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Effects of Carbon and Oxygen Impurities on

Luminescence Properties of BCNO Phosphor
Article in Journal of the American Ceramic Society January 2014
Impact Factor: 2.61 DOI: 10.1111/jace.12645

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J. Am. Ceram. Soc., 97 [1] 246250 (2014)

DOI: 10.1111/jace.12645
2013 The American Ceramic Society

Journal

Effects of Carbon and Oxygen Impurities on Luminescence

Properties of BCNO Phosphor

Xinghua Zhang, Lanlan Li, Zunming Lu, Jing Lin, Xuewen Xu, Yuanhui Ma, Xiaojing Yang,
Fanbin Meng, Jianling Zhao, and Chengchun Tang
School of Material Science and Engineering, Hebei University of Technology, Tianjin 300130, China
eects of carbon and oxygen impurities were investigated by
experimental and theoretical points of view. In experimental
part, BN was prepared using sodium borohydride (NaHB4)
and ammonium chloride (NH4Cl) as raw materials (RM)
without carbon and oxygen elements. In addition, BCNO
phosphors were prepared by urea combustion method12 using
boric acid (H3BO3), urea (CON2H4), and polyethylene glycol
(PEG) as RM. The spectra properties of BN and BCNO
phosphors with dierent PEG masses were investigated. In
theoretical part, the electronic structures of BN and BCNO
were calculated with rst-principle calculations and the
eects of carbon and oxygen impurity levels were discussed.
Finally, an energy level diagram was given to explain the
eects of nitrogen vacancies, carbon and oxygen impurities
on the luminescence properties of BCNO phosphors.

The BN and BCNO phosphors were prepared at 750C using

dierent methods and their structure and luminescent properties were investigated. All the prepared samples were turbostratic boron nitride structure. The SEM and high-resolution
TEM images show that the BCNO phosphors are polycrystalline in nature and include some nanocrystals. The carbon and
oxygen impurities have great eects on the excitation, emission, and absorption spectra of BN and BCNO phosphors. The
rst-principle calculations results indicate that the carbon and
oxygen impurities will produce energy levels in the band gap,
which can aect the spectra properties of BCNO phosphors.
The spectra properties of BN and BCNO phosphors can be
well explained by a simplied energy level diagram.

I.

Introduction

ORON nitride (BN) especially hexagonal BN-based materials13 have emerged as promising phosphors without
rare-earth doping. To modulate the emission spectra of BN,
much eort has been devoted to the development of boron
carbon nitride (BCN) materials.47 Both theoretical and
experimental results show the adjustable luminescence properties of BCN materials.810 However, the photoluminescence
(PL) intensity and quantum eciency of the BCN compounds are very low.11 Recently, Okuyama12 has synthesized
boron carbon oxynitride (BCNO) phosphors with high quantum eciency and tunable spectra using urea combustion
method. The BCNO phosphors have many advantages13 such
as low sintering temperatures (below 900C) under atmosphere pressure, low cost and nontoxicity, wide range of excitation from short ultraviolet to blue, and emission spectra
from violet to near-red regions, respectively.
BCNO phosphors have great potential applications in general lighting, automobiles, white light-emitting diode, phosphorus pigments, biological imaging, and DNA labeling.1416
However, the luminescence mechanism of BCNO phosphor
remains unclear at present. Up to now, there are two possible emission mechanisms for BCNO phosphors, one possible
emission mechanism is that the emission of BCNO phosphors may be induced by the closed-shell BO and BO2
anions that act as high-eciency luminescence centers.17 The
other possible emission mechanism is attributed to the impurity defects especially nitrogen vacancies in the BCNO nanocrystals which is responsible for the observed PL
properties.18 In addition to the nitrogen vacancies, the carbon and oxygen impurities also have great inuence on luminescence properties of BCNO phosphors. In this study, the

II.

Experiments

BN was prepared at 750C using NaBH4 and NH4Cl as RM.

NaBH4 and NH4Cl were milled suciently and pressed into a
disk. The disk was put into a crucible with a lid and placed in
furnace when the furnace increased to 750C. The disk was sintered at 750C for 12 h. BN was obtained after milling and
removing NaCl by washing the prepared compound, which
was dened as S1. The BCNO phosphors were prepared by
urea combustion method. First, the boric acid (B source), urea
(N source), and PEG (H(EG)nOH with Mw = 10 000, C
source) were dissolved in deionized water, and then the solution was stirred for 6 hours to form clear solution. Second, the
clear solution was heated to over 100C to evaporate water,
and solid precursor was obtained. At last, the solid precursor
was sintered at 750C for 45 min under atmosphere. After
washing and drying, the BCNO phosphors were obtained. In
this study, the boric acid and urea were xed at 0.02 and
0.10 mol, respectively, and the mass of PEG (10 000) was
changed from 0 to 1.4 g. The BCNO phosphors were prepared
with dierent masses of PEG (10 000) MPEG = 0, 0.2, 0.6, 0.9,
1.0, 1.1, and 1.4 g, which were dened as S2, S3, S4, S5, S6, S7,
and S8, respectively.
The phase structure of BN and BCNO phosphors was characterized by powder X-ray diraction (XRD) (Rigaku Ultima
IV, Tokyo, Japan). The morphology of the phosphors was
measured by a scanning electronic microscope (SEM, S4800,
Hitachi, Tokyo, Japan). The microstructure was measured by
a transmitted electronic microscope (TEM, JEM2100F,
JOEL, Tokyo, Japan). The excitation and emission spectra of
BN and BCNO phosphors were measured by a Hitachi
F7000 spectrophotometer (Tokyo, Japan). The ultraviolet
visiblenear-infrared (UVVISNIR) absorption spectra were
measured by a spectrophotometer (Hitachi, U4100). All the
measurements were performed at room temperature.

J. McKittrickcontributing editor

III.
Manuscript No. 33501. Received July 14, 2013; approved September 4, 2013.

Author to whom correspondence should be addressed. e-mail: zhangxinghua@hebut.edu.cn

Results and Discussion

Figure 1(a) shows the typical XRD patterns of S1 and S6 samples. The XRD patterns show the formation of turbostratic

246

January 2014

Eects of Carbon and Oxygen

247

(a)

(b)

Fig. 2. Excitation spectra monitored at 390 nm and emission

spectra excited by 215, 280, and 350 nm for specimen S1.

Fig. 1. (a) XRD patterns of specimens S1 and S6; (b) SEM image
and high-resolution TEM image (inset) of S6 sample.

boron nitride (t-BN) structure with two dominated peaks at

26.6 and 43.6 corresponding to (002) and (10) ((101) and
(100)) reections, respectively. Moreover, there were two distinct peaks for S1 at 31.7 and 45.4 which corresponding to
the crystal faces of cubic NaCl (JCPDS Card No. 05-0628) at
(200) and (220), respectively. The two peaks at 31.7 and 45.4
were induced by the NaCl remainder without washing out in
S1 sample. The XRD results indicated all the prepared samples with two methods are turbostratic boron nitride structure. Figure 1(b) shows the SEM image and high-resolution
TEM image [inset of Fig. 1(b)] of S6 sample. The particle
shape is irregular and its size changes from a hundred nanometers to several hundreds of nanometers. The high-resolution
TEM image indicates that the BCNO phosphor is polycrystalline in nature and is composed of several distinct nanocrystals,
each of which is approximately less than 5 nm in size.
Figure 2 shows the excitation spectrum monitored at
390 nm and emission spectra excited by 215, 280, and
350 nm of the S1 sample. As shown in Fig. 2, a very broad
band centered at 335 nm appears and superimposes with the
structured emission under a 215-nm excitation. For 280-nm
excitation, a structured band centered at 318 and 333 nm is
observed. The structured emission spectra between 300 and
350 nm excited by 280 and 215 nm are induced by the internal defects of BN, mostly by nitrogen vacancy.19 There is
also a broad band centered at 385 nm in the emission spectra
under a 280-nm excitation, and the emission peak is located
at 390 nm when the excitation wavelength is 350 nm. The
emission peak centered at 390 nm is likely induced by the
oxygen related defects.20 For excitation spectra of S1 sample
monitored by 390 nm, there are three distinct excitation
peaks centered around 215-, 280-, and 350-nm emission,
respectively. Although there are no carbon and oxygen elements in RM, oxidation is evidently inevitable in preparing

Fig. 3. Excitation spectra monitored at 390 nm and emission

spectra excited by 280, 315, and 350 nm for specimen S2.

S1 sample; therefore, both excitation and emission spectra

are originated from B-, N-, and O-related defects. The
215-nm (~5.7 eV) excitation is corresponding to the band
gap transition of BN, and the 280-nm (~4.4 eV) excitation is
likely to be correlated with intrinsic defects of BN such as N
vacancy, whereas the 350 nm (~3.5 eV) excitation may be
correlated with the oxygen-related defects in BN.2123
Figure 3 shows the excitation and emission spectra of S2
sample using boric acid and urea as RM. As there are carbon elements in urea and oxygen elements in boric acid, the
eects of carbon and oxygen cannot be ruled out for S2 sample. In the excitation spectra monitored at 390 nm, there are
two obvious peaks centered at 315 and 350 nm, and a shoulder peak located at 280 nm, respectively. Comparing with S1
sample, there is no 215-nm excitation peak for S2 sample,
which is probably induced by the carbon element of urea.
The little carbon may aect the electronic structure of BN,
which can be reected by UVVISNIR absorption spectra
(as shown in Fig. 5). In addition, a new excitation peak centered at 315 nm appears which may be correlated with carbon impurity defects.24 The 280-nm excitation is originated
from nitrogen-related defects and the 350-nm excitation is
likely induced by oxygen-related defects. The emission spectra of S2 sample excited by 280 nm are also dierent from
that of S1 sample. No structured emission band appears
between 300 and 350 nm, and a broad band centered at
365 nm displays between 300 and 500 nm. The broad emission spectra can be decomposed into two Gaussian curves:
one curve centered at 350 nm, which is mostly induced by
carbon-related defects, and the other curve centered at

248

Journal of the American Ceramic SocietyZhang et al.

Vol. 97, No. 1

(a)

(b)

Fig. 4. (a) Normalized excitation spectra monitored at the emission

peak position for specimens S3S8, respectively; (b) Normalized
emission spectra of S3S8 samples, and the inset shows the emission
peak position as a function of PEG(10 000) mass.

400 nm that may correspond to oxygen-related defects. The

above phenomenon can be clearly seen in the emission spectra excited by 315 nm, and the spectra are composed of contributions of two luminescence centers. The emission spectra
excited by 350 nm show one broad emission centered at
390 nm, which is induced by the oxygen-related defects. For
315-nm excitation, the emission spectrum is induced by the
transition from nitrogen-related defects levels to carbon and
oxygen-related defects levels. While for 350-nm excitation,
the one broad emission spectrum is mainly originated from
the transition from nitrogen-related defects levels to oxygenrelated defects levels.
Figure 4(a) shows the normalized excitation spectra monitored at the emission peak position for specimens S3S8,
respectively. The excitation spectrum of S3 sample monitored
at 385 nm shows a broad band between 280 and 360 nm.
With increasing mass of PEG (10 000) (specimens S4 and
S5), the excitation spectra show two obvious bands centered
at 280 and 370 nm, respectively. The 280-nm excitation is
related to the intrinsic defects of BCNO, mostly nitrogen
vacancy, and the 370-nm excitation is mostly correlated with
carbon- and oxygen-related defects. For further increasing
PEG (10 000) mass (specimens S7 and S8), the 280- and 370nm excitation peaks change to shoulder peaks, and a new
shoulder peak centered at 235 nm appears for S8 which may
be induced by the superuous carbon source. Compared with
specimens S1S2, specimens S3S7 have excitation peaks in
320400 nm range which change from 350 to 370 nm. The
change in excitation peak position is induced by the addition
of PEG (10 000) in preparing BCNO. With addition of PEG,
the electronic structure of BN is changed and carbon and
oxygen impurity levels will appear in band gap, which can be
veried by the calculation results (as shown in Fig. 6).

Fig. 5. UVVISNIR absorption spectra of specimens S1S7 in the

range 2401400 nm.

Figure 4(b) shows the emission spectra of S3S8 samples, and

the inset of Fig. 4(b) shows the emission peak position as a
function of PEG (10 000) mass. For S3 and S8 samples, the
emission spectra are in the range between 300 and 500 nm,
whereas the emission spectra for specimens S4S7 are in the
range between 400 and 600 nm. The peak position increases
from 385 nm for S3 to 545 nm for S6 and then decreases to
390 nm for S8, the redshift of emission peak is induced by
the composition of BCNO and especially the carbon impurity
concentration,25,26 and the blueshift of emission peak is
induced by the superuous carbon impurity.27 For S7 and S8
samples, the carbon concentration is saturated and the
redundant carbon has negative eects on the luminescence
properties of BCNO phosphors, which induces the blueshift
of emission peak and decrease in emission peak intensity.28
With further increasing carbon source content, there will be
no emission peak for the BCNO phosphors. From the excitation and emission spectra of BCNO phosphors, it can be
concluded that the spectra of BN is induced by the intrinsic
defects of BN and oxygen impurity defects, whereas the spectra of BCNO phosphors are mainly induced by the carbon
and oxygen impurity defects, which can be veried by the
absorption spectra and rst-principle calculations.
Figure 5 shows the UVVISNIR absorption spectra of
specimens S1S7 in the range 2401400 nm. For S1 sample,
the absorbance decreases with increasing wavelength and a
shoulder peak located at 270 nm appears in absorption spectra (inset of Fig. 5), which is induced by the intrinsic defects
of BN (mostly nitrogen vacancy). The band gap absorption
of BN is not observed as the spectrum is tested from
240 nm. There is a shoulder peak around 400 nm, which is
likely induced by the oxygen impurity level. For S2 sample,
the tendency of absorption spectra is similar to that of S1,
and an absorption peak centered at 260 nm appears, which
is possibly induced by the nitrogen vacancy level. For S3
sample, there are a shoulder peak located at 265 nm and two
peaks centered at 295 and 410 nm, respectively. The 265-nm
absorption is related to the intrinsic defects level of BN. The
295-nm (~4.2 eV) absorption is induced by the transition
between carbon impurity level and conduction band as carbon impurity will produce an energy level of ~4.1 eV below
conduction band in BN.29,30 The absorption peak centered at
410 nm (~3.0 eV) is possibly induced by the carbon and oxygen impurity defects. The nitrogen vacancy has two dierent
types, one type is three-boron center which introduces trapping levels at 1.0 eV below conduction band, and another
type is one-boron center which introduces trapping levels at
0.7 eV below conduction band.31,32 The 410-nm absorption
may be induced by the transition from carbon impurity level
to nitrogen vacancy level, and oxygen impurity level may
also have a contribution to the absorption.33 With increasing

January 2014

249

Eects of Carbon and Oxygen

(a)

(b)

(c)

Fig. 6. (a) Total density of state of BCNO and inset shows the
conguration of BCNO; (b) partial density of state of BCNO; (c)
schematic energy level diagram of BCNO phosphors.

MPEG, the 265- and 295-nm absorption peaks become not

obvious, and a broad absorption band in 250700 nm range
appears. The broad absorption spectra of BCNO phosphors
may be induced by the broadening of carbon and oxygen
impurity defects levels.
To better understand the BCNO phosphor, we performed
density functional theory calculations to explore the eects
of the carbon and oxygen impurities on the band structure of
BN bulk. Because of the known limitations of the ab initio
calculation when applied to systems involving large number
of atoms, a 5 9 5 9 2 supercell is chosen as a representative
of BN bulk. On the basis of the present experimental results
of BCNO, we replaced one nitrogen atom with carbon atom
and the other near nitrogen with oxygen atom to model the
partially carbon- and oxygen-doped BN [as shown in inset of
Fig. 6(a)]. In our studies, the band gap for pristine BN is calculated to be 4.1 eV, which achieves good agreement with
previous studies, indicating that the methodology adopted in
this work can give a reliable description of electronic structure
of BN bulk. As shown in Fig. 6(a), carbon- and oxygen-doped
BN is still a semiconductor and substitutional impurity induces
the occupied impurity states in the gap region which located
below conduction band for ~3 eV. Therefore, it is expected
that the carbon and oxygen substitutional doping will result in
pronounced modication in the electronic structure and optical properties of BN systems. From the partial density of state
[PDOS, Fig. 6(b)], the impurity band is not only contributed
by carbon and oxygen atoms but also donated by the boron
and nitrogen atoms near to the dopant.

On the basis of above results, a simplied energy level diagram can be tentatively constructed to explain the luminescence mechanism for BN and BCNO phosphors, as shown in
Fig. 6(c). For BN sample, there is no carbon-related levels,
and the 215-nm (~5.8 eV) excitation for S1 is induced by the
band gap transition. Nitrogen vacancy levels called threeboron center (VN3) and one-boron center (VN1) will appear
below conduction band 1.0 and 0.7 eV, respectively, and the
280-nm (~4.4 eV) excitation is induced by the transition from
valence band to nitrogen vacancy levels for all the samples.
In addition, oxygen impurity is inevitable in preparing BN
and it may produce an energy level of ~4.5 eV below the
conduction band. The 350-nm (~3.5 eV) excitation for specimen S1 may be induced by the transition from oxygen impurity levels to nitrogen vacancy levels. For BCNO samples,
when the carbon impurity concentration is little (S2), carbonrelated defects will produce an energy level of ~4.1 eV below
conduction band. Except 280- and 350-nm excitation peaks,
a 300-nm (~4.1 eV) excitation peak appears, which is induced
by the transition from carbon-related levels to conduction
band. With increasing carbon source, the 300-nm excitation
peak disappears, substituted by a broad excitation band
between 280 and 350 nm, which is probably induced by the
broadening of carbon-related levels. The emission spectra
can also be explained by the energy level diagram. For S1
sample, the emission is mainly induced by the transition from
nitrogen vacancy levels to oxygen impurity levels. For S2
sample, carbon impurity levels appear and the emission is
mainly induced by the transition from nitrogen vacancy levels to carbon impurity levels. With further increasing carbon
source, the carbon-related levels become broader and the carbon-related levels may shift with carbon impurity concentration in the range 2 ~ 3 eV, which results in the changeable
emission spectra of BCNO phosphors.21,24,34 The absorption
spectra are also correlated with the nitrogen vacancy levels,
carbon- and oxygen-related levels, which can be understood
by the energy level diagram.

IV.

Conclusions

In summary, the BN and BCNO phosphors were prepared

and the eects of carbon and oxygen impurities on the luminescence properties were investigated. Both BN and BCNO
samples were turbostratic boron nitride structure. The excitation spectra were changed from separated excitation peaks
for BN to a broad excitation band in 250400 nm for
BCNO, and the emission peak position of BCNO shifted to
long wavelength and then to short wavelength with increasing PEG mass. The absorption peak was narrow and located
around 260 nm for BN, while it became not obvious for
BCNO and a broad absorption band appeared in the range
250700 nm with increasing PEG mass. The theoretical calculation and experimental results indicated that the carbon
and oxygen might introduce impurity levels in the band gap
of BN, which has great eects on spectra properties of
BCNO. The spectral properties of BN and BCNO phosphors
could be explained well by a tentatively simplied energy
level diagram.

Acknowledgments
This work was supported by the National Natural Science Foundation of China
(nos. 51172760, 51171056, 11104073, and 51272064) and Natural Science Foundation of Hebei Province of China (nos. E2011202012 and E2012202044) and
Tianjin Key Technology R&G Program (11ZCKFGX01300).

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