Enhancing the adhesion strength of micro electroforming layer by ultrasonic agitation method and the application

Micro electroforming is widely used for fabricating micro metal devices in Micro Electro Mechanism System (MEMS). However, there is the problem of poor adhesion strength between micro electroforming layer and substrate. This dramatically influences the dimensional accuracy of the device. To solve this problem, ultrasonic agitation method is applied during the micro electroforming process. To explore the effect of the ultrasonic agitation on the adhesion strength, micro electroforming experiments were carried out under different ultrasonic power (0 W, 100 W, 150 W, 200 W, 250 W) and different ultrasonic frequencies (0 kHz, 40 kHz, 80 kHz, 120 kHz, 200 kHz). The effects of the ultrasonic power and the ultrasonic frequency on the micro electroforming process were investigated by polarization method and alternating current (a.c.) impedance method. The adhesion strength between the electroforming layer and the substrate was measured by scratch test. The compressive stress of the electroforming layer was measured by X-ray Diffraction (XRD) method. The crystallite size of the electroforming layer was measured by Transmission Electron Microscopy (TEM) method. The internal contact surface area of the electroforming layer was measured by cyclic voltammetry (CV) method. The experimental results indicate that the ultrasonic agitation can decrease the polarization overpotential and increase the charge transfer process. Generally, the internal contact surface area is increased and the compressive stress is reduced. And then the adhesion strength is enhanced. Due to the different depolarization effects of the ultrasonic power and the ultrasonic frequency, the effects on strengthening the adhesion strength are different. When the ultrasonic agitation is 200 W and 40 kHz, the effect on strengthening the adhesion strength is the best. In order to prove the effect which the ultrasonic agitation can improve the adhesion strength of the micro devices, micro pillar arrays were fabricated under ultrasonic agitation (200 W, 40 kHz). The experimental results show that the residual rate of the micro pillar arrays is increased about 17% by ultrasonic agitation method. This work contributes to fabricating the electroforming layer with large adhesion strength.     

Stress‐enhanced dislocation density reduction in multicrystalline silicon

Stress is generally perceived to be detrimental for multicrystalline silicon (mc‐Si), leading to dislocation multiplication during crystal growth and processing. Herein, we evaluate the role of stress as a driving force for dislocation density reduction in mc‐Si. At high temperatures, close to the melting point (>0.8T_m), we observe that the application of stress as well as the relief of residual stress, can modify the density of pre‐existing dislocations in as‐grown mc‐Si under certain conditions, leading to a net local reduction of dislocation density. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Residual stress and strain in CdZnTe wafer examined by X-ray diffraction methods

A non-destructive method based on X-ray diffraction was developed to measure the stress and strain in CdZnTe single crystal near the surface. From the experimental results and calculations, the residual stresses in CdZnTe single crystal were determined to be σ₁=30 MPa, σ₂=14 MPa, and τ₁₂=-4 MPa, respectively. The residual stress derived from the measurement strain in CdZnTe was thought to be composed of the thermal stress, the misfit stress, and the mechanical stress. The distributions of non-uniform strain in a CdZnTe wafer are about 3.9%, while the distributions of uniform strain in the CdZnTe wafer are 0.5%, much smaller than those of the non-uniform strain. PACS 02.10.Xm; 71.55.Gs; 61.10.Nz; 68.35.Gy; 81.40.Jj     

Relation between the internal stress measured in creep and the stress generated by the dislocation structure in the fcc metals

From the steady-state creep rate data treated as a function of the applied and the measured effective stress and temperature, a phenomenological dependence of the internal stress on the applied stress and temperature was derived. The result determined the expected character of the applied stress- and temperature dependences of the dislocation density, which was considered the microstructure parameter of the internal stress σ _i?=?α MGbρ ^1/2 (σ_i is the internal stress, α the dislocation interaction factor, M the Taylor factor, G the shear modulus, b the Burgers vector length and ρ the dislocation density). A scaling of the expected dislocation density by fitting it to measured dislocation density data yielded reasonable values of the parameter α in the Taylor formula, but the experimental data indicated a weaker applied stress dependence of the measured dislocation density than that of the expected dependence. An admission of an empirical formula fitting the dependence of dislocation density on the applied stress and temperature leads to a suggestion that the parameter α might be dependent on applied stress and temperature.     

Surface size effects under plastic deformation of microcrystals and nanocrystals

The size effects associated with the crystal surface as an effective sink for moving dislocations in a thin crystal and as a barrier for these dislocations in the presence of a high-strength film or a special hardened layer on the surface, which favor the accumulation of dislocations in the crystal, have been considered theoretically in terms of the kinetic equation for the density of dislocations concentrated in the crystal in the critical lengths of single-ended (unipolar) dislocation sources. The theoretical results have been illustrated by the experimental data available in the literature for microcrystals and nanocrystals of copper and aluminum. It has been found in accordance with these data that the dependence of the yield stress ??_2% of the crystal on the crystal transverse size D has the form ??_2% ?? D ^?0.75 when there is a free crystal surface for the escape ofthe dislocations and ??_2% ?? D ^?0.5 when there is a high-strength layer on the lateral surface of the crystal..     

Dislocations in GaAs single crystals grown by the Czochralski method

The influence was studied of growth conditions on the dislocation density in gallium arsenide single crystals grown by the Czochralski method from a gallium-enriched melt. Etching in a solution of 1 part cone. HNO₃ and 2 parts H₂O served to determine the dislocation density across and along a single crystal. The dislocation density along the crystal was found to depend mainly on the angle of crystal diameter increase.     

Effects of ultrasonic agitation on adhesion strength of micro electroforming Ni layer on Cu substrate

Micro electroforming is an important technology, which is widely used for fabricating micro metal devices in MEMS. The micro metal devices have the problem of poor adhesion strength, which has dramatically influenced the dimensional accuracy of the devices and seriously limited the development of the micro electroforming technology. In order to improve the adhesion strength, ultrasonic agitation method is applied during the micro electroforming process in this paper. To explore the effect of the ultrasonic agitation, micro electroforming experiments were carried out under ultrasonic and ultrasonic-free conditions. The effects of the ultrasonic agitation on the micro electroforming process were investigated by polarization and alternating current (a.c.) impedance methods. The real surface area of the electroforming layer was measured by cyclic voltammetry method. The compressive stress and the crystallite size of the electroforming layer were measured by X-ray Diffraction (XRD) method. The adhesion strength of the electroforming layer was measured by scratch test. The experimental results show that the imposition of the ultrasonic agitation decreases the polarization overpotential and increases the charge transfer process at the electrode–electrolyte interface during the electroforming process. The ultrasonic agitation increases the crystallite size and the real surface area, and reduces the compressive stress. Then the adhesion strength is improved about 47% by the ultrasonic agitation in average. In addition, mechanisms of the ultrasonic agitation improving the adhesion strength are originally explored in this paper. The mechanisms are that the ultrasonic agitation increases the crystallite size, which reduces the compressive stress. The lower the compressive stress is, the larger the adhesion strength is. Furthermore, the ultrasonic agitation increases the real surface area, enhances the mechanical interlocking strength and consequently increases the adhesion strength. This work contributes to fabricating the electroforming layer with large adhesion strength.     

离子束溅射制备Nb2O5光学薄膜的特性研究

研究了离子束溅射(IBS)制备的Nb₂O₅薄膜的光学特性、应力、薄膜微结构等特性,系统地分析了辅助离子源的离子束能量和离子束流对薄膜特性的影响.结果显示,在辅助离子源不同参数情况下,折射率在波长550 nm处为2.310—2.276,应力值为-281—-152 MPa.在合适的工艺参数下,消光系数可小于10^-4,薄膜具有很好的表面平整度.与用离子辅助沉积(IAD)制备的薄膜相比,IBS制备的薄膜具有更好的光学特性和薄膜微结构. 关键词： 2O₅薄膜')" href="#">Nb₂O₅薄膜 离子束溅射 光学特性 应力     

Slip band formation and mobile dislocation density generation in high rate deformation of single fcc crystals

The mechanisms for the nucleation, thickening, and growth of crystallographic slip bands from the sub-nanoscale to the microscale are studied using three-dimensional dislocation dynamics. In the simulations, a single fcc crystal is strained along the [111] direction at three different high strain rates: 10⁴, 10⁵, and 10⁶?s^??1. Dislocation inertia and drag are included and the simulations were conducted with and without cross-slip. With cross-slip, slip bands form parallel to active (111) planes as a result of double cross-slip onto fresh glide planes within localized regions of the crystal. In this manner, fine nanoscale slip bands nucleate throughout the crystal, and, with further straining, build up to larger bands by a proposed self-replicating mechanism. It is shown that slip bands are regions of concentrated glide, high dislocation multiplication rates, and high dislocation velocities. Cross-slip increases in activity proportionally with the product of the total dislocation density and the square root of the applied stress. Effects of cross-slip on work hardening are attributed to the role of cross-slip on mobile dislocation generation, rather than slip band formation. A new dislocation density evolution law is presented for high rates, which introduces the mobile density, a state variable that is missing in most constitutive laws.     

Influence of ultrasonic in low thermal expansion Fe-Ni electrodeposition process for micro-electroforming

The electrochemical mechanism of Fe-Ni electrodeposition under ultrasonic was investigated by electrochemistry methods. Linear scanning voltammetry and cyclic voltammetry were used to show that the deposition process changed from the diffusion control under static conditions to an electrochemical control under ultrasonic conditions. Chronoamperometry curves showed that the Fe-Ni deposit occurred by a mechanism that instantaneous nucleation is followed by three-dimensional growth under charge transfer control. Chronopotentiogram indicated that because of the intensity of the ultrasound stripping effect, high ultrasonic power is unsuitable for electroforming Fe-Ni alloy, and a high current density is also not appropriate. Thus, the optimum parameters for Fe-Ni electrodeposition under ultrasonic conditions are ultrasonic power between 80 and 100 W (power density 0.28–0.35 W/cm²), and a current density lower than 10 mA/cm² with temperature 323 K and pH 3. Experiments were performed to verify that the Fe-Ni masks prepared by ultrasonic-assisted electroforming had a good surface quality. The increase in ultrasonic power can obtain a larger grain size, thus got a low thermal expansion coefficient and a high hardness. Therefore, ultrasonic-assisted electrodeposition technology provides an effective and practically feasible manufacturing method for OLED Fe-Ni mask preparation.     

The size effects upon shock plastic compression of nanocrystals

For the first time a theoretical analysis of scale effects upon the shock plastic compression of nanocrystals is implemented in the context of a dislocation kinetic approach based on the equations and relationships of dislocation kinetics. The yield point of crystals τ_y is established as a quantitative function of their cross-section size D and the rate of shock deformation as τ_y ~ ε^2/3 D. This dependence is valid in the case of elastic stress relaxation on account of emission of dislocations from single-pole Frank–Read sources near the crystal surface.     

Characterization of defect type and dislocation density in double oxide heteroepitaxial CeO2/YSZ/Si(001) films

In order to qualitatively and quantitatively analyze the structural defects including the defect types and their concentrations in oxide heteroepitaxial films, a new X-ray rocking-curve width-fitting method was used in the case of doubleCeO₂/YSZ/Si (YSZ=yttria-stabilized ZrO₂) films that were prepared by pulsed laser deposition. Two main defect types, angular rotation and oriented curvature, were found in both CeO₂ and YSZ. Dislocation densities of CeO₂ and YSZ, which were obtained from the angular rotations, are functions of the YSZ thickness. A distinct two-step correlation between dislocation densities of CeO₂ and YSZ was found that as the dislocation density of YSZ is higher than 2.4×10¹¹ cm^-2, the dislocation density of CeO₂ shows a high sensitivity with that of YSZ compared with the low relativity in lower dislocation density (<2.4×10¹¹ cm^-2). In addition, YSZ always has higher dislocation densities and oriented curvatures than CeO₂ in each specimen, which can be attributed to the smaller mosaic domain sizes in YSZ than in CeO₂ as observed by high-resolution transmission electron microscopy. Received: 12 August 2002 / Accepted: 14 August 2002 / Published online: 4 December 2002 RID="*" ID="*"Corresponding author. Fax: +81-3/5734-3369, E-mail: chun_hua_chen@hotmail.com     

激光冲击对不锈钢焊接接头残余应力场的影响

针对不锈钢焊接接头存在残余应力且分布不均匀、容易发生应力腐蚀的问题,采用激光冲击强化对其进行处理,探究激光功率密度和冲击次数对表面残余应力状态的优化作用,并通过应力腐蚀试验验证优化效果。结果表明：随着功率密度增加,表面残余应力明显下降,但下降幅度逐渐减小,功率密度4.24 GW/cm2与2.83 GW/cm2冲击产生的残余应力相差不大,熔合区还存在残余拉应力,说明高功率密度不足以消除表面残余拉应力;随着冲击次数增加,残余拉应力显著降低,2.83 GW/cm2冲击3次之后,残余拉应力完全消除,局部最高应力梯度从54.7 MPa/mm下降到11.7 MPa/mm,获得了高数值、分布均匀的残余压应力层。激光冲击强化后,焊接试样的应力腐蚀断裂时间提高了33.48%,激光冲击强化产生的残余压应力是其应力腐蚀抗性提高的重要原因。     

激光冲击对不锈钢焊接接头残余应力场的影响

针对不锈钢焊接接头存在残余应力且分布不均匀、容易发生应力腐蚀的问题,采用激光冲击强化对其进行处理,探究激光功率密度和冲击次数对表面残余应力状态的优化作用,并通过应力腐蚀试验验证优化效果。结果表明:随着功率密度增加,表面残余应力明显下降,但下降幅度逐渐减小,功率密度4.24GW/cm2与2.83GW/cm2冲击产生的残余应力相差不大,熔合区还存在残余拉应力,说明高功率密度不足以消除表面残余拉应力;随着冲击次数增加,残余拉应力显著降低,2.83GW/cm2冲击3次之后,残余拉应力完全消除,局部最高应力梯度从54.7 MPa/mm下降到11.7 MPa/mm,获得了高数值、分布均匀的残余压应力层。激光冲击强化后,焊接试样的应力腐蚀断裂时间提高了33.48%,激光冲击强化产生的残余压应力是其应力腐蚀抗性提高的重要原因。     

Effect of temperature on the dislocation structure of the ordered alloy Ni3(Fe,Cr)

Transmission electron microscopy is used to study the dislocation structure of ordered polycrystalline Ni₃(Fe, Cr) alloy after deformation at temperatures of 293, 473, 673, and 773°K. The flow stress σ is plotted as a function of the density of dislocations ρ. It is observed that there is a direct proportionality between σ and ρ^1/2, which indicates that the relation τ= αGbρ^1/2 is satisfied, where τ is the shear stress, G is the shear modulus, b is the Burgers vector, and α is a coefficient weakly dependent on the density of dislocations. The values of α are found for different deformation temperatures from the slope of the lines. It is found that α decreases with increasing deformation temperature. When the temperature is increased from 293 to 773°K the reduction in α is about 20% in agreement with estimates of the resistance to motion by superdislocations caused by nonconservative drag of dislocation jogs.     

质子辐照对纯铝薄膜微观结构的影响

利用透射电子显微镜(TEM)详细分析了不同剂量的质子辐照纯铝薄膜样品的微观结构, 质子的能量E=160 keV.实验表明,质子辐照能够在Al薄膜中诱发空位位错圈,在实验范围内,位错密度随辐照剂量的增加而增加;质子辐照在1×10¹¹—4×10¹¹/mm²范围内随辐照剂量的增加,位错圈数量密度以及位错圈尺寸都随之增加.在较高剂量6×10¹¹/mm²辐照下,位错圈数量密度减小,但其尺寸显著 关键词： 质子辐照 空位簇缺陷 位错圈 微观结构     

Does power ultrasound (26 kHz) affect the hydrogen evolution reaction (HER) on Pt polycrystalline electrode in a mild acidic electrolyte?

In this study, we investigated the effects of power ultrasound (26 kHz, up to ∼75 W/cm², up to 100% acoustic amplitude, ultrasonic horn) on the hydrogen evolution reaction (HER) on a platinum (Pt) polycrystalline disc electrode in 0.5 M H₂SO₄ by cyclic and linear sweep voltammetry at 298 K. We also studied the formation of molecular hydrogen (H₂) bubbles on a Pt wire in the absence and presence of power ultrasound using ultra-fast camera imaging. It was found that ultrasound significantly increases currents towards the HER i.e. a ∼250% increase in current density was achieved at maximum ultrasonic power. The potential at a current density of −10 mA/cm² under silent conditions was found to be −46 mV and decreased to −27 mV at 100% acoustic amplitude i.e. a ΔE shift of ∼+20 mV, indicating the influence of ultrasound on improving the HER activity. A nearly 100% increase in the exchange current density (j_o) and a 30% decrease in the Tafel slope (b) at maximum ultrasonic power, was observed in the low overpotential region, although in the high overpotential region, the Tafel slopes (b) were not significantly affected when compared to silent conditions. In our conditions, ultrasound did not greatly affect the “real” surface area (A_r) and roughness factor (R) i.e. the microscopic surface area available for electron transfer. Overall, it was found that ultrasound did not dramatically change the mechanism of HER but instead, increased currents at the Pt surface area through effective hydrogen bubble removal.     

A cobalt (II) complex with 6-methylpicolinate: Synthesis,characterization, second- and third-order nonlinear optical properties,and DFT calculations

A cobalt(II) complex of 6-methylpicolinic acid, [Co(6-Mepic)₂(H₂O)₂]·2H₂O, was prepared and fully determined by single crystal X-ray crystal structure analysis as well as FT-IR, FT-Raman. UV–vis spectra were recorded within different solvents, to illustrate electronic transitions and molecular charge transfer within complex 1. The coordination sphere of complex 1 is a distorted octahedron according to single crystal X-ray results. Moreover, DFT (density functional theory) calculations with HSEH1PBE/6-311 G(d,p) level were carried out to back up the experimental results, and form base for future work in advanced level. Hyperconjugative interactions, intramolecular charge transfer (ICT), molecular stability and bond strength were researched by the using natural bond orbital (NBO) analysis. X-ray and NBO analysis results demonsrate that O−H···O hydrogen bonds between the water molecules and carboxylate oxygen atoms form a 2D supramolecular network, and also adjacent 2D networks connected by C−H···π and π···π interactions to form a 3D supramolecular network. Additionally, the second− and third−order nonlinear optical parameters of complex 1 were computed at DFT/HSEH1PBE/6-311 G(d,p) level. The refractive index (n) was calculated by using the Lorentz−Lorenz equation in order to investigate polarization behavior of complex 1 in different solvent polarities. The first−order static hyperpolarizability (β) value is found to be lower than pNA value because of the inversion symmetry around Co (II). But the second−order static hyperpolarizability (γ) value is 2.45 times greater than pNA value (15×10⁻³⁰ esu). According to these results, Co(II) complex can be considered as a candidate to NLO material. Lastly molecular electrostatic potential (MEP), frontier molecular orbital energies and related molecular parameters for complex 1 were evaluated.     

晶圆键合和激光剥离工艺对GaN基垂直结构发光二极管芯片残余应力的影响

GaN基发光二极管(LED)中的残余应力状态对器件的性能和稳定性有很大影响. 通过使用三种不同的键合衬底(Al₂O₃衬底, CuW衬底和Si衬底)以及改变键合温度(290 ℃, 320 ℃, 350 ℃和380 ℃), 并且使用不同的激光能量密度(875, 945和1015 mJ·cm^-2) 进行激光剥离, 制备了不同应力状态的GaN基LED器件. 对不同条件下GaN LED进行弯曲度、Raman 散射谱测试. 实验结果表明, 垂直结构LED中的残余应力的状态是键合衬底和键合金属共同作用的结果, 而键合温度影响着垂直结构LED中的残余应力的大小. 激光剥离过程中, 一定能量密度下激光剥离工艺一般不会对芯片中的残余应力造成影响, 但是如果该工艺对GaN 层造成了微裂缝, 则会在一定程度上起到释放残余应力的作用. 使用Si衬底键合后, 外延蓝宝石衬底翘曲变大, 对应制备的GaN基垂直结构 LED中的残余应力为张应力, 并且随着键合温度的上升而变大; 而Al₂O₃和CuW衬底制备的LED中的残余应力为压应力, 但使用Al₂O₃衬底键合制备的LED中压应力随键合温度上升而一定程度变大, CuW 衬底制备的LED中压应力随键合温度上升而下降.     

Mechanism of formation of cellular dislocation structures during propagation of intense shock waves in crystals

The mechanism of formation of a cellular dislocation structure in face-centered cubic (fcc) metal crystals subjected to shock compression at strain rates \(\dot \varepsilon \) > 10⁶ s^?1 has been considered theoretically within the dislocation kinetic approach based on the kinetic equation for the dislocation density (dislocation constitutive equation). A dislocation structure of the cellular type is formed in the case of a two-wave structure of the compression wave behind its shock front (elastic precursor). It has been found that, at pressures σ > 10 GPa, the dislocation cell size Λ _c depends on the pressure σ and the density ρ _G of geometrically necessary dislocations generated at the shock front according to the relationship Λ _c ～ ρ _G ^?n ～ σ^?m , where n = 1/4–1/2, m = 3/4–3/2, and m = 1, for different pressures and orientations of the crystal. It has been shown that, in copper and nickel crystals with the shock loading axis oriented along the [001] direction, the cellular structure is not formed after reaching the critical pressures σ _c equal to 31 and 45 GPa, respectively.