Characterization of SAC – x NiO nano-reinforced

lead-free solder joint in an ultra-fine

package assembly
Fakhrozi Che Ani
Engineering and Technology Services (ETS), Jabil Circuit, Penang, Malaysia,
and Institute of Microengineering and Nanoelectronics (IMEN), Universiti Kebangsaan Malaysia, Bangi, Malaysia
Azman Jalar
Institute of Microengineering and Nanoelectronics (IMEN), Universiti Kebangsaan Malaysia, Bangi, Malaysia
Abdullah Aziz Saad
School of Mechanical Engineering, Universiti Sains Malaysia, Seberang Perai Selatan, Malaysia
Chu Yee Khor
Faculty of Engineering Technology, Universiti Malaysia Perlis, Arau, Malaysia
Mohamad Aizat Abas and Zuraihana Bachok
School of Mechanical Engineering, Universiti Sains Malaysia, Seberang Perai Selatan, Malaysia, and
Norinsan Kamil Othman
School of Applied Physics, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, Bangi, Malaysia

Abstract
Purpose – This study aims to investigate the NiO nano-reinforced solder joint characteristics of ultra-fine electronic package.
Design/methodology/approach – Lead-free Sn-Ag-Cu (SAC) solder paste was mixed with various percentages of NiO nanoparticles to prepare the
new form of nano-reinforced solder paste. The solder paste was applied to assemble the ultra-fine capacitor using the reflow soldering process. A
focussed ion beam, high resolution transmission electron microscopy system equipped with energy dispersive X-ray spectroscopy (EDS) was used in
this study. In addition, X-ray inspection system, field emission scanning electron microscopy coupled with EDS, X-ray photoelectron spectroscopy
(XPS) and nanoindenter were used to analyse the solder void, microstructure, hardness and fillet height of the solder joint.
Findings – The experimental results revealed that the highest fillet height was obtained with the content of 0.01 Wt.% of nano-reinforced NiO,
which fulfilled the reliability requirements of the international IPC standard. However, the presence of the NiO in the lead-free solder paste only
slightly influenced the changes of the intermetallic layer with the increment of weighted percentage. Moreover, the simulation method was applied
to observe the distribution of NiO nanoparticles in the solder joint.
Originality/value – The findings are expected to provide a profound understanding of nano-reinforced solder joint’s characteristics of the ultra-fine
package.
Keywords SAC305, Ultra-fine package, Nano-reinforced lead-free solder, Nickel oxide nanoparticle
Paper type Research paper

1. Introduction Chen et al., 2010; Chellvarajoo et al., 2015a). An example of Pb-

Solder paste is a factor which determines various characteristics of
electronic packages and substrates such as their joint strength,
thermal, mechanical and electrical behaviours (Chellvarajoo et al.,
2015b). Pb-free solder paste is commonly used by electronic
packaging industries to eliminate the harmful effects of Pb on
human health and ecosystems (Chellvarajoo et al., 2015b; Efzan
Mhd Noor et al., 2013; Zhang et al., 2010; El-Daly et al., 2009;
The current issue and full text archive of this journal is available on
Emerald Insight at: www.emeraldinsight.com/0954-0911.htm
Soldering & Surface Mount Technology
31/2 (2019) 109–124
© Emerald Publishing Limited [ISSN 0954-0911]
[DOI 10.1108/SSMT-08-2018-0024]
free solder paste that is widely accepted as a replacement material
is the ternary tin-silver-copper (Sn-Ag-Cu: SAC) solder paste for
eutectic Sn-Pb solder in surface mount application (SMT) (Sujan
et al., 2014). Compared to Sn-Pb solders, the majority of the Pb-
free solder pastes require a higher thermal energy to melt. Because
of this nature, the Sn-based Pb-free low-temperature solder alloys
have restricted applications because of their expensive raw
materials and low reliability (Sn-58Bi: 138; Sn-52In:
118°C); this includes packages that are heat sensitive. Despite
The authors would like to thank the Universiti Kebangsaan Malaysia
(Research grant-DIP-2014-012), Universiti Sains Malaysia (RUI Grant 1001/
PMEKANIK/8014067) and Jabil Circuit Sdn Bhd for their financial support.
Received 13 August 2018
Revised 20 September 2018
Accepted 30 October 2018

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this, Sn-3.0Ag-9.5Cu (SAC 205) solder paste is the current best behaviour of NiO nanoparticles in SAC305 Pb-free solder
alternative in electronic assemblies. SAC 305, a mix of solder paste during the ultra-fine package assembly process may
alloys, is a top-tier paste because of its cost-effectiveness and introduce new and innovative ideas into this field.
efficiency (Efzan Mhd Noor et al., 2013; Sujan et al., 2014;
Ahmad et al., 2007). 2. Materials and methods
SAC 305 solder pastes are usually used in SMT, however,
there is still potential for improvements in terms of reliability 2.1 Preparation of the surface mount package with
(Collins et al., 2012; Kotadia et al., 2014). The dependability of nano-reinforced lead-free solder assembly
the solder joint in long-term service plays a crucial role in the The ultra-fine package assembly tested in this experiment was a
electronic packaging industry; thus, the recently developed Pb- 01005 capacitor (as shown in Figure 1(a)). The dimension of
free solder paste now features a much more dependable this ultra-fine package was 0.4 mm 0.2 mm. First, NiO
microstructure (El-Daly and Hammad, 2010), suitable nanoparticles (Aldrich, 98 per cent trace metal basis, particle
intermetallic layer (IMC), growth rate, and appropriate melting size: <25 nm) were mixed with the 96.5Sn –3.0Ag–0.5Cu
point and mechanical properties (Efzan Mhd Noor and Singh, solder paste (SAC305; Alpha OM-353) at a nominal
2014). A widely experimented method of enhancing reliability percentage of 0.01, 0.05 and 0.15 Wt.% using a mechanical
involves mixing small amounts of micro particles of rare earth stirrer (Fritsch Planetary Mill PULVERISETTE 5) for
metals such as Bi, Sb, Fe, Co, Mn, Ti, In, Ni, Ge, Cu, and Ag in approximately 10 minutes (300 rpm) to achieve homogeneity
SAC solder paste (Chellvarajoo et al., 2015b; Gao et al., 2010). prior to assembly. Lower amounts of NiO were distributed in
Because high-performance applications require a decrease in the solvent toward a lacey carbon coated copper grid prior to
particle size, the micro size particles were added to the SAC analysis of high resolution transmission electron microscopy
solder paste and slowly became nano size. Various types of (HRTEM) image. The average of particle size of the received
nanoparticles featuring distinctive properties and increased nanoparticles was deliberated using FEI Tecnai G2 F20
reliability have been used to reinforce the SAC solder alloys. The HRTEM. The HRTEM micrograph as shown in Figure 2
effects of TiO2 nanodopant on SAC305 solder paste were illustrates the NiO nanoparticles obtain an average particle size
examined by Tang et al. (2014). The average grain size and of 15 nm, which roughly corresponded to the particle size value
spacing between Ag3Sn grains in the solder matrix is lessened
because of TiO nanoparticle reinforcements in SAC 305. Figure 1 Ultra-fine package (01005 capacitor)
Furthermore, the micro-hardness of SAC305 solder matrix
steadily increased by 20 and 37 per cent after being doped with
0.05 and 0.1 Wt.% of TiO2 nanoparticles respectively. ZrO
ceramic nanoparticles were added into the SAC solder paste and
showed homogeneously distributed grains in the -Sn solder
matrix and unpinned particles in IMC layers. However, the IMC
layers were attached with Ni atoms from the Au/Ni metalized Cu
pads to form Sn-Ni-Cu structures which increased the joint
dependability (Gain et al., 2011a). The Fe NiO nanoelements
in the solder paste migrated towards the surface after the reflow
soldering process during a “copper sandwich” test (Chellvarajoo
et al., 2015b). The hardness of the joining increases because of
the binding fractions of Fe and Ni nanoparticles to the -Sn
microstructure. Migration of Cu atoms from the substrate which
are inhibited by the ceramic nanosolder pastes reduces the
thickness of IMC layers. Respectively, the nickel and oxygen
elements from NiO nanoparticles were from Block D, Period 4
element and Block P, Period 2 element from the periodic table.
Nickel is a ferromagnetic element which allows the movement of
electrons; nickel is also an extremely stable alloy in Pb-free
solders compared to other Block D, Period 4 elements
(Hemalatha et al., 2014; Gain et al., 2009). Thus, the doping of
NiO into SAC 305 Pb-free solder paste is designed specifically to
enhance the dependability of solder joints. There are very few
studies on the effects of ceramic nanoparticles doped into SAC
Pb-free solder paste after the reflow soldering process.
There are currently no studies involving NiO nanoparticles
as doping for SAC 305 Pb-free solder paste on the ultra-fine
package assembly in the reflow soldering process. Therefore,
this study considered the NiO nano-reinforced solder paste on
the real electronic assembly process to discover the effects of
the addition of NiO nanoparticles on the SAC 305 Pb-free
solder paste after the reflow soldering process. The unique

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Figure 2 HRTEM image of NiO nanoparticles Figure 3 Ultra-fine package (01005 capacitor)

specified by the supplier (<25 nm).The average particle size of

the 96.5Sn-3.0Ag-0.5Cu as acquired was 15 - 25 m (Type 5,
500/1635 mesh designation as per ASTM B214). Next, the
2.0 mm printed circuit board (PCB organic solderable
preservative surface finish) was used to mount the ultra-fine
package using nano reinforced, lead-free solder as shown in
Figure 1(b). Using a laser-cut, stainless steel stencil (nano
coated with 1:1 aperture 0.2 0.2 mm) and a steel squeegee,
nano reinforced lead-free solder paste was printed (DEK
Horizon) at 0.127 mm (thickness). By using the robotic Fuji
NXT equipment (customized nozzle), ultra-fine package was
mounted at the printed nano-reinforced lead-free solder paste.
The process of soldering was carried out with the presence of
lead-free reflow profile, under a nitrogen atmosphere, with the
full convection reflow oven (Vitronics Soltec XPM ). Lastly,
the reflowed PCBs were cleaned using an aqueous cleaning
microscopy. The minimum height of the fillet must be above
machine (Electrovert Aquastorm 200).
the thickness of the solder, plus 25 per cent termination
height (IPC, 2010a). After processing the reflow soldering,
2.2 Nano-reinforced lead-free solder joint the measurement of the fillet height is shown in Figure 3(b).
characterizations The relationship between the solder land dimensions,
X-ray inspection system (Nikon XT V 160) was used to component termination, solder volumes, and solder paste
investigate the voids formation in the ultra-fine solder joint. flux wetting behaviours are shown below (Wassink and
The distribution of NiO nanoparticles in the ultra-fine solder Verguld, 1995):
joint was investigated using a FEI Tecnai G2 F20 HRTEM
system equipped with an energy dispersive X-ray spectroscopy
(EDS). The common mechanical technique with a diamond
blade has a limitation in that it can eliminate the ultra-fine joint. Figure 4 Fillet height measurement points of ultra-fine packages
Thus, the HRTEM lamella of the ultra-fine joint was prepared (01005 capacitors)
using a progressive technique called FEI Helios NanoLab 650
Dual Beam System (Figure 3(a)). Besides this, an ion beam is
required to carry out the cross-sectioning to create HR-TEM
lamella sample and has both a finely focussed ion beam and a
high resolution electron beam joined into the system. Next,
HRTEM lamella was attached onto the molybdenum (Mo)
grid finger after been lifted out of bulk sample using an in-situ
lift out technique, also known as Omni probe needle. Then, it
was thinned down to the transparency of electron with a
thickness of less than 100 nm.
The joining reliability of the ultra-fine package can be
influenced by the height of the solder fillet in the ultra-fine
solder joint. It was measured using scanning electron

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Wp thickness of 0.127 mm and the volume fraction of solder in

h¼ d Hs f (1)
W paste is 0.5 mm.
The calculation is described below:
Based on the equation above, h is finished solder height, W is
solder paste stencil width, W is PCB solder pad width, d is 0:2mm
h¼ 0:127mm 0:5 1:4 (2)
stencil thickness, Hs is volume fraction of solder in paste, and f 0:2mm
is shape factor. The height of the circle segment is represented
by W (solder thickness 1 25 per cent of component Thus, h = 0.0889 mm (minimum).
termination height (IPC, 2010a) divided by the thickness of d Four columns of focussed area for fillet height measurement
of the square with the same area and same length W, which is are labelled i, ii, iii and iv. Each of the columns has ten rows
about 1.4). which are labelled a, b, c, d, e, f, g, h, i and j (Figure 4). Then,
An ultra-fine package (01005 Capacitor) uses a PCB solder each of the capacitors has two solder fillet heights: left and right.
with a pad width of 0.2 mm, stencil width of 0.2 mm and stencil Readings are recorded from the capacitors in rows a and j only.

Figure 5 Ultra-fine package (01005 capacitor)

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