Interface Reaction Between Electroless Ni–Sn–P Metallization and Lead-Free Sn–3.5Ag Solder with Suppressed Ni3P Formation

The voids formed in the Ni₃P layer during reaction between Sn-based solders and electroless Ni–P metallization is an important cause of rapid degradation of solder joint reliability. In this study, to suppress formation of the Ni₃P phase, an electrolessly plated Ni–Sn–P alloy (6–7 wt.% P and 19–21 wt.% Sn) was developed to replace Ni–P. The interfacial microstructure of electroless Ni–Sn–P/Sn–3.5Ag solder joints was investigated after reflow and solid-state aging. For comparison, the interfacial reaction in electroless Ni–P/Sn–3.5Ag solder joints under the same reflow and aging conditions was studied. It was found that the Ni–Sn–P metallization is consumed much more slowly than the Ni–P metallization during soldering. After prolonged reaction, no Ni₃P or voids are observed under SEM at the Ni–Sn–P/Sn–3.5Ag interface. Two main intermetallic compounds, Ni₃Sn₄ and Ni₁₃Sn₈P₃, are formed during the soldering reaction. The reason for Ni₃P phase suppression and the overall mechanisms of reaction at the Ni–Sn–P/Sn–3.5Ag interface are discussed.     

Acetylation of glycerol to synthesize bioadditives over niobic acid supported tungstophosphoric acid catalysts

Acetylation of glycerol to yield mono, di and triacetin (acetylated glycerol) was carried over niobic acid supported tungstophosphoric acid (TPA) catalysts. The catalysts with varying TPA content were prepared and characterized by different techniques. The characterization results reveal the presence of well-dispersed Keggin ion on support. The results suggest that the glycerol conversion and selectivities depend on the acidity of the catalysts, which in turn is related to the content of TPA on niobic acid. The change in conversion and selectivities during the acetylation also is attributed to the reaction time, catalyst concentration and glycerol to acetic acid molar ratio.     

Phase transformation behavior of nanocrystalline Ni-W-P alloys containing various W and P contents

In the present investigation, electroless (EL) ternary Ni-W-P coatings were prepared using hypophosphite based alkaline bath by varying sodium tungstate as tungsten source (5-80 g/L). Maximum amount of W incorporation (8.2 ± 1 wt.%) was obtained when the bath contained about 20 g/L of tungsten source. At very high concentrations of W source in the bath the deposit contained about 4 wt.% W and 2 wt.% P. All the as-deposited ternary coatings exhibited nodular surface morphology. X-ray diffractograms (XRD) obtained for as-deposited EL NiWP alloys indicated that crystallinity of the coatings increased with decrease in phosphorus content. Calculated grain size for the deposits varied from 1.2 to 12.7 nm when the tungsten source varied from 5 to 80 g/L in the bath. Higher crystallization temperatures were obtained due to W codeposition in NiP matrix. Presence of metastable phases such as Ni₅P₂ and NiP apart from stable Ni and Ni₃P was identified for the heat treated deposits (400 °C/1 h) containing lower amount of W and higher amount of P. Whereas other ternary deposits after the heat treatment predominantly revealed face centered cubic (f.c.c.) Ni (111) peak. Activation energy for the crystallization of all the alloys has been carried out by modified Kissinger method. Microhardness measurements were carried out on all the deposits isothermally heat treated at 600 °C for 1 h.     

Improvement in the properties of nickel by nano-Cr2O3 incorporation

Nano-ceramic composite coatings were prepared by the electrodeposition method using sulphamate electrolyte. Nickel was chosen as the metal matrix and nano-Cr₂O₃ particles were chosen as the reinforcement. The surface morphology and the particle distribution in the coating were analysed using field emission scanning electron microscope (FESEM). The particle content was obtained using energy dispersive X-ray analysis (EDAX). A change in the surface morphology of Ni was seen on the incorporation of Cr₂O₃ particles. The coatings were characterized for their structure and no change in the diffraction pattern was seen between plain Ni and Ni-Cr₂O₃ composite. The mechanical property like microhardness and tribological behaviour of the nano-composite coatings was studied and it was observed that the incorporation of Cr₂O₃ particles enhanced the mechanical properties of Ni matrix. The nano-composites were analysed for their thermal stability and corrosion resistance. An improvement in thermal stability was observed but no change in the corrosion behaviour of Ni was seen on the incorporation of nano chromium oxide particles.     

Selective Hydrogenolysis of Glycerol to 1, 2 Propanediol Over Cu–ZnO Catalysts

A series of Cu–ZnO catalysts with varying Cu to Zn weight ratio are prepared by co-precipitation method. The catalysts were characterized by surface area, XRD, TPR and N₂O chemisorption to measure Cu metal area. These catalysts were evaluated for hydrogenolysis of glycerol. The catalyst with Cu to Zn ratio of 50:50 is highly active under relatively low H₂ pressure. The catalysts are highly selective towards 1,2 propanediol (>93%). The glycerol conversion depends upon the bifunctional nature of catalyst where it requires both acidic sites and metal surface. The presence of sufficient amount with small particle size of ZnO and Cu are required for high conversion of glycerol and selectivity to 1,2 propanediol. Different reaction parameters are studied in order to optimize the reaction conditions.     

Nanocrystalline electroless nickel poly-alloy deposition: incorporation of W and Mo

Autocatalytic quaternary Ni–W–Mo–P films were prepared using alkaline citrate based baths and compared with binary Ni–P and ternary Ni–W–P, Ni–Mo–P coatings. Energy dispersive X-ray analysis showed that the binary Ni–P deposit contained 12·2 wt-%P. Codeposition of tungsten in Ni–P matrix resulted in ternary Ni–W–P with 4·1 wt-%P and 5·2 wt-%W. Incorporation of molybdenum led to a ternary Ni–Mo–P deposit containing 4·1 wt-%Mo and 11·2 wt-%P. Presence of both sodium tungstate and sodium molybdate in the basic bath resulted in a quaternary coating with 3·6 wt-%W, 6·7 wt-%Mo and 2·5 wt-%P. X-ray diffraction patterns of all the deposits revealed a single peak for Ni (1 1 1). The quaternary alloy exhibited a sharper peak showing the more crystalline nature of the deposit. Field emission scanning electron microscopy studies of the deposits showed the presence of smooth nodules for ternary deposits, but coarse and well defined nodules for quaternary deposits. Phase transformation behaviour of the ternary Ni–W–P deposit revealed a single exothermic peak at 440°C. However, ternary Ni–Mo–P deposit exhibited a split type high temperature peak at 397 and 461°C and the quaternary Ni–W–Mo–P deposit showed a single high temperature peak at 485°C. Microhardness measurements showed that the quaternary Ni–W–Mo–P deposit exhibited increased hardness of 920 HV(50 gf) when heat treated for 1 h at 400°C.     

Copolyperoxides of 2-(acetoacetoxy)ethyl methacrylate with methyl methacrylate and styrene; Synthesis,characterization, thermal analysis,and reactivity ratios

Copolyperoxides of 2-(acetoacetoxy)ethyl methacrylate (AEMA) with styrene (St) and methyl methacrylate (MMA) of different compositions have been synthesized in the presence of 2,2′-azobisisobutyronitrile as a free radical initiator under 100 psi oxygen pressure at 50 °C. The rates of oxidative copolymerization reactions are determined from the oxygen consumption (Δp) against time plot. Highly exothermic thermal degradations of these copolyperoxides are studied using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) and degradation products have been characterised by electron-impact mass spectroscopy (EI-MS). The NMR spectroscopy and EI-MS analysis confirm the alternating peroxy bonds in the main chain. The monomer reactivity ratios are computed by the Fineman–Ross and Kelen–Tüdös methods, using compositions obtained from ¹H and ¹³C NMR analysis. These copolymers can potentially be used as polymeric initiators for the radical polymerization of vinyl monomers, autocombustible fuel. Also, the β-carbonyl moieties along the side chain of the copolyperoxides can be utilized to prepare degradable polyperoxide–metal complexes.     

Effect of Surface Treatment on Bio-corrosion in Aluminum Alloy 2024-T3

Bio-corrosion is one of the major problems faced in any engineering/aerospace industry. The present study focuses on understanding the effect of surface treatment on AA2024-T3 on bio-corrosion in aircraft fuel tanks. The microbial attack on aluminum alloy (2024-T3) in aircraft fuel tanks by Pseudomonas aeruginosa was studied. Substrates with (1) chromate-free surface treatment (anodization; 2) Ormosil coatings doped with inhibitors/derivatives known for antimicrobial properties were evaluated for their bio-corrosion protection efficiency as compared to bare coupons. The coupons were immersed in aviation fuel spiked with the test culture. The changes in chemical parameters of test solution like pH were monitored periodically. A probable relationship between number of organisms, changes in pH and the extracellular protein (hypothesized to be produced by organisms) were evaluated. Our studies indicated that pH did not appear to play a crucial role in biofilm formation. Surface morphology of bare and anodized AA2024-T3 coupons before and after electrochemical impedance studies (EIS) was analyzed using FE-SEM. Anodized samples with least i_corr value of (0.075?×?10^?6 A cm^?2) and corrosion rate of (0.12?×?10^?2 mm/y) after 60 days showed distinct corrosion protection than bare and the coated samples. Additional evidence in support of corrosion protection efficiency of anodized was obtained by the biofilm barrier efficiency of 98.94%.     

Charge transport and photocurrent generation in PPAT:ZnO bulk heterojunction photovoltaic devices

In this paper, the blended systems composed of organic polymer and ZnO nano-particles were investigated through their optical and photo-electrochemical measurements for their potential applications in photovoltaic devices. The electrical and photoelectrical properties of the devices fabricated with the blend of poly (phenyl azo methane thiophene) (PPAT) and ZnO nano-particles sandwiched between ITO/PEDOT:PSS and metal electrode have been reported. Dependence of the performance this bulk heterojunction photovoltaic device on their composition has been investigated with respect to charge transport. We have observed that the electron mobility gradually increases on increasing ZnO concentration up to 60 wt.% and subsequently saturates to the bulk values. Similarly, the hole mobility in PPAT phase also shows an identical behavior and saturates beyond 50 wt.% ZnO, a value which is more than two orders of magnitude higher that that of the pure PPAT. The experimental electron and hole mobilities were used to study the photocurrent generation in PPAT:ZnO bulk heterojunction photovoltaic devices and discussed in detail. It is found that the device with 55 wt.% of ZnO in the blend shows maximum value of power conversion efficiency about 1.9%. The effect of controlled thermal annealing on the charge transport and generation of photocurrent in bulk heterojunction photovoltaic device made from blend film of PPAT:ZnO (55 wt.%) has also been studied with respect to the charge transport. It is concluded that the electron mobility dominates the charge transport of the device after thermal annealing. The hole mobility in PPAT phase of the blend is dramatically affected by thermal annealing. Additionally, upon thermal annealing the absorption spectrum of PPAT:ZnO blend under go a strong red shift, improving the spectral light harvesting, which results in an increase in the rate of charge carrier generation. The experimental results indicates that the most important factor leading to a strong enhancement of the efficiency, compared with non-annealed devices, is the increase in hole mobility in the PPAT phase of the blend and more light absorption by the blend.