纳米多孔金薄膜显微结构分析

 采用亚硫酸金钠为主盐,在阳极氧化铝模板上进行了化学镀和电镀金实验研究。通过扫描电子显微镜和X射线衍射分析测试表明:采用以上两种方法均能制备出纳米多孔金薄膜。两种方法制备的多孔金薄膜微观结构存在较大的差异。化学镀制备的多孔金薄膜微观上是枝晶状的,电镀制备的多孔金薄膜微观上由纳米线构成。     

Fabrication of microelectrodes deeply embedded in LiNbO3 using a femtosecond laser

We present a novel technique to fabricate deeply embedded microelectrodes in LiNbO₃ using femtosecond pulsed laser ablation and selective electroless plating. The fabrication process mainly consists of four steps, which are (1) micromachining of microgrooves on the surface of LiNbO₃ by femtosecond laser ablation; (2) formation of AgNO₃ films on substrates; (3) scanning the femtosecond laser beam in the fabricated microgrooves for modification of the inner surfaces; and (4) electroless copper plating. The void-free electroless copper plating is obtained with appropriate cross section of microgrooves and uniform initiation of the autocatalytic deposition on the inner surface of grooves. The dimension and shape of the microelectrodes could be accurately controlled by changing the conditions of femtosecond laser ablation, which in turn can control the distribution of electric field inside LiNbO₃ crystal for various applications, opening up a new approach to fabricate three-dimensional integrated electro-optic devices.     

Effect of nickel on the initial growth behavior of electroless Ni-Co-P alloy on silicon substrate

In this work the small amounts of NiSO₄ was added to a basic electroless plating bath of CoSO₄ with Na₂H₂PO₂ as reducing agent for the deposition of Co-Ni-P film on a silicon substrate. The initial growth behavior, containing plating rate, chemical composition, crystal structure, surface morphology and micro-structure, of the electroless plating film was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). The results showed that the growth morphology variation of the Co-Ni-P films deposited in the basic CoSO₄ + small amounts of NiSO₄ bath is the same as that of Co-P film deposited in the basic CoSO₄ bath, the plating rate of the Co-Ni-P film is much more rapid than that of the Co-P film, the Ni/Co wt.% in the Co-Ni-P film is greatly larger than that in the plating bath, and the structure of as-deposited film is crystalline at first stage and later stage.     

The pH effect on black spots in surface finish: Electroless nickel immersion gold

In order to understand the black spot generation after electroless nickel immersion gold (ENIG) plating, we investigated the pH effect with a combined approach of experiments and computer aided engineering (CAE). As the pH is increased in IG plating solution, the deprotonation of citric acid as chelating agent is enhanced to stabilize the solution by producing Ni-citrate complex ion. For the substitution reaction between nickel and gold, excess citrate ions (deprotonated citric acids) are adsorbed along nodal boundaries of Ni-P layer to decrease the surface reactivity. Since the low reactivity decreases the overall growth rate, the resulting homogeneous Au layer growth avoids the unfavorable galvanic cell corrosion to control black spot. Based on molecular orbital method and kinetic Monte Carlo calculation, our computational approach well explained the capability of citric acid as chelating agent and the Au growth rate along the nodal boundaries of Ni-P layer depending on the surface reactivity.     

Inhibition effect of self-assembled films formed by gold nanoparticles on iron surface

The self-assembled (SA) films formed by gold nanoparticles on iron surface had been proved to have inhibition effect for the substrate in 0.5 M H₂SO₄ solutions. The inhibition action was investigated using electrochemical impedance spectroscopy (EIS). The SA films formed by gold nanoparticles protected with sodium oleate had better corrosion protection to the iron substrate than only by sodium oleate. Scanning electron microscopy (SEM) was used to observe the imagines of the SA films. In addition, it was found that the gold nanoparticles could influence the nickel electroless plating films on the iron substrate. The structure and composition of the plating films were test by electron probe microanalyzer (EPMA). The mechanisms of the formation of the SA films and the nickel electroless plating reaction were also discussed.     

Growth behavior of electroless Ni-Co-P deposits on Fe

The electroless Ni-Co-P films were deposited on Fe film in plating baths using sodium hypophosphite as reducing agent and nickel and cobalt sulphates as ion source at pH value of 9 and plating temperature from 60 to 85 °C. The effect of the mol ratio of CoSO₄/CoSO₄ + NiSO₄ in plating bath on the growth behavior of electroless Ni-Co-P films was studied. The electroless Ni-Co-P films were characterized by transmission electron microscopy for the microstructure and thickness, and energy dispersive spectrometer for the composition. The results showed that the electroless Ni-Co-P films can be deposited on Fe films without the step of sensitization and activization; the surface of electroless Ni-Co-P film on Fe is quite even; the more the Co²⁺ ion in plating bath, the larger the activation energy and the smaller the plating rate of electroless Ni-Co-P films; and the mol ratio of Co/Co + Ni in film is larger than that in plating bath (with the exception of the film deposited in the bath with 0.9 mol ratio of CoSO₄/CoSO₄ + NiSO₄)     

Selective electroless nickel deposition on copper as a final barrier/bonding layer material for microelectronics applications

A low cost, selective electroless metallisation of integrated circuit (IC) copper bond pads with nickel and gold is demonstrated. This metallurgy can function as a barrier layer/bondable material when deposited as a thin layer or as the chip bump for flip chip applications when deposited to greater heights. Four alternative activation steps for selective electroless nickel deposition on bond pad copper are demonstrated. Selective low cost deposition has been achieved with a proprietary electroless plating bath developed at NMRC and three commercial baths on both sputtered copper substrates and electrolessly deposited copper on titanium nitride barrier layer material.     

ICF靶用泡沫铜的制备与表征

 以次磷酸钠为还原剂的化学镀进行导电化处理,研究了ICF靶用泡沫铜的电沉积工艺。采用扫描电子显微境和X射线衍射仪对制备过程中各阶段泡沫铜的微观结构进行了表征。结果表明：经化学镀后可获得晶粒尺寸小、分布均匀的铜沉积层。电沉积后铜沉积层主要由0.55 μm的小颗粒组成,并且出现突出大颗粒的形貌特征。在氢气氛围下,经700 ℃热处理后,铜颗粒进一步长大,沉积层结晶致密。制备的泡沫铜呈3维网络状结构,分布均匀,密度为0.19 g/cm³,孔径分布为400～600 μm,孔隙率达97.9％。     

Preparation of silver-coated glass frit and its application in silicon solar cells

A simple electroless plating process was employed to prepare silver-coated glass frits for solar cells. The surface of the glass frits was modified with polyvinyl-pyrrolidone(PVP) before the electroless plating process. Infrared(IR) spectroscopy,field emission scanning electron microscopy(FESEM), and x-ray diffraction(XRD) were used to characterize the PVP modified glass frits and investigate the mechanism of the modification process. It was found that the PVP molecules adsorbed on the glass frit surface and reduced the silver ions to the silver nanoparticles. Through epitaxial growth, these nanoparticles were uniformly deposited onto the surface of the glass frit. Silicon solar cells with this novel silver coating exhibited a photoelectric conversion efficiency increase of 0.33%. Compared with the electroless plating processes, this method provides a simple route to prepare silver-coated glass frits without introducing impurity ions.     

Fabrication of patterned gold microstructure by selective electroless plating

Patterned gold microstructures on glass or Si wafers have been fabricated by a novel method which is composed of selective electroless plating and microcontact printing. This process may be widely used for the production of fine metal patterns in printed circuits or as a substrate to form patterned SAMs. In addition, these patterned metal microstructures can be readily transferred to adhesive tape surface to fabricate flexible metal microstructure, which may be applied in all-plastic circuit.     

A novel process of electroless Ni-P plating with plasma electrolytic oxidation pretreatment

A novel Ni based coating - plasma electrolytic oxidation (PEO) pre-treatment followed by electroless nickel (EN) plating - has been developed to produce pore free Ni coatings on AZ91 magnesium alloy. The application of the PEO film between the nickel coating and the substrate acts as an effective barrier and catalytic layer for the subsequent nickel plating. The potentiodynamic tests indicated that the corrosion current density of the PEO + EN plating on AZ91 decreased by almost two orders of magnitudes compared to the traditional EN coating. Salt fog spray testing further proved this improvement. More importantly, the new technique does not use Cr⁺⁶ and HF in its pretreatment, therefore is a much environmentally friendlier process.     

Multiple activation of ion track etched polycarbonate for the electroless synthesis of metal nanotubes

In our study, we examined the formation of thin films of silver nanoparticles on polycarbonate and the influence of the silver loading on the electroless synthesis of metal nanotubes. Control of the silver film thickness occurred by consecutive dipping of the polymer template in tin(II) and silver(I) solutions. The deposition progress was studied using UV-Vis spectroscopy. The reaction mechanism relies on the adsorption of reactive ions on the polymer template as well as on the silver nanoparticles. The initial catalytic activity of silver-covered ion track etched polycarbonate is an important governing factor for the electroless synthesis of metal nanotubes with desired thickness and shape. Therefore, the presented method allows specific template preparation according to given synthetic demands. High aspect ratio copper, gold, and platinum nanotubes were produced by the combination of sufficiently activated templates with optimized electroless plating procedures.     

Microwire formation based on dielectrophoresis of electroless gold plated polystyrene microspheres

Microspheres coated with a perfectly conductive surface have many advantages in the applications of biosensors and micro-electromechanical systems.Polystyrene microspheres with the diameter of 10 μm were coated with a 50 nmthick gold layer using an electroless gold plating approach.Dielectrophoresis(DEP) for bare microspheres and shelled microspheres was theoretically analysed and the real part of the Clausius-Mossotti factor was calculated for the two kinds of microspheres.The experiments on the dielectrophoretic characterisation of the uncoated polystyrene microspheres and gold coated polystyrene microspheres(GCPMs) were carried out.Experimental results showed that the gold coated polystyrene microspheres were only acted by a positive dielectrophoretic force when the frequency was below 40M Hz,while the uncoated polystyrene microspheres were governed by a negative dielectrophoretic force in this frequency range.The gold coated polystyrene microspheres were exploited to form the microwire automatically according to their stable dielectrophoretic and electric characterisations.     

Qualitative electroless Ni/Au plating considerations for the solder mask on top of sequential build-up layers

Advanced printed circuit boards (PCBs) with sequential build-up (SBU) layers require alternating dielectric and copper layers on top of a core substrate. This can be achieved by lamination of resin coated copper (RCC) or by coating of dielectric polymers followed by copper deposition. The plating of electroless Ni/Au used as a solderability preservative on top of sequential build-up layers is investigated. For this application a solder mask polymer has to be applied in order to separate solder pads. Experiments showed that on parts of the underlying build-up layer exposed to the electroless Ni plating solution electroless Ni can grow. This overplating is caused by the remains of colloidal Pd/Sn catalyst on top of the build-up layer from preceding electroless Cu deposition. At very small features skipping of the plating can also take place. The overplating and skipping phenomena are influenced by a number of parameters, such as the temperature, the concentration of the stabilizer and pH. The dimensions of features on the board and the thickness of the solder-mask polymer also influence skipping. Based on qualitative analyses of the skipping and overplating phenomena rules of thumb for the solder mask design based on the plating conditions are proposed.     

石英光纤的金属镍锡涂敷工艺研究

为了实现石英光纤传感器的无胶金属化封装,需要在光纤表面涂敷金属层。先利用化学镀方法在石英光纤表面镀镍层,再利用电镀工艺电镀锡层,从而获得表面光亮、均匀、附着牢固、可焊性好的金属涂敷层。实验中研究了敏化、活化工艺对镀层的影响并提出一种效果较好的敏化活化方法。给出了石英光纤表面化学镀镍的最佳工艺条件。     

磁性ICF靶丸的化学镀工艺制备与表征

 采用化学镀工艺在ICF聚苯乙烯靶丸表面包覆了一层磁性的Ni-P合金镀层，并分别用扫描电子显微镜、能谱仪、X射线衍射仪以及振动样品磁强计对其形貌、组成、结构和磁性能进行了表征。结果表明：通过化学镀工艺制备的Ni-P合金镀层厚度约为4 μm，且为非晶结构，并具有一定的磁性；该磁性ICF靶丸可望用来进行磁悬浮实验研究。最后，对聚苯乙烯靶丸表面磁性涂层的制备机理进行了讨论。     

Preparation, characterization and microwave absorption properties of electroless Ni-Co-P-coated SiC powder

Silicon carbide particles reinforced nickel-cobalt-phosphorus matrix composite coatings were prepared by two-step electroless plating process (pre-treatment of sensitizing and subsequent plating) for the application to lightweight microwave absorbers, which were characterized by scanning electron microscopy (SEM), X-ray diffraction analysis (XRD), vibrating sample magnetometer (VSM) and vector network analyzer, respectively. The results show that Ni-Co-P deposits are uniform and mixture crystalline of α-Co and Ni₃P and exhibit low-specific saturation magnetization and low coercivity. Due to the conductive and ferromagnetic behavior of the Ni-Co thin films, high dielectric constant and magnetic loss can be obtained in the microwave frequencies. The maximum microwave loss of the composite powder less than −32 dB was found at the frequency of 6.30 GHz with a thickness of 2.5 mm when the initial atomic ratio of Ni-Co in the plating bath is 1.5.     

Field emission properties of carbon nanotube cathodes produced using composite plating

Field emission properties of carbon nanotube field emission cathodes (CNT-FECs) produced using composite plating are studied. The experiment uses a CNT suspension and electroless Ni plating bath to carry out composite plating. The CNTs were first purified by an acid solution, dispersed in a Ni electrobath, and finally co-deposited with Ni on glass substrates to synthesize electrically conductive films. Field emission scanning electron microscopy and Raman spectroscopy results show that the field emission characteristics and graphitic properties of CNT-FECs depend on the pH value of the electrobath. Experiments show that the optimum electrobath pH value is 5.4, achieving a field emission current density of 1.0 mA/cm² at an applied electric field of 1.5 V/μm. The proposed CNT-FECs possess good field emission characteristics and have potential for backlight unit application in liquid crystal displays.     

The effect of pH on synthesizing Ni-decorated MWCNTs and its application for Sn-58Bi solder

Nickel-decorated multi-walled carbon nanotubes (Ni-MWCNTs) were synthesized using a colloidal method and an electroless plating method to form Ni nanoparticles on the surface of MWCNTs. The Ni electroless plating process was optimized with solutions at various pH (5, 6, 7, and 8) levels. The Ni-MWCNTs fabricated at pH 7 show the most stable Ni nanoparticles on the surface of the MWNCTs. After optimization of the Ni plating process, the Ni-MWCNTs/Sn-58Bi composite solder were fabricated with varying contents of (0, 0.05, 0.1 and 0.2 wt%) Ni-MWCNTs. The experimental results show that Ni-MWCNTs enhance the mechanical properties of Sn-58Bi solder. The shear strength of Sn-58Bi solder improves by about 14% with 0.1 wt% Ni-MWCNTs. Furthermore, the microstructure evolution after a high temperature storage test shows that Ni-MWCNTs have an effect on grain refining and interrupt growth of the Intermetallic compound layer. The distribution of Ni-MWCNTs could be recognized with the results of EPMA.     

A plating method for metal coating of fiber Bragg grating

We present a method for metal coating optical fiber and in-fiber Bragg grating. The technology process which is based on electroless plating and electroplating method is described in detail. The fiber is firstly coated with a thin copper or nickel plate with electroless plating method. Then, a thicker nickel plate is coated on the surface of the conductive layer. Under the optimum conditions, the surfaces of chemical plating and electroplating coatings are all smooth and compact. There is no visible defect found in the cross-section. Using this two-step metallization method, the in-fiber Bragg grating can be well protected and its thermal sensitivity can be enhanced. After the metallization process, the fiber sensor is successfully embedded in the 42CrMo steel by brazing method. Thus a smart metal structure is achieved. The embedding results show that the plating method for metallization protection of in-fiber Bragg grating is effective.