Journal of Luminescence 184 (2017) 232–234

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Journal of Luminescence
journal homepage: www.elsevier.com/locate/jlumin

Full Length Article

Spectroscopic properties of neodymium-doped alumina (Nd3 þ :Al2O3)

translucent ceramics
Yan Gui, Qiuhong Yang n, Yingjie Shao, Ye Yuan
School of Materials Science and Engineering, Shanghai University, 200444, China

art ic l e i nf o a b s t r a c t

Article history: Nd2O3 doped Al2O3 translucent ceramics were fabricated using the conventional solid-state reaction and
Received 1 November 2016 vacuum sintering. The spectroscopic properties of the synthesized Nd3 þ :Al2O3 translucent ceramics
Received in revised form were analyzed and discussed. The results showed that the strong absorption peak at around 800 nm with
27 December 2016
an absorption cross section 3.25  10–20 cm2 of the Nd3 þ :Al2O3 translucent ceramics matched the
Accepted 28 December 2016
Available online 30 December 2016
emission wavelength of the commercial laser diode (LD). In addition, the synthesized translucent ceramic
had a strong emission peak at 1054 nm and the FWHM and the emission cross section of the peak of the
Keywords: material were found to be 7.53 nm and 1.38  10–19 cm2. The photoluminescence spectrum of the
Nd3 þ Nd3 þ :Al2O3 translucent ceramics exhibited the characteristic absorption and emission bands of Nd3 þ
Al2O3
ions in the host matrix.
Translucent ceramics
& 2017 Published by Elsevier B.V.
Spectroscopic properties

1. Introduction Nd:Al 2 O 3 a good possible candidate for high power laser

operation.
The Al2O3 single crystal is an excellent laser host because it has The photoluminescence of rare earth ion doped Al2O3 powders
many interesting properties, including high strength, high thermal [10,11], films [12–14] and xerogel [15] has been already extensively
conductivity, high transparency in the visible and up to the IR investigated. Recently, researchers in this field have been becom-
range; and a stable chemical composition and structure [1]. The ing interested in rare earth ion doped crystalline Al2O3 [16,17]. In
ruby (Cr3 þ :Al2O3) is the first crystal found to exhibit a laser this work, Nd3 þ :Al2O3 translucent ceramics were fabricated using
emission as demonstrated by Maiman at the Hughes Lab in 1960 a vacuum sintering method; and the spectroscopic properties of
[2,3], which established the foundation of modern laser technol- the synthesized Nd3 þ :Al2O3 translucent ceramics were in-
ogy. The wide gain and high quantum efficiency of Sapphire vestigated and discussed.
(Ti:Al2O3) is widely acknowledged as the properties that makes
this material the optimum ultrafast laser crystal [4]. However,
alumina doped with transition metal ions (Cr3 þ , Ti3 þ , etc.) cannot 2. Experimental
be pumped by LD, which is a hindrance to device miniaturization
and high efficiency. 2.1. Preparation
Nd 3 þ -doped solid-state laser hosts with a four-level system
Commercial high-purity α-Al2O3 (99.95%, Shanghai Fenghe
have a low laser power output threshold, high quantum effi-
Ceramics, co. LTD., China), with an average grain size of 0.4 μm,
ciency and a highly stimulated emission cross section [5]. In
and high purity Nd2O3 (99.99%, Shanghai Yuelong New Materials
addition, the strong absorption by Nd3 þ at about 808 nm wa-
Co. Ltd., China) were used as the starting material. These powders
velength matches the emission wavelength of the commercial
were blended together with MgO (98%) as sintering aids, in a
LD [6], which enables device reduction and high laser effi-
weight percentage of 99.4  99.9 wt% Al2O3, 0.1  0.5 wt% Nd2O3,
ciency. The most favored laser material Nd:YAG has the rela-
0.1 wt% MgO, and ball milled with high-purity zirconia balls for
tively low thermal conductivity (9  14 Wm  1 K  1 ) [7,8],
10 h in ethanol. Then the milled slurry was dried at 90 °C for 24 h
which has limited the development of the high power solid
in an oven and sieved. The powder mixture was pressed at 2 MPa
laser. Single crystal Al 2 O 3 has a much higher thermal con- into Ф15 mm pellets in a steel mold and then cold isostatically
ductivity than YAG at around 35 Wm  1 K  1 [9], which makes pressed at 200 MPa. The resulting green body sintering was con-
ducted at 1700–1750 °C for 5  15 h in a tungsten mesh-heated
n
Corresponding author. vacuum furnace under vacuum ( o1.0  10  3 Pa). The heating rate
E-mail address: [email protected] (Q. Yang). was 5 °C/min, and the cooling rate was 10 °C/min.

http://dx.doi.org/10.1016/j.jlumin.2016.12.042
0022-2313/& 2017 Published by Elsevier B.V.
 Y. Gui et al. / Journal of Luminescence 184 (2017) 232–234 233

2.2. Characterization

The sintered samples were double-side polished to  2 mm in

thickness for spectral analysis. The microstructure of the ceramics
was examined using optical microscopy (Model BX60, OLYPMUS,
Japan). The phase composition of the products was established
using powder X-ray diffraction analysis (Model D/MAX-2200, Ri-
gaku, Japan). In-line transmittance and absorption spectra were
obtained using a UV/VIS/NIR spectrometer (Model V-570, JASCO,
Japan) employing a Xe light as the pump source. The fluorescence
spectra were measured using a fluorescence spectrum analyzer
(Fluorolog-3, JobinYvonSpex, France) excited by 808 nm LD.

3. Results and discussion

Fig. 1 is the photograph of translucent Nd:Al2O3 ceramic (2 mm

thick) and as shown, printed letters are quite visible through the
ceramic disks as an indication of the translucence of the product.
Fig. 2. The in-line transmittance of Nd:Al2O3 ceramics at room temperature. The
The in-line transmittance of the Nd:Al2O3 translucent ceramics in inset is the transmittance of fused silica [19].
the range of 200 nm to 1500 nm is shown in Fig. 2, and as can be
seen it approached 20% at 1500 nm. The method used for the
synthesis of the transparent/translucent ceramics doped with rare
earth elements is also useful for preparing silicon solar cell light
convertors [18], but when the transparency of the materials fab-
ricated with this method is compared to the transmittance of
fused silica (as shown in the inset [19] of Fig. 2), it is clear that the
transparency of the alumina sample does not measure up and will
be the subject of improvement in future work. Ceramics have
various internal sites that scatter light, including residual pores,
grain boundaries, secondary phases (impurities) at the grain
boundaries and double refraction from birefringent materials [20].
These inconsistencies produce a reduction in the transmittance of
the material. Using a method to orientate the optical axes of the
grains parallel, it is possible to improve the in-line optical trans-
mission of the ceramics to around 70% [21]. This method shows
that uniaxial crystals can also produce polycrystalline ceramics
with excellent optical qualities. Fig. 3. Optical microscopic photograph of Nd:Al2O3 ceramics.
The microstructure of the synthesized Nd:Al2O3 translucent
ceramic etched at 1450 °C for 30 min is shown in Fig. 3, which
shows a few pores (black dots) concentrated at the grain bound-
aries and a small quantity of secondary phase (white dots). The
composition of the second phase was investigated using XRD
analysis. The resulting XRD pattern of 0.5 wt% Nd:Al2O3 is shown
in Fig. 4. The main phase was found to be Al2O3 (JCPDS: 05-0712),
which coexisted with a quantity of AlNd11O18 (JCPDS:48-1609). To
eliminate the secondary phase and porosity, the concentration of
the rare earth ions should be reduced, the sintering temperature
should be decreased, holding time should be reduced and che-
mical etching should be used in the further research.
The absorption spectrum of the 0.5 wt% Nd:Al2O3 translucent
ceramic at room temperature is shown in Fig. 5. Major absorption
bands ranged from 400 1000 nm were identified that were at-
tributed to the Nd3 þ ; and the five absorption peaks that corre-
sponded to the transition of the 4 f ground state electron from 4I9/2
level to different excited states after energy- absorbing are labeled
in this figure. The maximum absorption coefficient of 2.95 cm  1

Fig.4. XRD pattern of 0.5 wt% Nd:Al2O3.

was achieved at 582 nm, which corresponded to the

4
I9/2-2G7/2 þ 4G5/2 transition. There was a significant absorption
peak at around 800 nm at which the wavelength matched the
Fig. 1. Photograph of Nd:Al2O3 ceramics(2 mm thick) sintered in vacuum atmo- operating wavelength of the InGaAs LD, and the absorption cross
sphere at 1720 °C for 15 h. section sabs was calculated using the following formula [22]:
234 Y. Gui et al. / Journal of Luminescence 184 (2017) 232–234

4
F3/2-4I13/2 of Nd3 þ , as labeled in the figure. The energy level
diagram of Nd3 þ is shown in the inset of Fig. 6. The FWHM of the
peak at 1055 nm was 7.53 nm, and the emission cross section was
calculated using J-O theory to be 1.38  10–19 cm2. The Nd3 þ in-
duced emission properties indicated that Nd3 þ ions were doped
into the Al2O3.

4. Conclusion

In summary, Nd2O3 doped Al2O3 translucent ceramics have

been prepared using a solid-state reaction method and vacuum
sintering. The resulting 0.5 wt% Nd3 þ :Al2O3 consisted primarily of
a Al2O3 phase, but a small quantity of NdAl11O18 was detected with
a low equilibrium solubility of Nd3 þ in Al2O3. The spectroscopic
properties of the 0.5 wt% Nd3 þ :Al2O3 translucent ceramics were
investigated. It was found that an absorption peak at 800 nm was
Fig. 5. Absorption spectrum of 0.5 wt% Nd:Al2O3 ceramics at room temperature. presented with an absorption cross section 3.25  10–20 cm2 and
FWHM of 25.58 nm. The FWHM and the emission cross section of
the peak at 1055 nm were 7.53 nm and 1.38  10–19 cm2.

Acknowledgement

We would like to acknowledge Instrumental Analysis and Re-

search Center of Shanghai University for their kind help on XRD
measurement.

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