Characterisation of products of tricalcium silicate hydration in the presence of heavy metals

The hydration of tricalcium silicate (C(3)S) in the presence of heavy metal is very important to cement-based solidification/stabilisation (s/s) of waste. In this work, tricalcium silicate pastes and aqueous suspensions doped with nitrate salts of Zn(2+), Pb(2+), Cu(2+) and Cr(3+) were examined at different ages by X-ray powder diffraction (XRD), thermal analysis (DTA/TG) and (29)Si solid-state magic angle spinning/nuclear magnetic resonance (MAS/NMR). It was found that heavy metal doping accelerated C(3)S hydration, even though Zn(2+) doping exhibited a severe retardation effect at an early period of time of C(3)S hydration. Heavy metals retarded the precipitation of portlandite due to the reduction of pH resulted from the hydrolysis of heavy metal ions during C(3)S hydration. The contents of portlandite in the control, Cr(3+)-doped, Cu(2+)-doped, Pb(2+)-doped and Zn(2+)-doped C(3)S pastes aged 28 days were 16.7, 5.5, 5.5, 5.5, and <0.7%, respectively. Heavy metals co-precipitated with calcium as double hydroxides such as (Ca(2)Cr(OH)(7).3H(2)O, Ca(2)(OH)(4)4Cu(OH)(2).2H(2)O and CaZn(2)(OH)(6).2H(2)O). These compounds were identified as crystalline phases in heavy metal doping C(3)S suspensions and amorphous phases in heavy metal doping C(3)S pastes. (29)Si NMR data confirmed that heavy metals promoted the polymerisation of C-S-H gel in 1-year-old of C(3)S pastes. The average numbers of Si in C-S-H gel for the Zn(2+)-doped, Cu(2+)-doped, Cr(3+)-doped, control, and Pb(2+)-doped C(3)S pastes were 5.86, 5.11, 3.66, 3.62, and 3.52. And the corresponding Ca/Si ratios were 1.36, 1.41, 1.56, 1.57 and 1.56, respectively. This study also revealed that the presence of heavy metal facilitated the formation of calcium carbonate during C(3)S hydration process in the presence of carbon dioxide.

Wetting and Reaction of Sn-2.8Ag-0.5Cu-1.0Bi Solder with Cu and Ni Substrates

The wettability of newly developed Sn-2.8Ag-0.5Cu-1.0Bi lead-free solder on Cu and Ni substrates was assessed through the wetting balance tests. The wettability assessment parameters such as contact angle (Ï‘c) and maximum wetting force (Fw) were documented for three solder bath temperatures with three commercial fluxes, namely, no-clean (NC), nonactivated (R), and water-soluble organic acid flux (WS). It was found that the lead-free Sn-2.8Ag-0.5Cu-1.0Bi solder exhibited less wetting force, i.e., poorer wettability, than the conventional Sn-37Pb solder for all flux types and solder bath temperatures. The wettability of Sn-2.8Ag-0.5Cu-1.0Bi lead-free solder on Cu substrate was much higher than that on Ni substrate. Nonwetting for Sn-2.8Ag-0.5Cu-1.0Bi and Sn-Pb solders on Ni substrate occurred when R-type flux was used. A model was built and simulations were performed for the wetting balance test. The simulation results were found very close to the experimental results. It was also observed that larger values of immersion depth resulted in a decrease of the wetting force and corresponding meniscus height, whereas the increase in substrate perimeter enhanced the wettability. The wetting reactions between the solder and Cu/Ni substrates were also investigated, and it was found that Cu atoms diffused into the solder through the intermetallic compounds (IMCs) much faster than did the Ni atoms. Rapid formation of IMCs inhibited the wettability of Sn-2.8Ag-0.5Cu-1.0Bi solder compared to the Sn-Pb solder.

Effect of adding 0.3 wt% Ni into the Sn–0.7 wt%Cu solder: part I: wetting behavior on Cu and Ni substrates

Comparative wetting behavior of Sn-0.7Cu and Sn-0.7Cu-0.3Ni solders on Cu and Ni substrates were assessed through the wetting balance test. No-clean (NC), non-activated (R) and water soluble organic acid (WS) fluxes were used to assess the wetting behavior for three different solder bath temperatures of 255, 275 and 295 °C. Experimental results unveiled that adding of 0.3 wt% Ni into Sn-0.7Cu solder can improve the wetting on Cu substrate when NC and WS fluxes are used. However, such addition of Ni did not improve the wetting of Sn-0.7Cu solder for R-type flux. In the case of Ni substrate, addition of Ni helped to improve the wetting for all three types of fluxes as higher wetting forces were documented for Sn-0.7Cu-0.3Ni solder compared to the Sn-0.7Cu solder. Among the fluxes, worst performance was observed for R-type flux. Very large contact angles were recorded for both solders with this kind of flux. Experimental results also revealed that higher solder bath temperature played an important role to lower the contact angle, to increase the wetting force and to enhance the wetting. Computer modeling of wetting balance test also revealed that both the wetting force and meniscus height are inversely proportional to the contact angles. Besides, solder bath depth and radius do not affect significantly on the wetting behavior.

Effect of adding 0.3wt% Ni into the Sn-0.7wt% Cu solder - Part II: Growth of intermetallic layer with Cu during wetting and aging

The growth behavior of intermetallic layer with or without adding 0.3 wt% Ni into the Sn-0.7Cu solder was studied during the wetting reaction on Cu-substrate and thereafter in solid-state aging condition. The Cu-solder reaction couple was prepared at 255, 275 and 295 °C for 10 s. The samples reacted at 255 °C were then isothermally aged for 2-14 days at 150 °C. The reaction species formed for the Sn-0.7Cu/Cu and Sn-0.7Cu-0.3Ni/Cu soldering systems were Cu6Sn5 and (CuNi)6Sn5, respectively. The thickness of the intermetallic compounds formed at the solder/Cu interfaces and also in the bulk of both solders increased with the increase of reaction temperature. It was found that Ni-containing Sn-0.7Cu solder exhibited lower growth of intermetallic layer during wetting and in the early stage of aging and eventually exceeded the intermetallic layer thickness of Sn-0.7Cu/Cu soldering system after 6 days of aging. As the aging time proceeds, a non-uniform intermetallic layer growth tendency was observed for the case of Sn-0.7Cu-0.3Ni solder. The growth behavior of intermetallic layer during aging for both solders followed the diffusion-controlled mechanism. The intermetallic layer growth rate constants for Sn-0.7Cu and Sn-0.7Cu-0.3Ni solders were calculated as 1.41 × 10-17 and 1.89 × 10-17 m2/s, respectively which indicated that adding 0.3 wt% Ni with Sn-0.7Cu solder contributed to the higher growth of intermetallic layer during aging. © 2006 Elsevier B.V. All rights reserved.

Study of the rheological behaviour of Sn-Ag-Cu solder pastes and their correlation with printing performance

Solder paste plays an important role in the electronic assembly process by providing electrical, mechanical and thermal bonding between the components and the substrate. The rheological characterisation of pastes is an important step in the design and development of new paste formulations. With the ever increasing trend of miniaturisation of electronic products, the study of the rheological properties of solder pastes is becoming an integral part in the R&D of new paste formulations and in the quality monitoring and control during paste manufacture and electronic assembly process. This research work outlines some of the novel techniques which can be successfully used to investigate the rheology of leadfree solder pastes. The report also presents the results of the correlation of rheological properties with solder paste printing performance. Four different solder paste samples (namely paste P1, P2, P3 and P4) with different flux vehicle systems and particle size distributions were investigated in the study. As expected, all the paste samples showed shear thinning behaviour. Although the samples displayed similar flow behaviour at high shear rates, differences were observed at low shear rates. In the stencil printing trials, round deposits showed better results than rectangular deposits in terms of paste heights and aperture filling. Our results demonstrate a good correlation between higher paste viscosity and good printing performance. The results of the oscillatory and thixotropy tests were also successfully correlated to the printing behaviour of solder paste.