The influence of residual stress and crystallite size on the magnetic properties of electrodeposited nanocrystalline Pd-Co alloys

Nanocrystalline Pd-Co alloys were obtained by electrodeposition from an ammoniacal chloride bath. The influence of the crystallite size and the residual stress on the magnetic properties of the alloys was investigated. The residual stress increased as the applied current density was increased. It was associated to the high nucleation rate during electrodeposition and correlated to the lattice strain, estimated from the XRD patterns. Also from the XRD patterns the average crystallite size and the lattice constant were determined by Scherrer's and Rietveld's methods, respectively. Both parameters were directly influenced by the applied current density. Magnetic properties such as coercivity, remanence, saturation magnetization and squareness showed strong dependence on the residual stress and crystallite size. Coercivity higher than 1 kOe was achieved when a high current density was applied. High coercivity was attributed to the presence of residual stress and to the small crystallite size of deposits.     

退火热处理对纳米钨粉体性能的影响

采用工业化生产技术制备纳米钨粉体,对样品进行不同温度热处理;采用SEM、XRD、EDS和全自动比表面和孔隙度分析仪对样品的形貌、物相、含量和比表面、孔结构进行表征.通过计算品格变化率判断热处理后样品的晶格变化,并测量其粒径和孔容大小来解释晶粒的长大机理和孔结构的变化.结果表明:经热处理纳米钨粉体的晶格由收缩变为膨胀,且随热处理温度升高,比表面积和孔径均减小,粒径增大.当热处理温度达1200℃时,晶粒长大迅速,其长大机理根据晶界迁移解释.     

Yb_2O_3纳米晶的制备及其若干性质的研究

用溶胶 -凝胶法制备了不同粒径的 Yb2 O3纳米晶。XRD分析表明 :所合成的 Yb2 O3纳米晶属于立方晶系 ,空间群为 Ia3。TEM分析表明 :所合成的 Yb2 O3粒子基本呈球形。计算表明 :Yb2 O3的平均晶粒度随焙烧温度的升高而增大 ,而平均晶格畸变率随焙烧温度的升高和晶粒度的增大而减小 ,表明晶粒越小 ,晶格畸变越大 ,微晶发育越不完整。溶解性试验表明 :Yb2 O3晶粒度减小 ,表面活性增加。FTIR光谱分析表明 :纳米 Yb2 O3比普通的 Yb2 O3具有更高的表面活性 ,Yb- O键的吸收强度减弱 ,有微小的蓝移。     

Microstructural and mechanical study of nanocrystalline (Ti0.8W0.2)C synthesized by high-energy ball milling

The microstructural characteristics of nanocrystalline (Ti_0.8W_0.2)C elaborated by mechanical alloying process were investigated by using both X-ray diffraction and electron microscopy. The diffraction crystallite size (DCS) and the microstrain of (Ti_0.8W_0.2)C ball milled powders have been determined according to the Rietveld refinement method. The results obtained showed that the (Ti_0.8W_0.2)C diffraction crystallite size decreases and its microstrain increases as the milling duration increases. A transition from grain-size hardening to grain-size softening was observed at DCS = 8 nm. It is demonstrated that, as the grain size decreases, the plastic deformation mechanism undergoes a transition from an intragranular deformation by dislocation sliding to an intergranular deformation by grain boundary sliding, as a result of increasing volume fraction (39%) of the grain boundary (GB) zone.     

Microstructure evolution and thermal properties in nanocrystalline Fe during mechanical attrition

The microstructural evolution and thermal properties of nanocrystalline (nc) Fe during mechanical attrition were investigated by using quantitative X-ray diffraction and thermal analysis techniques. Upon milling of the Fe powders with coarse grains, grain refinement takes place gradually and a steady-state grain size in the nanometer regime is reached after a certain period of milling. With the further milling of the nc Fe within the stage of the steady-state grain size, we observed a grain boundary relaxation process that was manifested by evident decreases in the thermal expansion coefficient and the stored enthalpy, as well as slight decreases in the lattice strain and the Debye–Waller parameter. The grain boundary enthalpy of the nc Fe was estimated, showing a decreasing tendency with the milling time. The present work indicated with clear experimental evidence that the nc materials with the same grain size may exhibit very different properties that depend upon the microstructure of the numerous metastable grain boundaries.     

Microstructural changes of (Ti,W)C solid solution induced by ball milling

The effect of ball milling on microstructural change of (Ti,W)C solid solution was investigated. In addition to the particle size reduction with milling time, detailed studies using the X-ray diffraction line profiles were carried out to evaluate the microstructural parameters, including lattice parameter, crystallite size and microstrain. Nelson–Riley extrapolation and Williamson–Hall method are employed. The results suggest lattice expansion, with the lattice parameter increasing from 4.3212 Ǻ to 4.3241 Ǻ. The defects and surface stress generated during ball milling are deemed to be responsible for the increased d-spacing of (Ti,W)C solid solution with milling time. The crystallite size displays a diminishing trend with increasing milling time, which is consistent with the SEM observation. However, the microstrain developed is tensile in nature and firstly increases with up to 36 h milling, and then the strain reduces for further milling perhaps due to the strain relaxation by the formation of dislocations.     

金属熔体原子团簇的微观热收缩机制探讨

以多种纯金属及合金的X射线衍射实验结果为基础,结合理论分析,从自由体积的角度探讨金属熔体原子团簇的微观热收缩现象,进一步揭示微观热收缩的本质及机制:熔体中原子团簇的微观热收缩,是熔体中自由体积膨胀较之宏观体积膨胀更为严重的结果,团簇结构的变化是导致其出现热收缩的根本原因。     

New experimental insight into the mechanisms of nanoplasticity

The evolution of microstructure and texture of a nanocrystalline Pd–10 at.% Au alloy (initial grain size 16 nm) subjected to severe plastic deformation by high-pressure torsion (HPT) at room temperature is investigated by X-ray line profile analysis and X-ray microdiffraction, respectively. In addition, changes in the microhardness are measured and the texture is modeled. During HPT the microstructure changes: the crystallite size goes over the maximum, the dislocation density goes through a minimum and the density of stacking faults decreases at/up to a shear strain of ～1, corresponding to a grain size of 20 nm. Starting with a random texture, typical brass-type shear components develop at a shear strain above ～1. The microhardness with decreasing crystallite size goes over a maximum at ～20 nm. The correlated changes in microstructure, texture and strength strongly suggest the transition from a dislocation slip to a grain boundary sliding (GBS)-dominated deformation mechanism. The unexpected brass-type texture and its deviation from the ideal position can be simulated with the Taylor model assuming dominant partial dislocation slip and a certain contribution of GBS, respectively. Taken together, the results of many techniques applied to the same material, in particular those of the texture investigations, provide a more comprehensive and consistent picture of nanoplasticity than reported before for face-centered cubic metals.     

Plastic deformation behaviour of fine-grained materials

A phase mixture model in which a polycrystalline material is regarded as a mixture of a crystalline phase and a grain-boundary phase is presented. The model aims to describe the plastic deformation behaviour of fine-grained materials. The mechanical properties of the crystalline phase are modelled using unified viscoplastic constitutive relations, which take dislocation density evolution and diffusion creep into account. The total strain rate of a crystallite is calculated by summation of the contributions of dislocation, boundary diffusion and lattice diffusion mechanisms. The deformation mechanism for the grain-boundary phase is modelled as a diffusional flow of matter through the grain boundary. Using a simple rule of mixtures, the grain size dependence of the overall plastic deformation behaviour of the material is analysed. Rate effects are also investigated. The results of the calculations are compared with previously published experimental data.     

Long‐term atmospheric corrosion monitoring

The paper presents the analysis of corrosion rates of carbon steel, zinc, aluminium and copper after long‐term exposition as a function of time and environmental parameters. All experimental methodologies on the test sites were carried out according to ISO standards. The analysis of trends of environmental pollution and corrosion rates was performed for one year exposition of metals on three sites (urban/industrial, urban and rural atmosphere) in Poland. The corrosivity changes as a result of a reduction of corrosion rates of metals used are relatively smaller then the reduction of pollution. By using the equation C = Atⁿ, where C – corrosion rate after t years, A – corrosion rate after the first year of exposition, and results of long‐term corrosion rates, exponent n was determined for the different metals and sites from log‐log plots.     

水热沉淀法合成SnO_2纳米晶

用水热沉淀法合成了不同粒径的 Sn O2 纳米晶 ,属于四方晶系 ,空间群为 P4/ mnm。计算表明 :随焙烧温度的升高 ,Sn O2 晶粒度增大 ;而平均晶格畸变率则随晶粒度的增大而减小 ,表明粒子越小晶格畸变越大 ,晶粒发育越不完整。TEM分析结果表明 :所合成的 Sn O2 纳米粒子基本呈球形 ;随焙烧温度的升高 ,Sn O2 粒子的粒径增大。热失重分析表明 :水热沉淀法所合成的 Sn O2 纳米粉末中杂质含量很少 ,纯度高。     

水热沉淀法合成SnO2纳米晶

用水热沉淀法合成了不同粒径的ＳｎＯ２纳米晶,属于四方晶系,空间群为Ｐ４／ｍｎｍ。计算表明：随焙烧温度的升高,ＳｎＯ２晶粒度增则平均 格畸变率则随昌粒度的增大而减小,表明粒子越小昌格畸变越大,晶粒发育越失重分析表明;水热沉淀法所合成的ＳｎＯ２纳米粉末中杂质含量很少,纯度高。     

Primary water stress corrosion cracking (PWSCC) mechanism based on ordering reaction in Alloy 600

A PWSCC mechanism based on an ordering reaction in Alloy 600 is proposed. An activation energy for the ordering reaction in Alloy 600, Q = ～46 kcal/mole (～190 kJ/mole), are determined by a differential scanning calorimeter (DSC). The ordering reaction in Alloy 600 is an indispensable process during reactor operating conditions. The ordering reaction in Alloy 600 causes an anisotropic lattice contraction. This anisotropic contraction produces an additional stress. The stress level would be the maximum value about 70 and 300 MPa according to the lattice planes in Alloy 600 and Weld 182, respectively. In addition, the anisotropic contraction forms the micro cracks in the high angle grain boundary where the difference in lattice contraction is large. The formation of crack induces stress intensification at the crack tip, and this causes crack growth. The initiation and propagation of PWSCC is controlled by the formation, growth, and coalescence of micro cracks due to anisotropic lattice contraction by ordering. These whole processes are governed by the kinetics of the ordering reaction. This is the reason why the activation energy for PWSCC, Q pwscc = 40–50 kcal/mol, is consistent with that for the ordering reaction, Q ordering = 46 kcal/mol. This mechanism can be proved by the comparison of the initiation behavior in the ordered and the disordered specimens.     

Effect of crystallite size on structural and luminescent properties of nanostructured Eu:KGdF4 synthesised by co-precipitation method

The Eu³⁺:KGdF₄ powders with average crystallite size of 20 and 25 nm have been obtained from solution by co-precipitation method. Morphology of the as-received powders was examined by XRD and TEM methods. Behaviour of these two powdered batches, characterised by different size of nanocrystallites, versus thermal treatment has been studied by X-ray powder diffraction, thermogravimetric, infrared spectroscopy and emission spectroscopy methods. The phase transitions between low-temperature cubic, orthorhombic, trigonal and high-temperature cubic modifications of KGdF₄ were detected for both samples heated in 300–790 °C temperature range. Abundance of the particular polymorphic form observed at given temperature differs considerably for samples of different initial crystallite size. Besides, significant differences in number of lattice defects, water contents and emission properties were observed for these two samples. The properties of material precipitated from solution are also compared with structural and optical properties of the Eu³⁺:KGdF₄ fluoride synthesised by a solid-state reaction.     

脉冲电沉积块体纳米晶Co—Ni合金微观组织结构的研究

利用TEM、XRD、X射线能量散射谱（EDS）、位置敏感原子探针场离子显微镜(PoSAP)等方法研究了脉冲电沉积法制备的块体纳米晶Co-Ni合金的微观组织。结果表明：沉积层中Co含量随电解液中Co^2 离子浓度增加而显著增加;沉积层合金点阵参数随Co含量的增加按Vegard定律增加,同时晶粒尺寸减小;当晶粒尺寸减小到十几纳米时,出现附加的晶格膨胀效应;脉冲沉积与直流沉积相比,晶粒明显细化;PoSAP操作的在线观测和大量数据的计算机三维重构图表明,Co原子在沉积层中呈均匀分布;FIM观察分析表明纳米晶Co-Ni合金中存在三类晶间结构：正常晶界、非长程有序也非短有序的“类气态结构”和少量暗区。     

Effect of Al on Expansion Behavior of Mg–Al Alloys During Solidification

The cooling curves and the change of contraction/expansion during solidification and cooling were tested by using a selfmade device which could achieve the one-dimensional contraction instead of three-dimensional contraction of the casting.Then, the effects of Al content(0, 1.1, 3, 5, 10, 12.9, 15, 17, 19, 22, 24 and 30 wt%) on the thermal contraction/expansion of the binary Mg-Al as-cast alloys during solidification were obtained. The results showed that expanding instead of contraction was present in Mg-Al alloys with the addition of 0-30 wt% Al during solidification. The values of expansion significantly increased at first and then decreased with the increase in Al content. And the maximum expansion ratio of 0.44%(maximum expansion value: 0.841 mm) was present in the Mg-15 wt% Al alloy. Contraction instead of expansion occurred once the temperature drops to the temperature corresponding to the expansion value in total, indicating the occurrence of a continuous expansion during the solidification process in mushy zone for the Mg alloys with Al addition of 5-30 wt%. The expansion value in total consisted of two parts: the expansions occurring in the liquid-phase zone and mushy zone. The expansion in liquid zone was present in every Mg-Al alloy, and it contributed to the most proportion of the total expansion value when the Al content in Mg-Al alloy was lower than 10 wt% or higher than 22 wt%. However, the total expansion value was mainly determined by the solidification behavior in mushy zone when the Al content was among 10-22 wt% in Mg-Al alloys.     

铬含量对耐候钢熔敷金属韧性的影响

通过拉伸、冲击试验,利用金相显微镜、透射电镜、扫描电镜和电子背散射衍射技术分析了铬含量对耐候钢熔敷金属组织和韧性的影响.结果表明,两种熔敷金属的组织均为粒状贝氏体、针状铁素体和少量板条贝氏体.两种熔敷金属冲击韧性良好.与含1.0% Cr(质量分数)熔敷金属相比,含1.41% Cr熔敷金属中粒状贝氏体含量升高,针状铁素体含量降低,屈服强度增加6%,抗拉强度增加9%,冲击吸收功降低56%.此外,含1.41%Cr熔敷金属中M-A组元含量升高、大角度晶界比例下降、平均有效晶粒尺寸增加,显微裂纹的形核几率增加,裂纹扩展阻力降低,导致其韧性降低.     

用XRD线形分析法表征TiC粉体中的镶嵌尺寸与晶格畸变

采用XRD线形分析(双Voigt函数)法对球磨行星96h的TiC粉和纳米TiC粉中的镶嵌尺寸和晶格畸变进行了对比分析和表征,并采用TEM法印证。研究结果表明,球磨粉的平均镶嵌尺寸大约为纳米粉的40%,而球磨粉的平均晶格畸变大约为纳米粉的5倍。TEM的分析结果与XRD表征结果相吻合。     

Influence of Al2O3 nanoparticles on solubility extension of Cr in Cu by mechanical alloying

In this study, the effect of the presence of Al₂O₃ nanoparticles during mechanical alloying on the extension of Cr solid solubility in Cu was investigated. The lattice parameter, dislocation density and crystallite size were evaluated by the X-ray diffraction technique. Also, the microstructure was characterized by scanning electron microscopy and transmission electron microscopy. The final product was a nanocrystalline and supersaturated Cu–Cr solid solution with a mean crystallite size ranging from 8 to 19 nm depending on the composition. The Gibbs free energy changes in these systems due to the dislocation density and crystallite size variations during milling were calculated. It was found that the presence of Al₂O₃ nanoparticles was beneficial to the process, and this was particularly related to its significant contribution to the increase of strain part of Gibbs free energy changes.     

Interactions between non-screw lattice dislocations and coherent twin boundaries in face-centered cubic metals

In a first report [Jin ZH, Gumbsch P, Ma E, Albe K, Lu K, Hahn H, et al. Scripta Mater 2006;54:1163], interactions between screw dislocation and coherent twin boundary (CTB) were studied via molecular dynamics simulations for three face-centered cubic (fcc) metals, Cu, Ni and Al. To complement those preliminary results, purely stress-driven interactions between 60° non-screw lattice dislocation and CTB are considered in this paper. Depending on the material and the applied strain, slip has been observed to interact with the boundary in different ways. If a 60° dislocation is forced by an external stress into a CTB, it dissociates into different partial dislocations gliding into the twin as well as along the twin boundary. A sessile dislocation lock may be generated at the CTB if the transited slip is incomplete. The details of the interaction are controlled by the material-dependent energy barriers for the formation of Shockley partial dislocations from the site where the lattice dislocation impinges upon the boundary.