Ba3P5N10Br:Eu2+: A natural-white-light single emitter with a zeolite structure type

Article abstract of DOI:10.1002/anie.201410528

Illumination sources based on phosphor-converted light emitting diode (pcLED) technology are nowadays of great relevance. In particular, illumination-grade pcLEDs are attracting increasing attention. Regarding this, the application of a single warm-white-emitting phosphor could be of great advantage. Herein, we report the synthesis of a novel nitrido-phosphate zeolite Ba₃P₅N₁₀Br:Eu²⁺. Upon excitation by near-UV light, natural-white-light luminescence was detected. The synthesis of Ba₃P₅N₁₀Br:Eu²⁺ was carried out using the multianvil technique. The crystal structure of Ba₃P₅N₁₀Br:Eu²⁺ was solved and refined by single-crystal X-ray diffraction analysis and confirmed by Rietveld refinement and FTIR spectroscopy. Furthermore, spectroscopic luminescence measurements were performed. Through the synthesis of Ba₃P₅N₁₀Br:Eu²⁺, we have shown the great potential of nitridophosphate zeolites to serve as high-performance luminescence materials.

Full text of DOI:10.1002/anie.201410528

Angewandte
Chemie
DOI: 10.1002/anie.201410528
Zeolite Synthesis
Ba3P5N10Br:Eu2+: A Natural-White-Light Single Emitter with a Zeolite
Structure Type**
Alexey Marchuk and Wolfgang Schnick*
Abstract: Illumination sources based on phosphor-converted
light emitting diode (pcLED) technology are nowadays of
great relevance. In particular, illumination-grade pcLEDs are
attracting increasing attention. Regarding this, the application
of a single warm-white-emitting phosphor could be of great
advantage. Herein, we report the synthesis of a novel nitrido-
phosphate zeolite Ba3P5N10Br:Eu2+. Upon excitation by near-
UV light, natural-white-light luminescence was detected. The
synthesis of Ba3P5N10Br:Eu2+ was carried out using the
multianvil technique. The crystal structure of Ba3P5N10Br:Eu2+
was solved and refined by single-crystal X-ray diffraction
analysis and confirmed by Rietveld refinement and FTIR
spectroscopy. Furthermore, spectroscopic luminescence meas-
urements were performed. Through the synthesis of
Ba3P5N10Br:Eu2+, we have shown the great potential of
nitridophosphate zeolites to serve as high-performance
luminescence materials.
nitridophosphates exhibits a structural variety similar to or
even more diverse than that of silicates. The formal substi-
tution of O atoms by N atoms in a tetrahedral network
implies significant new structural possibilities. The structural
diversity of oxosilicates is limited to terminal or singly
bridging O atoms, whereas N atoms in nitridophosphates
may occur as N[1], N[2], N[3], or even N[4] atoms.[11] (The
superscripted numbers in square brackets following element
symbols define their coordination numbers.) Furthermore,
nitridic zeolites promise useful chemical and physical
properties (for example, adjustable acidity/basicity).
A
prominent example for these extended structural possibilities
of nitridophosphates as well as their potential in the field of
open-framework structures is the nitridic clathrate
P4N4(NH)4(NH3) that was discussed as a possible gas-storage
material.[12,13] Its network structure has been predicted for
silica but to date has only been found in this particular
nitride compound. Furthermore, two nitridic zeolites in the
compound class of nitridophosphates are known to date,
namely LixH12ꢀxꢀy+z[P12OyN24ꢀy]Xz (X = Cl, Br) and
Ba19P36O6+xN66ꢀxCl8+x (x ꢁ 4.54). Both represent unusual net-
work structure types, namely NPO (nitridophosphate one)
and NPT (nitridophosphate two), respectively.[14–17]
As a result of their high thermal and chemical stability as
well as highly cross-linked network structures, nitridic zeolites
are basically well suited as host lattices for Eu2+ doping.
Consequently, new interesting luminescent materials may be
expected with possible application in phosphor-converted
light-emitting diodes (pcLEDs). The constantly growing
relevance of pcLEDs makes further investigation of lumines-
cent materials an important research target. In particular,
white light sources based on LED technology are gaining
increasing attention. The Nobel Prize in Physics 2014 that was
awarded to Akasaki, Amano, and Nakamura “for the
invention of efficient blue light-emitting diodes which has
enabled bright and energy-saving white light sources” confirms
this assessment.[18] Several strategies are available to obtain
high quality pcLEDs for illumination. The strategy adopted in
industry is based on the multiphosphors-conversion
model.[19,20] In this case, for example, green (e.g.
Lu3Al5O12:Ce3+),[21] red (e.g. (Ba,Sr)2Si5N8:Eu2+),[22,23] and
yellow (e.g. Ca-a-SiAlON:Eu2+)[24,25] emitting phosphors are
mixed and coated on an InGaN semiconductor LED chip to
achieve white light. The main problem of this strategy,
however, is the differing thermal stability of the individual
phosphors, which often results in poor emission-color stabil-
ity. Moreover, the particle sizes of individual phosphor
materials have to be adapted to one another to avoid
agglomeration. Finally, the individual phosphors have to be
mixed very homogeneously in exact ratios. To alleviate these
Z
eolites find application in numerous technological areas
worldwide and have become an irreplaceable materials class
in modern industry. Classical zeolites, such as aluminosilicates
and aluminophosphates, are widely used, for example in the
fields of petroleum refining, in the petrochemical and fine
chemical industry as adsorbents, and as ion exchangers or
catalysts. Furthermore, this compound class also has the
potential for further applications in future technologies, for
example in sensors and electronic or optical systems.[1–6]
Prominent examples of the commercially most important
functional zeolites are Nax(H2O)16AlxSi96-xO192 (x < 27;
ZSM-5) and Na12(H2O)27[Al12Si12O48]8 (LTA), which exhibit
excellent chemical and thermal stability.[7,8]
Conventional oxidic zeolite structures are typically com-
posed of a three-dimensional network of vertex-sharing
[SiO4] and [AlO4] tetrahedra, in which a negative charge is
associated with each [AlO4] tetrahedron.[9,10] Given that the
element combination P/N is isoelectronic to Si/O, it is
reasonable to expect that the resulting compound class of
[*] A. Marchuk, Prof. Dr. W. Schnick
Department Chemie, Lehrstuhl fꢀr Anorganische Festkçrperchemie
Ludwig-Maximilians-Universitꢁt Mꢀnchen
Butenandtstrasse 5–13, 81377 Mꢀnchen (Germany)
E-mail: wolfgang.schnick@uni-muenchen.de
[**] We thank Dr. Peter Mayer for collecting single-crystal data, Petra
Huppertz and Detlef Wiechert (Lumileds Development Center
Aachen) for luminescence measurements, and Christian Minke for
EDX measurements. Furthermore, we gratefully acknowledge
financial support by the Fonds der Chemischen Industrie (FCI) and
the Deutsche Forschungsgemeinschaft DFG.
Supporting information for this article is available on the WWW
under http://dx.doi.org/10.1002/anie.201410528.
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difficulties, application of a single white-emitting phosphor
could be of great advantage. Several compounds, such as
Ba1.3Ca0.7SiO4:Eu2+,Mn2+,[26] Ba3MgSi2O8:Eu2+,Mn2+,[27] and
CaAl2Si2O8:Eu2+,Mn2+ [28] have been already investigated as
promising single-phase phosphors for near-UV white LEDs.
However, the co-doping with Eu2+ and Mn2+ ions may lead to
poor emission-color stability because of the different emitting
centers which exhibit different thermal-quenching behaviors.
In this Communication, we report the synthesis and
structural investigation of the novel nitridophosphate
Ba3P5N10Br with a zeolite-type structure. Doped with Eu2+,
Ba3P5N10Br exhibits natural-white-light luminescence upon
excitation by near-UV light, making this compound a promis-
ing candidate for use as a single white emitter in pcLEDs.
Ba3P5N10Br:Eu2+ was synthesized by the reaction of
stoichiometric amounts of Ba(N3)2, BaBr2, and P3N5 accord-
ing to Equation (1). EuCl2 (2 mol%) was used as the doping
agent. The synthesis was carried out using a Walker-type
multianvil assembly and a 1000 t hydraulic press at pressures
between 1 and 5 GPa and 10008C for 30 minutes.[29] Through
the thermolysis of Ba(N3)2 a high N2 partial pressure is
available. It prevents P3N5 from dissociation into its compo-
site elements under high pressure at reaction temperatures
above 10008C.[30] At ambient pressure, P3N5 already decom-
poses at temperatures above 8508C. The product was
obtained as an air-stable colorless (light yellow when doped
with Eu2+) crystalline solid (see Figure 1). To grow single
To clarify the chemical composition of the product,
energy-dispersive X-ray (EDX) spectroscopy has been car-
ried out. No elements other than Ba, P, N, and Br were
detected. The determined atomic ratio Ba/P/N/Br is in good
agreement with the predicted composition Ba3P5N10Br (see
Table S1 in the Supporting Information).
The crystal structure of Ba3P5N10Br:Eu2+ was solved and
refined from single-crystal X-ray diffraction data in the
orthorhombic space group Pnma (no. 62) using direct
methods.[33] As a result of the elongated displacement
ellipsoid of the N11 atom, it was possible to refine a split
position for this atom with occupancy of approximately 0.5
each (Figure S1). All atom positions were refined anisotropi-
cally. As a result of the small crystal size as well as significant
differences in the X-ray scattering power of N atoms com-
pared to Ba and Br atoms, a common anisotropic displace-
ment parameter for the N atom positions was refined. The
accuracy of the structure elucidation as well as phase purity of
the product was confirmed by Rietveld refinement (Figure 2).
Figure 2. Experimentally observed (black line) and calculated (light
gray line) X-ray powder diffraction pattern, positions of Bragg reflec-
tions (vertical bars) and difference profile (dark gray line) for the
Rietveld refinement of Ba3P5N10Br:Eu2+
.
Figure 1. SEM images of crystals of Ba3P5N10Br:Eu2+ measured on
a) 1mm or b) 10 mm scale.
The crystallographic details are summarized in the Support-
ing Information.
crystals of the compound which are large enough to be
suitable for single-crystal X-ray diffraction, the heating time
was increased up to 200 minutes.
The crystal structure of Ba3P5N10Br consists of a network
of all-side vertex-sharing PN4 tetrahedra, leading to three-
dimensional achter-ring channels, according to the nomencla-
ture introduced by Liebau.[10] These channels contain alter-
nately Ba and Br atoms (Figure 3). The PN4 tetrahedra form
condensed dreier, vierer, and achter rings. This condensation
results in turn in two slightly distorted CBUs (composite
building unit) both forming 344286 cages (Figure 4). Both
cages exhibit the same basic atom arrangement but differ
slightly in their degree of deformation.
The centers of the CBUs are occupied by Br atoms, which
are coordinated by six Ba atoms in a distorted octahedral
arrangement (Figure 4). These BaN6 octahedra are connected
to each other via shared edges forming a three-dimensional
network.
15 BaðN3Þ2 þ 3 BaBr2 þ 10 P3N5 ! 6 Ba3P5N10Br þ 40 N2
ð1Þ
At ambient pressure, the synthesis of Ba3P5N10Br was also
accomplished by heating a mixture of BaBr2, amorphous
HPN2, and NH4Br as mineralizer in evacuated and sealed
silica ampoules to 8008C for 84 h. A similar approach has
been already applied for the synthesis of various nitridophos-
phates exhibiting a sodalite-type structure.[16,31] However, by
this procedure Ba3P5N10Br was only accessible as a minor side
phase. To obtain a single-phase product, the reaction con-
ditions as well as the starting materials have to be optimized.
In addition to the starting materials named above, BaH2 and
P(NH2)4Br[32] may be used.
The framework topology of Ba3P5N10Br was determined
by the TOPOS software.[34] It is represented by the point
symbol (3.4.5.83)4(32.84) and is analogous to the topology of
2
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onal bipyramids. In contrast, the coordination spheres of
Ba4 and Ba5 centers represent irregular polyhedra consisting
of eight N atoms (2.713–3.347 ꢀ) and two Br atoms (3.360–
3.668 ꢀ). The N11a and N11b atoms represent one split
ꢀ
position of the N11 position. All bond lengths Ba N and
ꢀ
Ba Br correspond to those in other known compounds as
well as to the sum of the ionic radii.[36–40]
2+
ꢀ
The absence of N H groups in Ba3P5N10Br:Eu was
confirmed by FTIR spectroscopy (Figure S2). The FTIR
spectrum shows several groups of bands below 1500 cmꢀ1.
ꢀ ꢀ
These can be attributed to symmetric and asymmetric P N P
stretching modes, respectively. However, there are no
absorption bands around 3000 cmꢀ1, which would be typical
ꢀ
for N H valence vibrations.
By doping of Ba3P5N10Br with Eu2+ ions, natural-white-
light luminescence was detected upon excitation by near-UV
light (l = 400 nm). Figure 6 displays the excitation and
emission spectra of Ba3P5N10Br:Eu2+ crystallites. The excita-
tion spectrum reveals a maximum at l = 396 nm. Thus, this
compound can be effectively excited by near-UV light.
Excitation at l = 400 nm results in an emission spectrum
with two bands: one in the blue spectral region centered at l =
472 nm, and the other in the yellow spectral region centered
at l = 582 nm. The values of the full width at half maximum
(FWHM) are approximately 1502 cmꢀ1 (for the band at l =
472 nm) and 2374 cmꢀ1 (for the band at l = 582 nm). The
presence of two emission bands can be explained by
occupation of Eu2+ ions on different Ba lattice sites. The
example of Ba3MgSi2O8:Eu2+,Mn2+ demonstrates that the
differences in the coordination polyhedra of the different
Ba lattice sites has a strong influence on the number of
emission bands.[27] The combination of both emission bands
generates the resulting natural-white-light luminescence of
the title compound with a correlated color temperature
(CCT) of 3384 K, lumen equivalent of 372 lm/W, and CIE
Figure 3. Crystal structure of Ba3P5N10Br, viewed along [100]. Atom
colors: Ba=light gray, Br=black, PN4 tetrahedra=dark gray.
Figure 4. Topological representation of the two different 344286 cages
with cage content in Ba3P5N10Br with each connecting line representing
ꢀ ꢀ
a P N P bond. Atom colors (spheres): Ba=light gray, Br=black.
the JOZ zeolite framework type.[17,35] Despite
this structural analogy Ba3P5N10Br is not
porous and thus not prone to sorption of
water and hydrolysis.
ꢀ
The P N bond lengths range between 1.607
and 1.637 ꢀ and lie in the range of those
usually observed in similar nitridophos-
phates.[36,37] The N-P-N angles vary between
99.4 and 119.38 and thus differ slightly from the
regular tetrahedral angle. However, the range
is typical of other nitridophosphate zeo-
lites.[15,16]
The crystal structure of Ba3P5N10Br con-
tains five different crystallographic Ba posi-
tions, whose coordination spheres are shown in
Figure 5. Ba1 is coordinated ninefold by seven
N atoms (2.790–3.314 ꢀ) and two Br atoms
(3.341 and 3.391 ꢀ). The Ba2 and Ba3 posi-
tions are coordinated by six N atoms (2.753–
Figure 5. Coordination polyhedra and corresponding bond lengths [ꢂ] of the a) Ba1,
b) Ba2, c) Ba3, d) Ba4, and e) Ba5 positions in the crystal structure of Ba3P5N10Br.
3.009 ꢀ) and two Br atoms (3.174–3.241 ꢀ),
respectively, forming slightly distorted hexag- Thermal ellipsoids are set at 70% probability.
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Figure 6. Excitation (gray) and emission (black) spectra of
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In this Communication we presented a novel nitridophos-
phate Ba3P5N10Br with a zeolite-type structure. We were able
to characterize this compound by single-crystal X-ray dif-
fraction, powder X-ray diffraction, FTIR, and EDX spectros-
copy. The topology of Ba3P5N10Br corresponds to that of the
JOZ zeolite structure type. Doped with Eu2+, the title
compound exhibits natural-white-light luminescence upon
excitation by near-UV light. This feature makes
Ba3P5N10Br:Eu2+ a promising candidate for use as a single
white emitter in pcLEDs. Moreover, using the example of
Ba3P5N10Br:Eu2+, we have demonstrated that nitridic zeolites
are well suited as host lattices for high-performance lumines-
cence materials. Consequently, the synthesis of isotypic
compounds M3P5N10X:Eu2+ by the exchange of halide ion X
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Received: October 28, 2014
Revised: November 30, 2014
Published online: && &&, &&&&
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[33] Crystal data for Ba3P5N10Br: crystal size: 0.010 ꢂ 0.020 ꢂ
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13.2240(13), c = 13.8030(14) ꢀ, V= 2293.7(4) ꢀ3, Z = 8, 1diff
=
4.557 gcmꢀ3
,
Bruker
D8
Venture,
Mo-Ka radiation
(71.073 pm), multi-scan absorption correction, 31838 reflections,
Keywords: high-pressure chemistry ·
high-temperature chemistry · luminescence · nitrides · zeolites
2354 independent reflections, Rint = 0.0735, least-squares refine-
.
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2
2
4
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Communications
Zeolite Synthesis
Under pressure: A nitridophosphate zeo-
lite Ba3P5N10Br was synthesized by a high-
pressure/high-temperature reaction at
pressures between 1 and 5 GPa and
10008C and investigated by single-crystal
X-ray diffraction (see picture; Br=purple,
Ba=gray, PN4 tetrahedra=green).
A. Marchuk, W. Schnick*
&&& — &&&
Ba3P5N10Br:Eu2+: A Natural-White-Light
Single Emitter with a Zeolite Structure
Type
Doped with Eu2+ ions, it exhibits natural-
white-light luminescence as a single
emitter upon excitation by near-UV light.
6
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