Ceramics International 45 (2019) 15406–15411

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Controlled synthesis and near-infrared upconversion properties of 3D self- T

assembled NdVO4 microcrystals
Tiyi Lei, Yuemei Li, Wei Zheng, Jun Dong, Rui Wang∗
School of Chemistry and Chemical Engineering, Harbin Institute of Technology, No. 92, Xidazhi Street, Nangang District, Harbin, Heilongjiang Province, 150001, People's
Republic of China

A R T I C LE I N FO A B S T R A C T

Keywords: The morphology of microcrystals has an important influence on optical property. In this work, new 3D self-
3D structure assembled NdVO4 microcrystals with sphere and stick-shape morphology have been prepared by hydro-thermal
NdVO4 method. Crystal growth mechanism has been studied. The morphology transformation of 3D self-assembled
Self-assemble NdVO4 microcrystals is dependent on the reacting time of the precursor. The morphology of NdVO4 microcrystal
Near-infrared upconversion
changes as reacting time goes on. Moreover, energy level transition mechanism in NdVO4 microcrystal has been
discussed. NdVO4 microcrystals realized near-infrared (NIR) emissions at 750, 808 and 853 nm under 980 nm
laser. This study proved that NdVO4 microcrystals have good application prospects such as bio-imaging, pho-
tochemical catalysis and silicon-based solar cell.

1. Introduction selective adsorption effect. However, these surfactants increase the

Recently, NIR upconversion luminescent materials have attracted
significant attention due to their excellent potential application in bio-
imaging and silicon-based solar cell [1–3]. The NIR emission spectrum
around 800 nm lies in the window of both optical transparency for
biological tissues and favorable absorption area for silicon-based solar
cells [4,5]. The suitable emission spectrum determines the promising
application in bio-imaging and silicon-based solar cell. Besides, the
light absorption range in NIR region also determines the potential ap-
plication in photochemical catalysis [6].
There exists a definite correlation between optical property and
crystal morphology in NIR upconversion luminescent crystals [7–9]. It
is of great importance to investigate the relationship between NIR up-
conversion luminescent property and morphology. Crystals with de-
signed and uniform morphology always lead to specific application
[10]. Nice adjustment of the morphology and size of NIR upconversion
luminescent crystals plays an important part in optical property
[11,12]. Controlled synthesis of NIR upconversion luminescent crystals
with uniform morphology provides a promising approach for the ap-
plication in bio-imaging and silicon-based solar cell [10,13].
Upconversion luminescent crystals with uniform morphology have
been fabricated by multifarious methods, such as hydro-thermal, sol-gel
process and solid-state reaction [14–16]. Kinds of surfactants are ap-
plied to control the direction and speed of crystal growth owing to their
quenching effect of NIR upconversion luminescence [17–19]. It is the
main compromise way to synthesize crystals uniting NIR upconversion
luminescent property and morphology [15,16].
To date, rare earth orthovanadates with 1D or 2D structure has been
extensively reported [20,21]. A few LnVO4 crystals with 3D structure
have been mentioned in the related references. [10] In fact, NdVO4
microcrystal with 3D structure could be synthesized by the biased
growth of NdVO4 precursor [10].
Herein, 3D self-assembled NdVO4 microcrystals are synthesized by
hydro-thermal method, without any surfactant. Proving a simplified
approach to fabricate crystals with better luminescent property and
uniform morphology. The growth mechanism of 3D self-assembled
NdVO4 microcrystals is further investigated. It finds that morphology of
NdVO4 microcrystals transforms from sphere to stick-shape and returns
to the sphere as reacting time goes on. Furthermore, it provides a
simplified method to synthesize 3D self-assembled NIR upconversion
luminescent microcrystals, which are of significant importance in fur-
ther application in bio-imaging, silicon-based solar cell and photo-
chemical catalysis.

∗
Corresponding author.
E-mail address: wangrui001@hit.edu.cn (R. Wang).

https://doi.org/10.1016/j.ceramint.2019.05.037
Received 6 April 2019; Received in revised form 20 April 2019; Accepted 6 May 2019
Available online 07 May 2019
0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
T. Lei, et al.
2. Experiment
2.1. Synthesis
In the current study, all of the chemicals, including neodymium
nitrate pentahydrate (Nd(NO3)3·5H2O), sodium vanadate (Na3VO4) and
absolute ethyl alcohol, were analytical purity, without any further
purify. 3D self-assembled NdVO4 microcrystals were prepared within
several simple procedures. Firstly, 2.5 mmol Nd(NO3)3·5H2O was dis-
solved into 10 ml ultrapure water, forming solution A. Secondly,
2.5 mmol Na3VO4 was added to solution A, forming NdVO4 precursor.
Then, the pH value of the precursor was adjusted with nitric acid so-
lution. Next, the precursor was moved into a 25 mL Teflon-lined auto-
clave after vigorously stirred for 1 h. After that, the autoclave was he-
ated in an oven. After the autoclave cooled naturally, the precipitant
was collected and then washed with ultrapure water and absolute ethyl
alcohol in turn 3 times. Finally, the fabricated NdVO4 crystals were
dried at 80 °C for 10 h in an oven.
2.2. Characterization
The structure and phase of NdVO4 crystals were characterized by X-
ray diffraction (XRD). The special functional group and UV absorption
spectrum were measured via FT-IR spectrum and UV absorption spec-
trum. The morphology and size of NdVO4 microcrystals were in-
vestigated by scanning electron microscopy (SEM). The upconversion
emission spectrum of NdVO4 microcrystals was recorded via 980 nm
solid laser.
3. Result and discussion
3.1. Structure and phase characterization
Fig. 1 shows the XRD patterns of NdVO4 microcrystals prepared at
pH 1, 2, 4 and 6. All the diffraction peaks in NdVO4 microcrystals
fabricated at pH 1, 2, 4 and 6 agree well with the standard card (JCPDS
NO 15–0769). There is no any other peak, indicating that t-NdVO4
microcrystals are synthesized. The crystallization degree of t-NdVO4
microcrystals varies with precursor pH value. T-NdVO4 microcrystals
have good crystallization degree at pH 2.
3.2. Functional group characterization
Fig. 2 performs the FT-IR spectrum of t-NdVO4 crystals with dif-
ferent pH. The FT-IR spectrum contains several major absorption peaks
with wave number ranging from 400 to 4000 cm-1. For pure t-NdVO4
Fig. 1. XRD graph of t-NdVO4 microcrystals at pH 1, 2, 4 and 6.
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Ceramics International 45 (2019) 15406–15411
Fig. 2. FT-IR spectra of NdVO4 microcrystals at pH 2, 4 and 6.
crystals, strong absorption peaks at 524 cm-1 and 794 cm-1 represent for
Nd-O and V-O in NdVO4 microcrystals, respectively [22]. These results
proved that the t-NdVO4 crystalline phase has been formed, which
matches well with the XRD analysis. Besides, absorption bands at
around 1384 cm-1, 1620 cm-1 and 3433 cm-1 are associated with the
stretching vibrations and bonds of OH and H2O, respectively [23]. The
existence of OH in NdVO4 microcrystals could contribute to fluores-
cence quenching, which is extremely harmful for upconversion emis-
sion intensity [24]. The intensities of the absorption bands at 3433 cm-1
and 1620 cm-1 for NdVO4 microcrystals at pH 2, 4 and 6 are practically.
As for absorption peak at around 1384 cm-1, the intensity decreases for
NdVO4 microcrystal at pH 2, indicating minimum quenching ion con-
centration for luminescence. Hence, better luminescent property of
NdVO4 microcrystal is obtained at pH 2.
3.3. Morphology and size characterization
SEM images of NdVO4 microcrystals at pH 1, 2, 4 and 6 together
with EDS graph of the 3D stick-shape self-assembled NdVO4 micro-
crystal are shown in Fig. 3. NdVO4 microcrystal at pH 1 is shown in
Fig. 3(a). It is depicted that self-assembled sphere NdVO4 microcrystals
have been fabricated. Sphere NdVO4 microcrystals are assembled with
nanometer cubes. It is the first occasion for sphere NdVO4 microcrystal
assembled with nanometer cubes to be reported. Fig. 3(b) indicates
NdVO4 microcrystal at pH 2. 3D stick-shape self-assembled NdVO4
microcrystal is fabricated without any surfactant. It provides an alter-
native for crystals combining good NIR upconversion luminescence and
uniform morphology. In Fig. 3(b), there is no extra material around the
3D stick-shape self-assembled NdVO4 microcrystal, indicating a high
degree of self-assembly. NdVO4 microcrystal at pH 4 is shown in
Fig. 3(c). Caking nanometer cube NdVO4 crystals around 50 nm is
found. NdVO4 crystal at pH 6 is indicated in Fig. 3(d). NdVO4 micro-
crystal could be seen with pretty irregular morphology. With pH value
decreasing from 6 to 2, uniform morphology of NdVO4 crystal obtained.
Comparing NdVO4 microcrystal at pH 2 and pH 1, they are both in 3D
self-assembled structure that has never been mentioned in the related
references. Stick-shape self-assembled NdVO4 microcrystal is better
assembled when compared to sphere self-assembled NdVO4 micro-
crystal. NdVO4 microcrystals with 1D or 2D morphology have been
widely prepared due to the natural growth of NdVO4 crystals. Com-
pared to NdVO4 microcrystal with 1D or 2D morphology, 3D self-as-
sembled NdVO4 microcrystals possess many excellent qualities. For
example, enhanced light harvesting, which is of profound significance
for upconversion luminescence [10,25]. The EDS analysis of NdVO4
microcrystal at pH 2 is shown in Fig. 3(e). It is palpable for the ex-
istence of Nd, V together with O elements in the compound.
SEM graphs of 3D self-assembled NdVO4 microcrystals with
T. Lei, et al. Ceramics International 45 (2019) 15406–15411

Fig. 3. (a), (b), (c) and (d) are the SEM graphs of NdVO4 microcrystals at pH 1, 2, 4 and 6 prepared by hydro-thermal method while Fig. 3(e) indicates the EDS
analysis of 3D stick-shape self-assembled NdVO4 microcrystal.

Fig. 4. SEM graphs of 3D self-assembled NdVO4 microcrystals reacting for different time, (a) 18 h; (b) and (c), 24 h; (d), (e) and (f), 36 h.

different reaction times is shown in Fig. 4. When reacting for 18 h, 3D
sphere self-assembled NdVO4 microcrystals are properly assembled
with nanometer cubes. There is no extra NdVO4 crystal around them,
indicating that nanometer NdVO4 cubes assemble well. Fig. 4(b) and (c)
indicate the NdVO4 microcrystal reacting for 24 h. A conclusion comes
to us that stick-shape NdVO4 microcrystal assembles well with 24 h.
Fig. 4(b) displays the clearer local version of stick-shape 3D self-as-
sembled NdVO4 microcrystal. Stick-shape 3D self-assembled NdVO4
microcrystal is assembled with nanometer cubes. The edge length of
NdVO4 nanometer cubes is about 200 nm. Fig. 4(d), (e) and (f) indicate
the SEM graphs of 3D self-assembled NdVO4 microcrystal with 36 h.
The transition morphology between stick-shape and sphere 3D self-as-
sembled NdVO4 microcrystal is described in Fig. 4(d). There are large
quantities of 3D self-assembled spheres on the self-assembled stick-
shape trunk. It can be concluded from Fig. 4(e) that sphere 3D self-
assembled NdVO4 is successfully fabricated by hydro-thermal method
with 36 h. In this graph, the sphere 3D self-assembled NdVO4 micro-
crystal assembles well with nanometer cubes. Compared with Fig. 4(a),
the defect on the surface of sphere disappears and these two kinds of
spheres look changed so much. The spheres shown in Fig. 4(a) look
more like uniform spheres composed with cubes and several defect is
obviously seen on the surface. As for the spheres shown in Fig. 4(e),
they look more like irregular spheres. Fig. 4(f) indicates sphere 3D self-
assembled NdVO4 microcrystals with 36 h. They are in extremely well-
distributed morphology. In summary, the morphology of 3D self-as-
sembled NdVO4 microcrystal changes with the reacting time.
A possible growth mechanism of 3D self-assembled NdVO4 micro-
crystal has been proposed. Clearly in Scheme 1, 3D NdVO4 micro-
crystals are well assembled with 18–36 h. NdVO4 nanometer cubes
successfully assemble several 3D self-assembled microcrystals and
complete a series of transformation in microscopic morphology. 3D
sphere NdVO4 microcrystal is composed with 18 h 3D stick-shape
NdVO4 microcrystal is proposed with 24 h. Intermediate morphology
has been discovered when reacting for 36 h, serving as an important
evidence for clarifying the growth mechanism of 3D self-assembled
NdVO4 microcrystal. As seen in Scheme 1, it is composed of stick-shape
3D self-assembled trunk and numerous 3D self-assembled spheres. It
also provides a viable interpretation for the growth mechanism of self-
assembled NdVO4 microcrystals. Sphere 3D self-assembled NdVO4
microcrystals also have been discovered with 36 h. The discovery de-
monstrates the well growth of 3D self-assembled NdVO4 microcrystal. A
possible growth mechanism of 3D self-assembled NdVO4 microcrystal

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Scheme. 1. shows the possible growth mechanism of 3D self-assembled NdVO4 microcrystals.

has been proposed. Furthermore, an experience is gained that the de-

gree of self-assembly increases with the prolonging of reacting time.

3.4. Optical property characterization

The ultraviolet absorption spectrum of NdVO4 microcrystals at pH

2, 4 and 6 is shown in Fig. 5(a). Ultraviolet absorption peak of VO43− at
around 300 nm is pretty overt for NdVO4 microcrystal at pH 2, in-
dicating potential down-conversion application [26,27]. For NdVO4
microcrystal at pH 4 and 6, there is not absorption peak around 300 nm.
The absorption peaks around 600 nm and 750 nm are observed for
NdVO4 microcrystals at pH 2, 4 and 6. Moreover, the near-infrared
(NIR) upconversion spectra of NdVO4 microcrystals at pH 2, 4 and 6
has been clearly depicted in Fig. 5(b). NIR emission of 750 nm, 808 nm
and 853 nm originates from the 4I9/2 → 4F7/2,4I9/2 → 4F5/2 and 4I9/2 →
4
F7/2 of Nd3+,respectively [28,29]. The NdVO4 microcrystal with
highest upconversion luminescent intensity is obtained at pH 2.
NIR upconversion spectrum of NdVO4 microcrystals prepared at
different temperature and different time are shown in Fig. 6(a) and (b),
respectively. With reacting temperature increasing from 80 °C to 180 °C,
the intensity of NIR upconversion emission enhances. In Fig. 6(b), the
near-infrared emission intensity reaches the maximum with 24 h. With
reacting time increasing from 12 to 24 h, the intensity of NIR upcon-
version emission spectra sharply increases. With the reaction time
further increasing to 36 h, the intensity clearly decreases. The intensity
of NIR upconversion emission greatly changes with the conversion of
3D self-assembled NdVO4 microcrystal morphology. In fact, the NIR
upconversion luminescent microcrystals with reduced size come rela-
tively low luminescent efficiency owing to their low optical absorption
capability, surface fluorescence quenching effects [30,31].

3.5. Luminescent mechanism analysis

The variation of ln(intensity) versus ln(power) for all the emission
bands is shown in Fig. 7(a). The linear fittings of the experimental data
gave slopes with values at 2.76, 2.48 and 0.52 for the UC emission
bands peaking around 750 nm, 808 nm and 853 nm, respectively. It is
widely acknowledged that Ln If ∝ n Ln P, where If stands for the UC
emission intensity, P is the pumping power, and n indicates the ab-
sorbed laser photon number when emitting an UC photon [32]. In ad-
dition, non-radiation relaxation process has negative influence on the
academic photon number [33]. A conclusion is drawn that three
Fig. 5. (a), the ultraviolet absorption spectrum of NdVO4 microcrystals; (b), the
NIR up-conversion spectrum of NdVO4 microcrystals.
photons process are responsible for emission bands at 750 nm and
808 nm whereas one for 853 nm emission band. As is shown in
Fig. 7(b), the intensity of 853 nm emission band slowly enhances with
the power increasing from 0.09 W to 0.36 W. The simple 1 photon
process is in the majority at low laser power. With power further in-
creasing, the intensities of 750 nm and 808 nm emissions increase in

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Fig. 6. (a), NIR upconversion emission spectra for NdVO4 microcrystals at

different temperature. Fig. 6(b), for NdVO4 microcrystals with different re-
acting time. Fig. 7. (a), the Ln (If)-Ln(P) relationship for 750 nm, 808 nm and 853 nm
emission bands; Fig. 7(b), the intensity of upconversion emission spectra ex-
cited by 980 nm solid laser with different power.
large scale. On the contrary, the 853 nm emission band totally dis-
appears.
The vivid luminescent mechanism diagram of NIR emissions at
750 nm, 808 nm and 853 nm is performed in Fig. 8. Fig. 8 shows the
main energy level transition (ET) process of Nd3+ under 980 nm, non-
radiation relaxation progress included. Obviously, there exists a com-
petition between the ET process of 4I9/2 → 4F3/2 (853 nm) and 4I9/2 →
4
F5/2,4F7/2 (808 nm, 750 nm). Under low laser power, 4I9/2 jumps to
4
F3/2 through ET process, then generating 853 nm emission. When
power is 0.09 W, it is too low for the population of 4F5/2 and 4F7/2 state.
Besides, 4F5/2 and 4F7/2 could reduce to 4F3/2 state via non-radiation
relaxation process. With laser power increasing, it enables the electrons
population on 4F5/2 and 4F7/2 state. The 3 photons process gradually
dominates in ET process with power increasing.

4. Conclusion

In summary, 3D self-assembled NdVO4 microcrystals with uniform

sphere and stick-shape morphology were prepared by hydro-thermal
method without any organic surfactant. Self-assembled NdVO4 micro-
crystals with unusual morphology was reported for the first time. The
growth mechanism of 3D self-assembled NdVO4 microcrystals was ex-
plored, which provided a useful synthesis of crystals with specific
morphology. The relationship between optical property and mor-
phology was investigated. The route provided a simplified way to
synthesize luminescent materials which combined good optical per-
formance and uniform morphology. The NIR upconversion emission of
3D self-assembled NdVO4 microcrystals would be suitable for bio-
Fig. 8. The diagram of the ET process for Nd3+, under 980 nm solid laser.
imaging and silicon-based solar cell.
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