indicating the structure of the sample ismostly amorphous. The GFA of Zr_(55)Cu_(30)Ni_5Al_(10)alloys before and after melthydrogenation is comparatively investigated using wedge shaped samples. Criticalsection size of Zr_(55)Cu_(30)Ni_5Al_(10)alloys gradually increases with the increase ofhydrogen percentage in the gaseous mixture of hydrogen and argon. When thehydrogen percentage increased up to10%, critical section size reaches maximumvalue.
After melt hydrogenation, the fragility parameter and critical cooling rate arestudied. In contrast to non-hydrogenated Zr_(55)Cu_(30)Ni_5Al_(10)alloy, hydrogenated alloypossesses smaller fragility parameter and critical cooling rate. In addition, the change of Gibbs free energy difference of Zr_(55)Cu_(30)Ni_5Al_(10)alloy before and aftermelt hydrogenation is compared. It is found that the Gibbs free energy difference ofhydrogenated Zr_(55)Cu_(30)Ni_5Al_(10)alloy is samller than that of non-hydrogenatedZr_(55)Cu_(30)Ni_5Al_(10)alloy. They explain that hydrogenated Zr_(55)Cu_(30)Ni_5Al_(10)alloy has ahigh GFA from thermodynamics and dynamics.
The structural change of Zr_(55)Cu_(30)Ni_5Al_(10)alloys after melt hydrogenation isinvestigated based on positron annihilation life time spectroscopy (PALS) analysisand Bernal holes in dense random packing of hard spheres model. Three lifetimecomponents are identified, indicating the presence of three distinct size ranges foropen volume defects in the glass. The components are assigned to annihilation inthe interstitial holes in the densely packed, flow defects and sub-nanometer voids.The increase of the concentration of interstitial holes in the densely packed showthat the efficiently packed regions are increased after melt hydrogenation, lead to adenser random packed structure, which explains the increase of GFA in terms ofstructural points of view.
Room temperature mechanical properties of Zr_(55)Cu_(30)Ni_5Al_(10)andZr_(57)Al_(10)Cu_(15.4)Ni_(12.6)Nb_5are studied, and it is found that room temperaturecompression plasticity does not decrease, but it is greatly improved. Hydrogen-enhance plasticity is attributed to the formation of stress concentration induced byhydrogen which promotes proliferation and stability of shear band. Thus it canweaken the highly localized shear deformation, leading to larger plastic strain ofamorphous alloy.
首先研究了液态置氢对去除Zr_(55)Cu_(30)Ni_5Al_(10)合金中杂质元素氧的作用，发现液态置氢对非晶合金具有明显的脱氧作用。随着氢氩混合气氛中氢含量和熔炼时间的增加，合金中的氧含量逐渐降低。当氢氩混合气氛中氢含量为15%，熔炼时间为400s时，具有最佳的脱氧作用，随后凝固得到的合金呈完全的非晶态结构。根据吉布斯自由能的变化情况，可知在高温区时，氢与氧反应的吉布斯自由能较锆与氧反应的吉布斯自由能更低，因此氢与氧更容易发生反应，从而避免了锆与氧反应形成的氧化锆或者锆/氧团簇作为异质形核核心对非晶合金形成能力的有害作用。
对Zr_(55)Cu_(30)Ni_5Al_(10)合金进行液态置氢，发现随着氢氩混合气氛中氢含量的增加，钮扣锭中含有的晶体相CuZr_3和AlZr_2的数量逐渐减少，当氢含量达到10%时，钮扣锭中的晶体相会完全消失，结构呈现出完全的非晶态特征。采用楔形试样对比研究了液态置氢前后Zr_(55)Cu_(30)Ni_5Al_(10)合金的玻璃形成能力，发现随着氢氩混合气氛中氢含量的增加，Zr_(55)Cu_(30)Ni_5Al_(10)合金的临界尺寸逐渐增加，当氢含量增加到10%时，其临界尺寸达到最大值。
对液态置氢后的Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金的脆性参数和临界冷却速度的研究表明，置氢的Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金相对于其未置氢时具有更小的脆性参数和临界冷却速度。此外，还对比了置氢前后Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金的吉布斯自由能差的变化，发现置氢后Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金具有更低的吉布斯自由能差，从动力学与热力学的角度解释了液态置氢后Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金具有更大玻璃形成能力的原因。
根据正电子湮没寿命(PALS)研究结果，并结合硬球无规密堆模型中的Bernal孔洞结构，研究了液态置氢后Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金的结构变化。研究表明Zr_(55)Cu_(30)Ni_5Al_(10)非晶合金中存在三种湮没寿命成分，说明合金中存在三种不同尺寸的结构缺陷，对应的非晶结构分别为密堆垛结构中的间隙位置、流动缺陷位置与亚纳米孔洞。密堆垛结构中间隙缺陷浓度的增加，说明置氢后扩大了非晶合金中有效的堆垛区域，从而形成更加有效的致密堆垛，从结构的角度解释了Zr_(55)Cu_(30)Ni_5Al_(10)合金的玻璃形成能力提高的原因。
研究了液态置氢后Zr_(55)Cu_(30)Ni_5Al_(10)与Zr_(57)Al_(10)Cu_(15.4)Ni_(12.6)Nb_5两种块体非晶合金的室温力学性能，发现室温压缩塑性不但没有降低，反而有很大程度的提高。氢致塑性的增加归因于氢在非晶合金中形成了一些应力集中区，这些区域导致了剪切带的增殖与稳定化，从而起到弱化高度局域化的剪切变形，使非晶合金具有更大的塑性应变。
Bulk metallic glasses (BMGs) have a series of superior mechanical properties,e.g., high yield strengths, large elastic strain limits, good corrosion resistance, andgood soft magnetism and hard magnetism, which is a popular research for currentmaterial world. In this dissertation, hydrogen is added to Zr-based bulk metallicglasses (BMGs) by melt hydrogenation. Melt hydrogenation is a new hydrogenationmethod. In this method, the alloys are melted in the gaseous mixture of hydrogenand argon, and the hydrogen diffuses into alloy melt. The effects of melthydrogenation on the melt purification, glass-forming ability (GFA), mechanicalproperties and mechanisms are studied.
The removal effect of melt hydrogenation on the impurities of oxygen inZr_(55)Cu_(30)Ni_5Al_(10)alloy is studied first, and it is found that this method has significantdeoxidation effect in the process of melt hydrogenation. When the hydrogenpercentage in gaseous mixture and melting time are increased, oxygen content ofthe alloys gradually decreases. A hydrogen percentage of15%and melting durationof400s are effective in deoxidizing of these alloys and gaining the completelyamorphous alloy structure. Based on the change of Gibbs free energy, the Gibbsfree energy of reaction hydrogen with oxygen is lower than oxygen with zirconium.Therefore, hydrogen and oxygen is more prone to react. It will avoid the formationof zirconium oxide or zirconium/oxygen clusters which can deteriorate the GFA ofBMGs due to heterogeneous nucleation.
The melt hydrogenation is applied to Zr_(55)Cu_(30)Ni_5Al_(10)master alloys, and it isfound that the volume fraction of crystalline phases CuZr3and AlZr_2graduallydecreases with the increase of hydrogen percentage in the gaseous mixture ofhydrogen and argon, and the crystalline phases completely disappear when thehydrogen percentage increases up to10%, indicating the structure of the sample ismostly amorphous. The GFA of Zr_(55)Cu_(30)Ni_5Al_(10)alloys before and after melthydrogenation is comparatively investigated using wedge shaped samples. Criticalsection size of Zr_(55)Cu_(30)Ni_5Al_(10)alloys gradually increases with the increase ofhydrogen percentage in the gaseous mixture of hydrogen and argon. When thehydrogen percentage increased up to10%, critical section size reaches maximumvalue.
After melt hydrogenation, the fragility parameter and critical cooling rate arestudied. In contrast to non-hydrogenated Zr_(55)Cu_(30)Ni_5Al_(10)alloy, hydrogenated alloypossesses smaller fragility parameter and critical cooling rate. In addition, the change of Gibbs free energy difference of Zr_(55)Cu_(30)Ni_5Al_(10)alloy before and aftermelt hydrogenation is compared. It is found that the Gibbs free energy difference ofhydrogenated Zr_(55)Cu_(30)Ni_5Al_(10)alloy is samller than that of non-hydrogenatedZr_(55)Cu_(30)Ni_5Al_(10)alloy. They explain that hydrogenated Zr_(55)Cu_(30)Ni_5Al_(10)alloy has ahigh GFA from thermodynamics and dynamics.
The structural change of Zr_(55)Cu_(30)Ni_5Al_(10)alloys after melt hydrogenation isinvestigated based on positron annihilation life time spectroscopy (PALS) analysisand Bernal holes in dense random packing of hard spheres model. Three lifetimecomponents are identified, indicating the presence of three distinct size ranges foropen volume defects in the glass. The components are assigned to annihilation inthe interstitial holes in the densely packed, flow defects and sub-nanometer voids.The increase of the concentration of interstitial holes in the densely packed showthat the efficiently packed regions are increased after melt hydrogenation, lead to adenser random packed structure, which explains the increase of GFA in terms ofstructural points of view.
Room temperature mechanical properties of Zr_(55)Cu_(30)Ni_5Al_(10)andZr_(57)Al_(10)Cu_(15.4)Ni_(12.6)Nb_5are studied, and it is found that room temperaturecompression plasticity does not decrease, but it is greatly improved. Hydrogen-enhance plasticity is attributed to the formation of stress concentration induced byhydrogen which promotes proliferation and stability of shear band. Thus it canweaken the highly localized shear deformation, leading to larger plastic strain ofamorphous alloy.
引文
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