Internal Microstructure Investigation of Tin Whisker Growth Using FIB Technology

The problem of tin (Sn) whiskers has been a significant reliability issue in electronics for the past several decades. Despite the large amount of research conducted on this issue, a solution for mitigating the growth of whiskers remains a challenge for the research community. Whiskers have unpredictable growth and morphology, and a study of a whisker??s internal structure may provide further insights into the reason behind their complex growth. This study reports on the internal microstructure and morphology of complex-shaped Sn whiskers grown from an electroplated bright Sn layer on brass substrates exposed to ambient and 95% humid environment. The variables analyzed include surface and microstructure conditions of the film, and morphology and internal microstructure of the Sn whiskers using scanning electron microscopy with focused ion beam technology. Experimental results demonstrated that the whiskers with more complex morphology grow primarily from surfaces exposed to a controlled environment, and some of them have traits of polycrystalline growth rather than only single crystalline, as usually known.     

Tensile Behavior of Single-Crystal Tin Whiskers

The growth of metallic (predominantly Sn) whiskers from pure metallic platings has been studied for over 50 years. While the phenomenon of Sn whiskering has been studied for decades, very little is known about the mechanical properties of these materials. This can be attributed to the difficulty in handling, gripping, and testing such fine-diameter and high-aspect-ratio whiskers. We report on the stress–strain behavior of Sn whiskers inside a dual-beam focused ion beam (FIB) with a scanning electron microscope (SEM). Lift-out of the whiskers was conducted in situ in the FIB, and the whiskers were tested using a microelectromechanical system tensile testing stage. Using this technique, the whiskers had minimum exposure to ambient air and were not handled by hand. SEM images after fracture enabled reliable calculation of the whisker cross-sectional area. Tests on two different whiskers revealed relatively high tensile strengths of 720 MPa and 880 MPa, respectively, and a limited strain to failure of ～2% to 3%. For both whiskers, the Young’s modulus was between 42 GPa and 45 GPa. It is interesting to note that the whiskers were quite strong and had limited ductility. These findings are intriguing and provide a basis for further work to understand the effect of Sn whisker mechanical properties on short circuits in electronics.     

Tin Whisker Growth Induced by High Electron Current Density

The effect of electric current on the tin whisker growth on Sn stripes was studied. The Sn stripes, 1 μm in thickness, were patterned on silicon wafers. The design of the Sn stripes allowed the simultaneous study of the effect of current crowding and current density. Current stressing was performed in ovens set at 30, 50, or 70°C, and the current density used ranged from 4.5 × 10⁴ A/cm² to 3.6 × 10⁵ A/cm². It was found that the stress induced by the electric current caused the formation of many Sn whiskers. A higher current density caused more Sn whiskers to form. Of the three temperatures studied, 50°C was the most favorable one for the formation of the Sn whiskers. In addition, the current-crowding effect also influenced whisker growth.     

Mitigative Tin Whisker Growth Under Mechanically Applied Tensile Stress

Sn whisker/hillock growth is a result of the release of compressive stress in a Sn thin film. Filamentary Sn whiskers were formed on an electrodeposited Sn thin film aged at room temperature, while Sn hillocks were formed as the aging temperature was raised to 80°C and 150°C. By mechanically applying a tensile stress on the Sn thin film, the growth of the Sn whisker/hillock was significantly mitigated. This mitigation growth suggests that part of the compressive stress in the Sn thin film was neutralized by the mechanically applied tensile stress.     

Mitigation and Verification Methods for Sn Whisker Growth in Pb-Free Automotive Electronics

This work describes mitigation methods against Sn whisker growth in Pb-free automotive electronics using a conformal coating technique, with an additional focus on determining an effective whisker assessment method. We suggest effective whisker growth conditions that involve temperature cycling and two types of storage conditions (high-temperature/humidity storage and ambient storage), and analyze whisker growth mechanisms. In determining an efficient mitigation method against whisker growth, surface finish and conformal coating have been validated as effective means. In our experiments, the surface finish of components comprised Ni/Sn, Ni/SnBi, and Ni/Pd. The effects of acrylic silicone, and rubber coating of components were compared with uncoated performance under high-temperature/humidity storage conditions. An effective whisker assessment method during temperature cycling and under various storage conditions (high temperature/humidity and ambient) is indicated for evaluating whisker growth. Although components were finished with Ni/Pd, we found that whiskers were generated at solder joints and that conformal coating is a useful mitigation method in this regard. Although whiskers penetrated most conformal coating materials (acrylic, silicone, and rubber) after 3500 h of high-temperature/humidity storage, the whisker length was markedly reduced due to the conformal coatings, with silicone providing superior mitigation over acrylic and rubber.     

Effect of Crystal Orientation on Mechanically Induced Sn Whiskers on Sn-Cu Plating

Mechanically induced Sn whiskers formed on Sn-2%Cu plated on Cu with Ni underplating were examined by scanning electron microscopy and electron backscatter diffraction. The results revealed that Sn grains became larger under mechanical stress due to recrystallization and/or grain growth. The notable feature was formation of many twin interfaces. Most twin boundaries were {301}, and there were approximately 20 times more {301} twin boundaries compared with the as-deposited plating. The analysis clearly revealed that many whiskers nucleated from newly formed {301} twinned grains, which formed on columnar grains. Thus, twin formation plays a critical role in mechanically induced formation of whiskers.     

Optimum Thickness of Sn Film for Whisker Growth

By depositing different thicknesses of Sn films over a silicon wafer precoated with Cr and Ni adhesion layers and then by bending the tinned wafer using a dead load applied at the center to introduce the same compressive stresses in the Sn films, the growth rate of whiskers appeared to have a maximum for a certain thickness. This is explained by assuming the Sn atoms to flow along the vertical grain boundaries (perpendicular to the interface) into the interface between Sn and Ni and then along the interface to the root of the whisker through some more vertical grain boundaries. The resistance along the vertical grain boundaries appeared to control the rate of whisker growth for thick films.     

挠性电路板引脚嵌合部无铅镀层的锡须生长

以民用挠性印制电路板(FPC)引脚和连接器嵌合部无铅镀层为对象,通过研究引脚上的Ni/Sn无铅镀层的显微形貌和锡须尺寸,探讨了Ni/Sn无铅镀层的长期可靠性。结果表明,在25℃,RH为45%～55%的条件下,挠性印制电路板引脚和连接器嵌合部无铅镀层上生长的锡须呈现针状、柱状等多种不同的显微形貌,其中大部分是针状锡须,少量针状锡须的长度已超过了50μm临界值,很可能因锡须桥接引起电流泄漏和短路,对FPC互连可靠性产生威胁。抑制少量超长的针状晶须的生长,是防止风险的关键。     

The Role of Silver in Mitigation of Whisker Formation on Thin Tin Films

The mitigating effect of alloying Sn thin films with Ag on the formation of Sn whiskers was investigated by time-resolved investigations employing x-ray diffraction for phase and stress analyses and focused ion beam microscopy for morphological characterization of the surfaces and cross-sections of the specimens. The investigated Sn-6 wt.%Ag thin films were prepared by galvanic co-deposition. The results are compared with those obtained from investigation of pure Sn films and discussed with regard to current whisker-growth models. The simultaneous deposition of Sn and Ag leads to a fine-grained microstructure consisting of columnar and equiaxed grains, i.e. an imperfect columnar Sn film microstructure. Isolated Ag3Sn grains are present at the Sn grain boundaries in the as-deposited films. Pronounced grain growth was observed during aging at room temperature, which provides a global stress relaxation mechanism that prevents Sn whisker growth.     

Microstructure-Based Stress Modeling of Tin Whisker Growth

A 3-D finite element method (FEM) model considering the elasticity anisotropy, thermal expansion anisotropy, and plasticity of beta-Sn is established. The Voronoi diagrams are used to generate the geometric patterns of grains of the Sn coating on Cu leadframes. The crystal orientations are assigned to the Sn grains in the model using the X-ray diffraction (XRD) measurement data of the samples. The model is applied to the Sn-plated package leads under thermal cycling tests. The strain energy density (SED) is calculated for each grain. It is observed that the samples with higher calculated SED are more likely to have longer Sn whiskers and higher whisker density. The FEM model, combined with the XRD measurement of the Sn finish, can be used as an effective indicator of the Sn whisker propensity. This may expedite the qualification process significantly     

Investigation of Sn Whisker Growth in Electroplated Sn and Sn-Ag as a Function of Plating Variables and Storage Conditions

Sn whiskers are becoming a serious reliability issue in Pb-free electronic packaging applications. Among the numerous Sn whisker mitigation strategies, minor alloying additions to Sn have been proven effective. In this study, several commercial Sn and Sn-Ag baths of low-whisker formulations are evaluated to develop optimum mitigation strategies for electroplated Sn and Sn-Ag. The effects of plating variables and storage conditions, including plating thickness and current density, on Sn whisker growth are investigated for matte Sn, matte Sn-Ag, and bright Sn-Ag electroplated on a Si substrate. Two different storage conditions are applied: an ambient condition (30°C, dry air) and a high-temperature/high-humidity condition (55°C, 85% relative humidity). Scanning electron microscopy is employed to record the Sn whisker growth history of each sample up to 4000 h. Transmission electron microscopy, x-ray diffraction, and focused ion beam techniques are used to understand the microstructure, the formation of intermetallic compounds (IMCs), oxidation, the Sn whisker growth mechanism, and other features. In this study, it is found that whiskers are observed only under ambient conditions for both thin and thick samples regardless of the current density variations for matte Sn. However, whiskers are not observed on Sn-Ag-plated surfaces due to the equiaxed grains and fine Ag₃Sn IMCs located at grain boundaries. In addition, Sn whiskers can be suppressed under the high-temperature/high-humidity conditions due to the random growth of IMCs and the formation of thick oxide layers.     

Sn whisker evaluations in 3D microbumped structures

Sn whiskering remains a reliability concern in electronic applications. Despite extensive research on growth rates and mitigation strategies, no predictive theory is in place. Literature data are available for Cu/Sn-based films and coatings as well as for board-level and flip-chip solder bumps but data are scarce for scaled-down solder volumes and for higher intermetallic-to-solder ratios. The current work investigates whiskers in “isolated geometries” for 3D solder-capped Cu microbumps with >2 orders of magnitude smaller solder volumes compared to state-of-the-art. To the best of the authors’ knowledge, this is the first time Sn whisker growth is reported in isolated solder volumes (e.g. <8 μm-side cube). Whiskers propensity was evaluated using JEDEC industrial specifications. The tested structures were: 5/3.5 μm-thick Cu/Sn films and 15 μm-diameter electroplated solder capping (Sn, SnAg, SnCu) on Cu microbumps (as-plated vs. reflowed). Selected Sn whiskers and “whisker-like” features were analysed and identified experimentally with SEM, EDX and FIB. In the absence of a predictive model, first-order and “what if” calculations based on IMC molar volume and oxide cracking hypotheses were carried out. This approach quantifies “figures of merit” for Sn whisker propensity with (1) different bump-limiting metallization (BLM) cases e.g. Cu, Ni, Co and (2) further microbump scaling. Future research recommendations are outlined to mitigate manufacturing risks by controlling “sit time” between bumping and stacking.     

Hillock and Whisker Growth on Sn and SnCu Electrodeposits on a Substrate Not Forming Interfacial Intermetallic Compounds

Intermetallic compound (IMC) formation at the interface between the tin (Sn) plating and the copper (Cu) substrate of electronic components has been thought to produce compressive stress in Sn electrodeposits and cause the growth of Sn whiskers. To determine if interfacial IMC is a requirement for whisker growth, bright Sn and a Sn-Cu alloy were electroplated on a tungsten (W) substrate that does not form interfacial IMC with the Sn or Cu. At room temperature, conical Sn hillocks grew on the pure Sn deposits and Sn whiskers grew from the Sn-Cu alloy electrodeposits. These results demonstrate that interfacial IMC is not required for initial whisker growth.     

SnAgCuY钎料表面Sn晶须的旋转生长现象

研究了Sn3.8Ag0.7Cu1.0Y钎料表层上YSn3稀土相表面Sn晶须的生长行为。结果表明:室温时效条件下在YSn3的表面会出现Sn晶须的快速生长现象,生长速度最快可达10–10m/s,长度最长可达200μm。YSn3稀土相氧化的不均匀性是导致Sn晶须在生长时产生各种旋转现象的主要原因。     

Rapid method for testing efficacy of nano-engineered coatings for mitigating tin whisker growth

The risk of failure of electronic components due to tin (Sn) whiskers growth has become an issue with the current regulations limiting the use of lead in Sn solders. New strategies using engineered coatings for mitigating Sn whiskers are being developed. Typically, these coatings are evaluated by an aging process where whiskers are allowed to grow naturally. Unfortunately, this process can produce unreliable growth results and can take several years. Thus, faster, more reliable methods are needed. In this study, a simple, rapid (3–10 days), and cost-effective method was developed for testing the efficacy of nano-engineered coatings for mitigating the growth of Sn whiskers. This method consisted of a micro-indentation process using a ball-bearing adhered to a few hundred gram weight, which are placed in a stabilizing printed holder. For uncoated samples, Sn whiskers and hillocks were abundant near the indentation area, while only hillocks were found further outside the area (i.e., >0.2 mm). For samples coated with nano-engineered ceramic or polymeric coatings, the indentation method was observed to damage coatings only at the point of contact (e.g., no delamination), while still allowing Sn whiskers and hillocks to grow outside the indentation area.     

时效温度下钎料的稀土相CeSn3表面Sn晶须生长

于Sn3.8Ag0.7Cu钎料中添加过量的稀土Ce会在其内部形成大尺寸的稀土相CeSn3,将稀土相CeSn3暴露于空气中,研究在时效处理过程中时效温度对其表面Sn晶须生长的影响规律.结果表明:时效温度对稀土相CeSn3表面Sn晶须的生长产生显著影响.室温时效20 min后,其表面会形成少量的白色Sn颗粒:75℃时效20...     

Tin whisker formation of lead-free plated leadframes

This paper presents the evaluation results of whiskers on two kinds of lead-free finish materials at the plating temperature and under the reliability test. The rising plating temperature caused increasing the size of plating grain and shorting the growth of whisker. The whisker was grown under the temperature cycling the bent shaped in matte pure Sn finish and hillock shape in matte Sn–Bi. The whisker growth in Sn–Bi finish was shorter than that in Sn finish. In FeNi42 leadframe, the 8.0–10.0 μm diameter and the 25.0–45.0 μm long whisker was grown under 300 cycles. In the 300 cycles of Cu leadframe, only the nodule-shaped grew on the surface, and in the 600 cycles, a 3.0–4.0 μm short whisker grew. After 600 cycles, the 0.25 μm thin Ni₃Sn₄ formed on the Sn-plated FeNi42. However, we observed the amount of 0.76–1.14 μm thick Cu₆Sn₅ and 0.27 μm thin Cu₃Sn intermetallics were observed between the Sn and Cu interfaces. Therefore, the main growth factor of a whisker is the intermetallic compound in the Cu leadframe, and the coefficient of thermal expansion mismatch in FeNi42.     

Whisker growth on surface treatment in the pure tin plating

Whisker behavior at various surface treatment conditions of pure Sn plating are presented. The temperature cycling test for 600 cycles and the ambient storage for 1 year was performed, respectively. From the temperature cycling test, bent-shaped whiskers were observed on matte and semibright Sn plating, and flower-shaped whisker on bright Sn plating. The bright Sn plating has smaller whiskers than the other types of Sn plating, and the whisker growth density per unit area is also lower than the others. After 1 year under ambient storage, nodule growth of FeNi42 lead frame (LF) was observed in some parts. The Cu LF showed about a 9.0 μm hillock-shaped whisker. This result demonstrated that the main determinant of whisker growth was the number of temperature cycling (TC) in the FeNi42 LF, whereas it was the time and temperature in the Cu LF. Also, whisker growth and shape varied with the type of surface treatment and grain size of plating.     

A Statistical Study of Sn Whisker Population and Growth During Elevated Temperature and Humidity Tests

Storage tests at elevated temperature and humidity conditions have been widely adopted as one of the major acceleration tests for Sn whisker growth. However, the driving force associated and the nucleation and growth process of whiskers are yet to be fully understood. In this paper, Sn whisker growth on Cu leadframe material at two different test conditions is compared. Both loose and board-mounted components were used. At each read point, the length and location of every whisker observed was recorded. Statistical characteristics and growth rate of the whisker population will be presented for each of the tests conditions. On loose components, corrosion of the Sn finish was observed near the tip and the dam bar cut area of the leads with backscatter scanning electron microscopy (SEM) and optical microscopy. The entire population of whiskers was located in these corroded areas, and there were zero whiskers located in the noncorroded areas on the same leads. On board-mounted components, the corrosion level of the Sn finish, as well as the whisker population and length was greatly reduced compared to those on the loose components. These results suggest that the corrosion of Sn finish in high-temperature and high-humidity conditions is the major driving force for whisker growth. The cause for the difference between the loose and board-mounted components is also analyzed     

Cross-Interaction Study of Cu/Sn/Pd and Ni/Sn/Pd Sandwich Solder Joint Structures

Cross-interactions between Cu/Sn/Pd and Ni/Sn/Pd sandwich structures were investigated in this work. For the Cu/Sn/Pd case, the growth behavior and morphology of the interfacial (Pd,Cu)Sn₄ compound layer was very similar to that of the single Pd/Sn interfacial reaction. This indicates that the growth of the (Pd,Cu)Sn₄ layer at the Sn/Pd interface would not be affected by the opposite Cu/Sn interfacial reaction. We can conclude that there is no cross-interaction effect between the two interfacial reactions in the Cu/Sn/Pd sandwich structure. For the Ni/Sn/Pd case, we observed that: (1) after 300 s of reflow time, the (Pd,Ni)Sn₄ compound heterogeneously nucleated on the Ni₃Sn₄ compound layer at the Sn/Ni interface; (2) the growth of the interfacial PdSn₄ compound layer was greatly suppressed by the formation of the (Pd,Ni)Sn₄ compound at the Sn/Ni interface. We believe that this suppression of PdSn₄ growth is caused by heterogeneous nucleation of the (Pd,Ni)Sn₄ compound in the Ni₃Sn₄ compound layer, which decreases the free energy of the entire sandwich reaction system. The difference in the chemical potential of Pd in the PdSn₄ phase at the Pd/Sn interface and in the (Pd,Ni)Sn₄ phase at the Sn/Ni interface is the driving force for the Pd atomic flux across the molten Sn. The diffusion of Ni into the ternary (Pd,Ni)Sn₄ compound layer controls the Pd atomic flux across the molten Sn and the growth of the ternary (Pd,Ni)Sn₄ compound at the Sn/Ni interface.