IMR OpenIR
纳米孪晶材料加工硬化行为及电学性能的研究
其他题名An investigation on work hardening behavior and electrical properties of nano-twinned materials
陈先华
学位类型博士
导师卢柯
2007-12-25
学位授予单位中国科学院金属研究所
学位授予地点金属研究所
学位专业材料学
关键词脉冲电解沉积 Cu 纳米尺度孪晶 孪晶界/晶界 加工硬化 变形机理 尺寸效应 电阻率 316l不锈钢 强化效应
摘要力学性能和电学性能是工业材料两项至关重要的指标。大量实验与模拟结果表明相对于传统粗晶材料,尽管纳米晶体材料强度高,但塑性差,加工硬化能力小,导电性也差。这在很大程度上限制了其工程应用。作为特殊的低能界面,孪晶界对位错运动有着很强的阻碍作用,但孪晶界与位错之间的相互作用有别于传统大角晶界,且孪晶界对自由电子的散射作用很弱。目前关于高密度生长孪晶界对材料力学和电学性能的影响及其内在机制缺乏统一的认识和深入的理解。所以,深入系统地研究含有纳米尺度生长孪晶晶体材料的加工硬化行为及导电机理具有重要意义。 本研究工作针对上述问题,运用脉冲电解沉积技术和表面机械研磨处理制备了具有纳米尺度生长孪晶的纯Cu样品和纳米晶体316L奥氏体不锈钢(316L SS)样品,系统研究了其加工硬化与电学性能。主要研究结果包括: 1.利用脉冲电解沉积工艺,实现材料结构可控生长,制备出两类纳米孪晶Cu样品:(I)平均晶粒尺寸为400-500 nm,晶粒内孪晶片层平均宽度在15-90 nm范围变化;(II)保证孪晶片层宽度相当(~60 nm),而平均晶粒尺寸不同(460 nm和1500 nm)。 2.透射电镜观察表明Cu样品的晶界形态、能量与孪晶密度相关。高密度孪晶Cu样品的晶界平直,界面能较低;而晶内孪晶密度较低时,晶界相当弯曲,晶体学厚度大,具有高的界面能量。在纳米孪晶Cu中,绝大部分孪晶界为{111}/{111}共格孪晶界,但同时存在少量{211}/{211}及{11 44}/{223}非共格孪晶界。两种非共格孪晶界结构的一个显著特征是{111}面条纹连续通过界面。 3.分别利用单向连续拉伸、加载-卸载和室温轧制等一系列实验研究了在保持晶粒尺寸恒定时(400-500 nm),孪晶密度对纳米孪晶Cu加工硬化行为的影响。结果表明孪晶片层宽度减小(从90 nm到20 nm),材料的流变应力增加值和加工硬化率显著提高,这主要是由于塑性变形过程中高密度孪晶界有效地阻碍位错滑移。然而,纳米孪晶Cu的加工硬化指数随孪晶密度的提高仅从0.22增加到0.30,与晶粒尺寸相同但无孪晶的超细晶Cu相当,但明显高于纳米晶体材料的加工硬化指数。这说明引入高密度生长孪晶界可有效改善其加工硬化能力,但当孪晶片层宽度从90 nm减小到20 nm,亚微米晶粒中所存储的不可动位错密度却无大幅度增加,其原因可能是:(I)孪晶界的二维结构特性限制了位错锁结构在孪晶界上形成;(II)多滑移系之间的位错交互作用难以发生;(III)位错反应生成的Shockley不全位错可在孪晶界上滑移,贡献塑性变形,但对后续位错运动的阻碍作用有限。 4.通过对比孪晶片层宽度相当(~60 nm),而晶粒尺寸分别为450 nm和1500 nm的两种纳米孪晶Cu样品的力学性能,发现屈服强度与晶粒尺寸并无明显关系,而主要取决于孪晶片层厚度。但是晶粒尺寸增大, 样品的延伸率和加工硬化能力明显提高。平均晶粒尺寸为1500 nm时,纳米孪晶 Cu样品延伸率与加工硬化指数分别提高至15%和0.39,远高于晶粒尺寸为460 nm的Cu样品(3.5%和0.21),这是由于大晶粒尺寸增加了位错沿孪晶界方向的剪切通道长度和降低了动态回复。当非均匀塑性变形发生时,孪晶界消失和位错胞亚结构形成主导了大晶粒尺寸纳米孪晶Cu的动态回复过程,导致加工硬化率明显下降。塑性变形量和晶粒尺寸是决定纳米孪晶Cu中位错胞亚结构形成的两个重要因素。 5.通过电阻试验研究了相同晶粒尺寸的电解沉积亚微米晶Cu中孪晶密度对电阻的影响规律。孪晶片层宽度为15 nm时,Cu样品保持高强度的同时,也具有很好的导电性,室温电阻率为1.75 μΩ cm(即导电率相当于97%IACS),略高于粗晶Cu的值(1.69 μΩ cm)。电阻率随孪晶密度减小而增加,当孪晶片层宽度增加至90 nm时,Cu样品的室温电阻率提高到2.12 μΩ cm。纳米孪晶Cu的电阻率明显低于文献中报道的纳米晶体Cu。沉积态Cu样品相对于粗晶Cu增加的电阻率主要是源于晶界对电子的散射,而孪晶形成有效降低了晶界能量和晶界缺陷密度,导致样品的电阻率随孪晶密度增加而减小。室温轧制40%后,具有高密度孪晶的Cu样品室温电阻率显著增加,且孪晶密度越高,电阻率增加值越大。这是由于大量位错驻留在孪晶界和晶界附近而大幅度提高了两者的电阻率。纳米孪晶Cu样品实现了材料的高强度与高导电性结合。 6.采用表面机械研磨处理工艺制备了平均晶粒尺寸为40 nm的纳米晶体316L SS样品。室温单向拉伸实验表明纳米晶体316L SS的屈服强度高达1450 MPa(为粗晶材料的6倍),符合传统的Hall-Petch关系,强化源于高密度晶界对位错运动有效的阻碍。
其他摘要Mechanical and electrical properties are two of the most important criteria for industrial materials. Amounts of experiments and computer simulations indicated that nanocrystalline (nc) metals with a high density of grain boundaries (GBs) usually exhibit substantial high strength, very limited plastic strain, diminishing work hardening capacity and reduced conductivity, compared with their conventional coarse-grained (CG) counterparts. The above mentioned properties of nc metallic materials had been severely blocked their industrial applications. Twin boundaries (TBs), special type of low-energy boundaries, can serve as barriers to dislocation motions like conventional GBs. While the interaction between TBs and dislocations is basically different from that between GBs and dislocations. Meanwhile, the coherent TBs possess a very low capacity to scatter conduction electrons. Nevertheless, up to now, a clear scenery of the influence of high density of coherent TBs on mechanical and electrical properties of nc materials is still lacking. Therefore, understanding of intrinsic mechanisms for hardening and conducting of nanoscale coherent twin structures becomes more and more crucial. In this work, high-purity Cu specimens with nanoscale growth twins and nc 316L stainless steel (316L SS) samples were synthesized by means of pulsed electrodeposition (PED) technique and surface mechanical attrition treatment (SMAT), respectively. We systematically investigated the mechanical and electrical properties of these samples. The main results of this work are as follows: 1. Optimizing the microstructures by modifying deposition parameters, two kinds of ultrafine-grained (ufg) Cu samples with nanoscale twins were prepared by means of PED technique: (I) keeping average grain size constant (400~500 nm), while changing twin lamellar spacing from 15 to 90 nm; (II) keeping twin lamellar spacing constant (~60 nm), while changing grain size from 460 nm to 1500 nm. 2. Transmission electron microscope (TEM) observations revealed that GB morphology and energy are related to twin density in nano-twinned Cu (nt-Cu) samples. For the nt-Cu with high twin density, the faceted GBs with low interfacial energy are straight and clear. Whereas the GBs of the nt-Cu with relatively low twin density are quite curved and show large crystallographic width. There are a few {211}/{211} and {11 44}/{223} incoherent TBs in electrodeposited Cu samples, besides a high density of {111}/{111} coherent TBs. A striking feature of these structures is a bending of the {111} planes that run continuously through the incoherent boundaries. 3. Keeping the grain size of Cu specimens roughly constant (400-500 nm), the influence of twin lamellar spacing on work hardening response of nt-Cu was investigated by recourse to uniaxial continuous tensile, loading-unloading and cold rolling tests at room temperature (RT). Net flow stress increment and work hardening rate of the nt-Cu are enhanced substantially with decreasing twin lamellar spacing (from 90 nm to 20 nm), which may be due to that TB can be effective obstacles for the motion of dislocations. Whereas, the work hardening exponent increases slightly (from 0.22 to 0.30) with increasing twin density in nt-Cu, which is comparable to that of the ufg Cu with identical grain size but without twins and much higher than those of nc Cu samples. This suggests that the introduction of high density of TBs is beneficial to elevate the work hardening capacity of nt-Cu. However, the ability to store immobile dislocations can not be promoted evidently in the submicron grains when the twin lamellar spacing reduces from 90 nm to 20 nm. The possible factors as follows: (I) The twin lamellar structure is two-dimension, which limits dislocation interactions in three dimensions and consequently results in the absence of dislocation locks in the lattice and TBs. (II) Dislocation interactions from multi-slip systems can not occur extensively. (III) Reactant Shockley partials, being left at the TBs and leading to TB migration, do not contribute to work hardening significantly. 4. Comparing mechanical properties of two nt-Cu samples with similar twin spacing of ~60 nm but with different grain sizes (450 nm and 1500 nm, respectively), it is observed that the yield strength is independent on grain size, that indicated the high yield strength of nt-Cu originates from the strengthening of high density of TBs. However, both the ductility and the work hardening capacity show an increasing trend with increasing grain size in the nt-Cu. For the nt-Cu sample with a grain size of 1500 nm, the elongation to failure and work hardening exponent are as high as 15% and 0.39, both of which are much higher than those of nt-Cu with a grain size of 460 nm. The elevated ductility and work hardening ability may come from increasing the grain size so that there are a longer shear path of abundant dislocations along the TBs and suppressed dynamic recovery. When nonuniform plastic deformation occurs, the disappearance of TBs and the formation of dislocation cells dominate the dynamic recovery and consequently give rise to the diminishing of work hardening rate in the nt-Cu with a grain size of 1500 nm. A strong dependence of structural evolution on the grain size and strain was investigated systematically by TEM observations in nt-Cu. 5. The effect of twin density on electrical resistivities of nt-Cu samples is systematically investigated through holding grain size roughly identical. The electrical resistivity of the Cu specimen with a twin spacing of 15 nm at RT is 1.75 μΩ cm (the conductivity is about 97% IACS), which is comparable to that of CG pure Cu specimen. A reduction in twin density (with twin lamellar spacings of 35 nm and 90 nm, respectively) results in an increment in electrical resistivity from 1.75 to 2.12 μΩ cm. The increased electrical resistivities of the Cu samples were ascribed dominantly to the intrinsic GB scattering, while the GB defects and GB energy would decrease with increasing twin density. Plastic deformation would induce an apparent increase in the resistivity. The higher twin density, the higher increment of RT resistivity was detected in the Cu specimens subjected to 40% rolling strain. Both the deviated TBs and strained GBs may give rise to an increase in the resistivity. High strength and good conductivity are achieved simultaneously in the nt-Cu. 6. A nc 316L austenitic stainless steel sample with a mean grain size of 40 nm was prepared by means of SMAT. Uniaxial tensile tests at RT showed that nc 316L SS sample exhibits a yield strength as high as 1450 MPa, which is about six times higher than that of CG sample. This ultrahigh strength of the nc sample, which still follows the Hall-Petch relation extrapolated from CG structures, is attributed to the effective blockage of lattice dislocation motions by nanometer-sized grains.
页数137
语种中文
文献类型学位论文
条目标识符http://ir.imr.ac.cn/handle/321006/16932
专题中国科学院金属研究所
推荐引用方式
GB/T 7714
陈先华. 纳米孪晶材料加工硬化行为及电学性能的研究[D]. 金属研究所. 中国科学院金属研究所,2007.
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