Phosphor Concentration in Silicone and Its Effect on the Mechanical and Interfacial Properties of

Phosphor-Filled Silicone
Xing Chen 1, 2, Simin Wang1, 2, Xiaogang Liu1, 2, Sheng Liu1, 2, *
1 Institute of Microsystems, State Key Laboratory for Digital Manufacturing Equipment & Technology,
School of Mechanical & Engineering, Huazhong University of Science & Technology, Wuhan, China, 430074
2 Division of MOEMS, Wuhan National Laboratory for Optoelectronics, Wuhan, China, 430074
* victor_liu63@126.com
Abstract
The phenomenon that phosphor particles tend to settle in
silicone is widely known. Recent researchers have discussed
the effects of phosphor concentration on luminous efficacy of
LED packaging. But to produce reliable products, mechanical
and interfacial considerations are also essential. In this paper,
the mechanical behaviors and interfacial strength of silicone
with different levels of phosphor concentration are studied. In
our experiments, four groups of silicone samples with
different levels of phosphor concentration are prepared and
are subjected to the uniaxial tensile loads. The results of
tensile tests indicate that, for the same level of phosphor
addition, higher phosphor concentration will result in lower
tensile strength of the phosphor-filled silicone. SEM crosssection images show that the phosphor particles concentrate
in the bottom area of the silicone layer. The fractograph of
the material indicates that the crack initiates among the
bottom area where phosphor particles settle. Interfacial tests
of phosphor-filled silicone and GaN substrate are also
conducted. The results demonstrate that phosphor
concentration has negative effect on interfacial strength of
materials. Therefore, for LED package, uniformly distributed
phosphor in silicone is extremely demanded for mechanical
and interfacial considerations.
Introduction
Light emitting diodes (LEDs) continues to be of interest
for their intrinsic high energy efficiency, lack of pollution,
high quality, as well as compact size [1, 2]. Nevertheless,
further improvements in the lifetime, stability, and light
conversion efficiency are urgently demanded for LED devices
being adopted as next-generation lighting sources. To
improve the reliability of LED module, package materials
should be considered. Among various materials used in the
LED packaging, phosphor-filled silicone layer plays a crucial
role on optical performance, as well as long-time reliability,
of the LED module. Though the optical properties of
phosphor coating layer are frequently discussed by
researchers [3-6], the mechanical properties, which are
closely connected to the reliability of packaging, are rarely
concerned. Lack of mechanical behavior and interfacial
property of phosphor-filled silicone material highly limits the
quantitative assessment of the reliability of LED package.
It is known that the phosphor particles tend to settle
inside the phosphor encapsulant mixture during the curing
process. The non-uniform distribution of phosphor
throughout the cured encapsulant will significantly affect the
consistency of correlated color temperature (CCT) of LEDs

[7-9]. And we suppose such this phenomenon as phosphor

concentration could also affect the mechanical properties of
phosphor coating material. For these considerations, we are
motivated to investigate phosphor concentration in phosphorfilled silicone from mechanical and interfacial perspectives.
In our experiments, the well-distributed phosphor-filled
silicone is left to stand for various lengths of time (0h, 1h, 3h
and 10h) in order to prepare the silicone with different levels
of phosphor concentration. Tensile tests are adopted to obtain
mechanical properties of test samples, and engineering
stress-stain curves of samples are automatically recorded
during the tests. Fractograph of samples are investigated after
tensile tests by SEM method. Furthermore, interfacial tests of
phosphor-filled silicone on GaN substrates are conducted to
study the interfacial strength of material. Finally, the
conclusions are summarized and suggestions are proposed.
Experimental
Tensile tests are conducted to obtain mechanical
properties at first. SEM image of fracture surface of test
samples are investigated afterwards. Interfacial shearing tests
are carried out finally.
Phosphor particles are mixed into silicone with mass ratio
of phosphor-silicone of 0.3:1. After stirring and vacuumpumping, the phosphor-filled silicone is divided into four
groups. One group of silicone is cured immediately and the
other three groups are left to stand for 1 hour, 3 hours and 10
hours, respectively. After curing, the samples are mechanical
cut and smoothed according to ASTM 1708 standard (as
shown in Fig. 1 and Fig. 2).

Fig. 1 Dimensions of Test Samples (Unit: mm)

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Fig. 2 Photograph of Test Samples

Tensile tests are conducted by a mechanical testing
machine (Fig. 3). This machine, which has a portal frame
structure, provides a mechanical testing platform with load
range of 500N and displacement resolution of 0.08m. The
testing machine is calibrated according to ASTM standards
to guarantee accuracy and consistency.

Fig. 5 Samples for Shearing Tests

The force-displacement curves of test vehicles are
recorded by computer during shearing tests (Fig. 6).

Fig. 6 Photographs of Interfacial Shearing Tests

Fig. 3 Photograph of Mechanical Testing Machine
Fracture surfaces of samples are observed by SEM after
tensile tests. Frctographs of phosphor-filled silicone are
investigated.
In interfacial test part, samples are cured in square frames
on GaN substrates. The dimensions of the frame are shown in
Fig. 4. The phosphor-filled silicone is restricted to the inner
region of the frame so that the contact areas of silicones and
GaN substrates are the same for all the samples (as shown in
Fig. 5).

Experimental Results
Results of tensile tests will be presented firstly.

Fig. 7 Stress-strain Curves of Samples

Fig. 4 Dimensions of the Frame (Unit: mm)

The tensile curves obtained by mechanical testing

machine indicate that longer standing time of the sample
results in lower tensile strength of the material (as shown in
Fig. 7 and Fig. 8). Moreover, the non-linear behaviors of
phosphor-filled silicones become significant when the
standing time of the uncured samples reaches 10 hours.

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Fig. 8 Tensile Strengths of Test Samples

Studies of fractographs of tested samples demonstrate that
the crack initiates around region where phosphor particles
concentrate, and the crack propagates with a radial pattern
through the material till final collapse (as shown in Fig. 9).

Fig. 10 Fractographs of Four Groups of Samples

(Standing Time: (a) 0h, (b) 1h, (c) 3h, (d) 10h)
Results of interfacial shearing tests of phosphor-filled
silicones on GaN substrates also indicate that phosphor
concentration has negative effect on the interfacial strengths
of test samples. As shown in Fig. 11 and Fig. 12, the critical
shearing forces decrease along with the increase in standing
time of uncured samples.

Fig. 11 Shearing Curves of Samples

Fig. 9 Fractograph of the Test Sample

It can be seen from Fig. 10 (a)-(d) that more phosphor
particles concentrate around bottom area of silicone as the
standing time of silicone sample increases. This phenomenon
inevitably results in the reduction of tensile strength of
phosphor-filled silicone since such material is weakened by
the non-uniform distribution of phosphor particles.
Moreover, the highly non-uniform distribution is the reason
for the non-linear behaviors of the test samples.

Fig. 12 Critical Shearing Forces of Samples

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Since phosphor particle has poorer adhesion than pure

silicone, when phosphor particles are gathered in interfacial
region where the silicone and GaN substrate contact directly,
the adhesion property of the test sample will degrade [10,
11].
Conclusions
Mechanical and interfacial properties of phosphor-filled
silicone are studied in this paper. SEM method is adopted to
investigate the microstructure of test samples.
The results of experiments demonstrate that phosphor
concentration has negative effects on both the mechanical
property and the interfacial strength of phosphor-filled
silicone.
Therefore, the uniform distribution of phosphor particles
in silicone is highly demanded for mechanical and interfacial
considerations in LED packaging.

8.

D. Lu and C.P. Wong, Materials for Advanced

Packaging, Springer Science+Business Media, LLC
(2009).
9. C. Sommer et al., The Impact of Inhomogeneities in the
Phosphor Distribution on the Device Performance of
Phosphor-Converted High-Power White LED Light
Sources, IEEE Journal of Lightwave Technology, Vol.
28, No. 22 (2010), pp. 3226-3232.
10. Z. Suo, Singularities Interacting with Interfaces and
Cracks, International Journal of Solids and Structures,
Vol. 25, No. 10 (1989), pp. 1133-1142.
11. J.W. Hutchinson and Z. Suo, Mixed Mode Cracking in
Layered Materials, Advances in Applied Mechanics,
Vol. 29 (1992), pp. 63-191.

Acknowledgments
This work is supported by Nature Science Foundation of
China (NSFC) Key Project under grant number 50835005,
Guangdong Real Faith Optoelectronics Inc. and Shanghai
Fine MEMS Inc.
The authors gratefully acknowledge the assistance from
Lei Chen and give special thanks to Dr. Han Yan.
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