Characterization of twinning in electrodeposited Ni–Mn alloys

Twinning is ubiquitous in electroplated metals. Here, we identify and discuss unique aspects of twinning found in electrodeposited Ni–Mn alloys. Previous reports concluded that the twin boundaries effectively refine the grain size, which enhances mechanical strength. Quantitative measurements from transmission electron microscopy (TEM) images show that the relative boundary length in the as-plated microstructure primarily comprises twin interfaces. Detailed TEM characterization reveals a range of length scales associated with twinning beginning with colonies (～1000?nm) down to the width of individual twins, which is typically <50?nm. We also consider the connection between the crystallographic texture of the electrodeposit and the orientation of the twin planes with respect to the plating direction. The Ni–Mn alloy deposits in this work possess a {110}-fiber texture. While twinning can occur on {111} planes either perpendicular or oblique to the plating direction in {110}-oriented grains, plan-view TEM images show that twins form primarily on those planes parallel to the plating direction. Therefore, grains enclosed by twins and multiply twinned particles are produced. Another important consequence of a high twin density is the formation of large numbers of twin-related junctions. We measure an area density of twin junctions that is comparable to the density of dislocations in a heavily cold-worked metal.     

Thickness-dependent orientation evolution in nickel thin films grown on yttria-stabilized zirconia single crystals

Microstructure evolution along with crystallographic orientation change as a function of film thickness was investigated in Ni thin films grown on (100) yttria-stabilized zirconia (YSZ) single crystal substrates. Texture development with two different orientation relationships, OR1: Ni {111}//YSZ {100} and OR2: Ni {100}//YSZ {100}, cube on cube orientation were identified by X-ray diffraction and transmission electron microscopy depending on the film thickness. The observed orientation transition reveals the existence of a critical thickness (～320?nm) favoring two different orientations in sputtered Ni films on YSZ (100) substrate.     

Structure of Ba0.7Sr0.3TiO3 films grown by chemical solution deposition on polycor substrates

The structure of barium strontium titanate (BST) films grown by chemical solution deposition on polycor substrates was studied by transmission electron microscopy, high-resolution microscopy, and x-ray diffraction analysis. It was found that a grain structure inhomogeneous in cross section is formed after two-step crystallization at T = 700 and 950°C. There are equiaxed grains (44.2 nm in average size) in the BST-polycor interfacial region and a multilevel columnar structure (grain height up to 150 nm) with {100} texture in the film bulk. Grain growth inhibition during high-temperature annealing and underlayer formation in the interfacial region are caused by a change in the substrate structure, i.e., grain reorientation and {112} texture formation.     

CVD金刚石薄膜孪晶形成的原子机理分析

采用X射线衍射技术、电子背散射衍射技术和扫描电镜分别观察了不同甲烷浓度条件下沉积的CVD自支撑金刚石薄膜的宏观织构、晶界分布和表面形貌. 研究了一阶孪晶在金刚石晶体{111}面生长的原子堆垛过程. 结果表明，由于一阶孪晶〈111〉60°的取向差关系以及{111}面的原子堆垛结构，使{111}面上容易借助碳原子的偏转沉积产生一阶孪晶. 低甲烷浓度时，碳原子倾向于在表面能较低的{111}面沉积，为孪晶的形成提供了便利，且高频率孪晶使薄膜织构强度减弱. 甲烷浓度升高使生长激活能较小的{001}面成为主要前沿生长面，因而只有〈001〉晶向平行薄膜法向的晶粒能够不断长大，因此孪晶形核概率明显减小. 另外，在薄膜中发现二阶孪晶，并对二阶孪晶的形成进行了分析. 关键词： 金刚石薄膜 孪晶 原子机理 取向差     

Grain refinement and texture evolution during high precision machining of a Ni-based superalloy

Abstract

The grain refinement and texture evolution in the surface gradient microstructure of a Ni-based superalloy induced by high speed machining was studied in this research. The direct evidence of grain refinement induced by dislocation–twin interaction was revealed and the detailed grain refinement process was summarised as deformation twinning, dislocation-twin reaction, localied thinning of nanotwin lamellae and final fracture. The underlying dislocation–twin interaction mechanism was elucidated from the crystallographic perspective. Using electron backscatter diffraction and precession electron diffraction techniques, a multiscale texture analysis covering undeformed coarse grain region, ultrafine grain region and nanograin region was carried out. The texture evolution with decreasing depth to the machined surface was identified as cube in the bulk interior and a mixture of rotated cube {0?0?1}<1?1?0>, cube {1?0?0}<0?0?1>, copper {1?1?2}<1?1?1 > and Goss {1?1?0}<0?0?1> textures in the topmost 1.3-μm-thick nanograin layer. The intrinsic thermomechanical effects of high precision machining are responsible for crystallographic texture transformation.     

用于YBCO高温超导涂层的立方织构铜基带制备

Cu是制备双轴织构YBCO高温超导涂层的优良基带材料之一,立方织构的铜带可以提供良好的外延生长环境。文中采用轧制辅助双轴织构基带技术(RABiTS),研究了立方织构铜基带的制备工艺。将铜锭在初轧变形量达到88.4%后,进行400℃退火30min,再经二次轧制总变形量达到99.07%后,在氩气环境125—850℃之间不同温度下退火30min。用March-Dollase函数计算该系列样品的r值,其中850℃退火的样品具有最强的200择优取向,r值为0.25,用不完整极图对该样品的织构情况做进一步分析,用ODF函数定量计算了该样品立方织构的体积百分含量。该样品形成了较强的{001}<100>立方织构,体积百分含量为70.8%。     

Grain refinement and strengthening of austenitic stainless steels during large strain cold rolling

The microstructure/texture evolution and strengthening of 316?L-type and 304?L-type austenitic stainless steels during cold rolling were studied. The cold rolling was accompanied by the deformation twinning and micro-shear banding followed by the strain-induced martensitic transformation, leading to nanocrystalline microstructures consisting of flattened austenite and martensite grains. The fraction of ultrafine grains can be expressed by a modified Johnson-Mehl-Avrami-Kolmogorov equation, while inverse exponential function holds as a first approximation between the mean grain size (austenite or martensite) and the total strain. The deformation austenite was characterised by the texture components of Brass, {011}<211>, Goss, {011}<100>, and S, {123}<634>, whereas the deformation martensite exhibited a strong {223}<110> texture component along with remarkable γ-fibre, <111>∥ND, with a maximum at {111}<211>. The grain refinement during cold rolling led to substantial strengthening, which could be expressed by a summation of the austenite and martensite strengthening contributions.     

On the 2D-3D transition in epitaxial thin film growth

The theory is based on the fact that the equilibrium concentration of single atoms adsorbed on the surface of a monolayer island placed on a foreign substrate such that the substrate-deposit interaction is weaker than the deposit-deposit interaction is higher than the equilibrium concentration of atoms adsorbed on the surface of the same island now placed on a substrate of the same material. This higher adatom concentration leads to 2D nucleation on top of the monolayer island. The difference of the above equilibrium adatom concentrations appears as a driving force for the process of transformation of the initial monolayer island into a 3D island by detachment of atoms from the first monolayer island edges and their subsequent attachment to the edges of the second layer nucleus. The kinetics of this process are studied in detail, the following two cases being considered. The first case consists of breaking up and agglomeration of an initially continuous film into 3D crystals upon heating. The second case consists of change of the growth mode from layer to island mode during the vapour deposition when the substrate temperature increases. Expressions for the critical temperatures for these two phenomena to occur are derived. It is shown that they depend strongly on the substrate orientation, the critical temperature being higher for the 〈111〉 orientation in comparison with the 〈110〉 orientation, if substrate and deposit with a fcc lattice are considered. The theoretical results are compared with experimental data for deposition of Au on Mo{110}, Cu on W{110} and W{100} and Fe on Cu{111}.     

Studies on high-moment soft magnetic FeCo/Co thin films

The dependences of soft magnetic properties and microstructures of the sputtered FeCo (=FeFeCo薄膜 溅射条件 软磁性 高饱和磁化强度FeCo film, sputtering conditions, high saturation magnetization, soft magnetic properties2005-10-263/7/2006 12:00:00 AMThe dependences of soft magnetic properties and microstructures of the sputtered FeCo （=Fe65Co35） films on Co underlayer thickness tCo, FeCo thickness tFeCo, substrate temperature Ts and taxget-substrate spacing dT-s are studied. FeCo single layer generally shows a high coercivity with no obvious magnetic anisotropy. Excellent soft magnetic properties with saturation magnetization μ0Ms of 2.35 T and hard axis coercivity Hch of 0.25 kA/m in FeCo films can be achieved by introducing a Co underlayer. It is shown that sandwiching a Co underlayer causes a change in orientation and reduction in grain size from 70 nm to about 10 nm in the FeCo layer. The magnetic softness can be explained by the Hoffmann＇s ripple theory due to the effect of grain size. The magnetic anisotropy can be controlled by changing dT-S, and a maximum of 14.3 kA/m for anisotropic field Hk is obtained with dT-S=18.0 cm.     

Carbon ion beam-induced variation in orientation of crystal planes of polycrystalline Zn nanowires

In the present work, polycrystalline Zn nanowires are synthesised within polymeric templates by the electrochemical deposition technique. Free-standing Zn nanowires with diameters 100, 200, 400 nm were synthesised on copper substrate acting as cathode, using this technique. The synthesised nanowires were irradiated with 40 MeV C⁴⁺ ion beam for various fluencies at Inter University Accelerator Centre, New Delhi, India. The effect of carbon ion beam on the grain size and preferred orientation of crystal planes of Zn nanowires were studied. The Rigaku X-ray diffractometer was used for X-ray diffraction (XRD) spectra of pristine and irradiated Zn nanowires. Post irradiation XRD analysis showed variation in the intensity of peaks, indicating the change in the orientation of crystal planes of the material. The preferred orientation of the crystal lattice planes in the polycrystalline material was found using texture analysis. To quantitatively investigate the degree of preferred orientations, the texture coefficients (TC) were calculated. The variation of TC was used to demonstrate the effect of irradiation on preferred orientation.     

Laser induced copper electroless plating on polyimide with Q-switch Nd:YAG laser

The results of laser induced deposition of copper on polyimide substrate from copper electrolyte solution are reported. Unlike most work reported in the literatures where CW Ar⁺ lasers were used, a second harmonic (532 nm wavelength) Q-switch Nd:YAG laser was used for our experiments. The deposition process was conducted by laser-catalyzing of the polyimide surface and subsequent photothermal-accelerated reduction of copper-complex ions in an alkaline reducing environment. The characteristics of the deposited copper line were investigated in terms of laser beam scanning speed, and the number of scans. The surface morphology and chemical composition of the deposited copper were analyzed using field emission scanning electron microscope (FESEM) and energy dispersive spectrometer (EDX). The optimum processing conditions have been identified. The copper deposit was found to adhere well to the substrate.     

Mechanism of film growth of pulsed electrodeposition of nanocrystalline copper in presence of thiourea

This article reports the effect of addition of small amount of thiourea on mechanism of film growth, levelling and grain refinement of pulsed electrodeposition of nanocrystalline copper on stainless steel substrate using simple aqueous acidic copper sulphate solution prepared from 0.25 M CuSO₄·5H₂O and 0.5 M H₂SO₄. The amount of thiourea used in the electrolyte is 0 and 36 mg/l. The results indicate the change in morphology of the deposits with addition of thiourea leading to dendrite free copper deposits. The growth mechanism of the copper deposition is found to change from Volmer–Weber type to Frank-Vander Merwe type making the deposits smoother when deposited with thiourea addition. A small amount (36 mg/l) of thiourea addition leads to decrease in the average grain size of copper from 1160 nm to 14 nm. The results clearly reveal the formation of nanocrystalline copper by addition of thiourea with three orders of magnitude reduction in grain size as compared to the sample deposited without thiourea. Preferential segregation of sulphur (present in thiourea) along the grain boundaries of nanocrystalline copper is shown by energy filter imaging using ultra high resolution transmission electron microscope (TEM), thereby restricting the growth of copper grains during pulsed electrodeposition.     

Microstructural changes in amorphous Si/crystalline Al thin bilayer films upon annealing

Microstructural changes occurring in a sputter deposited Si (150 nm, amorphous)/Al (50 nm, crystalline); {111} fibre textured bilayer, upon annealing at 523 K for 60 min in a vacuum of 2.0×10^-4 Pa, were analyzed employing X-ray diffraction, Auger electron spectroscopy, scanning electron microscopy, atomic force microscopy and focused-ion beam imaging. After the annealing the Al and Si sublayers had largely exchanged their locations in the bilayer; i.e. the Si layer was adjacent to the substrate after annealing. Simultaneously, the amorphous Si layer had crystallized into an aggregate of {111} oriented nanocrystals, with a crystallite size of about 15 nm. The Al layer, now adjacent to the surface, had formed a uniformly net-shaped layer in association with an increase of the surface roughness. Upon this rearrangement, the already initially present Al {111} fibre texture had become stronger, the Al crystallites had grown laterally and the macrostress in the Al layer had relaxed. An extensive analysis of thermodynamic driving forces for the transformation indicated that the largest gain in energy upon transformation is due to the crystallization of the amorphous Si. The only identifiable driving force for the layer exchange appears to be the release of elastic energy upon the rearrangement of the Si and Al phases in the layer. PACS 61.43.D; 61.72.C; 62.40; 65.70; 68.55.J; 68.60.BThis revised version was published online in September 2004. Due to technical problems the PDF of the previous version was incomplete.     

Spin-valve magnetoresistive structures based on Co/Tb multilayer films

The effect of the layer thickness on the magnetic properties of {Co/Tb}_n, {Co/Tb}_n/Co, and {Co/Tb}_n/Co/Cu/Co multilayer films is studied. The dependence of the hysteresis and magnetoresistive properties of {Co(1 nm)/Tb(1 nm)}_n/Co(5 nm)/Cu(L _Cu)/Co(5 nm) structures on the thickness of the {Co/Tb}_n layer and copper spacing are obtained. The feasibility of spin-valve structures based on {Co/Tb}_n multilayer films with in-plane anisotropy is demonstrated.     

Thermal stability of Cu–Nb nanolamellar composites fabricated via accumulative roll bonding

In situ annealing within a neutron beam line and ex situ annealing followed by transmission electron microscopy were used to study the thermal stability of the texture, microstructure, and bi-metal interface in bulk nanolamellar Cu/Nb composites (h?=?18?nm individual layer thickness) fabricated via accumulative roll bonding, a severe plastic deformation technique. Compared to the bulk single-phase constituent materials, the nanocomposite is two orders of magnitude higher in hardness and significantly more thermally stable, e.g., no observed recrystallization in Cu at temperatures as high as 85% of the melting temperature. The nanoscale h?=?18?nm individual layer thickness is maintained up to 500°C, the lamellar structure thickens but is maintained up to 700°C, and recrystallization is suppressed even up to 900°C. With increasing temperature, the texture sharpens, and among the interfaces found in the starting material, the {112}_Cu?||?{112}_Nb interface with a Kurdjumov-Sachs orientation relationship shows the greatest thermal stability. Our results suggest that thickening of the individual layers under heat treatment coincides with thermally driven removal of energetically unfavorable bi-metal interfaces. Thus, we uncover a temperature regime that maintains the lamellar structure but alters the interface distribution such that a single, low energy, thermally stable interface prevails.     

Effects of underlayer materials and substrate temperatures on the structural and magnetic properties of Nd2Fe14B films

Thin films of Nd_2Fe_{14}B were fabricated on heated glass substrates by dc magnetron sputtering. Different material underlayers (Ta, Mo, or W) were used to examine the underlayer influence on the structural and magnetic properties of the NdFeB films. Deposited on a Ta buffer layer at 420℃, the 300 nm thick NdFeB films were shown to be isotropic. But when the substrate temperature T_s was elevated to 520℃, the Nd_2Fe_{14}B crystallites of (00l) plane were epitaxially grown on Ta (110) underlayer. In contrast, Mo (110) buffer layer could not induce any preferential orientation in NdFeB film irrespective of the substrate temperature or film thickness. The W buffer layer was found to be most effective for the nucleation of Nd_2Fe_{14}B crystallites with c-axis alignment perpendicular to the film plane when T_s<490℃. But at T_s=490℃ the magnetic layer became isotropic. The maximum coercivity obtained was about 995 kA/m for the 100nm film deposited on W underlayer at 490℃. These variations were tentatively explained in terms of the lattice misfit between the underlayer and the magnetic layer, combined with the considerations of underlayer morphologies.     

单晶铜纳米线屈服机理的原子模拟研究

采用分子静力学方法模拟了〈100〉单晶铜纳米线的拉伸变形过程,研究了纳米线屈服的机理. 结果表明：1） 纳米线初始屈服通过部分位错随机激活的{111}〈112〉孪生实现,后继屈服通过{111}〈112〉部分位错滑移实现;2） 纳米线变形初期不同滑移面上的部分位错在两面交线处相遇形成压杆位错,变形后期部分位错在刚性边界处塞积,两者都阻碍位错滑移,引起一定的强化作用. 关键词： 纳米线 屈服 位错 分子静力学     

High-resolution transmission electron microscopy study of crystallography and morphology of TiC precipitates in tempered steel

In spite of the significance of NaCl-type transition-metal carbides in steels, their crystallography and morphology have not been understood on an atomic scale. High-resolution electron microscopy was employed in the present work to examine the crystallography and morphology of TiC particles that precipitated in the quenched and tempered 0.05?wt%?C–0.20?wt%?Ti–2.0?wt%?Ni steel. Plate-like TiC precipitates with a thickness ranging from a couple of atomic layers to 20?nm were observed in steels by tempering at 550, 600 and 800°C. It was found that the Baker–Nutting orientation relationship is always satisfied with the ferrite matrix within about 5° for both the nanosized and the coarse TiC particles. The habit plane of the TiC precipitate is the (100) ferrite plane. A moderate tendency for the faceting of lateral interfaces on the {001} and {011} ferrite planes was found. The presence of interfacial misfit dislocations was revealed by examining the excess lattice fringes terminating at the interfaces between the TiC platelet and the ferrite matrix. The location and number of the excess lattice fringes terminating at the broad plane and the lateral interface were consistent with the mismatch in the atomic arrangement between the Baker–Nutting orientation relationship related TiC and ferrite.     

Growth and desorption of indium epitaxial layers investigated by high field microscopy

Growth of indium single crystals on tungsten field emission tips was carried out by deposition of indium from vapour in ultra high vacuum, using substrate temperatures in the range of 293–420 K. Two different tungsten tips were used as the substrate: a perfect W single crystal in one case and a bi-crystal with a distinct grain boundary in the other. No influence of the grain boundary on the epitaxial growth was found. Two orientation relationships were observed mostly: {111}In ∥ {110}W with 〈110〉In ∥ 〈111〉W and {111}In ∥ {100}W with 〈110〉In ∥ 〈110〉W. In the first case the growth was initiated by the indium nucleus created on the ledges of the {110}W plane. A field strength of 0.9 V/Å was found for the evaporation field of indium. The field strength of the desorption of In-W interfacial layer atoms was found to be 4.4–5.2 V/Å. A mechanism of the growth of indium crystals has been proposed.     

A novel Si-rich SiN bilayer passivation with thin-barrier AlGaN/GaN HEMTs for high performance millimeter-wave applications

We demonstrate a novel Si-rich SiN bilayer passivation technology for AlGaN/GaN high electron mobility transistors (HEMTs) with thin-barrier to minimize surface leakage current to enhance the breakdown voltage. The bilayer SiN with 20-nm Si-rich SiN and 100-nm Si$_{3}$N$_{4}$ was deposited by plasma-enhanced chemical vapor deposition (PECVD) after removing 20-nm SiO$_{2}$ pre-deposition layer. Compared to traditional Si$_{3}$N$_{4}$ passivation for thin-barrier AlGaN/GaN HEMTs, Si-rich SiN bilayer passivation can suppress the current collapse ratio from 18.54% to 8.40%. However, Si-rich bilayer passivation leads to a severer surface leakage current, so that it has a low breakdown voltage. The 20-nm SiO$_{2}$ pre-deposition layer can protect the surface of HEMTs in fabrication process and decrease Ga-O bonds, resulting in a lower surface leakage current. In contrast to passivating Si-rich SiN directly, devices with the novel Si-rich SiN bilayer passivation increase the breakdown voltage from 29 V to 85 V. Radio frequency (RF) small-signal characteristics show that HEMTs with the novel bilayer SiN passivation leads to $f_{\rm T}/f_{\rm max}$ of 68 GHz/102 GHz. At 30 GHz and $V_{\rm DS} = 20$ V, devices achieve a maximum $P_{\rm out}$ of 5.2 W/mm and a peak power-added efficiency (PAE) of 42.2%. These results indicate that HEMTs with the novel bilayer SiN passivation can have potential applications in the millimeter-wave range.