Ceramics International 42 (2016) 14526–14532

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Facile fabrication and luminescence characteristics of Ce:YAG phosphor

glass thick films coated on a glass substrate for white LEDs
Cheng Yang, Xiaojuan Liang n, Xiaoxuan Di, Pengzhi Li, Guangcai Hu, Rui Cao,
Weidong Xiang n
College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035, China

art ic l e i nf o a b s t r a c t

Article history: A pivotal step in providing a better fluorescent material that has high luminous efficacy and excellent
Received 15 May 2016 thermal stability is to utilize inexpensive phosphors for white light-emitting diodes (W-LEDs). Herein,
Received in revised form we demonstrate a feasible tape-casting technique for creating phosphor thick films that consist of Ce:
31 May 2016
YAG phosphor embedded in relatively low melting point glass frits on an ultrathin glass substrate with
Accepted 10 June 2016
Available online 14 June 2016
controllable film thickness. The glass matrix has ideal densification and interfaces with the glass sub-
strate at a relatively low temperature of 580 °C. Subsequently, the structure and optical properties of the
Keywords: phosphor layer are investigated. In addition, the effect of the phosphor concentration, thick film thick-
Tape casting ness and location (top or bottom) of the phosphor layer on the photoluminescence properties and
Glass
chromaticity are also discussed with respect to use in W-LEDs. Significantly, this promising structure has
Luminescent properties
excellent thermal stability and the potential to overcome current limitations of phosphors in high-power
White light-emitting diodes
W-LEDs. Finally, a high-performance W-LED based on the planar phosphor glass exhibits a luminous
efficiency of 108.45 lm W
1, a correlated color temperature of 5408 K and a color rendering index of 76.
& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

1. Introduction materials with high performance via excellent thermal properties

The development of nitride-based light-emitting diodes is one
of the major achievements in semiconductor science in the past
decade, especially for W- LEDs in lighting. Recently, W-LEDs, as a
new generation solid-state lighting source substitute for in-
candescent or fluorescent lamps, have attracted significant atten-
tion in lighting applications because of their excellent merits, in-
cluding a long lifespan, compactness, energy saving and environ-
ment-friendly features [1–5]. Currently, most current W-LEDs
structures, which are generated by the combination of a blue In-
GaN chip and yellow-emitting Y3Al5O12:Ce3 þ (Ce: YAG) phosphors
dispersed in an organic resin or silicone [6–8], are placed in or-
ganic resin, which causes deterioration of the phosphor due to the
accumulated heat emitting from the chip [9]. As a result, there are
several issues in W-LED performance, including degradation of the
luminous efficacy (LE) and shift of the chromaticity as well as re-
duction in long-term reliability, especially for high-power W-LEDs
[10–12]. In addition, the refractive index of silicone (1.50) is lower
than that of Ce: YAG crystal (1.84), which results in high level of
scattering light and low light extraction. Hence, the fluorescent
n
Corresponding authors.
E-mail addresses: lxj6126@126.com (X. Liang),
xiangweidong001@126.com (W. Xiang).
and long-term reliability are needed for high-power W-LEDs to be
suitable for general use [13].
Recently, substantial effort has been made to develop inorganic
fluorescent materials for W-LEDs. For examples, Ce: YAG transparent
ceramics [14,15], consisting of a glass with homogeneously pre-
cipitated Ce: YAG microcrystals via well-controlled thermal treat-
ment, exhibit excellent thermal resistance properties [16]. Un-
fortunately, it is difficult to control the crystallization of glass, re-
sulting in the low LE of transparent ceramic. Additionally, ceramics
have a high-cost and low reproducibility [17,18]. In addition, phos-
phor-in-glass, which possesses the host property like glass and re-
tains the optical performance of microcrystal phosphors, has been
investigated in detail, and it exhibits excellent thermal stability like
transparent ceramics but with a higher LE [19–22]. To improve
W-LEDs, a planar phosphor glass, which is a thick film of phosphor
coating the glass substrate, has been reported; it improves the lu-
minous and thermal properties as well as long-term stability for
W-LEDs [23–26]. To the best of our knowledge, on the one hand, this
structure could enhance the light extraction rate when phosphor
thick film interfaces with the chips while the glass substrate inter-
faces with air. On the other hand, the correlated color temperature
(CCT) and CIE chromaticity of the W-LEDs can be easily adjusted by
changing the film thickness and phosphor concentration.
This work demonstrates the successful tape-casting of a phos-
phor thick film on glass substrate, which consists of Ce: YAG

http://dx.doi.org/10.1016/j.ceramint.2016.06.065
0272-8842/& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
 C. Yang et al. / Ceramics International 42 (2016) 14526–14532
phosphor powder with a low melting temperature glass frit. The
tape-casting planar phosphor glasses (TPPGs) have a good density
and high visible transparency under sintering without a noticeable
reaction to phosphor. Subsequently, the structure, spectroscopic
characteristics and optical properties of such TPPGs are in-
vestigated. The phosphor layers positioned on the top or bottom of
the structure are also compared. In addition, the TPPG materials
show excellent thermal stability compared to Ce: YAG phosphor.
Therefore, this TPPG structure is very suitable for high power
W-LEDs, which is a light source consisting of multi-chips as in
wafer level package.
2. Experimental section
A yellow Ce: YAG phosphor (HangZhou YingHe Photoelectron
Materials Co. Ltd, China) was selected as a phosphor layer with a
low melting point silicate (SiO2-B2O3-ZnO-PbO) glass matrix. The
slurries were prepared by admixing the glass frits and Ce: YAG
phosphor with high-purity deionized water. The resultant slurries
were coated on an ultrathin heat-resistance optical glass substrate
with a diameter of 50 mm and thickness of 0.4 mm by the tape-
casting process; subsequently, the substrates that were covered
with phosphor tapes were placed in the oven, where they were
slowly heated from 20 to 200 °C for 9 h and dried at 200 °C for 2 h.
Then, they were sintered at 580 °C for 10 min in the muffle fur-
nace. To address the internal stresses, the composites were an-
nealed at 350 °C for 3 h and then naturally cooled to room tem-
perature. While the phosphor layer could be controlled by the
tape-casting process, the surface of the TPPGs was smooth even
without polishing following conventional melting-quenching.
Importantly, these composites could be easily fabricated into dif-
ferent shapes for test and application.
The absorption spectra and crystalline phase of the phosphor
layer were acquired using a UV/VIS Spectrophotometer (ModeV-
570, JASCO) and X-ray diffraction (XRD, D8 Advance, Bruker, Ger-
many), respectively. The cross-sectional microstructures were in-
vestigated using field emission scanning electron microscopy
(FESEM, JSM-6700F, JEOL Ltd., Tokyo, Japan). The photo-
luminescence (PL) and PL excitation (PLE) of the samples were
obtained using a spectrofluorometer (Edinburgh, FS5) equipped
with an Xe lamp. The temperature-dependent luminescence
properties were recorded on the same spectrophotometer, which
Fig. 1. (a) Photographs of TPPGs sintered at 580 °C for 10 min containing x wt% Ce: YAG (x ¼10, 12, and 15). (b)-(d) The cross sectional images of 10 wt%, 12 wt%, and 15 wt%
composites, respectively. (e) Optical transmission spectra of the glass substrate and TPPGs samples.
14527
was attached to a computer-controlled electric furnace and self-
made heating attachment. The decay curves of the samples were
measured by a spectrofluorometer (Edinburgh, FLS920) equipped
with a 460 nm pulsed diode laser (EI-EPL-460). The optical prop-
erties of the constructed W-LEDs, such as the color rendering in-
dex (CRI), chromaticity co-ordinates, CCT, and LE were evaluated
using an integrating sphere (PMS-50; Everfine Photo-E-Info Co.
Ltd, Hangzhou, China) at an operating current of 20 mA. All of the
measurements were performed at room temperature.
3. Results and discussion
A photograph of the as-received TPPGs with x wt% Ce: YAG
phosphor (x ¼10, 12, 15, 20) is partially presented in the Fig. 1(a).
The samples exhibit a bright yellow color because of the em-
bedded Ce: YAG phosphors and good transparency due to the re-
fractive index matching between the Ce: YAG crystal (1.84) and
PbO-based glass host (1.80) [27]. Even phosphor layers with a
thickness of approximately 157–160 mm are observed in the cross-
sectional FESEM images (Fig. 1b–d), indicating that their uni-
formity is easily controllable with the tape-casting process. Inter-
estingly, the interface, which is derived from the bonding between
the glass frit and glass substrate during sintering, is expected to be
excellent. The thick films reach the almost full densification at the
sintering temperature of 580 °C. In addition, as displayed in Fig. 1e,
the optical transmission spectrum of the glass substrate shows
that the transmission reaches 90% in the wavelength range of 500–
800 nm, after coating with the phosphor film, and it decreases
monotonously with increasing Ce: YAG phosphor levels, which is
mainly attributed to the strong absorption of Ce3 þ ions in the
spectral range of 400–500 nm.
The XRD patterns of the as-received phosphor thick films with
x wt% Ce: YAG (x ¼10, 12 and 15) phosphor sintered at 580 °C for
10 min are demonstrated in Fig. 2. For comparison, the XRD pat-
terns of the Ce: YAG phosphor powder and glass substrate were
included; meanwhile, the standard pattern of YAG (JCPDS no. 33-
0040) is shown for reference. Because of the glass is not crystal-
lized at this temperature, the structure of the films mainly de-
pends on that of the phosphor powder. All of the diffraction peaks
can be well matched with that of the standard pattern, indicating
that the phosphor is chemically stable with glass frit upon
sintering.
14528 C. Yang et al. / Ceramics International 42 (2016) 14526–14532
Fig. 2. XRD patterns of the as-received phosphor films with x wt% Ce: YAG phos-
phor (x¼ 10, 12, and 15) and the glass substrate. The standard pattern of YAG
(JCPDS no. 33-0040) is shown for reference.
The PL and PLE spectra of the TPPGs and corresponding Ce: YAG
phosphor powder are depicted in Fig. 3. Under blue light (460 nm)
excitation, the PL spectra of the TPPGs, which are close to the Ce:
YAG phosphor (Fig. 3a), exhibit a typical Ce3 þ : 5d -4 f strong
broadband emission that is centred at 540 nm [28]. The corre-
sponding PLE spectra show two absorption bands at 340 nm and
460 nm in the wavelength range of 300–500 nm, which are as-
signed to the 4f -5d transition of Ce3 þ ions: 4f (2F5/2) - 5d (2B1g)
and 4f (2F5/2) - 5d (2A1g), respectively (Fig. 3b) [28,29]. Notably,
with increasing Ce: YAG phosphor concentration, the relative in-
tensities of the spectra gradually increase. Moreover, the intensity
of the Ce3 þ 4 f (2F5/2) - 5d (2B1g) absorption transition centred at
340 nm was much weaker than that of Ce: YAG phosphor, which is
attributed to the absorption influence of PbO-based glass matrix in
the short wavelength region.
The lifetime on the order of nanoseconds is one of the char-
acteristics of the Ce3 þ electric-dipole allowing for 5d–4f transition.
The comparison of PL decay behaviors of the Ce: YAG phosphor
powder and x wt% Ce: YAG (x ¼10, 12 and 15) co-doped TPPG
composites are studied at an excitation of 460 nm and emission of
540 nm, as exhibited in Fig. 4. As expected, all decay curves have a
single-exponential decay and the decay curve can be expressed as
It = I0exp( −t/τ ) (1)
Fig. 3. (a) PL and PLE spectra of the sample with different concentrations and Ce: YAG phosphor powder. (b) Energy level diagram of the Ce3 þ ions.
Fig. 4. Decay curves of the Ce: YAG phosphor powder and TPPG composites con-
taining x wt% Ce: YAG (x ¼ 10,12, and 15) phosphors.
where It and I0 are the luminescence intensities at times t and t¼ 0,
respectively, and τ is the luminescence lifetime. According to
Fig. 3, on the basis of Eq. (1) and the decay curves, the lifetime
values were determined to be 59.05 ns, 58.84 ns, 58.86 ns and
58.87 ns, respectively. Interestingly, with increasing Ce: YAG
phosphor concentration, the decay behavior of the TPPGs is almost
the same as that of Ce: YAG phosphor, indicating that the erosion
of the Ce: YAG phosphor is very low in the present system.
To validate the potential application of as-received TPPG com-
posites, as a proof-of-concept experiment, the W-LED devices
constructed with x wt% Ce: YAG (x ¼10, 12, 15, and 20) co-doped
TPPGs composites on InGaN-based LED chips under a forward
current set at 20 mA are evaluated as presented in Fig. 5. Here, the
W-LEDs were fabricated using the phosphor thick film positioned
on the bottom of the structure, which will be discussed further. As
shown in the inset of Fig. 5, the electroluminescence (EL) spectrum
of the chip shows a blue-emitting band at approximately 460 nm,
while the EL spectra of TPPGs exhibit blue and yellow emission
bands, yielding white-light emission. Obviously, the higher the Ce:
YAG phosphor content, the higher the green-yellow component
intensity and the weaker the blue of W-LEDs, which is attributed
to the photon reabsorption. The corresponding photometric and
CIE chromaticity coordinates of the TPPG composites with differ-
ent Ce: YAG contents are measured and listed in Table 1. The re-
lated chromaticity coordinates are also plotted on the CIE-1931
 C. Yang et al. / Ceramics International 42 (2016) 14526–14532 14529

The value Duv, an important parameter providing information

about the distance and direction of color shifting from the
Planckian locus, can be calculated from the CIE-1976 chromaticity
coordinate (u0,v0) of the test source and closest point ( u0′ , v0′ ) on
the Planckian locus with the following expression [30].
1
⎡ 2 ⎛2 2 ⎞ ⎤2
2
Duv = ⎢ ( u′ − u0′ ) + ⎜ v′ − v0′ ⎟ ⎥ ⋅sgn( ν′ − v0′ )
⎢⎣ ⎝3 3 ⎠ ⎥⎦ (2)

where the math sgn(z) function returns the sign of a number with
sgn(z)¼ 1 for z Z0 and sgn(z) ¼1 for z o0. The measured CIE 1931
coordinate (x, y) can be converted into CIE 1976 one (u0, v0) using
the following formula:
4x 9y
u′ = ,v′ =
− 2x+12y+3 − 2x+12y+3 (3)

The thus-obtained Duv values are listed in Table 1, showing Duv

of Sample S2 is close to those of the target Duv [31]. Additionally,
considering the photometric and chromatic parameters for the
TPPG-based W-LEDs, Sample S2 one yields an admirable LE as high
as 108.45 lm/W and a good color quality.
In another experiment, the thickness is also supposed to impact
Fig. 5. CIE color coordinates of the W-LEDs fabricated by coupling the 460 nm blue the luminescence properties. Moreover, the sample thickness has
light with x wt% Ce: YAG phosphor (x ¼10, 12, 15, and 20). The insets show the been already reported in the literature [5,15]. To elucidate how the
normalized EL spectra for the fabricated W-LEDs and the photographs of W-LEDs thickness affects the properties of the W-LEDs, the luminescence
using the phosphor thick film positioned on the bottom of the structure. (For in-
terpretation of the references to color in this figure legend, the reader is referred to
spectra of 12 wt% TPPGs with thick film thicknesses from 120 to
the web version of this article.) 200 mm were measured, as shown in Fig. 6a. A typical broad
emission band centred at 540 nm was obtained under blue light
Table 1. excitation (460 nm). In addition, the PL intensity increases gra-
Photometric and chromatic parameters of the TPPG-based W-LEDs with different dually with increasing film thickness, which is attributed to the
phosphor concentrations. high proportion of the YAG crystalline phase enhancing the optical
Samples Ce: YAG CIE coordinates LE (lm/W) CCT (K) CRI Duv
performance. The Fig. 6b illustrates the typical decay curves for the
(wt%) TPPGs with different thicknesses. According to Eq. (1), the lifetime
x y values (58.95 ns) of the samples were not obviously altered, in-
dicating that the intrinsic properties of the Ce: YAG phosphor
S1 10 0.3044 0.3078 80.50 7264 81.5
0.0037
S2 12 0.3348 0.3542 108.45 5408 76.0 0.0005
crystal are little hindered.
S3 15 0.3584 0.4123 112.16 4786 68.4 0.0296 Finally, the W-LEDs were constructed by encapsulating various
S4 20 0.3880 0.4632 126.74 4306 63.8 0.0335 thicknesses (120–200 mm) of the 12 wt% TPPGs using the blue chip
with 460 nm to evaluate the device performance. Previously,
Fig. 7a and b demonstrated the structure of coated phosphor film
diagram in Fig. 5. It is found that the CCT decreases from 7264 K to
on the top (TF) or bottom (BF) side of the glass substrate. For both
4306 K, the CRI decreases from 81.5 to 63.8, the LE increases from
configurations, the other factors were kept same. As known, LE (η)
80.50 lm/W to 126.74 lm/W and the CIE coordinates shift toward
is most commonly obtained by the simple relationship of η ¼ Φ/P
the green-yellow region. where Φ is the emitted luminous flux and P is the input power of

Fig. 6. (a) PL spectra and (b) PL decay curves of the 12 wt% TPPGs composites and the corresponding thick film thickness (120–200 mm).
14530 C. Yang et al. / Ceramics International 42 (2016) 14526–14532

Fig. 7. Schematic illustrations of the W-LED structure consisting of tape-casting on the (a) top and (b) bottom sides of the glass structure. Thickness dependence of (c) LE,
(d) CRI, (e) CCT, and (f) CIE color coordinate of TPPGs-based W-LED in the top and bottom tape-casting cases. (g) Packaging photograph of the optimal conditions with InGaN
LED chips. (For interpretation of the references to color in this figure, the reader is referred to the web version of this article.)

the InGaN LED chips. Therefore, LE is determined by the luminous
flux. As apparent in Fig. 1e, a strong absorption peak at a wave-
length of 300–400 nm in the UV–vis spectrum of the glass sub-
strate was observed. This indicates that the photon energy is ab-
sorbed when the light passes through the glass substrate. As a
result, when increasing the phosphor layer thickness, the LE of BT
is higher than that of TP as for conformal-type W-LEDs, as illu-
strated in Fig. 7c; subsequently, the structure of the TP results in a
lower CCT and higher CRI (Fig. 7d and e). In addition, as shown in
Fig. 7f, the color coordinate of W-LEDs shifts from blue to white
and, finally, to yellow as a result of the yellow luminescence
monotonously intensifying (the inset of Fig. 5). Based on the
overall analysis, the optimal packing condition is found, which
involves a thickness of 160 mm when the phosphor film is applied
to the bottom side of the substrate. Lastly, an actual emitted
sample of white light conversion with the optimal conditions is
shown in Fig. 7g.
The thermal stability is a key parameter for luminescent ma-
terials and their practical applications in high-power W-LEDs.
Therefore, the temperature-dependent PL spectra (313–513 K) of
12 wt% TPPGs with a thickness of 160 mm under 460 nm excitation
are measured and shown in Fig. 8a. With increasing temperature,
the PL intensities gradually decrease. At 433 K, the emission in-
tensity of the TPPGs reaches 92.65% of that at room temperature,
as depicted in Fig. 8b, which is much better than the reported
phosphor-in- silicone (88% at 423 K) [22]. More importantly, at
523 K, the TPPG composite also maintains 80.45% emission
intensity.
In general, the PL intensity decreases with increasing tem-
perature due to the enhanced non-radiative transition [12]. Fur-
thermore, to better understand the thermal quenching character-
istics, we can evaluate the activation energy (ΔE) for thermal
quenching, which can be evaluated with Arrhenius as follows:
[12].
I0
IT =
1+exp( − Δ E/kT) (4)
where IT and I0 are the PL intensities of the TPPGs at room tem-
perature and the testing temperature (313–513 K), respectively; k
is the Boltzmann constant. Thus, the ΔE is approximately 0.45 eV
based on the slopes of fitting straight lines in Fig. 9, which is
higher than the commercial Ce: YAG phosphor (  0.3 eV) [32]. As
 C. Yang et al. / Ceramics International 42 (2016) 14526–14532
Fig. 8. (a) Temperature-dependent PL spectra for the TPPGs at an excitation of 460 nm over the temperature range of 313–513 K. (b) The variation in the relative integrated
intensities of the TPPG composites versus temperature.
Fig. 9. Plots of ln (I0/IT
1) versus 1/kT for the activation energy graph for thermal
quenching of the TPPG composites.
for activation energy, a higher value indicates higher thermal
stability. As a consequence, it is strongly expected to be an alter-
native to silicone as an encapsulating material in higher-power
W-LEDs.
4. Conclusions
A planar phosphor glass composite, fabricated by Ce: YAG
phosphor/glass thick film tape-casted on an ultrathin heat-re-
sistance optical glass substrate, is investigated as a novel type of
wafer level package for W-LEDs. The phosphor layer densified at
580 °C is chemically stable without other phases during sintering.
The PL emission intensity and luminescence properties of the
phosphor film depend on the phosphor concentration and samples
thickness. Impressively, the phosphor thick film positioned on top
of the structure for W-LEDs generated a high LE from minimizing
the loss of emitted light. Moreover, the phosphor thick film ex-
hibits a LE loss of only 7.35% when it is heated to 433 K, indicating
that the thermal stability of the TPPGs is better than for the Ce:
YAG phosphor in silicone, and the corresponding TPPG composites
could have potential applications in high-power W-LEDs.
14531
Acknowledgements
This work was supported by the Key Foundation of Natural
Science Foundation of Zhejiang Province (No. Z4110347), and the
National Natural Science Foundation of China (Nos. 51172165 and
51372172).
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