纳米镍—铁合金和纳米铜的力学行为及变形机制研究
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摘要
本文利用自制的一套具有循环过滤、搅拌、温控及阴极移动装置的电沉积设备成功制备出了高质量的纳米镍-铁合金材料。经过工艺参数和成分的优化,提出了可连续施镀,并有很高的镀厚能力及晶粒尺寸、晶粒结构和合金成分可控的电沉积工艺配方及工艺方法。制备的合金成分均匀、表面光亮、结晶细致。对电沉积过程中阴极表面液层中Fe2+离子浓度、H+离子浓度及pH值进行了测试。可知,在电沉积过程中Fe2+离子起着决定性的作用,由于阴极析氢导致H+浓度下降pH值上升,Fe2+首先生成氢氧化物沉积,并附着于阴极表面上,抑制了Ni2+离子到达阴极上放电还原,结果使Ni2+沉积速度减慢,而Fe2+优先沉积,通过这种异常共沉积获得了纳米镍铁合金。
研究了阴极电流密度对纳米镍铁合金(成分为Ni-20wt%Fe)的结构、微观组织及室温拉伸力学性能的影响。研究显示,电沉积制备的纳米镍铁合金材料是具有面心立方结构的γ相固溶体。随着电流密度的增大晶粒尺寸减小,强度和塑性应变都有增大的趋势。电流密度为7A/dm2时获得的纳米镍铁合金的平均晶粒尺寸为22nm左右,极限抗拉强度最大为1922Mpa,断裂应变最大为10.8%。电流密度为3A/dm2时获得的纳米镍铁合金平均晶粒尺寸为33nm左右,极限抗拉强度最大为1792Mpa,断裂应变最大为8.5%。通过断口形貌观察,不同电流密度下获得的纳米镍铁合金均表现出韧性断裂的断口特征,断口韧窝较深,尺寸大约为400~600nm。在断口侧面最大应变处可明显观察到颈缩现象和剪切带的存在。
对纳米镍铁合金(成分为Ni-20wt%Fe)和平均晶粒尺寸相近纳米镍进行了拉伸力学性能和断裂行为的比较研究。结果显示,随着应变速率的增加,纳米镍铁合金的抗拉强度和断裂应变均有增加,但是纳米镍的抗拉强度增加,断裂应变却有较大的降低。在试验的应变速率(1×10-5s-1-1s-1)范围内增大时,纳米镍铁合金极限抗拉强度从1762MPa增加到1939MPa,断裂应变从8.5%增加到9.3%,而纳米镍极限抗拉强度从1605MPa增加到1912MPa,其断裂应变从10.7%下降到5.8%。且塑性应变为2.0%时,纳米镍铁合金m=0.010,纳米镍m=0.024,纳米镍铁合金表现出较小的应变速率敏感性。断裂表面的对比分析显示,纳米镍铁合金和纳米镍均呈现明显的韧性断裂特征,在颈缩区域的表面可观察到大量几十至几百纳米的剪切带。纳米镍铁表现出裂纹钝化倾向,但纳米镍裂纹钝化倾向不明显。纳米镍铁和纳米镍表现出不同的塑性随应变速率不同的变化源于这种断裂发展过程的差异。固溶铁原子的加入造成了纳米镍铁合金层错能的变化引起的位错活动改变是导致两种材料塑性变化的主要因素。在高应变速率下是位错活动协调变形,而在低应变速率下位错活动和晶界变形共同协调变形。而应变速率敏感性不是影响塑性的决定因素。
对脉冲电刷镀制备的纳米铜进行了系统的循环试验和增量卸载试验,研究了复杂变形路径下位错的晶界发射和吸收过程。循环实验表明,在塑性变形期间有一个非常少见的惯性行为,加载过程中的变形结构(位错结构)可在卸载过程中完全恢复。在高应变速率下,纳米铜出现明显的惯性变形,其惯性应变随应变速率的增加而增加。当应变速率很小时,不出现惯性变形。在加载期间储备的高密度位错行为,主要归因于较高的应变速率。这些被储存起来的位错在卸载期间能被充分的吸收,主要归因于较慢的应力卸载速率,并由此导致产生较大的惯性应变。增量卸载实验显示,在高应变速率时,纳米铜的变形结构迅速释放,在极短的时间内可达到同一个水平。纳米铜中在高能量处的位错脱钉是主要的控制机制,在材料内部局部大的应力场会给位错脱钉增加困难,从而出现更多的位错缠结导致纳米金属材料产生强化效应。
Interests of scientists in the world on the nanocrystalline materials are focused on im-proving and optimizing their mechanical properties and revealing the strain rate sensitivity and mechanical fracture mechanism of these materials. As the grain size is decreased, an in-creasing fraction of atoms can be ascribed to the grain boundaries. Nanocrystalline materials exhibit various unique chemical, physical or mechanical properties such as increased strength/hardness, reduced elastic modulus and ductility in comparison with conventional polycrystalline materials. For the technical problems of materials preparing, nano-metal with high metallurgical quality, large-size and ideal micro-structure can not be prepared, which limit the understanding to the nature of plastic deformation of nano-metal. On the other hand, studies of experimental work, theoretical and simulation have shown the grain boundary processing and dislocation activities are two important mechanisms for controlling the me-chanical properties of nano-metals. To explore effect of mechanical activation and thermal activation caused by changing grain size, strain rate and other factors to these two mecha-nisms is the substance of the deformation mechanisms of nano-metallic. Therefore, it is es-sential to fabricate high-quality bulk nano-materials and their alloys using a new type of preparation process and undertake extensive studies on their microstructures and mechanical properties.
It was found that the irrationality process equipment, process recipes, process conditions and other factors seriously affected the preparation of nano-metals and alloy microstructure of nano-metals and alloys, which result a lot of difficulties to the study of properties and de-formation mechanisms of nano-mechanical. In this paper, a new electrodeposition technique used to make nanocrystalline materials was developed by changing and optimizing techno-logical conditions and technological parameters based on conventional electrodeposition technique, and the electrodeposited equipment is produced by us. A bull nanocrystalline Ni-Fe alloys and nanocrystalline Cu were prepared by this electrodeposition technique. Mi-crostructure and mechanical performance of these nanocrystalline materials were observed and analyzed by SEM, TEM, XRD and MTS.
Based on the above points, the following research work was conducted in this disserta-tion and the conclusions are presented as the following:
1) High-quality nanocrystalline Ni-Fe alloy was successfully fabricated through devel-oping composition of bath, adjustment technological conditions and technological parame-ters of electrodeposition, using the self-made electrodeposition equipment with cycle of fil-tering, mixing, temperature control and cathodic mobile. And a detailed discussion about the effect of the bath composition, pH, bath temperature, cathode current density, additives con-tent, and add cycle to the surface of micro-morphology, Vickers microhardness and micro-structure of nanocrystalline Ni-Fe alloy was given. The main ingredients were NiSO4.6H2O、FeSO4.7H2O、H3BO3、NaCl、Na3C6H5O7·2H2O、wetting agent、brightener A and brightener B. To corresponding, the optimum conditions were given as the following: Cathode current density is 5-7A/dm2; value of pH is 3.4-3.6; temperature is 60-62℃, cycle of filtration and speed of cathode mobile is 18 times / minute, journey is 120mm. Nanocrystalline Ni-Fe alloys synthesized using the above-mentioned ingredients and process conditions have uni-form composition, dense crystallization, shiny surface, no nodulation and pock marking, the highest microhardness could be more than 600HV. Analyzing the reaction mechanism of electroplating deposition and process of deposition, we can see that electrodeposition of nanocrystalline Ni-Fe alloys belong to an unusual co-deposition theory.
2) The components ,structure and microstructure of this nanocrystalline Ni-Fe alloys can be observed and analyzed by EDS, XRD, SEM,TEM and AFM. It was demonstrated that the percents of Fe is 20.78wt.% in this Ni-Fe alloy ,there is no detectable porosities or voids in this material, the grain sizes of this material are fine, the orientation of the crystal-lography is uniform. To statistic about hundreds of grain size, it can be obtained that the range of gain size is 10-100nm with the average grain size of about 28±5nm. Root-mean-square roughness of nanocrystalline Ni-Fe alloys has no brightener is 5.519nm, an average roughness is 4.417nm. While root-mean-square roughness of the one added brightener is 4.333nm, an average roughness is 3.392nm.
3) The effect of the cathodic current density to the structure, microstructure and room temperature tensile mechanical properties of nanocrystalline Ni-Fe alloys (component is Ni-20wt%Fe) was studied. The results shown that high-quality electrodeposition nanocrys-talline Ni-Fe alloys isγ-phase solid solution with face-centered cubic structure, No other phase exist in the XRD spectra of the samples synthesized under different current density. The grain sizes of nanocrystalline Ni-Fe alloys are fine, the orientation of the crystallography is uniform, there is no detectable porosities or voids in this material. When the current den-sity for the preparation of nanocrystalline Ni-Fe alloys is 7A/dm2, the average grain size is about 22nm, the maximum tensile strength is 1922Mpa, the largest fracture strain is 10.8%. When the current density for the preparation of nanocrystalline Ni-Fe alloys is 3A/dm2, the average grain size is about 33nm, the maximum tensile strength is 1792Mpa, the largest fracture strain is 8.5%. Observing the fracture surface, under different current density it was found that nanocrystalline Ni-Fe alloys showed the fracture characteristics of ductile fracture, at the side of the largest fracture strain, necking phenomenon and shear zones can be clearly observed.
4) Comparing tensile mechanical properties and fracture behavior of nanocrystalline Ni-Fe alloys (Ni-20wt% Fe) and nanocrystalline Ni with the similar average grain size, dur-ing the strain rate increases from 1×10-5s-1 to 1s-1, the result showed that the 0.2 percent yield strength of nanocrystalline Ni-Fe alloys increases from 1134MPa to 1368MPa, the ul-timate tensile strength increases from 1762MPa to 1939MPa, the changing range of breaking strain is 8.5% ~ 9.3% , the changing range of homogeneous strain is 6.3% to 7%, increasing basically with the strain rate increasing, but the fracture strain and the homogeneous strain have little change. At the same range of strain rate (1×10-5s-1~1s-1), with increasing of strain rate, the ultimate tensile strength of nanocrystalline Ni have an increase trend, but the frac-ture strain and the homogeneous strain decrease rapidly. When the plastic strain (εP) is 0.2%, the strain rate sensitivity index (m) of the nanocrystalline Ni-Fe alloys m = 0.017, for nanocrystalline Ni, m = 0.031. When the plastic strain (εP) is 2.0%, the strain rate sensitivity index (m) of the nanocrystalline Ni-Fe alloys m = 0.010, for nanocrystalline Ni, m = 0.024. To the plastic strain of 0.2% and 2.0%, the nanocrystalline Ni-Fe alloys showed smaller ten-sile strain rate sensitivity than the nanocrystalline Ni. Comparing fracture surface morphol-ogy of nanocrystalline Ni-Fe alloys and nanocrystalline Ni, it was found that there are micr-hunches of tens to hundreds of nanometer on the surface of nanocrystalline Ni-Fe al-loys. At the department of maximum strain, it was found a large number of weakening shear zone and the existence of obvious necking. These result showed that the addition of Fe atoms has changed the original crystal structure of Ni, leading to dislocation activity, atomic diffu-sion and grain boundary slipping may be the main mechanism for the facture. which could stabilize the ability of continuous deformation result in relatively good and almost invariable ductility.
5) Systematic cycling and the incremental unloading test was carried out on pulse elec-trical brush-plating nanocrystalline Cu to analysis dislocation emission-absorption process in complexity path. Little inertia strain(Δεip)indicated grain boundary sliding play a major accommodate role on the plastic deformation during loading at the low strain rates. At high strain rates, with the reduction of unloading stress rate, the significant increment of inertial strain (Δεip) confirm existence of thermal activation in the process of dislocations migration. The results showed that high-energy dislocation depinning is the main control mechanism in nc Cu, the strengthening of nc metals arises from the long-range stress field built-up due to the increased difficulty for the disloca-tion depinning in addition to the high internal stress built-up during loading.
研究了阴极电流密度对纳米镍铁合金(成分为Ni-20wt%Fe)的结构、微观组织及室温拉伸力学性能的影响。研究显示,电沉积制备的纳米镍铁合金材料是具有面心立方结构的γ相固溶体。随着电流密度的增大晶粒尺寸减小,强度和塑性应变都有增大的趋势。电流密度为7A/dm2时获得的纳米镍铁合金的平均晶粒尺寸为22nm左右,极限抗拉强度最大为1922Mpa,断裂应变最大为10.8%。电流密度为3A/dm2时获得的纳米镍铁合金平均晶粒尺寸为33nm左右,极限抗拉强度最大为1792Mpa,断裂应变最大为8.5%。通过断口形貌观察,不同电流密度下获得的纳米镍铁合金均表现出韧性断裂的断口特征,断口韧窝较深,尺寸大约为400~600nm。在断口侧面最大应变处可明显观察到颈缩现象和剪切带的存在。
对纳米镍铁合金(成分为Ni-20wt%Fe)和平均晶粒尺寸相近纳米镍进行了拉伸力学性能和断裂行为的比较研究。结果显示,随着应变速率的增加,纳米镍铁合金的抗拉强度和断裂应变均有增加,但是纳米镍的抗拉强度增加,断裂应变却有较大的降低。在试验的应变速率(1×10-5s-1-1s-1)范围内增大时,纳米镍铁合金极限抗拉强度从1762MPa增加到1939MPa,断裂应变从8.5%增加到9.3%,而纳米镍极限抗拉强度从1605MPa增加到1912MPa,其断裂应变从10.7%下降到5.8%。且塑性应变为2.0%时,纳米镍铁合金m=0.010,纳米镍m=0.024,纳米镍铁合金表现出较小的应变速率敏感性。断裂表面的对比分析显示,纳米镍铁合金和纳米镍均呈现明显的韧性断裂特征,在颈缩区域的表面可观察到大量几十至几百纳米的剪切带。纳米镍铁表现出裂纹钝化倾向,但纳米镍裂纹钝化倾向不明显。纳米镍铁和纳米镍表现出不同的塑性随应变速率不同的变化源于这种断裂发展过程的差异。固溶铁原子的加入造成了纳米镍铁合金层错能的变化引起的位错活动改变是导致两种材料塑性变化的主要因素。在高应变速率下是位错活动协调变形,而在低应变速率下位错活动和晶界变形共同协调变形。而应变速率敏感性不是影响塑性的决定因素。
对脉冲电刷镀制备的纳米铜进行了系统的循环试验和增量卸载试验,研究了复杂变形路径下位错的晶界发射和吸收过程。循环实验表明,在塑性变形期间有一个非常少见的惯性行为,加载过程中的变形结构(位错结构)可在卸载过程中完全恢复。在高应变速率下,纳米铜出现明显的惯性变形,其惯性应变随应变速率的增加而增加。当应变速率很小时,不出现惯性变形。在加载期间储备的高密度位错行为,主要归因于较高的应变速率。这些被储存起来的位错在卸载期间能被充分的吸收,主要归因于较慢的应力卸载速率,并由此导致产生较大的惯性应变。增量卸载实验显示,在高应变速率时,纳米铜的变形结构迅速释放,在极短的时间内可达到同一个水平。纳米铜中在高能量处的位错脱钉是主要的控制机制,在材料内部局部大的应力场会给位错脱钉增加困难,从而出现更多的位错缠结导致纳米金属材料产生强化效应。
Interests of scientists in the world on the nanocrystalline materials are focused on im-proving and optimizing their mechanical properties and revealing the strain rate sensitivity and mechanical fracture mechanism of these materials. As the grain size is decreased, an in-creasing fraction of atoms can be ascribed to the grain boundaries. Nanocrystalline materials exhibit various unique chemical, physical or mechanical properties such as increased strength/hardness, reduced elastic modulus and ductility in comparison with conventional polycrystalline materials. For the technical problems of materials preparing, nano-metal with high metallurgical quality, large-size and ideal micro-structure can not be prepared, which limit the understanding to the nature of plastic deformation of nano-metal. On the other hand, studies of experimental work, theoretical and simulation have shown the grain boundary processing and dislocation activities are two important mechanisms for controlling the me-chanical properties of nano-metals. To explore effect of mechanical activation and thermal activation caused by changing grain size, strain rate and other factors to these two mecha-nisms is the substance of the deformation mechanisms of nano-metallic. Therefore, it is es-sential to fabricate high-quality bulk nano-materials and their alloys using a new type of preparation process and undertake extensive studies on their microstructures and mechanical properties.
It was found that the irrationality process equipment, process recipes, process conditions and other factors seriously affected the preparation of nano-metals and alloy microstructure of nano-metals and alloys, which result a lot of difficulties to the study of properties and de-formation mechanisms of nano-mechanical. In this paper, a new electrodeposition technique used to make nanocrystalline materials was developed by changing and optimizing techno-logical conditions and technological parameters based on conventional electrodeposition technique, and the electrodeposited equipment is produced by us. A bull nanocrystalline Ni-Fe alloys and nanocrystalline Cu were prepared by this electrodeposition technique. Mi-crostructure and mechanical performance of these nanocrystalline materials were observed and analyzed by SEM, TEM, XRD and MTS.
Based on the above points, the following research work was conducted in this disserta-tion and the conclusions are presented as the following:
1) High-quality nanocrystalline Ni-Fe alloy was successfully fabricated through devel-oping composition of bath, adjustment technological conditions and technological parame-ters of electrodeposition, using the self-made electrodeposition equipment with cycle of fil-tering, mixing, temperature control and cathodic mobile. And a detailed discussion about the effect of the bath composition, pH, bath temperature, cathode current density, additives con-tent, and add cycle to the surface of micro-morphology, Vickers microhardness and micro-structure of nanocrystalline Ni-Fe alloy was given. The main ingredients were NiSO4.6H2O、FeSO4.7H2O、H3BO3、NaCl、Na3C6H5O7·2H2O、wetting agent、brightener A and brightener B. To corresponding, the optimum conditions were given as the following: Cathode current density is 5-7A/dm2; value of pH is 3.4-3.6; temperature is 60-62℃, cycle of filtration and speed of cathode mobile is 18 times / minute, journey is 120mm. Nanocrystalline Ni-Fe alloys synthesized using the above-mentioned ingredients and process conditions have uni-form composition, dense crystallization, shiny surface, no nodulation and pock marking, the highest microhardness could be more than 600HV. Analyzing the reaction mechanism of electroplating deposition and process of deposition, we can see that electrodeposition of nanocrystalline Ni-Fe alloys belong to an unusual co-deposition theory.
2) The components ,structure and microstructure of this nanocrystalline Ni-Fe alloys can be observed and analyzed by EDS, XRD, SEM,TEM and AFM. It was demonstrated that the percents of Fe is 20.78wt.% in this Ni-Fe alloy ,there is no detectable porosities or voids in this material, the grain sizes of this material are fine, the orientation of the crystal-lography is uniform. To statistic about hundreds of grain size, it can be obtained that the range of gain size is 10-100nm with the average grain size of about 28±5nm. Root-mean-square roughness of nanocrystalline Ni-Fe alloys has no brightener is 5.519nm, an average roughness is 4.417nm. While root-mean-square roughness of the one added brightener is 4.333nm, an average roughness is 3.392nm.
3) The effect of the cathodic current density to the structure, microstructure and room temperature tensile mechanical properties of nanocrystalline Ni-Fe alloys (component is Ni-20wt%Fe) was studied. The results shown that high-quality electrodeposition nanocrys-talline Ni-Fe alloys isγ-phase solid solution with face-centered cubic structure, No other phase exist in the XRD spectra of the samples synthesized under different current density. The grain sizes of nanocrystalline Ni-Fe alloys are fine, the orientation of the crystallography is uniform, there is no detectable porosities or voids in this material. When the current den-sity for the preparation of nanocrystalline Ni-Fe alloys is 7A/dm2, the average grain size is about 22nm, the maximum tensile strength is 1922Mpa, the largest fracture strain is 10.8%. When the current density for the preparation of nanocrystalline Ni-Fe alloys is 3A/dm2, the average grain size is about 33nm, the maximum tensile strength is 1792Mpa, the largest fracture strain is 8.5%. Observing the fracture surface, under different current density it was found that nanocrystalline Ni-Fe alloys showed the fracture characteristics of ductile fracture, at the side of the largest fracture strain, necking phenomenon and shear zones can be clearly observed.
4) Comparing tensile mechanical properties and fracture behavior of nanocrystalline Ni-Fe alloys (Ni-20wt% Fe) and nanocrystalline Ni with the similar average grain size, dur-ing the strain rate increases from 1×10-5s-1 to 1s-1, the result showed that the 0.2 percent yield strength of nanocrystalline Ni-Fe alloys increases from 1134MPa to 1368MPa, the ul-timate tensile strength increases from 1762MPa to 1939MPa, the changing range of breaking strain is 8.5% ~ 9.3% , the changing range of homogeneous strain is 6.3% to 7%, increasing basically with the strain rate increasing, but the fracture strain and the homogeneous strain have little change. At the same range of strain rate (1×10-5s-1~1s-1), with increasing of strain rate, the ultimate tensile strength of nanocrystalline Ni have an increase trend, but the frac-ture strain and the homogeneous strain decrease rapidly. When the plastic strain (εP) is 0.2%, the strain rate sensitivity index (m) of the nanocrystalline Ni-Fe alloys m = 0.017, for nanocrystalline Ni, m = 0.031. When the plastic strain (εP) is 2.0%, the strain rate sensitivity index (m) of the nanocrystalline Ni-Fe alloys m = 0.010, for nanocrystalline Ni, m = 0.024. To the plastic strain of 0.2% and 2.0%, the nanocrystalline Ni-Fe alloys showed smaller ten-sile strain rate sensitivity than the nanocrystalline Ni. Comparing fracture surface morphol-ogy of nanocrystalline Ni-Fe alloys and nanocrystalline Ni, it was found that there are micr-hunches of tens to hundreds of nanometer on the surface of nanocrystalline Ni-Fe al-loys. At the department of maximum strain, it was found a large number of weakening shear zone and the existence of obvious necking. These result showed that the addition of Fe atoms has changed the original crystal structure of Ni, leading to dislocation activity, atomic diffu-sion and grain boundary slipping may be the main mechanism for the facture. which could stabilize the ability of continuous deformation result in relatively good and almost invariable ductility.
5) Systematic cycling and the incremental unloading test was carried out on pulse elec-trical brush-plating nanocrystalline Cu to analysis dislocation emission-absorption process in complexity path. Little inertia strain(Δεip)indicated grain boundary sliding play a major accommodate role on the plastic deformation during loading at the low strain rates. At high strain rates, with the reduction of unloading stress rate, the significant increment of inertial strain (Δεip) confirm existence of thermal activation in the process of dislocations migration. The results showed that high-energy dislocation depinning is the main control mechanism in nc Cu, the strengthening of nc metals arises from the long-range stress field built-up due to the increased difficulty for the disloca-tion depinning in addition to the high internal stress built-up during loading.
引文
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