Performance and reliability of Al2O3 nanoparticles doped multicomponent Sn-3.0Ag-0.5Cu-Ni-Ge solder alloy

https://doi.org/10.1016/j.microrel.2020.113933Get rights and content

Highlights

  • The presence of nanoparticles, Ni and Ge refined the solder microstructure.

  • Ni-P coating significantly retarded the IMC growth at the joint interface.

  • Ni-P coating improved the thermal stability and mechanical integrity of the joint.

  • Nanocomposites and Ni-P coating substantially improved the joint reliability.

Abstract

The effect of Al2O3 nanoparticles addition on melting, microhardness, microstructural, and mechanical properties of multicomponent Sn-3Ag-0.5Cu-0.06Ni-0.01Ge (SACNiGe) solder alloy was investigated. The shear strength of the capacitor assemblies under varying high-temperature environments for different nanocomposites was assessed and the reliability of the joint was determined using Weibull analysis. The SACNiGe solder doped with 0.01 and 0.05 wt% Al2O3 nanoparticles to prepare nanocomposites and tested on the solder joints for their performance and reliability under different thermal conditions. Plain copper and Nisingle bondP layer coated substrates were used to investigate the effect of different surface finish on the joint reliability. The addition of ceramic nanoparticles in small amounts did not affect the melting parameters of the solder. In comparison with the bare solder alloy, nanocomposites yielded about 20% increase in tin-climb height and 14% higher microhardness. The dispersion of ceramic nanoparticles in the matrix and presence of Ni and Ge elements in the solder resulted in substantial microstructure refinement and about 24% supression in intermetallic compounds (IMCs) growth at the joint interface. In comparison with the bare Cu substrate, the Nisingle bondP coating on the substrate provided a strong diffusion barrier, promoted thin and complex (Cu, Ni)6Sn5 IMC layer formation at the interface, and significantly retarded the IMC growth kinetics under elevated temperature conditions. Under varying thermal conditions, nanoparticles doped solder compositions showed about 20% increase in the joint shear strength value. The reliability of joints improved appreciably with the addition of 0.05 wt% Al2O3 nanoparticles in the solder. Samples with SACNiGe+0.05Al2O3 nanocomposite reflowed on Nisingle bondP coating showed about 32% higher reliability than that on the uncoated-copper substrate. The SACNiGe solder joint performance and reliability could be significantly improved by minor weight percent addition of Al2O3 nanoparticles in the presence of Nisingle bondP coating on the substrate.

Introduction

The high functional compact devices need highly reliable electronic assembly. The integrity and reliability of the electronic assemblies under different working atmospheres largely depends on the quality and stable bonding of the solder joint [[1], [2], [3]]. A thin and uniform intermetallic compound (IMC) layer at the joint interface provides an essential electrical continuity, thermal support, and mechanical integrity to the attached components in the assembly. The electronic components repeatedly exposed to different thermal and mechanical stresses during their complete service life. Prolonged exposure of joint to the high-temperature environments accelerates interfacial IMC growth and coarsen the secondary IMC precipitates as well as β-Sn grains in the solder matrix. The excessive IMC growth is detrimental to the joint strength due to its inherent brittle nature and strong tendency to develop structural defects like Kirkendall voids and micro-cracks [[4], [5], [6], [7]].

Several environmental-friendly Sn-based alloys such as Sn-3.0Ag-0.5Cu, Sn-14Bi-5In, Sn-0.7Cu, Snsingle bond9Zn Sn-8Zn-3Bi, and Snsingle bond58Bi have been considered the most promising candidates to replace the toxic Snsingle bondPb alloy from electronic packaging systems [8]. Among them, the Sn-Ag-Cu (SAC) solder alloys are the most preferred lead-free solders for the replacement of conventional Snsingle bondPb solders in the electronics industry due to their good solderability and adequate mechanical strength [9]. Especially high-silver bearing SAC alloys are mostly used in electronic applications due to their better physical, thermal and mechanical properties. However, high melting temperatures (i.e. 217–221 °C) and high tin (Sn) content compared to Snsingle bondPb solders give rise to problems like high IMC growth velocity, high Cu dissolution from the substrate and IMC overgrowth [4,6,10]. The high silver content in solder promotes coarsening of Ag3Sn IMC particles in the solder bulk, which increases the brittleness of the joint, deteriorates its drop-impact strength and other mechanical properties under high-temperature working conditions. Studies showed that the addition of a small amount of nickel (Ni) in solder contributes to microstructure refinement and helps in forming a more stable Cu6Sn5 intermetallic (IMC) layer at the joint interface. Nickel also inhibits the cracking of Cu6Sn5 IMC layer as well as corrosion of Cu substrate on the circuit board [11,12]. The addition of a small fraction of germanium (Ge) in SAC solder acts as an antioxidant, which reduces the oxidation, improves the wettability, and prevents the bridging formation during soldering [13,14]. In the case of exposure of molten solder to the open environment, oxygen may cause oxide product formation and an increase in the dissolution rate of Cu. However, the presence of Ge in solder prevents the dissolution of Cu by preferentially reacting with oxygen [3,15]. The SnAgCu-NiGe solder is expected to be an advanced super lead-free solder. The presence of Ni and Ge in small weight percent improves the thermal stability and reliability of the solder joints under high-temperature working environments [16,17].

A lot of research work shows that the addition of second-phase particles and micro-alloying effectively improves the thermal, electrical, physical, and mechanical properties of the solder alloy. The addition of various materials like Ag, In, Ni, Al, Co, etc. and ceramic particles e.g., TiO2, Al2O3, ZrO2, and Ce2O3, etc. [[18], [19], [20], [21], [22], [23]], graphene, carbon nanotubes, and alloying with different metal particles being tested to improve the electrical, microstructural and mechanical properties of the solder [[24], [25], [26], [27], [28], [29], [30]]. The addition of nanoparticles in the solder has been proved to be an effective way to enhance the mechanical properties of the solder. The smaller size and high surface energy of the nanoparticles help in microstructure refinement and mechanical strengthening of the solder [24,31]. Studies showed that Al2O3 ceramic nanoparticle reinforcement results in enhanced wettability, suppression of the IMC layer, improvement in shear strength, and microhardness of the solder [24,32]. The TiO2 nanoparticles doped SAC305 solder nanocomposites showed a significant reduction in Ag3Sn IMC particle size and enhanced its distribution in the matrix. The microhardness and tensile strength were improved with nanoparticle reinforcement in the solder [33]. The minor weight percent addition of nano-SiO2 particles in SAC305 solder showed substantial improvement in the solder wettability and shear force of the joint. The nano-SiO2 particles help in microstructure refinement and suppression of IMCs at the joint interface [34]. The low-silver Sn-0.3Ag-0.7Cu solder doped with a small amount of α-Al2O3 nanoparticles showed significant improvement in solder wettability and shear force compared to plain solder. The doping of solder with a trace amount of nanoparticles substantially refined the solder microstructure and suppressed the Cu6Sn5 IMC growth rate. The nanocomposite displayed stronger corrosion resistance and higher joint reliability under high-temperature conditions compared to the plain solder [35,36]. Studies done by Liang et al. [16] showed the significant refinement in the solder microstructure and retardation in IMC growth with the addition of rare earth metals and ceramic nanoparticles in solder, which leads to the enhancement in the mechanical properties of the solder.

Studies suggest that along with the use of a high performing solder, the development of a reliable substrate for the electronics component in assembly is crucial for industrial application [[37], [38], [39], [40]]. The conventional copper metallization falls short as a reliable substrate for lead-free solders application. The high Cu depletion and rapid IMC growth on Cu substrate restrict its widespread usage in electronics assembly where high reliability of the joints is a deciding factor over the cost. The high IMC growth kinetics often leads to the development of micro-voids at the IMC interface and the excessive IMC thickness is more susceptible to the micro-cracks formation, which considerably deteriorates the joint reliability [[41], [42], [43]]. Electroless nickel-phosphorous (Nisingle bondP) coating is often used as a diffusion barrier, to impede the diffusion of Sn at the joint interface. Low deposition cost, consistency, corrosion resistance, excellent solderability, and simplicity of the deposition process, makes the Nisingle bondP coating on Cu substrate viable [38,39,44]. However, the phosphorus content in Nisingle bondP finish leads to a problem of the formation of phosphorus-rich layers (Ni3P and Ni-Sn-P) at the interface alongside the Snsingle bondCu and Nisingle bondSn IMCs. The extremely brittle P-rich layers lead to the spalling of IMCs at the interface, which causes the brittle fracture of the solder joint [38,40,45]. However, studies suggest that the presence of Cu in the solder inhibits the formation of Ni3P layer and significantly hider its growth by preferentially forming a Cusingle bondSn intermetallic layer over the substrate [46,47]. The diffusion barrier offered by the Cusingle bondSn IMC layer slows down the Ni out-diffusion to form complex Cu-Ni-Sn IMC at the interface, which arrests the IMC spalling. It is observed that improvement in reliability of the solder joint reflowed on Nisingle bondP coated substrate was more prominent for lead-free solders containing copper than copper-less solders [48].

The previous studies insist on minor weight percent addition of ceramic nanoparticles to enhance the solder properties. The high concentration addition of nanoparticles can lead to a significant deterioration in the physical and mechanical properties of the solder. The microstructural, thermal, and mechanical properties of the solder were improved with the addition of ceramic nanoparticles in minor weight percent [31,49,50]. The purpose of this study is to investigate the effect of Al2O3 ceramic nanoparticles addition on microstructure development, IMC growth, joint shear strength, and reliability of multicomponent Sn-Ag-Cu-Ni-Ge solder alloy under different thermal conditions. The additional benefits of ceramic nanoparticles reinforcement in grain refinement, IMC suppression, and dispersion strengthening of the solder were explored in this study. The nanocomposites were tested on plain Cu and Nisingle bondP coating as a substrate to assess the effect of different surface finish on the reliability of the solder joint. Our previous studies [[51], [52], [53], [54]] on development of high-silver (SAC305) and low-silver (SAC0307) content solder alloys with the addition of nanoparticles like Al2O3 and MWCNT showed that addition of nanoparticles in the range of 0.01–0.05 wt% brings out the maximum beneficial effects in physical, thermal and mechanical properties of the solder. It is also observed that samples reflowed for two reflow cycles yield optimal mechanical strength irrespective of the solder composition. Based on results from these studies, only minor weight percent (i.e. 0.01 and 0.05 wt%) addition of Al2O3 nanoparticles in SACNiGe solder were considered for the present investigation and samples were subjected to only two reflow cycles.

Section snippets

Preparation of nanocomposites of SACNiGe solder and solder joint assemblies

Procured Al2O3 nanoparticles (20–30 nm dia.) were first cleaned for impurities with 38% concentrate HCl acid bath. Cleaned nanoparticles were treated with a surfactant coating process [55] before the blending with commercial Sn-3.0Ag-0.5Cu-0.06Ni-0.01Ge solder paste; hereafter called as SACNiGe solder. The complete elemental composition of the SACNiGe solder alloy used in this study is presented in Table 1. One part of Polyvinylpyrrolidone (PVP-10) surfactant was mixed with five parts of

DSC analysis and wettability assessment of nanocomposites

The DSC curves for different nanocomposites of SACNiGe solder obtained from the endothermic and exothermic reactions are shown in Fig. 6. The onset and peak melting temperature for monolithic SACNiGe solder were obtained at 217.92 °C and 222.55 °C, respectively. The difference in onset and peak melting temperatures indicates the melting range of the solder. The different melting parameters for SACNiGe nanocomposites obtained from the DSC analysis are tabulated in Table 2. The doping of SACNiGe

Melting and wetting behaviour of nanocomposites

Generally, the melting temperature of an alloy reduces on the addition of any second-phase particles. The addition of nanoparticles in solder reduced the surface tension of the solder-melt, which leads to lowering its melting temperature. The nanoparticles reinforcement in 0.01 and 0.05 wt% slightly reduced the melting parameters of the SACNiGe solder. The marginal reduction in the undercooling of the nanocomposites reflects the growth in the nucleation sites in the solder-melt during

Conclusion

The influence of Al2O3 nanoparticles reinforcement and Nisingle bondP coating on the performance and reliability of the Sn-3Ag-0.5Cu-0.06Ni-0.01Ge solder joint was studied. The ceramic nanoparticles addition in minor weight percent enhanced the wettability, microhardness and shear strength of the solder joint. The dispersion of nanoparticles and the presence of Ni and Ge elements in the solder refined the joint microstructure and inhibited the interfacial IMC growth under high-temperature environments.

CRediT authorship contribution statement

Sanjay Tikale: Conceptualization, Methodology, Experimentation, Investigation, Formal analysis, Data curation, Writing- Original draft preparation. K. Narayan Prabhu: Supervision, Conceptualization, Investigation, Validation, Writing- Reviewing and Editing.

Declaration of competing interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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