硬质粒子扰动下铜电沉积研究

使用常规旋转电极电沉积技术,引入陶瓷球等一类硬质粒子,在旋转电极的带动下,使陶瓷球不断磨擦和撞击阴极表面而实现电铸铜.对比酸性溶液电铸铜和碱性溶液电铸铜,发现硬质粒子在电沉积过程中能扰动离子的放电过程,并影响电铸层的组织结构.但由于二者放电机理不同,前者形成的电铸层表面布满尖状毛刺,而后者则表面尖刺消失,但脆性大.SEM和XRD测试表明,由碱性电铸液沉积的电铸铜层,表面光亮平整,晶粒致密,大小约为100~300 nm,其结晶形态接近无序取向.     

Electroforming in the Industry 4.0 Era

In the Industry 4.0 Era, big data and automation will require precise knowledge that allows one to control, monitor and predict a process. Electroforming, which is the fabrication of free-standing components using electrodeposition, is rapidly gaining acceptance as a sustainable additive manufacturing technology. However, current knowledge of electroforming is based on empirical data, and academic engagement in this area has been limited. This article throws light on some of the complex issues surrounding the electrochemical and chemical behaviour during electroforming, which are yet unresolved. The differences between cathodic reactions in sulfamates and sulfates, ambiguities related to the role of boric acid and paucity of data on anode reactions are highlighted.     

纳米颗粒增强镍基MEMS器件材料的蠕变性能研究

利用同步辐射LIGA微铸复合工艺,将纳米氧化物增强颗粒复合到微电子机械系统(MEMS)结构材料中。制作了专用夹具,采用微力材料试验机测量了纳米Al2O3颗粒增强镍基复合材料的强度为1GPa;将恒加载速率/载荷法和恒载荷法相结合,利用纳米压痕仪测量了该材料的室温蠕变速率敏感指数m。结果表明,LIGA复合技术得到的纳米颗粒增强镍基复合材料具有较高的强度;MEMS器件材料在室温下会发生蠕变;材料在相同压深下最大载荷不随加载速率而改变,加载段粘弹性和粘塑性变形极少;主要由局部高应力导致压痕蠕变;材料的蠕变速率敏感指数m值为0.004,说明纳米Al2O3颗粒可有效增强基体材料的抗蠕变能力;且不同恒.P/P下获得的m值基本相同,表示此种材料对加载速率不敏感。     

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.     

Scaling up the fabrication of wafer-scale Ni-MoS2/WS2 nanocomposite moulds using novel intermittent ultrasonic-assisted dual-bath micro-electroforming

In the scale-up fabrication process for electroformed Ni-MoS₂/WS₂ composite moulds, the formulation of nanosheets is critical, since the size, charge, and their distribution can largely affect the hardness, surface morphology and tribological properties of the moulds. Additionally, the long-term dispersion of hydrophobic MoS₂/WS₂ nanosheets in a nickel sulphamate solution is problematic. In this work, we studied the effect of ultrasonic power, processing time, surfactant types and concentrations on the properties of nanosheets to elaborate their dispersion mechanism and control their size and surface charge in divalent nickel electrolyte. The formulation of MoS₂/WS₂ nanosheets was optimized for effective electrodeposition along with nickel ions. A novel strategy of intermittent ultrasonication in the dual bath was proposed to resolve the problem of long-term dispersion, overheating, and deterioration of 2D material deposition under direct ultrasonication. Such strategy was then validated by electroforming 4-inch wafer-scale Ni-MoS₂/WS₂ nanocomposite moulds. The results indicated that the 2D materials were successfully co-deposited into composite moulds without any defects, along with the mould microhardness increasing by ∼2.8 times, the coefficient of friction reducing by two times against polymer materials, and the tool life increasing up to 8 times. This novel strategy will contribute to the industrial manufacturing of 2D material nanocomposites under ultrasonication process.     

Synthesis and morphological investigation of pulsed current formed nano-structured lead dioxide

An electro-forming method was used for the preparation of nano-structured lead dioxide on lead substrate in 4.8 M H₂SO₄. A two electrode system composed of two similarly prepared lead electrodes was employed. A constant current was applied between two electrodes for a short time, followed by a relaxation period. A dark oxidation film of suitable stability and homogeneity was formed on the anode electrode. Different parameters including pulse height, pulse time (t_on) and relaxation time (t_off) were optimized. A change in morphology of lead dioxide from globular to nanofibriliar was observed when the pulse time and relaxation time varied from 0.01 to 10 and 0.1 to 5 s, respectively, at a pulse height of 25 mA cm⁻². A variation in pulse height caused a variation in diameter and length of nanofibers formed at a pulsed time of 0.1 s and relaxation time of 5 s. The scanning electron microscopy (SEM) showed that lead dioxide particles obtained under these conditions have nanofibriliar morphology with an average diameter in the range between 20 and 50 nm and length of 500–1000 nm.