Optical Materials 50 (2015) 2531

Contents lists available at ScienceDirect

Optical Materials
journal homepage: www.elsevier.com/locate/optmat

Nd:YAG transparent ceramics fabricated by direct cold isostatic pressing

and vacuum sintering
Lin Ge, Jiang Li , Zhiwei Zhou, Binglong Liu, Tengfei Xie, Jing Liu, Huamin Kou, Yun Shi, Yubai Pan ,
Jingkun Guo
Key Laboratory of Transparent and Opto-functional Advanced Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, Shanghai
200050, China

a r t i c l e i n f o a b s t r a c t

Article history: The sintering behavior of neodymium doped yttrium aluminum garnet (Nd:YAG) ceramics was investi-
Received 14 January 2015 gated on the basis of densication trajectory, microstructure evolution and transmittance. Nd:YAG
Received in revised form 27 April 2015 ceramics with in-line transmittance of 83.9% at 1064 nm and 82.5% at 400 nm were obtained by direct
Accepted 4 May 2015
cold isostatic pressing (CIP) at 250 MPa and solid-state reactive sintering at 1790 C for 30 h under vac-
Available online 28 May 2015
uum. Compared with the porosity and the average pore diameter of the sample from uniaxial
dry-pressing followed by CIP, those from direct CIP are much smaller. The samples pressed at 250 MPa
Keywords:
were sintered from 1500 C to 1750 C for 0.520 h to study their sintering behavior. At the temperature
Nd:YAG ceramics
Cold isostatic pressing
higher than 1500 C, pure YAG phase is formed, followed by the densication and grain growth process.
Shrinkage The relative density and the grain size increase with the increase of sintering time and temperature, and
Densication trajectory the sintering behavior is more sensitive to temperature than holding time. The mechanism controlling
Microstructure evolution densication and grain growth at sintering temperature of 1550 C is grain boundary diffusion.
2015 Elsevier B.V. All rights reserved.

1. Introduction formation occurs during sintering [25]. The merits of the SSR pro-
cess is that commercially available powders can be used, and thus
Transparent yttrium aluminum garnet (YAG, Y3Al5O12) materi- it is easier to implement for materials requiring dopants [26].
als are the most widely used laser gain hosts in solid-state lasers Nevertheless, numerous parameters of the fabrication process
[14]. After being doped with different rare-earth ions (Nd3+, for transparent ceramics using the reactive sintering route must
Yb3+, Eu3+, Er3+, Tm3+), YAG based solid-state lasers occupy a be controlled. The choice and treatment of starting powders [27
prominent place among different kinds of elds, such as advanced 30], the category and the amount of sintering aids [26,31,32], the
laser weapon, manufactory industry and medical treatment [511]. ball milling process [33], the forming method [3444], the sinter-
Among these rare-earth ions, Nd3+ isthemost common optically ing trajectory [45,46], the post-treatment process [47,48], and
active element dopant [1216]. For a long time, it was considered characterizations of laser ceramics [4951] have been widely stud-
the Nd:YAG single crystal conventionally grown by the Czochralski ied. In terms of the forming technologies, uniaxial dry-pressing,
method to be excellent laser host material, although it has several uniaxial dry-pressing followed by cold isostatic pressing (CIP)
limitations [1719]. In recent years, Nd:YAG ceramics have [3438], tape casting [3942], gel casting [43], and slip casting
attracted much attention owing to their exible structural design- [44] are widely used for green body preparation. Among these
ing and excellent laser properties. Many potential advantages of methods, uniaxial dry-pressing followed by CIP is the most popular
laser ceramics compared to single crystals have been cited multiple one to fabricate Nd:YAG transparent ceramics. However, the
times in literatures [2024], earliest by Ikesue et al. [25]. heterogeneity caused by the uniaxial dry-pressing may lead to
The solid state reaction (SSR) and wet chemical process are the the uneven distribution of density for the green body, which may
most important methods for synthesizing YAG. Ikesue et al.s work even not be eliminated effectively by the post cold isostatic press-
demonstrates the SSR approach is a process in which Al2O3 and ing. In order to improve the uniformity of the density and obtain
Y2O3 powders are mixed in stoichiometric amounts and phase ceramics with homogeneous microstructure, direct CIP is worth
to be used due to its isotropic pressure. To the best of our knowl-
edge, no Nd:YAG ceramics obtained by direct CIP without uniaxial
Corresponding authors. Tel.: +86 21 52412816; fax: +86 21 52413903.
dry-pressing were reported before.
E-mail addresses: [email protected] (J. Li), [email protected] (Y. Pan).

http://dx.doi.org/10.1016/j.optmat.2015.05.016
0925-3467/ 2015 Elsevier B.V. All rights reserved.
26 L. Ge et al. / Optical Materials 50 (2015) 2531

Here we used high purity commercial powders as raw materi-

als, and highly transparent Nd:YAG ceramics were obtained by
direct CIP and solid-state reactive sintering under vacuum. The
pore size distribution of the green body obtained from direct CIP
and uniaxial dry-pressing followed by CIP was compared. The
inuence of different molding pressures on the relative density,
grain size and the transmittance of Nd:YAG ceramics was exam-
ined. Besides, the green bodies formed from appropriate CIP pres-
sure were chosen to investigate their densication behavior and
microstructure evolution.

2. Experimental

High purity commercial a-Al2O3 (99.98%, Alfa Aesar, USA), Y2O3

(99.999%, Alfa Aesar, USA), and Nd2O3 (99.99%, Alfa Aesar, USA)
powders were weighted with chemical compositions of
Nd0.06Y2.94Al5O12 (2.0 at.% Nd:YAG). Appropriate amount of MgO Fig. 1. Densication trajectories of Nd:YAG transparent ceramics sintered at
(>99.99%, Alfa Aesar Company, USA) and TEOS (tetraethyl orthosil- various temperatures for 2 h with CIP pressures from 50 to 300 MPa.
icate, >99.99%, Alfa Aesar Company, USA) were added as sintering
aids. These powders were mixed and milled for 10 h in the solvent
temperature higher than 1700 C, there is almost no difference in
of ethyl alcohol. After dried and sieved through a 200-mesh screen,
density for all the samples from CIP with different pressure.
the powder mixtures were calcined at 600 C for 4 h in air to
The photograph of all the sintered (1790 C  30 h) and pol-
remove the organic components.
ished Nd:YAG ceramics with the thickness of 1.5 mm is showed
The powder mixtures were put in the thin rubber bags and then
in Fig. 2, from which we can see that they are all transparent. It
sealed. Discs of 17 mm in diameter and 5 mm in thickness were
can be seen from Fig. 3 that the transmittance increases with the
prepared from the above powder mixtures by CIP without
increase of the molding pressure below 250 MPa, especially obvi-
preforming. Pressing was carried out at the pressure range of
ous at the pressure range from 100 to 150 MPa. It is well known
50300 MPa with a dwell time of 1 min. For contrast, green body
that the density of green body has relationship with the molding
dry-pressed before CIP with a uniaxial pressure of 50 MPa was
pressure. The greater pressure put on the powder, the higher den-
prepared.
sity of the green body can be achieved. The migration distance of
The obtained green bodies were vacuum-sintered at 1790 C for
the particles in the samples with high density may be reduced dur-
30 h, and then the as-sintered ceramics were annealed at 1450 C
ing sintering, which is benecial for the densication process.
for 20 h in air to eliminate the oxygen vacancies. Finally, the
When the molding pressure is increased to 250 MPa, the transmit-
ceramics were mirror-polished to 1.5 mm on both surfaces for test-
tance of ceramics reaches 83.9% at 1064 nm and 82.5% at 400 nm,
ing their optical transmittances. Furthermore, green bodies were
which are approached with the theoretical values. However,
also sintered at the temperature range from 1500 to 1750 C for
because the density of the green body pressed at 250 MPa is high
various hours to analyze the densication trajectory. In order to
enough, there is no signicant change in the transmittance for
observe the microstructure evolution, the polished samples were
the sample pressed at 300 MPa compared to that at 250 MPa.
thermally etched at 1400 C or 1450 C for 3 h.
Thus, green bodies cold isostatically pressed at 250 MPa were
The pore size distributions of the green bodies were tested by
chosen to study their sintering behavior.
mercury injection apparatus (AutoPore IV 9510, Micromeritics,
The porosity and the pore size distribution of the green body
USA). The shrinkage of the sample during sintering was measured
can reect the molding quality directly. Table 1 lists the pore char-
with a thermo optical measurement system (TOM-AC,
acteristic of the samples shaped by direct CIP at 250 MPa and CIP
Fraunhofer-Gesellschaft, Germany) operated using a heating rate
with uniaxial dry-pressing. Obviously, the porosity and the average
of 10 C/min up to 1000 C and then 5 C/min to 1800 C. The rela-
pore diameter of the sample obtained by direct CIP are much smal-
tive density of the obtained ceramics was tested and calculated by
ler. Besides, the average pore diameter is larger than the median
the Archimedes method. The phase composition of the specimen
pore diameter for the green body prepared by CIP with
was identied by X-ray diffraction (XRD, D8 ADVANCE, Bruker
dry-uniaxial pressing, which means that there are a certain
AXS, GmbH). The microstructure of the as-sintered ceramics was
amount of large pores in this sample. This phenomenon was
observed by the eld emission scanning electron microscopy
caused by the uneven distribution of density which resulted from
(FESEM, S-4800, Hitachi, Japan). Then grain size of the sample
the uniaxial pressing. And the large pores were not be eliminated
was obtained by the linear intercept method [52] (more than 300
effectively even by the post CIP.
grains counted). The in-line transmittance of the polished ceramics
In order to explore the reaction process and the densication
was detected by a UVVISNIR spectrophotometer (Cary-5000,
behavior during sintering, the change along the height direction
Varian, USA).
of the sample was tested by a thermo-optical measurement

3. Results and discussion

In order to nd out the appropriate molding pressure to obtain

Nd:YAG ceramics with high density and high optical quality, vari-
ous pressures were chosen for cold isostatic pressing. Fig. 1 shows
the densication curves of Nd:YAG ceramics sintered at different
temperatures for 2 h with CIP pressures from 50 to 300 MPa. The
relative density of the ceramics increases with the increasing of Fig. 2. Photograph of Nd:YAG transparent ceramics sintered at 1790 C for 30 h
molding pressure and the sintering temperature. At the sintering from green bodies pressed at different pressures.
 L. Ge et al. / Optical Materials 50 (2015) 2531 27

Fig. 4. Shrinkage and shrinkage rate curves of Nd:YAG ceramics.

However, no matter whether the solid reaction occurs or not, den-

sication is ongoing during the whole sintering process. That is to
say, these two competitive processes, shrinkage and expansion,
occur simultaneously during the formation of YAG. It can be seen
from Fig. 4 that the ratio of expansion caused by phase transforma-
tion is greater than that of shrinkage. The expansion process ends
at about 1460 C, and then the Nd:YAG densication stage begins
(denoted as C in Fig. 4). From these results, one has to notice that
temperature range for the phase transformations of YAM to YAP
and further to YAG is in accordance with XRD results shown in
Fig. 5.
Fig. 6 exhibits SEM micrographs of ceramics sintered at
15001750 C for 2 h from green bodies CIP at 250 MPa. The sam-
ple sintered at 1500 C shows quite an amount of open pores gath-
Fig. 3. Transmittance curves of Nd:YAG transparent ceramics sintered at 1790 C ered at grain boundaries, whose sizes are larger than those of
for 30 h from green bodies pressed at 50300 MPa (a) 2001100 nm and (b) 1064
grains. The pores were removed largely with the increasing of tem-
and 400 nm wavelength. (For interpretation of the references to colour in this gure
legend, the reader is referred to the web version of this article.) perature, especially at the temperature range of 15001650 C.
This phenomenon can be conrmed by Fig. 7. No signicant pores
are remained at 1700 C or above. Besides, grain size increases
system, as shown in Fig. 4. The formation of YAG phase from Y2O3 rapidly from 0.8 lm to 12.2 lm with increase of temperature from
and Al2O3 powder mixtures includes three successive transforma- 1500 C to 1750 C, as can be seen in Fig. 7.
tions, which has already been reported in previous studies [32]. From 1500 C to 1750 C, there are three kinds of microstruc-
The reaction equations are as follows: tures of Nd:YAG ceramics as a function of sintering temperature
and holding time. First is open porous ceramics, correspond to
2Y2 O3 Al2 O3 ! Y4 Al2 O9 YAM 1 15001600 C, relative density ranging from 75% to 97% with a
Al2 O3 Y4 Al2 O9 ! 4YAlO3 YAP 2 grain size between 1 lm and 4 lm (Figs. 6ac and 7). Another is
relatively dense ceramics, correspond to 16001650 C, relative
Al2 O3 3YAlO3 ! Y3 Al5 O12 YAG 3
density ranging from 97% to 99% (Figs. 6cd and 7). The last is fully
Transformations (1) and (2) occur at the temperature range of
9001250 C (denoted as A in Fig. 4). The shrinkage rate peak
at 1143 C corresponds to a large amount of formation of YAP.
For sintering temperatures higher than 1250 C, the rest Al2O3
reacts with the YAP phase to form YAG (denoted as B in Fig. 4).
Because the density of perovskite YAP (5.35 g/cm3) is higher than
that of garnet YAG (4.55 g/cm3), sample will expand during this
transformation without considering the shrinkage process.

Table 1
Pore characteristic of the green bodies under different molding methods.

Molding Porosity Total pore Median pore Average pore

method (%) volume (mL/ diameter diameter (nm)
g) (nm)
Direct CIP 39.5 0.1511 100.8 97.0
CIP with 40.3 0.1526 98.3 107.0
uniaxial
dry-
pressing
Fig. 5. X-ray diffraction patterns for Nd:YAG sintered at 12001500 C for 2 h.
28 L. Ge et al. / Optical Materials 50 (2015) 2531

Fig. 6. SEM micrographs of Nd:YAG ceramics sintered at (a) 1500 C, (b) 1550 C, (c) 1600 C, (d) 1650 C, (e) 1700 C and (f) 1750 C for 2 h.

Fig. 7. Inuence of different CIP pressures on the densitygrain size trajectories. Fig. 8. Relative density and grain size of Nd:YAG ceramics versus sintering time at
1550 C.
dense samples, whose grain size increases rapidly with the
increase of temperature (Figs. 6df and 7). It indicates that the nal sintered at 1550 C for various hours were studied, as can be seen
densication stage of Nd:YAG ceramics is accompanied by signi- in Figs. 8 and 9. For the sample sintered for 0.5 h, lots of pores are
cant grain growth. In addition, at the same sintering temperature, gathered at grain boundaries. With the increase of holding time,
the relative density and grain size of the sample cold isostatically the pores are removed gradually and separated by the dense
pressed at 250 MPa are larger than that at 150 MPa or 50 MPa regions, and the densication rated decreases. However, there
(Fig. 7). are still some pores existing at grain boundaries even when
Pure Nd:YAG phase is fully formed when the temperature is the holding is as long as 20 h. It can be highlighted that the densi-
increased to 1500 C (Fig. 5). Densication behavior of the samples cation behavior seems to be more sensitive to the sintering
 L. Ge et al. / Optical Materials 50 (2015) 2531 29

Fig. 9. SEM micrographs of Nd:YAG ceramics sintered at 1550 C for (a) 0.5 h, (b) 1 h, (c) 3 h, (d) 5 h, (e) 10 h and (f) 20 h.

temperature than the holding time, which is in good agreement

with the microstructures shown in Fig. 6. The grain size increases
from 0.8 to 2.4 lm with the increase of holding time from 0.5 to
20 h, as shown in Fig. 8.
To identify the mechanism controlling grain growth, it is com-
mon to use the following formula [26]:
Gn  Gn0 Kt 4
where G is the average grain size, G0 is the initial grain size, K is a
rate constant depending on the mechanism controlling grain
growth, t is the holding time, and n is an exponent characteristic
of the grain growth mechanism. A standard analysis, based on for-
mula (4) and the use of n values of 2, 3, and 4, is performed with the
experimental points. The best t of the plot yields a value of 4 for n,
as can be seen in Fig. 10. As described by Brook [53], n = 2 indicates
that solid state mass transport is the dominant mechanism for Fig. 10. Plot of G4G40 function versus holding time and the straight line ts with
coarsening, n = 3 indicates that liquid phase mass transport occurs n = 4 for Nd:YAG ceramics at 1550 C.
in the sample, and n = 4 means that boundary diffusion control
the migration process.
where D is the relative density, dD/dt is the densication rate, K0 is a
For identication the mechanism controlling densication, the
rate constant depending on the mechanism controlling densica-
following relationship is used [54]:
tion, and m is an exponent characteristic of the densication mech-
1 dD K 0 anism. When densication is controlled by volume diffusion, m
5
D dt Gm equals to 3, and when densication is controlled by grain boundary
30 L. Ge et al. / Optical Materials 50 (2015) 2531

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