Author’s Accepted Manuscript

Long persistent luminescence and blue

photochromism in Eu2+-Dy3+ co-doped barium
silicate glass ceramic phosphor

Kazuki Asami, Jumpei Ueda, Setsuhisa Tanabe

www.elsevier.com/locate/jlumin

PII: S0022-2313(18)30977-3
DOI: https://doi.org/10.1016/j.jlumin.2018.11.006
Reference: LUMIN16076
To appear in: Journal of Luminescence
Received date: 2 July 2018
Revised date: 23 October 2018
Accepted date: 1 November 2018
Cite this article as: Kazuki Asami, Jumpei Ueda and Setsuhisa Tanabe, Long
persistent luminescence and blue photochromism in Eu2+-Dy3+ co-doped barium
silicate glass ceramic phosphor, Journal of Luminescence,
https://doi.org/10.1016/j.jlumin.2018.11.006
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 Long persistent luminescence and blue photochromism in Eu2+-Dy3+ co-doped barium
silicate glass ceramic phosphor

Kazuki Asami*, Jumpei Ueda, Setsuhisa Tanabe

Graduate School of Human and Environmental Studies, Kyoto University, Kyoto 606-8501, Japan

*
Corresponding author: Tel: +81-75-753-6817 asami.kazuki.68m@st.kyoto-u.ac.jp

Abstract
Eu2+ -Dy3+ co-doped barium silicate glass was prepared by a melt quenching method and cerammed at

various temperatures between 800 ºC and 1250 ºC to obtain the glass ceramic (GC) persistent phosphors.

The crystal phase of Ba5Si8O21 was primarily precipitated in the GC samples. From the persistent

luminescence decay curve measurement, the GC sample cerammed at 1250 ºC (GC1250) exhibited the

longest persistent luminescence over 16 h until the luminance becomes 2 mcd/m 2. The color of GC1250

sample was changed from white to blue after UV light illumination, and then bleached efficiently by red

light (660 nm) illumination or heat treatment at 200 ºC. From thermoluminescence (TL) glow curve

measurements, four different TL glow peaks were observed at 191 K, 278 K, 446 K, and 494 K. On the

other hand, after red-illumination following UV-illumination, the TL intensity of the only 446 K-peak was

selectively decreased in the TL glow curve. It was shown that the blue photochromism of GC 1250 sample

is strongly related with this glow peak.

Keywords: Glass-ceramics; Persistent luminescence; Europium; Photochromism

1
1 Introduction
Eu2+-doped barium silicate compounds have been used for optical materials like scintillators [1],

glass ceramics [2,3], phosphors by near-UV LED [4], and persistent phosphors [5–7]. The barium

silicate compound as a host material, includes many compositions with different ratios of BaO and

SiO2. The binary phase diagram of the BaO-SiO2 system [1,8] indicates that five different barium

silicate compounds—Ba2SiO4, BaSiO3, Ba2Si3O8, Ba5Si8O21, and BaSi2O5—can be fabricated by a

solid-state reaction. Furthermore, three types of barium silicate phosphors co-doped with Eu2+ and

trivalent lanthanide ion, Ln3+ such as BaSiO3:Eu2+-Nd3+-Tm3+ [5], Ba2Si3O8:Eu2+-Dy3+ [6], and

Ba5Si8O21:Eu2+-Dy3+ [7] have been reported to show persistent luminescence intensity of above

0.32 mcd/m2 for over 10 h. In addition, the BaO–SiO2 system as glass material has a wide

glass-forming region ((40BaO–60SiO2) ~ (0BaO–100SiO2)[9]) and the lowest melting point among

alkaline earth (Mg, Ca, Sr, Ba) silicate binary systems. The glass ceramic (GC), which is prepared

the cerammization of an as-made glass of a specific composition, has unique optical characteristics

[2,10–14]. In recent years, a substantial progress has been achieved in optical applications of GC

for wavelength conversion materials for solar cells, optical fibers and phosphors for white LEDs

[15–18]. In the GC samples of BaSi2O5:Eu2+, Nakanishi has reported the improvement of

luminescence quantum yield [2] and Herrmann has reported luminescence properties with the

change of the crystal system depending on the thermal treatment temperature [3]. In this study, the

Eu2+-Dy3+ co-doped barium silicate (BSO:Eu-Dy) GC samples were obtained by the heat-treatment

of BSO glass at various temperatures, and the persistent luminescence properties and

photochromism were investigated. Photochromism is a reversible phenomenon in which the color

of material changes by light irradiation. The GC sample heat-treated at 1250 ºC shows

photochromism strongly in which the surface color of the sample is changed from white to blue by

UV illumination and then it is bleached by red-light illumination. With respect to this photochromic

property, the coloration and bleaching properties were examined carefully by diffuse reflection

spectrum measurement under the various conditions such as different temperature and bleaching

time.

2
2 Experimental details
2.1 Fabrication of samples
The glass sample with the composition of 39.82 BaO-60 SiO2-0.08 EuO-0.1 DyO3/2 (mol%)

which is the same composition of 0.4% Eu2+- 0.5% Dy3+ co-doped Ba2Si3O8 was prepared by a

conventional melt quenching method using BaCO3 (3N), SiO2 (4N), Eu2O3 (4N) and Dy2O3 (4N)

powders as the starting materials. Additionally, 5 wt% of NH4Cl (3N) was used as flux. These

powders were homogeneously mixed in an alumina mortar, and calcinated at 850 ºC for 2 h in air

for the decarbonation of BaCO3. After calcination, the powder was ground and melted in an

alumina crucible at 1550 ºC for 2 h in N2/H2 atmosphere. The alumina crucible was sealed by an

alumina lid and buried in graphite powder in a larger alumina crucible to enhance reducing

atmosphere. The glass sample was obtained by pouring the melt on a stainless-steel plate and

cooling. The GC samples were obtained by thermal treatment at 800 ºC, 900 ºC, 950 ºC, 1000

ºC,1100 ºC and 1250 ºC for 6 h in N2/H2 atmosphere (denoted as GC800, GC900, GC1000,

GC1100 and GC1250, respectively). As references for persistent luminescence, ceramic samples

of 0.4% Eu2+- 0.5% Dy3+ co-doped Ba2Si3O8 and Ba5Si8O21 are prepared by a solid-state reaction

method. The mixed powders are calcinated at 850 ºC for 2 h in air for the decarbonation, after

which, the powder was ground and compacted to form a ceramic tablet (ϕ10 mm × 2 mm

thickness) under a uniaxial pressing of 20 MPa, and subsequently sintered at 1250 ˚C for 6 h in

N2/H2 atmosphere.

2.2 Measurement
The glass transition temperature (Tg) and the onset crystallization temperature (Tc) of the glass

obtained were measured by a thermogravimetry - differential thermal analysis (TG-DTA)

equipment (TG8120, RIGAKU). The crystalline phases of the samples obtained were analyzed by

X-ray powder diffraction (XRD) (Ultima IV, RIGAKU). The XRD measurements were performed

in the Bragg-Brentano geometry using Cu Kα X-ray source (30 kV and 40 mA). The

photoluminescence (PL) spectra of the obtained samples were measured using a CCD spectrometer
3
 (QE65Pro, Ocean Optics) and an optical fiber. A 365 nm UV-LED light source (LLS-365, Ocean

Optics) was used as the excitation source in the PL measurements. The PL excitation (PLE) spectra

were measured by a fluorescence spectrophotometer (RF-5300, Shimadzu). Persistent luminescence

decay curves were measured using a 300-W Xe lamp (MAX-302, Asahi Spectra Co., Ltd, Japan), a

luminance-measurement setup (BTC 112, Konica Minolta) with a radiance meter (Glacier X, B&W

Tek) and a photomultiplier tube (PMT, Hamamatsu Photonics R3896). The samples were

UV-illuminated for 5 min by the Xe-lamp with a UV module and subsequently the decay curve of

the persistent luminescence intensity was monitored by the PMT output. The absolute value of

luminance at 1 min after ceasing the UV light was evaluated using the radiance meter. The diffuse

reflectance spectra were collected by a spectrophotometer (Shimadzu, UV3600) equipped with an

integrating sphere. For the coloration of GC1250 sample, the UV-LED was used. The combination

of the same Xe lamp and a 660 nm bandpass filter was used as the light source for the bleaching

color of GC1250 sample. For the TL glow curve measurement, GC1250 sample was fixed into a

cryostat (Helitran LT3, Advanced Research Systems) to control the temperature. The sample was

excited by the UV light of the Xe lamp for 10 min and maintained for 10 min at 100 K.

Subsequently, the sample temperature was increased at the heating rate of 10 K/min up to 700 K.

3 Results and discussions

3.1 TG-DTA measurement of BSO:Eu-Dy as-made glass sample
Fig.1 shows the TG-DTA curve of the as-made BSO glass sample. From the DTA curve, the Tg

and the Tc were estimated to be 661 ºC and 849 ºC, respectively. These temperatures are in good

agreement with those of 40BaO-60SiO2 glass reported by Takahashi[19] (Tg = 706 ºC and Tc =

870 ºC measured at heating rate of 20 K/min). From the TG curve, the sample weight was almost

unchanged.

3.2 Structural properties of BSO:Eu-Dy as-made glass and GC samples

Fig. 2 shows the XRD patterns of the as-made glass and the GC by heat-treatment between 800
4
 ºC and 1250 ºC. In the as-made glass, a halo peak was observed at approximately 25°. With

increasing ceramming temperature, sharp peaks appear because of the crystallization of the glass.

From these peaks, the crystal phase of Ba5Si8O21 (indicated by black vertical bars in Fig. 2) is

primarily identified [20]. According to Takahashi’s report[19], in the 40BaO-60SiO2 glass, the

Ba5Si8O21 crystalline phase, which contains a slightly larger amount of SiO2 than the target

composition of Ba2Si3O8, initially precipitated as a crystal nucleus when the crystallization of

glass commenced.
3.3 Photoluminescence properties of BSO:Eu-Dy as-made glass and GC samples
Fig.3 shows the photograph of the obtained as-made glass and GC samples with different

ceramming temperature under white-LED (top line), UV light (2nd line), after ceasing UV light in

the dark field (3rd line) and in the bright field (4th line). The as-made glass sample was yellow

color and turned into white as the heat treatment temperature increased. In addition, the luminescent

color changes from orange to bluish green and luminescence intensity became stronger with

increasing ceramming temperature.

Fig.4 shows the PL and PLE spectra of Eu2+ and Dy3+ in the BSO as-made glass and the GC

samples. In the PL spectra of the as-made glass, GC800 and GC900 samples, a broad luminescence

band at approximately 580 nm (Eu2+: 5d → 4f) is observed and sharp peaks at 572 nm (Dy3+:4F9/2

→ 6H13/2) and 613 nm (Eu3+: 5D0 → 7F2) are observed. In their PLE spectra, the excitation band of

Eu2+ : 4f → 5d, some sharp 4f → 4f transitions peaks of Dy3+ and Eu3+ appear around 360 nm. With

increasing ceramming temperature, the Eu2+ emission band shifts to the shorter wavelength. This is

because that crystallization proceeds in the glass and the proportion of the crystal phase of

Ba5Si8O21:Eu2+ increases as heat treatment temperature rises. For the GC samples with ceramming

temperatures above 950 ºC, the peaks of emission spectra are located at around 480 nm which is

consistent with that in Eu2+ doped Ba5Si8O21 ceramic phosphor[1,7,21]. In the PLE spectra of

GC950, GC1000, GC1100 and GC1250 samples, the sharp excitation peaks disappeared and only

the broad exciton band of Eu2+ : 4f → 5d was observed.

5
3.4 Persistent luminescence properties of BSO:Eu-Dy as-made glass and GC samples
From the photograph of the third line in Fig.3 the blue persistent luminescence was observed in

GC 900-1250. Fig. 5 shows the persistent luminescence decay curves for the BSO:Eu-Dy GC

samples with different ceramming temperatures. For the GC samples with ceramming temperatures

above 950 ºC, the persistent luminance was remarkably improved. The duration when the

luminance reached down to 2 mcd/m2 of the as-made, GC800, GC900, GC 950, GC 1000, GC 1100

and GC1250 are 1.7, 2.9, 14.3, 326.7, 616.4, 689.5 and 961.4 min, respectively. GC1250 sample

shows the longest persistent luminescence among all the GC samples, which is about 8 and 10

times longer than those of Ba2Si3O8:Eu2+-Dy3+ [6] and Ba5Si8O21:Eu2+-Dy3+ [7] phosphors,

respectively. In general ceramic phosphors, the penetration depth of the excitation light is shallow.

But in glass ceramic samples, excitation light can reach deeply into the crystal phase due to the

residual glass phase. And since the process of crystallization in the GC sample is different from that

by the solid-state reaction method, the crystallinity and defect formation may affect the

improvement in persistent luminescence characteristics.

3.5 Photochromism property of GC1250 sample

The blue coloration of sample by UV light illumination was clearly observed in GC 1000 – 1250

(4th line of Fig.3 ). These samples are thought to be due to the large proportion of the crystal phase

in the GC. In particular, GC1250 showed the strongest coloration. The degree of coloring or

bleaching of GC1250 sample was investigated by diffuse reflection spectra. Fig. 5 (a) shows the

diffuse reflectance spectra of GC1250 sample before UV illumination (black line) and UV

illumination for 5 min (purple line). GC1250 sample absorbs light in a broad wavelength region

between 500 nm and 800 nm after UV illumination. Particularly, the diffuse reflectance at 680 nm

decreases significantly from 66.0% to 15.0%. The colored sample showed decolorization by

red-light (660 nm) illumination as shown in Fig. 5(a). Fig.5 (b) shows the illumination time

evolution of the diffuse reflectance spectra by red light illumination. With increasing red-light

illumination time, the diffuse reflectance of the absorption band in the region between 500 nm and

6
 800 nm becomes higher. From the result, the color of the sample is almost bleached after the

red-light illumination for 30 min. Fig.5 (c) shows the dependence of diffuse reflectance spectra of

GC1250 thermally bleached at different temperature for 1 min after photochromism. With

increasing temperature, the diffuse reflectance of the absorption band becomes higher and the

spectrum heat treated at 200 ºC returned to nearly the same as that before UV irradiation. From this

result, the colored sample is completely bleached by thermal treatment at 200 ºC. According to the

Eu2+ doped BaMgSiO4 photochromic ceramic reported by Akiyama’s group [22,23], it is considered

that photochromism occurs when electrons are trapped by oxygen vacancies and behave as F-like

color centers. Because the crystalline phase of GC1250 sample, Ba5Si8O21 is similar to BaMgSiO4

[22,23], it was assumed that electrons in the trap related to F-like color centers might have been

released at 200 ºC and the color of the sample was decolorized. In order to verify that, TL glow

curve measurement was carried out and shown in the next section.

3.6 Thermoluminescence glow curve of GC1250 sample

TL glow curve of GC1250 sample is shown as the solid black line in Fig.6. For GC1250 sample, a

primary intense peak at approximately 450 K and two weak peaks between 150 and 300 K were

observed. The obtained curve could be deconvoluted into four parts of Gaussian functions. From

the result, the GC sample has four electron traps with peaks at 191 K (Trap 1), 278 K (Trap 2), 446

K (Trap 3), and 494 K (Trap 4). According the TL results in ceramic samples of corresponding

composition (Ba5Si8O21:Eu2+-Dy3+) reported by Wang’s group [7], a main TL band covers from

300-475 K and it is assigned as oxygen vacancies. This band locates lower temperature side than

that of GC1250 sample because the heating rate in TL measurement is different. They also reported

that Dy3+ ions have roles of generating and stabilizing traps formed by oxygen vacancies [7]. From

the above report, it is considered that in GC samples, more electrons can be trapped by oxygen

vacancies generated by Dy3+ co-doping.

In the previous section, the diffuse reflection spectrum showed that the blue color of the GC1250

sample was bleached not only by raising temperature but also by red light illumination. From this, it

7
 was considered that the trap forming the color center was released by red light illumination. In

order to ascertain the traps causing photochromism, the UV charged GC1250 sample was

illuminated with red light (660 nm) for 5 min during keeping at 100 K on TL glow curve

measurement. The result is shown by the dashed red curve in Fig.6. The difference between TL

glow curves after UV charging and UV-red light illumination is also shown as the dotted blue line

in Fig.6. By the red-light illumination, the TL intensities of Trap 1 and Trap 2 were almost

unchanged. However, Trap 3 decreased significantly, and the peak shape of the difference closely

matches that of Trap 3. In addition, from the fact that the colored GC1250 sample could be

bleached by thermal treatment at 200 ºC (473 K), it can be considered that Trap 3 contributed to the

coloring of the sample. In Trap 4, it was concluded that the trapped electrons are hardly released

because the peak is located on the higher temperature side than room temperature, and the persistent

luminescence at room temperature does not contribute significantly.

From TL measurement with different illumination condition, the electron transfer processes of

persistent luminescence and photochromism in GC1250 sample were considered as follows. When

Eu2+ ions are excited by UV light, the excited electrons are trapped by oxygen vacancies which are

generated and stabilized by co-doping of Dy3+. And then, the color of sample changes to blue by the

absorption of captured electron in oxygen vacancy. Electrons captured by Trap 3 return to

luminescent centers gradually at room temperature and shows the persistent luminescence. And also,

electrons captured by Trap 3 are de-trapped by red-light illumination and the colored GC sample is

bleached.

4 Conclusions
Eu2+ -Dy3+ co-doped barium silicate glass ceramic persistent phosphors were obtained by heat

treatment of as-made glass at various temperatures between 800 ºC and 1250 ºC. In GC1250 sample, the

crystalline phase of Ba5Si8O21 was primarily precipitated. The duration of the persistent luminescence

when the luminance reaches down to 2 mcd/m2 is over 16 h in GC1250 sample. The color of GC1250

body changed from white to blue after UV light illumination and the color was bleached efficiently by

8
red light (660 nm) illumination or thermal treatment at 200 ºC. From the TL measurements with

different illumination conditions, we conclude that the 446 K-glow peak is strongly related to the blue

photochromism of GC1250 sample.

Acknowledgements

This work was supported by the Grant-in-Aid for Scientific Research on Innovative Areas “Mixed Anion” project

(JP16H06438, 16H06441) from MEXT. K. A. was supported by a Grant-in-Aid for Scientific Research from JSPS

Research Fellow (18J12693).

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10
Fig.1 TG-DTA curve of the as-made glass sample
Fig.2 XRD patterns of the as-made glass and GC samples
Fig.3 Photographs of BSO:Eu-Dy as-made glass and GC samples with different thermal treatment
temperature under white LED (1st line), UV light (2nd line), after ceasing UV light (3rd line) and coloration
(4th line).
Fig.4 PL (ex = 365 nm) and PLE spectra (em = 580 nm for the as-made glass, GC800 and GC900 samples;
em = 495 nm for GC950, GC1000, GC1100 and GC1250 samples) of Eu2+ -Dy3+ co-doped BSO as-made
glass and GC samples.
Fig.5 Persistent decay curve of the as-made glass and GCs with different ceramming temperature
Fig. 6 (a) Diffuse reflectance spectra of GC1250 sample before and after UV light illumination for 5 min. (b)
Illumination time evolution of reflectance spectra of GC1250 sample by red light illumination (660 nm) (c)
Dependence of diffuse reflectance spectra of GC1250 sample on the temperature of heating treatment (for 1 min in
air).
Fig. 7 TL glow curves of GC1250 sample with different illumination conditions (solid black line: UV light for 10 min,
dashed red line: UV light for 10 min + red light (660 nm) for 5 min) and difference (dotted blue line).

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