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a
Department of Electronic Engineering, City University of Hong Kong, 83, Tat Chee Avenue, Kowloon, Hong Kong
b
Photonic Manufacturing Service Ltd., Suites 2207-11, 22/F, Tower 1, The Gateway, 25 Canton Road, TST, Kowloon, Hong Kong
Received 19 June 2003; received in revised form 1 October 2003
Abstract
The demand for volume deployment of photonic components has increased, and with it the need to effectively
manufacture in a reproducible and cost effective way. Therefore, it is important to keep the assembly process consistent
and stable. A simple shear test setup was used in this study to determine the shear force that can be used as an instant
indicator to the process stability of fiber arrays assembly. The shear test was then used to study the effect of curing
conditions, surface roughness, and reliability test on the adhesion of the adhesive joints of single channel fiber arrays. In
general, shear force increases with the curing conditions. However, thermal-induced residue stress during improper
controlled curing process might lead to loss in ductility and reliability of the joints. Results showed that rough bonding
surface for the coverlid can provide better wettability and enhances the shear strength. However, it might result in
incomplete polymerization due to transmission loss of UV radiation during assembly process that was caused by the
uneven surface. Furthermore, rough surface can affect the flow of adhesive that could result in incomplete-fills. Adhesives
at the surrounding of V-grooves and edges of the joints were attacked by moisture at elevated temperature. This paper
also discussed in details the possible failure mechanism of adhesive joints after temperature and humidity test.
Ó 2003 Published by Elsevier Ltd.
Table 1
Curing conditions used in this experiment
Run Condition Power Time (s)
(mW/cm2 )
1 UV post-cure 1700 60
2 UV-85 °C 1700 60
3 UV 2000 60
4 UV 2000 30
5 UV 1700 60
6 UV 1700 30
7 UV 1700 15
8 UV 1500 60
Fig. 1. Cross-sectional view of a single channel fiber array. 9 UV 1500 30
10 UV 1000 60
11 UV 1000 30
paramount. In order to optimize their uses, it is neces-
sary to understand their behavior when exposed to cli-
matic and environmental aggressions. In particular, this surface, and surfaces induced by sand papers of 400 and
study reports on the mechanical stability of adhesive 600 grit sizes. Scan length of 500 lm with scan speed of
joint in fiber array. V-grooves on the fiber block are to 50 lm/s and stylus force of 66.8 mg was used in this
provide pitch alignment of multiple optical fiber and experiment.
epoxy adhesive is hereof used to form joining between
coverlid and fiber block in order to fix optical fiber in 2.3. Reliability test
position. Based on the three-point contact principal as
shown in Fig. 1, misalignment due to curing shrinkage The single channel fiber arrays that were prepared
can be ruled out. using curing condition 2 in Table 1 were subjected to a
This paper reports the performances, i.e., bondability temperature and humidity test, i.e., 85 °C and 85% RH
and reliability of epoxy adhesive joints. The effects of for 0, 25, 50, 75, 100, 125, and 150 h respectively.
curing condition and surface roughness to adhesion Chemical and structural changes of the cured and aged
strength and mechanical properties of epoxy joints were adhesive specimens were identified by comparing their
also reported. IR spectra obtained by Fourier transform infrared
spectroscopy (FT-IR). Perkin–Elmer Spectrum ONE
FT-IR spectrometer equipped with an attenuated total
2. Experimental procedures reflectance (ATR) of 4 cm1 resolution was utilized to
assemble the spectra range from 4000 to 650 cm1 of the
Fiber blocks with single channel V-groove and its samples. In quantitative analysis, relative absorbance
coverlids were prepared using Toshiba USM-20A Slic- intensities of the molecular bonds and groups were
ing machine. Epoxy-based UV-curable adhesive was determined. The corresponding relative intensities of the
used to affix the single channel optical fiber in between cured samples and the aged samples were compared. The
fiber block and coverlid. This model was selected be- base line method was used to calculate the absorbance
cause it represents most of the construction of adhesive intensities of different groups and molecules. The rela-
joint in optical devices, especially passive devices. tive absorbance intensities of any two peaks were cal-
culated as the ratio of their intensities. The relative
2.1. Curing conditions intensity, Er between the reactive peak, Ereactive and ref-
erence peak, Eref would be calculated using the following
The curing process of this adhesive consists of a rapid equation [5]:
polymerization initiated by UV-reactive photo-initiators Ereactive
and two stages of slow thermal polymerization, i.e., 85 Er ¼ : ð1Þ
Eref
°C for 2 h and followed by 60 °C for 10 h. These samples
were prepared by using various curing conditions, as The 1437 cm1 band which is due to CH2 deformation
shown in Table 1. vibration was used as the internal reference peak.
2.2. Surface roughness, Ra, induced by different grit size 2.4. Shear test
Alpha-Step Profiler Model 500 was used to determine The lid shear test was carried out by using an IN-
the surface roughness, Ra, of the glossy surface, abrasive STRON Mini 44 Tester with a cross-head speed of 5
C.W. Tan et al. / Microelectronics Reliability 44 (2004) 823–831 825
As the manufacturing of photonic device revolves the epoxy or at the interface. There are five potentially
into mass production mode, the consistency of the observed failure modes in this experiment as listed below
assembly process is becoming relatively important. and shown in Fig. 3:
Therefore, a reliable in situ monitor system is required in
addition to an on-line visual inspection. The purpose of 1. break at coverlid,
this shear test set-up is to provide immediate indication 2. break at adhesive/coverlid interface which is a adhe-
to line-personnel whether the process and/or the process sive failure,
parameters are operating within specifications. By 3. break at adhesive layer which is a cohesive failure,
referring to six-sigma standard, upper control limit 4. break at adhesive/fiber block interface which is an-
(UCL) and lower control limit (LCL) have been deter- other adhesive failure and,
mined instead of only an average value, as shown in Fig. 5. break at fiber block.
2. The UCL was determined to be 126.9 N and LCL was
35.8 N in which an average value of 81.4 N falls within As a result, all of these 20 samples have demonstrated
this range. These values can be used as the process the failure mode of number 2. Obviously, this bonding
control of the assembly process. Fig. 2 also shows the interface between adhesive and coverlid is the weakest
distribution of the shear force of 20 samples. among the five interfaces mentioned above.
Failure modes of sheared samples are remarkably as When these fracture surfaces were subjected to SEM
important as the shear force value. When the adhesive is examination, it was found that the optical fiber was still
properly cured, the cohesive strength within the glue line sitting in the V-groove and being covered by adhesive on
is great, and adhesion of the epoxy to other materials top of it. This observation can be clearly seen in Fig. 4a
should be so good, that failure under stress condition and b. There were adhesive stains and small quantity of
should often occur in one of the adherents rather than in adhesive remnants, mostly around the location of fiber
optic and V-groove were remaining on the coverlid, as
shown in Fig. 4c. These observations clearly showed that
140 this joining was fractured at the adhesive/coverlid
UCL
interface after shear test.
120
Fig. 4. SEM micrograph show the fracture surface at (a) top view at the fiber block, (b) enlarged view of (a), and (c) at coverlid.
90
80
70
Shear force, N
60
50
40
30
0 1 2 3 4 5 6 7 8 9 10 11 12
Run
Fig. 6. Shear force-vs.-displacement curves with the fracto-
Fig. 5. Shear force strength obtained from samples assembled
graph of samples prepared under different curing conditions.
under various curing conditions.
failure with increasing degree of cure. This indicates that the three curing conditions, i.e., UV curing only, UV
lower the curing degree, the less adhesive has been curing plus curing temperature of 85 °C, and UV plus
solidified that result in lower resistance to the force in post-cure at lower temperature for longer time frame.
shear direction. Since the curing condition of run 3 did The shear force-vs.-displacement curve of samples that
not increase the shear force significantly compared to did undergo UV curing only shows that the plastic
condition of run 6, the latter was chosen as the opti- deformation has taken place before the breaking point.
mized parameters for the rest of this study. A relatively long displacement, approximately 0.7 mm
The effects of post-cure and heat treatment on top of was observed before the adhesive joints reached the
the photo-initiation of UV radiation have significantly breaking point. In the attached SEM micrograph, it is
increased the shear force of fiber arrays. Fig. 6 compares clearly shown that the fracture surface is relatively
C.W. Tan et al. / Microelectronics Reliability 44 (2004) 823–831 827
rough, more plastic deformations and dimples are visi- sandpaper with grit size of 600, 400, and the abrasive
ble, thus they are less brittle compared to the joints with surface processed by vendor.
the other two curing conditions. Fig. 8 shows that rougher surface can provide
For samples that were exposed to UV radiation and stronger interfacial bonding to the adhesive, thus a
85 °C of heat curing, the shear force-vs.-displacement higher shear force is required to remove the coverlids
curve is much sharper. Though it broke at higher shear from the fiber arrays. Rough surface undoubtedly con-
force if compared to samples cured only with UV, tributed to a better adhesion force. However, rougher
shorter displacement was observed. It was observed that bonding surfaces of the coverlids will lead to uneven
the fracture surfaces of these samples were extremely surfaces of the adhesive, as shown in Fig 9. This rough
brittle. This reveals that the adhesive joints produced
under this condition might have suffered from a certain
240
extent of stresses such as thermal expansion stress, shear force 3500
220
shrinkage stress, and other forms of residual stress due surface roughness
200 3000
to non-uniform polymerization.
180
Among all samples the post-cured ones provide the 2500
Shear force, N
Ra, angstrom
160
smoothest curve and highest shear force. In addition, the 140
2000
fracture surface showed a less brittle surface with very 120
little plastic deformation. This indicates that the post- 100 1500
curing condition might have removed the residual stress 80
at the joints induced by the exposure to 85 °C during 1000
60
first stage of post-curing. Therefore, in order to get the 40
500
strongest and most reliable adhesive joints out of this 20
curing process, the condition with post-curing at lower 0 0
ABRASIVE SURFACE
SD 400
SD 600
temperature with longer time if favorable. Glossy SURFACE
Fig. 7. SEM micrographs of surfaces with various surface roughness (a) glossy surface, (b) abrasive surface, (c) by SD 600, and (d) by
SD 400.
828 C.W. Tan et al. / Microelectronics Reliability 44 (2004) 823–831
Fig. 11. Characteristic bands of ester (a) (mðCAOÞ 1180 cm1 ) and (b) (mðC@OÞ 1730 cm1 ).
Fig. 12. SEM micrographs of the top surface of fiber block after shear test for samples that have underwent temperature and humidity
test for (a) 0 h, (b) 50 h, (c) 100 h, and (d) 125 h.
830 C.W. Tan et al. / Microelectronics Reliability 44 (2004) 823–831
Fig. 13. SEM micrographs of bonding surfaces of coverlids after shear test for samples that have underwent temperature and humidity
test for (a) 0 h, (b) 50 h, and (c) 125 h.
structure degradation of the bulk adhesive. Con- the experimental results and observations obtained in
versely, it should be due to the degradation of the this study, it can be concluded as below:
adhesion strength at the interface within coverlid and (a) A shear test was setup and the shear force can be
adhesive. used as internal process control to provide immediate
Fig. 12 shows the hydrolysis marks (craters) at the indication of the process stability. The mean is approx-
surrounding of the exposed optical fiber. It begins with imately 81.4 N, while the upper control limit is about
bubble-like vacant; then these vacant were connected and 126.9 N and the lower control limit is about 35.8 N.
spread slowly. In Fig. 13 the moisture penetration path Only one failure mode was observed, a break at an
can clearly be seen which begins from the V-groove, i.e., adhesive/coverlid interface.
location of the optical fiber and the edges of the bonding. (b) Generally, the shear force increases with the cur-
The dark areas are the plasticizing mark of the adhesive. ing degree. Extreme curing condition, i.e., elevated
It has been well known that the bonding interface has temperature and short dwell time at post-curing, caused
the lowest surface energy if compared to the bulk mate- the adhesive joints losing their ductility. They became
rials. It is believed that moisture was penetrating via more brittle and relatively unreliable.
the bonding interface which lead to degradation of the (c) The surface roughness, Ra, has strongly enhanced
adhesion strength at the bonding interface. In view of the strength of the adhesive joints. However, in the
the fact that the adhesive/fiber block interface has been meantime it was affecting the curing uniformity and
strengthened by the fiber optic that was clamped firmly spread of adhesive that have huge impact to the coupling
by V-groove and the cured adhesive, the coverlid/adhe- efficiency. In addition, rough surface will cause flow
sive interface remains as the weakest point at this con- difficulty, thus affecting the fill up efficiency of adhesive.
struction. Selectively, this layer will consistently be So, rough surface or uneven surface should be avoided
observed as the failure mode, unless there is inconsis- in adhesive joints.
tency in this process or in the experimental setup. (d) The strength of the adhesive joint can be further
enhanced by using a coverlid with a rougher cutting edge
and a rougher flat-groove of the fiber block which can
form a stronger adhesion to the adhesive fillet.
4. Conclusions (e) Temperature and humidity tests have apparently
degraded the adhesion strength due to moisture
A simple shear test experimental setup was used to absorption, and FTIR results suggested that the joint
study the effect of curing conditions (thermal history), has experienced hydrolytic attacks when an increase in
surface roughness and reliability test on the adhesion carboxylic and hydroxyl group but a corresponding
strength of the adhesive joint in fiber arrays. Based on decrease in ester peaks was observed. The V-groove/
C.W. Tan et al. / Microelectronics Reliability 44 (2004) 823–831 831
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The authors would like to acknowledge the grant anisotropic conductive joints on polyimide flexible circuits.
from the Government of the Hong Kong Special Mat Sci Eng B 2003;98(3):255–64.
Administrative Region––Innovation and Technology [6] Tan CW, Chan YC, Yeung NH. Behavior of anisotropic
conductive joints under mechanical loading. Microelectron
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