Journal of Alloys and Compounds 669 (2016) 38e45

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Journal of Alloys and Compounds

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Calcining Temperatures of Sr1-3xEuxDy2xAl2O4 (x 00.12) Phosphors

Prepared Using the Potassium Carbonate Coprecipitation method
Chen-Jui Liang*, Hao-Yi Siao
Department of Materials Science and Engineering, Feng Chia University, Taichung 40724, Taiwan, ROC

a r t i c l e i n f o a b s t r a c t

Article history: This study investigated the optimal calcining temperatures of Sr1-3xEuxDy2xAl2O4 (x 00.12) phosphors
Received 20 November 2015 prepared by a new coprecipitation method using potassium carbonate as the precipitant. The results
Received in revised form show that the potassium carbonate coprecipitation method was useful and successful, and avoids the
26 January 2016
problems of residual precipitant presence and the elution of small metal ions. The optimal calcining
Accepted 29 January 2016
temperatures of the phosphors ranged from 920 to 950  C, which were lower than those obtained using
Available online 1 February 2016
other methods. An empirical model was established to examine the calcining temperatures of prepared
precursors. The average absolute relative error between the starting temperatures obtained from ther-
Keywords:
Luminescence
mogravimetric analysis and temperatures estimated by the empirical model was 0.23%. The emission
Optical materials intensity increment rate of the phosphors produced using the potassium carbonate coprecipitation
Chemical synthesis method between the doping amounts x of 0.01 and 0.06 is approximately 10-fold higher than that
Calcium aluminates produced using the solidestate reaction method. Emission intensities of the prepared phosphors were
increased approximately 23.5-fold when the doping amount was increased from 0.01 to 0.06.
Sr0.64Eu0.12Dy0.24Al2O4 phosphor has moderate surface characteristics and the highest surface Dy/Eu ratio
of all phosphors; therefore, its emission intensity is greater than those of other prepared phosphors.
2016 Elsevier B.V. All rights reserved.

1. Introduction polycrystalline solids from a mixture of solid starting materials.

Phosphor materials have considerable potential in several ap-
plications such as optical brighteners, copy and product pro-
tections, security labeling, conversion of high-energy radiation,
markers for analysis, lithography, photochemistry, bioimaging
detection, and medicine. Numerous studies have focused on
enhancing the properties of long-persistent [1e3], long-afterglow
[4e6], sunlight-activated [7e10], and elastic, mechano-, thermo-,
and lyoluminescences [11e15] to form high-performance phos-
phors. Synthesizing efcient phosphors requires not only the best
in high-temperature chemistry but also careful precursor prepa-
ration, proper handling, and high purity of starting materials.
Phosphor materials can be prepared using the following tech-
niques: solidestate reaction, solegel calcination, spray drying and
calcination, ultrasonic atomization and combustion, self-
propagating high-temperature synthesis, and coprecipitation. The
solidestate reaction method has been used widely for preparing
* Corresponding author.
E-mail address: cjliang@fcu.edu.tw (C.-J. Liang).
This method is necessary to heat solid mixtures to markedly higher
temperatures (10001500  C) for the reaction to occur at an
appreciable rate [16e18]. The solegel synthesis of ceramic oxides
demonstrates advantages such as high purity and favorable ho-
mogeneity. Dry gel particles are prered at 8501000  C to remove
the organic groups, followed by calcining at high temperature
(12001450  C) to crystallize and form luminescent centers
[19,20]. The spray drying and calcination method involves heating
the powder at approximately 750  C for 3 h, and then calcined at
1300  C for 3 h [21]. In the ultrasonic atomization and combustion
method, a solution created by ultrasonic atomization passes
through a tubular furnace with a temperature of 1500  C [22]. The
synthesis of phosphors by self-propagating high-temperature
synthesis is carried out in a reactor containing static argon gas at a
pressure of 0.5 MPa and temperature of >1800  C [23]. In copre-
cipitation methods, precipitants such as (NH4)2CO3, NH4OH,
CO(NH2)2 and oxalic acid are generally used [24e27]. A mixed ni-
trate solution is dumped into a highly revolving agitator and an
alkaline precipitant solution of approximately 1M is added in
droplets to produce a precursor. After being dried and washed, the
nal powders are obtained by calcining the dried precursor at

http://dx.doi.org/10.1016/j.jallcom.2016.01.227
0925-8388/ 2016 Elsevier B.V. All rights reserved.
 C.-J. Liang, H.-Y. Siao / Journal of Alloys and Compounds 669 (2016) 38e45
different temperatures from 1000 to 1300  C.
As mentioned, the nal calcining temperatures of most prepa-
ration methods are extremely high, thus resulting in high energy
expenditure. Although the nal calcining temperatures of the
coprecipitation methods are lower than those of other methods,
two problems must be avoided: residual precipitant inuences the
chemical homogeneity of mixed metal oxides when the precursors
are calcined, and small metal ions elute from the precursors when
washed with distilled water. Additionally, the crystal structure of
phosphors depends on the calcining temperature, as observed in
calcining
1  3xSrCO3s xEuOH3s 2xDyOH3s 2AlOH3s !Sr13x Eux Dy2x Al2 O3s 3 4:5xH2 O 1  3xCO2 0:75xO2
rare-earth-doped strontium aluminate systems [21]. However,
reducing energy use for industrial production and environmental
protection is crucial. This work introduces a new coprecipitation
method that involves using K2CO3 solution as the precipitant to
prepare phosphors that are efcient, have low-energy re-
quirements, have high purity, and demonstrate favorable homo-
geneity. The results show a direct relationship between the optimal
calcining temperature and the composition of the starting
materials.
2. Experimental
Sr1-3xEuxDy2xAl2O4 (x 00.12) phosphors were prepared using
the potassium carbonate coprecipitation method with 800 mL of
0.18 M K2CO3 solution (pH 10.98) as the precipitant and a stirring
rate of 500 rpm. Subsequently, 100 mL of metal nitrate solution,
contained 0.1280.20 M Sr(NO3)2, 00.048 M Eu(NO3)3,
00.096 M Dy(NO3)3, and 0.40 M Al(NO3)3, was added to the po-
tassium carbonate solution at an approximate rate of
10.0 mL min1. The precipitates were ltered out repeatedly,
washed with distilled water, and then dried in a vacuum oven at
110  C for 2 h. Next, the precursor of the phosphors was calcined in
a reducing environment of 10% H2 90% N2 with the calcination
process shown in Eq. (1):
1h 2h 6h
room temp,! 400 C!max, calcined temperature!max, calcined temperature!room temp,
The calcination process involved heating the coprecipitates from
room temperature to 400  C, which was maintained for 2 h for
maximum transformation of metal hydroxides to metal oxides. The
temperature was then raised to the maximum calcining tempera-
ture, which was maintained for an additional 6 h to complete the
transformation of metal oxides to phosphors. The maximum
calcination temperature of each precursor was determined using
Simultaneous DSC-TGA (TA Instrument, SDT2960) between 50 and
1200  C at a heating rate of 5  C min1.
An equilibrium pH of 9.16 was measured in the coprecipitates by
using 0.18 M K2CO3 solution as the precipitant. Between pH 4 and
10, aluminum, Al(OH)3 is nearly insoluble. Hydroxide compounds
of Sr are somewhat soluble at pH 9.16, but their carbonate com-
pounds are insoluble. Therefore, the loss of Sr ions in solution can
be minimized through this method. The 0.18 M K2CO3 solution was
39
at an optimal concentration for synthesizing Eu and Dy codoping
SrO,Al2O3 phosphors. Theoretically, the precursor mainly consists
of SrCO3 and M(III)(OH)3 (M(III) Al, Eu, Dy), according to the
following chemical reaction equations [24]:
Sr(NO3)2 K2CO3 / SrCO3)2 K2(NO3)2 (2)
2M(III)(NO3)3 3K2CO3 3H2O / 2M(III)(OH 3C 6N (3)
The calcination proceeds according to the following equation:
(4)
Infrared spectra of the precipitates were obtained using Fourier
transform infrared (FTIR) spectroscopy (Perkin Elmer, FT-IR Spec-
trometer Frontier). The crystalline phases of the prepared phos-
phors were identied using X-ray diffraction analysis (Bruker, D8
SSS) with Cu Ka radiation of 1.54 between 10 and 70 at a scan
rate of 0.5 min1. The morphologies and surface atomic percent-
ages of the phosphors were observed using a variable vacuum
scanning electron microscope and an energy dispersive spec-
trometer (Hitachi, S3000eN VVSEM). The BrunauereEmmette-
Teller (BET) surface properties were acquired using a high-
resolution surface area and porosimetry analyzer (Micromeritics,
ASAP 2020). The photoluminescent properties between wave-
lengths of 200 and 1500 nm were obtained by employing a cryo-
genic cathodoluminescence system (JEOL, JSM7001F) at an
accelerating voltage (VII) of 20 kV. Afterglow properties were
collected using uorescence spectrometry (Agilent, Cary Eclipse
FLR) after the samples were fully activated under a select excitation
spectrum.
3. Results and discussion
3.1. Preparation
The precursors were prepared and calcined as mentioned.
cooling
(1)
Fig. 1 shows the FTIR spectra of the precipitates obtained using the
potassium carbonate coprecipitation method. The FTIR spectra of
the precipitates were characterized by a broad band between
2700 and 3700 cm1 (OeH stretching), and three shaper bands at
2483 cm1 (OeH bending), 1646 cm1 (OeH bending),
and1168 cm1 (OeH stretching), all of which correspond to
structural M(III)(OH)3. The area of the broad band between 2700
and 3700 cm1 increases by increasing Eu and Dy doping
amounts. This demonstrates that the major precipitates of Eu and
Dy metals are Eu and Dy hydrates. SrCO3 presence was also
conrmed by the appearance of a shoulder on the two asymmetric
stretching CO3 bands at 1470 (main band) and 855 cm1. In
addition, three shaper symmetric stretching bands were located
at 1774, 1068, and 744 cm1. The main asymmetric stretching CO3
bands at 1470 cm1 separated into two bands, 1518 and
40 C.-J. Liang, H.-Y. Siao / Journal of Alloys and Compounds 669 (2016) 38e45
Fig. 1. FTIR spectra of the prepared precursors.
1401 cm1, when x  0.08. The results show that the potassium
carbonate coprecipitation method was useful and successful, and
avoids the problems of residual precipitant presence and the
elution of small metal ions.
DSC and TG curves of the prepared precursors are shown in
Fig. 2a and b, respectively. The calcining process can be expressed
by three main reactions: the dehydration of M(III)(OH)3 to form
M(III)2O3, the decomposition of SrCO3 to form SrO, and the
recombination of metal oxides to form alkaline earth metal alu-
minates. Three endothermic peaks are evident in the DSC curves
of the sample precursors (Fig. 2a). Their TG curves also show
favorable agreement with the DSC results. The two endothermic
peaks lower than 500  C can be assigned to the dehydration of
M(III)(OH)3 to form M(III)2O3. Because the dehydration of
Eu(OH)3, Dy(OH)3, and Al(OH)3 simultaneously occurred before
500  C, the patterns of DSC and TG varied considerably. The nal
peaks at 700e930  C can be assigned to the decomposition of
metal carbonates. The samples underwent dehydration and
decomposition reactions followed by a recombination of metal
oxides at higher temperature without weight loss to form alkaline
earth metals aluminates. The results show that the starting tem-
perature of the recombination of metal oxides decreases linearly
when the amount of Eu and Dy doping was increased (Fig. 2).
Table 1 presents the starting temperatures of the recombination of
the prepared precursors, which are shown in Fig. 2. The maximum
calcining temperature of the precursors is equal to or greater than
this starting temperature. For each phosphor, a temperature was
selected as the maximum calcining temperature that was higher
than its starting temperature of 20  C. In this study, the maximum
calcining temperature ranged from 920 to 960  C to form efcient
phosphors.
Because the starting temperature of the recombination of metal
oxides decreases linearly by increasing the doping amount of Eu
and Dy, a multiple regression analysis was performed using the
data of the prepared concentrations of metals in solution (Table 1).
The empirical equation resulting from the multiple regression
analysis is Eq. (5). The experimental results of the calcining tem-
peratures of Sr1-xEuxDy2xAl2O4 (x 01.2) phosphors through this
 C.-J. Liang, H.-Y. Siao / Journal of Alloys and Compounds 669 (2016) 38e45 41

Fig. 2. The DSC and TG patterns of Sr1-3xEuxDy2xAl2O4 (x 0  0.12) precursors.

empirical model are presented in Table 1. The average absolute
relative error between the starting temperatures obtained from
Fig. 2 and the temperatures estimated using Eq. (5) was 0.23%. The
results demonstrate that the empirical equation can provide a
quantication of the calcining temperature of Eu and Dy codoping
strontium aluminate phosphors, thereby enabling the synthesis
process to operate under optimal conditions for reducing energy
use.
Tcalcined temp. 2857.1  3040.7[Al]  3462.8[Sr]  3014.0[Eu]
4103.2[Dy] (5)
3.2. Structure
As mentioned, the maximum calcining temperature of each
phosphor in this study was higher than its starting temperature of
20  C. The X-ray diffraction (XRD) patterns of Sr1-3xEuxDy2xAl2O4
(x 00.12) phosphors are shown in Fig. 3. In undoped strontium
aluminates (x 0), SrAl2O4 is the main phase. The relative
amounts of each phase are in the following order: SrAl2O4 >
SrAl4O7 >> Sr4Al14O25. Twenty-seven characteristic XRD peaks of
the SrAl2O4 phase were observed in the Sr0.94Eu0.02Dy0.04Al2O4
phosphor curve, and four small peaks of the SrAl4O7 phase
occurred at 19.6 , 25.1, 32.1, and 32.6 2q. One shaper and two
trace peaks of the Sr4Al14O25 phase appeared at 23.8 , 34.3 , and
62.9 2q. The XRD patterns of Sr1-3xEuxDy2xAl2O4 phosphors with
a doping amount of x  0.04 were similar, and had amounts
similar to those of the SrAl4O7 and Sr4Al14O25 phases. However,
the amounts of the EuAlO3, EuAl12O19, and Dy2O3 phases slightly
increased by increasing the doping amount. The diffraction peaks
of the EuAl12O19 and Dy2O3 phases began to appear at x 0.04,
and the diffraction peaks of the EuAlO3 phase began to appear at

Table 1
Summary of data for multiple regression and the estimated results.

Structures Prepared concentrations of metals in solution, M Trecombin.a Testimateb

[Al] [Sr] [Eu] [Dy]

SrAl2O3 0.4032 0.2000 e e 938 938.6

Sr0.97Eu0.01Dy0.02Al2O4 0.4058 0.1941 0.0019 0.0039 930 929.4
Sr0.94Eu0.02Dy0.04Al2O4 0.4057 0.1681 0.0042 0.0283 928 931.7
Sr0.88Eu0.04Dy0.08Al2O4 0.4041 0.1881 0.0041 0.0081 927 923.3
Sr0.82Eu0.06Dy0.12Al2O4 0.4059 0.1760 0.0081 0.0161 926 927.2
Sr0.76Eu0.08Dy0.16Al2O4 0.4034 0.1640 0.0121 0.0241 920 916.7
Sr0.70Eu0.10Dy0.20Al2O4 0.4056 0.1520 0.0163 0.0320 915 913.2
Sr0.84Eu0.02Dy0.14Al2O4c 0.4030 0.1403 0.0204 0.0418 912 912.2
Sr0.64Eu0.12Dy0.24Al2O4 0.4073 0.1283 0.0246 0.0484 898 901.7
Mean error 2.1  C
Gross error 0.23%
a
The starting temperatures obtained from Fig. 2.
b
The temperatures estimated by Eq. (1).
c
An additional structure was using to facilitate the multiple regression.
42 C.-J. Liang, H.-Y. Siao / Journal of Alloys and Compounds 669 (2016) 38e45
Fig. 3. The XRD patterns of Sr1-3xEuxDy2xAl2O4 (x 0  0.12) phosphors.
x 0.08. Nevertheless, the peaks of these phases were extremely
small. It can be concluded that the points at which Eu and Dy
begin to become liberated from the strontium aluminate crystal
are x 0.04 and x 0.08, respectively. Therefore, a doping amount
that is too high does not enhance the formation of Eu emission
centers.
3.3. Surface characterization
The SEM images of Sr1-3xEuxDy2xAl2O4 (x 00.12) phosphors
are shown in Fig. 4. The surface of undoped strontium aluminate
(Fig. 4a) was sparsely covered with a ne grain of approximately
10 nm. These ne grains may be the nanocrystallites of the
SrAl4O7 phase compared with its XRD pattern (Fig. 3). Irregular
morphological grains of varying sizes were observed in the Eu
and Dy codoped strontium aluminate phosphors (Fig. 4beh). The
particle size is distributed over a wide range, and the grain
boundary is not clean. The average grain sizes of Sr1-3xEuxDy2x-
Al2O4 phosphors with the doping amounts of x 0.01, 0.02, 0.04,
0.06, 0.08, 0.10, and 0.12 were approximately 200, 170, 140, 80,
120, 180, and 120 nm (Fig. 4beh), respectively. As shown in
Fig. 4e, the morphologies of Sr0.82Eu0.06Dy0.12Al2O4 phosphors
with a lower grain size show uniform 1D nanostructures with
lengths of several hundreds of nanometers. The differences
among the microstructures may be attributed to the effect of
recombination of metal oxides. Europium and dysprosium hy-
droxides play a crucial role in the recombination of the calcining
process.
Table 2 presents the surface properties of prepared phos-
phors. The surface properties and atomic percentage of each
phosphor were measured using a BET technique with N2
adsorption and SEM-EDS, respectively. The ranges of the specic
surface area, pore volume, and average diameter for prepared
phosphors were 5.77e18.91 m2 g1, 0.0136e0.0364 cm3 g1, and
7.59e11.03 nm, respectively. The Sr0.82Eu0.06Dy0.12Al2O4 phos-
phor has a specic surface area, pore volume, and average
diameter close to the averages, which were 13.28 m2 g1,
0.0299 cm3 g1, and 9.24 nm, respectively. Clearly, there is an
effect of Eu and Dy codoping on surface properties of the phos-
phors. The ratio of surface Sr, Al, and O atoms of the undoped
strontium aluminate was 1:1.23:1.41. The amounts of surface Al
and O atoms were lower than the stoichiometric molar ratio of
SrAl2O4. In may refer to SrAl4O7 and Sr4Al14O25 phases in the bulk
of the undoped strontium aluminate (Fig. 3). The Al/Sr atom ra-
tios of the prepared phosphors when 0.02  x  0.10 ranged from
1.66 to 2.35, which was lower than their stoichiometric molar
 C.-J. Liang, H.-Y. Siao / Journal of Alloys and Compounds 669 (2016) 38e45 43

Fig. 4. SEM photographs and EDX surface element compositions of Sr1-3xEuxDy2xAl2O4 (x 0  0.12) phosphors. The subgures from (a) to (h) in sequence are x 0, 0.01, 0.02, 0.04,
0.06, 0.08, 0.10, and 0.12, respectively.

ratios but higher than the ratio of undoped strontium aluminate.
The Al/Sr atom ratio of higher Eu and Dy codoped strontium
aluminates (x 0.12) was 7.30. The reason can be ascribed to the
formation of the EuAlO3, EuAl12O19, and Dy2O3 phases on the
surface. The range of Dy/Eu atom ratios of the Eu and Dy codoped
phosphors was 1.42e1.87, with the minimum at x 0.06. These
results demonstrate that the precursors and phosphors of uni-
form molar stoichiometry are easily formed when uses the po-
tassium carbonate coprecipitation method. However, the
liberation of Eu and Dy from the strontium aluminate crystal
occurs when x  0.08.
44 C.-J. Liang, H.-Y. Siao / Journal of Alloys and Compounds 669 (2016) 38e45

Table 2
Surface characterizations for Sr1-3xEuxDy2xAl2O4 (x 0  0.12) phosphors.

Doping amount, x BET surface area (m2 g1)a Pore volume (cm3 g1)b Average pore diameter (nm)c Surface atomic percentage (%)d

Sr Al Eu Dy O

0 5.078 0.0136 10.74 27.46 33.85 e e 38.69

0.02 5.873 0.0159 10.81 11.12 21.74 0.37 0.68 66.09
0.04 18.33 0.0356 7.59 11.03 22.72 0.49 0.90 64.86
0.06 13.27 0.0264 7.97 11.94 21.45 0.81 1.15 64.65
0.08 15.03 0.0289 7.68 13.75 22.76 1.72 3.05 58.72
0.10 16.47 0.0364 8.83 13.79 32.41 3.63 6.61 43.56
0.12 18.91 0.0522 11.03 4.33 31.60 3.37 6.31 54.39
a
Surface areas were measured by a BET technique using N2 adsorption.
b
Single point total pore volume of pores less than 1360 diameter at P/Po 0.9860.
c
Average pore diameter for 4V/A by BET.
d
Surface atomic percentage were measurement by SEM-EDX.

3.4. Luminescence
Fig. 5 shows the emission spectra of the phosphors prepared by
employing a cryogenic cathodoluminescence system at room
temperature. The emission intensity of the prepared phosphors
varies according to the following sequence: Sr0.82Eu0.06-
Dy0.12Al2O4 > Sr0.88Eu0.04Dy0.08Al2O4 > Sr0.76Eu0.08Dy0.16Al2O4 >
Sr0.70Eu0.10Dy0.20Al2O4 > Sr0.96Eu0.02Dy0.04Al2O4 > Sr0.64Eu0.12-
Dy0.24Al2O4. In the emission spectra of the prepared phosphors,
the main and minor emission bands are observed at 523.4 nm and
573.0 nm, respectively. This suggests that the emission of
approximately 540 nm originates from the Eu2 4f65 d1 / 4f7(8S7/
2
2) transitions associated with the Eu ions, which are randomly
2
distributed at the three Sr sites. One weak emission band of the
prepared phosphors, with both x 0.01 and 0.02, is observed at
610.3 nm. Because the EuAlO3, EuAl12O19, and Dy2O3 phases occur
in the structure of Sr0.64Eu0.12Dy0.24Al2O4, the other types of
emission centers emit two spectra of 425.0 and 481.3 nm. The
peaks at 840.4 and 1037.6 nm are caused by wavelength doubling
and scattering of peaks at 425.0 and 523.4 nm, respectively,
because of the second harmonic. As mentioned, Sr0.64Eu0.12-
Dy0.24Al2O4 phosphor has moderate surface characteristics and
the highest surface Dy/Eu ratio; hence, its emission intensity is
greater than those of others.
The emission intensities of the prepared phosphors are
increased approximately 23.5-fold when the doping amount is
increased from 0.01 to 0.06 (Figs. 5 and 6). Furthermore, it can be
observed that the emission intensities of the prepared phosphors
with doping amounts ranging from 0.01 to 0.06 increase linearly
and rapidly (Fig. 6). The emission intensity increment rate of the
phosphors produced using the potassium carbonate coprecipita-
tion method between doping amounts of 0.01 and 0.06 is approx-
imately 10-fold higher than that produced using the solidestate
reaction method [28] (Fig. 6).

4. Conclusions

Synthesis using the potassium carbonate coprecipitation

Fig. 5. CL spectra of Sr1-3xEuxDy2xAl2O4 (x 0  0.12) phoshors.
method is simple, rapid, and successful. The method demon-
strates many advantages such as low energy requirements, sim-
ple equipment, high purity, favorable homogeneity, and short
time for preparing mixed metal oxides. The precipitant of po-
tassium carbonate provides optimal hydroxide and carbonate
ions under appropriate pH conditions for the coprecipitation
reaction of metals to form a well-mixed precursor. This reduces
the energy required for the recombination of metal oxides,
thereby reducing the nal calcining temperature of the crystal-
lization of Eu and Dy codoped strontium aluminates. The optimal
calcining temperature can be estimated accurately by using an
equation to form an efcient phosphor. The optimal calcining
temperature decreases by increasing the doping amount of Eu
and Dy metals. The emission intensity increment rate of the
phosphors produced using the potassium carbonate coprecipi-
tation method between the doping amounts of 0.01 and 0.06 is
approximately 10-fold higher than that produced using the sol-
idestate reaction method. The emission intensities of the pre-
pared phosphors are approximately 23.5-fold higher when the
doping amount is increased from 0.01 to 0.06. Equation (5) is
crucial for proper design and eld operation of a synthesis
reactor, particularly in reducing energy use and environmental
protection.
 C.-J. Liang, H.-Y. Siao / Journal of Alloys and Compounds 669 (2016) 38e45
Fig. 6. Emission intensities dependence of Eu2 concentration x for the present study (CL, VII 20 kV) and reported by Wang et al. (PL, lex 254 nm) [28].
Acknowledgments
The authors would like to thank the Ministry of Science and
Technology of the Republic of China, Taiwan, for nancially sup-
porting this research under Contract No. MOST-104-2218-E-035-
008.
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