Materials Research Bulletin 74 (2016) 9–14

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Materials Research Bulletin

journal homepage: www.elsevier.com/locate/matresbu

Synthesis and energy transfer studies of LaMgAl11O19:Cr3+, Nd3+

phosphors
Jicheng Zhu, Zhiguo Xia, Quanlin Liu*
School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083, China

A R T I C L E I N F O A B S T R A C T

Article history: Cr3+/Nd3+ co-activated LaMgAl11O19 phosphors have been synthesized by high temperature solid-state
Received 13 July 2015 method. In the LaMgAl11O19:Cr3+/Nd3+ system, Cr3+ can absorb the UV–vis photons (350–650 nm), and
Received in revised form 21 September 2015 then energy transfer takes place between Cr3+ and Nd3+, and finally the samples give near infrared
Accepted 30 September 2015
emission originated from Nd3+. Energy transfer from Cr3+ to Nd3+ is discussed via the variations of the
Available online 9 October 2015
lifetime values of Cr3+, and the mechanism has been ascribed to the dipole–quadrupole interaction. The
absorption of Cr3+ in the visible region and the following energy transfer from Cr3+ to Nd3+ indicated that
Keywords:
the material can potentially serve as spectral convertors to improve the photovoltaic conversion
A. Optical materials
B. Luminescence
efficiency of silicon-based solar cell.
B. Optical properties ã 2015 Elsevier Ltd. All rights reserved.
C. X-ray diffraction
D. Phosphors

1. Introduction
Solar cell, because of its free, green and abundant source of
energy properties, has been increasingly used in the field of new
energy [1]. Despite that the photovoltaic industry is developing
rapidly, the efficient conversion of solar energy into electricity
through photovoltaic cell remains a critical problem to be solved.
The energy dissipation that resulted from spectral mismatch
between solar photon and energy gap (Eg) of a solar cell may reach
70% [2,3]. In view of this problem, spectral conversion is a fine
option to improve the efficiency of solar cell [4–6]. Rare earth (RE)
ions doped luminescent materials (phosphors) showing near-
infrared emission have attracted increasing attention, therefore
the study on the phosphors for the application in enhancing the
efficiency of silicon-based solar cell become a hot issue [7].
Aluminate materials have been widely used as luminescence
host materials because of their good stability, simple and
environmental friendly processing [8]. Min et al. have prepared
several kinds of phosphors based on the matrix of LaMgAl11O19 for
white light-emitting diodes [9–15]. Previous studies demonstrate
that the LaMgAl11O19, which can be doped with a high concentra-
tion of rare earth ions without quenching, has the advantages of
high physical and chemical stability and low cost [14,15]. Moreover,
Nd3+ doped Lanthanide hexaaluminate (LaMgAl11O19:Nd3+) is
proved to be an interesting laser material [16]. Herein, Cr3+ has
* Corresponding author. Fax: +86 10 6233 4705.
E-mail address: qlliu@ustb.edu.cn (Q. Liu).
broad absorption bands in the near ultraviolet and visible region
due to the spin allowed 4A2/4T2 and 4A2/4T1 transitions, and thus it
has been widely used as a luminescent sensitizer for RE ions in
order to obtain high excitation efficiency. Viana firstly reported the
LaMgAl11O19:Cr3+, Nd3+ in order to improve laser performance of
LaMgAl11O19:Nd3+ crystals through Cr3+ sensitization [17–19],
however, they did not study the energy transfer mechanism and
the corresponding process. Other researches are also performed on
LaMgAl11O19:Cr3+ and LaMgAl11O19 (Ln = La, Nd, Gd) [20,21]. In this
research, we synthesized the pure phase of LaMgAl11O19:Cr3+, Nd3+
phosphor through solid state method. We also studied the
optimum concentration of doped ions, energy transfer mechanism
and the critical distance of energy transfer in the LaMgAl11O19:Cr3+,
Nd3+ phosphor in detail.
2. Experimental
The powder samples of LaMgAl11O19:Cr3+, Nd3+ phosphors were
obtained by a conventional solid-state reaction starting from La2O3
(99.9%), Al(OH)3 (99.9%), MgO (99.9%), Cr2O3 (99.9%) and Nd2O3
(99.9%). Among them, the La2O3 powders, which could absorb
atmospheric water rapidly, were weighed immediately after
heating at 800
C for 3 h. These raw materials were subsequently
mixed and ground together by grinding in an agate mortar. They
were sintered at 1600
C for 4 h for the first time. Then the powder
samples were ground and heated again at 1600
C for 4 h and 8 h,
respectively. Finally, we got the powder samples for future
measurement after three times’ sintering.

http://dx.doi.org/10.1016/j.materresbull.2015.09.031
0025-5408/ ã 2015 Elsevier Ltd. All rights reserved.
10 J. Zhu et al. / Materials Research Bulletin 74 (2016) 9–14

Fig. 1. The XRD patterns of LaMgAl11O19:Cr3 samples: (a) first time, 4 h; (b) second time, 4 h; (c) third time, 8 h.

The samples were identified by the X-ray powder diffraction
(Philips X’PertPW-3040) with Cu Ka radiation (l = 0.15406 nm)
operating at 45 kV and 40 mA. The photoluminescence excitation
(PLE) and emission (PL) spectra at room temperature were
measured on an Edinburgh FLSP920 Fluorescence Spectropho-
tometer with a Hamamatsu S900-R (red sensitive version)
photomultiplier tube (PMT). The decay curves were recorded on
the same instrument (FLSP920), and a mF900 flash lamp was used
as the excitation resource.
3. Results and discussion
Fig. 1 shows the XRD patterns of LaMgAl11O19:Cr3+ sample
obtained by different sintering batches and the PDF card (No.
26-0873) of LaMgAl11O19 is also presented for a comparison. From
Fig. 1a, the LaMgAl11O19 product synthesized at 1600
C for 4 h for
the first time exhibits a main phase of LaMgAl11O19, but some
amount of second phase LaAlO3 can be clearly found. After another
sintering at 1600
C/4 h, the diffraction peaks intensities of the

Fig. 2. The XRD patterns of phosphors La1xMgAl10.89O19:0.11Cr3+, xNd3+ (x = 0, 1%, 3%, 6%, 9% and 12%).
 J. Zhu et al. / Materials Research Bulletin 74 (2016) 9–14 11

These two bands can be assigned to the spin-allowed transitions

4
A2–4T1 and 4A2–4T2 of Cr3+, respectively. Fig. 3b shows the PL
spectra of La1xMgAl10.89O19:0.11Cr3+,xNd3+ phosphors when the
excitation wavelength is fixed at 419 nm. The sharp R-line emission
at 696 nm is assigned to 2E/4A2 transition of Cr3+. The weak bands
observed at 676 and 710 nm have been attributed to vibronic side
bands [22]. As can be seen from Fig. 3, it is very interesting to find
that the intensities of Cr3+ excitation and emission decreases when
the concentration of Nd3+ increases in La1xMgAl10.89O19:0.11Cr3+,
xNd3+. Fig. 4a shows the NIR PL spectra of the La1xMgA-
l10.89O19:0.11Cr3+,xNd3+ (x = 0–12%) phosphors. the NIR emission
originated from Nd3+:4F9/2/4I11/2 transition can be clearly observed
under the excitation of Cr3+:4T1 and 4T2 energy levels, which
indicates the energy transfer from Cr3+ to Nd3+. Under 419 nm
excitation, there is no NIR emission without Nd3+. With increasing
Nd3+ concentration, the emission intensity of Nd3+ increases,
maximizes at about x = 0.06, then decreases because of the
concentration quenching of Nd3+. On the contrary, Fig. 4b shows
the NIR PL spectra of the La0.97MgAl11(1y)O19:11yCr3+,3%Nd3+
phosphors by fixing Nd3+ concentration at 3% and changing Cr3+
content from 0 to 5%. There is also almost no NIR emission if the

Fig. 3. (a) PL spectra of La1xMgAl10.89O19:0.11Cr3+, xNd3+ (x = 0, 1%, 3%, 6%, 9% and

12%); (b) PLE spectra of La1xMgAl10.89O19:0.11Cr3+, xNd3+ (x = 0, 1%, 3%, 6%, 9% and
12%).

LaAlO3 decrease as shown in Fig. 1b. As can be seen in Fig. 1c, all the
second phase LaAlO3 disappeared when the samples were heated
at 1600
C/8 h for the third sintering. After sintering, smashing and
grinding and resintering, the raw materials can get full reaction,
then the single phase LaMgAl11O19 can be obtained. Therefore, we
should adopt the three times’ sintering technique in order to obtain
the pure phase of LaMgAl11O19, and all the following samples were
prepared via such a synthesis procedure as described in the
experimental section.
Fig. 2 demonstrates the XRD patterns of phosphors La1xMgA-
l10.89O19:0.11Cr3+,xNd3+ (x = 0, 1%, 3%, 6%, 9% and 12%). From Fig. 2,
it can be seen that the XRD patterns of all the as-prepared
phosphors are well-matched with the LaMgAl11O19 phase without
any other impurity phase. At the same time, the radii of Nd3+ ion
(0.98 Å) is very close to that of La3+ ion (1.03 Å) and the radii of Cr3+
(0.62 Å) is much closer to Al3+ (0.54 Å) instead of La3+. Therefore,
we conclude that Nd3+ and Cr3+ ions can be doped easily to replace
the La3+ and Al3+ ions in the LaMgAl11O19 lattice without any
structural changes.
The PLE spectra of the La1xMgAl10.89O19:0.11Cr3+,xNd3+ phos-
phors are shown in Fig. 3a. The concentration of the activator is
Fig. 4. (a) NIR PLE spectra of La1xMgAl10.89O19:0.11Cr3+, xNd3+ (x = 0, 1%, 3%, 6%, 9%
kept at 1% for Cr3+, and that for Nd3+ is changed from 0 to 12%. The and 12%); (b) NIR PLE spectra of La0.97MgAl11(1y)O19:11yCr3+, 3%Nd3+ (y = 0, 0.5%,
PLE spectra exhibit two intense bands centered at 419 and 566 nm. 1%, 3% and 5%).
12 J. Zhu et al. / Materials Research Bulletin 74 (2016) 9–14

6
1.2x10 70

(a.u.)
60

Energy transfer efiiciency (%)

3+
NIR emission intensity of Nd
5
9.0x10
50

5
40
6.0x10

30

5
3.0x10 20

10
0.0
0 2 4 6 8 10 12
3+
Concentration of Nd (% mol)
Fig. 5. The dependence of the Cr3+ emission, the Nd3+ NIR emission and the energy transfer efficiency of Cr3+–Nd3+ doping concentration for La1xMgAl10.89O19:0.11Cr3+, xNd3
+
(x = 0, 1%, 3%, 6%, 9% and 12%).

Nd3+ singly is doped into this system, and the NIR emission of Nd3+ In order to further understand the energy transfer process of
increase by increasing Cr3+, which also provides an evidence for the the Cr3+–Nd3+, Fig. 6 shows the representative Cr3+ decay curves
energy transfer from Cr3+ to Nd3+. The energy transfer efficiency (excited at 419 nm and monitored at 696 nm) of La1xMgA-
from Cr3+ to Nd3+ can be calculated based on the following l10.89O19:0.11Cr3+,xNd3+ phosphors. The luminescent decay curve of
expression [23,24]: all the samples can be fitted well with a biexponential function by
the following equation [30,31].
Ix
hT ¼ 1  ð1Þ    
I0 t t
I ¼ A1 exp þ A2 exp ð3Þ
here I0 and Ix are the corresponding emission intensity of donor Cr3
t1 t2
+
in the absence and the presence of the acceptor Nd3+, where I represents the luminescent intensity, A1 and A2 are
respectively, and hT is the calculation of the energy transfer constants, t is time, and t 1 and t 2 are the decay times for the
efficiency. It can be seen from Fig. 5 that the energy transfer exponential components. Using these parameters, the average
efficiency (hT) increases with the increasing Nd3+ concentration. decay time t can be determined by the formula given in the
The results of the energy transfer efficiency from Cr3+ to Nd3+ following:
under 419 nm excitation were calculated by Eq. (1) to be 13.2%,
ðA1 t 21 þ A2 t 22 Þ
20.9%, 37.2%, 52.0% and 65.2%, respectively. t¼ ð4Þ
In general, the resonant-type energy transfer from a sensitizer ðA1 t 1 þ A2 t 2 Þ
to an activator in the phosphor may take place by the exchange
interaction and electric multipolar interaction [25,26]. It is known
that if energy transfer takes the exchange interaction, the critical
distance between the sensitizer and activator should be shorter
than 5 Å [27]. The critical distance Rc for energy transfer from the
Cr3+ to Nd3+ ions was calculated using the concentration quenching
method. The critical distance Rc between Cr3+ and Nd3+ can be
estimated by the following formula suggested by Blasse [28,29]:
 
3V 1=3
Rc  2 ð2Þ
4pxc N
here N is the number of molecules in the unit cell, V is the unit cell
volume and xc is the critical concentration. For LaMgAl11O19 host,
N = 2, V = 594.8 Å3 and the critical concentration is about 0.1 from
the total concentration of Cr3+ and Nd3+ at which the energy
transfer efficiency is 0.5. According to the above equation, the
critical distance of energy transfer is estimated to be about 17.84 Å.
This value is much longer than 5 Å, indicating little possibility of
energy transfer via the exchange interaction mechanism. Thus,
energy transfer mechanism in this system is governed by the
Fig. 6. Ce3+ decay curves of La1xMgAl10.89O19:0.11Cr3+, xNd3+ (x = 0, 1%, 3%, 6%, 9%
electric multipolar interaction. and 12%) phosphors monitoring at 696 nm.
 J. Zhu et al. / Materials Research Bulletin 74 (2016) 9–14 13

14 14

12 12

10

3+
3+

R = 0.8756 10

Iso/Is of Cr
R = 0.9782
Iso/Is of Cr

8 8

6 6

4 4

2 2

2 4 6 8 10 12 0 2 4 6 8 10 12 14 16
CNd 3+
CNd
6/3
/10
3+

14 14

12 12
R = 0.9982
R = 0.9947
10 10
3+

3+
Iso/Is of Cr

Iso/Is of Cr

8 8

6 6

4 4

2 2

0 1 2 3 4 5 6 7 8 0 1 2 3 4
8/3 2 10/3 3
CNd 3+ /10 CNd 3+ /10
Fig. 7. The dependence of Is0/Is of Cr3+ on (a) C, (b) C6/3, (c) C8/3 and (d) C10/3.

The values of average decay times of the Cr3+ excited-state for
La1xMgAl10.89O19:0.11Cr3+,xNd3+ phosphors (x = 0, 1%, 3%, 6%, 9%
and 12%) were calculated to be 2.96, 2.57, 2.34, 1.86, 1.42 and
1.03 ms, respectively. It can be seen that the lifetime values for the
Cr3+ ions decreases monotonically as Nd3+ content increased,
which act as the strong evidence for the energy transfer from Cr3+
to Nd3+ ions.
According to Dexter’s energy-transfer formula of multipolar
interaction Reisfeld’s approximation the following relation can be
obtained by [32,33]:
h0
/ C n=3
h
where h0 and h are the emission quantum efficiency of Cr3+ in the
absence and presence of Nd3+, respectively; C is the concentration
of Nd3+, and n = 6, 8, or 10 for dipole–dipole, dipole–quadrupole, or
quadrupole–quadrupole interactions, respectively. The value h0/h
is approximately calculated by the ratio of related luminescence
intensities as [25].
Is0
/ C n=3
Is
where Is0 and Is are the luminescence intensities of Cr3+ in the
absence and presence of Nd3+, respectively, C is the concentration
of Nd3+. Plots of Is0/Is and Cn/3 based on the above equation are
shown in Fig. 7 The best linear behavior was observed when n is
equal to 8, indicating that energy transfer from Cr3+ to Nd3+ took
place via the dipole–quadrupole mechanism.
In order to demonstrated a clear schematic diagram on the
possible process for the usage of the spectral conversion of the
present phosphors, Fig. 8 comparatively gives the normalized PLE
spectrum of LaMgAl11O19:Cr3+, Nd3+ (red line), PL spectra of
LaMgAl11O19: Cr3+, Nd3+ (green line) and the AM 1.5G solar
ð5Þ spectrum (blue line) and spectral response of Si-based solar cell
(pink dot) are given as the background. It can be seen that the
LaMgAl11O19:Cr3+, Nd3+ phosphors can been excited successfully by
the intense sunlight range from 350 to 650 nm and emit near-
infrared light that match the Si-based solar cell very well. However,
many other spectral convert materials, such as co-doped YBO3:Ce3
+
, Yb3+, NaY(WO4)2:Yb3+, Pr3+ and KYF4:Tb3+,Yb3+ [34–36], can only
absorb the light from 300 to 400 nm in the short wavelength
region, which will restrict the application of these materials.
ð6Þ Therefore, the potential application for the spectral conversion in
14 J. Zhu et al. / Materials Research Bulletin 74 (2016) 9–14

AM 1.5 solar spectrum
3+ 3+
PLE of LaMgAl11O19:Cr , Nd
Intensity (a.u.)
Spectral response of c-Si
3+ 3+
PL of LaMgAl11O19:Cr , Nd
[6] B.S. Richard, A. Shalav, The role of polymers in the luminescence conversion of
sunlight for enhanced solar cell performance, Synth. Met. 154 (2005) 61–64.
[7] Q. Xia, M. Batentschuk, A. Osvet, P. Richter, D.-P. Ḧader, J. Schneider, C.J. Brabec,
L. Wondraczek, A. Winnacker, Enhanced photosynthetic activity in Spinacia
oleracea by spectral modification with a photoluminescent light converting
material, Opt. Express 21 (2013) A909–A916.

300 400 500 600 700 800 900 1000 1100
Wavelength (nm)
Fig. 8. Normalized PLE spectrum of LaMgAl11O19:Cr3+, Nd3+ (red line), PL spectra of
LaMgAl11O19: Cr3+, Nd3+ (green line). AM 1.5G solar spectrum (blue line) and
spectral response of c-Si (pink dot) are the background. (For interpretation of the
references to color in this figure legend, the reader is referred to the web version of
this article.)
the solar cell can be expected for the present LaMgAl11O19:Cr3+,
Nd3+ phosphors.
4. Conclusions
In summary, we have prepared LaMgAl11O19:Cr3+, Nd3+
phosphors by the solid state reaction. The pure phase of
LaMgAl11O19:Cr3+, Nd3+ phosphors can be obtained after three
times sintering. The phase structure and luminescence properties
have investigated in detail. The excitation spectra of the Cr3+ is
ranged from 350 to 650 nm, and then energy transfer occurs from
Cr3+ to Nd3+. The energy transfer can be proved by the decreasing
luminesence intensity and lifetime values of Cr3+ with increasing
codoping concentration of Nd3+. The energy transfer from the Cr3+
to Nd3+ ion has been demonstrated to be a resonant type via the
dipole–quadrupole mechanism in the Cr3+/Nd3+ co-doped LaM-
gAl11O19 phosphors. The energy transfer critical distance has also
been evaluated by the concentration quenching method. As the
Cr3+ has broadband absorption (350–650 nm) in the visible region
and Nd3+ can show strong NIR emission, the LaMgAl11O19:Cr3+,
Nd3+ phosphors were promising to act as spectral convertors for
silicon-based solar cell.
Acknowledgement
This present work was supported by the National Natural
Science Foundations of China (Grant Nos. 51272027, 51472028).
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